Conformational Polymorphism of Lithium Pinacolone Enolate.
Guang, Jie; Liu, Qiyong; Hopson, Russell; Kagan, Gerald; Li, Weibin; Monroe, Thomas B.; Williard, Paul G.; Journal of the American Chemical Society 138 (2016) 15177–15188; doi:10.1021/jacs.6b08177

data_4130967
_publ_section_title
;
 Conformational Polymorphism of Lithium Pinacolone Enolate.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15177
_journal_page_last               15188
_journal_paper_doi               10.1021/jacs.6b08177
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C18 H33 Li3 O3'
_chemical_formula_sum            'C18 H33 Li3 O3'
_chemical_formula_weight         318.28
_chemical_name_systematic        'Pinacolone enolate'
_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_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                102.936(3)
_cell_angle_beta                 115.200(3)
_cell_angle_gamma                99.243(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3259(14)
_cell_length_b                   10.7672(14)
_cell_length_c                   10.8895(15)
_cell_measurement_reflns_used    9008
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      20.76
_cell_measurement_theta_min      2.19
_cell_volume                     1021.7(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      198.21
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13239
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         20.76
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.6663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1274 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.8950.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.0345
_exptl_crystal_description       block
_exptl_crystal_F_000             348.1556
_exptl_crystal_recrystallization_method 'crystallization at -20 C'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.3780
_refine_diff_density_min         -0.2104
_refine_diff_density_rms         0.0421
_refine_ls_d_res_high            1.0025
_refine_ls_d_res_low             10.0423
_refine_ls_goodness_of_fit_ref   1.0574
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    45
_refine_ls_number_parameters     225
_refine_ls_number_reflns         2121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0574
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.9454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                1830
_reflns_number_total             2121
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja6b08177_si_002.cif
_cod_data_source_block           jg14may13_0m_a
_cod_database_code               4130967
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a X=CH2 refined with fixed occupancy and ADP/Uiso:
 C1(H1a,H1b), C7(H7a,H7b), C13(H13a,H13b)
2.b Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C10(H10a,H10b,H10c),
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C16(H16a,H16b,H16c), C17(H17a,H17b,
 H17c), C18(H18a,H18b,H18c)
;
_olex2_submission_original_sample_id jg14may13
_olex2_submission_special_instructions 'No special instructions were received'