

data_a

 

_audit_creation_method            SHELXL-97

_chemical_name_systematic

;

 ?

;

_chemical_name_common             ?

_chemical_melting_point           ?

_chemical_formula_moiety          ?

_chemical_formula_sum

 'C28 H30 Ce2 N4 O21 S'

_chemical_formula_weight          1070.86

 

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'

 'O'  'O'   0.0106   0.0060

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

 'Ce'  'Ce'  -0.2486   2.6331

 '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'

 

_symmetry_cell_setting            Triclinic

_symmetry_space_group_name_H-M    P-1

 

loop_

 _symmetry_equiv_pos_as_xyz

 'x, y, z'

 '-x, -y, -z'

 

_cell_length_a                    11.236(9)

_cell_length_b                    13.323(10)

_cell_length_c                    13.544(10)

_cell_angle_alpha                 67.549(11)

_cell_angle_beta                  66.568(11)

_cell_angle_gamma                 80.281(12)

_cell_volume                      1719(2)

_cell_formula_units_Z             2

_cell_measurement_temperature     296(2)

_cell_measurement_reflns_used     2420

_cell_measurement_theta_min       2.79

_cell_measurement_theta_max       26.38

 

_exptl_crystal_description        block

_exptl_crystal_colour             yellow

_exptl_crystal_size_max           0.18

_exptl_crystal_size_mid           0.16

_exptl_crystal_size_min           0.14

_exptl_crystal_density_meas       ?

_exptl_crystal_density_diffrn     2.069

_exptl_crystal_density_method     'not measured'

_exptl_crystal_F_000              1052

_exptl_absorpt_coefficient_mu     2.773

_exptl_absorpt_correction_type    multi-scan

_exptl_absorpt_correction_T_min   0.6352

_exptl_absorpt_correction_T_max   0.6975

_exptl_absorpt_process_details    sadabs

 

_exptl_special_details

;

 ?

;

 

_diffrn_ambient_temperature       296(2)

_diffrn_radiation_wavelength      0.71073

_diffrn_radiation_type            MoK\a

_diffrn_radiation_source          'fine-focus sealed tube'

_diffrn_radiation_monochromator   graphite

_diffrn_measurement_device_type   'Bruker APEX-II CCD'

_diffrn_measurement_method        'φ and ω scans'

_diffrn_detector_area_resol_mean  ?

_diffrn_standards_number          0

_diffrn_standards_interval_count  0

_diffrn_standards_interval_time   0

_diffrn_standards_decay_%         0

_diffrn_reflns_number             8363

_diffrn_reflns_av_R_equivalents   0.0444

_diffrn_reflns_av_sigmaI/netI     0.0901

_diffrn_reflns_limit_h_min        -12

_diffrn_reflns_limit_h_max        13

_diffrn_reflns_limit_k_min        -15

_diffrn_reflns_limit_k_max        15

_diffrn_reflns_limit_l_min        -10

_diffrn_reflns_limit_l_max        16

_diffrn_reflns_theta_min          1.65

_diffrn_reflns_theta_max          25.00

_reflns_number_total              5933

_reflns_number_gt                 4177

_reflns_threshold_expression      >2sigma(I)

 

_computing_data_collection        'Bruker APEX2'

_computing_cell_refinement        'Bruker SAINT'

_computing_data_reduction         'Bruker SAINT'

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics     'Bruker SHELXTL'

_computing_publication_material   'Bruker SHELXTL'

 

_refine_special_details

;

 Refinement of F² against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F², conventional R-factors R are based

 on F, with F set to zero for negative F². The threshold expression of

 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F² are statistically about twice as large as those based on F, and R-

 factors based on ALL data will be even larger.

;

 

_refine_ls_structure_factor_coef  Fsqd

_refine_ls_matrix_type            full

_refine_ls_weighting_scheme       calc

_refine_ls_weighting_details

 'calc w=1/[σ²(Fo²)+(0.1255P)²+0.0000P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary      direct

_atom_sites_solution_secondary    difmap

_atom_sites_solution_hydrogens    geom

_refine_ls_hydrogen_treatment     constr

_refine_ls_extinction_method      none

_refine_ls_extinction_coef        ?

