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_1575600
_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         'C41 H49 Bi Fe N2 O4'
_chemical_formula_sum            'C41 H49 Bi Fe N2 O4'
_chemical_formula_weight         898.65
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-29
_audit_creation_method
;FinalCif V132 by Daniel Kratzert, Freiburg 2024, 
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                   12.6242(7)
_cell_length_b                   16.1575(10)
_cell_length_c                   18.7294(12)
_cell_measurement_reflns_used    4422
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      22.931
_cell_measurement_theta_min      2.358
_cell_volume                     3820.3(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
'Bruker BIS 8.5.1.2 Release/2023-09-07 and APEX5 2023.9-2'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16183
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.644
_diffrn_reflns_theta_min         1.829
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.9
_diffrn_source_power             0.045
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.723
_exptl_absorpt_correction_T_max  0.050160
_exptl_absorpt_correction_T_min  0.023650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0990 before and 0.0529 after correction.
 
For component 2:
 wR2(int) was 0.1372 before and 0.0555 after correction.
 The Ratio of minimum to maximum transmission is 0.47.

Final HKLF 4 output contains 209029 reflections, Rint = 0.0605
 (151661 with I > 3sig(I), Rint = 0.0564)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: from a mixture of dichloromethane and acetonitrle.'
_exptl_crystal_size_max          0.667
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.372
_refine_diff_density_max         1.769
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Flack x determined using 4739 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.051(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         16183
_refine_ls_number_restraints     621
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0347P)^2^+12.5622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                15051
_reflns_number_total             16183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03374h3.cif
_cod_data_source_block           ag_2215_cg_0m_4
_cod_database_code               1575600
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5755(9)
 0.4245(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C41A-C40A \\sim C37A-C41A \\sim C37A-C38A \\sim C39A-C38A \\sim C39A-C40A
 with sigma of 0.02
 C2-C11 \\sim C2-C11A
 with sigma of 0.02
 C13-C11 \\sim C13A-C11A
 with sigma of 0.02
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 C11-C14 \\sim C11A-C14A
 with sigma of 0.02
 C2-C13 \\sim C2-C13A
 with sigma of 0.04
 C2-C12 \\sim C2-C12A
 with sigma of 0.04
 C2-C14 \\sim C2-C14A
 with sigma of 0.04
 C13-C12 \\sim C13A-C12A
 with sigma of 0.04
 C13-C14 \\sim C13A-C14A
 with sigma of 0.04
 C12-C14 \\sim C12A-C14A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C18 \\sim C17 \\sim C19: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.005 within 2A
5. Rigid body (RIGU) restrains
 C5, Bi1, Fe1, O1, N1, N2, O2, C35, C37A, C38A, C39A, C40A, C41A, C36B, C37B,
 C38B, C39B, C40B, C41B, C36A, C1, C6, C15, C20, C21, C26, O3, O1B, O4A, C2,
 C16, C19, C22, C25, C3, C11, C11A, C4, C17, C18, C23, C27, C24, C13, C12, C14,
 C13A, C12A, C14A, C7, C31, C28, C30, C29, C10, C9, C8, C32, C34, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41B, C40B, C37B, C38B, C39B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41A, C40A, C39A, C38A, C37A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C13, C12, C11, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C14A, C13A, C11A, C12A, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C11A)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C11)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
 Fixed Sof: C37A(0.5) H37A(0.5) C38A(0.5) H38A(0.5) C39A(0.5) H39A(0.5)
 C40A(0.5) H40A(0.5) C41A(0.5) H41A(0.5) O1B(0.5) C36B(0.5) C37B(0.5) H37B(0.5)
 C38B(0.5) H38B(0.5) C39B(0.5) H39B(0.5) C40B(0.5) H40B(0.5) C41B(0.5)
 H41B(0.5) O4A(0.5) C36A(0.5)
7.a Ternary CH refined with riding coordinates:
 C38A(H38A), C38B(H38B), C39B(H39B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C24(H24), C22(H22), C18(H18), C16(H16), C17(H17), C19(H19),
 C37A(H37A), C39A(H39A), C40A(H40A), C41A(H41A), C37B(H37B), C40B(H40B),
 C41B(H41B)
7.c Fitted pentagon refined as free rotating group:
 C37A(C38A,C39A,C40A,C41A), C37B(C38B,C39B,C40B,C41B)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C13(H13A,H13B,
 H13C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C),
 C14(H14A,H14B,H14C), C13A(H13D,H13E,H13F), C12A(H12D,H12E,H12F), C14A(H14D,
 H14E,H14F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.264
_shelx_estimated_absorpt_t_max   0.431
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              87572