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_7133328
_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         '0.667(C64 H44 La), 0.667(C16 H40 K O8)'
_chemical_formula_sum            'C53.33 H56 K0.67 La0.67 O5.33'
_chemical_formula_weight         900.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-23 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            3
_cell_length_a                   15.91860(10)
_cell_length_b                   10.15370(10)
_cell_length_c                   21.3582(2)
_cell_measurement_reflns_used    49234
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.2440
_cell_measurement_theta_min      3.3450
_cell_volume                     3445.25(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (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      100.00(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 0.999
_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     -3.00  26.00   0.50    0.15    --  -47.94  19.00  30.00   58
  2  \w    -63.00  24.00   0.50    0.15    --  -47.94  57.00   0.00  174
  3  \w     -9.00  23.00   0.50    0.15    --  -47.94  19.00 120.00   64
  4  \w     -3.00  23.00   0.50    0.15    --  -47.94  19.00  90.00   52
  5  \w     -9.00  24.00   0.50    0.15    --  -47.94  19.00 -30.00   66
  6  \w     -8.00  27.00   0.50    0.15    --  -47.94  19.00-120.00   70
  7  \w    -11.00  24.00   0.50    0.15    --  -47.94  19.00   0.00   70
  8  \w    -25.00   2.00   0.50    0.15    --   47.94 -19.00-120.00   54
  9  \w     36.00 114.00   0.50    0.15    --   47.94  46.00-107.41  156
 10  \w      3.00  78.00   0.50    0.15    --   47.94 -99.00-180.00  150
 11  \w     34.00  88.00   0.50    0.15    --   47.94-125.00 150.00  108
 12  \w    -22.00   5.00   0.50    0.15    --   47.94 -19.00  90.00   54
 13  \w    108.00 160.00   0.50    0.60    --  113.25  45.00 150.00  104
 14  \w    127.00 153.00   0.50    0.60    --  113.25  60.00-178.54   52
 15  \w     64.00 109.00   0.50    0.60    --  113.25-114.00  58.82   90
 16  \w     96.00 140.00   0.50    0.60    --  113.25 -86.00  13.95   88
 17  \w     43.00  71.00   0.50    0.60    --  113.25 -86.00  13.95   56
 18  \w     83.00 108.00   0.50    0.60    --  113.25-106.00  74.58   50
 19  \w     45.00  72.00   0.50    0.60    --  113.25 -98.00-153.19   54
 20  \w     44.00  69.00   0.50    0.60    --  113.25 -61.00 120.00   50
 21  \w     43.00  70.00   0.50    0.60    --  113.25 -61.00 -60.00   54
 22  \w     73.00 111.00   0.50    0.60    --  113.25 -85.00-143.78   76
 23  \w    101.00 145.00   0.50    0.60    --  113.25  30.00 150.00   88
 24  \w    137.00 172.00   0.50    0.60    --  113.25 125.00-150.00   70
 25  \w    106.00 135.00   0.50    0.60    --  113.25 -77.00-150.00   58
 26  \w     45.00  70.00   0.50    0.60    --  113.25 -61.00  60.00   50
 27  \w    129.00 168.00   0.50    0.60    --  113.25  15.00 -90.00   78
 28  \w    134.00 160.00   0.50    0.60    --  113.25  45.00 -60.00   52
 29  \w    109.00 135.00   0.50    0.60    --  113.25  44.00 171.34   52
 30  \w    108.00 149.00   0.50    0.60    --  113.25  45.00   0.00   82
 31  \w    140.00 166.00   0.50    0.60    --  113.25 125.00 120.00   52
 32  \w     80.00 106.00   0.50    0.60    --  113.25 -94.00 -90.00   52
 33  \w     66.00  92.00   0.50    0.60    --  113.25 -70.00  91.48   52
 34  \w     49.00  78.00   0.50    0.60    --  113.25-106.00  74.58   58
 35  \w    107.00 165.00   0.50    0.60    --  113.25  61.00 -90.00  116
