Assembly of [V15Sb6O42(H2O)]6− cluster shells into higher dimensional aggregates via weak Sb⋯N/Sb⋯O intercluster interactions and a new polyoxovanadate with a discrete [V16Sb4O42(H2O)]8− cluster shell
Antonova, Elena; Näther, Christian; Bensch, Wolfgang; CrystEngComm 14 (2012) 6853–; doi:10.1039/c2ce25896j

data_7238514
_publ_section_title
;
 Assembly of [V15Sb6O42(H2O)]6&#x2212; cluster shells into higher
 dimensional aggregates via weak Sb&#x22EF;N/Sb&#x22EF;O intercluster
 interactions and a new polyoxovanadate with a discrete
 [V16Sb4O42(H2O)]8&#x2212; cluster shell
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6853
_journal_paper_doi               10.1039/c2ce25896j
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'O42 Sb6 V15, 3(Co C6 H18 N4 O), 2(O)'
_chemical_formula_sum            'C18 H58 Co3 N12 O47 Sb6 V15'
_chemical_formula_weight         2872.96
_chemical_name_common            '(Co(N4C6H18)(H2O))3V15Sb6O42(H2O)H2O '
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.3811(5)
_cell_length_b                   12.3811(5)
_cell_length_c                   41.398(3)
_cell_measurement_reflns_used    16570
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.9
_cell_measurement_theta_min      5.5
_cell_volume                     5495.8(5)
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_collection       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       '\f scans'
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            16570
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    4.737
_exptl_absorpt_correction_T_max  0.7001
_exptl_absorpt_correction_T_min  0.3560
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate crystal'
_exptl_crystal_F_000             4092
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.511
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_coef       0.00027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5856
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                5371
_reflns_number_total             5856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25896j.txt
_cod_data_source_block           ea430
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Numerical' was
changed to 'numerical' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        5495.7(5)
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7238514