_refine_ls_number_reflns          5933

_refine_ls_number_parameters      505

_refine_ls_number_restraints      0

_refine_ls_R_factor_all           0.1077

_refine_ls_R_factor_gt            0.0594

_refine_ls_wR_factor_ref          0.1939

_refine_ls_wR_factor_gt           0.1574

_refine_ls_goodness_of_fit_ref    1.042

_refine_ls_restrained_S_all       1.042

_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_symmetry_multiplicity

 _atom_site_calc_flag

 _atom_site_refinement_flags

 _atom_site_disorder_assembly

 _atom_site_disorder_group

Ce1 Ce 0.56570(6) 0.25261(5) 0.63163(5) 0.0260(2) Uani 1 1 d . . .

Ce2 Ce 1.20661(5) 0.41492(4) 0.31475(4) 0.0226(2) Uani 1 1 d . . .

S1 S 1.3097(3) 0.1693(2) 0.4097(2) 0.0366(7) Uani 1 1 d . . .

O1 O 0.7308(8) 0.1790(8) 0.9170(7) 0.052(2) Uani 1 1 d . . .

O2 O 0.6930(8) 0.2363(7) 0.7545(6) 0.042(2) Uani 1 1 d . . .

O3 O 0.4249(8) 0.3739(6) 0.5192(6) 0.0355(18) Uani 1 1 d . . .

O4 O 0.2407(8) 0.4031(6) 0.4854(6) 0.041(2) Uani 1 1 d . . .

O5 O 0.7703(8) 0.3485(7) 0.4991(7) 0.042(2) Uani 1 1 d . . .

O6 O 0.9732(7) 0.3759(6) 0.4562(6) 0.0311(17) Uani 1 1 d . . .

O7 O 1.4147(7) 0.5091(6) 0.2022(6) 0.0294(17) Uani 1 1 d . . .

O8 O 1.5671(8) 0.6069(7) 0.0452(6) 0.040(2) Uani 1 1 d . . .

O9 O 1.1750(7) 0.2125(6) 0.4257(7) 0.0394(19) Uani 1 1 d . . .

O10 O 1.3902(8) 0.2664(6) 0.3488(7) 0.0396(19) Uani 1 1 d . . .

O11 O 1.3231(10) 0.1121(8) 0.5181(8) 0.065(3) Uani 1 1 d . . .

O12 O 1.3421(9) 0.1002(8) 0.3399(8) 0.063(3) Uani 1 1 d . . .

N1 N 0.4529(8) 0.1796(7) 0.8606(7) 0.028(2) Uani 1 1 d . . .

N2 N 0.3089(8) 0.2456(7) 0.7319(7) 0.026(2) Uani 1 1 d . . .

N3 N 1.0086(8) 0.4804(7) 0.2387(7) 0.0253(19) Uani 1 1 d . . .

N4 N 1.2465(9) 0.5578(6) 0.1021(6) 0.026(2) Uani 1 1 d . . .

C1 C 0.6609(11) 0.1926(8) 0.8619(9) 0.031(2) Uani 1 1 d . . .

C2 C 0.5236(10) 0.1580(8) 0.9265(9) 0.030(2) Uani 1 1 d . . .

C3 C 0.4700(12) 0.1087(10) 1.0455(9) 0.038(3) Uani 1 1 d . . .

H3A H 0.5207 0.0958 1.0894 0.046 Uiso 1 1 calc R . .

C4 C 0.3466(12) 0.0803(9) 1.0962(9) 0.038(3) Uani 1 1 d . . .

H4A H 0.3111 0.0472 1.1755 0.046 Uiso 1 1 calc R . .

C5 C 0.2682(10) 0.0999(9) 1.0300(9) 0.034(3) Uani 1 1 d . . .

C6 C 0.3248(10) 0.1519(8) 0.9139(8) 0.027(2) Uani 1 1 d . . .

C7 C 0.1342(13) 0.0705(10) 1.0770(10) 0.051(4) Uani 1 1 d . . .

