7β-Chloro-6,14-<i>endo</i>-etheno-6,7,8,14-tetrahydrothebaine
Parrish, Damon; Chen, Weibin; Coop, Andrew; Deschamps, Jeffrey R.; Acta Crystallographica Section E 60 (2004) o793–o794; doi:10.1107/S1600536804008670

data_2203623
_publ_section_title
;
 7\b-Chloro-6,14-<i>endo</i>-etheno-6,7,8,14-tetrahydrothebaine
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o793
_journal_page_last               o794
_journal_paper_doi               10.1107/S1600536804008670
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C21 H24 Cl N O3'
_chemical_formula_moiety         'C21 H24 Cl N O3'
_chemical_formula_sum            'C21 H24 Cl N O3'
_chemical_formula_weight         373.86
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.7262(4)
_cell_length_b                   19.8316(10)
_cell_length_c                   23.6182(13)
_cell_measurement_reflns_used    7584
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.68
_cell_volume                     3618.8(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction
;
SAINT (Bruker, 2000) and XPREP (Bruker, 1997)
;
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_sigmaI/netI    0.1079
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29542
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  variable
_diffrn_standards_number         598
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.275
_refine_ls_abs_structure_details 'Flack (1983), 3864 Friedels'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         8828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0274P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                5974
_reflns_number_total             8828
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6200.cif
_cod_data_source_block           3
_cod_database_code               2203623
_cod_database_fobs_code          2203623