Sandwich-type HfIV and ZrIVcomplexes composed of tri-lacunary Keggin polyoxometalates: structure of [M3(μ-OH)3(A-α-PW9O34)2]9− (M = Hf and Zr)
Saku, Yoshio; Sakai, Yoshitaka; Shinohara, Akira; Hayashi, Kunihiko; Yoshida, Shoko; Kato, Chika N.; Yoza, Kenji; Nomiya, Kenji; Dalton Transactions  (2009) 805–813; doi:10.1039/b813710m

data_7000379
_publ_section_title
;
 Sandwich-type HfIV and ZrIVcomplexes composed of tri-lacunary Keggin
 polyoxometalates: structure of [M3(\m-OH)3(A-\a-PW9O34)2]9&#x2212; (M
 = Hf and Zr)
;
_journal_coden_ASTM              DTARAF
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              805
_journal_page_last               813
_journal_paper_doi               10.1039/b813710m
_journal_year                    2009
_chemical_formula_sum            'C28 H113 N7 O83 P2 W18 Zr3'
_chemical_formula_weight         5521.15
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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            16
_cell_length_a                   29.237(2)
_cell_length_b                   36.741(3)
_cell_length_c                   38.239(3)
_cell_measurement_temperature    90(2)
_cell_volume                     41076(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            108012
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    20.498
_exptl_absorpt_correction_T_max  0.3279
_exptl_absorpt_correction_T_min  0.0662
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             39616
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.507
_refine_diff_density_min         -1.606
_refine_diff_density_rms         0.491
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         12767
_refine_ls_number_restraints     1650
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0550P)^2^+1367.3883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                10733
_reflns_number_total             12767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B813710M.txt
_cod_data_source_block           yos002s
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_cell_volume        41077(5)
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               7000379