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_4024853
_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         'C7 H11 F5 O2'
_chemical_formula_sum            'C7 H11 F5 O2'
_chemical_formula_weight         222.16
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.332(3)
_cell_length_b                   20.815(7)
_cell_length_c                   4.4127(14)
_cell_measurement_reflns_used    2687
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.4217
_cell_measurement_theta_min      1.9567
_cell_volume                     857.2(5)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_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_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.952
_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  0.0992
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3946
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.5000
_exptl_crystal_size_mid          0.1200
_exptl_crystal_size_min          0.0100
_refine_diff_density_max         1.723
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.371
_refine_ls_extinction_coef       0.04(4)
_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   1.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         772
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.925
_refine_ls_R_factor_all          0.2049
_refine_ls_R_factor_gt           0.1595
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3786
_refine_ls_wR_factor_ref         0.4403
_reflns_number_gt                625
_reflns_number_total             772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901360e_si_001_1.cif
_cod_data_source_block           3B
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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      Pnma
_cod_database_code               4024853