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 131 (2009) 13548–13554; doi:10.1021/ja905806h

data_4105050
_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              13548
_journal_page_last               13554
_journal_paper_doi               10.1021/ja905806h
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C24 H56 Mg O15'
_chemical_formula_weight         609.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 97.990(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.3954(7)
_cell_length_b                   31.990(3)
_cell_length_c                   16.2225(17)
_cell_measurement_reflns_used    6358
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.09
_cell_measurement_theta_min      23.19
_cell_volume                     3286.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.647
_diffrn_measured_fraction_theta_max 0.742
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7589
_diffrn_reflns_theta_full        55.00
_diffrn_reflns_theta_max         68.08
_diffrn_reflns_theta_min         23.19
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.7365
_exptl_absorpt_correction_T_min  0.6629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         3642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+4.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                3567
_reflns_number_total             3642
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905806h_si_002_4.cif
_cod_data_source_block           "'Magesium_a,a'-di-tert-butylsuccinate'"
_cod_original_cell_volume        3286.8(6)
_cod_database_code               4105050