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_4123648
_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            'C42 H98 Li4 N9 O7 P3'
_chemical_formula_weight         961.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2344(14)
_cell_length_b                   15.0550(19)
_cell_length_c                   32.394(3)
_cell_measurement_temperature    198.(2)
_cell_volume                     5966.6(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      198.(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8208
_diffrn_reflns_theta_full        17.12
_diffrn_reflns_theta_max         17.12
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_process_details
;
;
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2104
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.316
_refine_ls_abs_structure_details
;
Flack x determined using 1234 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         3510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.208
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          2.945
_refine_ls_shift/su_mean         0.118
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.3917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2489
_refine_ls_wR_factor_ref         0.2591
_reflns_number_gt                3188
_reflns_number_total             3510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b01906_si_004.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4123646--4123648.cif.'
_cod_database_code               4123648
_shelx_res_checksum              40792
_shelx_hkl_checksum              90971