(1<i>R</i>,3<i>S</i>)-Methyl 2-benzyl-6,7-dimethoxy-1-phenyl-1,2,3,4-tetrahydroisoquinoline-3-carboxylate
Naicker, Tricia; McKay, Michael; Govender, Thavendran; Kruger, Hendrik G.; Maguire, Glenn E. M.; Acta Crystallographica Section E 65 (2009) o3278–; doi:10.1107/S1600536809050521

data_2224292
_publ_section_title
;
 (1<i>R</i>,3<i>S</i>)-Methyl
 2-benzyl-6,7-dimethoxy-1-phenyl-1,2,3,4-tetrahydroisoquinoline-3-carboxylate
;
_journal_coeditor_code           HG2607
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3278
_journal_paper_doi               10.1107/S1600536809050521
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C26 H27 N O4'
_chemical_formula_moiety         'C26 H27 N O4'
_chemical_formula_sum            'C26 H27 N O4'
_chemical_formula_weight         417.49
_chemical_melting_point          420
_chemical_name_common            tetrahydroisoquinoline
_chemical_name_systematic
;
(1<i>R</i>,3<i>S</i>)-Methyl 2-benzyl-6,7-dimethoxy-1-phenyl-1,2,3,4-
tetrahydroisoquinoline-3-carboxylate
;
_space_group_IT_number           1
_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                73.3650(10)
_cell_angle_beta                 74.6940(10)
_cell_angle_gamma                75.7370(10)
_cell_formula_units_Z            1
_cell_length_a                   6.01990(10)
_cell_length_b                   9.2592(2)
_cell_length_c                   11.0429(2)
_cell_measurement_reflns_used    7546
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.88
_cell_measurement_theta_min      4.27
_cell_volume                     559.045(19)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
ORTEP-3 for Windows (Farrugia, 1997)
;
_computing_structure_refinement
'SHELXL97 (Sheldrick, 2008) and X-SEED (Barbour, 2001)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker Kappa Duo APEXII diffractometer'
_diffrn_measurement_method       '0.5\% \f scans and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7546
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.88
_diffrn_reflns_theta_min         4.27
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             222
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.159
_refine_ls_abs_structure_details 'Flack (1983), 1483 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(14)
_refine_ls_extinction_coef       0.0426(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXS97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3561
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0475P)^2^+0.0785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                3536
_reflns_number_total             3561
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2607.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        559.045(18)
_cod_database_code               2224292
_cod_database_fobs_code          2224292