Bis(5,8-diazoniadispiro[4.2.4.2]tetradecane) hexakis(thiocyanato-κ<i>N</i>)nickelate(II) dihydrate
Mao-Ping Song; Lin-Ke Li; Ben-Lai Wu; Yun-Yin Niu; Acta Crystallographica Section E 63 (2007) m2217–m2217; doi:10.1107/S1600536807035416

data_2214853
_publ_section_title
;
 Bis(5,8-diazoniadispiro[4.2.4.2]tetradecane)
 hexakis(thiocyanato-\k<i>N</i>)nickelate(II) dihydrate
;
_journal_coeditor_code           RZ2160
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2217
_journal_page_last               m2217
_journal_paper_doi               10.1107/S1600536807035416
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C12 H24 N2)2 [Ni (NCS)6], 2H2 O'
_chemical_formula_moiety         '2(C12 H24 N2 2+), C6 N6 Ni S6 4-, 2(H2 O)'
_chemical_formula_sum            'C30 H52 N10 Ni O2 S6'
_chemical_formula_weight         835.89
_chemical_name_systematic
;
Bis(5,8-diazoniadispiro[4.2.4.2]tetradecane)
hexakis(thiocyanato-\kN)nickel(II) dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.186(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.959(6)
_cell_length_b                   13.537(8)
_cell_length_c                   14.718(9)
_cell_measurement_reflns_used    5316
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.55
_cell_volume                     1973(2)
_computing_cell_refinement       'SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemen SMART CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10750
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.403
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0548P)^2^+0.9458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                3220
_reflns_number_total             3660
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2160.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2214853
_cod_database_fobs_code          2214853