[Bis[tris(3,5-dimethylpyrazolyl)methane]nickel(II)][tetrachloronickelate(II)]‒methanol‒water (1/1/1)
Annie Michaud; Frédéric-Georges Fontaine; Davit Zargarian; Acta Crystallographica Section E 61 (2005) m904–m906; doi:10.1107/S1600536805011128

data_2205757
_publ_section_title
;[Bis[tris(3,5-dimethylpyrazolyl)methane]nickel(II)][tetrachloronickelate(II)]--methanol--water
 (1/1/1)
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m904
_journal_page_last               m906
_journal_paper_doi               10.1107/S1600536805011128
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ni (C16 H22 N6)2] [Ni Cl4] , C H4 O , H2 O'
_chemical_formula_moiety
'C32 H44 N12 Ni 2+ , Cl4 Ni 2- , C H4 O , H2 O'
_chemical_formula_sum            'C33 H50 Cl4 N12 Ni2 O2'
_chemical_formula_weight         906.07
_chemical_name_systematic
;
[Bis[tris(3,5-dimethylpyrazolyl)methane]nickel(II)][tetrachloronickel(II)]
methanol water solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.1180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2998(2)
_cell_length_b                   18.5245(3)
_cell_length_c                   21.9660(3)
_cell_measurement_reflns_used    36297
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      72.60
_cell_measurement_theta_min      2.38
_cell_volume                     4180.26(12)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'UdMX (local program)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 2K/Platform CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49482
_diffrn_reflns_theta_full        72.59
_diffrn_reflns_theta_max         72.59
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  60
_diffrn_standards_number         376
_exptl_absorpt_coefficient_mu    3.846
_exptl_absorpt_correction_T_max  0.7395
_exptl_absorpt_correction_T_min  0.2871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1899
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.569
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8242
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0509
_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^)+(0.1017P)^2^+0.294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1561
_reflns_number_gt                7048
_reflns_number_total             8242
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6402.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2205757
_cod_database_fobs_code          2205757