One-pot synthesis of (1<i>RS</i>,21<i>SR</i>)-diethyl 2-[23-amino-22-ethoxycarbonyl-8,11,14-trioxa-25-azatetracyclo[19.3.1.0^2,7^.0^15,20^]pentacosa-2,4,6,15(20),16,18,22-heptaen-25-yl]but-2-endioate
Tran, Thi Thanh Van; Le, Tuan Anh; Truong, Hong Hieu; Dao, Thi Nhung; Soldatenkov, Anatoly T.; Khrustalev, Victor N.; Acta Crystallographica Section E 74 (2018) 1281–1284; doi:10.1107/S205698901801160X

data_2243190
_publ_section_title
;
 One-pot synthesis of (1<i>RS</i>,21<i>SR</i>)-diethyl
 2-[23-amino-22-ethoxycarbonyl-8,11,14-trioxa-25-azatetracyclo[19.3.1.0^2,7^.0^15,20^]pentacosa-2,4,6,15(20),16,18,22-heptaen-25-yl]but-2-endioate
;
_journal_coeditor_code           LD2144
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1281
_journal_page_last               1284
_journal_paper_doi               10.1107/S205698901801160X
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C30 H34 N2 O9'
_chemical_formula_moiety         'C30 H34 N2 O9'
_chemical_formula_sum            'C30 H34 N2 O9'
_chemical_formula_weight         566.59
_chemical_name_systematic
;(1<i>RS</i>,21<i>SR</i>)-Diethyl
2-[23-amino-22-ethoxycarbonyl-8,11,14-trioxa-25-azatetracyclo[19.3.1.0^2,7^.0^15,20^]pentacosa-2,4,6,15(20),16,18,22-heptaen-25-yl]but-2-endioate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                89.044(2)
_cell_angle_beta                 86.658(2)
_cell_angle_gamma                82.896(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1172(9)
_cell_length_b                   10.3752(10)
_cell_length_c                   14.7482(14)
_cell_measurement_reflns_used    5654
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.24
_cell_measurement_theta_min      2.40
_cell_volume                     1381.9(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, 2015)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2015)'
_computing_structure_refinement  '<i>SHELXTL</i> (Sheldrick, 2015)'
_computing_structure_solution    '<i>SHELXTL</i> (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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  0.0459
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27765
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.751
_diffrn_reflns_theta_min         1.978
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         10063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0509P)^2^+0.1608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                6502
_reflns_number_total             10063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ld2144sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1382.0(2)
_cod_database_code               2243190
_cod_database_fobs_code          2243190
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.995
_shelx_hkl_checksum              31963
_shelx_res_checksum              85133
_shelxl_version_number           2014/6