A dielectric anomaly observed for doubly reduced mixed-valence polyoxometalate
Nakamura, Ippei; Tsunashima, Ryo; Nishihara, Sadafumi; Inoue, Katsuya; Akutagawa, Tomoyuki; Chem. Commun.  (2017) –; doi:10.1039/C7CC03361C

data_7120218
_publ_section_title
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 A dielectric anomaly observed for doubly reduced mixed-valence
 polyoxometalate
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03361C
_journal_year                    2017
_chemical_formula_sum            'C47 H63 Mo12 N14 O45 P'
_chemical_formula_weight         2726.36
_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
_audit_update_record
;
2017-04-17 deposited with the CCDC.
2017-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                114.6658(7)
_cell_angle_beta                 106.7857(7)
_cell_angle_gamma                95.9885(7)
_cell_formula_units_Z            1
_cell_length_a                   11.9970(7)
_cell_length_b                   12.9020(7)
_cell_length_c                   14.6379(8)
_cell_measurement_reflns_used    4681
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      2.21
_cell_volume                     1904.30(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22708
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.034
_exptl_absorpt_correction_T_max  0.9605
_exptl_absorpt_correction_T_min  0.8225
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1322
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.194
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1075
_refine_ls_number_reflns         16942
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0498
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                13684
_reflns_number_total             16942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc03361c2.cif
_cod_data_source_block           ydkr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7120218