Asymmetry of the "Strongest" OHO Hydrogen Bond, in the Monoanion of (\±)-α,α'-Di-tert-butylsuccinate
Charles L. Perrin; Jonathan S. Lau; Yeong-Joon Kim; Phaneendrasai Karri; Curtis Moore; Arnold L. Rheingold; Journal of the American Chemical Society 132 (2010) 2099–2100; doi:10.1021/ja9104733

data_4101893
_publ_section_title
;
 Asymmetry of the "Strongest" OHO Hydrogen Bond, in the Monoanion of
 (\+-)-\a,\a'-Di-tert-butylsuccinate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2099
_journal_page_last               2100
_journal_paper_doi               10.1021/ja9104733
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C16.5 H23 K2 N1.5 O5.75'
_chemical_formula_weight         412.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.253(8)
_cell_angle_beta                 106.079(8)
_cell_angle_gamma                95.609(8)
_cell_formula_units_Z            4
_cell_length_a                   12.9463(13)
_cell_length_b                   13.1712(14)
_cell_length_c                   14.2459(15)
_cell_measurement_reflns_used    6761
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      65.00
_cell_measurement_theta_min      3.48
_cell_volume                     2249.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15380
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.22
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    3.967
_exptl_absorpt_correction_T_max  0.7420
_exptl_absorpt_correction_T_min  0.3373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.488
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         6976
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0808
_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^)+(0.1493P)^2^+5.2946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2183
_refine_ls_wR_factor_ref         0.2644
_reflns_number_gt                4496
_reflns_number_total             6976
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja9104733_si_002.cif
_cod_data_source_block           per21
_cod_original_formula_sum        'C16.50 H23 K2 N1.50 O5.75'
_cod_database_code               4101893