 
data_1
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C34 H17 N5 S2'
_chemical_formula_sum
 'C34 H17 N5 S2' 
_chemical_formula_weight          559.64

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    8.283(2)
_cell_length_b                    12.815(4)
_cell_length_c                    16.686(4)
_cell_angle_alpha                 67.954(7)
_cell_angle_beta                  78.039(6)
_cell_angle_gamma                 84.714(7)
_cell_volume                      1605.8(7)
_cell_formula_units_Z             2
_cell_measurement_temperature     123(2)
_cell_measurement_reflns_used     9489
_cell_measurement_theta_min       2.514
_cell_measurement_theta_max       27.447
 
_exptl_crystal_description        block
_exptl_crystal_colour             red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.157          
_exptl_crystal_F_000              576
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.100
_exptl_crystal_size_mid           0.080
_exptl_crystal_size_min           0.080
_exptl_absorpt_coefficient_mu     0.195
_shelx_estimated_absorpt_T_min    0.981
_shelx_estimated_absorpt_T_max    0.985
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.981
_exptl_absorpt_correction_T_max   0.985
_exptl_absorpt_process_details    'SADABS, Bruker(2000)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       123(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             9489
_diffrn_reflns_av_unetI/netI      0.0713
_diffrn_reflns_av_R_equivalents   0.0451
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          2.514
_diffrn_reflns_theta_max          24.999
_diffrn_reflns_theta_full         24.999
_diffrn_measured_fraction_theta_max   0.976
_diffrn_measured_fraction_theta_full  0.976
_diffrn_reflns_Laue_measured_fraction_max    0.976
_diffrn_reflns_Laue_measured_fraction_full   0.976
_diffrn_reflns_point_group_measured_fraction_max   0.976
_diffrn_reflns_point_group_measured_fraction_full  0.976
_reflns_number_total              5511
_reflns_number_gt                 4248
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1240P)²+1.9088P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          5511
_refine_ls_number_parameters      370
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0900
_refine_ls_R_factor_gt            0.0745
_refine_ls_wR_factor_ref          0.2263
_refine_ls_wR_factor_gt           0.2183
_refine_ls_goodness_of_fit_ref    1.086
_refine_ls_restrained_S_all       1.086
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.1546(5) 0.0164(4) -0.1045(3) 0.0276(9) Uani 1 1 d . . . . .
C2 C 0.0723(4) -0.1636(3) -0.0997(2) 0.0253(8) Uani 1 1 d . . . . .
C3 C 0.1419(5) -0.1034(3) -0.0579(3) 0.0264(8) Uani 1 1 d . . . . .
C4 C 0.1936(5) -0.1596(3) 0.0197(3) 0.0271(8) Uani 1 1 d . . . . .
H4 H 0.1773 -0.2386 0.0436 0.032 Uiso 1 1 calc R U . . .
C5 C 0.2686(4) -0.1167(3) 0.0701(3) 0.0271(8) Uani 1 1 d . . . . .
C6 C 0.3236(6) -0.1836(3) 0.1461(3) 0.0378(10) Uani 1 1 d . . . . .
H6 H 0.3190 -0.2634 0.1684 0.045 Uiso 1 1 calc R U . . .
C7 C 0.3866(6) -0.1238(3) 0.1875(3) 0.0363(10) Uani 1 1 d . . . . .
H7 H 0.4258 -0.1583 0.2413 0.044 Uiso 1 1 calc R U . . .
C8 C 0.3856(5) -0.0091(3) 0.1416(2) 0.0254(8) Uani 1 1 d . . . . .
C9 C 0.4495(4) 0.0801(3) 0.1610(2) 0.0231(8) Uani 1 1 d . . . . .
C10 C 0.4438(5) 0.1934(3) 0.1041(2) 0.0250(8) Uani 1 1 d . . . . .
H10 H 0.3958 0.2110 0.0535 0.030 Uiso 1 1 calc R U . . .
C11 C 0.5044(5) 0.2792(3) 0.1185(2) 0.0256(8) Uani 1 1 d . . . . .
H11 H 0.4998 0.3548 0.0787 0.031 Uiso 1 1 calc R U . . .
C12 C 0.5730(5) 0.2522(3) 0.1935(2) 0.0243(8) Uani 1 1 d . . . . .
C13 C 0.5781(4) 0.1397(3) 0.2532(2) 0.0216(8) Uani 1 1 d . . . . .
C14 C 0.5177(4) 0.0538(3) 0.2366(2) 0.0227(8) Uani 1 1 d . . . . .
H14 H 0.5226 -0.0220 0.2761 0.027 Uiso 1 1 calc R U . . .
C15 C 0.6491(4) 0.1424(3) 0.3242(2) 0.0228(8) Uani 1 1 d . . . . .
C16 C 0.6841(4) 0.2557(3) 0.3052(2) 0.0238(8) Uani 1 1 d . . . . .
C17 C 0.7552(5) 0.2867(3) 0.3625(2) 0.0278(9) Uani 1 1 d . . . . .
H17 H 0.7820 0.3628 0.3487 0.033 Uiso 1 1 calc R U . . .
C18 C 0.7846(5) 0.2037(3) 0.4390(2) 0.0283(9) Uani 1 1 d . . . . .
H18 H 0.8295 0.2238 0.4791 0.034 Uiso 1 1 calc R U . . .
C19 C 0.7508(4) 0.0905(3) 0.4601(2) 0.0227(8) Uani 1 1 d . . . . .
C20 C 0.6824(4) 0.0596(3) 0.4027(2) 0.0227(8) Uani 1 1 d . . . . .
H20 H 0.6585 -0.0170 0.4167 0.027 Uiso 1 1 calc R U . . .
