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_7714442
_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 H26 N Ni O P S'
_chemical_formula_sum            'C19 H26 N Ni O P S'
_chemical_formula_weight         406.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-10-08
_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                 117.900(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3743(5)
_cell_length_b                   8.0671(2)
_cell_length_c                   16.2293(5)
_cell_measurement_reflns_used    4354
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.2720
_cell_measurement_theta_min      5.4490
_cell_volume                     1894.60(12)
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_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    -16.00  16.00   1.00    3.87    --  -35.62  17.00-113.00   32
  2  \w   -107.00  -2.00   1.00    3.87    --  -35.62 -17.00  77.00  105
  3  \w     -7.00  18.00   1.00    3.87    --   35.62 -17.00  77.00   25
  4  \w     30.00  55.00   1.00    3.87    --   35.62  17.00-113.00   25
  5  \w    101.00 126.00   1.00   15.47    --  107.12  17.00-113.00   25
  6  \w     38.00 115.00   1.00   15.47    --  107.12 -17.00  77.00   77
  7  \w   -106.00 -53.00   1.00    3.87    --  -35.62 178.00   0.00   53
  8  \w    -65.00 -40.00   1.00    3.87    --  -35.62-178.00 -30.00   25
  9  \w     20.00 101.00   1.00    3.87    --   35.62  57.00  60.00   81
 10  \w      1.00  63.00   1.00    3.87    --   35.62 -99.00   0.00   62
 11  \w     61.00  86.00   1.00    3.87    --   35.62-178.00  90.00   25
 12  \w     40.00 128.00   1.00   15.47    --  107.12 -30.00-150.00   88
 13  \w     86.00 177.00   1.00   15.47    --  107.12  30.00 -90.00   91
 14  \w     40.00 123.00   1.00   15.47    --  107.12 -61.00 150.00   83
 15  \w     41.00  91.00   1.00   15.47    --  107.12 -95.00   0.00   50
 16  \w     51.00  77.00   1.00   15.47    --  107.12 -95.00-150.00   26
 17  \w     81.00 123.00   1.00   15.47    --  107.12 -77.00-150.00   42
 18  \w     40.00  65.00   1.00   15.47    --  107.12 -77.00-150.00   25
;
_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      -0.0510366000
_diffrn_orient_matrix_UB_12      -0.0410098000
_diffrn_orient_matrix_UB_13      -0.1048439000
_diffrn_orient_matrix_UB_21      0.0915929000
_diffrn_orient_matrix_UB_22      0.0141919000
_diffrn_orient_matrix_UB_23      -0.0046283000
_diffrn_orient_matrix_UB_31      0.0182801000
_diffrn_orient_matrix_UB_32      -0.1860008000
_diffrn_orient_matrix_UB_33      0.0227825000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7590
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.434
_diffrn_reflns_theta_min         5.454
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62111
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.414
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3584
_refine_ls_number_restraints     828
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0942
_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^)+(0.0525P)^2^+36.5272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2522
_refine_ls_wR_factor_ref         0.2570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3068
_reflns_number_total             3584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03109h2.cif
_cod_data_source_block           mjx-20220915
_cod_original_cell_volume        1894.60(11)
_cod_database_code               7714442
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'N1 C1 P1 Ni1 O1 S1'
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.851
_diffrn_oxdiff_digest_frames
;
015b8d7dc5937d1d54eca839e19829d9420002883a6
;
_diffrn_oxdiff_digest_hkl
;
019897e8f18945d0d17f08935eac8cd213ac9e
;
_reflns_odcompleteness_completeness 99.75
_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
C2 \\sim C7 \\sim C1 \\sim C6 \\sim C3 \\sim C5 \\sim C11 \\sim C8 \\sim C16
\\sim C12 \\sim C4 \\sim C9 \\sim C18 \\sim C10 \\sim C15 \\sim C17 \\sim C19
\\sim C13 \\sim C14: within 6.6A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C8(H8), C4(H4), C9(H9), C10(H10)
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              59515
_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 3.686
_oxdiff_exptl_absorpt_empirical_full_min 0.385