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_4037081
_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         'C34 H35 N5 O2'
_chemical_formula_sum            'C34 H35 N5 O2'
_chemical_formula_weight         545.67
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-16T20:35:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.439(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4458(2)
_cell_length_b                   10.5223(2)
_cell_length_c                   21.9420(4)
_cell_measurement_reflns_used    9671
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      76.8863
_cell_measurement_theta_min      3.5971
_cell_volume                     2834.59(9)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0976051
_diffrn_orient_matrix_UB_12      0.0919127
_diffrn_orient_matrix_UB_13      0.0078868
_diffrn_orient_matrix_UB_21      0.0482255
_diffrn_orient_matrix_UB_22      -0.0728274
_diffrn_orient_matrix_UB_23      -0.05013
_diffrn_orient_matrix_UB_31      -0.0624033
_diffrn_orient_matrix_UB_32      0.0875685
_diffrn_orient_matrix_UB_33      -0.0499459
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.054
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23246
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.092
_diffrn_reflns_theta_min         3.837
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.048
_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     375
_refine_ls_number_reflns         5959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.044
_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^)+(0.0643P)^2^+0.8585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0
_reflns_number_gt                4914
_reflns_number_total             5959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b01430_si_002.cif
_cod_data_source_block           ea300_2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4037081