Bis[tris(1<i>H</i>-pyrazol-1-yl-κ<i>N</i>^2^)methane]nickel(II) bis{[tris(1<i>H</i>-pyrazol-1-yl-κ<i>N</i>^2^)methane]tris(thiocyanato-κ<i>N</i>)nickelate(II)} methanol disolvate
Lyubartseva, Ganna; Parkin, Sean; Mallik, Uma Prasad; Acta Crystallographica Section E 67 (2011) m1656–m1657; doi:10.1107/S1600536811045144

data_2232877
_publ_section_title
;
 Bis[tris(1<i>H</i>-pyrazol-1-yl-\k<i>N</i>^2^)methane]nickel(II)
 bis{[tris(1<i>H</i>-pyrazol-1-yl-\k<i>N</i>^2^)methane]tris(thiocyanato-\k<i>N</i>)nickelate(II)}
 methanol disolvate
;
_journal_coeditor_code           NG5255
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1656
_journal_page_last               m1657
_journal_paper_doi               10.1107/S1600536811045144
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Ni (C10 H10 N6)2] [Ni (N C S)3 (C10 H10 N6)]2, 2C H4 O'
_chemical_formula_moiety
'Ni (C10 H10 N6)2 2+, 2 Ni (C N S)3 (C10 H10 N6) -,2C H4 O'
_chemical_formula_sum            'C48 H48 N30 Ni3 O2 S6'
_chemical_formula_weight         1445.65
_chemical_name_systematic
;
Bis[tris(1<i>H</i>-pyrazol-1-yl-\k<i>N</i>^2^)methane]nickel(II)
bis{[tris(1<i>H</i>-pyrazol-1-yl-\k<i>N</i>^2^)methane]tris(thiocyanato-
\k<i>N</i>)nickelate(II)} methanol disolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.5900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.4463(8)
_cell_length_b                   7.3287(2)
_cell_length_c                   27.2689(7)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      67.75
_cell_measurement_theta_min      2.86
_cell_volume                     6171.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELX97 (Sheldrick, 2008) and local procedures
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8 Proteum'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'graded multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41685
_diffrn_reflns_theta_full        67.99
_diffrn_reflns_theta_max         67.99
_diffrn_reflns_theta_min         2.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.516
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in APEX2; Bruker, 2006)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.339
_refine_diff_density_min         -0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5605
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0515P)^2^+28.6001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                4932
_reflns_number_total             5605
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng5255.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2232877
_cod_database_fobs_code          2232877