 36  \w     46.00  86.00   0.50    0.60    --  113.25-125.00 120.00   80
 37  \w    122.00 167.00   0.50    0.60    --  113.25  15.00-150.00   90
 38  \w    141.00 172.00   0.50    0.60    --  113.25 125.00 -90.00   62
 39  \w     98.00 124.00   0.50    0.60    --  113.25 125.00 -30.00   52
 40  \w     96.00 132.00   0.50    0.60    --  113.25 125.00 120.00   72
 41  \w     93.00 127.00   0.50    0.60    --  113.25 -77.00 -60.00   68
 42  \w     44.00  69.00   0.50    0.60    --  113.25 -94.00 150.00   50
 43  \w     42.00  67.00   0.50    0.60    --  113.25 -61.00-180.00   50
 44  \w     51.00  94.00   0.50    0.60    --  113.25-125.00 -30.00   86
 45  \w    112.00 138.00   0.50    0.60    --  113.25  77.00   0.00   52
 46  \w    141.00 167.00   0.50    0.60    --  113.25  77.00   0.00   52
 47  \w    153.00 178.00   0.50    0.60    --  113.25 125.00-180.00   50
 48  \w     95.00 121.00   0.50    0.60    --  113.25 125.00-150.00   52
 49  \w     97.00 157.00   0.50    0.60    --  113.25 125.00  60.00  120
 50  \w     59.00  85.00   0.50    0.60    --  113.25 -77.00-150.00   52
 51  \w    102.00 156.00   0.50    0.60    --  113.25  30.00  60.00  108
 52  \w     44.00  70.00   0.50    0.60    --  113.25 -61.00 150.00   52
 53  \w    100.00 150.00   0.50    0.60    --  113.25  15.00-120.00  100
 54  \w     47.00 103.00   0.50    0.60    --  113.25 -94.00 -30.00  112
 55  \w     43.00  68.00   0.50    0.60    --  113.25 -77.00 -30.00   50
 56  \w    110.00 135.00   0.50    0.60    --  113.25 -77.00 -30.00   50
 57  \w    106.00 167.00   0.50    0.60    --  113.25  61.00 120.00  122
 58  \w    102.00 137.00   0.50    0.60    --  113.25  45.00  90.00   70
 59  \w    107.00 135.00   0.50    0.60    --  113.25 -75.00 174.23   56
 60  \w     44.00  70.00   0.50    0.60    --  113.25 -61.00-150.00   52
 61  \w     54.00 100.00   0.50    0.60    --  113.25 -94.00-180.00   92
 62  \w     43.00  68.00   0.50    0.60    --  113.25 -94.00 120.00   50
 63  \w    110.00 135.00   0.50    0.60    --  113.25  77.00-120.00   50
 64  \w     43.00  68.00   0.50    0.60    --  113.25 -61.00  30.00   50
 65  \w     76.00 101.00   0.50    0.60    --  113.25 -94.00  30.00   50
 66  \w     42.00  70.00   0.50    0.60    --  113.25 -94.00  30.00   56
 67  \w     59.00  85.00   0.50    0.60    --  113.25-125.00   0.00   52
 68  \w    143.00 174.00   0.50    0.60    --  113.25  77.00-120.00   62
 69  \w     57.00  83.00   0.50    0.60    --  113.25 -82.00  43.78   52
 70  \w     97.00 131.00   0.50    0.60    --  113.25 -82.00  43.78   68
 71  \w    106.00 133.00   0.50    0.60    --  113.25  30.00 -30.00   54
 72  \w    139.00 172.00   0.50    0.60    --  113.25  30.00 -30.00   66
 73  \w     65.00 116.00   0.50    0.60    --  113.25 -77.00  90.00  102
 74  \w     51.00  76.00   0.50    0.60    --  113.25 -94.00-120.00   50
 75  \w     42.00  97.00   0.50    0.60    --  113.25 -94.00   0.00  110
 76  \w    143.00 176.00   0.50    0.60    --  113.25  77.00  90.00   66
 77  \w    142.00 176.00   0.50    0.60    --  113.25  77.00 120.00   68
 78  \w    111.00 137.00   0.50    0.60    --  113.25  45.00 -90.00   52
 79  \w    136.00 178.00   0.50    0.60    --  113.25  61.00  30.00   84
 80  \w    136.00 174.00   0.50    0.60    --  113.25 125.00 -30.00   76
 81  \w     50.00  75.00   0.50    0.60    --  113.25 -77.00-120.00   50
 82  \w    105.00 131.00   0.50    0.60    --  113.25 -77.00-120.00   52
 83  \w     81.00 106.00   0.50    0.60    --  113.25 -94.00 120.00   50
