Ethyl 27-oxo-15-oxa-2,20-diazahexacyclo[18.6.1.0^1,8^.0^2,6^.0^9,14^.0^21,26^]heptacosa-9,11,13,21,23,25-hexaene-7-carboxylate
Narayanan, Sibi; Srinivasan, Thothadri; Purushothaman, Santhanagopalan; Raghunathan, Raghavachary; Velmurugan, Devadasan; Acta Crystallographica Section E 69 (2013) o23–o24; doi:10.1107/S1600536812049082

data_2237117
_publ_section_title
;
 Ethyl
 27-oxo-15-oxa-2,20-diazahexacyclo[18.6.1.0^1,8^.0^2,6^.0^9,14^.0^21,26^]heptacosa-9,11,13,21,23,25-hexaene-7-carboxylate
;
_journal_coeditor_code           BT6853
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o23
_journal_page_last               o24
_journal_paper_doi               10.1107/S1600536812049082
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C27 H30 N2 O4'
_chemical_formula_moiety         'C27 H30 N2 O4'
_chemical_formula_sum            'C27 H30 N2 O4'
_chemical_formula_weight         446.53
_chemical_name_systematic
;
Ethyl 27-oxo-15-oxa-2,20-
diazahexacyclo[18.6.1.0^1,8^.0^2,6^.0^9,14^.0^21,26^]heptacosa-
9,11,13,21,23,25-hexaene-7-carboxylate
;
_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                103.988(4)
_cell_angle_beta                 95.023(4)
_cell_angle_gamma                113.775(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9327(5)
_cell_length_b                   10.0068(5)
_cell_length_c                   14.6379(11)
_cell_measurement_reflns_used    5603
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.5
_cell_volume                     1136.41(13)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w and \f 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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20472
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9784
_exptl_absorpt_correction_T_min  0.9742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            'white crystalline'
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5603
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0559P)^2^+0.2150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                4378
_reflns_number_total             5603
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6853.cif
_cod_data_source_block           I
_cod_database_code               2237117
_cod_database_fobs_code          2237117