Bis(acetato-κ<i>O</i>)tetrakis(1<i>H</i>-pyrazole-κ<i>N</i>^1^)nickel(II)
Blaz̆ena Papánková; Svoboda, Ingrid; Fuess, Hartmut; S̆intálová, Katka; Acta Crystallographica, Section E 61 (2005) m2036–m2038; doi:10.1107/S1600536805029193

data_2206892
_publ_section_title
;
Bis(acetato-\k<i>O</i>)tetrakis(1<i>H</i>-pyrazole-\k<i>N</i>^1^)nickel(II)
;
_journal_coeditor_code           BV6029
_journal_issue                   10
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              m2036
_journal_page_last               m2038
_journal_paper_doi               10.1107/S1600536805029193
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ni (C2 H3 O2)2 (C3 H4 N2)4]'
_chemical_formula_moiety         'C16 H22 N8 Ni O4'
_chemical_formula_sum            'C16 H22 N8 Ni O4'
_chemical_formula_weight         449.13
_chemical_name_systematic
;
Bis(acetato-\kO)tetrakis(1H-pyrazole-\kN^1^)nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.97(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.925(5)
_cell_length_b                   14.920(7)
_cell_length_c                   13.969(7)
_cell_measurement_reflns_used    401
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      13.707
_cell_measurement_theta_min      2.528
_cell_volume                     2043.2(18)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2002)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2002)
;
_computing_data_reduction
;
CrysAlis RED
;
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997; Farrugia, 2005)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur with Sapphire CCD detector
;
_diffrn_measurement_method
;
Rotation method data acquisition using \w
;
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12234
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.10
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  0.6930
_exptl_absorpt_correction_T_min  0.6171
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.466
_refine_ls_extinction_coef       0.0070(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4173
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0732P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                3171
_reflns_number_total             4173
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bv6029.cif
_cod_data_source_block           I
_cod_original_cell_volume        2043.2(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2206892