Molecular conductors from bis(ethylenedithio)tetrathiafulvalene with tris(oxalato)rhodate
Martin, Lee; Morritt, Alexander L.; Lopez, Jordan R.; Nakazawa, Yasuhiro; Akutsu, Hiroki; Imajo, Shusaku; Ihara, Yoshihiko; Zhang, Bin; Zhang, Yan; Guo, Yanjun; Dalton Trans.  (2017) –; doi:10.1039/C7DT00881C

data_7043588
_publ_section_title
;
 Molecular conductors from bis(ethylenedithio)tetrathiafulvalene with
 tris(oxalato)rhodate
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00881C
_journal_year                    2017
_chemical_formula_moiety         'C52 H38 F1 O13 Rh1 S32'
_chemical_formula_sum            'C52 H38 F O13 Rh S32'
_chemical_formula_weight         2018.88
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2017-03-09 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1002(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.32638(12)
_cell_length_b                   19.9527(3)
_cell_length_c                   35.0343(5)
_cell_measurement_reflns_used    12891
_cell_measurement_temperature    294
_cell_measurement_theta_max      28
_cell_measurement_theta_min      4
_cell_volume                     7207.87(17)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      294
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            24844
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.227
_diffrn_reflns_theta_min         3.098
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.112
_refine_diff_density_max         1.11
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6318
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.0010413
_refine_ls_shift/su_mean         0.0000469
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.146E+04 0.237E+04 0.147E+04 623. 151. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0821
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0821
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              46
_reflns_limit_l_min              0
_reflns_number_gt                5960
_reflns_number_total             7488
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.82
_oxford_diffrn_Wilson_scale      1.43
_oxford_refine_ls_r_factor_ref   0.0451
_oxford_refine_ls_scale          0.8910(16)
_oxford_reflns_number_all        6318
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7dt00881c2.cif
_cod_data_source_block           1
_cod_original_cell_volume        7207.87(10)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C52 H38 F1 O13 Rh1 S32'
_cod_database_code               7043588