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_7049735
_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         'C18 H36 Bi2 N2 S2'
_chemical_formula_sum            'C18 H36 Bi2 N2 S2'
_chemical_formula_weight         762.57
_chemical_name_systematic        Bis-tert-butylthiocyanatobismuthan
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_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            4
_cell_length_a                   12.8551(12)
_cell_length_b                   14.8107(11)
_cell_length_c                   13.3604(9)
_cell_measurement_reflns_used    21640
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.84
_cell_measurement_theta_min      1.46
_cell_volume                     2543.7(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21640
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.593
_exptl_absorpt_coefficient_mu    13.985
_exptl_absorpt_correction_T_max  0.0424
_exptl_absorpt_correction_T_min  0.0182
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'STOE X-AREA, LANA 1.71.3'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_preparation
'Hexagonal platelet cut into smaller triangular platelett. Compound is X-ray sensitive especially to CuKa radiation.'
_exptl_crystal_size_rad          0.054
_refine_diff_density_max         1.555
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details
;
 Flack x determined using 1775 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0444P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4234
_reflns_number_total             4997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00408d1.cif
_cod_data_source_block           tBu2BiSCN
_cod_depositor_comments
'Adding full bibliography for 7049733--7049739.cif.'
_cod_database_code               7049735
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N2, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C4AA) = Uanis(C3)
Uanis(C0AA) = Uanis(C5)
Uanis(C8) = Uanis(C26)
Uanis(C2AA) = Uanis(C9)
Uanis(C3AA) = Uanis(C7)
Uanis(C4) = Uanis(C1AA)
4.a Me refined with riding coordinates:
 C1AA(H1AA,H1AB,H1AC)
4.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C5(H5A,
 H5B,H5C), C7(H7A,H7B,H7C), C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC),
 C26(H26A,H26B,H26C), C4AA(H4AA,H4AB,H4AC), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              44232
_olex2_submission_special_instructions 'No special instructions were received'