C21 C 0.6800(5) 0.4373(3) 0.1775(2) 0.0265(8) Uani 1 1 d . . . . .
C22 C 0.7627(5) 0.4706(3) 0.0901(3) 0.0296(9) Uani 1 1 d . . . . .
H22 H 0.7874 0.4173 0.0620 0.036 Uiso 1 1 calc R U . . .
C23 C 0.8079(5) 0.5804(3) 0.0453(3) 0.0349(10) Uani 1 1 d . . . . .
H23 H 0.8633 0.6033 -0.0144 0.042 Uiso 1 1 calc R U . . .
C24 C 0.7738(6) 0.6588(3) 0.0858(3) 0.0393(11) Uani 1 1 d . . . . .
H24 H 0.8072 0.7346 0.0546 0.047 Uiso 1 1 calc R U . . .
C25 C 0.6902(6) 0.6253(4) 0.1729(3) 0.0398(11) Uani 1 1 d . . . . .
H25 H 0.6673 0.6785 0.2011 0.048 Uiso 1 1 calc R U . . .
C26 C 0.6405(5) 0.5153(3) 0.2183(3) 0.0331(9) Uani 1 1 d . . . . .
H26 H 0.5800 0.4932 0.2769 0.040 Uiso 1 1 calc R U . . .
C27 C 0.7901(4) 0.0056(3) 0.5439(2) 0.0248(8) Uani 1 1 d . . . . .
C28 C 0.8355(5) -0.1696(3) 0.6673(2) 0.0279(9) Uani 1 1 d . . . . .
C29 C 0.8757(5) -0.0748(3) 0.6771(2) 0.0292(9) Uani 1 1 d . . . . .
H29 H 0.9168 -0.0765 0.7267 0.035 Uiso 1 1 calc R U . . .
C30 C 0.8512(4) 0.0248(3) 0.6082(2) 0.0234(8) Uani 1 1 d . . . . .
H30 H 0.8739 0.0974 0.6056 0.028 Uiso 1 1 calc R U . . .
C31 C 0.8400(5) -0.2794(3) 0.7329(2) 0.0294(9) Uani 1 1 d . . . . .
H31 H 0.8758 -0.2822 0.7842 0.035 Uiso 1 1 calc R U . . .
C32 C 0.8015(5) -0.3807(4) 0.7339(3) 0.0351(10) Uani 1 1 d . . . . .
C33 C 0.7501(7) -0.3950(4) 0.6626(3) 0.0482(12) Uani 1 1 d . . . . .
C34 C 0.8047(6) -0.4791(4) 0.8101(3) 0.0456(12) Uani 1 1 d . . . . .
N1 N 0.1642(5) 0.1109(3) -0.1416(3) 0.0401(9) Uani 1 1 d . . . . .
N2 N 0.0158(4) -0.2127(3) -0.1309(2) 0.0343(8) Uani 1 1 d . . . . .
N3 N 0.6387(4) 0.3217(3) 0.2254(2) 0.0246(7) Uani 1 1 d . . . . .
N4 N 0.7107(9) -0.4081(5) 0.6034(4) 0.093(2) Uani 1 1 d . . . . .
N5 N 0.8022(6) -0.5579(4) 0.8730(3) 0.0647(13) Uani 1 1 d . . . . .
S1 S 0.29685(11) 0.02273(8) 0.05042(6) 0.0249(3) Uani 1 1 d . . . . .
S2 S 0.76699(12) -0.13528(8) 0.56854(6) 0.0281(3) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 N1 1.137(5) . ?
C1 C3 1.439(6) . ?
C2 N2 1.136(5) . ?
C2 C3 1.437(5) . ?
C3 C4 1.362(5) . ?
C4 C5 1.421(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.378(6) . ?
C5 S1 1.721(4) . ?
C6 C7 1.401(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.379(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.468(5) . ?
C8 S1 1.721(4) . ?
C9 C14 1.402(5) . ?
C9 C10 1.408(5) . ?
C10 C11 1.367(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(5) . ?
C11 H11 0.9500 . ?
C12 N3 1.392(5) . ?
C12 C13 1.414(5) . ?
C13 C14 1.388(5) . ?
C13 C15 1.441(5) . ?
C14 H14 0.9500 . ?
C15 C20 1.404(5) . ?
C15 C16 1.410(5) . ?
C16 N3 1.391(5) . ?
C16 C17 1.408(5) . ?
C17 C18 1.371(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.399(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.393(5) . ?
C19 C27 1.493(5) . ?
C20 H20 0.9500 . ?
C21 C26 1.389(6) . ?
C21 C22 1.397(6) . ?
C21 N3 1.428(5) . ?
C22 C23 1.368(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.394(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.381(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C30 1.382(5) . ?
C27 S2 1.715(4) . ?
C28 C29 1.364(6) . ?
C28 C31 1.425(5) . ?
C28 S2 1.740(4) . ?
C29 C30 1.393(5) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.358(6) . ?
C31 H31 0.9500 . ?
C32 C34 1.418(6) . ?
C32 C33 1.420(6) . ?
C33 N4 1.175(7) . ?
C34 N5 1.149(6) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N1 C1 C3 179.5(5) . . ?
N2 C2 C3 178.5(4) . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 C1 124.0(4) . . ?
C2 C3 C1 115.6(3) . . ?
C3 C4 C5 129.2(4) . . ?
C3 C4 H4 115.4 . . ?
C5 C4 H4 115.4 . . ?
C6 C5 C4 123.6(4) . . ?
C6 C5 S1 109.7(3) . . ?
C4 C5 S1 126.6(3) . . ?
C5 C6 C7 114.3(4) . . ?
C5 C6 H6 122.9 . . ?
C7 C6 H6 122.9 . . ?
C8 C7 C6 112.4(4) . . ?
C8 C7 H7 123.8 . . ?
C6 C7 H7 123.8 . . ?
C7 C8 C9 128.6(3) . . ?
C7 C8 S1 110.6(3) . . ?
C9 C8 S1 120.8(3) . . ?
C14 C9 C10 118.9(3) . . ?
C14 C9 C8 120.4(3) . . ?
C10 C9 C8 120.7(3) . . ?
C11 C10 C9 122.9(3) . . ?
C11 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
C10 C11 C12 117.9(3) . . ?
C10 C11 H11 121.1 . . ?
C12 C11 H11 121.1 . . ?
N3 C12 C11 130.0(3) . . ?
N3 C12 C13 108.9(3) . . ?
C11 C12 C13 121.0(3) . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 C15 133.3(3) . . ?
C12 C13 C15 106.6(3) . . ?
C13 C14 C9 119.3(3) . . ?
C13 C14 H14 120.4 . . ?
C9 C14 H14 120.4 . . ?
C20 C15 C16 119.2(3) . . ?
