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_7715147
_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         'C164.898 H125.796 K8 O8'
_chemical_formula_sum            'C164.9 H125.79 K8 O8'
_chemical_formula_weight         2548.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-18
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2465(4)
_cell_length_b                   24.7118(4)
_cell_length_c                   28.6260(5)
_cell_measurement_reflns_used    29126
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      71.9860
_cell_measurement_theta_min      3.1740
_cell_volume                     14322.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.941
_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     52.00 116.00   0.50    9.29    --   46.35 158.00-128.00  128
  2  \w   -109.00 -17.00   0.50    9.29    --  -92.45 119.00  76.00  184
  3  \w   -168.00 -75.00   0.50    9.29    --  -92.45-122.00 -97.00  186
  4  \w     39.00 178.00   0.50    9.29    --  108.07  12.00 -98.00  278
  5  \w    -35.00  24.00   0.50    9.29    --   46.35 -12.00  89.00  118
  6  \w     74.00 106.00   0.50    9.29    --   46.35 125.00 -60.00   64
  7  \w    -41.00  33.00   0.50    9.29    --  -47.35  38.00  30.00  148
  8  \w     -6.00  34.00   0.50    9.29    --  -47.35  12.00 -98.00   80
  9  \w    -48.00 -11.00   0.50    9.29    --  -92.45  45.00-150.00   74
 10  \w    -49.00 -15.00   0.50    9.29    --  -92.45  45.00 -60.00   68
 11  \w     26.00  51.00   0.50    9.29    --   97.10 -45.00  60.00   50
 12  \w     77.00 105.00   0.50    9.29    --  108.07 -95.00 -30.00   56
 13  \w     48.00  73.00   0.50    9.29    --  108.07 -95.00 -30.00   50
 14  \w     35.00  82.00   0.50    9.29    --  108.07 -95.00 -90.00   94
;
_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      0.0124300000
_diffrn_orient_matrix_UB_12      -0.0340404000
_diffrn_orient_matrix_UB_13      -0.0442493000
_diffrn_orient_matrix_UB_21      -0.0011095000
_diffrn_orient_matrix_UB_22      0.0518432000
_diffrn_orient_matrix_UB_23      -0.0299086000
_diffrn_orient_matrix_UB_31      0.0749961000
_diffrn_orient_matrix_UB_32      0.0063928000
_diffrn_orient_matrix_UB_33      0.0069171000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            72419
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.159
_diffrn_reflns_theta_min         3.088
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.584
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
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    1.182
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             5325
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         14282
_refine_ls_number_restraints     1246
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0930P)^2^+7.5317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11956
_reflns_number_total             14282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00211c2.cif
_cod_data_source_block           elu230015_fa
_cod_depositor_comments
'Adding full bibliography for 7715143--7715147.cif.'
_cod_original_formula_sum        'C164.90 H125.79 K8 O8'
_cod_database_code               7715147
_chemical_oxdiff_formula         'C20 H23 K1 O1 Si1'
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.683
_diffrn_oxdiff_digest_frames
;
01b55740b005ecaa278382756d96a3b7ef01578166c
;
_diffrn_oxdiff_digest_hkl
;
015014877ae46d8502db67d10d72ed63c80149
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H77(0.55098) C83(0.44902) H83A(0.44902) H83B(0.44902) H83C(0.44902)
4.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), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74),
  C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82)
4.b X=CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C34(H34A,H34B), C50(H50A,H50B)
4.c Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              81442
_shelx_fab_checksum              25123
_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 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.710