Silver(I)-Ethynide Clusters Constructed with Phosphonate-Functionized Polyoxovanadates
Yun-Peng Xie; Thomas C. W. Mak; Journal of the American Chemical Society 133 (2011) 3760–3763; doi:10.1021/ja1112035

data_4105785
_publ_section_title
;
 Silver(I)-Ethynide Clusters Constructed with Phosphonate-Functionized
 Polyoxovanadates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3760
_journal_page_last               3763
_journal_paper_doi               10.1021/ja1112035
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_sum            'C233 H284 Ag43 N11 O97 P12 V18'
_chemical_formula_weight         10717.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 99.636(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.597(7)
_cell_length_b                   23.139(7)
_cell_length_c                   33.025(10)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.25
_cell_volume                     17778(9)
_computing_cell_refinement       SAINT(Bruker,2001)
_computing_data_collection       APEX2(Bruker,2003)
_computing_data_reduction        APEX2(Bruker,2003)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            312311
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    2.874
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orang-red
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_description       block
_exptl_crystal_F_000             10300
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         5.144
_refine_diff_density_min         -4.103
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details 'Flack (1983), 41495 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.019(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3273
_refine_ls_number_reflns         85247
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+136.8319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                68221
_reflns_number_total             85247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1112035_si_002_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        17777(9)
_cod_database_code               4105785