Diaquabis(pyridine-2-carboxamide-κ^2^<i>N</i>^1^,<i>O</i>^2^)nickel(II) disaccharinate tetrahydrate
Paşaoğlu, Hümeyra; Tezcan, Fatma; Yeşilel, Okan Z.; ölmez, Halis; Içbudak, Hasan; Büyükgüngör, Orhan; Acta Crystallographica Section C 60 (2004) m335–m337; doi:10.1107/S0108270104012648

data_2014129
_publ_section_title
;
 Diaquabis(pyridine-2-carboxamide-\k^2^<i>N</i>^1^,<i>O</i>^2^)nickel(II)
 disaccharinate tetrahydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m335
_journal_page_last               m337
_journal_paper_doi               10.1107/S0108270104012648
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac
'[Ni (C6 H6 N2 O)2 (H2 O)2] (C7 H4 N O3 S)2, 4H2 O'
_chemical_formula_moiety         'C12 H16 N4 Ni O4 2+, 2C7 H4 N O3 S -, 4H2 O'
_chemical_formula_sum            'C26 H32 N6 Ni O14 S2'
_chemical_formula_weight         775.41
_chemical_name_systematic
;
Diaquabis(pyridine-2-carboxamide-\k^2^N^1^,O^2^)nickel(II) disaccharinate
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           SHELXL-97
_cell_angle_alpha                81.560(6)
_cell_angle_beta                 72.655(6)
_cell_angle_gamma                64.257(6)
_cell_formula_units_Z            1
_cell_length_a                   8.4478(7)
_cell_length_b                   8.8751(7)
_cell_length_c                   12.3854(9)
_cell_measurement_reflns_used    13935
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      2.55
_cell_volume                     798.24(12)
_computing_cell_refinement       X-AREA
_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)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS-II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18441
_diffrn_reflns_theta_full        28.97
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         2.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.8275
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.632
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4207
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                3267
_reflns_number_total             4243
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1063.cif
_cod_data_source_block           I
_cod_original_cell_volume        798.24(11)
_cod_database_code               2014129
_cod_database_fobs_code          2014129