1,3-Thiazolidine derivatives from regioselective [2+3]-cycloadditions of azomethine ylides with thioketones
Domagała, Małgorzata; Linden, Anthony; Olszak, Tomasz A.; Mlostoń, Grzegorz; Heimgartner, Heinz; Acta Crystallographica Section C 59 (2003) o250–o253; doi:10.1107/S0108270103006504

data_2013294
_publ_section_title
;
 1,3-Thiazolidine derivatives from regioselective [2+3]-cycloadditions
 of azomethine ylides with thioketones
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o250
_journal_page_last               o253
_journal_paper_doi               10.1107/S0108270103006504
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C31 H25 N O4 S'
_chemical_formula_moiety         'C31 H25 N O4 S'
_chemical_formula_sum            'C31 H25 N O4 S'
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_chemical_melting_point          476.0(10)
_chemical_name_systematic
;
dimethyl
(4RS)-3,4-diphenyl-1,3-thiazolidine-5-spiro-9'-[9H]fluorene-2,2-dicarboxylate
;
_space_group_IT_number           2
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_atom_sites_solution_primary     direct
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_cell_angle_beta                 97.910(10)
_cell_angle_gamma                98.520(10)
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_cell_length_b                   11.233(2)
_cell_length_c                   12.459(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.25
_cell_measurement_theta_min      20.04
_cell_volume                     1305.7(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1989)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1989)'
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_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
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_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Rigaku AFC-5S'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0166
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_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18942
_diffrn_reflns_theta_full        32.58
_diffrn_reflns_theta_max         32.58
_diffrn_reflns_theta_min         3.40
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.9366
_exptl_absorpt_correction_T_min  0.8971
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(de Meulenaer & Tompa, 1965)'
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_refine_diff_density_min         -0.243
_refine_ls_extinction_coef       0.045(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         9471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0687P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                6330
_reflns_number_total             9471
_reflns_threshold_expression     I>2\s(I)
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_cod_database_code               2013294
_cod_database_fobs_code          2013294