Three component synthesis of oxa-bridged tetracyclic tetrahydroquinolines.
González-Zamora, E; Fayol, A.; Bois-Choussy, M; Chiaroni, A.; Zhu, J.; Chemical communications (Cambridge, England)  (2001) 1684–1685; doi:10.1039/b104317j

data_7125475
_publ_section_title
;
 Three component synthesis of oxa-bridged tetracyclic
 tetrahydroquinolines.
;
_journal_issue                   17
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1684
_journal_page_last               1685
_journal_paper_doi               10.1039/b104317j
_journal_year                    2001
_chemical_compound_source        'Chemical synthesis'
_chemical_formula_moiety         'C31 H39 N3 O4'
_chemical_formula_structural     'C31 H39 N3 O4'
_chemical_formula_sum            'C31 H39 N3 O4'
_chemical_formula_weight         517.65
_chemical_name_common            MEXI01
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.64(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.049(5)
_cell_length_b                   9.982(5)
_cell_length_c                   20.886(8)
_cell_measurement_reflns_used    13968
_cell_measurement_temperature    293(2)
_cell_volume                     2903(2)
_computing_cell_refinement
;
'DENZO (Otwinowski & Minor, 1997)  COLLECT (Hooft, 1998)' 
;
_computing_data_collection
;
'DENZO (Otwinowski & Minor, 1997)  COLLECT (Hooft, 1998)' 
;
_computing_data_reduction        'HKL package (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'R3M (Riche, 1983) ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius kappaCCD area-detector diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8306
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0118(37)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.101
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_restrained_S_obs      1.181
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          -0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[\s^2^(Fo^2^)+(0.1122P)^2^+1.5059P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2294
_refine_ls_wR_factor_ref         0.1998
_reflns_number_gt                3303
_reflns_number_total             4665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104317j.txt
_cod_data_source_block           mexi
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

data item '_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.1122P)^2^+1.5059P] where P==(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. A new data item '_refine_ls_weighting_details'
was created with the value set to
'w==1/[\s^2^(Fo^2^)+(0.1122P)^2^+1.5059P] where P==(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2903.0(21)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7125475