H7A H 0.0962 0.0296 1.1544 0.061 Uiso 1 1 calc R . .

C8 C 0.0632(12) 0.1020(10) 1.0092(10) 0.040(3) Uani 1 1 d . . .

H8A H -0.0235 0.0829 1.0412 0.048 Uiso 1 1 calc R . .

C9 C 0.1162(10) 0.1618(9) 0.8938(9) 0.033(3) Uani 1 1 d . . .

C10 C 0.2472(10) 0.1863(9) 0.8435(8) 0.029(2) Uani 1 1 d . . .

C11 C 0.0455(12) 0.2028(11) 0.8204(11) 0.045(3) Uani 1 1 d . . .

H11A H -0.0418 0.1866 0.8487 0.054 Uiso 1 1 calc R . .

C12 C 0.1045(11) 0.2669(10) 0.7065(10) 0.040(3) Uani 1 1 d . . .

H12A H 0.0574 0.2949 0.6584 0.048 Uiso 1 1 calc R . .

C13 C 0.2375(11) 0.2886(8) 0.6653(9) 0.032(3) Uani 1 1 d . . .

C14 C 0.3061(10) 0.3595(9) 0.5463(9) 0.028(2) Uani 1 1 d . . .

C15 C 0.8783(10) 0.3835(9) 0.4322(9) 0.027(2) Uani 1 1 d . . .

C16 C 0.8912(11) 0.4497(8) 0.3081(9) 0.028(2) Uani 1 1 d . . .

C17 C 0.7804(11) 0.4763(9) 0.2766(9) 0.034(3) Uani 1 1 d . . .

H17A H 0.6989 0.4502 0.3289 0.041 Uiso 1 1 calc R . .

C18 C 0.7986(10) 0.5413(9) 0.1667(10) 0.033(3) Uani 1 1 d . . .

H18A H 0.7287 0.5617 0.1423 0.040 Uiso 1 1 calc R . .

C19 C 0.9239(12) 0.5775(8) 0.0898(9) 0.037(3) Uani 1 1 d . . .

C20 C 1.0275(11) 0.5479(8) 0.1286(8) 0.028(2) Uani 1 1 d . . .

C21 C 0.9532(12) 0.6483(9) -0.0294(9) 0.036(3) Uani 1 1 d . . .

H21A H 0.8865 0.6699 -0.0578 0.043 Uiso 1 1 calc R . .

C22 C 1.0718(12) 0.6827(9) -0.0984(9) 0.034(3) Uani 1 1 d . . .

H22A H 1.0870 0.7263 -0.1745 0.041 Uiso 1 1 calc R . .

C23 C 1.1776(11) 0.6543(8) -0.0582(8) 0.027(2) Uani 1 1 d . . .

C24 C 1.1517(9) 0.5864(8) 0.0569(8) 0.021(2) Uani 1 1 d . . .

C25 C 1.3017(12) 0.6881(9) -0.1239(8) 0.036(3) Uani 1 1 d . . .

H25A H 1.3218 0.7303 -0.2010 0.044 Uiso 1 1 calc R . .

C26 C 1.3962(11) 0.6620(9) -0.0801(9) 0.034(3) Uani 1 1 d . . .

H26A H 1.4803 0.6858 -0.1263 0.041 Uiso 1 1 calc R . .

C27 C 1.3654(10) 0.5982(8) 0.0367(9) 0.027(2) Uani 1 1 d . . .

C28 C 1.4570(9) 0.5701(9) 0.0963(9) 0.024(2) Uani 1 1 d . . .

O1W O 0.4684(9) 0.0702(8) 0.6752(9) 0.067(3) Uani 1 1 d . . .

H1W H 0.4074 0.0297 0.7296 0.100 Uiso 1 1 d R . .

H2W H 0.5158 0.0136 0.6731 0.100 Uiso 1 1 d R . .

O2W O 0.5169(7) 0.4267(6) 0.6615(6) 0.0366(19) Uani 1 1 d . . .

H3W H 0.5339 0.4888 0.6089 0.055 Uiso 1 1 d R . .

