Synthesis and characterization of two polyoxometalates consisting of different Cu-ligand hydrogen phosphate units
Yan, Jinshuang; Zhao, Xiaofang; Huang, Jiao; Gong, Kaining; Han, Zhangang; Zhai, Xueliang; Journal of Solid State Chemistry 211 (2014) 200–205; doi:10.1016/j.jssc.2013.12.029

data_1562470
_publ_section_title
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 Synthesis and characterization of two polyoxometalates consisting of
 different Cu-ligand hydrogen phosphate units
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              200
_journal_page_last               205
_journal_paper_doi               10.1016/j.jssc.2013.12.029
_journal_volume                  211
_journal_year                    2014
_chemical_formula_sum            'C72 H84 Cu6 N12 O60 P5 W12'
_chemical_formula_weight         4819.80
_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
_cell_angle_alpha                92.596(6)
_cell_angle_beta                 92.460(5)
_cell_angle_gamma                102.299(5)
_cell_formula_units_Z            1
_cell_length_a                   11.303(4)
_cell_length_b                   14.935(5)
_cell_length_c                   16.547(5)
_cell_measurement_reflns_used    4858
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.28
_cell_volume                     2722.4(16)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13344
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    13.936
_exptl_absorpt_correction_T_max  0.2645
_exptl_absorpt_correction_T_min  0.2004
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.940
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2217
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.362
_refine_diff_density_min         -3.379
_refine_diff_density_rms         0.427
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         9440
_refine_ls_number_restraints     1674
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0822P)^2^+85.1064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1946
_reflns_number_gt                7016
_reflns_number_total             9440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2014-211-200.cif
_cod_data_source_block           compound-2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1562470