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_7130079
_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 F2 N'
_chemical_formula_sum            'C21 H18 Bi F2 N'
_chemical_formula_weight         531.34
_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                 101.586(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0487(3)
_cell_length_b                   13.9834(4)
_cell_length_c                   12.3014(4)
_cell_measurement_reflns_used    8948
_cell_measurement_temperature    153
_cell_measurement_theta_max      28.6110
_cell_measurement_theta_min      2.0690
_cell_volume                     1693.31(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
_diffrn_detector                 'Bruker APEX area detector'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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 11.32 0.30 4.99 -- 28.00 73.57 -25.67 30
;
_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      0.0142762000
_diffrn_orient_matrix_UB_12      0.0489804000
_diffrn_orient_matrix_UB_13      0.0121253000
_diffrn_orient_matrix_UB_21      0.0691747000
_diffrn_orient_matrix_UB_22      -0.0079324000
_diffrn_orient_matrix_UB_23      -0.0020881000
_diffrn_orient_matrix_UB_31      -0.0142983000
_diffrn_orient_matrix_UB_32      0.0105819000
_diffrn_orient_matrix_UB_33      -0.0575376000
_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  0.0150
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9898
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.069
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.435
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71507
_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    2.084
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_recrystallization_method 'Recrystallized from CH2Cl2/heptane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0199
_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^)+(0.0214P)^2^+3.6859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0460
_refine_ls_wR_factor_ref         0.0469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3466
_reflns_number_total             3716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00751g2.cif
_cod_data_source_block           bismatrneF2-Compoud-8b
_cod_database_code               7130079
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C21H18Bi1F2N1
_chemical_oxdiff_usercomment     BismatoraneF2
_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), C21(H21A,H21B)
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),
 C16(H16), C17(H17), C18(H18), C19(H19)
;
_shelx_res_checksum              63886
_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 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.716