H4W H 0.5414 0.4400 0.7070 0.055 Uiso 1 1 d R . .

O3W O 0.6020(8) 0.2314(7) 0.4407(7) 0.048(2) Uani 1 1 d . . .

H5W H 0.6554 0.1786 0.4508 0.072 Uiso 1 1 d R . .

H6W H 0.5275 0.2044 0.4677 0.072 Uiso 1 1 d R . .

O4W O 0.7360(10) 0.1060(7) 0.6050(9) 0.063(3) Uani 1 1 d . . .

H7W H 0.6842 0.0533 0.6386 0.095 Uiso 1 1 d R . .

H8W H 0.7615 0.1225 0.5328 0.095 Uiso 1 1 d R . .

O5W O 1.1444(7) 0.5946(6) 0.3345(6) 0.0318(17) Uani 1 1 d . . .

H9W H 1.0895 0.5910 0.4006 0.048 Uiso 1 1 d R . .

H10W H 1.2013 0.6430 0.2910 0.048 Uiso 1 1 d R . .

O6W O 1.2578(8) 0.3176(6) 0.1717(6) 0.0355(18) Uani 1 1 d . . .

H11W H 1.3242 0.3541 0.1215 0.053 Uiso 1 1 d R . .

H12W H 1.2800 0.2597 0.2165 0.053 Uiso 1 1 d R . .

O7W O 0.2692(12) 0.9381(10) 0.8529(11) 0.094(4) Uani 1 1 d . . .

H13W H 0.2248 0.8928 0.9169 0.142 Uiso 1 1 d R . .

H14W H 0.2571 0.9290 0.7988 0.142 Uiso 1 1 d R . .

O8W O 0.9565(10) 0.1192(10) 0.6312(11) 0.090(4) Uani 1 1 d . . .

H15W H 0.8876 0.1500 0.6639 0.136 Uiso 1 1 d R . .

H16W H 1.0213 0.1470 0.5708 0.136 Uiso 1 1 d R . .

O9W O 0.7744(12) 0.0927(9) 0.3344(10) 0.086(4) Uani 1 1 d . . .

H17W H 0.7227 0.0408 0.3804 0.129 Uiso 1 1 d R . .

H18W H 0.8225 0.1015 0.3654 0.129 Uiso 1 1 d R . .

 


 

_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

Ce1 O2W 2.441(7) . ?

Ce1 O5 2.469(9) . ?

Ce1 O4W 2.517(8) . ?

Ce1 O2 2.525(7) . ?

Ce1 O3 2.570(7) . ?

Ce1 O3W 2.571(7) . ?

Ce1 O1W 2.596(10) . ?

Ce1 N2 2.656(9) . ?

Ce1 N1 2.676(8) . ?

Ce2 O4 2.434(7) 1_655 ?

Ce2 O7 2.462(8) . ?

Ce2 O5W 2.463(7) . ?

Ce2 O9 2.542(8) . ?

Ce2 O6 2.554(8) . ?

Ce2 O6W 2.559(7) . ?

Ce2 O10 2.658(7) . ?

Ce2 N4 2.683(8) . ?

Ce2 N3 2.693(7) . ?

Ce2 S1 3.224(3) . ?

S1 O11 1.429(9) . ?

S1 O12 1.466(9) . ?

S1 O10 1.469(9) . ?

S1 O9 1.486(8) . ?

O1 C1 1.234(12) . ?

O2 C1 1.261(13) . ?

O3 C14 1.263(13) . ?

O4 C14 1.237(11) . ?

O4 Ce2 2.434(7) 1_455 ?

O5 C15 1.227(13) . ?

O6 C15 1.211(12) . ?

O7 C28 1.281(12) . ?

O8 C28 1.230(13) . ?

N1 C2 1.341(12) . ?

N1 C6 1.371(14) . ?

N2 C13 1.345(12) . ?

N2 C10 1.352(13) . ?

N3 C16 1.302(14) . ?

N3 C20 1.366(12) . ?

N4 C27 1.340(13) . ?

N4 C24 1.363(12) . ?

