Syntheses and X-ray crystal structures of zirconium(IV) and hafnium(IV) complexes containing monovacant wells-Dawson and Keggin polyoxotungstates.
Kato, Chika Nozaki; Shinohara, Akira; Hayashi, Kunihiko; Nomiya, Kenji; Inorganic chemistry 45 (2006) 8108–8119; doi:10.1021/ic060656e

data_4350336
_publ_section_title
;
 Syntheses and X-ray crystal structures of zirconium(IV) and hafnium(IV)
 complexes containing monovacant wells-Dawson and Keggin
 polyoxotungstates.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8108
_journal_page_last               8119
_journal_paper_doi               10.1021/ic060656e
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C40 H134 N10 O85 P2 W22 Zr'
_chemical_formula_weight         6313.43
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                118.7480(10)
_cell_angle_beta                 91.9300(10)
_cell_angle_gamma                100.8770(10)
_cell_formula_units_Z            4
_cell_length_a                   21.1348(16)
_cell_length_b                   25.5295(19)
_cell_length_c                   25.8012(19)
_cell_measurement_reflns_used    6571
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      20.70
_cell_measurement_theta_min      2.18
_cell_volume                     11860.3(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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1728
_diffrn_reflns_av_sigmaI/netI    0.2515
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            159331
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    21.449
_exptl_absorpt_correction_T_max  0.8141
_exptl_absorpt_correction_T_min  0.0935
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.536
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             11288
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         8.956
_refine_diff_density_min         -5.309
_refine_diff_density_rms         0.761
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2377
_refine_ls_number_reflns         58425
_refine_ls_number_restraints     1584
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.2160
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.548
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1923
_refine_ls_wR_factor_ref         0.2592
_reflns_number_gt                25050
_reflns_number_total             58425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060656esi20060418_114209.cif
_cod_data_source_block           k-zr
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4350336