Chiral thiahelicene-based alkyl phosphine-borane complexes: synthesis, X-ray characterization, and theoretical and experimental investigations of optical properties.
Dova, Davide; Cauteruccio, Silvia; Prager, Stefan; Dreuw, Andreas; Graiff, Claudia; Licandro, Emanuela; The Journal of organic chemistry 80 (2015) 3921–3928; doi:10.1021/acs.joc.5b00243

data_4036139
_publ_section_title
;
 Chiral thiahelicene-based alkyl phosphine-borane complexes: synthesis,
 X-ray characterization, and theoretical and experimental investigations
 of optical properties.
;
_journal_issue                   8
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3921
_journal_page_last               3928
_journal_paper_doi               10.1021/acs.joc.5b00243
_journal_volume                  80
_journal_year                    2015
_chemical_formula_sum            'C39.5 H50 B Cl P S4'
_chemical_formula_weight         730.27
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 118.668(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.939(5)
_cell_length_b                   11.4367(17)
_cell_length_c                   22.415(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     8084(2)
_computing_cell_refinement       'APEX II (Bruker, 2008)'
_computing_data_collection       'APEX II (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'omega scan'
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            64390
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6488
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         12323
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1704
_reflns_number_gt                7448
_reflns_number_total             12323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5b00243_si_001.cif
_cod_data_source_block           monosubstituted_ddd38
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C39.50 H50 B Cl P S4'
_cod_database_code               4036139