Two multi-copper-containing heteropolyoxotungstates constructed from the lacunary Keggin polyoxoanion and the high-nuclear spin cluster.
Zhang, Zhiming; Qi, Yanfei; Qin, Chao; Li, Yangguang; Wang, Enbo; Wang, Xinlong; Su, Zhongmin; Xu, Lin; Inorganic chemistry 46 (2007) 8162–8169; doi:10.1021/ic7012864

data_4339441
_publ_section_title
;
 Two multi-copper-containing heteropolyoxotungstates constructed from the
 lacunary Keggin polyoxoanion and the high-nuclear spin cluster.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8162
_journal_page_last               8169
_journal_paper_doi               10.1021/ic7012864
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'Cu14 H77 Na16 O164.5 Si4 W32'
_chemical_formula_weight         9962.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   27.629(6)
_cell_length_b                   22.898(5)
_cell_length_c                   16.095(3)
_cell_measurement_reflns_used    8327
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.13
_cell_volume                     9327(4)
_computing_cell_refinement       auto
_computing_data_collection       auto
_computing_data_reduction        auto
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.1325
_diffrn_reflns_av_sigmaI/netI    0.1081
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35297
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    21.362
_exptl_absorpt_correction_T_max  0.014
_exptl_absorpt_correction_T_min  0.005
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8798
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.916
_refine_diff_density_min         -1.916
_refine_diff_density_rms         0.389
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         8327
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0523P)^2^+208.9460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1410
_reflns_number_gt                5314
_reflns_number_total             8327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7012864-file003.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        9327(3)
_cod_original_sg_symbol_H-M      C2/m
_cod_original_formula_sum        'Cu14 H77 Na16 O164.50 Si4 W32'
_cod_database_code               4339441