New structures based on the mixed valence polyoxometalate cluster [V12B18O60H6]n−
Hermosilla-Ibáñez, Patricio; Car, Pierre Emmanuel; Vega, Andrés; Costamagna, Juan; Caruso, Francesco; Pivan, Jean-Yves; Fur, Eric Le; Spodine, Evgenia; Venegas-Yazigi, Diego; CrystEngComm 14 (2012) 5604–; doi:10.1039/c2ce25436k

data_7208302
_publ_section_title
;
 New structures based on the mixed valence polyoxometalate cluster
 [V12B18O60H6]n&#x2212;
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              5604
_journal_paper_doi               10.1039/c2ce25436k
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety
'Na8(H3 O)[Ni(H2 O)5][V12 B18 O60 H6]12.5(H2 O) '
_chemical_formula_sum            'B72 H181 Na32 Ni4 O314 V48'
_chemical_formula_weight         9400.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.4520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   19.3555(10)
_cell_length_b                   21.7874(11)
_cell_length_c                   16.0415(8)
_cell_measurement_reflns_used    1560
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      24.40
_cell_measurement_theta_min      2.30
_cell_volume                     6758.6(6)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45481
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    2.046
_exptl_absorpt_correction_T_max  0.625
_exptl_absorpt_correction_T_min  0.226
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   EvalCCD
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4440.0
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.64
_exptl_crystal_size_min          0.23
_refine_diff_density_max         4.927
_refine_diff_density_min         -1.635
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         8727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0873P)^2^+105.5648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1708
_reflns_number_gt                8188
_reflns_number_total             8744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25436k.txt
_cod_data_source_block           Compound(1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'H181 B72 Na32 Ni4 O314 V48'
_cod_database_code               7208302