[(TMEDA)Li(μ-PPh2)2K(TMEDA)(THF)]: a heterobimetallic molecular lithium–potassium phosphide complex
Crabbe, Michelle H.; O’Meara, Danielle; Kennedy, Alan R.; Weetman, Catherine E.; Mulvey, Robert E.; Chemical Communications 61 (2025) 9436–9439; doi:10.1039/D5CC02154E

data_7134583
_publ_section_title
;
 [(TMEDA)Li(\m-PPh2)2K(TMEDA)(THF)]: a heterobimetallic molecular
 lithium--potassium phosphide complex
;
_journal_issue                   52
_journal_name_full               'Chemical Communications'
_journal_page_first              9436
_journal_page_last               9439
_journal_paper_doi               10.1039/D5CC02154E
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C40 H60 K Li N4 O P2'
_chemical_formula_sum            'C40 H60 K Li N4 O P2'
_chemical_formula_weight         720.90
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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             2025-03-26
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-28 deposited with the CCDC.	2025-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.125(1)
_cell_angle_beta                 107.078(1)
_cell_angle_gamma                100.987(1)
_cell_formula_units_Z            2
_cell_length_a                   12.0377(1)
_cell_length_b                   12.2718(1)
_cell_length_c                   14.9623(1)
_cell_measurement_reflns_used    35034
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.8970
_cell_measurement_theta_min      3.0940
_cell_volume                     2070.12(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -68.00  27.00   0.50    0.80    --  -41.33  76.00 145.00  190
  2  \w   -110.00 -15.00   0.50    0.80    --  -41.33 -76.00  19.00  190
  3  \w   -110.00 -15.00   0.50    0.80    --  -41.33 -76.00  19.00  190
  4  \w   -101.00 -35.00   0.50    0.80    -- -104.00  76.00 145.00  132
  5  \w   -172.00 -77.00   0.50    0.80    -- -104.00 -76.00  19.00  190
  6  \w   -172.00 -77.00   0.50    0.80    -- -104.00 -76.00  19.00  190
  7  \w     36.00 101.00   0.50    0.80    --  104.00 -76.00  19.00  130
  8  \w     77.00 173.00   0.50    0.80    --  104.00  76.00 145.00  192
  9  \w   -107.00 -26.00   0.50    0.80    --  -41.33 -38.00-150.00  162
 10  \w    -43.00 -11.00   0.50    0.80    --  -41.33 -88.00  12.14   64
 11  \w   -107.00 -26.00   0.50    0.80    --  -41.33 -38.00-150.00  162
 12  \w    -43.00 -12.00   0.50    0.80    --  -41.33 -84.00 179.06   62
 13  \w    -24.00  34.00   0.50    0.80    --  -41.33  12.00-180.00  116
 14  \w    -43.00  25.00   0.50    0.80    --  -41.33  38.00 150.00  136
 15  \w    -31.00  29.00   0.50    0.80    --  -41.33  25.00  90.00  120
 16  \w     26.00 108.00   0.50    0.80    --   41.33  38.00 -90.00  164
 17  \w     11.00  43.00   0.50    0.80    --   41.33  87.00 -48.14   64
 18  \w    -27.00  68.00   0.50    0.80    --   41.33 -76.00  19.00  190
 19  \w     -4.00  79.00   0.50    0.80    --   41.33-104.00-150.00  166
 20  \w    -34.00  24.00   0.50    0.80    --   41.33 -12.00 -90.00  116
 21  \w     26.00 108.00   0.50    0.80    --   41.33  38.00 -90.00  164
 22  \w    -25.00  43.00   0.50    0.80    --   41.33 -38.00  30.00  136
 23  \w     11.00  43.00   0.50    0.80    --   41.33  88.00-112.77   64
 24  \w     19.00 100.00   0.50    0.80    --   41.33-138.00-180.00  162
 25  \w     10.00  43.00   0.50    0.80    --   41.33  89.00 -47.71   66
 26  \w     -4.00  79.00   0.50    0.80    --   41.33-104.00   0.00  166
 27  \w    -27.00  68.00   0.50    0.80    --   41.33 -77.00-150.00  190
 28  \w    -27.00  68.00   0.50    0.80    --   41.33 -76.00  19.00  190
 29  \w     15.00 110.00   0.50    0.80    --   41.33  76.00 145.00  190
 30  \w    -27.00  68.00   0.50    0.80    --   41.33 -77.00-150.00  190
 31  \w    -25.00  43.00   0.50    0.80    --   41.33 -38.00 -60.00  136
 32  \w    -29.00  31.00   0.50    0.80    --   41.33 -25.00-120.00  120
