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_7238515
_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
'Co C8 N6 H26,O42 Sb6 V15 Co C18 N12 H64,O42 Sb6 V15, 13H2O'
_chemical_formula_sum            'C62 H214 Co6 N42 O97 Sb12 V30'
_chemical_formula_weight         6443.53
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 113.717(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.8795(11)
_cell_length_b                   22.9567(9)
_cell_length_c                   32.2932(13)
_cell_measurement_reflns_used    83827
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      48.3
_cell_measurement_theta_min      3.4
_cell_volume                     18922.8(14)
_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      170(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            82381
_diffrn_reflns_theta_full        24.12
_diffrn_reflns_theta_max         24.12
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    3.685
_exptl_absorpt_correction_T_max  0.2084
_exptl_absorpt_correction_T_min  0.1742
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             12480
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.855
_refine_diff_density_min         -2.575
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2169
_refine_ls_number_reflns         29704
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0861P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                21252
_reflns_number_total             29704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25896j.txt
_cod_data_source_block           ea428a
_cod_original_cell_volume        18922.7(13)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7238515