Crystal structure of trans-diaqua-bis(methyl methylcarbamohydrazonothioato-κ2 N,N′) nickel(II) iodide semihydrate, C6H22N6O2NiS2I2·0.5H2O
Belošević, Svetlana; Leovac, Vukadin M.; Radanović, Mirjana M.; Bogdanović, Milica G.; Radnović, Nikola D.; Rodić, Marko V.; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 475–477; doi:10.1515/ncrs-2023-0040

data_8107472
_publ_section_title
;
 Crystal structure of trans-diaqua-bis(methyl
 methylcarbamohydrazonothioato-\k2 N,N&#x2032;) nickel(II) iodide
 semihydrate, C6H22N6O2NiS2I2&#x00B7;0.5H2O
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              475
_journal_page_last               477
_journal_paper_doi               10.1515/ncrs-2023-0040
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         '(C6 H22 N6 Ni O2 S2 2+), 2(I 1-), 0.5(H2 O)'
_chemical_formula_sum            'C6 H23 I2 N6 Ni O2.5 S2'
_chemical_formula_weight         595.93
_chemical_name_common
; trans-diaqua-bis(N4-methyl-S-methylisothiosemicarbazide)nickel(II) iodide 
semihydrate 
;
_chemical_name_systematic
; trans-diaqua-bis(methyl (E)-methylcarbamohydrazonothioate)nickel(II) iodide 
semihydrate 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   .
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 109.451(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2282(4)
_cell_length_b                   21.9200(7)
_cell_length_c                   11.4906(4)
_cell_measurement_reflns_used    6103
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.7480
_cell_measurement_theta_min      2.6250
_cell_volume                     1954.19(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 [1]'
_computing_data_collection       'CrysAlisPro 1.171.42.49 [1]'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 [1]'
_computing_molecular_graphics    'PLATON [4]'
_computing_publication_material  'PLATON [4]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SHELXT-2018/2 [2]'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3280
_diffrn_detector_type            'Sapphire3 (Oxford Diffraction)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.905
_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     35.00  95.00   1.00   10.00    --   19.01 178.00  90.00   60
  2  \w     -2.00  88.00   1.00   10.00    --   19.01  57.00 -90.00   90
  3  \w    -51.00  49.00   1.00   10.00    --   19.01 -77.00 150.00  100
  4  \w    -25.00  24.00   1.00   10.00    --  -18.39 -99.00 -30.00   49
  5  \w     35.00  95.00   1.00   10.00    --   19.01 178.00   0.00   60
  6  \w     -2.00  88.00   1.00   10.00    --   19.01  57.00-150.00   90
  7  \w    -11.00  14.00   1.00   10.00    --   19.01  77.00   0.00   25
  8  \w     -2.00  88.00   1.00   10.00    --   19.01  57.00 120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Gemini S (Oxford Diffraction)'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass fibre'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0205794000
_diffrn_orient_matrix_UB_12      -0.0312359000
_diffrn_orient_matrix_UB_13      -0.0037422000
_diffrn_orient_matrix_UB_21      0.0321374000
_diffrn_orient_matrix_UB_22      -0.0017324000
_diffrn_orient_matrix_UB_23      0.0653562000
_diffrn_orient_matrix_UB_31      -0.0830301000
_diffrn_orient_matrix_UB_32      -0.0083932000
_diffrn_orient_matrix_UB_33      0.0004191000
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4196
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        26.320
_diffrn_reflns_theta_max         28.993
_diffrn_reflns_theta_min         2.643
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         4196
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0563P)^2^+0.0081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1113
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2990
_reflns_number_total             4196
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
; Component 2 rotated by 179.8879\% around 
 [0.91 0.00 -0.42] (reciprocal) or 
 [1.00 0.00 -0.00] (direct)
;
_cod_data_source_file            suppl_j_ncrs-2023-0040_suppl_001.cif
_cod_data_source_block           Ni
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C6 H23 I2 N6 Ni O2.50 S2'
_cod_database_code               8107472
_shelx_shelxl_version_number     2018/3
_oxdiff_twin_integration_method  simultaneous
_shelx_res_checksum              19911
_shelx_hkl_checksum              92754