Inverse bilayer structure of mononuclear Co^II^ and Ni^II^ complexes of the type <i>M</i>(H~2~O)~3~(SO~4~)(4-CNpy)~2~
Das, Birinchi K.; Bora, Sanchay J.; Bhattacharyya, Manjit K.; Barman, Rama K.; Acta Crystallographica Section B 65 (2009) 467–473; doi:10.1107/S0108768109021090

data_2104408
_publ_section_title
;
 Inverse bilayer structure of mononuclear Co^II^ and Ni^II^ complexes
 of the type <i>M</i>(H~2~O)~3~(SO~4~)(4-CNpy)~2~
;
_journal_coeditor_code           ZB5003
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              467
_journal_page_last               473
_journal_paper_doi               10.1107/S0108768109021090
_journal_volume                  65
_journal_year                    2009
_chemical_formula_sum            'C12 H16 N4 Ni O8 S'
_chemical_formula_weight         435.06
_chemical_name_systematic
;
Tris(aqua)bis(4-cyanopyridine)nickel(II) sulphate.H~2~O
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2117(8)
_cell_length_b                   8.4275(4)
_cell_length_c                   12.5984(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1821.42(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELHS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker AXS CCD'
_diffrn_measurement_method       '\f 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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            10611
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.756796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.332
_refine_ls_extinction_coef       0.0026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0315P)^2^+0.4846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                3447
_reflns_number_total             4058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zb5003.cif
_cod_data_source_block           niso4
_cod_original_sg_symbol_H-M      P2~1~/c
_cod_database_code               2104408
_cod_database_fobs_code          2104408