Synthesis, Structure, and Unusual Reactivity of a Stable 3-(Oxazolidin-2-ylidene)thiophen-2-one.
Aitken, R. Alan; Harper, Andrew D.; Slawin, Alexandra M. Z.; The Journal of organic chemistry 81 (2016) 10527–10531; doi:10.1021/acs.joc.6b01309

data_4037031
_publ_section_title
;
 Synthesis, Structure, and Unusual Reactivity of a Stable
 3-(Oxazolidin-2-ylidene)thiophen-2-one.
;
_journal_issue                   21
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10527
_journal_page_last               10531
_journal_paper_doi               10.1021/acs.joc.6b01309
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C36 H33 N9 O8 S2'
_chemical_formula_sum            'C36 H33 N9 O8 S2'
_chemical_formula_weight         783.83
_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             2016-05-05
_audit_creation_method           'by CrystalStructure 4.2'
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.715(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.8788(9)
_cell_length_b                   17.3089(14)
_cell_length_c                   21.8706(10)
_cell_measurement_reflns_used    6141
_cell_measurement_temperature    125
_cell_measurement_theta_max      73.15
_cell_measurement_theta_min      3.34
_cell_volume                     4059.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus, et al., 2007)'
_diffrn_ambient_temperature      125
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1180
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44778
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         78.036
_diffrn_reflns_theta_min         4.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.694
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.211
_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            colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632.00
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.94
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.303
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8240
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1693
_refine_ls_R_factor_gt           0.1237
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3559
_refine_ls_wR_factor_ref         0.3882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4706
_reflns_number_total             8240
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo6b01309_si_005.cif
_cod_data_source_block           14
_cod_database_code               4037031
_shelx_res_checksum              1239
_shelx_hkl_checksum              32961