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_1571257
_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         'C43 H43 N3 P2'
_chemical_formula_sum            'C43 H43 N3 P2'
_chemical_formula_weight         663.788
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-12-13
_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                90
_cell_angle_beta                 92.258(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4142(13)
_cell_length_b                   15.1667(13)
_cell_length_c                   18.9994(18)
_cell_measurement_reflns_used    9177
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.41
_cell_volume                     3574.5(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      100.0
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9981
_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  0.0556
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.9983
_diffrn_reflns_Laue_measured_fraction_max 0.9981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            135973
_diffrn_reflns_point_group_measured_fraction_full 0.9983
_diffrn_reflns_point_group_measured_fraction_max 0.9981
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1035 before and 0.0644 after correction.
The Ratio of minimum to maximum transmission is 0.9519.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1409.507
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.9742
_refine_diff_density_min         -0.4898
_refine_diff_density_rms         0.0581
_refine_ls_d_res_high            0.6989
_refine_ls_d_res_low             9.6020
_refine_ls_goodness_of_fit_ref   1.0422
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    70
_refine_ls_number_parameters     449
_refine_ls_number_reflns         10939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0422
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+1.8735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -17
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -13
_reflns_number_gt                9699
_reflns_number_total             10939
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4sc00197d2.cif
_cod_data_source_block           mo_ja23_117_0m_a
_cod_depositor_comments
'Adding full bibliography for 1571257--1571259.cif.'
_cod_database_code               1571257
_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:
 C18(H18a,H18b), C31(H31a,H31b)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3a), C5(H5), C9(H9), C11(H11), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
  C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43)
2.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C17(H17a,H17b,
 H17c)
;
_olex2_submission_special_instructions 'No special instructions were received'