Synthesis by deamination reaction and crystal structure at 120K of (16<i>Z</i>,19<i>E</i>)-18-oxo-<i>N</i>-(pyridin-2-yl)-6,7,9,10-tetrahydro-18<i>H</i>-dibenzo[<i>h</i>,<i>o</i>][1,4,7]trioxacyclohexadecine-17-carboxamide
Wodajo, Ayalew T.; Tran, Thi Thanh Van; Truong, Hong Hieu; Tskhovrebov, Alexander G.; Le, The Duan; Khrustalev, Victor N.; Le, Tuan Anh; Acta Crystallographica Section E 76 (2020) 1454–1457; doi:10.1107/S2056989020010968

data_2243541
_publ_section_title
;
 Synthesis by deamination reaction and crystal structure at 120K of
 (16<i>Z</i>,19<i>E</i>)-18-oxo-<i>N</i>-(pyridin-2-yl)-6,7,9,10-tetrahydro-18<i>H</i>-dibenzo[<i>h</i>,<i>o</i>][1,4,7]trioxacyclohexadecine-17-carboxamide
;
_journal_coeditor_code           YK2136
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1454
_journal_page_last               1457
_journal_paper_doi               10.1107/S2056989020010968
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C27 H24 N2 O5'
_chemical_formula_moiety         'C27 H24 N2 O5'
_chemical_formula_sum            'C27 H24 N2 O5'
_chemical_formula_weight         456.48
_chemical_name_systematic
(16<i>Z</i>,19<i>E</i>)-18-Oxo-<i>N</i>-(pyridin-2-yl)-6,7,9,10-tetrahydro-18<i>H</i>-dibenzo[<i>h</i>,<i>o</i>][1,4,7]trioxacyclohexadecine-17-carboxamide
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 97.552(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.021(6)
_cell_length_b                   16.519(5)
_cell_length_c                   8.079(3)
_cell_measurement_reflns_used    1174
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.8
_cell_measurement_theta_min      2.5
_cell_volume                     2251.9(13)
_computing_cell_refinement
;
SAINT (Bruker, 2001)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2001)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2015<i>b</i>)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2015<i>b</i>)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.1139
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13715
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.414
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0735P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1689
_reflns_number_gt                2301
_reflns_number_total             4398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yk2136sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243541
_cod_database_fobs_code          2243541
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.995
_shelx_hkl_checksum              80545
_shelx_res_checksum              22801
_shelxl_version_number           2014/6