Facile Synthetic Route to Highly Luminescent Sila[7]helicene
Oyama, Hiromi; Nakano, Koji; Harada, Takunori; Kuroda, Reiko; Naito, Masanobu; Nobusawa, Kazuyuki; Nozaki, Kyoko; Organic Letters 15 (2013) 2104–; doi:10.1021/ol4005036

data_1511910
_publ_section_title
;
 Facile Synthetic Route to Highly Luminescent Sila[7]helicene
;
_journal_issue                   9
_journal_name_full               'Organic Letters'
_journal_page_first              2104
_journal_paper_doi               10.1021/ol4005036
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C30 H22 Si'
_chemical_formula_weight         410.57
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   7.199(3)
_cell_length_b                   14.568(5)
_cell_length_c                   20.830(8)
_cell_measurement_reflns_used    1942
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2541
_cell_measurement_theta_min      34.0459
_cell_volume                     2184.5(14)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.2371
_diffrn_reflns_av_sigmaI/netI    0.1730
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32132
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         6.08
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_T_max  0.9031
_exptl_absorpt_correction_T_min  0.8189
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(9)
_refine_ls_extinction_coef       0.0024(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0998
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2328
_refine_ls_wR_factor_ref         0.2671
_reflns_number_gt                2122
_reflns_number_total             3905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4005036_si_002.cif
_cod_data_source_block           ydkr
_cod_original_cell_volume        2184.4(13)
_cod_database_code               1511910