Bromine-rich complexes of bismuth: experimental and theoretical studies.
Adonin, Sergey A.; Gorokh, Igor D.; Novikov, Alexander S.; Samsonenko, Denis G.; Plyusnin, Pavel E.; Sokolov, Maxim N.; Fedin, Vladimir P.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2683–2689; doi:10.1039/c7dt04779g

data_7045343
_publ_section_title
;
 Bromine-rich complexes of bismuth: experimental and theoretical studies.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2683
_journal_page_last               2689
_journal_paper_doi               10.1039/c7dt04779g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C21 H30 Bi Br8 N3'
_chemical_formula_weight         1172.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-12-04 deposited with the CCDC.
2018-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.857(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2266(2)
_cell_length_b                   17.8388(4)
_cell_length_c                   17.6539(4)
_cell_measurement_reflns_used    5767
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.22
_cell_measurement_theta_min      3.81
_cell_volume                     3220.25(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17474
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.545
_diffrn_reflns_theta_min         3.616
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    15.417
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.419
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.118
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         7605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6054
_reflns_number_total             7605
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c7dt04779g2.cif
_cod_data_source_block           IG137
_cod_depositor_comments
'Adding full bibliography for 7045343--7045345.cif.'
_cod_original_cell_volume        3220.24(13)
_cod_database_code               7045343
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.077
_shelx_estimated_absorpt_t_max   0.221
_shelx_res_checksum              30043