Mixed Valence Creutz‒Taube Ion Analogues Incorporating Thiacrowns: Synthesis, Structure, Physical Properties, and Computational Studies
Adams, Harry; Costa, Paulo J.; Newell, Mike; Vickers, Steven J.; Ward, Michael D.; Félix, Vítor; Thomas, Jim A.; Inorganic Chemistry 48 (2009) 5584–5584; doi:10.1021/ic900536a

data_4302400
_publ_section_title
;
 Mixed Valence Creutz--Taube Ion Analogues Incorporating Thiacrowns:
 Synthesis, Structure, Physical Properties, and Computational Studies
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5584
_journal_page_last               5584
_journal_paper_doi               10.1021/ic900536a
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C20 H36 Cl2 F12 N2 P2 Ru2 S8'
_chemical_formula_weight         1123.97
_space_group_IT_number           137
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2a'
_symmetry_space_group_name_H-M   'P 42/n m c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.286(2)
_cell_length_b                   21.286(2)
_cell_length_c                   9.5157(15)
_cell_measurement_reflns_used    1845
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      43.205
_cell_measurement_theta_min      4.689
_cell_volume                     4311.5(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0917
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18201
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.7637
_exptl_absorpt_correction_T_min  0.6555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.496
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1659
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.2008
_reflns_number_gt                1040
_reflns_number_total             1659
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4338555
_cod_data_source_file            ic900536a_si_001.cif
_cod_data_source_block           iaj151m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4311.3(10)
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_database_code               4302400