C20 C15 C13 133.6(3) . . ?
C16 C15 C13 107.2(3) . . ?
N3 C16 C17 130.0(3) . . ?
N3 C16 C15 108.8(3) . . ?
C17 C16 C15 121.2(3) . . ?
C18 C17 C16 117.9(4) . . ?
C18 C17 H17 121.0 . . ?
C16 C17 H17 121.0 . . ?
C17 C18 C19 122.3(4) . . ?
C17 C18 H18 118.8 . . ?
C19 C18 H18 118.8 . . ?
C20 C19 C18 119.7(3) . . ?
C20 C19 C27 121.7(3) . . ?
C18 C19 C27 118.6(3) . . ?
C19 C20 C15 119.6(3) . . ?
C19 C20 H20 120.2 . . ?
C15 C20 H20 120.2 . . ?
C26 C21 C22 120.4(4) . . ?
C26 C21 N3 120.0(4) . . ?
C22 C21 N3 119.5(3) . . ?
C23 C22 C21 119.6(4) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C24 120.8(4) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C25 119.5(4) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C26 C25 C24 120.4(4) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 119.3(4) . . ?
C25 C26 H26 120.3 . . ?
C21 C26 H26 120.3 . . ?
C30 C27 C19 127.8(4) . . ?
C30 C27 S2 111.7(3) . . ?
C19 C27 S2 120.5(3) . . ?
C29 C28 C31 123.3(3) . . ?
C29 C28 S2 110.5(3) . . ?
C31 C28 S2 126.1(3) . . ?
C28 C29 C30 114.2(3) . . ?
C28 C29 H29 122.9 . . ?
C30 C29 H29 122.9 . . ?
C27 C30 C29 112.2(3) . . ?
C27 C30 H30 123.9 . . ?
C29 C30 H30 123.9 . . ?
C32 C31 C28 130.4(4) . . ?
C32 C31 H31 114.8 . . ?
C28 C31 H31 114.8 . . ?
C31 C32 C34 120.3(4) . . ?
C31 C32 C33 123.6(4) . . ?
C34 C32 C33 116.1(4) . . ?
N4 C33 C32 178.6(7) . . ?
N5 C34 C32 177.8(6) . . ?
C16 N3 C12 108.6(3) . . ?
C16 N3 C21 124.9(3) . . ?
C12 N3 C21 125.7(3) . . ?
C5 S1 C8 92.89(18) . . ?
C27 S2 C28 91.43(19) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C2 C3 C4 C5 178.3(4) . . . . ?
C1 C3 C4 C5 -0.4(7) . . . . ?
C3 C4 C5 C6 -176.5(4) . . . . ?
C3 C4 C5 S1 6.6(6) . . . . ?
C4 C5 C6 C7 -177.2(4) . . . . ?
S1 C5 C6 C7 0.1(5) . . . . ?
C5 C6 C7 C8 -2.0(6) . . . . ?
C6 C7 C8 C9 -176.3(4) . . . . ?
C6 C7 C8 S1 3.0(5) . . . . ?
C7 C8 C9 C14 -2.5(6) . . . . ?
S1 C8 C9 C14 178.3(3) . . . . ?
C7 C8 C9 C10 177.3(4) . . . . ?
S1 C8 C9 C10 -1.9(5) . . . . ?
C14 C9 C10 C11 1.0(6) . . . . ?
C8 C9 C10 C11 -178.8(3) . . . . ?
C9 C10 C11 C12 -0.6(6) . . . . ?
C10 C11 C12 N3 -178.0(4) . . . . ?
C10 C11 C12 C13 -0.7(5) . . . . ?
N3 C12 C13 C14 179.3(3) . . . . ?
C11 C12 C13 C14 1.5(5) . . . . ?
N3 C12 C13 C15 0.4(4) . . . . ?
C11 C12 C13 C15 -177.5(3) . . . . ?
C12 C13 C14 C9 -1.0(5) . . . . ?
C15 C13 C14 C9 177.6(4) . . . . ?
C10 C9 C14 C13 -0.2(5) . . . . ?
C8 C9 C14 C13 179.6(3) . . . . ?
C14 C13 C15 C20 -0.4(7) . . . . ?
C12 C13 C15 C20 178.3(4) . . . . ?
C14 C13 C15 C16 -178.7(4) . . . . ?
C12 C13 C15 C16 0.1(4) . . . . ?
C20 C15 C16 N3 -179.1(3) . . . . ?
C13 C15 C16 N3 -0.5(4) . . . . ?
C20 C15 C16 C17 1.5(5) . . . . ?
C13 C15 C16 C17 -179.9(3) . . . . ?
N3 C16 C17 C18 178.6(4) . . . . ?
C15 C16 C17 C18 -2.1(6) . . . . ?
C16 C17 C18 C19 1.8(6) . . . . ?
C17 C18 C19 C20 -1.0(6) . . . . ?
C17 C18 C19 C27 178.7(3) . . . . ?
C18 C19 C20 C15 0.4(5) . . . . ?
C27 C19 C20 C15 -179.4(3) . . . . ?
C16 C15 C20 C19 -0.6(5) . . . . ?
C13 C15 C20 C19 -178.7(4) . . . . ?
C26 C21 C22 C23 1.3(6) . . . . ?
N3 C21 C22 C23 -177.5(3) . . . . ?
C21 C22 C23 C24 0.6(6) . . . . ?
C22 C23 C24 C25 -1.0(6) . . . . ?
C23 C24 C25 C26 -0.4(6) . . . . ?
C24 C25 C26 C21 2.3(6) . . . . ?
C22 C21 C26 C25 -2.8(6) . . . . ?
N3 C21 C26 C25 176.1(3) . . . . ?
C20 C19 C27 C30 -177.1(3) . . . . ?
C18 C19 C27 C30 3.2(6) . . . . ?
C20 C19 C27 S2 5.1(5) . . . . ?
C18 C19 C27 S2 -174.6(3) . . . . ?
C31 C28 C29 C30 -175.4(4) . . . . ?
S2 C28 C29 C30 0.7(4) . . . . ?
C19 C27 C30 C29 -179.0(3) . . . . ?
S2 C27 C30 C29 -1.1(4) . . . . ?
C28 C29 C30 C27 0.2(5) . . . . ?
C29 C28 C31 C32 178.7(4) . . . . ?
S2 C28 C31 C32 3.2(6) . . . . ?
C28 C31 C32 C34 -175.6(4) . . . . ?
C28 C31 C32 C33 1.8(7) . . . . ?
C17 C16 N3 C12 -179.9(4) . . . . ?
C15 C16 N3 C12 0.8(4) . . . . ?
C17 C16 N3 C21 10.3(6) . . . . ?
C15 C16 N3 C21 -169.1(3) . . . . ?
C11 C12 N3 C16 176.9(4) . . . . ?
C13 C12 N3 C16 -0.7(4) . . . . ?
C11 C12 N3 C21 -13.4(6) . . . . ?
C13 C12 N3 C21 169.0(3) . . . . ?
C26 C21 N3 C16 -54.4(5) . . . . ?
C22 C21 N3 C16 124.5(4) . . . . ?
C26 C21 N3 C12 137.5(4) . . . . ?
C22 C21 N3 C12 -43.7(5) . . . . ?
C6 C5 S1 C8 1.3(3) . . . . ?
C4 C5 S1 C8 178.6(4) . . . . ?
C7 C8 S1 C5 -2.5(3) . . . . ?
C9 C8 S1 C5 176.9(3) . . . . ?
C30 C27 S2 C28 1.2(3) . . . . ?
C19 C27 S2 C28 179.4(3) . . . . ?
C29 C28 S2 C27 -1.1(3) . . . . ?
C31 C28 S2 C27 174.9(4) . . . . ?
 
