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_7208303
_publ_section_title
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 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
'Na5(H3 O)4[Ni(N2 C2 H8)(H2 O)3] [V12 B18 O60 H6] 9(H2 O)'
_chemical_formula_sum            'C4 H99 B36 N4 Na10 Ni2 O152 V24'
_chemical_formula_weight         4594.86
_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                90.000(5)
_cell_angle_beta                 92.496(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   19.442(5)
_cell_length_b                   21.810(5)
_cell_length_c                   16.070(5)
_cell_measurement_reflns_used    5278
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.81
_cell_volume                     6808(3)
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28634
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.009
_exptl_absorpt_correction_T_max  0.563
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   EvalCCD
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4332.0
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.466
_refine_diff_density_min         -1.882
_refine_diff_density_rms         0.377
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         7681
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1312P)^2^+108.4171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2114
_refine_ls_wR_factor_ref         0.2406
_reflns_number_gt                5797
_reflns_number_total             7763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25436k.txt
_cod_data_source_block           compound_2
_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_database_code               7208303