C1 C2 1.489(16) . ?

C2 C3 1.395(15) . ?

C3 C4 1.326(17) . ?

C3 H3A 0.9300 . ?

C4 C5 1.420(15) . ?

C4 H4A 0.9300 . ?

C5 C6 1.371(14) . ?

C5 C7 1.439(18) . ?

C6 C10 1.440(13) . ?

C7 C8 1.354(17) . ?

C7 H7A 0.9300 . ?

C8 C9 1.379(16) . ?

C8 H8A 0.9300 . ?

C9 C10 1.390(15) . ?

C9 C11 1.409(15) . ?

C11 C12 1.386(18) . ?

C11 H11A 0.9300 . ?

C12 C13 1.411(16) . ?

C12 H12A 0.9300 . ?

C13 C14 1.476(15) . ?

C15 C16 1.529(14) . ?

C16 C17 1.420(14) . ?

C17 C18 1.357(15) . ?

C17 H17A 0.9300 . ?

C18 C19 1.407(17) . ?

C18 H18A 0.9300 . ?

C19 C20 1.400(14) . ?

C19 C21 1.457(15) . ?

C20 C24 1.392(15) . ?

C21 C22 1.323(17) . ?

C21 H21A 0.9300 . ?

C22 C23 1.434(14) . ?

C22 H22A 0.9300 . ?

C23 C25 1.364(16) . ?

C23 C24 1.409(14) . ?

C25 C26 1.348(15) . ?

C25 H25A 0.9300 . ?

C26 C27 1.408(14) . ?

C26 H26A 0.9300 . ?

C27 C28 1.466(13) . ?

O1W H1W 0.8500 . ?

O1W H2W 0.8500 . ?

O2W H3W 0.8499 . ?

O2W H4W 0.8501 . ?

O3W H5W 0.8500 . ?

O3W H6W 0.8500 . ?

O4W H7W 0.8499 . ?

O4W H8W 0.8500 . ?

O5W H9W 0.8500 . ?

O5W H10W 0.8500 . ?

O6W H11W 0.8501 . ?

O6W H12W 0.8500 . ?

O7W H13W 0.8500 . ?

O7W H14W 0.8500 . ?

O8W H15W 0.8500 . ?

O8W H16W 0.8500 . ?

O9W H17W 0.8500 . ?

O9W H18W 0.8500 . ?

 

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

O2W Ce1 O5 79.2(3) . . ?

O2W Ce1 O4W 145.0(3) . . ?

O5 Ce1 O4W 74.4(3) . . ?

O2W Ce1 O2 78.1(3) . . ?

O5 Ce1 O2 74.1(3) . . ?

O4W Ce1 O2 72.9(3) . . ?

O2W Ce1 O3 69.4(2) . . ?

O5 Ce1 O3 96.0(3) . . ?

O4W Ce1 O3 135.4(3) . . ?

O2 Ce1 O3 147.3(3) . . ?

O2W Ce1 O3W 123.3(2) . . ?

O5 Ce1 O3W 76.6(3) . . ?

O4W Ce1 O3W 72.2(3) . . ?

O2 Ce1 O3W 139.1(3) . . ?

O3 Ce1 O3W 63.3(2) . . ?

O2W Ce1 O1W 144.5(3) . . ?

O5 Ce1 O1W 135.6(3) . . ?

O4W Ce1 O1W 67.3(3) . . ?

O2 Ce1 O1W 113.2(3) . . ?

O3 Ce1 O1W 95.8(3) . . ?

O3W Ce1 O1W 71.1(3) . . ?

O2W Ce1 N2 79.1(3) . . ?

O5 Ce1 N2 152.6(3) . . ?

O4W Ce1 N2 131.8(3) . . ?

O2 Ce1 N2 117.3(3) . . ?

O3 Ce1 N2 60.4(2) . . ?

O3W Ce1 N2 101.8(3) . . ?

O1W Ce1 N2 65.7(3) . . ?

O2W Ce1 N1 81.2(3) . . ?

O5 Ce1 N1 132.4(3) . . ?

O4W Ce1 N1 100.1(3) . . ?

