New Sb12and Sb14Polyoxometalate Frameworks Derived from Arylstibonic Acids: [LiH3(p-MeC6H4Sb)12O28]4‒and [BaH10(p-MeC6H4Sb)14O34]
Nicholson, Brian K.; Clark, Christopher J.; Wright, Cody E.; Telfer, Shane G.; Groutso, Tania; Organometallics 30 (2011) 6612–; doi:10.1021/om200739a

data_4065372
_publ_section_title
;
 New Sb12and Sb14Polyoxometalate Frameworks Derived from Arylstibonic
 Acids: [LiH3(p-MeC6H4Sb)12O28]4--and [BaH10(p-MeC6H4Sb)14O34]
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6612
_journal_paper_doi               10.1021/om200739a
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety
'C84 H84 Li4 O31 Sb12, 2(Li H 8 O4), Br, 10(H2 O)'
_chemical_formula_sum            'C84 H133 Br Li6 O49 Sb12'
_chemical_formula_weight         3509.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.5271(3)
_cell_length_b                   29.5173(4)
_cell_length_c                   35.9883(5)
_cell_measurement_reflns_used    4192
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     23930.0(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      89(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1091
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            448303
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    3.079
_exptl_absorpt_correction_T_max  0.6552
_exptl_absorpt_correction_T_min  0.4688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             13552
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.740
_refine_diff_density_min         -1.669
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1266
_refine_ls_number_reflns         28508
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+311.7491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                19734
_reflns_number_total             28508
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200739a_si_003.cif
_cod_data_source_block           cclim
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4065372