Ethyl 23-benzyl-8,11,14-trioxa-23,28,29-triazapentacyclo[19.7.1.0^2,7^.0^15,20^.0^22,27^]nonacosa-2,4,6,15(20),16,18,21,26-octaene-26-carboxylate
Hieu, Truong Hong; Anh, Le Tuan; Soldatenkov, Anatoly T.; Vasil'ev, Vasily G.; Khrustalev, Victor N.; Acta Crystallographica Section E 69 (2013) o565–o566; doi:10.1107/S1600536813007241

data_2237607
_publ_section_title
;
 Ethyl
 23-benzyl-8,11,14-trioxa-23,28,29-triazapentacyclo[19.7.1.0^2,7^.0^15,20^.0^22,27^]nonacosa-2,4,6,15(20),16,18,21,26-octaene-26-carboxylate
;
_journal_coeditor_code           CV5393
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o565
_journal_page_last               o566
_journal_paper_doi               10.1107/S1600536813007241
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C33 H35 N3 O5'
_chemical_formula_moiety         'C33 H35 N3 O5'
_chemical_formula_sum            'C33 H35 N3 O5'
_chemical_formula_weight         553.64
_chemical_name_systematic
'Ethyl 23-benzyl-8,11,14-trioxa-23,28,29-triazapentacyclo[19.7.1.0^2,7^.0^15,20^.0^22,27^]nonacosa-2,4,6,15(20),16,18,21,26-octaene-26-carboxylate'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.8650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5304(5)
_cell_length_b                   12.6363(5)
_cell_length_c                   10.7246(5)
_cell_measurement_reflns_used    5715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.76
_cell_measurement_theta_min      2.49
_cell_volume                     1425.29(11)
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18837
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         8289
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0431P)^2^+0.123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                6878
_reflns_number_total             8289
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv5393.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2237607
_cod_database_fobs_code          2237607