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_7714441
_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         'C19 H25 Cl N Ni O P'
_chemical_formula_sum            'C19 H25 Cl N Ni O P'
_chemical_formula_weight         408.53
_chemical_name_systematic        tBu-PCN-Ni-Cl
_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
_audit_creation_date             2022-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-21 deposited with the CCDC.	2023-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8845(2)
_cell_length_b                   12.3506(2)
_cell_length_c                   13.4163(2)
_cell_measurement_reflns_used    5418
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      71.4970
_cell_measurement_theta_min      4.8780
_cell_volume                     1950.56(5)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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   -103.00 -12.00   1.00    1.00    --  -35.62 -75.00 -78.00   91
  2  \w    -15.00  10.00   1.00    1.00    --  -35.62  75.00  49.00   25
  3  \w    -10.00  15.00   1.00    1.00    --   35.62 -75.00 -78.00   25
  4  \w     87.00 113.00   1.00    2.26    --  107.12 -75.00 -78.00   26
  5  \w     44.00  73.00   1.00    2.26    --  107.12 -75.00 -78.00   29
  6  \w    128.00 174.00   1.00    2.26    --  107.12  75.00  49.00   46
  7  \w    -96.00 -36.00   1.00    1.00    --  -35.62-178.00 -90.00   60
  8  \w    -16.00  10.00   1.00    1.00    --  -35.62  77.00-150.00   26
  9  \w    -61.00 -32.00   1.00    1.00    --  -35.62  77.00-150.00   29
 10  \w     76.00 108.00   1.00    1.00    --   35.62-178.00 -30.00   32
 11  \w     55.00 107.00   1.00    1.00    --   35.62-178.00-150.00   52
 12  \w     56.00  93.00   1.00    1.00    --   35.62  75.00  49.00   37
 13  \w     57.00  95.00   1.00    1.00    --   35.62 178.00-120.00   38
 14  \w     50.00  76.00   1.00    2.26    --  107.12-111.00-180.00   26
 15  \w     83.00 171.00   1.00    2.26    --  107.12  77.00   0.00   88
 16  \w     60.00 150.00   1.00    2.26    --  107.12 178.00 150.00   90
 17  \w     46.00 105.00   1.00    2.26    --  107.12-111.00 -90.00   59
 18  \w     85.00 110.00   1.00    2.26    --  107.12 -95.00 -90.00   25
 19  \w     37.00  85.00   1.00    2.26    --  107.12 -15.00  90.00   48
 20  \w    102.00 145.00   1.00    2.26    --  107.12 -15.00  90.00   43
 21  \w     85.00 111.00   1.00    2.26    --  107.12-111.00-180.00   26
 22  \w     81.00 135.00   1.00    2.26    --  107.12 178.00 -60.00   54
;
_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      -0.0785005000
_diffrn_orient_matrix_UB_12      0.0996113000
_diffrn_orient_matrix_UB_13      -0.0154069000
_diffrn_orient_matrix_UB_21      -0.0243733000
_diffrn_orient_matrix_UB_22      -0.0251353000
_diffrn_orient_matrix_UB_23      -0.1133448000
_diffrn_orient_matrix_UB_31      -0.1018847000
_diffrn_orient_matrix_UB_32      -0.0707201000
_diffrn_orient_matrix_UB_33      0.0186348000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8433
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.437
_diffrn_reflns_theta_min         4.663
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65340
_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    1.391
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3719
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0441P)^2^+0.4393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3296
_reflns_number_total             3719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03109h2.cif
_cod_data_source_block           dm-20211210-c
_cod_database_code               7714441
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'P1 C1 Ni1 N1'
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.933
_diffrn_oxdiff_digest_frames
;
0128b21cd47e93e0c0421e7c59f849902d00030ddd0
;
_diffrn_oxdiff_digest_hkl
;
01bf9e3d412ff0c200af7ec03bd2706b9c5c1a
;
_reflns_odcompleteness_completeness 99.95
_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. Rigid bond restraints
 O1, P1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O1, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 P1, O1
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C9(H9)
3.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C18(H18A,H18B,
 H18C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              94058
_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 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.674