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_1575603
_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_formula_moiety         '4(C41 H49 As Fe N2 O4), 3(C2 H3 N)'
_chemical_formula_sum            'C170 H205 As4 Fe4 N11 O16'
_chemical_formula_weight         3181.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-28
_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                 90.710(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1002(7)
_cell_length_b                   24.3068(19)
_cell_length_c                   29.174(2)
_cell_measurement_reflns_used    9381
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.570
_cell_measurement_theta_min      2.256
_cell_volume                     7870.8(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
'Bruker BIS V6.2.15/2021-03-16 && 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 0.999
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_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  0.0522
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            153146
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.595
_diffrn_reflns_theta_min         2.127
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6913
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1164 before and 0.0504 after correction.
The Ratio of minimum to maximum transmission is 0.6913.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       needle
_exptl_crystal_F_000             3332
_exptl_crystal_recrystallization_method 'from acetonitrile.'
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     963
_refine_ls_number_reflns         26489
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+3.9605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22520
_reflns_number_total             26489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03374h3.cif
_cod_data_source_block           mo_2026_cg_0m
_cod_original_cell_volume        7870.9(10)
_cod_database_code               1575603
_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
 N6-C85
 1.14 with sigma of 0.02
 C85-C86
 1.46 with sigma of 0.02
 N6-C86
 2.59 with sigma of 0.04
3. Others
 Fixed Sof: N6(0.5) C85(0.5) C86(0.5) H86A(0.5) H86B(0.5) H86C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C65(H65), C17(H17), C20(H20), C82(H82), C5(H5), C67(H67), C58(H58), C81(H81),
 C3(H3), C47(H47), C60(H60), C26(H26), C24(H24), C59(H59), C61(H61), C45(H45),
 C78(H78), C19(H19), C39(H39), C38(H38), C80(H80), C40(H40), C18(H18), C79(H79),
  C37(H37), C41(H41)
4.b Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C75(H75A,H75B,
 H75C), C49(H49A,H49B,H49C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C51(H51A,
 H51B,H51C), C74(H74A,H74B,H74C), C69(H69A,H69B,H69C), C53(H53A,H53B,H53C),
 C13(H13A,H13B,H13C), C50(H50A,H50B,H50C), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C), C55(H55A,H55B,H55C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C33(H33A,
 H33B,H33C), C71(H71A,H71B,H71C), C9(H9A,H9B,H9C), C29(H29A,H29B,H29C),
 C70(H70A,H70B,H70C), C84(H84A,H84B,H84C), C54(H54A,H54B,H54C), C86(H86A,H86B,
 H86C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.579
_shelx_estimated_absorpt_t_max   0.909
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              42623