6-Oxo-5-[(trifluoromethyl)sulfonyl]-1,2,4a,5,6,11b-hexahydro-1,3-dioxolo[4,5-<i>j</i>]phenanthridin-2-yl benzoate
Wu, Chunli; Li, Pan; Shi, Xiufang; Pan, Xiaotao; Wu, Jizhou; Acta Crystallographica Section E 67 (2011) o382–; doi:10.1107/S1600536811001085

data_2229307
_publ_section_title
;
 6-Oxo-5-[(trifluoromethyl)sulfonyl]-1,2,4a,5,6,11b-hexahydro-1,3-dioxolo[4,5-<i>j</i>]phenanthridin-2-yl
 benzoate
;
_journal_coeditor_code           ZQ2082
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o382
_journal_paper_doi               10.1107/S1600536811001085
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C22 H16 F3 N O7 S'
_chemical_formula_moiety         'C22 H16 F3 N O7 S'
_chemical_formula_sum            'C22 H16 F3 N O7 S'
_chemical_formula_weight         495.42
_chemical_melting_point_gt       394
_chemical_melting_point_lt       397
_chemical_name_systematic
;
6-Oxo-5-[(trifluoromethyl)sulfonyl]-1,2,4a,5,6,11b-hexahydro-1,3-
dioxolo[4,5-<i>j</i>]phenanthridin-2-yl benzoate
;
_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                114.351(2)
_cell_angle_beta                 95.1450(10)
_cell_angle_gamma                97.0720(10)
_cell_formula_units_Z            2
_cell_length_a                   5.3521(5)
_cell_length_b                   15.5146(16)
_cell_length_c                   15.5615(14)
_cell_measurement_reflns_used    1287
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.47
_cell_volume                     1154.07(19)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5980
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_correction_T_min  0.9125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0699P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1627
_reflns_number_gt                2079
_reflns_number_total             4008
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zq2082.cif
_cod_data_source_block           I
_cod_database_code               2229307
_cod_database_fobs_code          2229307