Bis[3-chloro-6-(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)picolinato]nickel(II) tetrahydrate
Zhao, Kai; Yin, Xian-Hong; Feng, Yu; Zhu, Jie; Lin, Cui-Wu; Acta Crystallographica Section E 64 (2008) m64–m65; doi:10.1107/S1600536807063003

data_2217336
_publ_section_title
;
 Bis[3-chloro-6-(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)picolinato]nickel(II)
 tetrahydrate
;
_journal_coeditor_code           TK2215
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m64
_journal_page_last               m65
_journal_paper_doi               10.1107/S1600536807063003
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C11 H9 Cl N3 O2)2] , 4H2 O'
_chemical_formula_moiety         'C22 H18 Cl2 N6 Ni O4 , 4H2 O'
_chemical_formula_sum            'C22 H26 Cl2 N6 Ni O8'
_chemical_formula_weight         632.10
_chemical_name_systematic
;
Bis[3-chloro-6-(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)picolinato]nickel(II)
tetrahydrate
;
_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           SHELXL97
_cell_angle_alpha                92.593(2)
_cell_angle_beta                 105.206(3)
_cell_angle_gamma                113.820(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5907(10)
_cell_length_b                   11.2776(17)
_cell_length_c                   14.2659(19)
_cell_measurement_reflns_used    3154
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.4
_cell_volume                     1342.0(3)
_computing_cell_refinement       'SMART (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.022
_diffrn_reflns_av_sigmaI/netI    0.048
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6957
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.41
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_gt           0.040
_refine_ls_shift/su_max_lt       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^)+(0.0567P)^2^+0.1899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.097
_refine_ls_wR_factor_ref         0.107
_reflns_number_gt                3549
_reflns_number_total             4644
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2215.cif
_cod_data_source_block           I
_cod_database_code               2217336
_cod_database_fobs_code          2217336