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_1568801
_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         'C46 H68 Bi N5 O4 S2, 0.5(C6 H14)'
_chemical_formula_sum            'C49 H75 Bi N5 O4 S2'
_chemical_formula_weight         1071.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-10-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-03 deposited with the CCDC.	2023-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.0206(10)
_cell_length_b                   10.3986(3)
_cell_length_c                   29.7870(9)
_cell_measurement_reflns_used    9534
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.56
_cell_measurement_theta_min      5.00
_cell_volume                     10227.9(5)
_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)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            317789
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.667
_diffrn_reflns_theta_min         2.676
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.882
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4408
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.371
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         10464
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0230P)^2^+28.4942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9343
_reflns_number_total             10464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00917c3.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 1568798--1568802.cif.'
_cod_database_code               1568801
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.384
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N03-H03 = N04-H04
 0.91 with sigma of 0.02
 C95A-C96A \\sim C95B-C96B \\sim C91A-C92A \\sim C91B-C92B
 with sigma of 0.02
 C92A-C93A \\sim C92B-C93B \\sim C94A-C95A \\sim C94B-C95B
 with sigma of 0.02
 C93A-C94A \\sim C93B-C94B
 with sigma of 0.02
 C16A-C103 \\sim C16B-C103
 with sigma of 0.02
 C17A-C18A \\sim C17B-C18B
 with sigma of 0.02
 C16A-C17A \\sim C16A-C18A \\sim C16B-C17B \\sim C16B-C18B
 with sigma of 0.02
 C26-C28A \\sim C26-C28B \\sim C26-C27
 with sigma of 0.02
3. Rigid bond restraints
 C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C91A) = Uanis(C91B)
Uanis(C92A) = Uanis(C92B)
Uanis(C93A) = Uanis(C93B)
Uanis(C94A) = Uanis(C94B)
Uanis(C95A) = Uanis(C95B)
Uanis(C96A) = Uanis(C96B)
Uanis(C103) = Uanis(C203)
Uanis(C16A) = Uanis(C16B)
Uanis(C17A) = Uanis(C17B)
Uanis(C18A) = Uanis(C18B)
Uanis(C28A) = Uanis(C28B) = Uanis(C27)
5. Rigid body (RIGU) restrains
 C91A, C92A, C93A, C94A, C95A, C96A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91B, C92B, C93B, C94B, C95B, C96B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16A, C17A, C18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16B, C17B, C18B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27, C28A, C28B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(2)
 Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(2)
 Sof(C91B)=Sof(H91D)=Sof(H91E)=Sof(H91F)=Sof(C92B)=Sof(H92C)=Sof(H92D)=
 Sof(C93B)=Sof(H93C)=Sof(H93D)=Sof(C94B)=Sof(H94C)=Sof(H94D)=Sof(C95B)=
 Sof(H95C)=Sof(H95D)=Sof(C96B)=Sof(H96D)=Sof(H93E)=Sof(H96E)=0.5*(1-FVAR(4))
 Sof(C91A)=Sof(H91A)=Sof(H91B)=Sof(H91C)=Sof(C92A)=Sof(H92A)=Sof(H92B)=
 Sof(C93A)=Sof(H93A)=Sof(H93B)=Sof(C94A)=Sof(H94A)=Sof(H94B)=Sof(C95A)=
 Sof(H95A)=Sof(H95B)=Sof(C96A)=Sof(H96A)=Sof(H96B)=Sof(H96C)=0.5*FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C13(H13), C20(H20), C23(H23), C10(H10), C16A(H16A), C16B(H16B)
7.b Secondary CH2 refined with riding coordinates:
 C92A(H92A,H92B), C93A(H93A,H93B), C94A(H94A,H94B), C95A(H95A,H95B), C92B(H92C,
 H92D), C93B(H93C,H93D), C94B(H94C,H94D), C95B(H95C,H95D)
7.c Aromatic/amide H refined with riding coordinates:
 C301(H301), C202(H202), C304(H304), C303(H303), C102(H102), C402(H402),
 C405(H405), C302(H302), C204(H204), C403(H403), C404(H404), C104(H104)
7.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C12(H12A,H12B,H12C), C5(H5A,H5B,H5C),
  C27(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F), C17A(H17A,
 H17B,H17C), C18A(H18A,H18B,H18C), C17B(H17D,H17E,H17F), C18B(H18D,H18E,H18F),
 C91A(H91A,H91B,H91C), C96A(H96A,H96B,H96C), C91B(H91D,H91E,H91F), C96B(H96D,
 H93E,H96E)
;
_shelx_res_checksum              77398
_olex2_submission_special_instructions 'No special instructions were received'