Honeycomb supramolecular frameworks of organic‒inorganic hybrid cluster composed of cation radical and Keggin-type polyoxometalate
Zhang, Shangxi; Lu, Xiaofeng; Sun, Jibin; Zhao, Yali; Shao, Xiangfeng; CrystEngComm 17 (2015) 4110–; doi:10.1039/C5CE00510H

data_7220322
_publ_section_title
;
 Honeycomb supramolecular frameworks of organic--inorganic hybrid cluster
 composed of cation radical and Keggin-type polyoxometalate
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4110
_journal_paper_doi               10.1039/C5CE00510H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C67 H36 Cl2 Mo12 O40 P S36'
_chemical_formula_sum            'C67 H36 Cl2 Mo12 O40 P S36'
_chemical_formula_weight         3888.27
_chemical_name_common            (TT-TTF)3(PMo12O40)
_chemical_name_systematic
;
(TT-TTF)3(PMo12O40)
;
_chemical_properties_physical    Heat-sensitive
_chemical_temperature_decomposition 423
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-08 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   23.7742(3)
_cell_length_b                   23.7742(3)
_cell_length_c                   13.7571(2)
_cell_measurement_reflns_used    14432
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.4620
_cell_measurement_theta_min      3.4150
_cell_volume                     6733.94(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    Mercury
_computing_publication_material  Mercury
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27533
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    1.753
_exptl_absorpt_correction_T_max  0.7790
_exptl_absorpt_correction_T_min  0.6490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal block'
_exptl_crystal_F_000             3774
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'The crystals were obtained by slow diffusion of two components through a three-layer technique'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         10406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+5.4269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                8903
_reflns_number_total             10406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00510h2.cif
_cod_data_source_block           100k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '423,
decomposed'. The value '423, decomposed' was changed to '423'.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7220322.cif.
;
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               7220322