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_4109177
_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            'C76 H90 Mn5 N O42 Sb12'
_chemical_formula_weight         3425.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c 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                   38.1126(17)
_cell_length_b                   25.3743(11)
_cell_length_c                   27.1887(12)
_cell_measurement_reflns_used    13725
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.65
_cell_measurement_theta_min      2.205
_cell_volume                     26294(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67090
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            108629
_diffrn_reflns_theta_full        19.60
_diffrn_reflns_theta_max         19.60
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    2.947
_exptl_absorpt_correction_T_max  0.9627
_exptl_absorpt_correction_T_min  0.8092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       Plate
_exptl_crystal_F_000             13008
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.440
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     941
_refine_ls_number_reflns         13725
_refine_ls_number_restraints     475
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0997P)^2^+304.3424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.2058
_reflns_number_gt                10325
_reflns_number_total             13725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja068214psi20070119_111543.cif
_cod_data_source_block           e132
_cod_database_code               4109177