Racemic 2,10-dibenzyloxy-12-chloro-3,9-dimethoxy-5,8,13,13a-tetrahydro-6<i>H</i>-dibenzo[<i>a,g</i>]quinolizine
Ding, Yu; Yao, Guang-Min; Chen, Yi-Lang; Yang, Yu-She; Acta Crystallographica Section E 61 (2005) o2020–o2021; doi:10.1107/S1600536805017307

data_2206200
_publ_section_title
;Racemic
 2,10-dibenzyloxy-12-chloro-3,9-dimethoxy-5,8,13,13a-tetrahydro-6<i>H</i>-dibenzo[<i>a,g</i>]quinolizine
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2020
_journal_page_last               o2021
_journal_paper_doi               10.1107/S1600536805017307
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C33 H32 Cl N O4'
_chemical_formula_moiety         'C33 H32 Cl N O4'
_chemical_formula_sum            'C33 H32 Cl N O4'
_chemical_formula_weight         542.05
_chemical_melting_point          422
_chemical_name_common
12-chloro-2,10-dibenzyloxy-3,9-dimethoxytetrahydroprotoberberine
_chemical_name_systematic
;
2,10-dibenzyloxy-12-chloro-3,9-dimethoxy-5,8,13,13a-
tetrahydro-6H-dibenzo[a,g]quinolizine
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_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                 126.549(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.4833(18)
_cell_length_b                   21.6089(18)
_cell_length_c                   16.0523(14)
_cell_measurement_reflns_used    3475
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      44.918
_cell_measurement_theta_min      4.951
_cell_volume                     5707.9(9)
_computing_cell_refinement       'SAINT (Bruker,2000)'
_computing_data_collection       'SMART (Bruker,2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f 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  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16679
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.417
_exptl_crystal_size_min          0.398
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.087
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0924P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                3798
_reflns_number_total             6226
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6192.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'C 2/c'
_cod_database_code               2206200
_cod_database_fobs_code          2206200