Bis(tripyrazol-1-ylmethane)nickel(II) tetracyanidonickelate(II) dihydrate
Lyubartseva, Ganna; Parkin, Sean; Acta Crystallographica Section E 65 (2009) m1530–; doi:10.1107/S1600536809046108

data_2224386
_publ_section_title
;
 Bis(tripyrazol-1-ylmethane)nickel(II) tetracyanidonickelate(II)
 dihydrate
;
_journal_coeditor_code           OM2294
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1530
_journal_paper_doi               10.1107/S1600536809046108
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C10 H10 N6)2] [Ni (C N)4], 2H2 O'
_chemical_formula_moiety         'C20 H20 N12 Ni 2+, C4 N4 Ni 2-, 2(H2 O)'
_chemical_formula_sum            'C24 H24 N16 Ni2 O2'
_chemical_formula_weight         686.01
_chemical_name_systematic
;
Bis(tripyrazol-1-ylmethane)nickel(II) tetracyanidonickelate(II) dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.5129(11)
_cell_angle_beta                 75.2713(12)
_cell_angle_gamma                89.2534(12)
_cell_formula_units_Z            1
_cell_length_a                   8.4840(2)
_cell_length_b                   8.7355(2)
_cell_length_c                   10.7522(3)
_cell_measurement_reflns_used    3304
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     745.09(3)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (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 9.1
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13964
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.317
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.800
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3404
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0568P)^2^+0.2597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                2664
_reflns_number_total             3404
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2294.cif
_cod_data_source_block           I
_cod_database_code               2224386
_cod_database_fobs_code          2224386