8-(4-Methoxyphenyl)-3,5-bis[(<i>E</i>)-1-(4-methoxyphenyl)methylidene]-1,2,3,5,6,7-hexahydrodicyclopenta[<i>b</i>,<i>e</i>]pyridine
Jonathan D. Crane; John Crompton; Acta Crystallographica Section E 59 (2003) o2003–o2004; doi:10.1107/S1600536803026758

data_2202976
_publ_section_title
8-(4-Methoxyphenyl)-3,5-bis[(<i>E</i>)-1-(4-methoxyphenyl)methylidene]-1,2,3,5,6,7-hexahydrodicyclopenta[<i>b</i>,<i>e</i>]pyridine
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2003
_journal_page_last               o2004
_journal_paper_doi               10.1107/S1600536803026758
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C34 H31 N O3'
_chemical_formula_moiety         'C34 H31 N O3'
_chemical_formula_sum            'C34 H31 N O3'
_chemical_formula_weight         501.60
_chemical_name_systematic
;
8-(4-Methoxyphenyl)-3,5-bis[(E)-1-(4-methoxyphenyl)methylidene]-
1,2,3,5,6,7-hexahydrodicyclopenta[b,e]pyridine
;
_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
_cell_angle_alpha                75.096(9)
_cell_angle_beta                 85.572(10)
_cell_angle_gamma                78.964(10)
_cell_formula_units_Z            2
_cell_length_a                   5.8866(7)
_cell_length_b                   10.8186(12)
_cell_length_c                   20.898(2)
_cell_measurement_reflns_used    13469
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.25
_cell_measurement_theta_min      2.02
_cell_volume                     1261.8(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2001)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  WinGX
_computing_structure_refinement
'WinGX (Farrugia, 1999) and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'X-STEP32 (Stoe & Cie, 2001) and SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe IPDS-II area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_sigmaI/netI    0.1104
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_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            27584
_diffrn_reflns_theta_full        32.25
_diffrn_reflns_theta_max         32.25
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.275
_refine_ls_extinction_coef       0.025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         8874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0619P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                4469
_reflns_number_total             8874
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6199.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2202976
_cod_database_fobs_code          2202976