Synthesis, Structure and Properties of Trivalent and Pentavalent Tricarbabismatranes
Shimada, Shigeru; Yin, Shuang-Feng; Choe, Yoong-Kee; Chemical Communications  (2022) –; doi:10.1039/D2CC00751G

data_7130081
_publ_section_title
;
 Synthesis, Structure and Properties of Trivalent and Pentavalent
 Tricarbabismatranes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00751G
_journal_year                    2022
_chemical_formula_moiety         'C24 H26 Bi Cl2 N'
_chemical_formula_sum            'C24 H26 Bi Cl2 N'
_chemical_formula_weight         608.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-01-24 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.724(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3838(4)
_cell_length_b                   8.4575(2)
_cell_length_c                   17.0618(4)
_cell_measurement_reflns_used    11413
_cell_measurement_temperature    153
_cell_measurement_theta_max      28.7680
_cell_measurement_theta_min      1.8100
_cell_volume                     2218.88(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'Bruker APEX area detector'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

 # Type Start End Width t~exp~ \w \q \k \f Frames
 1 \w 2.33 183.94 0.30 4.99 -- 28.00 73.57 -25.67 606
 2 \w 2.33 132.69 0.30 4.99 -- 28.00 73.57 64.33 435
 3 \w 2.33 71.26 0.30 4.99 -- 28.00 73.57 154.33 230
 4 \w 2.33 17.31 0.30 4.99 -- 28.00 73.57 -25.67 50
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0315635000
_diffrn_orient_matrix_UB_12      -0.0606345000
_diffrn_orient_matrix_UB_13      0.0030945000
_diffrn_orient_matrix_UB_21      -0.0031356000
_diffrn_orient_matrix_UB_22      -0.0055489000
_diffrn_orient_matrix_UB_23      -0.0414821000
_diffrn_orient_matrix_UB_31      0.0334903000
_diffrn_orient_matrix_UB_32      -0.0576382000
_diffrn_orient_matrix_UB_33      0.0007535000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12692
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.728
_diffrn_reflns_theta_min         2.388
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.197
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_description       prism
_exptl_crystal_F_000             1176
_exptl_crystal_recrystallization_method 'Recrystallized from ether'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+5.3824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4392
_reflns_number_total             4717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00751g2.cif
_cod_data_source_block           AzabismocineCl2-Compound7a
_cod_database_code               7130081
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H26Bi1Cl2N1
_chemical_oxdiff_usercomment     tBuAzabismocine-Cl2Ph
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              79726
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.844