Dimethyl 2-[22,24-dimethyl-23-oxo-8,11,14-trioxa-25-azatetracyclo[19.3.1.0^2,7^.0^15,20^]pentacosa-2,4,6,15(20),16,18-hexaen-25-yl]but-2-enedioate
Anh, Le Tuan; Hieu, Truong Hong; Soldatenkov, Anatoly T.; Kolyadina, Nadezhda M.; Khrustalev, Victor N.; Acta Crystallographica Section E 68 (2012) o1588–o1589; doi:10.1107/S1600536812018867

data_2234956
_publ_section_title
;
 Dimethyl
 2-[22,24-dimethyl-23-oxo-8,11,14-trioxa-25-azatetracyclo[19.3.1.0^2,7^.0^15,20^]pentacosa-2,4,6,15(20),16,18-hexaen-25-yl]but-2-enedioate
;
_journal_coeditor_code           CV5289
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1588
_journal_page_last               o1589
_journal_paper_doi               10.1107/S1600536812018867
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C29 H33 N O8'
_chemical_formula_moiety         'C29 H33 N O8'
_chemical_formula_sum            'C29 H33 N O8'
_chemical_formula_weight         523.56
_chemical_name_systematic
;
Dimethyl 2-(22,24-dimethyl-23-oxo-8,11,14-trioxa-25-
azatetracyclo[19.3.1.0^2,7^.0^15,20^]pentacosa-2,4,6,15(20),16,18-
hexaen-25-yl)but-2-enedioate
;
_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                79.0770(10)
_cell_angle_beta                 78.2180(10)
_cell_angle_gamma                69.8000(10)
_cell_formula_units_Z            2
_cell_length_a                   8.8135(4)
_cell_length_b                   8.9469(4)
_cell_length_c                   18.3067(9)
_cell_measurement_reflns_used    7696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.60
_cell_measurement_theta_min      2.29
_cell_volume                     1315.05(11)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17255
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         7669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0585P)^2^+0.545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                6322
_reflns_number_total             7669
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv5289.cif
_cod_data_source_block           I
_cod_database_code               2234956
_cod_database_fobs_code          2234956