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_7120220
_publ_section_title
;
 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            'C21 H32 Mo6 N6 O25 P0.5'
_chemical_formula_weight         1359.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                62.519(3)
_cell_angle_beta                 79.896(4)
_cell_angle_gamma                89.318(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8074(2)
_cell_length_b                   12.9424(2)
_cell_length_c                   13.237
_cell_measurement_reflns_used    4881
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0357
_cell_volume                     1910.38(8)
_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      173(2)
_diffrn_detector_area_resol_mean 14.7275
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details
;
scan:
    Number of images: 720
               Slice: -65.0000 - 115.0000
         Image width: 0.2500
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 54.8861
              2theta: 24.9603
scan:
    Number of images: 720
               Slice: -65.0000 - 115.0000
         Image width: 0.2500
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 54.8861
              2theta: 24.9603
scan:
    Number of images: 720
               Slice: -65.0000 - 115.0000
         Image width: 0.2500
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 54.8861
              2theta: 24.9603

;
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16652
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    2.031
_exptl_absorpt_correction_T_max  0.7768
_exptl_absorpt_correction_T_min  0.4308
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1319
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.773
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         8216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.147
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0690
_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          0.2559
_refine_ls_wR_factor_ref         0.2586
_reflns_number_gt                7970
_reflns_number_total             8216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc03361c2.cif
_cod_data_source_block           crystalclear
_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.

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' 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_cell_volume        1910.45(4)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C21 H32 Mo6 N6 O25 P0.50'
_cod_database_code               7120220