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_4023207
_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_sum            'C56 H65 F9 N2 O10'
_chemical_formula_weight         1097.10
_chemical_name_common            'compound 2-H+'
_chemical_name_systematic
; 
 (3R*,5S*,7aR*,9aS*)-3,5-di(4-methoxyphenyl)perhydrocyclopenta[ij]
 quinolizine trifluoroacetate 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             10/09/2007
_audit_creation_method           SHELXL-97
_audit_update_record             13/09/2007
_cell_angle_alpha                110.3030(10)
_cell_angle_beta                 98.6520(10)
_cell_angle_gamma                107.6590(10)
_cell_formula_units_Z            2
_cell_length_a                   11.3651(10)
_cell_length_b                   16.3126(14)
_cell_length_c                   17.2329(15)
_cell_measurement_reflns_used    667
_cell_measurement_temperature    273(2)
_cell_volume                     2735.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'bruker APEX2'
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27537
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.9890
_exptl_absorpt_correction_T_min  0.9782
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10142
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1169P)^2^+0.5474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2000
_refine_ls_wR_factor_ref         0.2462
_reflns_number_gt                5004
_reflns_number_total             10142
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo702172u-File005.cif
_cod_data_source_block           121bnh
_cod_database_code               4023207