Synthesis and crystal structures of novel tertiary butyl substituted (pseudo-)halogen bismuthanes.
Ritter, Christian; Ringler, Benjamin; Dankert, Fabian; Conrad, Matthias; Kraus, Florian; von Hänisch, Carsten; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5253–5262; doi:10.1039/c9dt00408d

data_7049739
_publ_section_title
;
 Synthesis and crystal structures of novel tertiary butyl substituted
 (pseudo-)halogen bismuthanes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5253
_journal_page_last               5262
_journal_paper_doi               10.1039/c9dt00408d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C8 H18 Bi Br'
_chemical_formula_sum            'C8 H18 Bi Br'
_chemical_formula_weight         403.11
_chemical_name_systematic        Bis-tert-butylbromobismutan
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-23 deposited with the CCDC.    2019-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7248(7)
_cell_length_b                   11.8780(6)
_cell_length_c                   14.0210(7)
_cell_measurement_reflns_used    9395
_cell_measurement_temperature    110
_cell_measurement_theta_max      31.834
_cell_measurement_theta_min      2.693
_cell_volume                     2285.7(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20895
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.693
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.866
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.1659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1536 before and 0.0628 after correction. The Ratio of minimum to maximum transmission is 0.2224. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.343
_exptl_crystal_description       needle
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.071
_refine_diff_density_max         2.135
_refine_diff_density_min         -1.870
_refine_diff_density_rms         0.270
_refine_ls_extinction_coef       0.00088(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+4.3190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2137
_reflns_number_total             2251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00408d1.cif
_cod_data_source_block           tBu2BiBr
_cod_depositor_comments
'Adding full bibliography for 7049733--7049739.cif.'
_cod_database_code               7049739
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.348
_shelx_estimated_absorpt_t_min   0.053
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              37780
_olex2_submission_special_instructions 'No special instructions were received'