_refine_diff_density_max    0.755
_refine_diff_density_min   -0.452
_refine_diff_density_rms    0.090



#===END

 

data_2
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C45 H27 Cl3 N4 S' 
_chemical_formula_weight          762.11

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    10.649(10)
_cell_length_b                    11.826(11)
_cell_length_c                    17.306(16)
_cell_angle_alpha                 109.939(14)
_cell_angle_beta                  100.431(15)
_cell_angle_gamma                 92.727(14)
_cell_volume                      2001(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     291(2)
_cell_measurement_reflns_used     7011
_cell_measurement_theta_min       2.527
_cell_measurement_theta_max       20.086
 
_exptl_crystal_description        block
_exptl_crystal_colour             red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.265          
_exptl_crystal_F_000              784
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.120
_exptl_crystal_size_mid           0.120
_exptl_crystal_size_min           0.120
_exptl_absorpt_coefficient_mu     0.318
_shelx_estimated_absorpt_T_min    0.963
_shelx_estimated_absorpt_T_max    0.963
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.963
_exptl_absorpt_correction_T_max   0.963
_exptl_absorpt_process_details    'SADABS, Bruker(2000)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       291(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type    'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             10873
_diffrn_reflns_av_unetI/netI      0.0866
_diffrn_reflns_av_R_equivalents   0.0408
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.280
_diffrn_reflns_theta_max          25.000
_diffrn_reflns_theta_full         25.000
_diffrn_measured_fraction_theta_max   0.993
_diffrn_measured_fraction_theta_full  0.993
_diffrn_reflns_Laue_measured_fraction_max    0.993
_diffrn_reflns_Laue_measured_fraction_full   0.993
_diffrn_reflns_point_group_measured_fraction_max   0.993
_diffrn_reflns_point_group_measured_fraction_full  0.993
_reflns_number_total              7011
_reflns_number_gt                 3339
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1019P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          7011
_refine_ls_number_parameters      478
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1322
_refine_ls_R_factor_gt            0.0651
_refine_ls_wR_factor_ref          0.1956
_refine_ls_wR_factor_gt           0.1668
_refine_ls_goodness_of_fit_ref    0.904
_refine_ls_restrained_S_all       0.904
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C -0.4212(4) 0.1737(4) 0.5331(3) 0.0704(11) Uani 1 1 d . . . . .
C2 C -0.5264(5) 0.1919(5) 0.5706(3) 0.0939(14) Uani 1 1 d . . . . .
H2 H -0.5163 0.2186 0.6287 0.113 Uiso 1 1 calc R U . . .
C3 C -0.6468(4) 0.1692(5) 0.5188(4) 0.1015(16) Uani 1 1 d . . . . .
H3 H -0.7192 0.1790 0.5424 0.122 Uiso 1 1 calc R U . . .
C4 C -0.6618(5) 0.1321(5) 0.4321(4) 0.1058(17) Uani 1 1 d . . . . .
H4 H -0.7435 0.1228 0.3989 0.127 Uiso 1 1 calc R U . . .
C5 C -0.5581(5) 0.1089(4) 0.3945(3) 0.0881(14) Uani 1 1 d . . . . .
H5 H -0.5695 0.0793 0.3363 0.106 Uiso 1 1 calc R U . . .
C6 C -0.4350(4) 0.1305(3) 0.4454(3) 0.0708(11) Uani 1 1 d . . . . .
C7 C -0.3084(4) 0.1150(3) 0.4271(3) 0.0685(11) Uani 1 1 d . . . . .
C8 C -0.2631(6) 0.0703(4) 0.3527(3) 0.0891(14) Uani 1 1 d . . . . .
H8 H -0.3206 0.0433 0.3010 0.107 Uiso 1 1 calc R U . . .
C9 C -0.1337(6) 0.0666(5) 0.3560(3) 0.0975(15) Uani 1 1 d . . . . .
H9 H -0.1032 0.0375 0.3067 0.117 Uiso 1 1 calc R U . . .
C10 C -0.0479(5) 0.1065(4) 0.4340(3) 0.0950(15) Uani 1 1 d . . . . .
H10 H 0.0395 0.1038 0.4350 0.114 Uiso 1 1 calc R U . . .
C11 C -0.0878(4) 0.1503(4) 0.5100(3) 0.0827(13) Uani 1 1 d . . . . .
H11 H -0.0295 0.1767 0.5614 0.099 Uiso 1 1 calc R U . . .
C12 C -0.2206(4) 0.1522(4) 0.5048(2) 0.0679(10) Uani 1 1 d . . . . .
C13 C -0.2349(4) 0.2280(3) 0.6575(2) 0.0610(10) Uani 1 1 d . . . . .
C14 C -0.1444(4) 0.1653(4) 0.6882(2) 0.0645(10) Uani 1 1 d . . . . .
H14 H -0.1166 0.0989 0.6511 0.077 Uiso 1 1 calc R U . . .
C15 C -0.0948(4) 0.2004(3) 0.7736(2) 0.0634(10) Uani 1 1 d . . . . .
H15 H -0.0329 0.1575 0.7926 0.076 Uiso 1 1 calc R U . . .
C16 C -0.1350(3) 0.2989(3) 0.8327(2) 0.0537(9) Uani 1 1 d . . . . .
C17 C -0.2258(3) 0.3630(3) 0.7995(2) 0.0567(9) Uani 1 1 d . . . . .
H17 H -0.2549 0.4290 0.8362 0.068 Uiso 1 1 calc R U . . .
C18 C -0.2719(4) 0.3301(3) 0.7146(2) 0.0643(10) Uani 1 1 d . . . . .
H18 H -0.3286 0.3762 0.6947 0.077 Uiso 1 1 calc R U . . .
C19 C -0.0900(3) 0.3277(3) 0.9240(2) 0.0513(8) Uani 1 1 d . . . . .
C20 C 0.0310(3) 0.3008(3) 0.9554(2) 0.0535(9) Uani 1 1 d . . . . .
H20 H 0.0869 0.2718 0.9196 0.064 Uiso 1 1 calc R U . . .
C21 C 0.0675(3) 0.3175(3) 1.0403(2) 0.0510(8) Uani 1 1 d . . . . .
C22 C -0.0165(3) 0.3622(3) 1.0952(2) 0.0515(9) Uani 1 1 d . . . . .
C23 C -0.1373(3) 0.3906(3) 1.0650(2) 0.0585(9) Uani 1 1 d . . . . .
H23 H -0.1930 0.4206 1.1008 0.070 Uiso 1 1 calc R U . . .
C24 C -0.1711(3) 0.3729(3) 0.9809(2) 0.0571(9) Uani 1 1 d . . . . .
H24 H -0.2513 0.3916 0.9605 0.068 Uiso 1 1 calc R U . . .
C25 C 0.1827(3) 0.2957(3) 1.0901(2) 0.0510(8) Uani 1 1 d . . . . .
C26 C 0.2978(3) 0.2532(3) 1.0718(2) 0.0562(9) Uani 1 1 d . . . . .
H26 H 0.3112 0.2321 1.0173 0.067 Uiso 1 1 calc R U . . .
C27 C 0.3934(3) 0.2423(3) 1.1355(2) 0.0573(9) Uani 1 1 d . . . . .
C28 C 0.3687(4) 0.2752(4) 1.2166(3) 0.0691(11) Uani 1 1 d . . . . .
H28 H 0.4319 0.2684 1.2590 0.083 Uiso 1 1 calc R U . . .
C29 C 0.2560(4) 0.3171(4) 1.2373(3) 0.0699(11) Uani 1 1 d . . . . .
H29 H 0.2431 0.3382 1.2919 0.084 Uiso 1 1 calc R U . . .
C30 C 0.1619(4) 0.3265(3) 1.1724(2) 0.0581(9) Uani 1 1 d . . . . .
C31 C -0.0118(4) 0.4098(4) 1.2490(2) 0.0612(10) Uani 1 1 d . . . . .
C32 C -0.0210(4) 0.3379(4) 1.2983(3) 0.0817(12) Uani 1 1 d . . . . .
H32 H 0.0056 0.2610 1.2826 0.098 Uiso 1 1 calc R U . . .
C33 C -0.0699(5) 0.3826(6) 1.3702(3) 0.1028(16) Uani 1 1 d . . . . .
H33 H -0.0746 0.3356 1.4033 0.123 Uiso 1 1 calc R U . . .
C34 C -0.1115(5) 0.4945(6) 1.3935(3) 0.1004(16) Uani 1 1 d . . . . .
H34 H -0.1446 0.5234 1.4418 0.121 Uiso 1 1 calc R U . . .
C35 C -0.1037(5) 0.5638(5) 1.3445(3) 0.0988(15) Uani 1 1 d . . . . .
H35 H -0.1325 0.6398 1.3601 0.119 Uiso 1 1 calc R U . . .
C36 C -0.0539(4) 0.5233(4) 1.2725(3) 0.0818(12) Uani 1 1 d . . . . .
H36 H -0.0489 0.5717 1.2403 0.098 Uiso 1 1 calc R U . . .
C37 C 0.5153(3) 0.1984(3) 1.1182(2) 0.0623(10) Uani 1 1 d . . . . .
C38 C 0.6159(4) 0.1791(5) 1.1731(3) 0.0882(14) Uani 1 1 d . . . . .
H38 H 0.6164 0.1948 1.2296 0.106 Uiso 1 1 calc R U . . .
C39 C 0.7169(4) 0.1335(4) 1.1349(3) 0.0839(13) Uani 1 1 d . . . . .
