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_4065371
_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         'C98 H108 Ba O34 Sb14, 4(H2 O)'
_chemical_formula_sum            'C98 H114 Ba O38 Sb14'
_chemical_formula_weight         3741.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.274(7)
_cell_angle_beta                 104.929(7)
_cell_angle_gamma                97.805(7)
_cell_formula_units_Z            2
_cell_length_a                   15.7738(7)
_cell_length_b                   16.6220(8)
_cell_length_c                   23.8580(17)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      71.8
_cell_measurement_theta_min      6.6
_cell_volume                     5755.0(7)
_computing_cell_refinement       'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_source         'Rigaku MM007 rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_av_sigmaI/netI    0.1298
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31362
_diffrn_reflns_theta_full        50.43
_diffrn_reflns_theta_max         50.43
_diffrn_reflns_theta_min         6.60
_exptl_absorpt_coefficient_mu    28.860
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.274
_refine_diff_density_min         -1.809
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         11072
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0852
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1015P)^2^+53.3298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2122
_refine_ls_wR_factor_ref         0.2429
_reflns_number_gt                7473
_reflns_number_total             11072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200739a_si_002.cif
_cod_data_source_block           cscocb13
_cod_original_cell_volume        5755.0(6)
_cod_database_code               4065371