Extreme Oxatriquinanes: Structural Characterization of α-Oxyoxonium Species with Extraordinarily Long Carbon-Oxygen Bonds
Gorkem Gunbas; William L. Sheppard; James C. Fettinger; Marilyn M. Olmstead; Mark Mascal; Journal of the American Chemical Society 135 (2013) 8173–8176; doi:10.1021/ja4032715

data_4119855
_publ_section_title
;
 Extreme Oxatriquinanes: Structural Characterization of \a-Oxyoxonium
 Species with Extraordinarily Long Carbon-Oxygen Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8173
_journal_page_last               8176
_journal_paper_doi               10.1021/ja4032715
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C9 H15 O2, C F3 O3 S'
_chemical_formula_sum            'C10 H15 F3 O5 S'
_chemical_formula_weight         304.28
_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                 107.445(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9055(12)
_cell_length_b                   9.8677(11)
_cell_length_c                   14.8112(17)
_cell_measurement_reflns_used    4499
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      67.8
_cell_measurement_theta_min      32.4
_cell_volume                     1241.7(3)
_computing_cell_refinement       'SAINT (Bruker, 2012''
_computing_data_collection       'Apex2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012''
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART Apex DUO'
_diffrn_measurement_method       '\f and \w'
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4194
_diffrn_reflns_theta_full        68.14
_diffrn_reflns_theta_max         68.14
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    2.865
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0626P)^2^+0.1073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                2230
_reflns_number_total             2275
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja4032715_si_001.cif
_cod_data_source_block           gg08
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4119855