Two Cycles with One Catch: Hydrazine in Ugi 4-CR and Its Postcyclizations.
Wang, Yuanze; Patil, Pravin; Kurpiewska, Katarzyna; Kalinowska-Tluscik, Justyna; Dömling, Alexander; ACS combinatorial science 19 (2017) 193–198; doi:10.1021/acscombsci.7b00009

data_4514032
_publ_section_title
;
 Two Cycles with One Catch: Hydrazine in Ugi 4-CR and Its
 Postcyclizations.
;
_journal_issue                   3
_journal_name_full               'ACS combinatorial science'
_journal_page_first              193
_journal_page_last               198
_journal_paper_doi               10.1021/acscombsci.7b00009
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C26 H32 N12 O2'
_chemical_formula_sum            'C26 H32 N12 O2'
_chemical_formula_weight         544.63
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
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_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-09-20T16:36:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.397(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3819(6)
_cell_length_b                   8.1017(3)
_cell_length_c                   23.2784(9)
_cell_measurement_reflns_used    5840
_cell_measurement_temperature    130(2)
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_cell_measurement_theta_min      3.868
_cell_volume                     2711.54(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0431976
_diffrn_orient_matrix_UB_12      -0.0412497
_diffrn_orient_matrix_UB_13      0.0024618
_diffrn_orient_matrix_UB_21      -0.0065612
_diffrn_orient_matrix_UB_22      0.0386267
_diffrn_orient_matrix_UB_23      0.0269698
_diffrn_orient_matrix_UB_31      -0.022832
_diffrn_orient_matrix_UB_32      0.0668999
_diffrn_orient_matrix_UB_33      -0.0140113
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11596
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.528
_diffrn_reflns_theta_min         2.886
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0118(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.045
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+1.8193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0
_reflns_number_gt                2718
_reflns_number_total             3188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            co7b00009_si_004.cif
_cod_data_source_block           yz118_1
_cod_depositor_comments
'Adding full bibliography for 4514032--4514036.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4514032
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.973