Ring-Opening 1,3-Halochalcogenation of Cyclopropane Dicarboxylates.
Wallbaum, Jan; Garve, Lennart K. B.; Jones, Peter G.; Werz, Daniel B.; Organic letters 19 (2017) 98–101; doi:10.1021/acs.orglett.6b03375

data_1544941
_publ_section_title
;
 Ring-Opening 1,3-Halochalcogenation of Cyclopropane Dicarboxylates.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              98
_journal_page_last               101
_journal_paper_doi               10.1021/acs.orglett.6b03375
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C26 H28 Cl2 O8 S2'
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_cell_angle_beta                 105.999(4)
_cell_angle_gamma                96.045(4)
_cell_formula_units_Z            1
_cell_length_a                   7.5065(4)
_cell_length_b                   8.2625(3)
_cell_length_c                   12.1071(5)
_cell_measurement_reflns_used    23893
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      3.8010
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Siemens XP'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0379
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_diffrn_reflns_limit_k_min       -10
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_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29780
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.22
_diffrn_reflns_theta_min         3.81
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.805
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             314
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.194
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_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5481
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.1354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                5410
_reflns_number_total             5481
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b03375_si_001.cif
_cod_data_source_block           lentwi
_cod_depositor_comments          'Adding full bibliography for 1544941.cif.'
_cod_original_cell_volume        715.11(5)
_cod_database_code               1544941