 33  \w   -109.00 -38.00   0.50    0.80    -- -104.00 112.00 120.00  142
 34  \w   -171.00 -87.00   0.50    0.80    -- -104.00 -42.00  60.00  168
 35  \w   -172.00 -90.00   0.50    0.80    -- -104.00 -33.00 -90.00  164
 36  \w   -176.00 -82.00   0.50    0.80    -- -104.00 -94.00  60.00  188
 37  \w   -170.00 -67.00   0.50    0.80    -- -104.00-133.00-180.00  206
 38  \w   -118.00 -38.00   0.50    0.80    -- -104.00 133.00   0.00  160
 39  \w   -105.00 -35.00   0.50    0.80    -- -104.00  77.00  60.00  140
 40  \w   -105.00 -35.00   0.50    0.80    -- -104.00  77.00  60.00  140
 41  \w   -105.00 -35.00   0.50    0.80    -- -104.00  77.00-150.00  140
 42  \w   -118.00 -38.00   0.50    0.80    -- -104.00 133.00 120.00  160
 43  \w   -109.00 -38.00   0.50    0.80    -- -104.00 112.00  90.00  142
 44  \w    -68.00 -36.00   0.50    0.80    -- -104.00  59.00 -90.00   64
 45  \w    -68.00 -36.00   0.50    0.80    -- -104.00  59.00 120.00   64
 46  \w   -172.00 -82.00   0.50    0.80    -- -104.00 -59.00 -30.00  180
 47  \w   -105.00 -35.00   0.50    0.80    -- -104.00  77.00  90.00  140
 48  \w   -174.00 -78.00   0.50    0.80    -- -104.00 -87.00   0.00  192
 49  \w   -120.00 -36.00   0.50    0.80    -- -104.00 135.00 -34.37  168
 50  \w   -171.00 -85.00   0.50    0.80    -- -104.00 -50.00 -60.00  172
 51  \w   -109.00 -38.00   0.50    0.80    -- -104.00 112.00   0.00  142
 52  \w   -172.00 -90.00   0.50    0.80    -- -104.00 -33.00-120.00  164
 53  \w   -109.00 -38.00   0.50    0.80    -- -104.00 112.00-120.00  142
 54  \w   -106.00 -31.00   0.50    0.80    -- -104.00  94.00-120.00  150
 55  \w   -118.00 -38.00   0.50    0.80    -- -104.00 133.00  60.00  160
 56  \w   -118.00 -38.00   0.50    0.80    -- -104.00 133.00 -60.00  160
 57  \w   -171.00 -85.00   0.50    0.80    -- -104.00 -50.00   0.00  172
 58  \w   -171.00 -85.00   0.50    0.80    -- -104.00 -50.00   0.00  172
 59  \w   -118.00 -38.00   0.50    0.80    -- -104.00 133.00 -60.00  160
 60  \w   -172.00 -82.00   0.50    0.80    -- -104.00 -59.00 -30.00  180
 61  \w   -114.00 -38.00   0.50    0.80    -- -104.00 127.00-157.83  152
 62  \w   -106.00 -80.00   0.50    0.80    -- -104.00  96.00-160.75   52
 63  \w    -63.00 -38.00   0.50    0.80    -- -104.00 112.00 -60.00   50
 64  \w   -107.00 -72.00   0.50    0.80    -- -104.00 112.00 -60.00   70
 65  \w    -95.00 -46.00   0.50    0.80    -- -104.00  94.00   0.00   98
 66  \w   -109.00 -79.00   0.50    0.80    -- -104.00 112.00 150.00   60
 67  \w   -171.00 -89.00   0.50    0.80    -- -104.00 -42.00-150.00  164
 68  \w    -99.00 -67.00   0.50    0.80    -- -104.00-133.00-180.00   64
 69  \w   -105.00 -37.00   0.50    0.80    -- -104.00  77.00 -60.00  136
 70  \w   -118.00 -91.00   0.50    0.80    -- -104.00 133.00 150.00   54
 71  \w   -133.00-107.00   0.50    0.80    -- -104.00 -25.00  30.00   52
 72  \w   -101.00 -75.00   0.50    0.80    -- -104.00  77.00-120.00   52
 73  \w   -174.00-135.00   0.50    0.80    -- -104.00 -25.00  30.00   78
 74  \w    -83.00 -36.00   0.50    0.80    -- -104.00  68.00   0.00   94
 75  \w   -166.00-131.00   0.50    0.80    -- -104.00 -59.00 120.00   70
 76  \w   -169.00-112.00   0.50    0.80    -- -104.00 -42.00  90.00  114
 77  \w   -103.00 -77.00   0.50    0.80    -- -104.00  77.00   0.00   52
 78  \w    -64.00 -38.00   0.50    0.80    -- -104.00  77.00   0.00   52
 79  \w   -172.00 -92.00   0.50    0.80    -- -104.00 -25.00 -30.00  160
 80  \w    -63.00 -38.00   0.50    0.80    -- -104.00 133.00 150.00   50
 81  \w   -103.00 -55.00   0.50    0.80    -- -104.00  94.00  90.00   96
 82  \w    -90.00 -64.00   0.50    0.80    -- -104.00  94.00 120.00   52
 83  \w    -83.00 -43.00   0.50    0.80    -- -104.00  68.00 -90.00   80
 84  \w    -62.00 -36.00   0.50    0.80    -- -104.00  96.00-160.75   52
 85  \w    -62.00 -36.00   0.50    0.80    -- -104.00  59.00 -60.00   52
 86  \w    -88.00 -62.00   0.50    0.80    -- -104.00 133.00 -90.00   52