 84  \w     78.00 104.00   0.50    0.60    --  113.25 -94.00  60.00   52
 85  \w    103.00 165.00   0.50    0.60    --  113.25  30.00  90.00  124
 86  \w     85.00 111.00   0.50    0.60    --  113.25-125.00 -90.00   52
 87  \w     73.00  99.00   0.50    0.60    --  113.25-125.00 -60.00   52
 88  \w     84.00 110.00   0.50    0.60    --  113.25-125.00  60.00   52
 89  \w    111.00 136.00   0.50    0.60    --  113.25  77.00-150.00   50
 90  \w    117.00 143.00   0.50    0.60    --  113.25  77.00 -60.00   52
 91  \w    144.00 170.00   0.50    0.60    --  113.25  61.00-180.00   52
 92  \w    134.00 160.00   0.50    0.60    --  113.25  61.00 -60.00   52
 93  \w    147.00 172.00   0.50    0.60    --  113.25  15.00-180.00   50
 94  \w    103.00 128.00   0.50    0.60    --  113.25  30.00-180.00   50
 95  \w     57.00  83.00   0.50    0.60    --  113.25 -75.00 174.23   52
 96  \w     81.00 106.00   0.50    0.60    --  113.25 -98.00-153.19   50
 97  \w    134.00 167.00   0.50    0.60    --  113.25 125.00 -60.00   66
 98  \w    132.00 159.00   0.50    0.60    --  113.25 125.00  30.00   54
 99  \w     81.00 106.00   0.50    0.60    --  113.25 -98.00-121.72   50
100  \w    110.00 135.00   0.50    0.60    --  113.25 -77.00-180.00   50
101  \w    110.00 136.00   0.50    0.60    --  113.25 -77.00 150.00   52
102  \w     44.00  75.00   0.50    0.60    --  113.25 -98.00-121.72   62
;
_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      -0.0914253000
_diffrn_orient_matrix_UB_12      0.0150427000
_diffrn_orient_matrix_UB_13      0.0187650000
_diffrn_orient_matrix_UB_21      0.0300706000
_diffrn_orient_matrix_UB_22      -0.0152408000
_diffrn_orient_matrix_UB_23      0.0695665000
_diffrn_orient_matrix_UB_31      0.0121691000
_diffrn_orient_matrix_UB_32      0.1502163000
_diffrn_orient_matrix_UB_33      0.0051841000
_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  0.0571
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            80267
_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         79.956
_diffrn_reflns_theta_min         3.363
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.769
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (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            'light orange'
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0462P)^2^+1.7685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7245
_reflns_number_total             7503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02570a2.cif
_cod_data_source_block           pla23116_refinalized
_cod_depositor_comments
'Adding full bibliography for 7133320--7133330.cif.'
_cod_database_code               7133328
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'La K O8 C64 H60'
_chemical_oxdiff_usercomment     NJK-07-091
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.377
_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.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C34(H34A,H34B), C38(H38A,H38B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C16(H16), C2(H2), C5(H5), C20(H20), C28(H28), C26(H26), C10(H10),
 C22(H22), C17(H17), C31(H31), C19(H19), C25(H25), C23(H23), C14(H14), C29(H29),
  C24(H24), C30(H30), C11(H11), C18(H18), C13(H13), C12(H12)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              47750
_shelx_hkl_checksum              3196
_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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.821