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_7133442
_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         'C70 H66 Li2 O2 P4 S2'
_chemical_formula_sum            'C70 H66 Li2 O2 P4 S2'
_chemical_formula_weight         1141.10
_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             2023-11-04
_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
_cell_angle_beta                 106.0010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.7042(2)
_cell_length_b                   11.10570(10)
_cell_length_c                   18.8325(2)
_cell_measurement_reflns_used    21114
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.4420
_cell_measurement_theta_min      4.6560
_cell_volume                     2956.21(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -83.00 -45.00   0.50    0.40    --  -47.03 120.00-178.00   76
  2  \w    -79.00 -53.00   0.50    0.40    --  -47.03 154.00 -19.00   52
  3  \w    -86.00 -53.00   0.50    0.40    --  -47.03-154.00 -59.00   66
  4  \w     32.00  82.00   0.50    0.40    --   47.03-120.00  98.00  100
  5  \w     70.00 111.00   0.50    0.40    --   47.03-154.00 -59.00   82
  6  \w    -76.00 -51.00   0.50    1.60    --  -91.75 120.00-178.00   50
  7  \w    -91.00 -66.00   0.50    1.60    --  -91.75 154.00 -19.00   50
  8  \w   -126.00 -98.00   0.50    1.60    --  -91.75-120.00  98.00   56
  9  \w    132.00 158.00   0.50    1.60    --  105.91 154.00 -19.00   52
 10  \w     78.00 125.00   0.50    1.60    --  105.91 154.00 -19.00   94
 11  \w     66.00  91.00   0.50    1.60    --  105.91-154.00 -59.00   50
 12  \w    100.00 164.00   0.50    1.60    --  105.91 120.00-178.00  128
 13  \w     79.00 110.00   0.50    1.60    --  105.91-120.00  98.00   62
 14  \w   -119.00 -24.00   0.50    0.40    --  -47.03 -77.00 -60.00  190
 15  \w   -116.00 -49.00   0.50    0.40    --  -47.03 -57.00 -30.00  134
 16  \w   -115.00 -79.00   0.50    0.40    --  -47.03-125.00 -90.00   72
 17  \w    -18.00  25.00   0.50    0.40    --  -47.03  19.00-120.00   86
 18  \w    -23.00  27.00   0.50    0.40    --  -47.03  19.00  90.00  100
 19  \w    -83.00 -58.00   0.50    1.60    --  -91.75-154.00 -59.00   50
 20  \w   -163.00 -81.00   0.50    1.60    --  -91.75 -30.00 150.00  164
 21  \w    -48.00 -21.00   0.50    1.60    --  -91.75  45.00-120.00   54
 22  \w    -48.00 -23.00   0.50    1.60    --  -91.75  45.00  60.00   50
 23  \w    -81.00 -25.00   0.50    1.60    --  -91.75 125.00 -30.00  112
 24  \w    -80.00 -30.00   0.50    1.60    --  -91.75 125.00 -60.00  100
 25  \w   -133.00 -86.00   0.50    1.60    --  -91.75-154.00 -59.00   94
 26  \w    -48.00 -22.00   0.50    1.60    --  -91.75  45.00 -30.00   52
 27  \w   -160.00 -96.00   0.50    1.60    --  -91.75 -61.00 120.00  128
 28  \w    -46.00 -21.00   0.50    1.60    --  -91.75  45.00   0.00   50
 29  \w     54.00 104.00   0.50    1.60    --  105.91 -94.00-150.00  100
 30  \w     45.00 110.00   0.50    1.60    --  105.91-125.00-150.00  130
 31  \w     34.00  95.00   0.50    1.60    --  105.91 -77.00  90.00  122
 32  \w     52.00 110.00   0.50    1.60    --  105.91-125.00  60.00  116
 33  \w     39.00  67.00   0.50    1.60    --  105.91 -61.00 120.00   56
 34  \w     84.00 171.00   0.50    1.60    --  105.91  77.00-120.00  174
 35  \w     40.00  72.00   0.50    1.60    --  105.91 -61.00 150.00   64
 36  \w    150.00 175.00   0.50    1.60    --  105.91  45.00  90.00   50
 37  \w     95.00 122.00   0.50    1.60    --  105.91  45.00  90.00   54
 38  \w     94.00 168.00   0.50    1.60    --  105.91  30.00   0.00  148
 39  \w     50.00 105.00   0.50    1.60    --  105.91 -97.00 -42.34  110
 40  \w     85.00 112.00   0.50    1.60    --  105.91-125.00-180.00   54
 41  \w     34.00 106.00   0.50    1.60    --  105.91-102.00 -83.84  144
 42  \w     42.00  71.00   0.50    1.60    --  105.91 -61.00  90.00   58
 43  \w     34.00  64.00   0.50    1.60    --  105.91 -94.00 -60.00   60
;
_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      0.0697169000
_diffrn_orient_matrix_UB_12      0.0653211000
_diffrn_orient_matrix_UB_13      0.0647005000
_diffrn_orient_matrix_UB_21      0.0213730000
_diffrn_orient_matrix_UB_22      0.0922151000
_diffrn_orient_matrix_UB_23      -0.0544018000
_diffrn_orient_matrix_UB_31      -0.0809359000
_diffrn_orient_matrix_UB_32      0.0805478000
_diffrn_orient_matrix_UB_33      0.0098196000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35590
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.997
_diffrn_reflns_theta_min         3.127
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.193
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.257
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0524P)^2^+1.9154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4961
_reflns_number_total             5382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03167a2.cif
_cod_data_source_block           PD-447_auto_a
_cod_depositor_comments
'Adding full bibliography for 7133440--7133443.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7133442
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.506
_shelx_estimated_absorpt_t_max   0.844
_cell_oxdiff_length_a            14.7103(3)
_cell_oxdiff_length_b            11.10116(14)
_cell_oxdiff_length_c            18.8310(2)
_cell_oxdiff_angle_alpha         89.9966(10)
_cell_oxdiff_angle_beta          105.9858(14)
_cell_oxdiff_angle_gamma         90.0217(12)
_cell_oxdiff_volume              2956.22(7)
_cell_oxdiff_measurement_reflns_used 21114
_oxdiff_exptl_absorpt_empirical_full_min 0.706
_oxdiff_exptl_absorpt_empirical_full_max 1.394
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01e699fa046379967cdf69fa035e84b5990379488e4
;
_diffrn_oxdiff_digest_hkl
;
010ca92a1077c4c513c016c5dc176396b8a6e8
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C35 H33 Li1 S1 O1 P2'
_chemical_oxdiff_usercomment     'vapor diffusion tol-thf/hex'
_shelx_res_checksum              62104
_shelx_hkl_checksum              75750