Hydrogen Bonds in Radical Cation Salts of TTF(CH2OH)4: First Complete Series with the Octahedral Rhenium Cluster Anions [Re6S8-nCl6+n]n-4(n= 0, 1, 2, 3)
Perruchas, Sandrine; Boubekeur, Kamal; Batail, Patrick; Crystal Growth & Design 5 (2005) 1585–; doi:10.1021/cg0500573

data_4505114
_publ_section_title
;
 Hydrogen Bonds in Radical Cation Salts of TTF(CH2OH)4:&#x2009; First
 Complete Series with the Octahedral Rhenium Cluster Anions
 [Re6S8-nCl6+n]n-4(n= 0, 1, 2, 3)
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1585
_journal_paper_doi               10.1021/cg0500573
_journal_volume                  5
_journal_year                    2005
_chemical_formula_moiety         C40H48Cl6O16Re6S24
_chemical_formula_sum            'C40 H48 Cl6 O16 Re6 S24'
_chemical_formula_weight         2884.12
_chemical_name_common            '(TTF(CH2OH)4)4, Re6S8Cl6'
_chemical_name_systematic
;
[TTF(CH2OH)4]4[Re6S8Cl6]
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c 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                   16.393(2)
_cell_length_b                   16.393(2)
_cell_length_c                   26.063(5)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.05
_cell_volume                     7003.9(18)
_computing_cell_refinement       'SELECT, CELL  [STOE-IPDS]'
_computing_data_collection       'EXPOSE [STOE-IPDS]'
_computing_data_reduction        'INTEGRATE [STOE-IPDS]'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       'rotation, phi incr. 0.9'
_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  0.0975
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            42978
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    11.333
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.735
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5408
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.979
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0245
_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
 [0.00000+1.00000exp(1.60(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0242P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0485
_reflns_number_gt                2243
_reflns_number_total             3388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0500573si20050213_123249.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        7004(2)
_cod_original_sg_symbol_Hall     '-P 4a 2ac '
_cod_original_sg_symbol_H-M      P4/ncc
_cod_database_code               4505114