A new structural family of heteropolytungstate lacunary complexes with the uranyl, UO22+, cation
Gaunt, Andrew J.; May, Iain; Copping, Roy; Bhatt, Anand I.; Collison, David; Danny Fox, O.; Travis Holman, K.; Pope, Michael T.; Dalton Transactions  (2003) 3009–; doi:10.1039/b302955g

data_7012956
_publ_section_title
;
 A new structural family of heteropolytungstate lacunary complexes with
 the uranyl, UO22+, cation
;
_journal_issue                   15
_journal_name_full               'Dalton Transactions'
_journal_page_first              3009
_journal_paper_doi               10.1039/b302955g
_journal_year                    2003
_chemical_formula_sum            'H102 N12 O97 Te2 U2 W18'
_chemical_formula_weight         5863.48
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 99.706(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.244(2)
_cell_length_b                   11.5781(14)
_cell_length_c                   47.682(6)
_cell_measurement_reflns_used    7404
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4955
_cell_measurement_theta_min      2.212
_cell_volume                     9384(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'XSHELL, Bruker'
_computing_publication_material  'XP, Bruker; Diamond 2.1e, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SMART platform CCD, Bruker'
_diffrn_measurement_method       '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  0.1019
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            85184
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    26.138
_exptl_absorpt_correction_T_max  0.029904
_exptl_absorpt_correction_T_min  0.005988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             10312
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.436
_refine_diff_density_min         -3.151
_refine_diff_density_rms         0.397
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         16590
_refine_ls_number_restraints     520
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+249.9294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                12136
_reflns_number_total             16590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302955g.txt
_cod_data_source_block           01083b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        9383(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012956