Domino reaction of cyclic sulfamidate imines with Morita-Baylis-Hillman acetates promoted by DABCO: a metal-free approach to functionalized nicotinic acid derivatives.
Majee, Debashis; Biswas, Soumen; Mobin, Shaikh M.; Samanta, Sampak; Organic & biomolecular chemistry 15 (2017) 3286–3297; doi:10.1039/c7ob00240h

data_7155543
_publ_section_title
;
 Domino reaction of cyclic sulfamidate imines with Morita-Baylis-Hillman
 acetates promoted by DABCO: a metal-free approach to functionalized
 nicotinic acid derivatives.
;
_journal_issue                   15
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3286
_journal_page_last               3297
_journal_paper_doi               10.1039/c7ob00240h
_journal_volume                  15
_journal_year                    2017
_chemical_formula_sum            'C20 H16 N2 O4'
_chemical_formula_weight         348.35
_space_group_crystal_system      triclinic
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
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_audit_update_record
;
2016-12-10 deposited with the CCDC.
2017-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                105.058(4)
_cell_angle_beta                 98.466(3)
_cell_angle_gamma                99.563(3)
_cell_formula_units_Z            2
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_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.4070
_cell_measurement_theta_min      3.5320
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_computing_molecular_graphics    Ortep3
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
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_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_number            10763
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.231
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_exptl_absorpt_coefficient_mu    0.095
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_exptl_absorpt_correction_T_min  0.77304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
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_refine_diff_density_rms         0.044
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+0.2823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3537
_reflns_number_total             5548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ob00240h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7155543.cif.'
_cod_original_cell_volume        862.59(6)
_cod_database_code               7155543
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              60634
_shelx_hkl_checksum              91465