Helical organization of chiral binaphthyl tetrathiafulvalene primary amides through hydrogen bonding interactions
Saad, Ali; Jeannin, Olivier; Fourmigué, Marc; CrystEngComm 12 (2010) 3866–; doi:10.1039/c004320f

data_7238292
_publ_section_title
;
 Helical organization of chiral binaphthyl tetrathiafulvalene primary
 amides through hydrogen bonding interactions
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              3866
_journal_paper_doi               10.1039/c004320f
_journal_volume                  12
_journal_year                    2010
_chemical_absolute_configuration rmad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H22 O6 S4'
_chemical_formula_sum            'C32 H22 O6 S4'
_chemical_formula_weight         630.74
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-09-28T17:23:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.52(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.007(13)
_cell_length_b                   7.425(2)
_cell_length_c                   11.354(5)
_cell_measurement_reflns_used    2454
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.42
_cell_measurement_wavelength     0.71073
_cell_volume                     2843.6(19)
_computing_cell_refinement       'Bruker SMART, 2006'
_computing_data_collection       'Bruker SMART, 2006'
_computing_data_reduction        'Bruker SAINT, 2006'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by SAINT Bruker-AXS'
_diffrn_orient_matrix_UB_11      0.252255E-1
_diffrn_orient_matrix_UB_12      0.420702E-1
_diffrn_orient_matrix_UB_13      -0.163921E-1
_diffrn_orient_matrix_UB_21      0.131404E-1
_diffrn_orient_matrix_UB_22      0.6811E-3
_diffrn_orient_matrix_UB_23      0.897902E-1
_diffrn_orient_matrix_UB_31      0.83643E-2
_diffrn_orient_matrix_UB_32      -0.127947
_diffrn_orient_matrix_UB_33      -0.49119E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9709
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         2.63
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.38
_exptl_absorpt_correction_T_max  1.
_exptl_absorpt_correction_T_min  0.511556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5732
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+2.0928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                4944
_reflns_number_total             5732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c004320f.txt
_cod_data_source_block           ast11
_cod_original_cell_volume        2843.5(18)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7238292