Hexaaquadodeca-μ-chloro-hexaniobium(II,III) dichloride 2,2'-bipyridine trisolvate
Maria S. Tarasenko; Alexander V. Virovets; Nikolai G. Naumov; Vladimir E. Fedorov; Acta Crystallographica Section E 62 (2006) m175–m178; doi:10.1107/S1600536805040171

data_2207757
_publ_section_title
;
 Hexaaquadodeca-\m-chloro-hexaniobium(II,III) dichloride
 2,2'-bipyridine trisolvate
;
_journal_coeditor_code           CV6596
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m175
_journal_page_last               m178
_journal_paper_doi               10.1107/S1600536805040171
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Nb6 Cl12 (H2 O)6] Cl2 , 3C10 H8 N2'
_chemical_formula_moiety         'Cl12 H12 Nb6 O6 2+ , 2Cl - , 3C10 H8 N2'
_chemical_formula_sum            'C30 H36 Cl14 N6 Nb6 O6'
_chemical_formula_weight         1630.41
_chemical_name_common            none
_chemical_name_systematic
;
Hexaaquadodeca-\m-chloro-hexaniobium(II,III) dichloride 2,2'-bipyridine
trisolvate
;
_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           SHELXL97
_cell_angle_alpha                74.822(4)
_cell_angle_beta                 74.551(4)
_cell_angle_gamma                70.901(4)
_cell_formula_units_Z            1
_cell_length_a                   10.1546(12)
_cell_length_b                   11.2503(15)
_cell_length_c                   12.2583(11)
_cell_measurement_reflns_used    3551
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      28.1615
_cell_measurement_theta_min      2.4819
_cell_volume                     1251.8(3)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2005)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker X8 APEX CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12802
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.121
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.270
_refine_diff_density_min         -0.674
_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     298
_refine_ls_number_reflns         5658
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0401P)^2^+1.4105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                4317
_reflns_number_total             5658
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6596.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2207757
_cod_database_fobs_code          2207757