The new dual anion solvent-free nickel complex based on the pyridine-4-carbohydrazide ligand
Kuang, Bao-long; Zhao, Bin-shan; Lu, Zu-jia; Wang, Ting-wei; Xie, Zhi-ming; Sun, Mou; Yu, Qi-yao; Zhang, Jian-guo; New Journal of Chemistry 48 (2024) 12873–12876; doi:10.1039/D4NJ02087A

data_7063284
_publ_section_title
;
 The new dual anion solvent-free nickel complex based on the
 pyridine-4-carbohydrazide ligand
;
_journal_issue                   29
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12873
_journal_page_last               12876
_journal_paper_doi               10.1039/D4NJ02087A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C12 H16 N8 Ni O8, 2(Cl O4)'
_chemical_formula_sum            'C12 H16 Cl2 N8 Ni O16'
_chemical_formula_weight         657.94
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-05-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-06-11 deposited with the CCDC.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.269(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1017(4)
_cell_length_b                   15.6632(7)
_cell_length_c                   14.8448(8)
_cell_measurement_reflns_used    2911
_cell_measurement_temperature    120.65(10)
_cell_measurement_theta_max      27.9420
_cell_measurement_theta_min      3.9550
_cell_volume                     2265.90(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.65(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0971
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.8237
_diffrn_measurement_details
;
  1 omega   10.00   76.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       16.0852   57.0000   90.0000 66

  2 omega   51.00   83.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       16.0852   57.0000  120.0000 32

  3 omega  -19.00   41.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       16.0852  -99.0000    0.0000 60

  4 omega  -10.00   24.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0070  -99.0000 -150.0000 34

  5 omega   19.00   78.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       16.0852   57.0000 -150.0000 59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0410816000
_diffrn_orient_matrix_UB_12      0.0173946000
_diffrn_orient_matrix_UB_13      0.0422883000
_diffrn_orient_matrix_UB_21      0.0496060000
_diffrn_orient_matrix_UB_22      -0.0325249000
_diffrn_orient_matrix_UB_23      0.0017988000
_diffrn_orient_matrix_UB_31      0.0340164000
_diffrn_orient_matrix_UB_32      0.0263171000
_diffrn_orient_matrix_UB_33      -0.0256998000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11196
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+2.4259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                3479
_reflns_number_total             4358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4nj02087a2.cif
_cod_data_source_block           exp_8879
_cod_depositor_comments          'Adding full bibliography for 7063284.cif.'
_cod_original_cell_volume        2265.91(18)
_cod_database_code               7063284
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H9(0.025) H5(0.022) H2(0.024) H3(0.026) H3A(0.025) H3B(0.025)
 H1(0.029) H6(0.027) H6A(0.023) H6B(0.023) H10(0.03) H4(0.028) H4A(0.036)
 H12(0.025) H11(0.033) H5A(0.029)
 Fixed X: H9(0.3277) H5(0.5733) H2(0.8562) H3(1.0969) H3A(0.6442) H3B(0.7193)
 H1(1.3985) H6(1.075) H6A(0.712) H6B(0.7883) H10(0.1161) H4(1.3151) H4A(0.0501)
 H12(0.3882) H11(0.1742) H5A(1.2924)
 Fixed Y: H9(0.0568) H5(0.0724) H2(0.1554) H3(0.1888) H3A(0.1566) H3B(0.2286)
 H1(0.0266) H6(-0.0394) H6A(0.0002) H6B(0.0722) H10(0.1047) H4(0.1531)
 H4A(0.2353) H12(0.285) H11(0.3272) H5A(-0.0705)
 Fixed Z: H9(0.3916) H5(0.4315) H2(0.0407) H3(0.0813) H3A(0.07) H3B(0.1222)
 H1(0.1235) H6(0.2025) H6A(0.3523) H6B(0.4036) H10(0.4025) H4(0.0708)
 H4A(0.3518) H12(0.2825) H11(0.2943) H5A(0.1871)
;
_olex2_submission_special_instructions 'No special instructions were received'