Crystal structure of 8-methyl-8-azabicyclo(3.2.1)octan-3-one, C~8~H~13~NO
Staples, Richard J.; Qi, Yan; Zeitschrift für Kristallographie - New Crystal Structures 222 (2007) 225–226; doi:

data_8102126
_publ_section_title
;
Crystal structure of 8-methyl-8-azabicyclo(3.2.1)octan-3-one, C~8~H~13~NO
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              225
_journal_page_last               226
_journal_volume                  222
_journal_year                    2007
_chemical_compound_source        'Purchased from Aldrich'
_chemical_formula_moiety         'C8 H13 N O'
_chemical_formula_sum            'C8 H13 N O'
_chemical_formula_weight         139.19
_chemical_name_common            tropinone
_chemical_name_systematic
;
8-methyl-8-azabicyclo(3.2.1)octan-3-one
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.887(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.380(3)
_cell_length_b                   7.1365(19)
_cell_length_c                   20.973(6)
_cell_measurement_reflns_used    840
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      3.00
_cell_volume                     1508.2(7)
_computing_cell_refinement       'SMART [5](BRUKER, V5.625, 2001)'
_computing_data_collection       'ASTRO (BRUKER, V5.007, 1997)'
_computing_data_reduction        'SAINT [6](BRUKER, V6.22, 2001)'
_computing_molecular_graphics    'SHELXTL [9](BRUKER, 2000, V6.1)'
_computing_publication_material  'XCIF [9](Sheldrick and BRUKER, 1997, V5.1)'
_computing_structure_refinement  'SHELXL-97 [8](Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 [7](Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'omega, 0.3 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            4636
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_correction_T_min  0.9840
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             608
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0514P)^2^+1.3633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                1552
_reflns_number_total             1772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2009.cff
_cod_data_source_block           class1806
_cod_original_sg_symbol_H-M      C12/c1
_cod_original_formula_sum        'C8 H13 N1 O1'
_cod_database_code               8102126