The lithium effect in ketenyl anion chemistry.
Duari, Prakash; Mondal, Sunita; Jörges, Mike; Gessner, Viktoria H.; Chemical communications (Cambridge, England) 60 (2024) 9372–9375; doi:10.1039/d4cc03167a

data_7133443
_publ_section_title
;
 The lithium effect in ketenyl anion chemistry.
;
_journal_issue                   70
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9372
_journal_page_last               9375
_journal_paper_doi               10.1039/d4cc03167a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C36 H36 Li2 O6 P2'
_chemical_formula_sum            'C36 H36 Li2 O6 P2'
_chemical_formula_weight         640.47
_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             2023-11-14
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-07-31 deposited with the CCDC.	2024-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.527(2)
_cell_angle_beta                 91.990(2)
_cell_angle_gamma                100.300(2)
_cell_formula_units_Z            4
_cell_length_a                   14.2502(3)
_cell_length_b                   15.4854(3)
_cell_length_c                   15.5126(3)
_cell_measurement_reflns_used    14366
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.9510
_cell_measurement_theta_min      6.3130
_cell_volume                     3365.56(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (G.M. Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_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     90.00 168.00   0.50    1.00    --  105.91  62.00-125.00  156
  2  \w    111.00 173.00   0.50    1.00    --  105.91  30.00 -60.00  124
  3  \w     53.00 117.00   0.50    0.25    --   47.03  62.00-125.00  128
  4  \w     93.00 174.00   0.50    1.00    --  105.91  30.00 -30.00  162
  5  \w     96.00 178.00   0.50    1.00    --  105.91  15.00  30.00  164
  6  \w     75.00 105.00   0.50    1.00    --  105.91 -94.00  30.00   60
  7  \w     80.00 109.00   0.50    1.00    --  105.91-117.00  40.16   58
  8  \w     35.00  89.00   0.50    0.25    --   47.03-125.00 -30.00  108
  9  \w     36.00  70.00   0.50    1.00    --  105.91-125.00-150.00   68
 10  \w     85.00 112.00   0.50    1.00    --  105.91-125.00-150.00   54
 11  \w     79.00 106.00   0.50    1.00    --  105.91 -94.00-150.00   54
 12  \w     39.00  65.00   0.50    1.00    --  105.91 -94.00-150.00   52
 13  \w     69.00 106.00   0.50    1.00    --  105.91-125.00 -60.00   74
 14  \w     36.00  95.00   0.50    1.00    --  105.91 -94.00 -30.00  118
 15  \w     78.00 103.00   0.50    1.00    --  105.91 -94.00 -90.00   50
 16  \w     46.00  72.00   0.50    1.00    --  105.91-117.00  40.16   52
 17  \w     34.00  60.00   0.50    1.00    --  105.91 -94.00  60.00   52
 18  \w     69.00 106.00   0.50    1.00    --  105.91 -94.00  60.00   74
 19  \w     74.00 101.00   0.50    1.00    --  105.91 -94.00  90.00   54
 20  \w     73.00 104.00   0.50    1.00    --  105.91 -94.00 150.00   62
 21  \w     44.00  71.00   0.50    1.00    --  105.91 -94.00 150.00   54
 22  \w     35.00  68.00   0.50    1.00    --  105.91 -94.00  90.00   66
 23  \w     46.00  71.00   0.50    1.00    --  105.91 -94.00  30.00   50
 24  \w     40.00  92.00   0.50    1.00    --  105.91 -77.00 -30.00  104
 25  \w     40.00  73.00   0.50    1.00    --  105.91 -61.00-120.00   66
 26  \w     13.00  45.00   0.50    0.25    --   47.03 -62.00  96.00   64
 27  \w    -18.00  12.00   0.50    0.25    --   47.03 -62.00  96.00   60
