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_7715145
_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_formula_moiety         '0.167(C108 H78 Na6 O6), 0.667(C6 H6)'
_chemical_formula_sum            'C22 H17 Na O'
_chemical_formula_weight         320.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-21
_audit_creation_method
;
Olex2 1.5-ac5-023
(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                81.860(2)
_cell_angle_beta                 85.940(2)
_cell_angle_gamma                63.004(2)
_cell_formula_units_Z            6
_cell_length_a                   12.3035(3)
_cell_length_b                   13.3928(3)
_cell_length_c                   17.4184(4)
_cell_measurement_reflns_used    18519
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      77.8470
_cell_measurement_theta_min      2.5490
_cell_volume                     2531.60(11)
_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-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (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 0.998
_diffrn_measured_fraction_theta_max 0.921
_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    -25.00  29.00   0.50    0.81    --  -49.76  19.00 150.00  108
  2  \w    -27.00  29.00   0.50    0.81    --  -49.76  19.00 -90.00  112
  3  \w    -27.00  29.00   0.50    0.81    --  -49.76  19.00-150.00  112
  4  \w     75.00 111.00   0.50    0.81    --   48.76 125.00-120.00   72
  5  \w     90.00 138.00   0.50    0.81    --  108.00 125.00-150.00   96
  6  \w    100.00 125.00   0.50    0.81    --   96.11 112.00   4.00   50
  7  \w     91.00 116.00   0.50    0.81    --  108.00 112.00   4.00   50
  8  \w    118.00 155.00   0.50    0.81    --   96.11  77.00 -30.00   74
  9  \w    139.00 164.00   0.50    0.81    --  108.00  45.00  30.00   50
 10  \w    111.00 137.00   0.50    0.81    --  108.00  45.00  30.00   52
 11  \w     75.00 100.00   0.50    0.81    --   96.11  77.00 -30.00   50
 12  \w    -28.00  16.00   0.50    0.81    --   48.76 -19.00 -30.00   88
 13  \w     18.00  45.00   0.50    0.81    --   96.11 -45.00 120.00   54
 14  \w     35.00  71.00   0.50    0.81    --  108.00 -61.00 120.00   72
 15  \w     40.00  71.00   0.50    0.81    --  108.00 -61.00  60.00   62
 16  \w     52.00  77.00   0.50    0.81    --   96.11 -77.00  30.00   50
 17  \w     24.00  54.00   0.50    0.81    --   96.11-125.00 -30.00   60
 18  \w     36.00  91.00   0.50    0.81    --  108.00-125.00   0.00  110
 19  \w     42.00  67.00   0.50    0.81    --   96.11-112.00 -88.00   50
 20  \w     39.00  64.00   0.50    0.81    --  108.00-125.00-120.00   50
 21  \w     56.00  82.00   0.50    0.81    --  108.00-112.00 -88.00   52
 22  \w     81.00 106.00   0.50    0.81    --  108.00-125.00-120.00   50
 23  \w     15.00  41.00   0.50    0.81    --   48.76-112.00 -88.00   52
 24  \w   -107.00 -48.00   0.50    0.81    --  -99.00 106.00-113.15  118
 25  \w   -107.00 -71.00   0.50    0.81    --  -99.00 107.00 -27.80   72
 26  \w   -125.00 -71.00   0.50    0.81    --  -99.00 143.00  31.67  108
 27  \w    -99.00 -69.00   0.50    0.81    --  -92.01 112.00   4.00   60
 28  \w    -88.00  -4.00   0.50    0.81    --  -49.76 112.00   4.00  168
 29  \w    -49.00 -17.00   0.50    0.81    --  -92.01  45.00 -90.00   64
 30  \w    -51.00 -24.00   0.50    0.81    --  -92.01  45.00-150.00   54
 31  \w   -105.00 -23.00   0.50    0.81    --  -92.01  77.00-150.00  164
 32  \w    -46.00 -20.00   0.50    0.81    --  -92.01  45.00-180.00   52
 33  \w    -51.00 -14.00   0.50    0.81    --  -92.01  45.00 -60.00   74
 34  \w    -48.00 -19.00   0.50    0.81    --  -92.01  45.00 -30.00   58
 35  \w    -71.00 -17.00   0.50    0.81    --  -92.01  61.00  30.00  108
 36  \w    -44.00 -16.00   0.50    0.81    --  -92.01  45.00 120.00   56
 37  \w   -168.00 -76.00   0.50    0.81    --  -92.01 -45.00 -30.00  184
 38  \w   -163.00 -82.00   0.50    0.81    --  -92.01-112.00 -88.00  162
 39  \w   -119.00 -81.00   0.50    0.81    --  -49.76-125.00-180.00   76
 40  \w   -111.00 -78.00   0.50    0.81    --  -49.76-125.00  60.00   66
;
_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      0.0170236000
_diffrn_orient_matrix_UB_12      -0.0729664000
_diffrn_orient_matrix_UB_13      -0.0649703000
_diffrn_orient_matrix_UB_21      0.0545539000
_diffrn_orient_matrix_UB_22      -0.1073413000
_diffrn_orient_matrix_UB_23      0.0588916000
_diffrn_orient_matrix_UB_31      -0.1283848000
_diffrn_orient_matrix_UB_32      0.0087261000
_diffrn_orient_matrix_UB_33      0.0171326000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29892
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.717
_diffrn_reflns_theta_min         2.563
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.888
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.00068(14)
_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   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.8656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8312
_reflns_number_total             10031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00211c2.cif
_cod_data_source_block           elu230001_fa
_cod_depositor_comments
'Adding full bibliography for 7715143--7715147.cif.'
_cod_database_code               7715145
_chemical_oxdiff_formula         'C20 H23 Na1 O1 '
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.835
_diffrn_oxdiff_digest_frames
;
01403703c5b295ae20c7373a2d2caee80603220e0ed
;
_diffrn_oxdiff_digest_hkl
;
01a5ac70335aa3f39fa9aa94e3dd943353adbf
;
_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), C49(H49), C50(H50), C51(H51), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
 C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
2.b X=CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C34(H34A,H34B)
;
_shelx_res_checksum              32631
_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 1.344
_oxdiff_exptl_absorpt_empirical_full_min 0.686