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_1575599
_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         'C18 H36 K N2 O6, C34 H44 N2 O2 P'
_chemical_formula_sum            'C52 H80 K N4 O8 P'
_chemical_formula_weight         959.27
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-05-27
_audit_creation_method
;FinalCif V151 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-06-05 deposited with the CCDC.	2025-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.68860(10)
_cell_length_b                   13.68860(10)
_cell_length_c                   49.9629(9)
_cell_measurement_reflns_used    9224
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      78.460
_cell_measurement_theta_min      3.729
_cell_volume                     8107.68(17)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 0.994
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1083
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            216313
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.233
_diffrn_reflns_theta_min         3.728
_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
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_T_max  0.8959
_exptl_absorpt_correction_T_min  0.7011
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1188 before and 0.0994 after correction.
The Ratio of minimum to maximum transmission is 0.7826.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       needle
_exptl_crystal_F_000             3108
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 4615 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         11488
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0808P)^2^+2.9608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                10426
_reflns_number_total             11488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03374h3.cif
_cod_data_source_block           cu_1307_cg_0m
_cod_original_cell_volume        8107.67(19)
_cod_database_code               1575599
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.753
_shelx_estimated_absorpt_t_max   0.916
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_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. Uiso/Uaniso restraints and constraints
C11A \\sim C11B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C27B \\sim C27A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
3. Rigid body (RIGU) restrains
 C11B, C12B, C13B, C14B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C28A, C27A, C29A, C30A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C30B, C27B, C29B, C28B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C27B)=1-FVAR(1)
 Sof(C27A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13B)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C11B)=1-FVAR(2)
 Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13A)=Sof(H13A)=
 Sof(H13B)=Sof(H13C)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
  C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B)
5.b Me refined with riding coordinates:
 C12A(H12A,H12B,H12C), C12B(H12D,H12E,H12F), C13A(H13A,H13B,H13C), C13B(H13D,
 H13E,H13F), C14A(H14A,H14B,H14C), C14B(H14D,H14E,H14F), C28A(H28A,H28B,H28C),
 C28B(H28D,H28E,H28F), C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C30A(H30A,
 H30B,H30C), C30B(H30D,H30E,H30F)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C26(H26)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              99194