 
data_CM064_a
 
_audit_creation_method            'SHELXL-2016/6'
_shelx_SHELXL_version_number      '2016/6'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C48 H40 B2'
_chemical_formula_sum
 'C48 H40 B2' 
_chemical_formula_weight          638.42

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'
 'B'  'B'   0.0090   0.0039
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_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+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    9.4061(5)
_cell_length_b                    11.8145(7)
_cell_length_c                    15.8718(9)
_cell_angle_alpha                 90
_cell_angle_beta                  95.270(2)
_cell_angle_gamma                 90
_cell_volume                      1756.35(17)
_cell_formula_units_Z             2
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9868
_cell_measurement_theta_min       4.67
_cell_measurement_theta_max       72.12
 
_exptl_crystal_description        block
_exptl_crystal_colour             red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.207          
_exptl_crystal_F_000              676
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.168
_exptl_crystal_size_mid           0.094
_exptl_crystal_size_min           0.082
_exptl_absorpt_coefficient_mu     0.504
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6995
_exptl_absorpt_correction_T_max   0.7536
_exptl_absorpt_process_details    Bruker-SADABS
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    Cu/K(alpha)_ImuS_Microsource               
_diffrn_measurement_device_type   Bruker-Kappa-D8Quest_Photon100 
_diffrn_measurement_method        omega_and_phi_scan
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             28092
_diffrn_reflns_av_unetI/netI      0.0200
_diffrn_reflns_av_R_equivalents   0.0394
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          4.673
_diffrn_reflns_theta_max          72.214
_diffrn_reflns_theta_full         67.679
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              3467
_reflns_number_gt                 3116
_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        'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0606P)²+0.6113P] 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          3467
_refine_ls_number_parameters      229
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0465
_refine_ls_R_factor_gt            0.0419
_refine_ls_wR_factor_ref          0.1130
_refine_ls_wR_factor_gt           0.1082
_refine_ls_goodness_of_fit_ref    1.034
_refine_ls_restrained_S_all       1.034
_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
B1 B 0.70912(14) 0.70317(11) 0.39521(8) 0.0189(3) Uani 1 1 d . . . . .
C1 C 0.56989(12) 0.77861(10) 0.38511(7) 0.0195(3) Uani 1 1 d . . . . .
C2 C 0.43431(13) 0.72827(11) 0.37487(7) 0.0223(3) Uani 1 1 d . . . . .
C3 C 0.31186(14) 0.79536(12) 0.36637(8) 0.0280(3) Uani 1 1 d . . . . .
H3 H 0.221024 0.759888 0.357937 0.034 Uiso 1 1 calc R U . . .
C4 C 0.31927(15) 0.91275(13) 0.36991(8) 0.0309(3) Uani 1 1 d . . . . .
C5 C 0.45398(16) 0.96226(11) 0.38129(8) 0.0307(3) Uani 1 1 d . . . . .
H5 H 0.461301 1.042368 0.384572 0.037 Uiso 1 1 calc R U . . .
C6 C 0.57839(14) 0.89754(11) 0.38800(7) 0.0249(3) Uani 1 1 d . . . . .
C7 C 0.41959(14) 0.60105(11) 0.37468(9) 0.0295(3) Uani 1 1 d . . . . .
H7A H 0.415831 0.574064 0.432816 0.044 Uiso 1 1 calc R U . . .
H7B H 0.501753 0.567059 0.350497 0.044 Uiso 1 1 calc R U . . .
H7C H 0.331610 0.579432 0.340594 0.044 Uiso 1 1 calc R U . . .
C8 C 0.18422(18) 0.98301(17) 0.36214(10) 0.0485(4) Uani 1 1 d . . . . .
H8A H 0.126331 0.962946 0.309770 0.073 Uiso 1 1 calc R U . . .
H8B H 0.209156 1.063499 0.360916 0.073 Uiso 1 1 calc R U . . .
H8C H 0.129705 0.968111 0.410689 0.073 Uiso 1 1 calc R U . . .
C9 C 0.72213(16) 0.95459(12) 0.39787(10) 0.0358(3) Uani 1 1 d . . . . .
H9A H 0.766145 0.950288 0.344342 0.054 Uiso 1 1 calc R U . . .
H9B H 0.783530 0.916479 0.442386 0.054 Uiso 1 1 calc R U . . .
H9C H 0.710268 1.034117 0.413310 0.054 Uiso 1 1 calc R U . . .
C10 C 0.79522(12) 0.66842(10) 0.32100(7) 0.0199(2) Uani 1 1 d . . . . .
C11 C 0.76547(13) 0.71233(10) 0.23332(7) 0.0209(3) Uani 1 1 d . . . . .
C12 C 0.63261(13) 0.69524(10) 0.18815(8) 0.0223(3) Uani 1 1 d . . . . .
H12 H 0.558011 0.660043 0.215038 0.027 Uiso 1 1 calc R U . . .
C13 C 0.60866(14) 0.72917(11) 0.10446(8) 0.0256(3) Uani 1 1 d . . . . .
H13 H 0.519397 0.713850 0.073565 0.031 Uiso 1 1 calc R U . . .
C14 C 0.71467(15) 0.78551(11) 0.06550(8) 0.0285(3) Uani 1 1 d . . . . .
H14 H 0.697456 0.809918 0.008446 0.034 Uiso 1 1 calc R U . . .
C15 C 0.84523(15) 0.80581(12) 0.11024(9) 0.0311(3) Uani 1 1 d . . . . .
H15 H 0.917306 0.845590 0.084224 0.037 Uiso 1 1 calc R U . . .
C16 C 0.87143(14) 0.76818(11) 0.19324(8) 0.0268(3) Uani 1 1 d . . . . .
H16 H 0.962404 0.780598 0.222994 0.032 Uiso 1 1 calc R U . . .
C17 C 0.90515(12) 0.59432(10) 0.33677(7) 0.0198(2) Uani 1 1 d . . . . .
H17 H 0.956326 0.573179 0.290332 0.024 Uiso 1 1 calc R U . . .
C18 C 0.95103(12) 0.54467(10) 0.41865(7) 0.0184(2) Uani 1 1 d . . . . .
C19 C 1.06320(12) 0.46338(9) 0.42669(7) 0.0179(2) Uani 1 1 d . . . . .
C20 C 1.12411(12) 0.41764(10) 0.35490(7) 0.0198(2) Uani 1 1 d . . . . .
H20 H 1.089354 0.442445 0.299898 0.024 Uiso 1 1 calc R U . . .
C21 C 1.23131(13) 0.33896(10) 0.36331(8) 0.0213(3) Uani 1 1 d . . . . .
H21 H 1.268616 0.308740 0.314429 0.026 Uiso 1 1 calc R U . . .
C22 C 1.28632(12) 0.30280(10) 0.44433(8) 0.0201(2) Uani 1 1 d . . . . .
H22 H 1.363656 0.250790 0.449357 0.024 Uiso 1 1 calc R U . . .
C23 C 1.23051(12) 0.34115(9) 0.51694(7) 0.0188(2) Uani 1 1 d . . . . .
C24 C 0.88572(12) 0.57930(10) 0.49153(7) 0.0178(2) 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
B1 C10 1.5450(17) . ?
B1 C23 1.5477(17) 3_766 ?
B1 C1 1.5800(17) . ?
C1 C2 1.4030(17) . ?
C1 C6 1.4078(17) . ?
C2 C3 1.3945(17) . ?
C2 C7 1.5094(18) . ?
C3 C4 1.390(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(2) . ?
C4 C8 1.5131(19) . ?
C5 C6 1.3938(18) . ?
C5 H5 0.9500 . ?
C6 C9 1.5060(19) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C17 1.3604(17) . ?
C10 C11 1.4874(16) . ?
C11 C16 1.3963(17) . ?
C11 C12 1.3971(17) . ?
C12 C13 1.3859(17) . ?
C12 H12 0.9500 . ?
C13 C14 1.3903(19) . ?
C13 H13 0.9500 . ?
C14 C15 1.382(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.3908(18) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.4547(16) . ?
C17 H17 0.9500 . ?
C18 C24 1.4190(16) . ?
C18 C19 1.4238(16) . ?
C19 C20 1.4277(16) . ?
C19 C24 1.4337(15) 3_766 ?
C20 C21 1.3690(17) . ?
C20 H20 0.9500 . ?
C21 C22 1.4077(17) . ?
C21 H21 0.9500 . ?
C22 C23 1.3857(17) . ?
C22 H22 0.9500 . ?
C23 C24 1.4386(16) 3_766 ?
 
