10,16-Dichloro-6,20-dioxa-3,23-diazatetracyclo[23.3.1.0^7,12^.0^14,19^]nonacosa-1(29),7,9,11,14(19),15,17,25,27-nonaene-4,22-dione methanol monosolvate
Pojarová, Michaela; Dušek, Michal; Sedláková, Zdeňka; Makrlík, Emanuel; Acta Crystallographica Section E 68 (2012) o805–o806; doi:10.1107/S1600536812007052

data_2233819
_publ_section_title
;
 10,16-Dichloro-6,20-dioxa-3,23-diazatetracyclo[23.3.1.0^7,12^.0^14,19^]nonacosa-1(29),7,9,11,14(19),15,17,25,27-nonaene-4,22-dione
 methanol monosolvate
;
_journal_coeditor_code           GK2457
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o805
_journal_page_last               o806
_journal_paper_doi               10.1107/S1600536812007052
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C25 H22 Cl2 N2 O4, C H4 O'
_chemical_formula_moiety         'C25 H22 Cl2 N2 O4, C H4 O'
_chemical_formula_sum            'C26 H26 Cl2 N2 O5'
_chemical_formula_weight         517.39
_chemical_melting_point_gt       316
_chemical_melting_point_lt       318
_chemical_name_systematic
;
10,16-Dichloro-6,20-dioxa-3,23-
diazatetracyclo[23.3.1.0^7,12^.0^14,19^]nonacosa-
1(29),7,9,11,14(19),15,17,25,27-nonaene-4,22-dione
methanol monosolvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   21.9905(3)
_cell_length_b                   8.18640(10)
_cell_length_c                   26.6760(3)
_cell_measurement_reflns_used    6415
_cell_measurement_temperature    119.9
_cell_measurement_theta_max      67.06
_cell_measurement_theta_min      3.31
_cell_volume                     4802.29(10)
_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      119.9
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur A Gemini Ultra
;
_diffrn_measurement_method       '\w scan'
_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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42959
_diffrn_reflns_theta_full        65.08
_diffrn_reflns_theta_max         65.08
_diffrn_reflns_theta_min         3.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.782
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4099
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+2.1383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                3364
_reflns_number_total             4099
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gk2457.cif
_cod_data_source_block           I
_cod_database_code               2233819
_cod_database_fobs_code          2233819