pH-Dependent Syntheses and Crystal Structures of a Series of Organic-Inorganic Hybrids Constructed from Keggin or Wells-Dawson Polyoxometalates and Silver Coordination Compounds
Hongxun Yang; Shuiying Gao; Jian Lü; Bo Xu; Jingxiang Lin; Rong Cao; Inorganic Chemistry 49 (2010) 736–744; doi:10.1021/ic902091p

data_4314608
_publ_section_title
;
 pH-Dependent Syntheses and Crystal Structures of a Series of
 Organic-Inorganic Hybrids Constructed from Keggin or Wells-Dawson
 Polyoxometalates and Silver Coordination Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              736
_journal_page_last               744
_journal_paper_doi               10.1021/ic902091p
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C50 H50 Ag4 N10 O66 P2 W18'
_chemical_formula_weight         5649.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            4
_cell_length_a                   24.789(5)
_cell_length_b                   22.241(5)
_cell_length_c                   17.334(4)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4758
_cell_measurement_theta_min      3.0696
_cell_volume                     9557(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Mercury70 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0873
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            71318
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.18
_diffrn_standards_number         11871
_exptl_absorpt_coefficient_mu    22.502
_exptl_absorpt_correction_T_max  0.509
_exptl_absorpt_correction_T_min  0.064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Semi-empirical from equivalents'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             9992
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.342
_refine_diff_density_min         -3.245
_refine_diff_density_rms         0.444
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         10962
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.098
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+98.4203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1466
_reflns_number_gt                9409
_reflns_number_total             10962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902091p_si_002_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314608