Crystal structure of 22,24,25-trimethyl-8,11,14-trioxa-25-azatetracyclo[19.3.1.0^2,7^.0^15,20^]pentacosa-2,4,6,15(20),16,18-hexaen-23-one
Nguyen, Van Tuyen; Truong, Hong Hieu; Le, Tuan Anh; Soldatenkov, Anatoly T.; Thi, Tuyet Anh Dang; Tran, Thi Thanh Van; Esina, Natalia Ya.; Khrustalev, Victor N.; Acta Crystallographica Section E 73 (2017) 118–121; doi:10.1107/S2056989016020508

data_2241999
_publ_section_title
;
 Crystal structure of
 22,24,25-trimethyl-8,11,14-trioxa-25-azatetracyclo[19.3.1.0^2,7^.0^15,20^]pentacosa-2,4,6,15(20),16,18-hexaen-23-one
;
_journal_coeditor_code           XU5896
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              118
_journal_page_last               121
_journal_paper_doi               10.1107/S2056989016020508
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C24 H29 N O4'
_chemical_formula_moiety         'C24 H29 N O4'
_chemical_formula_sum            'C24 H29 N O4'
_chemical_formula_weight         395.48
_chemical_name_systematic
22,24,25-Trimethyl-8,11,14-trioxa-25-azatetracyclo[19.3.1.0^2,7^.0^15,20^]pentacosa-2,4,6,15(20),16,18-hexaen-23-one
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           '<i>SHELXTL</i> (Sheldrick, 2015)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1468(5)
_cell_length_b                   20.3402(11)
_cell_length_c                   12.0155(7)
_cell_measurement_reflns_used    4090
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      3.02
_cell_volume                     1991.1(2)
_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>SHELXL2015</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0653
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25079
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.562
_diffrn_reflns_theta_min         1.969
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0561
_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^)+(0.046P)^2^+1.66P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1298
_reflns_number_gt                2469
_reflns_number_total             3128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xu5896sup1.cif
_cod_data_source_block           I
_cod_database_code               2241999
_cod_database_fobs_code          2241999
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.987
_shelx_hkl_checksum              93933
_shelx_res_checksum              45681
_shelxl_version_number           2014/6