2-(4-Chlorophenyl)-5-methyl-6,7,8,9,10,11-hexahydrocycloocta[<i>e</i>][1,3]oxazolo[3,2-<i>a</i>]pyridin-12-ium perchlorate
Dmitry V. Albov; Victor B. Rybakov; Eugene V. Babaev; Leonid A. Aslanov; Acta Crystallographica Section E 60 (2004) o1301–o1302; doi:10.1107/S1600536804014345

data_2204063
_publ_section_title
;2-(4-Chlorophenyl)-5-methyl-6,7,8,9,10,11-hexahydrocycloocta[<i>e</i>][1,3]oxazolo[3,2-<i>a</i>]pyridin-12-ium
 perchlorate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1301
_journal_page_last               o1302
_journal_paper_doi               10.1107/S1600536804014345
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C20 H21 Cl N O +, Cl O4-'
_chemical_formula_moiety         'C20 H21 Cl N O +, Cl O4-'
_chemical_formula_sum            'C20 H21 Cl2 N O5'
_chemical_formula_weight         426.28
_chemical_melting_point          584
_chemical_name_systematic
;
2-(4-Chlorophenyl)-5-methyl-6,7,8,9,10,11-
hexahydrocycloocta[e][1,3]oxazolo[3,2-a]pyridin-12-ium perchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.013(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8301(9)
_cell_length_b                   18.6827(19)
_cell_length_c                   13.8840(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34
_cell_measurement_theta_min      30
_cell_volume                     1978.9(4)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w/2\t'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3977
_diffrn_reflns_theta_full        74.90
_diffrn_reflns_theta_max         74.90
_diffrn_reflns_theta_min         4.03
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    3.231
_exptl_absorpt_correction_T_max  0.5502
_exptl_absorpt_correction_T_min  0.4871
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3977
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0584P)^2^], where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                2581
_reflns_number_total             3977
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6346.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C20 H21 Cl2 N1 O5'
_cod_database_code               2204063
_cod_database_fobs_code          2204063