Novel spirocyclic systems via multicomponent aza-Diels–Alder reaction
Llona-Minguez, Sabin; Throup, Adam; Steiner, Emilie; Lightowler, Molly; Van der Haegen, Sandra; Homan, Evert; Eriksson, Lars; Stenmark, Pål; Jenmalm-Jensen, Annika; Helleday, Thomas; Org. Biomol. Chem.  (2017) –; doi:10.1039/C7OB02069D

data_7155873
_publ_section_title
;
 Novel spirocyclic systems via multicomponent aza-Diels--Alder reaction
;
_journal_name_full               'Org. Biomol. Chem.'
_journal_paper_doi               10.1039/C7OB02069D
_journal_year                    2017
_chemical_formula_moiety         'C17 H26 N2 O5 S'
_chemical_formula_sum            'C17 H26 N2 O5 S'
_chemical_formula_weight         370.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'CCDC enCIFer and SHELXL-2014/7'
_audit_update_record
;
2017-09-05 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.692(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5689(12)
_cell_length_b                   10.3588(6)
_cell_length_c                   11.1945(7)
_cell_measurement_reflns_used    7079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.12
_cell_measurement_theta_min      2.68
_cell_volume                     1803.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'Apex3 (Bruker,2016)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  Encifer(CCDC)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.10
_diffrn_measured_fraction_theta_full 0.829
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_device_type  'Bruker D8 Advance'
_diffrn_measurement_method       '\w scans at different \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1587
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 0.829
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            53810
_diffrn_reflns_point_group_measured_fraction_full 0.829
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.680
_diffrn_source                   '1myS, Incotec'
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colour_less
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.99
_exptl_transmission_factor_min   0.96
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0012(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0393P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1572
_reflns_number_total             2837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ob02069d2.cif
_cod_data_source_block           r_756007
_cod_database_code               7155873
_shelx_res_checksum              91817