Bis(ethylenedithio)tetrathiafulvalene Radical Salts with Anderson Type Heteropolymolybdates Containing Tris(alkoxo) Ligands
Liu, Cai-Ming; Huang, Yong-Hong; Zhang, De-Qing; Gao, Song; Jiang, Feng-Chi; Zhang, Jian-Ying; Zhu, Dao-Ben; Crystal Growth & Design 5 (2005) 1531–; doi:10.1021/cg050004l

data_4505079
_publ_section_title
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 Bis(ethylenedithio)tetrathiafulvalene Radical Salts with Anderson Type
 Heteropolymolybdates Containing Tris(alkoxo) Ligands
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1531
_journal_paper_doi               10.1021/cg050004l
_journal_volume                  5
_journal_year                    2005
_chemical_formula_sum            'C60 H58 Mn Mo6 O31 S40'
_chemical_formula_weight         3188.04
_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
_cell_angle_alpha                99.53(3)
_cell_angle_beta                 100.79(3)
_cell_angle_gamma                99.37(3)
_cell_formula_units_Z            1
_cell_length_a                   9.427(2)
_cell_length_b                   12.546(3)
_cell_length_c                   22.514(5)
_cell_measurement_temperature    150(2)
_cell_volume                     2527.4(11)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2001)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2001)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2001)'
_computing_molecular_graphics    'SHELXL (Siemens, 1994)'
_computing_publication_material  'SHELXL (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Rigaku R-AXIS 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  0.0805
_diffrn_reflns_av_sigmaI/netI    0.3418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16250
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         0.94
_exptl_absorpt_coefficient_mu    1.742
_exptl_absorpt_correction_T_max  1.2013
_exptl_absorpt_correction_T_min  0.7859
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_meas      Empirical
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Thin plate'
_exptl_crystal_F_000             1583
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.073
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.250
_refine_ls_extinction_coef       0.00322(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.675
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         10957
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.675
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0654P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1488
_reflns_number_gt                3845
_reflns_number_total             10957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050004lsi20050106_030312.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'PSI scan'
changed to 'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2527.4(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505079