6-Allyl-8,8-dimethyl-3-oxo-2-(1-phenylethyl)-2-azabicyclo[4.3.0]non-1(9)-ene-5-carboxylic Acid, a Key Compound in the Asymmetric Synthesis of Quadrone
Chiaroni, Angèle; Riche, Claude; Dumas Franc̨oise; Mauduit, Marc; Miet, Christine; Acta Crystallographica Section C 54 (1998) 401–403; doi:10.1107/S0108270197015448

data_2007070
_publ_section_title
;6-Allyl-8,8-dimethyl-3-oxo-2-(1-phenylethyl)-2-azabicyclo[4.3.0]non-1(9)-ene-5-carboxylic
 Acid, a Key Compound in the Asymmetric Synthesis of Quadrone
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              401
_journal_page_last               403
_journal_paper_doi               10.1107/S0108270197015448
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C22 H27 N O3'
_chemical_formula_structural     'C22 H27 N O3'
_chemical_formula_sum            'C22 H27 N O3'
_chemical_formula_weight         353.45
_chemical_melting_point          423
_chemical_name_systematic
;
[N-(1'-Phenylethyl)-2-azabicyclo[4,3,0]-6-allyl-8,8-dimethyl-3-oxonon
-5-yl]-carboxylic acid
;
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.154(7)
_cell_length_b                   13.154(7)
_cell_length_c                   11.869(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.2
_cell_measurement_theta_min      8.7
_cell_volume                     2054(2)
_computing_cell_refinement       'Philips PW1100/20 software'
_computing_data_collection       'Philips PW1100/20 software'
_computing_data_reduction        'PHIL (Riche, 1981)'
_computing_molecular_graphics    'R3M (Riche, 1983) and  ORTEP (Johnson, 1963)'
_computing_publication_material  'ACTACIF (Riche, 1992)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Philips PW1100'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3951
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 600
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.54
_refine_diff_density_max         0.121
_refine_diff_density_min         -0.092
_refine_ls_abs_structure_details 'given by chemistry'
_refine_ls_extinction_coef       0.045(3)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.083
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_hydrogen_treatment    'H atoms: see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         1897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.329
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.040
_refine_ls_R_factor_obs          .031
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0942P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.095
_refine_ls_wR_factor_obs         .073
_reflns_number_observed          1682
_reflns_number_total             1899
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            cf1188.cif
_cod_data_source_block           cf1188
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 'Tetragonal' changed to 'tetragonal'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0942P] where P = (Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0942P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2007070