Bis(methanol-1κ<i>O</i>)tetra-μ-pyridazine-1:2κ^4^<i>N</i>:<i>N</i>';2:3κ^4^<i>N</i>:<i>N</i>'-di-μ-thiocyanato-1:2κ^2^<i>N</i>:<i>N</i>;2:3κ^2^<i>N</i>:<i>N</i>-tetrathiocyanato-1κ^2^<i>N</i>,3κ^2^<i>N</i>-trinickel(II) methanol tetrasolvate
Wöhlert, Susanne; Jess, Inke; Näther, Christian; Acta Crystallographica Section E 68 (2012) m940–m941; doi:10.1107/S1600536812026864

data_2235498
_publ_section_title
;
 Bis(methanol-1\k<i>O</i>)tetra-\m-pyridazine-1:2\k^4^<i>N</i>:<i>N</i>';2:3\k^4^<i>N</i>:<i>N</i>'-di-\m-thiocyanato-1:2\k^2^<i>N</i>:<i>N</i>;2:3\k^2^<i>N</i>:<i>N</i>-tetrathiocyanato-1\k^2^<i>N</i>,3\k^2^<i>N</i>-trinickel(II)
 methanol tetrasolvate
;
_journal_coeditor_code           HP2040
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m940
_journal_page_last               m941
_journal_paper_doi               10.1107/S1600536812026864
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni3 (N C S)6 (C4 H4 N2)4 (C H4 O)2], 4C H4 O'
_chemical_formula_moiety         'C24 H24 N14 Ni3 O2 S6, 4(C H4 O)'
_chemical_formula_sum            'C28 H40 N14 Ni3 O6 S6'
_chemical_formula_weight         1037.23
_chemical_name_systematic
;
Bis(methanol-1\k<i>O</i>)tetra-\m-pyridazine-
1:2\k^4^<i>N</i>:<i>N</i>';2:3\k^4^<i>N</i>:<i>N</i>'-di-\m-thiocyanato-
1:2\k^2^<i>N</i>:<i>N</i>;2:3\k^2^<i>N</i>:<i>N</i>-tetrathiocyanato-
1\k^2^<i>N</i>,3\k^2^<i>N</i>-trinickel(II) methanol tetrasolvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6689(12)
_cell_length_b                   15.0760(7)
_cell_length_c                   17.9479(10)
_cell_measurement_reflns_used    31891
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.55
_cell_volume                     4780.9(5)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2008)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2008)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2008)'
_computing_molecular_graphics
'XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011)'
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31891
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  0.8179
_exptl_absorpt_correction_T_min  0.7461
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.1274
_exptl_crystal_size_mid          0.0909
_exptl_crystal_size_min          0.0724
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.522
_refine_ls_extinction_coef       0.0022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+2.6878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                3190
_reflns_number_total             4093
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hp2040.cif
_cod_data_source_block           I
_cod_database_code               2235498
_cod_database_fobs_code          2235498