1-(4-Chlorophenacyl)-4-methyl-5,6,7,8,9,10-hexahydrocycloocta[<i>b</i>]pyridin-2(1<i>H</i>)-one
Dmitry V. Albov; Victor B. Rybakov; Eugene V. Babaev; Leonid A. Aslanov; Acta Crystallographica Section E 60 (2004) o1219–o1221; doi:10.1107/S1600536804014163

data_2203929
_publ_section_title
1-(4-Chlorophenacyl)-4-methyl-5,6,7,8,9,10-hexahydrocycloocta[<i>b</i>]pyridin-2(1<i>H</i>)-one
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1219
_journal_page_last               o1221
_journal_paper_doi               10.1107/S1600536804014163
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C20 H22 Cl1 N1 O2'
_chemical_formula_moiety         'C20 H22 Cl1 N1 O2'
_chemical_formula_sum            'C20 H22 Cl N O2'
_chemical_formula_weight         343.84
_chemical_melting_point          454
_chemical_name_systematic
;
1-(4-Chlorophenacyl)-4-methyl-5,6,7,8,9,10-hexahydrocycloocta[b]pyridin-
2(1H)-one
;
_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_method           SHELXL-97
_cell_angle_alpha                111.20(4)
_cell_angle_beta                 93.80(4)
_cell_angle_gamma                96.76(3)
_cell_formula_units_Z            2
_cell_length_a                   8.239(3)
_cell_length_b                   9.115(3)
_cell_length_c                   12.420(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      13
_cell_volume                     857.6(9)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4125
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.9596
_exptl_absorpt_correction_T_min  0.9508
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.417
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0608P)^2^+0.1283P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                2645
_reflns_number_total             4125
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6344.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C20 H22 Cl1 N1 O2'
_cod_database_code               2203929