Lithium, sodium and potassium enolate aggregates and monomers: syntheses and structures.
Davison, Nathan; Hemingway, Jack M.; Waddell, Paul G.; Lu, Erli; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4719–4728; doi:10.1039/d4dt00211c

data_7715143
_publ_section_title
;
 Lithium, sodium and potassium enolate aggregates and monomers: syntheses
 and structures.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4719
_journal_page_last               4728
_journal_paper_doi               10.1039/d4dt00211c
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C96 H66 Li6 O6, 2(C6 H6)'
_chemical_formula_sum            'C108 H78 Li6 O6'
_chemical_formula_weight         1513.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-24
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-11-11 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.189(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4816(5)
_cell_length_b                   16.7761(4)
_cell_length_c                   25.2397(6)
_cell_measurement_reflns_used    16644
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      75.8970
_cell_measurement_theta_min      3.4760
_cell_volume                     8200.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -79.00 -74.00   0.50    1.00    --  -99.00  70.00   0.00   10
  2  \w    -79.00 -74.00   0.50    1.00    --  -99.00  70.00  90.00   10
  3  \w    -29.00 -24.00   0.50    0.25    --  -49.63  70.00  90.00   10
  4  \w      0.00   5.00   0.50    0.25    --  -49.63  60.00   0.00   10
  5  \w     28.00  33.00   0.50    0.25    --   48.88 -70.00  90.00   10
  6  \w     74.00  79.00   0.50    1.00    --  102.18 -70.00  90.00   10
  7  \w     36.00 120.00   0.50    0.25    --   48.76  72.00   7.00  168
  8  \w    -16.00  30.00   0.50    0.25    --   48.76 -72.00-122.00   92
  9  \w    -95.00 -29.00   0.50    0.25    --  -49.76 -72.00-122.00  132
 10  \w    -87.00 -31.00   0.50    1.00    --  -92.01  72.00   7.00  112
 11  \w   -162.00 -71.00   0.50    1.00    --  -92.01 -72.00-122.00  182
 12  \w     38.00  91.00   0.50    1.00    --  108.00 -72.00-122.00  106
 13  \w    -30.00  26.00   0.50    0.25    --   48.76 -19.00  30.00  112
 14  \w    -19.00   7.00   0.50    0.25    --  -49.76  19.00   0.00   52
 15  \w   -122.00 -77.00   0.50    0.25    --  -49.76-125.00 -30.00   90
 16  \w   -100.00 -73.00   0.50    1.00    --  -92.01 -61.00 -90.00   54
 17  \w    -45.00 -14.00   0.50    1.00    --  -92.01  45.00-180.00   62
 18  \w   -149.00 -67.00   0.50    1.00    --  -92.01 -77.00 120.00  164
 19  \w   -144.00-117.00   0.50    1.00    --  -92.01 -61.00 -90.00   54
 20  \w    -48.00 -16.00   0.50    1.00    --  -92.01  45.00-150.00   64
 21  \w   -108.00 -19.00   0.50    1.00    --  -92.01 125.00   0.00  178
 22  \w    -63.00 -20.00   0.50    1.00    --  -92.01  61.00-150.00   86
 23  \w   -169.00 -72.00   0.50    1.00    --  -92.01 -30.00 -60.00  194
 24  \w     20.00  51.00   0.50    1.00    --   96.11 -45.00 -90.00   62
 25  \w    143.00 169.00   0.50    1.00    --   96.11  61.00 -90.00   52
 26  \w     79.00 108.00   0.50    1.00    --   96.11  61.00 -90.00   58
 27  \w     18.00  43.00   0.50    1.00    --   96.11 -45.00 150.00   50
 28  \w     18.00  50.00   0.50    1.00    --   96.11 -45.00-120.00   64
 29  \w     20.00  46.00   0.50    1.00    --   96.11 -45.00 -30.00   52
 30  \w     18.00  46.00   0.50    1.00    --   96.11 -45.00  60.00   56
 31  \w     44.00  86.00   0.50    1.00    --  108.00 -95.00 150.00   84
 32  \w     43.00  68.00   0.50    1.00    --  108.00 -61.00   0.00   50
 33  \w     94.00 120.00   0.50    1.00    --  108.00  30.00-120.00   52
 34  \w     81.00 106.00   0.50    1.00    --  108.00 -95.00  60.00   50
 35  \w     81.00 106.00   0.50    1.00    --  108.00-125.00  30.00   50
 36  \w     40.00  68.00   0.50    1.00    --  108.00 -61.00  60.00   56
 37  \w    104.00 178.00   0.50    1.00    --  108.00  30.00 -60.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0665574000
_diffrn_orient_matrix_UB_12      0.0112983000
_diffrn_orient_matrix_UB_13      0.0272083000
_diffrn_orient_matrix_UB_21      -0.0247546000
_diffrn_orient_matrix_UB_22      0.0642777000
_diffrn_orient_matrix_UB_23      -0.0413475000
_diffrn_orient_matrix_UB_31      -0.0362272000
_diffrn_orient_matrix_UB_32      -0.0647123000
_diffrn_orient_matrix_UB_33      -0.0364502000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40731
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.428
_diffrn_reflns_theta_min         3.485
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 4343 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.63(9)
_refine_ls_extinction_coef       0.00013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         13627
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+1.2194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.654
_reflns_Friedel_fraction_full    0.706
_reflns_Friedel_fraction_max     0.611
_reflns_number_gt                12135
_reflns_number_total             13627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00211c2.cif
_cod_data_source_block           elu230003_fa
_cod_depositor_comments
'Adding full bibliography for 7715143--7715147.cif.'
_cod_database_code               7715143
_chemical_oxdiff_formula         'C20 H23 Li1 O1 Si1'
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.946
_diffrn_oxdiff_digest_frames
;
015429ca097e09fc68f415757de160701b02846a019
;
_diffrn_oxdiff_digest_hkl
;
01c2956ca57681825ae387a1bac42fff260291
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C28(H28), C29(H29),
  C30(H30), C31(H31), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
 C44(H44), C45(H45), C46(H46), C47(H47), C53(H53), C54(H54), C55(H55), C56(H56),
  C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C69(H69), C70(H70),
 C71(H71), C72(H72), C74(H74), C76(H76), C77(H77), C78(H78), C79(H79), C85(H85),
  C86(H86), C87(H87), C88(H88), C90(H90), C92(H92), C93(H93), C94(H94),
 C95(H95), C97(H97), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C106(H106), C107(H107), C108(H108)
2.b X=CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C34(H34A,H34B), C50(H50A,H50B), C66(H66A,H66B),
 C82(H82A,H82B)
;
_shelx_res_checksum              4559
_shelx_shelxl_version_number     2019/1
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.286
_oxdiff_exptl_absorpt_empirical_full_min 0.658