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_7714443
_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 H27 Cl N Ni O P'
_chemical_formula_sum            'C20 H27 Cl N Ni O P'
_chemical_formula_weight         422.55
_chemical_name_systematic        Me-tBu-POCN-Ni-Cl
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5348(2)
_cell_length_b                   12.0028(2)
_cell_length_c                   14.9796(3)
_cell_measurement_reflns_used    4236
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.4010
_cell_measurement_theta_min      4.7090
_cell_volume                     2073.92(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (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      149.99(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    -68.00   1.00   1.00    1.05    --  -35.62 107.00 175.00   69
  2  \w     33.00  58.00   1.00    1.05    --   35.62  70.00 -66.00   25
  3  \w     16.00  78.00   1.00    1.05    --   35.62-107.00  77.00   62
  4  \w    104.00 141.00   1.00    4.19    --  107.12  70.00 -66.00   37
  5  \w    100.00 150.00   1.00    4.19    --  107.12  55.00  91.00   50
  6  \w     61.00  86.00   1.00    4.19    --  107.12 -70.00 162.00   25
  7  \w     44.00  70.00   1.00    4.19    --  107.12-107.00  77.00   26
  8  \w   -101.00 -39.00   1.00    1.05    --  -35.62 -57.00 120.00   62
  9  \w     58.00  84.00   1.00    1.05    --   35.62 178.00  90.00   26
 10  \w    139.00 176.00   1.00    4.19    --  107.12  45.00-150.00   37
 11  \w     40.00  66.00   1.00    4.19    --  107.12 -95.00  30.00   26
 12  \w     91.00 136.00   1.00    4.19    --  107.12  45.00-150.00   45
 13  \w     38.00 110.00   1.00    4.19    --  107.12 -95.00-180.00   72
 14  \w     38.00  98.00   1.00    4.19    --  107.12 -95.00 -60.00   60
;
_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      0.0773685000
_diffrn_orient_matrix_UB_12      0.0678965000
_diffrn_orient_matrix_UB_13      -0.0639703000
_diffrn_orient_matrix_UB_21      -0.1040560000
_diffrn_orient_matrix_UB_22      0.0746583000
_diffrn_orient_matrix_UB_23      -0.0237251000
_diffrn_orient_matrix_UB_31      0.0322545000
_diffrn_orient_matrix_UB_32      0.0792747000
_diffrn_orient_matrix_UB_33      0.0769137000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6014
_diffrn_reflns_point_group_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.541
_diffrn_reflns_theta_min         4.721
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.312
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (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    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1170 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(14)
_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     233
_refine_ls_number_reflns         3510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0335P)^2^+0.2878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.558
_reflns_Friedel_fraction_full    0.756
_reflns_Friedel_fraction_max     0.721
_reflns_number_gt                3393
_reflns_number_total             3510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03109h2.cif
_cod_data_source_block           mjx-20220322
_cod_database_code               7714443
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 N1 P1 Ni1 Cl1'
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.937
_diffrn_oxdiff_digest_frames
;
01d67f6ba11519a5d6d6e7b9d62941ed7200031ac49
;
_diffrn_oxdiff_digest_hkl
;
01197451003209decacde95465822828af668b
;
_reflns_odcompleteness_completeness 99.86
_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:
 C8(H8), C11(H11), C5(H5), C4(H4), C10(H10), C3(H3)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C15(H15A,H15B,
 H15C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              11857
_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 1.745
_oxdiff_exptl_absorpt_empirical_full_min 0.754