Synthesis of spirocyclic thiazolidinediones using ring-closing metathesis and one-pot sequential ring-closing/cross metathesis.
Dhara, Kalyan; Paladhi, Sushovan; Midya, Ganesh Chandra; Dash, Jyotirmayee; Organic & biomolecular chemistry 9 (2011) 3801–3807; doi:10.1039/c0ob01248c

data_7151835
_publ_section_title
;
 Synthesis of spirocyclic thiazolidinediones using ring-closing
 metathesis and one-pot sequential ring-closing/cross metathesis.
;
_journal_issue                   10
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3801
_journal_page_last               3807
_journal_paper_doi               10.1039/c0ob01248c
_journal_volume                  9
_journal_year                    2011
_chemical_formula_sum            'C12.67 H12 N O2 S'
_chemical_formula_weight         242.29
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.971(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            3
_cell_length_a                   6.1705(7)
_cell_length_b                   7.7879(8)
_cell_length_c                   18.703(3)
_cell_measurement_temperature    296(2)
_cell_volume                     895.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6657
_diffrn_reflns_theta_full        22.62
_diffrn_reflns_theta_max         22.62
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.258
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             381
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                927
_reflns_number_total             1192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ob01248c.txt
_cod_data_source_block           jd_kd_52l_01
_cod_original_cell_volume        895.38(18)
_cod_database_code               7151835