Lithium Pinacolone Enolate Solvated by Hexamethylphosphoramide.
Guang, Jie; Liu, Qiyong Peter; Hopson, Russell; Williard, Paul G.; Journal of the American Chemical Society 137 (2015) 7347–7356; doi:10.1021/jacs.5b01906

data_4123646
_publ_section_title
;
 Lithium Pinacolone Enolate Solvated by Hexamethylphosphoramide.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7347
_journal_page_last               7356
_journal_paper_doi               10.1021/jacs.5b01906
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C48 H118 Li6 N12 O10 P4'
_chemical_formula_weight         1189.06
_chemical_name_common            jg04apr13
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.0990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2709(7)
_cell_length_b                   14.4105(7)
_cell_length_c                   20.9053(9)
_cell_measurement_reflns_used    9685
_cell_measurement_temperature    198.(2)
_cell_measurement_theta_max      25.1891
_cell_measurement_theta_min      2.2819
_cell_volume                     3627.5(3)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      198.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24399
_diffrn_reflns_theta_full        25.22
_diffrn_reflns_theta_max         25.22
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.259
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         11789
_refine_ls_number_restraints     419
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          4.746
_refine_ls_shift/su_mean         0.154
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+0.4771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1661
_reflns_number_gt                9308
_reflns_number_total             11789
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b01906_si_005.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4123646--4123648.cif.'
_cod_database_code               4123646