Tris(ethylenediamine)nickel(II) 1<i>H</i>-pyrazole-3,5-dicarboxylate 1.67-hydrate
Demirtaş, Güneş; Dege, Necmi; Yeşilel, Okan Zafer; Erer, Hakan; Büyükgüngör, Orhan; Acta Crystallographica Section E 66 (2010) m925–m926; doi:10.1107/S1600536810027066

data_2226821
_publ_section_title
;
 Tris(ethylenediamine)nickel(II) 1<i>H</i>-pyrazole-3,5-dicarboxylate
 1.67-hydrate
;
_journal_coeditor_code           CI5127
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m925
_journal_page_last               m926
_journal_paper_doi               10.1107/S1600536810027066
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C2 H8 N2)3] (C5 H2 N2 O4), 1.67H2 O'
_chemical_formula_moiety
'C6 H24 N6 Ni1 2+, C5 H2 N2 O4 2-, 1.67(H2 O)'
_chemical_formula_sum            'C11 H29.33 N8 Ni O5.67'
_chemical_formula_weight         423.133
_chemical_name_systematic
;
Tris(ethylenediamine)nickel(II) 1<i>H</i>-pyrazole-3,5-dicarboxylate
1.67-hydrate
;
_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                72.008(5)
_cell_angle_beta                 75.446(5)
_cell_angle_gamma                73.480(4)
_cell_formula_units_Z            6
_cell_length_a                   12.8145(7)
_cell_length_b                   12.9218(7)
_cell_length_c                   18.6311(13)
_cell_measurement_reflns_used    64545
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      1.68
_cell_volume                     2767.5(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX (Farrugia, 1999) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'w-scan rotation'
_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  0.0905
_diffrn_reflns_av_sigmaI/netI    0.1032
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42996
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.9492
_exptl_absorpt_correction_T_min  0.5819
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.353
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.249
_refine_diff_density_min         -1.589
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         11465
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0702P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                6232
_reflns_number_total             11465
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci5127.cif
_cod_data_source_block           I
_cod_database_code               2226821
_cod_database_fobs_code          2226821