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_7130080
_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         'C21 H18 Bi Cl2 N'
_chemical_formula_sum            'C21 H18 Bi Cl2 N'
_chemical_formula_weight         564.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                81.331(2)
_cell_angle_beta                 87.085(2)
_cell_angle_gamma                86.766(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3127(2)
_cell_length_b                   9.8342(2)
_cell_length_c                   11.5270(2)
_cell_measurement_reflns_used    5558
_cell_measurement_temperature    153
_cell_measurement_theta_max      28.7460
_cell_measurement_theta_min      2.0970
_cell_volume                     929.21(3)
_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
_diffrn_detector                 'Bruker APEX area detector'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.982
_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      0.0065984000
_diffrn_orient_matrix_UB_12      -0.0130456000
_diffrn_orient_matrix_UB_13      -0.0589625000
_diffrn_orient_matrix_UB_21      -0.0000014000
_diffrn_orient_matrix_UB_22      0.0718271000
_diffrn_orient_matrix_UB_23      -0.0200360000
_diffrn_orient_matrix_UB_31      0.0852868000
_diffrn_orient_matrix_UB_32      -0.0026067000
_diffrn_orient_matrix_UB_33      0.0018803000
_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  0.0111
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5574
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         1.789
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.778
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57533
_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    2.017
_exptl_crystal_description       prism
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+2.3093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3636
_reflns_number_total             3747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00751g2.cif
_cod_data_source_block           Compound9
_cod_database_code               7130080
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C21H18Bi1Cl2N1
_chemical_oxdiff_usercomment     Bismatrane_SO2Cl2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B)
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),
 C18(H18), C19(H19), C20(H20), C21(H21)
;
_shelx_res_checksum              65464
_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 1.788
_oxdiff_exptl_absorpt_empirical_full_min 0.686