Dimethyl 2-[24-acetyl-28-oxo-8,11,14-trioxa-24,27-diazapentacyclo[19.5.1.1^22,26^.0^2,7^.0^15,20^]octacosa-2,4,6,15(20),16,18-hexaen-27-yl]but-2-enedioate
Hieu, Truong Hong; Anh, Le Tuan; Soldatenkov, Anatoly T.; Kolyadina, Nadezhda M.; Khrustalev, Victor N.; Acta Crystallographica Section E 68 (2012) o2431–o2432; doi:10.1107/S1600536812030644

data_2235959
_publ_section_title
;
 Dimethyl
 2-[24-acetyl-28-oxo-8,11,14-trioxa-24,27-diazapentacyclo[19.5.1.1^22,26^.0^2,7^.0^15,20^]octacosa-2,4,6,15(20),16,18-hexaen-27-yl]but-2-enedioate
;
_journal_coeditor_code           RK2370
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2431
_journal_page_last               o2432
_journal_paper_doi               10.1107/S1600536812030644
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C31 H34 N2 O9'
_chemical_formula_moiety         'C31 H34 N2 O9'
_chemical_formula_sum            'C31 H34 N2 O9'
_chemical_formula_weight         578.60
_chemical_melting_point_gt       522
_chemical_melting_point_lt       524
_chemical_name_systematic
;
Dimethyl 2-(24-acetyl-28-oxo-8,11,14-trioxa-24,27-
diazapentacyclo[19.5.1.1^22,26^.0^2,7^.0^15,20^]octacosa-
2,4,6,15(20),16,18-hexaen-27-yl)but-2-enedioate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.6140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6634(6)
_cell_length_b                   26.3883(18)
_cell_length_c                   11.4375(8)
_cell_measurement_reflns_used    6686
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      2.27
_cell_volume                     2875.6(3)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2001)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2005)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2001)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXTL</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36500
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2003)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         8396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0451
_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^)+(0.046P)^2^+1.09P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                6209
_reflns_number_total             8396
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2370.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2235959
_cod_database_fobs_code          2235959