Bis(amidophenolate)-supported pnictoranides: Lewis acid-induced electromerism in a bismuth complex.
Karnbrock, Simon B. H.; Köster, Jan F; Becker, Isabelle; Golz, Christopher; Meyer, Franc; Gimferrer, Martí; Alcarazo, Manuel; Chemical science 16 (2025) 14178–14185; doi:10.1039/d5sc03374h

data_1575597
_publ_section_title
;
 Bis(amidophenolate)-supported pnictoranides: Lewis acid-induced
 electromerism in a bismuth complex.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              14178
_journal_page_last               14185
_journal_paper_doi               10.1039/d5sc03374h
_journal_volume                  16
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H45 Bi N2 O2, C7 H8'
_chemical_formula_sum            'C41 H53 Bi N2 O2'
_chemical_formula_weight         814.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-29
_audit_creation_method
;FinalCif V123 by Daniel Kratzert, Freiburg 2023, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-04-30 deposited with the CCDC.	2025-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.186(4)
_cell_length_b                   18.226(14)
_cell_length_c                   19.858(15)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.290
_cell_measurement_theta_min      2.235
_cell_volume                     3687(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
'Bruker BIS V6.2.15/2021-03-15 && APEX4 2022.1-1'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Ag'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46132
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.726
_diffrn_reflns_theta_min         2.051
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.39
_diffrn_source_power             0.0695
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.818
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6894
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0709 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.6894.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       needle
_exptl_crystal_F_000             1648
_exptl_crystal_recrystallization_method 'from toluene solution.'
_exptl_crystal_size_max          0.406
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.347
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
;
 Flack x determined using 3286 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.053(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         9412
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0390P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                8200
_reflns_number_total             9412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03374h3.cif
_cod_data_source_block           mo_2028_cg_0m
_cod_database_code               1575597
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 C36-C37 \\sim C36A-C37A
 with sigma of 0.02
 C36-C41 \\sim C36A-C41A
 with sigma of 0.02
 C37-C38 \\sim C37A-C38A
 with sigma of 0.02
 C38-C39 \\sim C38A-C39A
 with sigma of 0.02
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 C40-C41 \\sim C40A-C41A
 with sigma of 0.02
 C35-C37 \\sim C35A-C37A
 with sigma of 0.04
 C35-C41 \\sim C35A-C41A
 with sigma of 0.04
 C36-C38 \\sim C36A-C38A
 with sigma of 0.04
 C36-C40 \\sim C36A-C40A
 with sigma of 0.04
 C37-C39 \\sim C37A-C39A
 with sigma of 0.04
 C37-C41 \\sim C37A-C41A
 with sigma of 0.04
 C38-C40 \\sim C38A-C40A
 with sigma of 0.04
 C39-C41 \\sim C39A-C41A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C35, C36, C37, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, C36, C41, C40, C39, C38, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C35A, C36A, C37A, C38A, C39A, C40A, C41A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C37A)=Sof(H37A)=Sof(C36A)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=
 Sof(C41A)=Sof(H41A)=Sof(C40A)=Sof(H40A)=Sof(C39A)=Sof(H39A)=Sof(C38A)=
 Sof(H38A)=1-FVAR(1)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(C37)=Sof(H37)=Sof(C38)=
 Sof(H38)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C24(H24),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C37A(H37A), C41A(H41A),
 C40A(H40A), C39A(H39A), C38A(H38A)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C35A(H35D,H35E,H35F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.245
_shelx_estimated_absorpt_t_max   0.910
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              62468