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_4123647
_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            'C44 H100 Li4 N12 O8 P4'
_chemical_formula_weight         1077.00
_chemical_name_common            jg11mar13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                94.906(6)
_cell_angle_beta                 104.544(6)
_cell_angle_gamma                101.318(7)
_cell_formula_units_Z            2
_cell_length_a                   12.280(2)
_cell_length_b                   12.436(2)
_cell_length_c                   22.118(4)
_cell_measurement_reflns_used    9439
_cell_measurement_temperature    213.(2)
_cell_measurement_theta_max      26.2080
_cell_measurement_theta_min      2.6111
_cell_volume                     3173.4(9)
_computing_cell_refinement       'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37720
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.310
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.522
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         11576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0781
_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^)+(0.1257P)^2^+3.7757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2108
_refine_ls_wR_factor_ref         0.2373
_reflns_number_gt                8148
_reflns_number_total             11576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b01906_si_002.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4123646--4123648.cif.'
_cod_database_code               4123647