A Polyoxometalate Transfer Reagent: Synthesis, Structure, and Reactivity of Zirconocene Polyoxometalate [(PNbW11O40)2ZrCp2]6-
Emil V. Radkov; Victor G. Young; Robert H. Beer; Journal of the American Chemical Society 121 (1999) 8953–8954; doi:10.1021/ja9905039

data_4116544
_publ_section_title
;
 A Polyoxometalate Transfer Reagent: Synthesis, Structure, and Reactivity
 of Zirconocene Polyoxometalate [(PNbW11O40)2ZrCp2]6-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8953
_journal_page_last               8954
_journal_paper_doi               10.1021/ja9905039
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source        'Prof. R. Beer - Columbia University'
_chemical_formula_sum            'C108 H229 N7 Nb2 O80 P2 W22 Zr'
_chemical_formula_weight         7289.66
_chemical_name_common            96092
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                73.468(1)
_cell_angle_beta                 76.193(1)
_cell_angle_gamma                84.178(1)
_cell_formula_units_Z            2
_cell_length_a                   14.3725(2)
_cell_length_b                   26.2888(1)
_cell_length_c                   26.5749(4)
_cell_measurement_temperature    173(2)
_cell_volume                     9341.7(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            45157
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         0.81
_exptl_absorpt_coefficient_mu    13.746
_exptl_absorpt_correction_T_max  0.382
_exptl_absorpt_correction_T_min  0.004
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.592
_exptl_crystal_description       Needle
_exptl_crystal_F_000             6692
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.559
_refine_diff_density_min         -4.526
_refine_diff_density_rms         0.414
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.132
_refine_ls_goodness_of_fit_obs   1.161
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1474
_refine_ls_number_reflns         29655
_refine_ls_number_restraints     2304
_refine_ls_restrained_S_all      1.110
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_obs          0.0818
_refine_ls_shift/esd_max         0.031
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+861.4382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1783
_refine_ls_wR_factor_obs         0.1622
_reflns_number_observed          24156
_reflns_number_total             29661
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9905039.cif
_cod_data_source_block           96092
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+861.4382P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+861.4382P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116544