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_7049736
_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         'C9 H18 Bi N'
_chemical_formula_sum            'C9 H18 Bi N'
_chemical_formula_weight         349.22
_chemical_name_systematic        Bis-tert-butylcyanobismutan
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_symmetry_space_group_name_Hall  'P 4n 2n'
_symmetry_space_group_name_H-M   'P 42 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                   13.3118(6)
_cell_length_b                   13.3118(6)
_cell_length_c                   6.2820(3)
_cell_measurement_reflns_used    1102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      1.53
_cell_volume                     1113.20(9)
_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(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            11435
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_min         2.164
_exptl_absorpt_coefficient_mu    15.787
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'STOE X-AREA, LANA 1.71.3'
_exptl_crystal_colour            beige
_exptl_crystal_density_diffrn    2.084
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.045
_exptl_crystal_size_rad          0.0573
_exptl_transmission_factor_max   0.0656
_exptl_transmission_factor_min   0.0380
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0093P)^2^+6.6568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0490
_reflns_Friedel_coverage         0.616
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                989
_reflns_number_total             1104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00408d1.cif
_cod_data_source_block           tBu2BiCN
_cod_depositor_comments
'Adding full bibliography for 7049733--7049739.cif.'
_cod_original_cell_volume        1113.20(11)
_cod_database_code               7049736
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(4)
 0.49(4)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C002)
4. Others
 Fixed Sof: C002(0.5) N1(0.5)
5.a Idealised Me refined as rotating group:
 C004(H00A,H00B,H00C), C005(H00D,H00E,H00F), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              18155
_olex2_submission_special_instructions 'No special instructions were received'