Chair to Boat Interconversion and Face to Face Interactions in Isomeric Aryl-Substituted Perhydrocyclopentaquinolizines
Lodovico Lunazzi; Andrea Mazzanti; Shaik Rafi; H. Surya Prakash Rao; Journal of Organic Chemistry 73 (2008) 678–688; doi:10.1021/jo702172u

data_4023206
_publ_contact_author
;
Dr. Andrea Mazzanti
University of Bologna
Department of Organic Chemistry A.Mangini
Viale Risorgimento 4
40136 Bologna
Italy
;
_publ_contact_author_email       mazzand@ms.fci.unibo.it
_publ_contact_author_fax         '[039]051 209 3654'
_publ_contact_author_phone       '[039]051 209 3633'
_publ_section_title
;
 Chair to Boat Interconversion and Face to Face Interactions
 in Isomeric Aryl-Substituted Perhydrocyclopentaquinolizines
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              678
_journal_page_last               688
_journal_paper_doi               10.1021/jo702172u
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C25 H32 N O2, C2 F3 O2, C H Cl3'
_chemical_formula_sum            'C56 H66 Cl6 F6 N2 O8'
_chemical_formula_weight         1221.81
_chemical_name_common            'compound 2H+'
_chemical_name_systematic
; 
 (3S*,5R*,7aR*,9aS*)-3,5-di(4-methoxyphenyl)perhydrocyclopenta[ij]
 quinolizine trifluoroacetate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             14/06/2007
_audit_creation_method           SHELXL-97
_audit_update_record             13/09/2007
_cell_angle_alpha                90.00
_cell_angle_beta                 95.429(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6403(16)
_cell_length_b                   13.4738(13)
_cell_length_c                   25.472(3)
_cell_measurement_temperature    273(2)
_cell_volume                     5685.4(10)
_computing_cell_refinement       'Bruker APEX V1.27'
_computing_data_collection       'Bruker APEX V1.27'
_computing_data_reduction        'Bruker APEX V1.27'
_computing_molecular_graphics    'Mercury 1.4.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_measurement_method       'Bruker APEX2'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57235
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.9284
_exptl_absorpt_correction_T_min  0.8338
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         11172
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1147P)^2^+1.6459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2100
_reflns_number_gt                7514
_reflns_number_total             11172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo702172u-File004.cif
_cod_data_source_block           p21c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4023206