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_4505112
_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         C20H24Cl14Mo6O8S8
_chemical_formula_sum            'C20 H24 Cl14 Mo6 O8 S8'
_chemical_formula_weight         1720.81
_chemical_name_common            '2 TTF(CH2OH)4, Mo6Cl14'
_chemical_name_systematic
;
[TTF(CH2OH)4]2[Mo6Cl14]
;
_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                62.475(13)
_cell_angle_beta                 70.948(14)
_cell_angle_gamma                84.463(14)
_cell_formula_units_Z            1
_cell_length_a                   9.4212(11)
_cell_length_b                   12.0528(14)
_cell_length_c                   12.1076(16)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      1.95
_cell_volume                     1150.0(3)
_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 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       'rotation, phi incr. 1.9'
_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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11533
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    2.805
_exptl_absorpt_correction_T_max  0.693
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.485
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             826
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0406P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                3440
_reflns_number_total             4115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0500573si20050213_123249.cif
_cod_data_source_block           2b
_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        1150.0(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505112