Tetraaqua{5-[(pyridin-2-ylmethylidene)amino]benzene-1,3-dicarboxylato-κ^2^<i>N</i>,<i>N</i>'}nickel(II) tetrahydrate
Wang, Huan-Huan; Duan, Guang-He; Wang, Lin; Xie, Ya-Bo; Acta Crystallographica Section E 68 (2012) m964–; doi:10.1107/S1600536812027122

data_2235586
_publ_section_title
;
 Tetraaqua{5-[(pyridin-2-ylmethylidene)amino]benzene-1,3-dicarboxylato-\k^2^<i>N</i>,<i>N</i>'}nickel(II)
 tetrahydrate
;
_journal_coeditor_code           QK2036
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m964
_journal_paper_doi               10.1107/S1600536812027122
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni (C14 H8 N2 O4) (H2 O)4], 4H2 O'
_chemical_formula_moiety         'C14 H16 N2 Ni O8, 4(H2 O)'
_chemical_formula_sum            'C14 H24 N2 Ni O12'
_chemical_formula_weight         471.06
_chemical_name_systematic
;
Tetraaqua{5-[(pyridin-2-ylmethylidene)amino]benzene-1,3-dicarboxylato-
\k^2^<i>N</i>,<i>N</i>'}nickel(II) tetrahydrate
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 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                 95.86(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.998(2)
_cell_length_b                   7.4536(15)
_cell_length_c                   12.271(3)
_cell_measurement_reflns_used    4687
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.73
_cell_volume                     1000.7(4)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\p and \w scans'
_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  0.0114
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4844
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.322
_refine_ls_abs_structure_details 'Flack (1983), 1482 Friedel pairs'
_refine_ls_abs_structure_Flack   0.012(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3243
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0183
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                3186
_reflns_number_total             3243
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            qk2036.cif
_cod_data_source_block           I
_cod_original_cell_volume        1000.7(3)
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2235586
_cod_database_fobs_code          2235586