H39 H 0.7915 0.1165 1.1640 0.101 Uiso 1 1 calc R U . . .
C40 C 0.6966(3) 0.1159(3) 1.0509(3) 0.0652(10) Uani 1 1 d . . . . .
C41 C 0.7849(4) 0.0691(3) 0.9983(3) 0.0659(10) Uani 1 1 d . . . . .
H41 H 0.8596 0.0490 1.0252 0.079 Uiso 1 1 calc R U . . .
C42 C 0.7780(4) 0.0491(3) 0.9159(3) 0.0641(10) Uani 1 1 d . . . . .
C43 C 0.8814(4) -0.0011(4) 0.8770(3) 0.0739(12) Uani 1 1 d . . . . .
C44 C 0.6714(4) 0.0739(4) 0.8627(3) 0.0705(11) Uani 1 1 d . . . . .
C45 C 0.4145(5) 0.3337(5) 0.8218(4) 0.1014(16) Uani 1 1 d . . . . .
H45 H 0.4877 0.2874 0.8126 0.122 Uiso 1 1 calc R U . . .
Cl1 Cl 0.4102(3) 0.3785(3) 0.92487(16) 0.2119(12) Uani 1 1 d . . . . .
Cl2 Cl 0.43377(16) 0.45515(15) 0.79059(13) 0.1398(7) Uani 1 1 d . . . . .
Cl3 Cl 0.2745(2) 0.23973(19) 0.7622(2) 0.2120(12) Uani 1 1 d . . . . .
N1 N -0.2882(3) 0.1901(3) 0.5698(2) 0.0698(9) Uani 1 1 d . . . . .
N2 N 0.0409(3) 0.3669(3) 1.17534(18) 0.0567(8) Uani 1 1 d . . . . .
N3 N 0.9658(4) -0.0391(3) 0.8470(3) 0.0909(12) Uani 1 1 d . . . . .
N4 N 0.5857(4) 0.0952(4) 0.8208(2) 0.0930(12) Uani 1 1 d . . . . .
S1 S 0.54854(9) 0.16049(9) 1.01948(7) 0.0647(3) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C2 1.383(6) . ?
C1 C6 1.403(6) . ?
C1 N1 1.418(5) . ?
C2 C3 1.381(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.388(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.446(6) . ?
C7 C8 1.398(6) . ?
C7 C12 1.407(5) . ?
C8 C9 1.372(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.398(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.392(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.403(6) . ?
C11 H11 0.9300 . ?
C12 N1 1.401(5) . ?
C13 C14 1.383(5) . ?
C13 C18 1.401(5) . ?
C13 N1 1.423(5) . ?
C14 C15 1.383(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.407(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.415(5) . ?
C16 C19 1.478(5) . ?
C17 C18 1.372(5) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.400(5) . ?
C19 C24 1.413(5) . ?
C20 C21 1.391(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.410(5) . ?
C21 C25 1.454(5) . ?
C22 N2 1.393(4) . ?
C22 C23 1.399(5) . ?
C23 C24 1.374(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.395(5) . ?
C25 C30 1.406(5) . ?
C26 C27 1.404(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.402(5) . ?
C27 C37 1.463(5) . ?
C28 C29 1.380(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.402(5) . ?
C29 H29 0.9300 . ?
C30 N2 1.399(5) . ?
C31 C36 1.386(6) . ?
C31 C32 1.405(6) . ?
C31 N2 1.429(5) . ?
C32 C33 1.383(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.366(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.375(7) . ?
C34 H34 0.9300 . ?
C35 C36 1.386(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C38 1.380(5) . ?
C37 S1 1.720(4) . ?
C38 C39 1.398(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.371(6) . ?
C39 H39 0.9300 . ?
C40 C41 1.427(6) . ?
C40 S1 1.738(4) . ?
C41 C42 1.350(6) . ?
C41 H41 0.9300 . ?
C42 C44 1.436(6) . ?
C42 C43 1.441(6) . ?
C43 N3 1.152(5) . ?
C44 N4 1.153(5) . ?
C45 Cl1 1.689(6) . ?
C45 Cl2 1.714(5) . ?
C45 Cl3 1.739(6) . ?
C45 H45 0.9800 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C2 C1 C6 121.8(4) . . ?
C2 C1 N1 130.1(4) . . ?
C6 C1 N1 108.1(4) . . ?
C3 C2 C1 117.7(5) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C2 C3 C4 121.2(5) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 121.1(5) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 118.9(5) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C5 C6 C1 119.2(4) . . ?
C5 C6 C7 133.0(4) . . ?
C1 C6 C7 107.8(4) . . ?
C8 C7 C12 119.4(4) . . ?
C8 C7 C6 133.7(4) . . ?
C12 C7 C6 106.8(4) . . ?
C9 C8 C7 119.9(5) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 119.8(5) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 122.8(5) . . ?
C11 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
C10 C11 C12 116.3(4) . . ?
C10 C11 H11 121.9 . . ?
C12 C11 H11 121.9 . . ?
C11 C12 N1 129.1(4) . . ?
C11 C12 C7 121.9(4) . . ?
N1 C12 C7 109.1(4) . . ?
C14 C13 C18 118.4(3) . . ?
C14 C13 N1 120.7(4) . . ?
C18 C13 N1 120.9(3) . . ?
C15 C14 C13 120.8(4) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 122.0(3) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 H15 119.0 . . ?
C15 C16 C17 116.1(3) . . ?
C15 C16 C19 121.1(3) . . ?
C17 C16 C19 122.7(3) . . ?
C18 C17 C16 121.6(3) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C13 121.0(3) . . ?
C17 C18 H18 119.5 . . ?
C13 C18 H18 119.5 . . ?
C20 C19 C24 118.0(3) . . ?
C20 C19 C16 120.5(3) . . ?
C24 C19 C16 121.3(3) . . ?
C21 C20 C19 120.0(3) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.4(3) . . ?
C20 C21 C25 132.6(3) . . ?
C22 C21 C25 107.0(3) . . ?
N2 C22 C23 130.5(3) . . ?
N2 C22 C21 109.0(3) . . ?
C23 C22 C21 120.5(3) . . ?
C24 C23 C22 118.0(3) . . ?
C24 C23 H23 121.0 . . ?
C22 C23 H23 121.0 . . ?
C23 C24 C19 123.2(3) . . ?
C23 C24 H24 118.4 . . ?
C19 C24 H24 118.4 . . ?
C26 C25 C30 119.9(3) . . ?
C26 C25 C21 133.8(3) . . ?
C30 C25 C21 106.3(3) . . ?
C25 C26 C27 120.2(3) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C28 C27 C26 117.8(3) . . ?
C28 C27 C37 120.8(3) . . ?
C26 C27 C37 121.5(3) . . ?
C29 C28 C27 123.9(4) . . ?
C29 C28 H28 118.1 . . ?
C27 C28 H28 118.1 . . ?
C28 C29 C30 117.2(4) . . ?
C28 C29 H29 121.4 . . ?
C30 C29 H29 121.4 . . ?
N2 C30 C29 129.4(4) . . ?
N2 C30 C25 109.4(3) . . ?
C29 C30 C25 121.1(3) . . ?
C36 C31 C32 119.5(4) . . ?
C36 C31 N2 119.9(4) . . ?
C32 C31 N2 120.6(4) . . ?
C33 C32 C31 119.4(5) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C34 C33 C32 121.3(5) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C33 C34 C35 119.1(5) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C34 C35 C36 121.6(5) . . ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C31 C36 C35 119.2(4) . . ?
C31 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C38 C37 C27 128.1(4) . . ?
C38 C37 S1 110.5(3) . . ?
C27 C37 S1 121.4(3) . . ?
C37 C38 C39 113.0(4) . . ?
C37 C38 H38 123.5 . . ?
C39 C38 H38 123.5 . . ?
C40 C39 C38 114.3(4) . . ?
C40 C39 H39 122.8 . . ?
C38 C39 H39 122.8 . . ?
C39 C40 C41 124.6(4) . . ?
C39 C40 S1 109.6(3) . . ?
C41 C40 S1 125.8(3) . . ?
C42 C41 C40 130.7(4) . . ?
C42 C41 H41 114.6 . . ?
C40 C41 H41 114.6 . . ?
C41 C42 C44 123.7(4) . . ?
C41 C42 C43 119.7(4) . . ?
C44 C42 C43 116.6(4) . . ?
N3 C43 C42 178.6(5) . . ?
N4 C44 C42 179.2(5) . . ?
Cl1 C45 Cl2 111.5(3) . . ?
Cl1 C45 Cl3 109.7(3) . . ?
Cl2 C45 Cl3 110.4(3) . . ?
Cl1 C45 H45 108.4 . . ?
Cl2 C45 H45 108.4 . . ?
Cl3 C45 H45 108.4 . . ?
C12 N1 C1 108.1(3) . . ?
C12 N1 C13 126.3(3) . . ?
C1 N1 C13 125.4(3) . . ?
C22 N2 C30 108.3(3) . . ?
C22 N2 C31 126.3(3) . . ?
C30 N2 C31 125.4(3) . . ?
C37 S1 C40 92.6(2) . . ?
 
