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_7133440
_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 Se2'
_chemical_formula_sum            'C70 H66 Li2 O2 P4 Se2'
_chemical_formula_weight         1234.90
_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             2023-10-22
_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                 97.1570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.72650(10)
_cell_length_b                   9.50190(10)
_cell_length_c                   20.4394(2)
_cell_measurement_reflns_used    26409
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.8840
_cell_measurement_theta_min      2.8200
_cell_volume                     3030.50(5)
_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 0.976
_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    108.00 178.00   0.50    0.44    --  105.91  45.00 -90.00  140
  2  \w     96.00 171.00   0.50    0.44    --  105.91 125.00 -90.00  150
  3  \w     96.00 132.00   0.50    0.44    --  105.91 125.00   0.00   72
  4  \w    135.00 169.00   0.50    0.44    --  105.91 125.00   0.00   68
  5  \w    118.00 143.00   0.50    0.44    --  105.91 102.00 142.00   50
  6  \w    -58.00  23.00   0.50    0.11    --  -47.28  57.00 120.00  162
  7  \w    -39.00  26.00   0.50    0.11    --  -47.28  38.00  60.00  130
  8  \w    -48.00 -22.00   0.50    0.44    --  -91.75  45.00   0.00   52
  9  \w    -47.00 -21.00   0.50    0.44    --  -91.75  45.00 -60.00   52
 10  \w    -48.00 -23.00   0.50    0.44    --  -91.75  45.00-120.00   50
 11  \w    -48.00 -21.00   0.50    0.44    --  -91.75  45.00-150.00   54
 12  \w    -14.00  11.00   0.50    0.11    --  -47.28  19.00-150.00   50
 13  \w    -48.00 -20.00   0.50    0.44    --  -91.75  45.00  90.00   56
 14  \w    -70.00  13.00   0.50    0.11    --  -47.28 102.00 142.00  166
 15  \w    -84.00 -43.00   0.50    0.44    --  -91.75 125.00 150.00   82
 16  \w    -74.00 -49.00   0.50    0.44    --  -91.75 102.00 142.00   50
 17  \w   -163.00 -78.00   0.50    0.44    --  -91.75 -15.00  30.00  170
 18  \w   -108.00 -82.00   0.50    0.11    --  -47.28 -19.00  90.00   52
 19  \w   -120.00 -76.00   0.50    0.44    --  -91.75 -61.00 150.00   88
 20  \w   -161.00-127.00   0.50    0.44    --  -91.75 -61.00 150.00   68
 21  \w   -160.00 -71.00   0.50    0.44    --  -91.75 -77.00 120.00  178
 22  \w   -164.00 -79.00   0.50    0.44    --  -91.75 -15.00   0.00  170
 23  \w   -138.00-111.00   0.50    0.44    --  -91.75-102.00  39.00   54
 24  \w   -119.00 -86.00   0.50    0.11    --  -47.28-125.00 150.00   66
 25  \w   -119.00 -91.00   0.50    0.11    --  -47.28-125.00  90.00   56
 26  \w   -118.00 -83.00   0.50    0.11    --  -47.28-125.00-120.00   70
 27  \w   -118.00 -87.00   0.50    0.11    --  -47.28-125.00-150.00   62
 28  \w     34.00  63.00   0.50    0.44    --  105.91 -94.00 -60.00   58
 29  \w     60.00 111.00   0.50    0.44    --  105.91-125.00-180.00  102
 30  \w     36.00 111.00   0.50    0.44    --  105.91-125.00 -90.00  150
 31  \w     83.00 110.00   0.50    0.44    --  105.91-125.00 -60.00   54
 32  \w     43.00 112.00   0.50    0.44    --  105.91-125.00  30.00  138
 33  \w     51.00 104.00   0.50    0.44    --  105.91-125.00  60.00  106
 34  \w     33.00  77.00   0.50    0.44    --  105.91 -94.00  60.00   88
 35  \w     81.00 106.00   0.50    0.44    --  105.91 -94.00  60.00   50
 36  \w     64.00 106.00   0.50    0.44    --  105.91-102.00  39.00   84
 37  \w     44.00 106.00   0.50    0.44    --  105.91 -94.00  90.00  124
 38  \w      9.00  70.00   0.50    0.11    --   47.28-102.00  39.00  122
 39  \w     74.00  99.00   0.50    0.44    --  105.91 -94.00 -60.00   50
 40  \w     42.00  73.00   0.50    0.44    --  105.91 -61.00 -90.00   62
 41  \w     35.00  63.00   0.50    0.44    --  105.91 -61.00 -60.00   56
 42  \w     49.00  74.00   0.50    0.44    --  105.91 -61.00 -30.00   50
;
_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      -0.0980477000
_diffrn_orient_matrix_UB_12      0.0079772000
_diffrn_orient_matrix_UB_13      -0.0012143000
_diffrn_orient_matrix_UB_21      0.0117756000
_diffrn_orient_matrix_UB_22      0.0473020000
_diffrn_orient_matrix_UB_23      0.0726384000
_diffrn_orient_matrix_UB_31      0.0014299000
_diffrn_orient_matrix_UB_32      0.1548215000
_diffrn_orient_matrix_UB_33      -0.0222225000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38788
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.746
_diffrn_reflns_theta_min         2.832
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.869
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.545
_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    1.353
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0422P)^2^+3.1317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5859
_reflns_number_total             6214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03167a2.cif
_cod_data_source_block           PD-440_auto_a
_cod_depositor_comments
'Adding full bibliography for 7133440--7133443.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7133440
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.500
_shelx_estimated_absorpt_t_max   0.689
_cell_oxdiff_length_a            15.7232(2)
_cell_oxdiff_length_b            9.50480(13)
_cell_oxdiff_length_c            20.4401(2)
_cell_oxdiff_angle_alpha         89.9348(11)
_cell_oxdiff_angle_beta          97.2173(11)
_cell_oxdiff_angle_gamma         89.9948(11)
_cell_oxdiff_volume              3030.49(7)
_cell_oxdiff_measurement_reflns_used 26409
_oxdiff_exptl_absorpt_empirical_full_min 0.624
_oxdiff_exptl_absorpt_empirical_full_max 2.036
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
0106e17d3e74f56483180527d34abb82e2037126cc9
;
_diffrn_oxdiff_digest_hkl
;
01d2fa598c6f1b9eacb9bc5f2c405cdc1a4689
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C35 H34 P2 Li1 Se1 O1'
_chemical_oxdiff_usercomment     'vapor diffudion thf-hex'
_shelx_res_checksum              23463
_shelx_hkl_checksum              4494