Organic‒inorganic hybrids based on monovacant Keggin-type polyoxotungstates and 3d‒4f heterometals
Zhao, Hai-Yan; Zhao, Jun-Wei; Yang, Bai-Feng; He, Huan; Yang, Guo-Yu; CrystEngComm 15 (2013) 8186–; doi:10.1039/c3ce41007b

data_7210585
_publ_section_title
;
 Organic--inorganic hybrids based on monovacant Keggin-type
 polyoxotungstates and 3d--4f heterometals
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              8186
_journal_paper_doi               10.1039/c3ce41007b
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C8 H67 Cu2 N8 O56 Si Tb W11'
_chemical_formula_weight         3508.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           1
_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                65.085(4)
_cell_angle_beta                 74.281(3)
_cell_angle_gamma                75.437(3)
_cell_formula_units_Z            1
_cell_length_a                   11.3955(4)
_cell_length_b                   12.1907(5)
_cell_length_c                   12.5537(5)
_cell_measurement_reflns_used    8235
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4011
_cell_measurement_theta_min      2.8437
_cell_volume                     1503.55(11)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_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  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11036
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.85
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    22.931
_exptl_absorpt_correction_T_max  0.2967
_exptl_absorpt_correction_T_min  0.1303
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    3.874
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1570
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         7.136
_refine_diff_density_min         -5.185
_refine_diff_density_rms         0.614
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         7688
_refine_ls_number_restraints     493
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1394P)^2^+53.0477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1860
_refine_ls_wR_factor_ref         0.1881
_reflns_number_gt                7231
_reflns_number_total             7688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41007b.txt
_cod_data_source_block           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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1503.55(10)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7210585