A new decavanadate with a tricobalt(II) cation and 18-crown-6, tris{hexaaquacobalt(II)} decavanadate bis(18-crown-6) decahydrate
Lee, Uk; Jung, Yeon-Hwa; Joo, Hea-Chung; Park, Ki-Min; Acta Crystallographica Section E 59 (2003) m421–m424; doi:10.1107/S1600536803011747

data_2202667
_publ_section_title
;
 A new decavanadate with a tricobalt(II) cation and 18-crown-6,
 tris{hexaaquacobalt(II)} decavanadate bis(18-crown-6) decahydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m421
_journal_page_last               m424
_journal_paper_doi               10.1107/S1600536803011747
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac
'[Co (H2 O)6]3 [V10 O28], (C12 H24 O6)2, 10H2 O'
_chemical_formula_moiety
'2(C12 H24 O6), O28 V10, 3(H12 Co O6), 10(H2 O)'
_chemical_formula_sum            'C24 H104 Co3 O68 V10'
_chemical_formula_weight         2167.26
_chemical_name_systematic        ?
_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           SHELXL-97
_cell_angle_alpha                101.33(3)
_cell_angle_beta                 92.63(2)
_cell_angle_gamma                84.26(2)
_cell_formula_units_Z            1
_cell_length_a                   12.285(4)
_cell_length_b                   13.924(3)
_cell_length_c                   11.120(3)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      10.5
_cell_measurement_theta_min      9.6
_cell_volume                     1855.1(9)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe & Cie, 1996)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       \w/2-\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8466
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        3.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.972
_exptl_absorpt_correction_T_max  0.8116
_exptl_absorpt_correction_T_min  0.6084
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1996)'
_exptl_crystal_colour            'pale blue--brown'
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             1103
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.481
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0423P)^2^+2.3315P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                6530
_reflns_number_total             8466
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6059.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               2202667
_cod_database_fobs_code          2202667