C5-Morpholinomethylation of N1-sulfonylcytosines by a one-pot microwave assisted Mannich reaction.
Matić, Josipa; Nekola, Irena; Višnjevac, Aleksandar; Kobetić, Renata; Martin-Kleiner, Irena; Kralj, Marijeta; Žinić, Biserka; Organic & biomolecular chemistry 16 (2018) 2678–2687; doi:10.1039/c8ob00253c

data_7156156
_publ_section_title
;
 C5-Morpholinomethylation of N1-sulfonylcytosines by a one-pot microwave
 assisted Mannich reaction.
;
_journal_issue                   15
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2678
_journal_page_last               2687
_journal_paper_doi               10.1039/c8ob00253c
_journal_volume                  16
_journal_year                    2018
_chemical_formula_moiety         'C15 H20 N4 O4 S, 2(H2 O)'
_chemical_formula_sum            'C15 H24 N4 O6 S'
_chemical_formula_weight         388.44
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_date             2017-11-27T14:02:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-12-01 deposited with the CCDC.
2018-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                95.807(4)
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_cell_angle_gamma                98.710(4)
_cell_formula_units_Z            2
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_cell_length_b                   9.2289(4)
_cell_length_c                   15.5715(7)
_cell_measurement_reflns_used    4590
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      75.717
_cell_measurement_theta_min      4.865
_cell_measurement_wavelength     1.54184
_cell_volume                     922.86(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
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_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4323
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_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0797653
_diffrn_orient_matrix_UB_12      -0.141107
_diffrn_orient_matrix_UB_13      -0.0348579
_diffrn_orient_matrix_UB_21      -0.0050029
_diffrn_orient_matrix_UB_22      0.0505765
_diffrn_orient_matrix_UB_23      -0.0913389
_diffrn_orient_matrix_UB_31      0.2248874
_diffrn_orient_matrix_UB_32      0.0802006
_diffrn_orient_matrix_UB_33      0.0206286
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_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
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_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.881
_diffrn_reflns_theta_min         2.866
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
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_exptl_absorpt_correction_T_min  0.87044
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_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
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_refine_ls_number_reflns         3769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0537
_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^)+(0.1092P)^2^+0.1241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0
_reflns_number_gt                3369
_reflns_number_total             3769
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           tscjos
_cod_depositor_comments          'Adding full bibliography for 7156156.cif.'
_cod_database_code               7156156