pH-Dependent Assembly of Keggin-Based Supramolecular Architecture
Pei-Qing Zheng; Yan-Ping Ren; La-Sheng Long; Rong-Bin Huang; Lan-Sun Zheng; Inorganic Chemistry 44 (2005) 1190–1192; doi:10.1021/ic048708s

data_4308742
_publ_section_title
;
pH-Dependent Assembly of Keggin-Based Supramolecular Architecture
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1190
_journal_page_last               1192
_journal_paper_doi               10.1021/ic048708s
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C50 H88 N10 Ni2 O102 Si2 W24'
_chemical_formula_weight         7047.30
_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                 100.935(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.043(2)
_cell_length_b                   25.291(4)
_cell_length_c                   18.492(3)
_cell_measurement_temperature    298(2)
_cell_volume                     6448.4(17)
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Smart Apex 2000'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0734
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            55938
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    21.720
_exptl_absorpt_correction_T_max  0.1391
_exptl_absorpt_correction_T_min  0.0869
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    3.630
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             6268
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.659
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.369
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.279
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         10193
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.072
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+319.4176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                9531
_reflns_number_total             10193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048708ssi20040915_085656.cif
_cod_data_source_block           complex_1
_cod_original_cell_volume        6448.3(16)
_cod_database_code               4308742