Synthesis, crystal structures, HF-EPR, and magnetic properties of six-coordinate transition metal (Co, Ni, and Cu) compounds with a 4-amino-1,2,4-triazole Schiff-base ligand
Zhang, Ya-Jie; Yin, Lei; Li, Jing; Hu, Zhao-Bo; Ouyang, Zhong-Wen; Song, You; Wang, Zhenxing; RSC Advances 10 (2020) 12833–12840; doi:10.1039/C9RA10851C

data_7240236
_publ_section_title
;
 Synthesis, crystal structures, HF-EPR, and magnetic properties of
 six-coordinate transition metal (Co, Ni, and Cu) compounds with a
 4-amino-1,2,4-triazole Schiff-base ligand
;
_journal_issue                   22
_journal_name_full               'RSC Advances'
_journal_page_first              12833
_journal_page_last               12840
_journal_paper_doi               10.1039/C9RA10851C
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C20 H22 N8 Ni O6'
_chemical_formula_sum            'C20 H22 N8 Ni O6'
_chemical_formula_weight         529.16
_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     dual
_audit_creation_date             2019-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-04 deposited with the CCDC.	2020-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.169(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0895(2)
_cell_length_b                   15.5758(3)
_cell_length_c                   7.7921(2)
_cell_measurement_reflns_used    3177
_cell_measurement_temperature    293
_cell_measurement_theta_max      76.1660
_cell_measurement_theta_min      2.8330
_cell_volume                     1078.39(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -29.00  67.00   0.50    0.05    --   43.80 -57.00  30.00  192
  2  \w     53.00  78.00   0.50    0.05    --   43.80-134.00 167.00   50
  3  \w     38.00 114.00   0.50    0.10    --  111.75-134.00 167.00  152
  4  \w     83.00 125.00   0.50    0.10    --  111.75-134.00 -12.00   84
  5  \w     53.00  79.00   0.50    0.10    --  111.75 -94.00-150.00   52
  6  \w     39.00 108.00   0.50    0.10    --  111.75 -94.00-180.00  138
  7  \w     39.00 134.00   0.50    0.10    --  111.75 -45.00 -60.00  190
  8  \w     88.00 114.00   0.50    0.10    --  111.75  30.00  60.00   52
  9  \w    136.00 178.00   0.50    0.10    --  111.75  30.00  60.00   84
 10  \w    140.00 165.00   0.50    0.10    --  111.75  45.00 150.00   50
 11  \w    111.00 137.00   0.50    0.10    --  111.75 134.00  54.00   52
 12  \w     91.00 136.00   0.50    0.10    --  111.75  45.00 150.00   90
 13  \w     41.00  72.00   0.50    0.10    --  111.75 -94.00 -30.00   62
 14  \w    -52.00 -21.00   0.50    0.05    --  -43.80 -57.00-120.00   62
 15  \w   -104.00 -65.00   0.50    0.10    --  -90.25-134.00 -12.00   78
 16  \w   -118.00 -92.00   0.50    0.05    --  -43.80-134.00 -12.00   52
 17  \w    -88.00 -54.00   0.50    0.05    --  -43.80 134.00-125.00   68
 18  \w    -82.00 -57.00   0.50    0.10    --  -90.25 134.00-125.00   50
 19  \w   -113.00 -71.00   0.50    0.05    --  -43.80 -57.00-120.00   84
 20  \w   -155.00 -96.00   0.50    0.10    --  -90.25 -94.00  90.00  118
 21  \w   -114.00 -77.00   0.50    0.05    --  -43.80-134.00 167.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0613710000
_diffrn_orient_matrix_UB_12      -0.0922266000
_diffrn_orient_matrix_UB_13      0.0007490000
_diffrn_orient_matrix_UB_21      -0.1584344000
_diffrn_orient_matrix_UB_22      -0.0357274000
_diffrn_orient_matrix_UB_23      -0.0024562000
_diffrn_orient_matrix_UB_31      -0.0343580000
_diffrn_orient_matrix_UB_32      0.0001640000
_diffrn_orient_matrix_UB_33      -0.2022808000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5599
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.065
_diffrn_reflns_theta_max         67.065
_diffrn_reflns_theta_min         4.977
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1924
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0405P)^2^+0.7782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1753
_reflns_number_total             1924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra10851c2.cif
_cod_data_source_block           wangzhengxin-ni-20190117
_cod_depositor_comments          'Adding full bibliography for 7240236.cif.'
_cod_database_code               7240236
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni C H O N Cl'
_shelx_estimated_absorpt_t_max   0.713
_shelx_estimated_absorpt_t_min   0.713
_reflns_odcompleteness_completeness 99.90
_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, All O(H) groups
2. Restrained distances
 O3-H3B
 0.85 with sigma of 0.01
3.a Rotating group:
 O3(H3A)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              89342
_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 1.159
_oxdiff_exptl_absorpt_empirical_full_min 0.902