Bis[μ~2~-1-(2-carboxybenzoyl)thiosemicarbazide(3{-})]hexapyridinetrinickel(II) pyridine monosolvate monohydrate
Cao, Fan; Li, Leilei; Li, Dacheng; Acta Crystallographica Section E 67 (2011) m1803–; doi:10.1107/S1600536811048367

data_2232977
_publ_section_title
;
 Bis[\m~2~-1-(2-carboxybenzoyl)thiosemicarbazide(3{-})]hexapyridinetrinickel(II)
 pyridine monosolvate monohydrate
;
_journal_coeditor_code           VM2135
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1803
_journal_paper_doi               10.1107/S1600536811048367
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Ni3 (C9 H6 N3 O3 S1)2 (C5 H5 N1)6], C5 H5 N, 2H2 O'
_chemical_formula_moiety         'C48 H42 N12 Ni3 O6 S2, C5 H5 N, 2(H2 O)'
_chemical_formula_sum            'C53 H51 N13 Ni3 O8 S2'
_chemical_formula_weight         1238.32
_chemical_name_systematic
;
Bis[\m~2~-1-(2-carboxybenzoyl)thiosemicarbazide(3-)]hexapyridinetrinickel(II)
pyridine monosolvate monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 90.9120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.490(3)
_cell_length_b                   8.8510(7)
_cell_length_c                   17.8941(16)
_cell_measurement_reflns_used    1906
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.5305
_cell_measurement_theta_min      2.2725
_cell_volume                     5461.9(8)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0959
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13285
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_T_max  0.8444
_exptl_absorpt_correction_T_min  0.6655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.470
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                2586
_reflns_number_total             4808
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            vm2135.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2232977
_cod_database_fobs_code          2232977