Stereoselective synthesis of configurationally stable functionalized ethano-bridged Tröger bases.
Michon, Christophe; Sharma, Ankit; Bernardinelli, Gérard; Francotte, Eric; Lacour, Jérôme; Chemical communications (Cambridge, England) 46 (2010) 2206–2208; doi:10.1039/b925065d

data_7105363
_publ_section_title
;
 Stereoselective synthesis of configurationally stable functionalized
 ethano-bridged Tr\"oger bases.
;
_journal_issue                   13
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2206
_journal_page_last               2208
_journal_paper_doi               10.1039/b925065d
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C25 H24 N2 O'
_chemical_formula_sum            'C25 H24 N2 O'
_chemical_formula_weight         368.5
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.0.1
_audit_creation_date             2007-11-20
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record             2010-02-11
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                90.00000
_cell_formula_units_Z            8
_cell_length_a                   23.9934(10)
_cell_length_b                   23.9934(10)
_cell_length_c                   6.8262(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      3.7
_cell_volume                     3929.7(3)
_computing_cell_refinement       'CELL (Stoe & Cie, 1999)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 1999)'
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_molecular_graphics    xtal_gx3
_computing_publication_material  xtal_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 6
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Stoe Ipds'
_diffrn_measurement_method       \f
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .087
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            22803
_diffrn_reflns_theta_full        25.8
_diffrn_reflns_theta_max         25.8
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .076
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          .28
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .18
_refine_diff_density_max         .252
_refine_diff_density_min         -.553
_refine_ls_abs_structure_details
;
The crystal structure is non-centrosymmetric, achiral, non-polar
but could show optical activity (see H.D. Flack, Helv. Chim. Acta 2003,
86, 905-921). Consequently, and in order to keep an acceptable value
of the data to parameter ratio, the Friedel opposites were not merged
and the Flack parameter was refined.
As expected for compounds containing only C, N and O atoms (here
Friedif=4 for MoKa), the associated uncertainty is very large and
do not allows to obtain any accurate result from this parameter.
;
_refine_ls_abs_structure_Flack   .37(277)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05(2)
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2304
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           .034
_refine_ls_shift/su_max          .0008
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     \w=1/[\s^2^(Fo)+0.0002(Fo^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .023
_reflns_Friedel_coverage         .878
_reflns_number_gt                2304
_reflns_number_total             3854
_reflns_threshold_expression     'refl observed if Fo > 1.99 \s(Fo)'
_cod_data_source_file            b925065d.txt
_cod_data_source_block           CHON
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               7105363