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_7714444
_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         'C20 H24 Cl F3 N Ni O P'
_chemical_formula_sum            'C20 H24 Cl F3 N Ni O P'
_chemical_formula_weight         476.53
_chemical_name_systematic        CF3-tBu-POCNP-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
_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
;
2023-07-21 deposited with the CCDC.	2023-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.397(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3139(3)
_cell_length_b                   10.1907(2)
_cell_length_c                   15.4819(4)
_cell_measurement_reflns_used    5175
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      71.3380
_cell_measurement_theta_min      5.1350
_cell_volume                     2130.14(9)
_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      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_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    -52.00 -26.00   1.00    5.59    --  -35.62  58.00-113.00   26
  2  \w    -96.00 -35.00   1.00    5.59    --  -35.62 -58.00 105.00   61
  3  \w     -3.00  31.00   1.00    5.59    --  -35.62  58.00-113.00   34
  4  \w     26.00  53.00   1.00    5.59    --   35.62 -58.00 105.00   27
  5  \w     44.00 119.00   1.00   22.34    --  107.12 -58.00 105.00   75
  6  \w    112.00 174.00   1.00   22.34    --  107.12  58.00-113.00   62
  7  \w     57.00 104.00   1.00    5.59    --   35.62 178.00 150.00   47
  8  \w     67.00 103.00   1.00    5.59    --   35.62  77.00-120.00   36
  9  \w      9.00  53.00   1.00    5.59    --   35.62  77.00-120.00   44
 10  \w     60.00  98.00   1.00    5.59    --   35.62 178.00  60.00   38
 11  \w      5.00  73.00   1.00    5.59    --   35.62 -99.00 120.00   68
 12  \w     14.00  75.00   1.00    5.59    --   35.62 -99.00 -60.00   61
 13  \w     39.00  64.00   1.00    5.59    --   35.62  58.00-113.00   25
 14  \w     38.00 100.00   1.00   22.34    --  107.12 -95.00  30.00   62
 15  \w     49.00  89.00   1.00   22.34    --  107.12-111.00 120.00   40
 16  \w     37.00 129.00   1.00   22.34    --  107.12 -30.00-180.00   92
 17  \w     78.00 104.00   1.00   22.34    --  107.12 -95.00 -90.00   26
 18  \w     77.00 113.00   1.00   22.34    --  107.12-111.00 150.00   36
 19  \w    103.00 129.00   1.00   22.34    --  107.12 111.00   0.00   26
 20  \w     42.00  68.00   1.00   22.34    --  107.12-111.00 150.00   26
 21  \w     95.00 137.00   1.00   22.34    --  107.12  45.00-150.00   42
 22  \w     39.00 110.00   1.00   22.34    --  107.12-111.00 -30.00   71
;
_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      0.0004220000
_diffrn_orient_matrix_UB_12      -0.1033773000
_diffrn_orient_matrix_UB_13      -0.0725029000
_diffrn_orient_matrix_UB_21      0.1139222000
_diffrn_orient_matrix_UB_22      0.0072283000
_diffrn_orient_matrix_UB_23      0.0310638000
_diffrn_orient_matrix_UB_31      0.0070504000
_diffrn_orient_matrix_UB_32      -0.1099798000
_diffrn_orient_matrix_UB_33      0.0700794000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9153
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.484
_diffrn_reflns_theta_min         3.647
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.505
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76179
_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    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.510
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4075
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1231P)^2^+6.9550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2154
_refine_ls_wR_factor_ref         0.2242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3538
_reflns_number_total             4075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03109h2.cif
_cod_data_source_block           mjx-20220520
_cod_database_code               7714444
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'N1 C1 P1 F1 Ni1 O1 S1'
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.966
_diffrn_oxdiff_digest_frames
;
016c25d81c354d2c6b7427ac5be5a95b2f00027349f
;
_diffrn_oxdiff_digest_hkl
;
01bde0c12207b0e2cd08aa8ecbbde59ee6a337
;
_reflns_odcompleteness_completeness 99.93
_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. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3: within 4.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C5(H5), C4(H4), C8(H8), C3(H3)
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              59230
_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 1.798
_oxdiff_exptl_absorpt_empirical_full_min 0.201