O2 Ce1 N1 59.5(3) . . ?

O3 Ce1 N1 116.6(2) . . ?

O3W Ce1 N1 148.0(3) . . ?

O1W Ce1 N1 77.2(3) . . ?

N2 Ce1 N1 59.6(2) . . ?

O4 Ce2 O7 87.0(3) 1_655 . ?

O4 Ce2 O5W 74.1(2) 1_655 . ?

O7 Ce2 O5W 78.9(2) . . ?

O4 Ce2 O9 80.4(3) 1_655 . ?

O7 Ce2 O9 126.7(2) . . ?

O5W Ce2 O9 142.8(2) . . ?

O4 Ce2 O6 82.2(3) 1_655 . ?

O7 Ce2 O6 159.1(2) . . ?

O5W Ce2 O6 80.9(2) . . ?

O9 Ce2 O6 69.0(2) . . ?

O4 Ce2 O6W 142.6(2) 1_655 . ?

O7 Ce2 O6W 90.4(2) . . ?

O5W Ce2 O6W 141.7(2) . . ?

O9 Ce2 O6W 71.5(2) . . ?

O6 Ce2 O6W 109.0(2) . . ?

O4 Ce2 O10 70.3(2) 1_655 . ?

O7 Ce2 O10 73.6(3) . . ?

O5W Ce2 O10 135.6(2) . . ?

O9 Ce2 O10 53.3(2) . . ?

O6 Ce2 O10 118.6(2) . . ?

O6W Ce2 O10 73.2(2) . . ?

O4 Ce2 N4 138.0(3) 1_655 . ?

O7 Ce2 N4 60.7(2) . . ?

O5W Ce2 N4 73.8(2) . . ?

O9 Ce2 N4 139.8(2) . . ?

O6 Ce2 N4 118.4(2) . . ?

O6W Ce2 N4 68.9(2) . . ?

O10 Ce2 N4 118.7(2) . . ?

O4 Ce2 N3 134.9(2) 1_655 . ?

O7 Ce2 N3 119.6(2) . . ?

O5W Ce2 N3 76.4(2) . . ?

O9 Ce2 N3 105.0(3) . . ?

O6 Ce2 N3 60.0(2) . . ?

O6W Ce2 N3 77.4(2) . . ?

O10 Ce2 N3 147.9(2) . . ?

N4 Ce2 N3 59.8(3) . . ?

O4 Ce2 S1 75.35(18) 1_655 . ?

O7 Ce2 S1 100.07(17) . . ?

O5W Ce2 S1 149.45(16) . . ?

O9 Ce2 S1 26.67(18) . . ?

O6 Ce2 S1 94.42(17) . . ?

O6W Ce2 S1 68.41(17) . . ?

O10 Ce2 S1 26.78(19) . . ?

N4 Ce2 S1 132.59(17) . . ?

N3 Ce2 S1 127.2(2) . . ?

O11 S1 O12 112.1(6) . . ?

O11 S1 O10 109.5(5) . . ?

O12 S1 O10 111.2(5) . . ?

O11 S1 O9 110.6(6) . . ?

O12 S1 O9 108.7(5) . . ?

O10 S1 O9 104.5(5) . . ?

O11 S1 Ce2 128.5(4) . . ?

O12 S1 Ce2 119.3(4) . . ?

O10 S1 Ce2 54.6(3) . . ?

O9 S1 Ce2 50.2(3) . . ?

C1 O2 Ce1 129.0(8) . . ?

C14 O3 Ce1 124.6(6) . . ?

C14 O4 Ce2 144.9(6) . 1_455 ?

C15 O5 Ce1 171.9(7) . . ?

C15 O6 Ce2 126.4(7) . . ?

C28 O7 Ce2 128.3(6) . . ?

S1 O9 Ce2 103.2(4) . . ?

S1 O10 Ce2 98.6(4) . . ?

C2 N1 C6 117.9(9) . . ?

C2 N1 Ce1 120.7(7) . . ?

C6 N1 Ce1 121.0(6) . . ?

C13 N2 C10 117.9(9) . . ?

