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_1545210
_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 O3 S'
_chemical_formula_sum            'C14 H19 N5 O3 S'
_chemical_formula_weight         337.4
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-27T13:46:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.0
_cell_angle_beta                 108.045(5)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   14.5899(6)
_cell_length_b                   10.9383(3)
_cell_length_c                   21.1354(11)
_cell_measurement_reflns_used    6138
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.5297
_cell_measurement_theta_min      3.0017
_cell_volume                     3207.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.9960
_diffrn_measured_fraction_theta_max 0.9697
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21584
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         28.5297
_diffrn_reflns_theta_min         3.0017
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69522
_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    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                5471
_reflns_number_total             7468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b03807_si_003.cif
_cod_data_source_block           php966_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1545210
_cell_oxdiff_length_a            14.5817(5)
_cell_oxdiff_length_b            10.9362(4)
_cell_oxdiff_length_c            21.1423(8)
_cell_oxdiff_angle_alpha         89.966(3)
_cell_oxdiff_angle_beta          107.969(3)
_cell_oxdiff_angle_gamma         90.048(3)
_cell_oxdiff_volume              3207.1(2)
_cell_oxdiff_measurement_reflns_used 6138