Structures of nickel chloride and thiolate complexes supported by PCN and POCOP pincer ligands and catalytic reactivity of the chloride complexes
Mao, Jia-Xue; Chang, Jiarui; Zhang, Jie; Chen, Xuenian; Dalton Transactions  (2023) –; doi:10.1039/D3DT03109H

data_7714445
_publ_section_title
;
 Structures of nickel chloride and thiolate complexes supported by PCN and
 POCOP pincer ligands and catalytic reactivity of the chloride complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03109H
_journal_year                    2023
_chemical_formula_moiety         'C25 H30 N Ni O P S'
_chemical_formula_sum            'C25 H30 N Ni O P S'
_chemical_formula_weight         482.24
_chemical_name_systematic        tBu-POCN-Ni-SPh
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-09-07 deposited with the CCDC.	2023-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.4614(2)
_cell_length_b                   12.6536(2)
_cell_length_c                   19.6198(2)
_cell_measurement_reflns_used    8202
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.5390
_cell_measurement_theta_min      4.5080
_cell_volume                     4583.25(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_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    -11.00  15.00   1.00    1.00    --  -35.62  91.00  -0.00   26
  2  \w    -59.00 -34.00   1.00    1.00    --  -35.62  91.00  -0.00   25
  3  \w     23.00  48.00   1.00    1.00    --   35.62-112.00 160.00   25
  4  \w    116.00 142.00   1.00    1.62    --  107.12  35.00 172.00   26
  5  \w     47.00 112.00   1.00    1.62    --  107.12-112.00 160.00   65
  6  \w     64.00 123.00   1.00    1.62    --  107.12 -91.00-114.00   59
  7  \w   -104.00 -17.00   1.00    1.00    --  -35.62 -38.00 150.00   87
  8  \w     20.00  63.00   1.00    1.00    --   35.62  57.00 -30.00   43
  9  \w     65.00 105.00   1.00    1.00    --   35.62-178.00  60.00   40
 10  \w     57.00  92.00   1.00    1.00    --   35.62 178.00-120.00   35
 11  \w     90.00 173.00   1.00    1.62    --  107.12  61.00 150.00   83
 12  \w     44.00  97.00   1.00    1.62    --  107.12-111.00-150.00   53
 13  \w     39.00 104.00   1.00    1.62    --  107.12 -95.00  30.00   65
 14  \w     74.00 112.00   1.00    1.62    --  107.12 -35.00  15.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0728310000
_diffrn_orient_matrix_UB_12      -0.0591806000
_diffrn_orient_matrix_UB_13      0.0023232000
_diffrn_orient_matrix_UB_21      0.0372500000
_diffrn_orient_matrix_UB_22      0.0942462000
_diffrn_orient_matrix_UB_23      -0.0354265000
_diffrn_orient_matrix_UB_31      0.0163620000
_diffrn_orient_matrix_UB_32      0.0494228000
_diffrn_orient_matrix_UB_33      0.0700475000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13054
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.603
_diffrn_reflns_theta_min         4.507
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.855
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0481P)^2^+2.5713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3897
_reflns_number_total             4373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03109h2.cif
_cod_data_source_block           20220511-mjx
_cod_database_code               7714445
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 P1 Ni1 S1 N1 O1'
_diffrn_oxdiff_digest_frames
;
01884cf2744b33d51b6f24fac5b69ada2400028da17
;
_diffrn_oxdiff_digest_hkl
;
0147c9710f50311abde2807cc8c9befd4f456c
;
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C17(H17), C13(H13), C8(H8), C11(H11), C4(H4), C9(H9),
 C10(H10), C14(H14), C16(H16), C15(H15)
2.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C24(H24A,H24B,
 H24C), C23(H23A,H23B,H23C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              93982
_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 1.584
_oxdiff_exptl_absorpt_empirical_full_min 0.785