Tetraphenylpentalenide organolanthanide complexes.
Katzer, Nicholas J.; Kaur, Mandeep; Sen, Asmita; Nimaiyar, Rupal; Autschbach, Jochen; Arnold, Polly L.; Hintermair, Ulrich; Chemical communications (Cambridge, England) 60 (2024) 9749–9752; doi:10.1039/d4cc02570a

data_7133321
_publ_section_title
;
 Tetraphenylpentalenide organolanthanide complexes.
;
_journal_issue                   72
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9749
_journal_page_last               9752
_journal_paper_doi               10.1039/d4cc02570a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C48 H62 K2 O8'
_chemical_formula_sum            'C48 H62 K2 O8'
_chemical_formula_weight         845.17
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-18 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.8280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.14420(10)
_cell_length_b                   13.06880(10)
_cell_length_c                   16.74600(10)
_cell_measurement_reflns_used    34332
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      79.6210
_cell_measurement_theta_min      4.1070
_cell_volume                     2334.47(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_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 0.995
_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    -26.00   8.00   0.50    0.05    --   47.94 -19.00-180.00   68
  2  \w    -25.00  34.00   0.50    0.05    --   47.94 -37.00 -60.00  118
  3  \w    -26.00   8.00   0.50    0.05    --   47.94 -19.00 -30.00   68
  4  \w    -26.00   8.00   0.50    0.05    --   47.94 -19.00 120.00   68
  5  \w     85.00 111.00   0.50    0.21    --  113.25 -82.00  57.53   52
  6  \w     57.00 111.00   0.50    0.21    --  113.25-125.00  60.00  108
  7  \w     48.00  80.00   0.50    0.21    --  113.25-125.00 -60.00   64
  8  \w     86.00 111.00   0.50    0.21    --  113.25-125.00 -60.00   50
  9  \w     44.00 125.00   0.50    0.21    --  113.25-143.00 -91.18  162
 10  \w     44.00  91.00   0.50    0.21    --  113.25-125.00-150.00   94
 11  \w     47.00 108.00   0.50    0.21    --  113.25-106.00 -22.31  122
 12  \w      0.00  80.00   0.50    0.05    --   47.94 -99.00-120.00  160
 13  \w     42.00  83.00   0.50    0.21    --  113.25 -94.00  30.00   82
 14  \w     75.00 105.00   0.50    0.21    --  113.25 -94.00  90.00   60
 15  \w     70.00 104.00   0.50    0.21    --  113.25 -94.00 120.00   68
 16  \w     68.00 103.00   0.50    0.21    --  113.25 -94.00 150.00   70
 17  \w     78.00 107.00   0.50    0.21    --  113.25-104.00  48.50   58
 18  \w     43.00  69.00   0.50    0.21    --  113.25 -94.00   0.00   52
 19  \w     71.00  97.00   0.50    0.21    --  113.25 -94.00 -90.00   52
 20  \w     77.00 103.00   0.50    0.21    --  113.25 -90.00-174.44   52
 21  \w     68.00 106.00   0.50    0.21    --  113.25 -94.00-180.00   76
 22  \w     42.00 106.00   0.50    0.21    --  113.25 -94.00-150.00  128
 23  \w     42.00  86.00   0.50    0.21    --  113.25 -94.00-120.00   88
 24  \w     89.00 115.00   0.50    0.21    --  113.25 -88.00  46.29   52
 25  \w     57.00  82.00   0.50    0.21    --  113.25 -88.00  46.29   50
 26  \w     43.00  73.00   0.50    0.21    --  113.25 -82.00  57.53   60
 27  \w    103.00 128.00   0.50    0.21    --  113.25 -86.00 170.86   50
 28  \w     42.00  71.00   0.50    0.21    --  113.25 -61.00  90.00   58
 29  \w     58.00 112.00   0.50    0.21    --  113.25 -77.00  90.00  108
 30  \w     98.00 132.00   0.50    0.21    --  113.25 -77.00 -90.00   68
 31  \w     84.00 111.00   0.50    0.21    --  113.25 -77.00 -60.00   54
 32  \w     53.00  79.00   0.50    0.21    --  113.25 -77.00 -60.00   52
 33  \w     42.00  88.00   0.50    0.21    --  113.25 -77.00 -90.00   92
 34  \w     43.00  75.00   0.50    0.21    --  113.25 -77.00-150.00   64
 35  \w     51.00  80.00   0.50    0.21    --  113.25 -77.00-180.00   58
 36  \w     78.00 125.00   0.50    0.21    --  113.25 -77.00-150.00   94
 37  \w    100.00 135.00   0.50    0.21    --  113.25 -76.00 -41.98   70
 38  \w    105.00 131.00   0.50    0.21    --  113.25 -77.00   0.00   52
 39  \w     42.00  67.00   0.50    0.21    --  113.25 -61.00 -90.00   50
 40  \w     43.00  70.00   0.50    0.21    --  113.25 -61.00 -30.00   54
 41  \w     43.00  69.00   0.50    0.21    --  113.25 -61.00-120.00   52
 42  \w     44.00  70.00   0.50    0.21    --  113.25 -77.00  30.00   52
 43  \w     42.00  71.00   0.50    0.21    --  113.25 -61.00  60.00   58
 44  \w     46.00  73.00   0.50    0.21    --  113.25 -62.00 107.82   54
 45  \w    100.00 171.00   0.50    0.21    --  113.25  15.00  30.00  142
 46  \w    124.00 168.00   0.50    0.21    --  113.25  61.00 150.00   88
 47  \w    118.00 145.00   0.50    0.21    --  113.25  61.00 120.00   54
 48  \w    150.00 178.00   0.50    0.21    --  113.25  61.00 120.00   56
 49  \w    118.00 145.00   0.50    0.21    --  113.25  77.00  60.00   54
