Planar bismuth triamides: a tunable platform for main group Lewis acidity and polymerization catalysis
Hannah, Tyler J.; McCarvell, W. Michael; Kirsch, Tamina; Bedard, Joseph; Hynes, Toren; Mayho, Jacqueline; Bamford, Karlee L.; Vos, Cyler W.; Kozak, Christopher M.; George, Tanner; Masuda, Jason D.; Chitnis, S. S.; Chemical Science 14 (2023) 4549–4563; doi:10.1039/D3SC00917C

data_1568802
_publ_section_title
;
 Planar bismuth triamides: a tunable platform for main group Lewis acidity
 and polymerization catalysis
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              4549
_journal_page_last               4563
_journal_paper_doi               10.1039/D3SC00917C
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C94 H114 Bi2 Br4 N8 O8 S4, C6 H6, 1[C6H6], 1[C6H6]'
_chemical_formula_sum            'C112 H132 Bi2 Br4 N8 O8 S4'
_chemical_formula_weight         2584.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-04 deposited with the CCDC.	2023-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                83.424(4)
_cell_angle_beta                 89.804(4)
_cell_angle_gamma                66.363(4)
_cell_formula_units_Z            2
_cell_length_a                   16.4085(16)
_cell_length_b                   18.9240(19)
_cell_length_c                   19.8569(19)
_cell_measurement_reflns_used    9363
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.25
_cell_volume                     5605.3(10)
_computing_cell_refinement       'SAINT V8.40A (Bruker AXS Inc., 2018)'
_computing_data_reduction        'SAINT V8.40A (Bruker AXS Inc., 2018)'
_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      150.00
_diffrn_detector                 '100 \\times 140 mm^2^ CMOS sensor'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            292086
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.743
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.693
_exptl_absorpt_correction_T_max  0.0206
_exptl_absorpt_correction_T_min  0.0053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0840 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.2573.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       block
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.145
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1159
_refine_ls_number_reflns         23818
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0781P)^2^+23.2870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17861
_reflns_number_total             23818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00917c3.cif
_cod_data_source_block           mo_2022_08_25_jdm_sc_tjh186_0m_a
_cod_depositor_comments
'Adding full bibliography for 1568798--1568802.cif.'
_cod_database_code               1568802
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.540
_diffrn_source_source            'microfocus sealed tube'
_olex2_refinement_description
;
1. Restrained distances
 C99-C100
 1.39 with sigma of 0.02
 C98-C97 = C97-C96
 1.39 with sigma of 0.02
 C99-C98 = C96-C95 = C95-C100
 1.39 with sigma of 0.02
 C99-C95
 2.38 with sigma of 0.04
 C99-C97 = C97-C95 = C96-C100
 2.37 with sigma of 0.04
 C98-C96
 2.36 with sigma of 0.04
 C99-C98 \\sim C98-C97 \\sim C97-C96 \\sim C96-C95 \\sim C95-C100 \\sim C100-C99
 with sigma of 0.02
 C99-C95 \\sim C99-C97 \\sim C95-C97 \\sim C96-C98 \\sim C96-C100 \\sim C100-C98
 with sigma of 0.04
2. Restrained planarity
 C95, C96, C97, C98, C99, C100
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C95 \\sim C96 \\sim C97 \\sim C98 \\sim C99 \\sim C100: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C95, C96, C97, C98, C99, C100
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C25(H25), C34(H34), C37(H37), C40(H40), C66(H66),
 C69(H69), C72(H72), C81(H81), C84(H84), C87(H87)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C9(H9), C11(H11), C12(H12), C15(H15), C17(H17),
 C30(H30), C32(H32), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49),
  C51(H51), C52(H52), C56(H56), C58(H58), C59(H59), C62(H62), C64(H64),
 C77(H77), C79(H79), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95),
  C96(H96), C97(H97), C98(H98), C99(H99), C100(H100)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,
 H70C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C82(H82A,
 H82B,H82C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C),
 C88(H88A,H88B,H88C), C89(H89A,H89B,H89C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15939
_shelx_fab_checksum              55024
_olex2_submission_special_instructions 'No special instructions were received'