 87  \w   -114.00 -82.00   0.50    0.80    -- -104.00 -94.00  60.00   64
 88  \w     50.00  76.00   0.50    0.80    --  104.00-112.00 -30.00   52
 89  \w    133.00 163.00   0.50    0.80    --  104.00  68.00  30.00   60
 90  \w     80.00 105.00   0.50    0.80    --  104.00  68.00  30.00   50
 91  \w     80.00 171.00   0.50    0.80    --  104.00  68.00  60.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1142098000
_diffrn_orient_matrix_UB_12      -0.0879341000
_diffrn_orient_matrix_UB_13      -0.0123278000
_diffrn_orient_matrix_UB_21      0.0153807000
_diffrn_orient_matrix_UB_22      -0.0500773000
_diffrn_orient_matrix_UB_23      -0.0890845000
_diffrn_orient_matrix_UB_31      0.0734240000
_diffrn_orient_matrix_UB_32      -0.0785893000
_diffrn_orient_matrix_UB_33      0.0596542000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41792
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         72.940
_diffrn_reflns_theta_min         3.096
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.106
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.107a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         8218
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0667P)^2^+0.9143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7911
_reflns_number_total             8218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02154e2.cif
_cod_data_source_block           dom240119-01_auto
_cod_depositor_comments          'Adding full bibliography for 7134583.cif.'
_cod_database_code               7134583
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Li1 K1 P2 C30 H25 N2'
_diffrn_oxdiff_digest_hkl
;
012daec476070894deed1fdab83226009228fc
;
_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. Restrained distances
 C37-C38 = C38-C39 = C39-C40 = C33-C34
 1.53 with sigma of 0.01
 O1-C37 = O1-C40 = O1-C37A = O1-C40A
 1.43 with sigma of 0.01
 C37A-C38A = C38A-C39A = C39A-C40A = C33A-C34A
 1.53 with sigma of 0.01
 N4-C36 = N4-C35 = N4-C34 = N3-C31 = N3-C33 = N3-C32 = N3A-C31A
 1.48 with sigma of 0.01
 N3A-C32A = N3A-C33A = N4A-C34A = N4A-C35A = N4A-C36A
 1.48 with sigma of 0.01
3. Rigid bond restraints
 O1, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, C38A, C39A, C37A, C40A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, N4, C31, C32, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33A, C34A, N3A, N4A, C32A, C36A, C31A, C35A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.02 within 1.7A
O1 \\sim C38A \\sim C39A \\sim C37A \\sim C40A: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.02 within 1.7A
N3 \\sim N4 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
C33A \\sim C34A \\sim N3A \\sim N4A \\sim C32A \\sim C36A \\sim C31A \\sim
C35A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
within 1.7A
Uanis(C40) = Uanis(C40A)
Uanis(C39) = Uanis(C39A)
Uanis(C38) = Uanis(C38A)
Uanis(N4) = Uanis(N4A)
Uanis(N3) = Uanis(N3A)
5. Others
 Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C37A)=
 Sof(H37C)=Sof(H37D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(1)
 Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(N3A)=Sof(N4A)=
 Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C35A)=Sof(H35D)=
 Sof(H35E)=Sof(H35F)=1-FVAR(2)
 Sof(N3)=Sof(N4)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C33(H33A,H33B), C34(H34A,H34B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C38A(H38C,H38D),
 C39A(H39C,H39D), C37A(H37C,H37D), C40A(H40C,H40D), C33A(H33C,H33D), C34A(H34C,
 H34D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24)
6.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C32A(H32D,H32E,H32F), C36A(H36D,H36E,H36F), C31A(H31D,H31E,H31F),
 C35A(H35D,H35E,H35F)
;
_shelx_res_checksum              51666
_shelx_hkl_checksum              75895
_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 4.224
_oxdiff_exptl_absorpt_empirical_full_min 0.598