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
C10 B1 C23 114.98(10) . 3_766 ?
C10 B1 C1 124.07(10) . . ?
C23 B1 C1 120.95(10) 3_766 . ?
C2 C1 C6 118.37(11) . . ?
C2 C1 B1 120.58(11) . . ?
C6 C1 B1 121.04(11) . . ?
C3 C2 C1 120.28(12) . . ?
C3 C2 C7 119.40(11) . . ?
C1 C2 C7 120.31(11) . . ?
C4 C3 C2 121.70(13) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 117.80(12) . . ?
C3 C4 C8 120.38(14) . . ?
C5 C4 C8 121.82(14) . . ?
C4 C5 C6 121.81(12) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 120.02(12) . . ?
C5 C6 C9 120.12(12) . . ?
C1 C6 C9 119.86(12) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C17 C10 C11 118.11(11) . . ?
C17 C10 B1 118.26(10) . . ?
C11 C10 B1 123.63(10) . . ?
C16 C11 C12 118.47(11) . . ?
C16 C11 C10 120.67(11) . . ?
C12 C11 C10 120.81(11) . . ?
C13 C12 C11 120.60(12) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 120.31(12) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 119.63(12) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 120.20(13) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C11 120.71(12) . . ?
C15 C16 H16 119.6 . . ?
C11 C16 H16 119.6 . . ?
C10 C17 C18 125.59(11) . . ?
C10 C17 H17 117.2 . . ?
C18 C17 H17 117.2 . . ?
C24 C18 C19 119.62(10) . . ?
C24 C18 C17 119.80(11) . . ?
C19 C18 C17 120.57(10) . . ?
C18 C19 C20 122.15(10) . . ?
C18 C19 C24 120.16(11) . 3_766 ?
C20 C19 C24 117.63(10) . 3_766 ?
C21 C20 C19 121.68(11) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C20 C21 C22 120.05(11) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 121.67(11) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C22 C23 C24 118.59(10) . 3_766 ?
C22 C23 B1 120.20(11) . 3_766 ?
C24 C23 B1 121.20(10) 3_766 3_766 ?
C18 C24 C19 120.16(11) . 3_766 ?
C18 C24 C23 119.62(10) . 3_766 ?
C19 C24 C23 120.21(10) 3_766 3_766 ?
 
