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_7133441
_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         'C46 H66 Li2 N6 O2 P2 Se2'
_chemical_formula_sum            'C46 H66 Li2 N6 O2 P2 Se2'
_chemical_formula_weight         968.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-29
_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                 103.328(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.8320(7)
_cell_length_b                   9.4158(2)
_cell_length_c                   11.2461(3)
_cell_measurement_reflns_used    7456
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.3410
_cell_measurement_theta_min      4.8620
_cell_volume                     2455.63(11)
_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      100(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 0.964
_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   -118.00 -33.00   0.50    1.30    --  -46.90 -51.00 144.00  170
  2  \w     75.00 119.00   0.50    1.30    --   46.90  51.00 -69.00   88
  3  \w      0.00  26.00   0.50    1.30    --   46.90 -51.00 144.00   52
  4  \w     29.00  56.00   0.50    1.30    --   46.90 -51.00 144.00   54
  5  \w    -50.00 -25.00   0.50    5.50    --  -91.75  51.00 -69.00   50
  6  \w   -162.00 -79.00   0.50    5.50    --  -91.75 -51.00 144.00  166
  7  \w    149.00 175.00   0.50    5.50    --  105.91  51.00 -69.00   52
  8  \w     34.00  60.00   0.50    5.50    --  105.91 -51.00 144.00   52
  9  \w   -119.00 -93.00   0.50    1.30    --  -46.90-125.00   0.00   52
 10  \w    -54.00  25.00   0.50    1.30    --  -46.90  51.00 -69.00  158
 11  \w   -119.00 -73.00   0.50    1.30    --  -46.90-125.00  90.00   92
 12  \w   -112.00 -85.00   0.50    1.30    --  -46.90-125.00 120.00   54
 13  \w    -72.00 -13.00   0.50    1.30    --  -46.90 125.00 -30.00  118
 14  \w     56.00  85.00   0.50    1.30    --   46.90-125.00   0.00   58
 15  \w    -48.00 -23.00   0.50    5.50    --  -91.75  45.00  30.00   50
 16  \w    -46.00 -21.00   0.50    5.50    --  -91.75  45.00   0.00   50
 17  \w    -68.00 -37.00   0.50    5.50    --  -91.75  61.00 -90.00   62
 18  \w   -163.00 -85.00   0.50    5.50    --  -91.75 -45.00  30.00  156
 19  \w    -58.00 -24.00   0.50    5.50    --  -91.75  61.00  90.00   68
 20  \w    -67.00 -20.00   0.50    5.50    --  -91.75  61.00 120.00   94
 21  \w    -48.00 -21.00   0.50    5.50    --  -91.75  45.00 120.00   54
 22  \w     35.00  65.00   0.50    5.50    --  105.91 -94.00  30.00   60
 23  \w     93.00 141.00   0.50    5.50    --  105.91  30.00 -60.00   96
 24  \w     33.00 106.00   0.50    5.50    --  105.91 -94.00   0.00  146
 25  \w     76.00 104.00   0.50    5.50    --  105.91 -77.00 120.00   56
 26  \w     55.00 107.00   0.50    5.50    --  105.91-104.00 164.24  104
 27  \w     95.00 171.00   0.50    5.50    --  105.91  45.00-150.00  152
 28  \w     71.00  97.00   0.50    5.50    --  105.91-125.00 -90.00   52
 29  \w     54.00 111.00   0.50    5.50    --  105.91-125.00   0.00  114
 30  \w     48.00  89.00   0.50    5.50    --  105.91 -94.00  90.00   82
 31  \w     42.00  87.00   0.50    5.50    --  105.91 -94.00-120.00   90
 32  \w     95.00 155.00   0.50    5.50    --  105.91  77.00 -60.00  120
 33  \w     77.00 102.00   0.50    5.50    --  105.91 -77.00-120.00   50
 34  \w     34.00  62.00   0.50    5.50    --  105.91 -77.00-120.00   56
 35  \w     95.00 122.00   0.50    5.50    --  105.91 125.00  30.00   54
 36  \w     69.00 102.00   0.50    5.50    --  105.91 -94.00  30.00   66
 37  \w     38.00 111.00   0.50    5.50    --  105.91-125.00-180.00  146
;
_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      0.0329946000
_diffrn_orient_matrix_UB_12      0.0018979000
_diffrn_orient_matrix_UB_13      0.1350276000
_diffrn_orient_matrix_UB_21      0.0251163000
_diffrn_orient_matrix_UB_22      -0.1477543000
_diffrn_orient_matrix_UB_23      -0.0156663000
_diffrn_orient_matrix_UB_31      0.0518850000
_diffrn_orient_matrix_UB_32      0.0702360000
_diffrn_orient_matrix_UB_33      -0.0367312000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13004
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.898
_diffrn_reflns_theta_min         3.812
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.818
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.423
_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            colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.970
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Flack x determined using 1766 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4663
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0571
_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^)+(0.1285P)^2^+3.5312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1781
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.904
_reflns_Friedel_fraction_max     0.820
_reflns_number_gt                4394
_reflns_number_total             4663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03167a2.cif
_cod_data_source_block           PD-499-3
_cod_depositor_comments
'Adding full bibliography for 7133440--7133443.cif.'
_cod_original_cell_volume        2455.63(12)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7133441
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.539
_shelx_estimated_absorpt_t_max   0.786
_cell_oxdiff_length_a            23.8364(10)
_cell_oxdiff_length_b            9.4161(3)
_cell_oxdiff_length_c            11.2436(3)
_cell_oxdiff_angle_alpha         89.983(2)
_cell_oxdiff_angle_beta          103.328(3)
_cell_oxdiff_angle_gamma         89.982(3)
_cell_oxdiff_volume              2455.63(13)
_cell_oxdiff_measurement_reflns_used 7456
_oxdiff_exptl_absorpt_empirical_full_min 0.530
_oxdiff_exptl_absorpt_empirical_full_max 2.191
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C92 H132 Li4 N12 O4 P4 Se4'
_chemical_oxdiff_usercomment     'vapor diffusion tol-thf/hex in freezer'
_shelx_res_checksum              72075
_shelx_hkl_checksum              63062