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_1571259
_publ_section_title
;
 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         'C43 H40 Bi N3 P2'
_chemical_formula_sum            'C43 H40 Bi N3 P2'
_chemical_formula_weight         869.745
_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             2023-10-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-19 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                72.803(4)
_cell_angle_beta                 83.022(3)
_cell_angle_gamma                86.907(3)
_cell_formula_units_Z            4
_cell_length_a                   12.5454(10)
_cell_length_b                   14.8524(15)
_cell_length_c                   20.970(2)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      2.20
_cell_volume                     3704.3(6)
_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      100.00
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9961
_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  0.0972
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.9995
_diffrn_reflns_Laue_measured_fraction_max 0.9961
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            153010
_diffrn_reflns_point_group_measured_fraction_full 0.9995
_diffrn_reflns_point_group_measured_fraction_max 0.9961
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.99
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.880
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0952 before and 0.0708 after correction.
The Ratio of minimum to maximum transmission is 0.8356.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       plate
_exptl_crystal_F_000             1716.399
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.0788
_refine_diff_density_min         -1.6544
_refine_diff_density_rms         0.2243
_refine_ls_d_res_high            0.7474
_refine_ls_d_res_low             10.2288
_refine_ls_goodness_of_fit_ref   1.0131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    140
_refine_ls_number_parameters     891
_refine_ls_number_reflns         18487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0131
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+8.3695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              19
_reflns_limit_k_min              -18
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                13910
_reflns_number_total             18487
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4sc00197d2.cif
_cod_data_source_block           mo_ja23_ja_ii_18_0m_a
_cod_depositor_comments
'Adding full bibliography for 1571257--1571259.cif.'
_cod_original_cell_volume        3704.2(6)
_cod_database_code               1571259
_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.a Secondary CH2 refined with riding coordinates:
 C74(H74a,H74b), C61(H61a,H61b), C31(H31a,H31b), C18(H18a,H18b)
2.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C54(H54), C76(H76), C30(H30), C11(H11), C52(H52), C77(H77),
 C48(H48), C9(H9), C5(H5), C3(H3), C64(H64), C65(H65), C86(H86), C70(H70),
 C43(H43), C69(H69), C82(H82), C26(H26), C78(H78), C83(H83), C73(H73), C24(H24),
  C66(H66), C80(H80), C63(H63), C67(H67), C22(H22), C20(H20), C37(H37),
 C29(H29), C71(H71), C79(H79), C42(H42), C72(H72), C23(H23), C21(H21), C33(H33),
  C28(H28), C85(H85), C84(H84), C35(H35), C40(H40), C39(H39), C36(H36),
 C27(H27), C34(H34), C41(H41)
2.c Idealised Me refined as rotating group:
 C59(H59a,H59b,H59c), C58(H58a,H58b,H58c), C57(H57a,H57b,H57c), C15(H15a,H15b,
 H15c), C60(H60a,H60b,H60c), C17(H17a,H17b,H17c), C14(H14a,H14b,H14c), C16(H16a,
 H16b,H16c)
;
_olex2_submission_special_instructions 'No special instructions were received'