Reverse-Keggin Ions: Polycondensation of Antimonate Ligands Give Inorganic Cryptand
Viswanathan Baskar; Maheswaran Shanmugam; Madeleine Helliwell; Simon J. Teat; Richard E. P. Winpenny; Journal of the American Chemical Society 129 (2007) 3042–3043; doi:10.1021/ja068214p

data_4109178
_publ_section_title
;
 Reverse-Keggin Ions: Polycondensation of Antimonate Ligands Give
 Inorganic Cryptand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3042
_journal_page_last               3043
_journal_paper_doi               10.1021/ja068214p
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C83 H84 Mn5 N4 O38 Sb12'
_chemical_formula_weight         3481.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_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                 101.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.397(4)
_cell_length_b                   25.825(5)
_cell_length_c                   22.624(5)
_cell_measurement_reflns_used    7590
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      2.28
_cell_volume                     11116(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1269
_diffrn_reflns_av_sigmaI/netI    0.0923
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            69921
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    3.486
_exptl_absorpt_correction_T_max  0.6229
_exptl_absorpt_correction_T_min  0.5424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_description       Plate
_exptl_crystal_F_000             6604
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.028
_refine_diff_density_min         -3.795
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         26059
_refine_ls_number_restraints     601
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+45.4395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1950
_refine_ls_wR_factor_ref         0.2095
_reflns_number_gt                20119
_reflns_number_total             26059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja068214psi20070119_111606.cif
_cod_data_source_block           repw265p21n
_cod_original_cell_volume        11115(4)
_cod_database_code               4109178