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_7133325
_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         'C64 H44 Tb, C16 H40 K O8'
_chemical_formula_sum            'C80 H84 K O8 Tb'
_chemical_formula_weight         1371.49
_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             2023-09-23
_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                 94.6430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.62410(10)
_cell_length_b                   10.22140(10)
_cell_length_c                   21.5624(2)
_cell_measurement_reflns_used    48670
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      79.2060
_cell_measurement_theta_min      3.3590
_cell_volume                     3432.22(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(11)
_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 0.996
_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    -76.00 -44.00   0.50    1.04    --  -47.94 103.00-139.00   64
  2  \w    -37.00   4.00   0.50    1.04    --  -47.94 103.00-139.00   82
  3  \w    -73.00 -47.00   0.50    4.14    --  -91.75 103.00-139.00   52
  4  \w    118.00 143.00   0.50    4.14    --  113.25 103.00-139.00   50
  5  \w     81.00 107.00   0.50    4.14    --  113.25-103.00 118.00   52
  6  \w     43.00  72.00   0.50    4.14    --  113.25-103.00 118.00   58
  7  \w    -18.00   8.00   0.50    1.04    --   10.00  88.00  46.51   52
  8  \w    -14.00  12.00   0.50    1.04    --   10.00  80.00 165.83   52
  9  \w    -16.00   9.00   0.50    1.04    --   10.00  84.00  92.75   50
 10  \w    -17.00   8.00   0.50    1.04    --   10.00  86.00 -49.47   50
 11  \w     -1.00  24.00   0.50    1.04    --   18.00  67.00-114.64   50
 12  \w      6.00  31.00   0.50    1.04    --   22.00  61.00 -72.88   50
 13  \w     13.00  40.00   0.50    1.04    --   26.00  55.00  -7.68   54
 14  \w     17.00  42.00   0.50    1.04    --   30.00  55.00-144.27   50
 15  \w     18.00  44.00   0.50    1.04    --   30.00  53.00-108.01   52
 16  \w    -55.00 -29.00   0.50    1.04    --  -42.00 -49.00  87.36   52
 17  \w    -10.00  27.00   0.50    1.04    --  -47.94  19.00   0.00   74
 18  \w     -8.00  23.00   0.50    1.04    --  -47.94  19.00 120.00   62
 19  \w    -16.00  25.00   0.50    1.04    --  -47.94  19.00-120.00   82
 20  \w    -22.00   7.00   0.50    1.04    --   47.94 -19.00-180.00   58
 21  \w    -21.00  34.00   0.50    1.04    --   47.94 -37.00-150.00  110
 22  \w     20.00  80.00   0.50    1.04    --   47.94-103.00 118.00  120
 23  \w   -159.00-126.00   0.50    4.14    --  -91.75 -61.00-150.00   66
 24  \w   -163.00-112.00   0.50    4.14    --  -91.75 -77.00 -30.00  102
 25  \w   -157.00-118.00   0.50    4.14    --  -91.75 -61.00-120.00   78
 26  \w    -51.00 -21.00   0.50    4.14    --  -91.75  45.00   0.00   60
 27  \w   -147.00-122.00   0.50    4.14    --  -91.75-103.00 118.00   50
 28  \w    -51.00 -26.00   0.50    4.14    --  -91.75  45.00-180.00   50
 29  \w     81.00 106.00   0.50    4.14    --  113.25 -94.00 -30.00   50
 30  \w    149.00 175.00   0.50    4.14    --  113.25  61.00 -90.00   52
 31  \w     42.00  67.00   0.50    4.14    --  113.25 -61.00 -90.00   50
 32  \w     45.00 110.00   0.50    4.14    --  113.25-125.00 120.00  130
 33  \w     45.00  70.00   0.50    4.14    --  113.25 -61.00-150.00   50
 34  \w     42.00  75.00   0.50    4.14    --  113.25 -94.00 -30.00   66
 35  \w     44.00  70.00   0.50    4.14    --  113.25 -77.00 -30.00   52
 36  \w    108.00 133.00   0.50    4.14    --  113.25  30.00  30.00   50
 37  \w    102.00 149.00   0.50    4.14    --  113.25 125.00 -90.00   94
 38  \w    109.00 146.00   0.50    4.14    --  113.25  61.00 -90.00   74