_refine_diff_density_max    0.387
_refine_diff_density_min   -0.316
_refine_diff_density_rms    0.047



#===END
 
data_3
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C44 H26 N4 S'
_chemical_formula_sum
 'C44 H26 N4 S' 
_chemical_formula_weight          642.75

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    10.498(4)
_cell_length_b                    11.830(4)
_cell_length_c                    18.204(6)
_cell_angle_alpha                 105.686(6)
_cell_angle_beta                  91.636(7)
_cell_angle_gamma                 93.649(6)
_cell_volume                      2169.7(13)
_cell_formula_units_Z             2
_cell_measurement_temperature     291(2)
_cell_measurement_reflns_used     15805
_cell_measurement_theta_min       2.220
_cell_measurement_theta_max       27.759
 
_exptl_crystal_description        block
_exptl_crystal_colour             red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     0.984          
_exptl_crystal_F_000              668
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.10
_exptl_absorpt_coefficient_mu     0.104
_shelx_estimated_absorpt_T_min    0.988
_shelx_estimated_absorpt_T_max    0.990
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.988
_exptl_absorpt_correction_T_max   0.990
_exptl_absorpt_process_details    'SADABS, Bruker(2000)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       291(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             15805
_diffrn_reflns_av_unetI/netI      0.2506
_diffrn_reflns_av_R_equivalents   0.0996
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          1.946
_diffrn_reflns_theta_max          24.999
_diffrn_reflns_theta_full         24.999
_diffrn_measured_fraction_theta_max   0.987
_diffrn_measured_fraction_theta_full  0.987
_diffrn_reflns_Laue_measured_fraction_max    0.987
_diffrn_reflns_Laue_measured_fraction_full   0.987
_diffrn_reflns_point_group_measured_fraction_max   0.987
_diffrn_reflns_point_group_measured_fraction_full  0.987
_reflns_number_total              7550
_reflns_number_gt                 2500
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0542P)²+0.2800P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          7550
_refine_ls_number_parameters      442
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.2039
_refine_ls_R_factor_gt            0.0925
_refine_ls_wR_factor_ref          0.2149
_refine_ls_wR_factor_gt           0.1893
_refine_ls_goodness_of_fit_ref    0.972
_refine_ls_restrained_S_all       0.972
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
S1 S 1.04664(13) 0.15681(12) 1.02184(9) 0.0567(5) Uani 1 1 d . . . . .
N3 N 0.4958(4) 0.3086(3) 1.1793(3) 0.0503(12) Uani 1 1 d . . . . .
N4 N 0.3497(4) 0.3759(4) 0.6570(3) 0.0642(13) Uani 1 1 d . . . . .
C12 C 0.6204(5) 0.2701(4) 1.1725(3) 0.0455(14) Uani 1 1 d . . . . .
C10 C 0.8227(5) 0.2154(4) 1.2053(3) 0.0585(15) Uani 1 1 d . . . . .
H10 H 0.8797 0.2015 1.2415 0.070 Uiso 1 1 calc R U . . .
C16 C 0.4544(5) 0.3276(4) 1.1094(3) 0.0433(13) Uani 1 1 d . . . . .
C20 C 0.5372(4) 0.3135(4) 0.9848(3) 0.0509(14) Uani 1 1 d . . . . .
H20 H 0.6034 0.2985 0.9514 0.061 Uiso 1 1 calc R U . . .
C17 C 0.3398(5) 0.3656(4) 1.0887(3) 0.0491(14) Uani 1 1 d . . . . .
H17 H 0.2747 0.3824 1.1227 0.059 Uiso 1 1 calc R U . . .
C15 C 0.5525(5) 0.2996(4) 1.0582(3) 0.0456(13) Uani 1 1 d . . . . .
C27 C 0.4000(4) 0.3591(4) 0.8838(3) 0.0453(13) Uani 1 1 d . . . . .
C30 C 0.3531(5) 0.3798(5) 0.7350(3) 0.0542(15) Uani 1 1 d . . . . .
C33 C 0.4913(5) 0.2472(5) 0.6750(3) 0.0580(15) Uani 1 1 d . . . . .
C19 C 0.4220(4) 0.3502(4) 0.9611(3) 0.0475(14) Uani 1 1 d . . . . .
C8 C 0.9883(5) 0.1640(4) 1.1115(3) 0.0537(15) Uani 1 1 d . . . . .
C11 C 0.7012(5) 0.2464(4) 1.2269(3) 0.0561(15) Uani 1 1 d . . . . .
H11 H 0.6751 0.2511 1.2759 0.067 Uiso 1 1 calc R U . . .
C18 C 0.3268(5) 0.3775(4) 1.0159(3) 0.0507(14) Uani 1 1 d . . . . .
H18 H 0.2514 0.4050 1.0017 0.061 Uiso 1 1 calc R U . . .
C9 C 0.8621(5) 0.2044(4) 1.1322(3) 0.0499(14) Uani 1 1 d . . . . .
C3 C 1.3058(5) 0.0734(4) 0.9229(4) 0.0600(17) Uani 1 1 d . . . . .
C13 C 0.6551(5) 0.2644(4) 1.0986(3) 0.0444(13) Uani 1 1 d . . . . .
C4 C 1.2873(5) 0.0659(4) 0.9957(4) 0.0596(16) Uani 1 1 d . . . . .
