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_7715144
_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         '2(C28 H41 Li N4 O), C7 H8'
_chemical_formula_sum            'C63 H90 Li2 N8 O2'
_chemical_formula_weight         1005.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-03
_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                 95.153(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4692(2)
_cell_length_b                   17.6687(4)
_cell_length_c                   13.5637(2)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      77.6440
_cell_measurement_theta_min      4.1110
_cell_volume                     2976.20(9)
_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 0.999
_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    -51.00 -17.00   0.50    1.17    --  -92.01  45.00-120.00   68
  2  \w    -25.00  29.00   0.50    1.17    --  -49.76  19.00-120.00  108
  3  \w    -27.00  29.00   0.50    1.17    --  -49.76  19.00 -60.00  112
  4  \w    -27.00  29.00   0.50    1.17    --  -49.76  19.00   0.00  112
  5  \w    -45.00 -17.00   0.50    1.17    --  -92.01  45.00 -90.00   56
  6  \w    -46.00 -21.00   0.50    1.17    --  -92.01  45.00 -30.00   50
  7  \w    -51.00 -20.00   0.50    1.17    --  -92.01  45.00   0.00   62
  8  \w   -109.00 -46.00   0.50    1.17    --  -92.01 117.00 129.00  126
  9  \w    -77.00 -52.00   0.50    1.17    --  -49.76 117.00 129.00   50
 10  \w   -145.00-120.00   0.50    1.17    --  -92.01-117.00  42.00   50
 11  \w    -89.00 -61.00   0.50    1.17    --  -49.76-162.00-107.00   56
 12  \w   -137.00 -51.00   0.50    1.17    --  -92.01-162.00-107.00  172
 13  \w     41.00 129.00   0.50    1.17    --  108.00-162.00-107.00  176
 14  \w     29.00 110.00   0.50    1.17    --   96.11-125.00 -60.00  162
 15  \w     46.00  98.00   0.50    1.17    --   48.76-117.00  42.00  104
 16  \w     49.00  74.00   0.50    1.17    --  108.00-117.00  42.00   50
 17  \w     59.00 106.00   0.50    1.17    --  108.00 -95.00  30.00   94
 18  \w     35.00  67.00   0.50    1.17    --  108.00 -61.00  30.00   64
 19  \w     45.00  70.00   0.50    1.17    --  108.00 -61.00  90.00   50
 20  \w     26.00  51.00   0.50    1.17    --   96.11 -45.00 120.00   50
 21  \w     25.00  51.00   0.50    1.17    --   96.11 -45.00 -60.00   52
 22  \w     18.00  51.00   0.50    1.17    --   96.11 -45.00-120.00   66
 23  \w     22.00  48.00   0.50    1.17    --   96.11 -45.00-180.00   52
 24  \w     36.00  61.00   0.50    1.17    --  108.00 -61.00-150.00   50
 25  \w     21.00  49.00   0.50    1.17    --   96.11 -45.00 -90.00   56
 26  \w     99.00 124.00   0.50    1.17    --   96.11 117.00 129.00   50
 27  \w     74.00  99.00   0.50    1.17    --   48.76 125.00 -30.00   50
 28  \w     54.00  83.00   0.50    1.17    --   48.76 162.00 -80.00   58
;
_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      -0.0491381000
_diffrn_orient_matrix_UB_12      0.0060871000
_diffrn_orient_matrix_UB_13      0.1000204000
_diffrn_orient_matrix_UB_21      -0.0128987000
_diffrn_orient_matrix_UB_22      0.0861471000
_diffrn_orient_matrix_UB_23      -0.0146945000
_diffrn_orient_matrix_UB_31      -0.1130346000
_diffrn_orient_matrix_UB_32      -0.0124049000
_diffrn_orient_matrix_UB_33      -0.0528268000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.316
_diffrn_reflns_theta_min         4.119
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.858
_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    1.122
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.00110(15)
_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   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5969
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.4827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4825
_reflns_number_total             5969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00211c2.cif
_cod_data_source_block           elu230006_fa
_cod_depositor_comments
'Adding full bibliography for 7715143--7715147.cif.'
_cod_database_code               7715144
_chemical_oxdiff_formula         'C32 H53 Li1 N4 O1 Si1'
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.894
_diffrn_oxdiff_digest_frames
;
0191e215742374f4b43aca3b51fc1248b102206fc18
;
_diffrn_oxdiff_digest_hkl
;
01725a1c67b32592baed3b878ff070787b748e
;
_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. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
3. 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
4. Others
 Fixed Sof: C29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5)
 C33(0.5) H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25),
 C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
5.c X=CH2 refined with riding coordinates:
 C14(H14A,H14B)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              83234
_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 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.705