[V16Sb4O42(H2O){VO(C6H14N2)2}4]: A Terminal Expansion to a Polyoxovanadate Archetype
Adam Wutkowski; Christian Näther; Paul Kögerler; Wolfgang Bensch; Inorganic Chemistry 47 (2008) 1916–1918; doi:10.1021/ic800042r

data_4304940
_publ_section_title
;
[V16Sb4O42(H2O){VO(C6H14N2)2}4]: A Terminal Expansion to a Polyoxovanadate
Archetype
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1916
_journal_page_last               1918
_journal_paper_doi               10.1021/ic800042r
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C54 H126 N18 O57 Sb4 V20'
_chemical_formula_weight         3445.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.004(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.6528(11)
_cell_length_b                   21.0096(11)
_cell_length_c                   22.8018(16)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.56
_cell_volume                     6441.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'phi 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  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41457
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.279
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.083
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         13882
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0605P)^2^+7.5030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                11503
_reflns_number_total             13882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800042r-file002.cif
_cod_data_source_block           aw9
_cod_database_code               4304940