H4 H 1.3530 0.0336 1.0167 0.072 Uiso 1 1 calc R U . . .
C24 C 0.2764(6) 0.3566(7) 1.3754(4) 0.088(2) Uani 1 1 d . . . . .
H24 H 0.2270 0.3673 1.4180 0.105 Uiso 1 1 calc R U . . .
C28 C 0.3109(5) 0.4360(4) 0.8666(4) 0.0540(15) Uani 1 1 d . . . . .
H28 H 0.2671 0.4814 0.9064 0.065 Uiso 1 1 calc R U . . .
C31 C 0.4402(5) 0.3012(4) 0.7471(3) 0.0538(15) Uani 1 1 d . . . . .
C25 C 0.3310(6) 0.2508(6) 1.3458(4) 0.0796(19) Uani 1 1 d . . . . .
H25 H 0.3207 0.1906 1.3696 0.096 Uiso 1 1 calc R U . . .
N2 N 1.5189(5) 0.0169(4) 0.8591(3) 0.0830(17) Uani 1 1 d . . . . .
C6 C 1.1861(6) 0.0837(5) 1.1168(4) 0.0724(18) Uani 1 1 d . . . . .
H6 H 1.2513 0.0520 1.1386 0.087 Uiso 1 1 calc R U . . .
N1 N 1.1346(5) 0.1369(5) 0.8384(3) 0.0882(18) Uani 1 1 d . . . . .
C23 C 0.2971(6) 0.4454(6) 1.3403(4) 0.084(2) Uani 1 1 d . . . . .
H23 H 0.2617 0.5168 1.3603 0.100 Uiso 1 1 calc R U . . .
C26 C 0.4013(5) 0.2350(5) 1.2803(3) 0.0634(16) Uani 1 1 d . . . . .
H26 H 0.4344 0.1627 1.2596 0.076 Uiso 1 1 calc R U . . .
C29 C 0.2868(5) 0.4461(4) 0.7940(3) 0.0580(15) Uani 1 1 d . . . . .
H29 H 0.2273 0.4962 0.7849 0.070 Uiso 1 1 calc R U . . .
C14 C 0.7799(5) 0.2320(4) 1.0788(3) 0.0507(14) Uani 1 1 d . . . . .
H14 H 0.8072 0.2291 1.0302 0.061 Uiso 1 1 calc R U . . .
C7 C 1.0747(5) 0.1229(5) 1.1540(4) 0.0706(18) Uani 1 1 d . . . . .
H7 H 1.0607 0.1209 1.2038 0.085 Uiso 1 1 calc R U . . .
C1 C 1.2114(6) 0.1098(5) 0.8765(4) 0.0632(17) Uani 1 1 d . . . . .
C32 C 0.4633(5) 0.2920(4) 0.8210(3) 0.0554(15) Uani 1 1 d . . . . .
H32 H 0.5218 0.2403 0.8291 0.066 Uiso 1 1 calc R U . . .
C22 C 0.3690(5) 0.4317(5) 1.2759(3) 0.0684(17) Uani 1 1 d . . . . .
H22 H 0.3812 0.4930 1.2533 0.082 Uiso 1 1 calc R U . . .
C5 C 1.1868(5) 0.0984(4) 1.0437(4) 0.0536(15) Uani 1 1 d . . . . .
C34 C 0.4332(6) 0.2951(5) 0.6221(3) 0.0670(17) Uani 1 1 d . . . . .
C35 C 0.4606(7) 0.2569(6) 0.5438(4) 0.085(2) Uani 1 1 d . . . . .
H35 H 0.4218 0.2888 0.5082 0.102 Uiso 1 1 calc R U . . .
C38 C 0.5801(6) 0.1626(5) 0.6510(4) 0.0774(19) Uani 1 1 d . . . . .
H38 H 0.6224 0.1313 0.6858 0.093 Uiso 1 1 calc R U . . .
C21 C 0.4230(5) 0.3242(5) 1.2454(3) 0.0538(15) Uani 1 1 d . . . . .
C37 C 0.6028(7) 0.1266(6) 0.5730(5) 0.096(2) Uani 1 1 d . . . . .
H37 H 0.6599 0.0692 0.5561 0.115 Uiso 1 1 calc R U . . .
C36 C 0.5454(8) 0.1720(6) 0.5216(4) 0.098(2) Uani 1 1 d . . . . .
H36 H 0.5635 0.1454 0.4703 0.118 Uiso 1 1 calc R U . . .
C2 C 1.4235(6) 0.0403(4) 0.8854(4) 0.0634(17) Uani 1 1 d . . . . .
C40 C 0.3438(7) 0.5218(5) 0.5851(4) 0.0779(19) Uani 1 1 d . . . . .
H40 H 0.4314 0.5191 0.5791 0.093 Uiso 1 1 calc R U . . .
C39 C 0.2819(6) 0.4524(5) 0.6236(3) 0.0628(16) Uani 1 1 d . . . . .
C41 C 0.2744(9) 0.5969(7) 0.5546(4) 0.094(2) Uani 1 1 d . . . . .
H41 H 0.3177 0.6435 0.5282 0.113 Uiso 1 1 calc R U . . .
C42 C 0.1505(11) 0.6050(8) 0.5616(5) 0.119(3) Uani 1 1 d . . . . .
H42 H 0.1076 0.6560 0.5406 0.143 Uiso 1 1 calc R U . . .
C43 C 0.0845(8) 0.5354(8) 0.6013(5) 0.121(3) Uani 1 1 d . . . . .
H43 H -0.0024 0.5418 0.6084 0.145 Uiso 1 1 calc R U . . .
C44 C 0.1508(7) 0.4547(6) 0.6309(4) 0.092(2) Uani 1 1 d . . . . .
H44 H 0.1071 0.4045 0.6547 0.110 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
S1 C8 1.743(5) . ?
S1 C5 1.745(5) . ?
N3 C12 1.411(6) . ?
N3 C16 1.412(6) . ?
N3 C21 1.418(6) . ?
N4 C34 1.376(7) . ?
N4 C30 1.407(7) . ?
N4 C39 1.433(7) . ?
C12 C11 1.382(7) . ?
C12 C13 1.389(6) . ?
C10 C9 1.380(7) . ?
C10 C11 1.389(7) . ?
C10 H10 0.9300 . ?
C16 C17 1.388(6) . ?
C16 C15 1.404(6) . ?
C20 C15 1.396(7) . ?
C20 C19 1.405(6) . ?
C20 H20 0.9300 . ?
C17 C18 1.374(7) . ?
C17 H17 0.9300 . ?
C15 C13 1.433(6) . ?
C27 C32 1.414(7) . ?
C27 C28 1.430(6) . ?
C27 C19 1.452(7) . ?
C30 C29 1.382(7) . ?
C30 C31 1.399(7) . ?
C33 C34 1.389(7) . ?
C33 C38 1.402(7) . ?
C33 C31 1.431(7) . ?
C19 C18 1.423(7) . ?
C8 C7 1.369(7) . ?
C8 C9 1.462(6) . ?
C11 H11 0.9300 . ?
C18 H18 0.9300 . ?
C9 C14 1.398(7) . ?
C3 C4 1.371(7) . ?
C3 C1 1.444(8) . ?
C3 C2 1.453(8) . ?
C13 C14 1.418(6) . ?
C4 C5 1.395(7) . ?
C4 H4 0.9300 . ?
C24 C23 1.380(8) . ?
C24 C25 1.389(8) . ?
C24 H24 0.9300 . ?
C28 C29 1.377(7) . ?
C28 H28 0.9300 . ?
C31 C32 1.394(7) . ?
C25 C26 1.397(8) . ?
C25 H25 0.9300 . ?
N2 C2 1.140(6) . ?
C6 C5 1.387(7) . ?
