A Bicyclic Cyclopropane Carboxylic Acid Lactone from a Solid–Liquid PTC Reaction
Zsolt Böcskei; Zoltán Hell; Zoltán Finta; László Töke; Kálmán Simon; Acta Crystallographica Section C 54 (1998) 1694–1695; doi:10.1107/S0108270198007951

data_2007834
_publ_section_title
;
 A Bicyclic Cyclopropane Carboxylic Acid Lactone from a Solid--Liquid
 PTC Reaction
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1694
_journal_page_last               1695
_journal_paper_doi               10.1107/S0108270198007951
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C11 H13 Cl3 O4'
_chemical_formula_sum            'C11 H13 Cl3 O4'
_chemical_formula_weight         315.56
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.939(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.291(2)
_cell_length_b                   11.009(2)
_cell_length_c                   20.1850(11)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      59.03
_cell_measurement_theta_min      40.99
_cell_volume                     1394.7(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
1996)
;
_computing_data_reduction
'TEXSAN: PROCESS (Molecular Structure Corporation, 1992)'
_computing_publication_material  'TEXSAN: FINISH'
_computing_structure_refinement  SHELXL93
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       AFC6S
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3044
_diffrn_reflns_theta_max         75.18
_diffrn_reflns_theta_min         4.39
_diffrn_standards_decay_%        3.14
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.004
_exptl_absorpt_correction_T_max  0.406
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   '\y scan (North et al., 1968)'
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.328
_refine_ls_extinction_coef       0.0249(14)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.088
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_obs          0.0587
_refine_ls_shift/esd_max         0.016
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0470P)^2^+2.8628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1896
_refine_ls_wR_factor_obs         0.1399
_reflns_number_observed          1588
_reflns_number_total             2778
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka1266.cif
_cod_data_source_block           hz55
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0470P)^2^+2.8628P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0470P)^2^+2.8628P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_Hall     '-P 2yab'
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2007834