Bis[tris(ethylenediamine-κ^2^<i>N</i>,<i>N</i>')cobalt(III)] octakis-μ-~3~-oxido-hexadeca-μ~2~-oxido-tetradecaoxido-μ~12~-tetraoxosilicato-octamolybdenum(VI)hexavanadium(IV,V) hexahydrate
Lu, Yu-Kun; Tian, Ming-Ming; Xu, Shu-Gang; Lü, Ren-Qing; Liu, Yun-Qi; Acta Crystallographica Section E 67 (2011) m1776–m1777; doi:10.1107/S1600536811048197

data_2232678
_publ_section_title
;
 Bis[tris(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')cobalt(III)]
 octakis-\m-~3~-oxido-hexadeca-\m~2~-oxido-tetradecaoxido-\m~12~-tetraoxosilicato-octamolybdenum(VI)hexavanadium(IV,V)
 hexahydrate
;
_journal_coeditor_code           GK2413
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1776
_journal_page_last               m1777
_journal_paper_doi               10.1107/S1600536811048197
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co (C2 H8 N2)3]2 [Mo8 V6 O42 Si], 6H2 O'
_chemical_formula_moiety
'2(C6 H24 Co N6 3+), Mo8 O42 Si V6 6-, 6(H2 O)'
_chemical_formula_sum            'C12 H60 Co2 Mo8 N12 O48 Si V6'
_chemical_formula_weight         2359.83
_chemical_name_systematic
;
Bis[tris(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')cobalt(III)]
octakis-\m-~3~-oxido-hexadeca-\m~2~-oxido-tetradecaoxido-\m~12~-
tetraoxosilicato-octamolybdenum(VI)hexavanadium(IV,V) hexahydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.744(4)
_cell_length_b                   21.498(4)
_cell_length_c                   13.623(3)
_cell_measurement_reflns_used    4213
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      2.18
_cell_volume                     6075(2)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_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  0.0801
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45336
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.127
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4568
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.042
_refine_diff_density_min         -1.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0462P)^2^+70.2923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                3951
_reflns_number_total             5404
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gk2413.cif
_cod_data_source_block           I
_cod_database_code               2232678
_cod_database_fobs_code          2232678