2,17-Dichloro-8,9,10,11-tetrahydro-19<i>H</i>-dibenzo[<i>k</i>,<i>n</i>][1,10,4,7]dioxadiazacyclopentadecine-7,12(6<i>H</i>,13<i>H</i>)-dione
Pojarová, Michaela; Dušek, Michal; Sedláková, Zdeňka; Makrlík, Emanuel; Acta Crystallographica Section E 68 (2012) o1698–o1699; doi:10.1107/S1600536812020351

data_2234896
_publ_section_title
;
 2,17-Dichloro-8,9,10,11-tetrahydro-19<i>H</i>-dibenzo[<i>k</i>,<i>n</i>][1,10,4,7]dioxadiazacyclopentadecine-7,12(6<i>H</i>,13<i>H</i>)-dione
;
_journal_coeditor_code           AA2058
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1698
_journal_page_last               o1699
_journal_paper_doi               10.1107/S1600536812020351
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C19 H18 Cl2 N2 O4'
_chemical_formula_moiety         'C19 H18 Cl2 N2 O4'
_chemical_formula_sum            'C19 H18 Cl2 N2 O4'
_chemical_formula_weight         409.25
_chemical_name_systematic
;
2,17-Dichloro-8,9,10,11-tetrahydro-19<i>H</i>-
dibenzo[<i>k</i>,<i>n</i>][1,10,4,7]dioxadiazacyclopentadecine-
7,12(6<i>H</i>,13<i>H</i>)-dione
;
_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                90.0
_cell_angle_beta                 93.588(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   12.0877(3)
_cell_length_b                   8.73462(15)
_cell_length_c                   17.3712(4)
_cell_measurement_reflns_used    16650
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      67.0527
_cell_measurement_theta_min      3.6607
_cell_volume                     1830.48(7)
_computing_cell_refinement       'Crysalis PRO (Agilent, 2010)'
_computing_data_collection       'Crysalis PRO (Agilent, 2010)'
_computing_data_reduction        'Crysalis PRO (Agilent, 2010)'
_computing_molecular_graphics
'Mercury (Macrae <i>et al.</i>, 2006) and ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Agilent Xcalibur Atlas Gemini ultra'
_diffrn_measurement_method
;
Rotation method data acquisition using \w
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19596
_diffrn_reflns_theta_full        67.14
_diffrn_reflns_theta_max         67.14
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    3.443
_exptl_absorpt_correction_T_max  0.342
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.3135
_exptl_crystal_size_mid          0.2206
_exptl_crystal_size_min          0.2086
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3271
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0376P)^2^+0.7612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                3210
_reflns_number_total             3271
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            aa2058.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2234896