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_4109180
_publ_contact_author
; 
 Madeleine Helliwell and Eswar
;
_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            'C157 H163.5 N6.5 Na9 O82.5 Sb24'
_chemical_formula_weight         6590.35
_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                104.8440(10)
_cell_angle_beta                 100.5190(10)
_cell_angle_gamma                96.9590(10)
_cell_formula_units_Z            2
_cell_length_a                   19.2278(12)
_cell_length_b                   21.1616(14)
_cell_length_c                   29.4465(19)
_cell_measurement_reflns_used    8843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     11207.8(13)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            89644
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    2.938
_exptl_absorpt_correction_T_max  0.7577
_exptl_absorpt_correction_T_min  0.5911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_description       plate
_exptl_crystal_F_000             6268
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.699
_refine_diff_density_min         -1.917
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2161
_refine_ls_number_reflns         44992
_refine_ls_number_restraints     1155
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+143.5934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1823
_reflns_number_gt                31629
_reflns_number_total             44992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja068214psi20070119_111717.cif
_cod_data_source_block           z:\repw271d\work\repw271a
_cod_depositor_comments
;

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C314 H327 N13 Na18 O165 Sb48'
_cod_original_formula_weight         13180.71
_cod_original_formula_units_Z            1
_cod_original_cell_volume        11207.8(12)
_cod_database_code               4109180