De Novo Assembly of Highly Substituted Morpholines and Piperazines.
Patil, Pravin; Madhavachary, Rudrakshula; Kurpiewska, Katarzyna; Kalinowska-Tłuścik, Justyna; Dömling, Alexander; Organic letters 19 (2017) 642–645; doi:10.1021/acs.orglett.6b03807

data_1545211
_publ_section_title
;
 De Novo Assembly of Highly Substituted Morpholines and Piperazines.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              642
_journal_page_last               645
_journal_paper_doi               10.1021/acs.orglett.6b03807
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C14 H19 N5 O'
_chemical_formula_sum            'C14 H19 N5 O'
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
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_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-06-01T13:06:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.698(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5604(3)
_cell_length_b                   7.8775(2)
_cell_length_c                   15.7761(5)
_cell_measurement_reflns_used    11957
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_cell_measurement_theta_max      29.293
_cell_measurement_theta_min      2.8851
_cell_volume                     1435.09(7)
_computing_cell_refinement
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
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_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
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_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130.0(1)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0464528
_diffrn_orient_matrix_UB_12      -0.0559874
_diffrn_orient_matrix_UB_13      -0.0077337
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_diffrn_orient_matrix_UB_32      -0.0705402
_diffrn_orient_matrix_UB_33      0.0077938
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_k_max       10
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_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         29.358
_diffrn_reflns_theta_min         2.891
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.82553
_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    1.265
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
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_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0543P)^2^+0.6545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0
_reflns_number_gt                3325
_reflns_number_total             3648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b03807_si_004.cif
_cod_data_source_block           mcr159_1
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               1545211
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.967