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
C10 B1 C1 C2 93.91(14) . . . . ?
C23 B1 C1 C2 -86.41(14) 3_766 . . . ?
C10 B1 C1 C6 -87.50(14) . . . . ?
C23 B1 C1 C6 92.19(14) 3_766 . . . ?
C6 C1 C2 C3 1.09(16) . . . . ?
B1 C1 C2 C3 179.72(11) . . . . ?
C6 C1 C2 C7 -177.71(11) . . . . ?
B1 C1 C2 C7 0.93(16) . . . . ?
C1 C2 C3 C4 -1.70(18) . . . . ?
C7 C2 C3 C4 177.10(12) . . . . ?
C2 C3 C4 C5 0.77(18) . . . . ?
C2 C3 C4 C8 -178.82(12) . . . . ?
C3 C4 C5 C6 0.76(19) . . . . ?
C8 C4 C5 C6 -179.66(12) . . . . ?
C4 C5 C6 C1 -1.35(18) . . . . ?
C4 C5 C6 C9 178.31(12) . . . . ?
C2 C1 C6 C5 0.40(17) . . . . ?
B1 C1 C6 C5 -178.23(11) . . . . ?
C2 C1 C6 C9 -179.26(11) . . . . ?
B1 C1 C6 C9 2.11(17) . . . . ?
C23 B1 C10 C17 6.54(15) 3_766 . . . ?
C1 B1 C10 C17 -173.76(11) . . . . ?
C23 B1 C10 C11 -172.88(10) 3_766 . . . ?
C1 B1 C10 C11 6.83(18) . . . . ?
C17 C10 C11 C16 -56.86(16) . . . . ?
B1 C10 C11 C16 122.55(13) . . . . ?
C17 C10 C11 C12 120.89(13) . . . . ?
B1 C10 C11 C12 -59.69(16) . . . . ?
C16 C11 C12 C13 2.43(18) . . . . ?
C10 C11 C12 C13 -175.37(11) . . . . ?
C11 C12 C13 C14 -3.01(18) . . . . ?
C12 C13 C14 C15 1.15(19) . . . . ?
C13 C14 C15 C16 1.2(2) . . . . ?
C14 C15 C16 C11 -1.8(2) . . . . ?
C12 C11 C16 C15 -0.04(19) . . . . ?
C10 C11 C16 C15 177.76(12) . . . . ?
C11 C10 C17 C18 178.77(11) . . . . ?
B1 C10 C17 C18 -0.68(17) . . . . ?
C10 C17 C18 C24 -4.64(18) . . . . ?
C10 C17 C18 C19 176.76(11) . . . . ?
C24 C18 C19 C20 174.19(10) . . . . ?
C17 C18 C19 C20 -7.21(17) . . . . ?
C24 C18 C19 C24 -2.87(17) . . . 3_766 ?
C17 C18 C19 C24 175.73(10) . . . 3_766 ?
C18 C19 C20 C21 -179.57(11) . . . . ?
C24 C19 C20 C21 -2.44(16) 3_766 . . . ?
C19 C20 C21 C22 -1.29(17) . . . . ?
C20 C21 C22 C23 2.88(18) . . . . ?
C21 C22 C23 C24 -0.57(17) . . . 3_766 ?
C21 C22 C23 B1 178.22(10) . . . 3_766 ?
C19 C18 C24 C19 2.88(17) . . . 3_766 ?
C17 C18 C24 C19 -175.74(10) . . . 3_766 ?
C19 C18 C24 C23 -178.12(10) . . . 3_766 ?
C17 C18 C24 C23 3.26(16) . . . 3_766 ?
 
_refine_diff_density_max    0.260
_refine_diff_density_min   -0.203
_refine_diff_density_rms    0.042



