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_7715146
_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         'C28 H41 N4 Na O'
_chemical_formula_sum            'C28 H41 N4 Na O'
_chemical_formula_weight         472.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 103.504(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3331(5)
_cell_length_b                   12.8913(5)
_cell_length_c                   19.8712(9)
_cell_measurement_reflns_used    7799
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      69.2080
_cell_measurement_theta_min      3.9900
_cell_volume                     2822.9(2)
_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 0.921
_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    -22.00   3.00   0.50    5.34    --   49.01 -14.00-144.00   50
  2  \w    -22.00   3.00   0.50    5.34    --  -49.76  14.00  26.00   50
  3  \w   -126.00 -70.00   0.50    5.34    --  -49.76 -14.00-144.00  112
  4  \w   -169.00-141.00   0.50    5.34    --  -92.01 -14.00-144.00   56
  5  \w   -136.00 -38.00   0.50    5.34    --  -92.01 -14.00-144.00  196
  6  \w     29.00  55.00   0.50    5.34    --   96.11  14.00  26.00   52
  7  \w     90.00 138.00   0.50    5.34    --  108.00  14.00  26.00   96
  8  \w     12.00 125.00   0.50    5.34    --   49.01  14.00  26.00  226
  9  \w    -42.00  29.00   0.50    5.34    --  -49.76  38.00 150.00  142
 10  \w    -79.00 -34.00   0.50    5.34    --  -92.01  77.00-180.00   90
 11  \w    -49.00 -14.00   0.50    5.34    --  -92.01  45.00-120.00   70
 12  \w    -50.00 -19.00   0.50    5.34    --  -92.01  45.00 120.00   62
 13  \w   -105.00 -29.00   0.50    5.34    --  -92.01  77.00 120.00  152
 14  \w    -50.00 -22.00   0.50    5.34    --  -92.01  45.00-180.00   56
 15  \w     22.00  47.00   0.50    5.34    --   96.11 -45.00 -90.00   50
 16  \w     69.00 106.00   0.50    5.34    --   96.11  14.00  26.00   74
 17  \w     18.00  51.00   0.50    5.34    --   96.11 -45.00 -30.00   66
 18  \w     36.00  66.00   0.50    5.34    --  108.00 -61.00 120.00   60
 19  \w     34.00  70.00   0.50    5.34    --  108.00 -61.00-150.00   72
 20  \w     53.00 106.00   0.50    5.34    --  108.00 -95.00  90.00  106
 21  \w     35.00  70.00   0.50    5.34    --  108.00 -61.00   0.00   70
 22  \w     44.00  69.00   0.50    5.34    --  108.00 -61.00 -90.00   50
;
_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      0.0206016000
_diffrn_orient_matrix_UB_12      -0.0118471000
_diffrn_orient_matrix_UB_13      0.0790528000
_diffrn_orient_matrix_UB_21      0.1370060000
_diffrn_orient_matrix_UB_22      0.0187721000
_diffrn_orient_matrix_UB_23      0.0081409000
_diffrn_orient_matrix_UB_31      -0.0197392000
_diffrn_orient_matrix_UB_32      0.1172905000
_diffrn_orient_matrix_UB_33      0.0066317000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19536
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.782
_diffrn_reflns_theta_min         4.012
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.857
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0853P)^2^+1.4341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4539
_reflns_number_total             5608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00211c2.cif
_cod_data_source_block           elu230005_fa
_cod_depositor_comments
'Adding full bibliography for 7715143--7715147.cif.'
_cod_database_code               7715146
_chemical_oxdiff_formula         'C32 H53 N4 Na1 O1 Si1'
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.868
_diffrn_oxdiff_digest_frames
;
01701dc5f645ba54f2386bda7195f117da019585dc0
;
_diffrn_oxdiff_digest_hkl
;
016fdee114c92103df6dc80e734e9e2ae1c4d6
;
_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.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)
2.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)
2.c X=CH2 refined with riding coordinates:
 C14(H14A,H14B)
2.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)
;
_shelx_res_checksum              4789
_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 1.394
_oxdiff_exptl_absorpt_empirical_full_min 0.443