Synthesis and structure of dinuclear hafnium(IV) and zirconium(IV) complexes sandwiched between 2 mono-lacunary α-Keggin polyoxometalates
Nomiya, Kenji; Saku, Yoshio; Yamada, Shingo; Takahashi, Wataru; Sekiya, Hiromi; Shinohara, Akira; Ishimaru, Megumi; Sakai, Yoshitaka; Dalton Transactions  (2009) 5504–5511; doi:10.1039/b902296a

data_7001682
_publ_section_title
;
 Synthesis and structure of dinuclear hafnium(IV) and zirconium(IV)
 complexes sandwiched between 2 mono-lacunary \a-Keggin
 polyoxometalates
;
_journal_issue                   28
_journal_name_full               'Dalton Transactions'
_journal_page_first              5504
_journal_page_last               5511
_journal_paper_doi               10.1039/b902296a
_journal_year                    2009
_chemical_formula_sum            'C32 H116 N8 O89 P2 W22 Zr2'
_chemical_formula_weight         6326.41
_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-97
_cell_angle_alpha                78.825(3)
_cell_angle_beta                 79.372(3)
_cell_angle_gamma                88.416(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8103(19)
_cell_length_b                   20.785(3)
_cell_length_c                   23.081(4)
_cell_measurement_reflns_used    5497
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.42
_cell_volume                     5462.9(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0766
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            38940
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    23.374
_exptl_absorpt_correction_T_max  0.5407
_exptl_absorpt_correction_T_min  0.1273
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.846
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5628
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         6.946
_refine_diff_density_min         -4.442
_refine_diff_density_rms         0.642
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1312
_refine_ls_number_reflns         26585
_refine_ls_number_restraints     3822
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0924P)^2^+85.2448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1734
_reflns_number_gt                19844
_reflns_number_total             26585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902296a.txt
_cod_data_source_block           wt001p-1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7001682