 39  \w    137.00 163.00   0.50    4.14    --  113.25  15.00   0.00   52
 40  \w    111.00 137.00   0.50    4.14    --  113.25  77.00 -90.00   52
 41  \w     68.00 108.00   0.50    4.14    --  113.25-125.00  90.00   80
 42  \w     96.00 131.00   0.50    4.14    --  113.25 125.00 -30.00   70
 43  \w    102.00 132.00   0.50    4.14    --  113.25  15.00   0.00   60
 44  \w     88.00 114.00   0.50    4.14    --  113.25 -79.00 142.85   52
 45  \w     58.00  84.00   0.50    4.14    --  113.25-125.00-150.00   52
 46  \w     44.00  69.00   0.50    4.14    --  113.25 -61.00  30.00   50
 47  \w     63.00 108.00   0.50    4.14    --  113.25-125.00-180.00   90
 48  \w     74.00 105.00   0.50    4.14    --  113.25 -94.00   0.00   62
 49  \w    140.00 166.00   0.50    4.14    --  113.25 125.00-180.00   52
 50  \w    139.00 165.00   0.50    4.14    --  113.25  30.00 -90.00   52
 51  \w     61.00  91.00   0.50    4.14    --  113.25 -94.00 120.00   60
 52  \w    134.00 167.00   0.50    4.14    --  113.25  15.00 120.00   66
 53  \w     42.00  67.00   0.50    4.14    --  113.25 -61.00 -60.00   50
 54  \w    145.00 170.00   0.50    4.14    --  113.25 125.00 -30.00   50
 55  \w     47.00  75.00   0.50    4.14    --  113.25 -94.00 -60.00   56
 56  \w     79.00 106.00   0.50    4.14    --  113.25 -94.00 -60.00   54
 57  \w     44.00  69.00   0.50    4.14    --  113.25 -77.00 150.00   50
 58  \w     45.00  71.00   0.50    4.14    --  113.25 -94.00   0.00   52
 59  \w    128.00 177.00   0.50    4.14    --  113.25  77.00 120.00   98
 60  \w     50.00  75.00   0.50    4.14    --  113.25 -77.00  30.00   50
 61  \w    101.00 133.00   0.50    4.14    --  113.25 -77.00  30.00   64
 62  \w     56.00 106.00   0.50    4.14    --  113.25-125.00  30.00  100
 63  \w    131.00 171.00   0.50    4.14    --  113.25 125.00 -60.00   80
 64  \w     45.00  70.00   0.50    4.14    --  113.25 -61.00-120.00   50
 65  \w     66.00 118.00   0.50    4.14    --  113.25 -83.00-141.43  104
 66  \w     76.00 102.00   0.50    4.14    --  113.25 -77.00 -30.00   52
 67  \w    102.00 144.00   0.50    4.14    --  113.25  45.00  30.00   84
 68  \w     95.00 161.00   0.50    4.14    --  113.25 125.00  60.00  132
 69  \w     44.00  69.00   0.50    4.14    --  113.25 -61.00   0.00   50
 70  \w    148.00 173.00   0.50    4.14    --  113.25  30.00-150.00   50
 71  \w     65.00 105.00   0.50    4.14    --  113.25 -94.00 -90.00   80
 72  \w    122.00 172.00   0.50    4.14    --  113.25  77.00  30.00  100
 73  \w    121.00 146.00   0.50    4.14    --  113.25  45.00 -60.00   50
 74  \w    141.00 167.00   0.50    4.14    --  113.25  61.00 150.00   52
 75  \w    109.00 134.00   0.50    4.14    --  113.25  61.00 150.00   50
 76  \w     44.00  71.00   0.50    4.14    --  113.25 -61.00  90.00   54
 77  \w     43.00  70.00   0.50    4.14    --  113.25 -61.00 120.00   54
 78  \w    135.00 172.00   0.50    4.14    --  113.25  61.00   0.00   74
 79  \w     64.00  90.00   0.50    4.14    --  113.25 -77.00 120.00   52
 80  \w    103.00 132.00   0.50    4.14    --  113.25 -77.00 120.00   58
 81  \w    102.00 143.00   0.50    4.14    --  113.25  45.00  60.00   82
 82  \w    109.00 138.00   0.50    4.14    --  113.25  30.00-150.00   58
 83  \w    110.00 141.00   0.50    4.14    --  113.25  61.00-120.00   62
 84  \w     50.00  76.00   0.50    4.14    --  113.25 -94.00  90.00   52
 85  \w     80.00 106.00   0.50    4.14    --  113.25 -94.00 150.00   52
 86  \w     42.00  68.00   0.50    4.14    --  113.25 -94.00 150.00   52
 87  \w    104.00 130.00   0.50    4.14    --  113.25  30.00 120.00   52
 88  \w    147.00 173.00   0.50    4.14    --  113.25  30.00 120.00   52
 89  \w     53.00 106.00   0.50    4.14    --  113.25 -94.00-150.00  106
