Functionalized Thiophene-Based [7]Helicene: Chirooptical Properties versus Electron Delocalization
Andrzej Rajca; Maren Pink; Shuzhang Xiao; Makoto Miyasaka; Suchada Rajca; Kausik Das; Kristin Plessel; Journal of Organic Chemistry 74 (2009) 7504–7513; doi:10.1021/jo901769c

data_4024899
_publ_section_title
;
Functionalized Thiophene-Based [7]Helicene: Chirooptical Properties versus
Electron Delocalization
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7504
_journal_page_last               7513
_journal_paper_doi               10.1021/jo901769c
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C48 H62 Br2 S5'
_chemical_formula_sum            'C48 H62 Br2 S5'
_chemical_formula_weight         959.10
_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                86.056(3)
_cell_angle_beta                 78.703(3)
_cell_angle_gamma                80.682(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9503(11)
_cell_length_b                   12.8178(15)
_cell_length_c                   18.659(2)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      18.5
_cell_measurement_theta_min      2.3
_cell_volume                     2301.2(5)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      95(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details      '0.5 degree frames measured for 1 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48595
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42591
_diffrn_reflns_theta_full        18.38
_diffrn_reflns_theta_max         18.38
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    1.080
_exptl_absorpt_correction_T_max  0.9978
_exptl_absorpt_correction_T_min  0.9787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.00
_refine_diff_density_max         4.627
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         10306
_refine_ls_number_restraints     480
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0966
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1530P)^2^+18.7212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2632
_refine_ls_wR_factor_ref         0.2802
_reflns_number_gt                8012
_reflns_number_total             10306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901769c_si_001.cif
_cod_data_source_block           0591
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4024899