C6 C7 1.410(7) . ?
C6 H6 0.9300 . ?
N1 C1 1.164(7) . ?
C23 C22 1.390(8) . ?
C23 H23 0.9300 . ?
C26 C21 1.382(7) . ?
C26 H26 0.9300 . ?
C29 H29 0.9300 . ?
C14 H14 0.9300 . ?
C7 H7 0.9300 . ?
C32 H32 0.9300 . ?
C22 C21 1.405(7) . ?
C22 H22 0.9300 . ?
C34 C35 1.417(8) . ?
C35 C36 1.372(8) . ?
C35 H35 0.9300 . ?
C38 C37 1.400(8) . ?
C38 H38 0.9300 . ?
C37 C36 1.344(9) . ?
C37 H37 0.9300 . ?
C36 H36 0.9300 . ?
C40 C39 1.362(8) . ?
C40 C41 1.398(9) . ?
C40 H40 0.9300 . ?
C39 C44 1.388(8) . ?
C41 C42 1.318(10) . ?
C41 H41 0.9300 . ?
C42 C43 1.398(10) . ?
C42 H42 0.9300 . ?
C43 C44 1.424(9) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C8 S1 C5 92.1(3) . . ?
C12 N3 C16 108.9(4) . . ?
C12 N3 C21 125.6(5) . . ?
C16 N3 C21 125.5(4) . . ?
C34 N4 C30 107.3(5) . . ?
C34 N4 C39 127.3(5) . . ?
C30 N4 C39 125.0(5) . . ?
C11 C12 C13 123.3(5) . . ?
C11 C12 N3 129.5(5) . . ?
C13 C12 N3 107.1(4) . . ?
C9 C10 C11 122.3(5) . . ?
C9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C17 C16 C15 122.0(5) . . ?
C17 C16 N3 130.1(4) . . ?
C15 C16 N3 107.9(4) . . ?
C15 C20 C19 120.3(5) . . ?
C15 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C18 C17 C16 117.2(5) . . ?
C18 C17 H17 121.4 . . ?
C16 C17 H17 121.4 . . ?
C20 C15 C16 119.6(5) . . ?
C20 C15 C13 133.6(5) . . ?
C16 C15 C13 106.7(5) . . ?
C32 C27 C28 115.9(5) . . ?
C32 C27 C19 122.6(4) . . ?
C28 C27 C19 121.6(5) . . ?
C29 C30 C31 121.7(6) . . ?
C29 C30 N4 130.0(5) . . ?
C31 C30 N4 108.3(5) . . ?
C34 C33 C38 119.7(5) . . ?
C34 C33 C31 106.2(5) . . ?
C38 C33 C31 134.1(6) . . ?
C20 C19 C18 117.2(5) . . ?
C20 C19 C27 121.7(4) . . ?
C18 C19 C27 121.1(5) . . ?
C7 C8 C9 128.4(5) . . ?
C7 C8 S1 109.8(4) . . ?
C9 C8 S1 121.8(4) . . ?
C12 C11 C10 117.4(5) . . ?
C12 C11 H11 121.3 . . ?
C10 C11 H11 121.3 . . ?
C17 C18 C19 123.7(5) . . ?
C17 C18 H18 118.2 . . ?
C19 C18 H18 118.2 . . ?
C10 C9 C14 119.2(5) . . ?
C10 C9 C8 119.8(5) . . ?
C14 C9 C8 120.9(5) . . ?
C4 C3 C1 124.1(5) . . ?
C4 C3 C2 121.3(5) . . ?
C1 C3 C2 114.6(6) . . ?
C12 C13 C14 117.6(5) . . ?
C12 C13 C15 109.3(4) . . ?
C14 C13 C15 133.0(5) . . ?
C3 C4 C5 131.0(6) . . ?
C3 C4 H4 114.5 . . ?
C5 C4 H4 114.5 . . ?
C23 C24 C25 118.6(6) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
C29 C28 C27 123.2(5) . . ?
C29 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
C32 C31 C30 119.1(5) . . ?
C32 C31 C33 133.3(5) . . ?
C30 C31 C33 107.6(5) . . ?
C24 C25 C26 119.8(6) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C5 C6 C7 111.8(5) . . ?
C5 C6 H6 124.1 . . ?
C7 C6 H6 124.1 . . ?
C24 C23 C22 122.1(6) . . ?
C24 C23 H23 118.9 . . ?
C22 C23 H23 118.9 . . ?
C21 C26 C25 121.6(6) . . ?
C21 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C28 C29 C30 118.4(5) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C9 C14 C13 120.1(5) . . ?
C9 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C8 C7 C6 115.3(6) . . ?
C8 C7 H7 122.3 . . ?
C6 C7 H7 122.3 . . ?
N1 C1 C3 178.7(6) . . ?
C31 C32 C27 121.7(5) . . ?
C31 C32 H32 119.2 . . ?
C27 C32 H32 119.2 . . ?
C23 C22 C21 119.4(6) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C6 C5 C4 122.3(5) . . ?
C6 C5 S1 111.0(4) . . ?
C4 C5 S1 126.7(5) . . ?
N4 C34 C33 110.5(5) . . ?
N4 C34 C35 129.0(6) . . ?
C33 C34 C35 120.4(6) . . ?
C36 C35 C34 118.7(7) . . ?
C36 C35 H35 120.6 . . ?
C34 C35 H35 120.6 . . ?
C37 C38 C33 117.8(6) . . ?
C37 C38 H38 121.1 . . ?
C33 C38 H38 121.1 . . ?
C26 C21 C22 118.4(5) . . ?
C26 C21 N3 121.6(5) . . ?
C22 C21 N3 120.0(5) . . ?
C36 C37 C38 122.6(7) . . ?
C36 C37 H37 118.7 . . ?
C38 C37 H37 118.7 . . ?
C37 C36 C35 120.8(7) . . ?
C37 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
N2 C2 C3 176.8(7) . . ?
C39 C40 C41 119.3(7) . . ?
C39 C40 H40 120.3 . . ?
C41 C40 H40 120.3 . . ?
C40 C39 C44 120.2(6) . . ?
C40 C39 N4 121.2(6) . . ?
C44 C39 N4 118.7(6) . . ?
C42 C41 C40 123.1(8) . . ?
C42 C41 H41 118.5 . . ?
C40 C41 H41 118.5 . . ?
C41 C42 C43 118.9(8) . . ?
C41 C42 H42 120.6 . . ?
C43 C42 H42 120.6 . . ?
C42 C43 C44 119.8(8) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C39 C44 C43 118.7(7) . . ?
C39 C44 H44 120.7 . . ?
C43 C44 H44 120.7 . . ?
 
_refine_diff_density_max    0.252
_refine_diff_density_min   -0.255
_refine_diff_density_rms    0.063




#===END



