(2<i>E</i>,4<i>E</i>)-8-Methyl-2,4-bis(3-thienylmethylene)-8-azabicyclo[3.2.1]octan-3-one
Sonar, Vijayakumar N.; Parkin, Sean; Crooks, Peter A.; Acta Crystallographica Section E 61 (2005) o3445–o3446; doi:10.1107/S160053680503028X

data_2206839
_publ_section_title
(2<i>E</i>,4<i>E</i>)-8-Methyl-2,4-bis(3-thienylmethylene)-8-azabicyclo[3.2.1]octan-3-one
_journal_coeditor_code           AC6202
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3445
_journal_page_last               o3446
_journal_paper_doi               10.1107/S160053680503028X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C18 H17 N O S2'
_chemical_formula_moiety         'C18 H17 N O S2'
_chemical_formula_sum            'C18 H17 N O S2'
_chemical_formula_weight         327.45
_chemical_name_systematic
(2E,4E)-8-Methyl-2,4-bis-thiophen-3-ylmethylene-8-azabicyclo[3.2.1]octan-3-one
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3783(4)
_cell_length_b                   10.5680(6)
_cell_length_c                   7.3257(3)
_cell_measurement_reflns_used    994
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1500.23(11)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1995)'
_computing_publication_material  'SHELXL97 and local procedures'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1668
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.9164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(SCALEPACK, Version 0.95.373; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.196
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs'
_refine_ls_abs_structure_Flack   0.47(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         1668
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0376P)^2^+0.3768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                1551
_reflns_number_total             1668
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ac6202.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'C 2c -2 '
_cod_database_code               2206839
_cod_database_fobs_code          2206839