ZrIV-Monosubstituted Keggin-Type Dimeric Polyoxometalates: Synthesis, Characterization, Catalysis of H2O2-Based Oxidations, and Theoretical Study
Kholdeeva, Oxana A.; Maksimov, Gennadii M.; Maksimovskaya, Raisa I.; Vanina, Marina P.; Trubitsina, Tatiana A.; Naumov, Dmitry Yu.; Kolesov, Boris A.; Antonova, Nadya S.; Carbó, Jorge J.; Poblet, Josep M.; Inorganic Chemistry 45 (2006) 7224–7234; doi:10.1021/ic0608142

data_4332760
_publ_section_title
;
 ZrIV-Monosubstituted Keggin-Type Dimeric Polyoxometalates:&#x00A0;
 Synthesis, Characterization, Catalysis of H2O2-Based Oxidations, and
 Theoretical Study
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7224
_journal_page_last               7234
_journal_paper_doi               10.1021/ic0608142
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C128 H290 N8 O80 P2 W22 Zr2'
_chemical_formula_weight         7510.76
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 109.130(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.104(2)
_cell_length_b                   47.406(7)
_cell_length_c                   15.344(2)
_cell_measurement_reflns_used    8299
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.64
_cell_volume                     10380(2)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52539
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.09
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.319
_exptl_absorpt_correction_T_max  0.202
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP (Bruker, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6980
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.734
_refine_diff_density_min         -2.154
_refine_diff_density_rms         0.265
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1106
_refine_ls_number_reflns         19122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0690
_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^)+(0.0160P)^2^+418.7996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                13678
_reflns_number_total             19122
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic0608142sup1.cif
_cod_data_source_block           hold004
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4332760