 28  \w     34.00  75.00   0.50    1.00    --  105.91 -62.00  96.00   82
 29  \w     96.00 171.00   0.50    1.00    --  105.91 125.00 -30.00  150
 30  \w    110.00 136.00   0.50    1.00    --  105.91 125.00 -60.00   52
 31  \w    143.00 171.00   0.50    1.00    --  105.91 125.00 -60.00   56
 32  \w    -64.00  24.00   0.50    0.25    --  -47.03  62.00-125.00  176
 33  \w    -50.00 -24.00   0.50    1.00    --  -91.75  62.00-125.00   52
 34  \w    -68.00 -21.00   0.50    1.00    --  -91.75  61.00 -60.00   94
 35  \w    -48.00 -23.00   0.50    1.00    --  -91.75  45.00 -60.00   50
 36  \w    -46.00 -21.00   0.50    1.00    --  -91.75  45.00-120.00   50
 37  \w    -48.00 -23.00   0.50    1.00    --  -91.75  45.00 -30.00   50
 38  \w    -21.00   6.00   0.50    0.25    --  -47.03  19.00-180.00   54
 39  \w    -57.00 -31.00   0.50    1.00    --  -91.75  61.00  60.00   52
 40  \w    -48.00 -22.00   0.50    1.00    --  -91.75  45.00  90.00   52
 41  \w    -60.00 -25.00   0.50    1.00    --  -91.75  61.00 150.00   70
 42  \w    -61.00 -14.00   0.50    0.25    --  -47.03 125.00 150.00   94
 43  \w   -143.00-112.00   0.50    1.00    --  -91.75 -45.00-150.00   62
 44  \w   -118.00 -78.00   0.50    0.25    --  -47.03-125.00-180.00   80
 45  \w   -116.00 -81.00   0.50    0.25    --  -47.03-125.00-150.00   70
 46  \w   -114.00 -30.00   0.50    0.25    --  -47.03 -62.00  96.00  168
 47  \w   -163.00 -86.00   0.50    1.00    --  -91.75 -62.00  96.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0715940000
_diffrn_orient_matrix_UB_12      -0.0213103000
_diffrn_orient_matrix_UB_13      0.0698271000
_diffrn_orient_matrix_UB_21      0.0669280000
_diffrn_orient_matrix_UB_22      0.0872238000
_diffrn_orient_matrix_UB_23      -0.0176587000
_diffrn_orient_matrix_UB_31      -0.0498470000
_diffrn_orient_matrix_UB_32      0.0465237000
_diffrn_orient_matrix_UB_33      0.0684778000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22471
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.831
_diffrn_reflns_theta_min         2.851
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         22471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0673P)^2^+7.1882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.2099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20188
_reflns_number_total             22471
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9596\% 
 around [-0.00 -0.00 1.00] (reciprocal) or [0.04 0.02 1.00] (direct)
;
_cod_data_source_file            d4cc03167a2.cif
_cod_data_source_block           SMO-225
_cod_depositor_comments
'Adding full bibliography for 7133440--7133443.cif.'
_cod_database_code               7133443
_shelx_shelxl_version_number     2019/3
_cell_oxdiff_length_a            14.2502(3)
_cell_oxdiff_length_b            15.4854(3)
_cell_oxdiff_length_c            15.5126(3)
_cell_oxdiff_angle_alpha         90.5275(15)
_cell_oxdiff_angle_beta          91.9898(16)
_cell_oxdiff_angle_gamma         100.2998(15)
_cell_oxdiff_volume              3365.57(11)
_cell_oxdiff_measurement_reflns_used 14366
_oxdiff_exptl_absorpt_empirical_full_min 0.584
_oxdiff_exptl_absorpt_empirical_full_max 1.737
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_twin_items               2
_chemical_oxdiff_formula         'C72 H72 Li4 O12 P4'
_chemical_oxdiff_usercomment     'tHF toluene /pen'
_shelx_res_checksum              38868
_shelx_hkl_checksum              88371