Combining geometric constraint and redox non-innocence within an ambiphilic PBiP pincer ligand.
Coburger, Peter; Buzanich, Ana Guilherme; Emmerling, Franziska; Abbenseth, Josh; Chemical science 15 (2024) 6036–6043; doi:10.1039/d4sc00197d

data_1571258
_publ_section_title
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 Combining geometric constraint and redox non-innocence within an
 ambiphilic PBiP pincer ligand.
;
_journal_issue                   16
_journal_name_full               'Chemical science'
_journal_page_first              6036
_journal_page_last               6043
_journal_paper_doi               10.1039/d4sc00197d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C46 H40 Bi N3 O3 P2 W, 1[C7H8]'
_chemical_formula_sum            'C53 H48 Bi N3 O3 P2 W'
_chemical_formula_weight         1229.760
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-18 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                92.010(2)
_cell_angle_beta                 101.049(2)
_cell_angle_gamma                103.267(2)
_cell_formula_units_Z            4
_cell_length_a                   10.9439(7)
_cell_length_b                   21.0052(10)
_cell_length_c                   21.9721(12)
_cell_measurement_reflns_used    2551
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      21.78
_cell_measurement_theta_min      2.50
_cell_volume                     4808.4(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9942
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1025
_diffrn_reflns_av_unetI/netI     0.1049
_diffrn_reflns_Laue_measured_fraction_full 0.9982
_diffrn_reflns_Laue_measured_fraction_max 0.9942
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58362
_diffrn_reflns_point_group_measured_fraction_full 0.9982
_diffrn_reflns_point_group_measured_fraction_max 0.9942
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.97
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.157
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1094 before and 0.0684 after correction.
The Ratio of minimum to maximum transmission is 0.7092.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       block
_exptl_crystal_F_000             2379.248
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.6167
_refine_diff_density_min         -1.8077
_refine_diff_density_rms         0.2775
_refine_ls_d_res_high            0.8275
_refine_ls_d_res_low             10.3458
_refine_ls_goodness_of_fit_ref   0.9746
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    141
_refine_ls_number_parameters     987
_refine_ls_number_reflns         17672
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.9746
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                11050
_reflns_number_total             17672
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4sc00197d2.cif
_cod_data_source_block           mo_ja23_JA_i_85_0m_a
_cod_depositor_comments
'Adding full bibliography for 1571257--1571259.cif.'
_cod_original_formula_sum        'C53 H48 Bi1 N3 O3 P2 W1'
_cod_database_code               1571258
_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
 C71-C76 = C71-C72
 1.395 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24)
4.a Secondary CH2 refined with riding coordinates:
 C92(H92a,H92b), C64(H64a,H64b), C31(H31a,H31b), C18(H18a,H18b)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C33(H33), C43(H43), C51(H51), C57(H57), C86(H86), C79(H79),
 C88(H88), C82(H82), C9(H9), C87(H87), C49(H49), C72(H72), C70(H70), C3(H3),
 C76(H76), C20(H20), C78(H78), C37(H37), C39(H39), C42(H42), C55(H55), C80(H80),
  C84(H84), C27(H27), C69(H69), C24(H24), C73(H73), C75(H75), C74(H74), C5(H5),
 C34(H34), C29(H29), C28(H28), C30(H30), C26(H26), C81(H81), C36(H36), C23(H23),
  C68(H68), C35(H35), C40(H40), C22(H22), C66(H66), C85(H85), C41(H41),
 C67(H67), C21(H21)
4.c Idealised Me refined as rotating group:
 C60(H60a,H60b,H60c), C16(H16a,H16b,H16c), C15(H15a,H15b,H15c), C62(H62a,H62b,
 H62c), C17(H17a,H17b,H17c), C61(H61a,H61b,H61c), C63(H63a,H63b,H63c), C14(H14a,
 H14b,H14c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'