 50  \w    108.00 175.00   0.50    0.21    --  113.25  61.00 -60.00  134
 51  \w    120.00 175.00   0.50    0.21    --  113.25  77.00 -90.00  110
 52  \w    107.00 143.00   0.50    0.21    --  113.25  61.00-120.00   72
 53  \w    146.00 175.00   0.50    0.21    --  113.25  77.00-150.00   58
 54  \w    145.00 170.00   0.50    0.21    --  113.25  61.00-120.00   50
 55  \w    105.00 173.00   0.50    0.21    --  113.25  45.00-150.00  136
 56  \w    101.00 135.00   0.50    0.21    --  113.25  30.00-150.00   68
 57  \w    112.00 172.00   0.50    0.21    --  113.25  15.00  60.00  120
 58  \w    103.00 152.00   0.50    0.21    --  113.25  30.00 150.00   98
 59  \w    111.00 137.00   0.50    0.21    --  113.25  61.00  90.00   52
 60  \w    140.00 166.00   0.50    0.21    --  113.25  61.00  90.00   52
 61  \w    106.00 146.00   0.50    0.21    --  113.25  15.00 -90.00   80
 62  \w    122.00 148.00   0.50    0.21    --  113.25  15.00-120.00   52
 63  \w    100.00 140.00   0.50    0.21    --  113.25  15.00 -60.00   80
 64  \w    103.00 178.00   0.50    0.21    --  113.25 111.00  87.37  150
 65  \w    133.00 159.00   0.50    0.21    --  113.25 125.00 150.00   52
 66  \w    126.00 163.00   0.50    0.21    --  113.25 125.00  90.00   74
 67  \w    122.00 154.00   0.50    0.21    --  113.25 125.00   0.00   64
 68  \w    108.00 158.00   0.50    0.21    --  113.25 125.00 -60.00  100
 69  \w    149.00 175.00   0.50    0.21    --  113.25 125.00-120.00   52
 70  \w    119.00 145.00   0.50    0.21    --  113.25 125.00-180.00   52
 71  \w    102.00 128.00   0.50    0.21    --  113.25 125.00-120.00   52
 72  \w    138.00 170.00   0.50    0.21    --  113.25 117.00 120.62   64
 73  \w    -71.00  16.00   0.50    0.05    --  -47.94  77.00   0.00  174
 74  \w    -42.00  25.00   0.50    0.05    --  -47.94  37.00 -90.00  134
 75  \w    -16.00  28.00   0.50    0.05    --  -47.94  19.00 -30.00   88
 76  \w    -42.00  25.00   0.50    0.05    --  -47.94  37.00 150.00  134
 77  \w    -16.00  28.00   0.50    0.05    --  -47.94  19.00 120.00   88
 78  \w    -16.00  28.00   0.50    0.05    --  -47.94  19.00   0.00   88
 79  \w    -16.00  28.00   0.50    0.05    --  -47.94  19.00  30.00   88
 80  \w    -53.00 -20.00   0.50    0.21    --  -91.75  45.00 150.00   66
 81  \w   -163.00 -97.00   0.50    0.21    --  -91.75 -52.00 -87.45  132
;
_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      0.0011411000
_diffrn_orient_matrix_UB_12      -0.1163938000
_diffrn_orient_matrix_UB_13      -0.0142589000
_diffrn_orient_matrix_UB_21      -0.0757053000
_diffrn_orient_matrix_UB_22      -0.0162816000
_diffrn_orient_matrix_UB_23      0.0627251000
_diffrn_orient_matrix_UB_31      -0.1229717000
_diffrn_orient_matrix_UB_32      0.0089150000
_diffrn_orient_matrix_UB_33      -0.0714467000
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51712
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.078
_diffrn_reflns_theta_min         4.144
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.192
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.95a (Rigaku Oxford Diffraction, 2023)
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            'intense red'
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0047(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5064
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0501P)^2^+0.4437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4747
_reflns_number_total             5064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02570a2.cif
_cod_data_source_block           pla23074_refinalized
_cod_depositor_comments
'Adding full bibliography for 7133320--7133330.cif.'
_cod_database_code               7133321
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'K2 O8 C50 H70'
_chemical_oxdiff_usercomment     NJK-07-043
_shelx_estimated_absorpt_t_max   0.721
_shelx_estimated_absorpt_t_min   0.621
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C23-C22 \\sim C26-C25
 with sigma of 0.02
 O5-C22 \\sim O3-C25 \\sim O4-C26 \\sim O4-C23
 with sigma of 0.02
 O3-C21 \\sim O5-C21 \\sim O4-C24
 with sigma of 0.02
3. Others
 Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(O5)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=1-FVAR(1)
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(O3)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=
 Sof(H26A)=Sof(H26B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C18(H18A,H18B), C25(H25A,H25B), C22(H22A,H22B), C26(H26A,
 H26B), C23(H23A,H23B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C10(H10), C12(H12), C7(H7), C9(H9), C8(H8), C15(H15),
 C14(H14), C13(H13)
4.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C21(H21D,H21E,H21F), C21(H21A,H21B,H21C), C20(H20A,H20B,
 H20C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              86033
_shelx_hkl_checksum              1162
_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 1.143
_oxdiff_exptl_absorpt_empirical_full_min 0.906