Diastereoselective Synthesis of 2,3,4,5,6-Pentafluoroheptanes
Daniel Farran; Alexandra M. Z. Slawin; Peer Kirsch; David O'Hagan; Journal of Organic Chemistry 74 (2009) 7168–7171; doi:10.1021/jo901360e

data_4024855
_publ_section_title
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Diastereoselective Synthesis of 2,3,4,5,6-Pentafluoroheptanes
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_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7168
_journal_page_last               7171
_journal_paper_doi               10.1021/jo901360e
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C21 H23 F5 O6 S2'
_chemical_formula_sum            'C21 H23 F5 O6 S2'
_chemical_formula_weight         530.51
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.885(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.544(4)
_cell_length_b                   6.009(2)
_cell_length_c                   30.390(9)
_cell_measurement_reflns_used    5102
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.3968
_cell_measurement_theta_min      2.0386
_cell_volume                     2285.4(13)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1300
_diffrn_reflns_av_sigmaI/netI    0.1292
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            13693
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.2100
_exptl_crystal_size_mid          0.0300
_exptl_crystal_size_min          0.0100
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.005(2)
_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   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1948
_refine_ls_R_factor_gt           0.1507
_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^)+(0.1938P)^2^+23.1298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4221
_refine_ls_wR_factor_ref         0.4478
_reflns_number_gt                2501
_reflns_number_total             4140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901360e_si_001_3.cif
_cod_data_source_block           16B
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4024855