C13 N2 Ce1 118.4(7) . . ?

C10 N2 Ce1 122.9(6) . . ?

C16 N3 C20 118.5(8) . . ?

C16 N3 Ce2 120.0(6) . . ?

C20 N3 Ce2 121.5(7) . . ?

C27 N4 C24 119.2(8) . . ?

C27 N4 Ce2 118.6(6) . . ?

C24 N4 Ce2 122.1(7) . . ?

O1 C1 O2 126.4(11) . . ?

O1 C1 C2 118.1(10) . . ?

O2 C1 C2 115.5(9) . . ?

N1 C2 C3 121.8(11) . . ?

N1 C2 C1 114.3(9) . . ?

C3 C2 C1 123.9(10) . . ?

C4 C3 C2 119.9(10) . . ?

C4 C3 H3A 120.0 . . ?

C2 C3 H3A 120.0 . . ?

C3 C4 C5 120.4(10) . . ?

C3 C4 H4A 119.8 . . ?

C5 C4 H4A 119.8 . . ?

C6 C5 C4 117.1(10) . . ?

C6 C5 C7 118.5(10) . . ?

C4 C5 C7 124.4(11) . . ?

N1 C6 C5 122.8(9) . . ?

N1 C6 C10 117.1(9) . . ?

C5 C6 C10 120.0(10) . . ?

C8 C7 C5 120.4(11) . . ?

C8 C7 H7A 119.8 . . ?

C5 C7 H7A 119.8 . . ?

C7 C8 C9 121.6(12) . . ?

C7 C8 H8A 119.2 . . ?

C9 C8 H8A 119.2 . . ?

C8 C9 C10 119.9(10) . . ?

C8 C9 C11 124.2(11) . . ?

C10 C9 C11 115.9(10) . . ?

N2 C10 C9 125.0(9) . . ?

N2 C10 C6 115.7(10) . . ?

C9 C10 C6 119.2(9) . . ?

C12 C11 C9 120.8(12) . . ?

C12 C11 H11A 119.6 . . ?

C9 C11 H11A 119.6 . . ?

C11 C12 C13 118.4(10) . . ?

C11 C12 H12A 120.8 . . ?

C13 C12 H12A 120.8 . . ?

N2 C13 C12 121.9(10) . . ?

N2 C13 C14 116.4(10) . . ?

C12 C13 C14 121.7(9) . . ?

O4 C14 O3 126.6(10) . . ?

O4 C14 C13 117.1(10) . . ?

O3 C14 C13 116.1(9) . . ?

O6 C15 O5 126.3(10) . . ?

O6 C15 C16 117.1(10) . . ?

O5 C15 C16 116.4(9) . . ?

N3 C16 C17 124.8(10) . . ?

N3 C16 C15 114.4(9) . . ?

C17 C16 C15 120.7(10) . . ?

C18 C17 C16 117.1(11) . . ?

C18 C17 H17A 121.4 . . ?

C16 C17 H17A 121.4 . . ?

C17 C18 C19 119.5(9) . . ?

C17 C18 H18A 120.2 . . ?

C19 C18 H18A 120.2 . . ?

C20 C19 C18 119.5(9) . . ?

C20 C19 C21 116.8(11) . . ?

C18 C19 C21 123.7(10) . . ?

N3 C20 C24 118.3(9) . . ?

N3 C20 C19 120.5(10) . . ?

C24 C20 C19 121.2(9) . . ?

C22 C21 C19 122.0(10) . . ?

C22 C21 H21A 119.0 . . ?

C19 C21 H21A 119.0 . . ?

C21 C22 C23 121.3(10) . . ?

C21 C22 H22A 119.4 . . ?

C23 C22 H22A 119.4 . . ?

C25 C23 C24 117.6(9) . . ?

C25 C23 C22 124.5(9) . . ?

C24 C23 C22 117.9(10) . . ?

N4 C24 C20 117.9(9) . . ?

N4 C24 C23 121.3(9) . . ?

C20 C24 C23 120.8(9) . . ?

C26 C25 C23 121.8(10) . . ?

