Artificial Macrocycles by Ugi Reaction and Passerini Ring Closure.
Abdelraheem, Eman M. M.; Kurpiewska, Katarzyna; Kalinowska-Tłuścik, Justyna; Dömling, Alexander; The Journal of organic chemistry 81 (2016) 8789–8795; doi:10.1021/acs.joc.6b01430

data_4037082
_publ_section_title
;
 Artificial Macrocycles by Ugi Reaction and Passerini Ring Closure.
;
_journal_issue                   19
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8789
_journal_page_last               8795
_journal_paper_doi               10.1021/acs.joc.6b01430
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C22 H30 N6 O4'
_chemical_formula_sum            'C22 H30 N6 O4'
_chemical_formula_weight         442.52
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
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_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
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_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-16T20:46:49-00:00
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_cell_angle_alpha                90
_cell_angle_beta                 90
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_cell_formula_units_Z            8
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_cell_length_b                   9.4461(2)
_cell_length_c                   37.9520(9)
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_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.1231
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_cell_volume                     4517.62(16)
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        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
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        CrysAlisPro, Agilent Technologies,
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        (compiled Jul 11 2012,15:38:31)
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_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0151467
_diffrn_orient_matrix_UB_12      0.035576
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_diffrn_orient_matrix_UB_22      0.0137691
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_diffrn_orient_matrix_UB_31      0.0138308
_diffrn_orient_matrix_UB_32      -0.1586115
_diffrn_orient_matrix_UB_33      -0.0082948
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0545
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_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
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_diffrn_reflns_number            29925
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.263
_diffrn_reflns_theta_min         4.211
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.67337
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_exptl_absorpt_process_details
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
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        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       prism
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_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0433
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_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+1.6922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0
_reflns_number_gt                3792
_reflns_number_total             4341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b01430_si_003.cif
_cod_data_source_block           exp_3290
_cod_database_code               4037082
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.806