Crystal structure of tetramethyltetrathiafulvalenium (1<i>S</i>)-camphor-10-sulfonate dihydrate
Sommer, Mathieu; Allain, Magali; Mézière, Cécile; Pop, Flavia; Giffard, Michel; Acta Crystallographica Section E 71 (2015) 748–751; doi:10.1107/S2056989015010294

data_2240808
_publ_section_title
;
 Crystal structure of tetramethyltetrathiafulvalenium
 (1<i>S</i>)-camphor-10-sulfonate dihydrate
;
_journal_coeditor_code           BG2555
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              748
_journal_page_last               751
_journal_paper_doi               10.1107/S2056989015010294
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C10 H12 S4 +, C10 H15 O4 S -, 2H2 O'
_chemical_formula_moiety         'C10 H12 S4 +, C10 H15 O4 S -, 2(H2 O)'
_chemical_formula_sum            'C20 H31 O6 S5'
_chemical_formula_weight         527.75
_chemical_name_common
;
Tetramethyltetrathiafulvalenium (1<i>S</i>)-camphor-10-sulfonate dihydrate
;
_chemical_name_systematic
;
Tetramethyltetrathiafulvalenium
(<i>S</i>)-(7,7-dimethyl-2-methylidenebicyclo[2.2.1]heptan-1-yl)methanesulfonate
dihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.331(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1612(6)
_cell_length_b                   12.537(2)
_cell_length_c                   26.906(4)
_cell_measurement_reflns_used    14430
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.27
_cell_volume                     2415.0(6)
_computing_cell_refinement
;
DIRAX (Duisenberg, 1992)
;
_computing_data_collection
;
COLLECT (Hooft, 2008)
;
_computing_data_reduction
;
EvalCCD (Duisenberg <i>et al.</i>,  2000)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2014)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            27748
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.334
_refine_ls_abs_structure_details
;
Flack (1983), 4218 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.15(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         9990
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.7423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                7458
_reflns_number_total             9990
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg2555sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2240808
_cod_database_fobs_code          2240808