6a-Methyl-2,3,3-trioxo-octahydro-1-oxa-3lamda*6*-thia-cyclopenta[cd]pentalene- 6b-carboxylic acid ethyl ester
Gelbrich, Thomas; Lucas, Matthew; Hursthouse, Michael B.; Harrowven, David C.; Crystal Structure Report Archive  (2000) 533–; doi:

data_1519269
_publ_section_title
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 6a-Methyl-2,3,3-trioxo-octahydro-1-oxa-3lamda*6*-thia-cyclopenta[cd]pentalene-
 6b-carboxylic acid ethyl ester
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_journal_name_full               'Crystal Structure Report Archive'
_journal_page_first              533
_journal_year                    2000
_chemical_formula_sum            'C12 H16 O6 S'
_chemical_formula_weight         288.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.078(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9623(4)
_cell_length_b                   10.1397(4)
_cell_length_c                   11.9175(5)
_cell_measurement_reflns_used    6502
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.97
_cell_measurement_theta_min      2.91
_cell_volume                     1323.81(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7489
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  0.9839
_exptl_absorpt_correction_T_min  0.9564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0109(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.8020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                2051
_reflns_number_total             2572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            eCrystal-533.cif
_cod_data_source_block           s92
_cod_depositor_comments
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Citation :
Gelbrich, Thomas and Lucas, Matthew and Hursthouse, Michael B. and 
Harrowven, David C (2000) 
University of Southampton, Crystal Structure Report Archive. 
(doi:10.5258/ecrystals/533)

More at:
http://ecrystals.chem.soton.ac.uk/533/
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_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1519269