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_4036140
_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            'C58 H84 B2 P2 S4'
_chemical_formula_weight         993.05
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                82.239(3)
_cell_angle_beta                 89.817(3)
_cell_angle_gamma                68.130(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0104(14)
_cell_length_b                   13.3519(19)
_cell_length_c                   23.116(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2837.3(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            40163
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6446
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         14074
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                8672
_reflns_number_total             14074
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo5b00243_si_001.cif
_cod_data_source_block           disubstituted_zz3tri075
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4036140