Optically active diaryl tetrahydroisoquinoline derivatives
Naicker, Tricia; Govender, Thavendran; Kruger, Hendrik G.; Maguire, Glenn E. M.; Acta Crystallographica Section C 67 (2011) o100–o103; doi:10.1107/S0108270110053357

data_2018019
_publ_section_title
;
 Optically active diaryl tetrahydroisoquinoline derivatives
;
_journal_coeditor_code           SF3143
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o100
_journal_page_last               o103
_journal_paper_doi               10.1107/S0108270110053357
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C40 H43 N O3 Si'
_chemical_formula_moiety         'C40 H43 N O3 Si'
_chemical_formula_sum            'C40 H43 N O3 Si'
_chemical_formula_weight         613.84
_chemical_melting_point          459
_chemical_name_common            N-BenzylTIQdiphenyltrimethylsilyl
_chemical_name_systematic
;
(1<i>R</i>,3<i>S</i>)-2-benzyl-3-[diphenyl(trimethylsiloxy)methyl]-
6,7-dimethoxy-1-phenyl-1,2,3,4-tetrahydroisoquinoline
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.287(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.045(10)
_cell_length_b                   17.008(15)
_cell_length_c                   18.489(15)
_cell_measurement_reflns_used    37993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.95
_cell_measurement_theta_min      1.91
_cell_volume                     3350(5)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEXII DUO'
_diffrn_measurement_method       '0.5\% \f scans and \w'
_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  0.0636
_diffrn_reflns_av_sigmaI/netI    0.0992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37993
_diffrn_reflns_theta_full        28.95
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.9892
_exptl_absorpt_correction_T_min  0.9764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flat
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.405
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_coef       0.0031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         17263
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0476P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                11255
_reflns_number_total             17263
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3143.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2018019
_cod_database_fobs_code          2018019