Acid-Induced Surface Functionalization of Polyoxometalate by Enclosure in a Polyhedral Silver-Alkynyl Cage
Guang-Gang Gao; Ping-Shing Cheng; Thomas C. W. Mak; Journal of the American Chemical Society 131 (2009) 18257–18259; doi:10.1021/ja907900b

data_4105504
_publ_section_title
;
 Acid-Induced Surface Functionalization of Polyoxometalate by Enclosure in
 a Polyhedral Silver-Alkynyl Cage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18257
_journal_page_last               18259
_journal_paper_doi               10.1021/ja907900b
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C146 H188 Ag40 F36 Mo6 O48'
_chemical_formula_weight         8285.34
_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                 93.970(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.290(3)
_cell_length_b                   20.470(3)
_cell_length_c                   27.561(4)
_cell_measurement_reflns_used    3543
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.80
_cell_volume                     12545(3)
_computing_cell_refinement       SAINT(Bruker,2001)
_computing_data_collection       APEX2(Bruker,2003)
_computing_data_reduction        APEX2(Bruker,2003)
_computing_molecular_graphics    DIAMOND
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SMART CCD APEX II'
_diffrn_measurement_method       '\w and \f'
_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  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            115952
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    3.383
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_description       block
_exptl_crystal_F_000             6866
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.446
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         24459
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0978P)^2^+49.8709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1957
_reflns_number_gt                14304
_reflns_number_total             24459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja907900b_si_002_2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4105504