C26 C25 H25A 119.1 . . ?

C23 C25 H25A 119.1 . . ?

C25 C26 C27 118.9(11) . . ?

C25 C26 H26A 120.5 . . ?

C27 C26 H26A 120.5 . . ?

N4 C27 C26 120.9(9) . . ?

N4 C27 C28 114.9(9) . . ?

C26 C27 C28 124.2(10) . . ?

O8 C28 O7 123.4(9) . . ?

O8 C28 C27 120.0(9) . . ?

O7 C28 C27 116.6(9) . . ?

Ce1 O1W H1W 136.0 . . ?

Ce1 O1W H2W 121.3 . . ?

H1W O1W H2W 88.6 . . ?

Ce1 O2W H3W 125.6 . . ?

Ce1 O2W H4W 121.5 . . ?

H3W O2W H4W 96.3 . . ?

Ce1 O3W H5W 92.6 . . ?

Ce1 O3W H6W 91.8 . . ?

H5W O3W H6W 107.0 . . ?

Ce1 O4W H7W 96.6 . . ?

Ce1 O4W H8W 99.7 . . ?

H7W O4W H8W 109.7 . . ?

Ce2 O5W H9W 112.8 . . ?

Ce2 O5W H10W 114.9 . . ?

H9W O5W H10W 125.8 . . ?

Ce2 O6W H11W 96.5 . . ?

Ce2 O6W H12W 91.5 . . ?

H11W O6W H12W 110.5 . . ?

H13W O7W H14W 109.6 . . ?

H15W O8W H16W 129.3 . . ?

H17W O9W H18W 110.6 . . ?

 

loop_

 _geom_hbond_atom_site_label_D

 _geom_hbond_atom_site_label_H

 _geom_hbond_atom_site_label_A

 _geom_hbond_distance_DH

 _geom_hbond_distance_HA

 _geom_hbond_distance_DA

 _geom_hbond_angle_DHA

 _geom_hbond_site_symmetry_A

O1W H1W O7W  0.85 1.93 2.777(16) 180.0 1_545

O1W H2W O12  0.85 2.01 2.848(12) 168.1 2_756

O2W H3W O3  0.85 1.95 2.797(11) 176.0 2_666

O2W H4W O7  0.85 1.86 2.700(10) 171.1 2_766

O3W H5W O9W  0.85 2.18 2.801(14) 129.4 .

O3W H5W O4W  0.85 2.41 2.998(12) 127.3 .

O3W H6W O10  0.85 2.49 2.996(11) 119.2 1_455

O3W H6W O11  0.85 2.51 3.354(14) 169.7 1_455

O3W H6W O1W  0.85 2.57 3.006(13) 112.9 .

O4W H7W O12  0.85 2.01 2.757(14) 146.4 2_756

O4W H7W O1W  0.85 2.26 2.835(15) 124.8 .

O4W H8W O3W  0.85 2.53 2.998(12) 115.9 .

O5W H9W O6  0.85 1.98 2.763(10) 153.0 2_766

O5W H10W O2  0.85 1.92 2.726(12) 158.3 2_766

O6W H11W O8  0.85 2.00 2.708(11) 140.6 2_865

O6W H12W O12  0.85 2.35 3.197(12) 179.7 .

O6W H12W O9  0.85 2.46 2.980(10) 120.2 .

O6W H12W O10  0.85 2.58 3.110(10) 121.1 .

O7W H13W O1  0.85 2.31 2.904(15) 127.7 2_667

O7W H14W O9W  0.85 2.10 2.949(17) 179.5 2_666

O8W H15W O2  0.85 2.39 3.239(15) 179.5 .

O8W H16W O9  0.85 2.03 2.876(14) 179.3 .

O9W H17W O11  0.85 1.99 2.781(15) 154.9 2_756

 

_diffrn_measured_fraction_theta_max    0.979

_diffrn_reflns_theta_full              25.00

_diffrn_measured_fraction_theta_full   0.979

_refine_diff_density_max    4.384

_refine_diff_density_min   -3.487

_refine_diff_density_rms    0.345

