Reversible CO binding at a nickel complex supported by an ambiphilic PBiP tridentate ligand.
Yoo, Dagyum; Brannan, Alexander C.; Lim, Soohyun; Lee, Heui Beom; Lee, Yunho; Chemical communications (Cambridge, England) 61 (2025) 11453–11456; doi:10.1039/d5cc02850g

data_7134759
_publ_section_title
;
 Reversible CO binding at a nickel complex supported by an ambiphilic PBiP
 tridentate ligand.
;
_journal_issue                   61
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11453
_journal_page_last               11456
_journal_paper_doi               10.1039/d5cc02850g
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C24 H36 Bi Cl Ni P2'
_chemical_formula_sum            'C24 H36 Bi Cl Ni P2'
_chemical_formula_weight         689.61
_chemical_properties_physical    Air-sensitive,Moisture-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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-02
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-13 deposited with the CCDC.	2025-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.5020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.92990(10)
_cell_length_b                   15.7754(2)
_cell_length_c                   20.8624(2)
_cell_measurement_reflns_used    14081
_cell_measurement_temperature    100
_cell_measurement_theta_max      78.9620
_cell_measurement_theta_min      3.5190
_cell_volume                     2609.73(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00  89.00   0.50    1.13    --    0.00  57.00 -90.00  232
  2  \w    -33.00  24.00   0.50    1.13    --    0.00  77.00  60.00  114
  3  \w     26.00  86.00   0.50    1.13    --    0.00  77.00  60.00  120
  4  \w     61.00 126.00   0.50    1.00    --  105.20 -61.00  90.00  130
  5  \w     19.00 140.00   0.50    1.00    --  105.20 -82.00  90.00  242
  6  \w     30.00 131.00   0.50    1.00    --  105.20 -45.00 -90.00  202
  7  \w     76.00 103.00   0.50    1.00    --  105.20 -45.00  90.00   54
  8  \w     83.00 134.00   0.50    1.00    --  105.20  77.00-150.00  102
  9  \w     84.00 180.00   0.50    1.00    --  105.20  82.00  30.00  192
 10  \w     18.00  44.00   0.50    1.00    --  105.20 -61.00  90.00   52
 11  \w     17.00  43.00   0.50    1.00    --  105.20 -61.00   0.00   52
 12  \w     84.00 121.00   0.50    1.00    --  105.20 -61.00   0.00   74
 13  \w     16.00 126.00   0.50    1.00    --  105.20 -61.00 -90.00  220
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1052420000
_diffrn_orient_matrix_UB_12      0.0759568000
_diffrn_orient_matrix_UB_13      -0.0235576000
_diffrn_orient_matrix_UB_21      -0.1596799000
_diffrn_orient_matrix_UB_22      -0.0557145000
_diffrn_orient_matrix_UB_23      -0.0003108000
_diffrn_orient_matrix_UB_31      -0.0344928000
_diffrn_orient_matrix_UB_32      0.0253226000
_diffrn_orient_matrix_UB_33      0.0700577000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16407
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.845
_diffrn_reflns_theta_min         3.513
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    16.131
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.144
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       0.00039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+9.7998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5449
_reflns_number_total             5517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02850g2.cif
_cod_data_source_block           bip2nicl
_cod_depositor_comments
'Adding full bibliography for 7134759--7134764.cif.'
_cod_database_code               7134759
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C H P Cl Bi Ni'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_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.a Ternary CH refined with riding coordinates:
 C20(H20), C17(H17), C23(H23), C14(H14)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C3(H3), C4(H4), C6(H6), C12(H12), C9(H9), C5(H5)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C24(H24A,H24B,
 H24C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C13(H13A,
 H13B,H13C)
;
_shelx_res_checksum              18421
_shelx_hkl_checksum              84017
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.893
_oxdiff_exptl_absorpt_empirical_full_min 0.568