 90  \w     96.00 158.00   0.50    4.14    --  113.25 125.00 120.00  124
 91  \w     56.00  82.00   0.50    4.14    --  113.25 -94.00-120.00   52
 92  \w    111.00 174.00   0.50    4.14    --  113.25  77.00-120.00  126
 93  \w    141.00 167.00   0.50    4.14    --  113.25  61.00-180.00   52
 94  \w    106.00 178.00   0.50    4.14    --  113.25  61.00  60.00  144
 95  \w     58.00 101.00   0.50    4.14    --  113.25 -94.00  30.00   86
 96  \w     95.00 122.00   0.50    4.14    --  113.25 -77.00-120.00   54
 97  \w     81.00 106.00   0.50    4.14    --  113.25 -94.00  60.00   50
 98  \w    102.00 131.00   0.50    4.14    --  113.25  45.00 -30.00   58
 99  \w     67.00  93.00   0.50    4.14    --  113.25-125.00-120.00   52
100  \w     80.00 110.00   0.50    4.14    --  113.25-125.00   0.00   60
101  \w     42.00  70.00   0.50    4.14    --  113.25 -61.00-180.00   56
102  \w    147.00 176.00   0.50    4.14    --  113.25  30.00  30.00   58
103  \w    109.00 146.00   0.50    4.14    --  113.25  61.00-150.00   74
104  \w    133.00 170.00   0.50    4.14    --  113.25  15.00-180.00   74
105  \w    131.00 157.00   0.50    4.14    --  113.25  15.00  90.00   52
106  \w    115.00 141.00   0.50    4.14    --  113.25  45.00-120.00   52
107  \w    108.00 134.00   0.50    4.14    --  113.25  30.00-120.00   52
108  \w    134.00 160.00   0.50    4.14    --  113.25  30.00 150.00   52
109  \w     44.00  70.00   0.50    4.14    --  113.25 -61.00 150.00   52
110  \w    100.00 135.00   0.50    4.14    --  113.25 -76.00 -33.43   70
111  \w     42.00  68.00   0.50    4.14    --  113.25 -61.00 -30.00   52
;
_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      0.0271346000
_diffrn_orient_matrix_UB_12      -0.0393642000
_diffrn_orient_matrix_UB_13      0.0676906000
_diffrn_orient_matrix_UB_21      0.0951044000
_diffrn_orient_matrix_UB_22      0.0159536000
_diffrn_orient_matrix_UB_23      -0.0126746000
_diffrn_orient_matrix_UB_31      -0.0031014000
_diffrn_orient_matrix_UB_32      0.1446083000
_diffrn_orient_matrix_UB_33      0.0198260000
_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  0.0700
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            82493
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.191
_diffrn_reflns_theta_min         3.367
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.047
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.676
_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_density_diffrn    1.327
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0386P)^2^+3.4342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7273
_reflns_number_total             7466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02570a2.cif
_cod_data_source_block           pla23115_refinalized
_cod_depositor_comments
'Adding full bibliography for 7133320--7133330.cif.'
_cod_database_code               7133325
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Tb C80 H64 K O8'
_chemical_oxdiff_usercomment     NJK-07-073
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.393
_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), C39(H39A,H39B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C2(H2), C32(H32), C26(H26), C5(H5), C22(H22), C28(H28), C16(H16),
 C10(H10), C11(H11), C23(H23), C31(H31), C25(H25), C19(H19), C24(H24), C14(H14),
  C17(H17), C18(H18), C29(H29), C13(H13), C30(H30), C12(H12)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C36(H36A,H36B,H36C), C33(H33A,H33B,H33C), C37(H37A,H37B,
 H37C)
;
_shelx_res_checksum              90327
_shelx_hkl_checksum              21879
_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 3.663
_oxdiff_exptl_absorpt_empirical_full_min 0.545