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_7133324
_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 Ce, C16 H40 K O8'
_chemical_formula_sum            'C80 H84 Ce K O8'
_chemical_formula_weight         1352.69
_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             2023-09-14
_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                 94.0560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.84690(10)
_cell_length_b                   10.17870(10)
_cell_length_c                   21.4308(2)
_cell_measurement_reflns_used    44064
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      79.5520
_cell_measurement_theta_min      3.3650
_cell_volume                     3448.15(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.99a (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 0.998
_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    -56.00  25.00   0.50    1.47    --  -47.94  57.00 -90.00  162
  2  \w     -2.00  26.00   0.50    1.47    --  -47.94  19.00 -90.00   56
  3  \w    -63.00  25.00   0.50    1.47    --  -47.94  57.00  30.00  176
  4  \w   -118.00 -86.00   0.50    1.47    --  -47.94 -46.00-156.31   64
  5  \w    -62.00 -36.00   0.50    1.47    --  -47.94 -46.00-156.31   52
  6  \w    -16.00  19.00   0.50    1.47    --  -47.94  19.00 -30.00   70
  7  \w    -16.00  24.00   0.50    1.47    --  -47.94  19.00-180.00   80
  8  \w    -81.00 -33.00   0.50    1.47    --  -47.94 125.00  90.00   96
  9  \w    -85.00 -37.00   0.50    1.47    --  -47.94 -41.00 -95.88   96
 10  \w   -120.00 -94.00   0.50    1.47    --  -47.94 -41.00 -95.88   52
 11  \w    -26.00  -1.00   0.50    1.47    --   47.94 -19.00 -30.00   50
 12  \w     46.00  86.00   0.50    1.47    --   47.94-125.00 150.00   80
 13  \w   -139.00-106.00   0.50    5.89    --  -91.75 -61.00-150.00   66
 14  \w   -108.00 -80.00   0.50    5.89    --  -91.75 -45.00 -60.00   56
 15  \w    111.00 172.00   0.50    5.89    --  113.25  77.00  60.00  122
 16  \w     56.00  94.00   0.50    5.89    --  113.25 -94.00  60.00   76
 17  \w     83.00 111.00   0.50    5.89    --  113.25 -82.00  51.08   56
 18  \w    150.00 175.00   0.50    5.89    --  113.25  77.00 150.00   50
 19  \w    104.00 129.00   0.50    5.89    --  113.25  15.00  30.00   50
 20  \w    146.00 178.00   0.50    5.89    --  113.25 103.00-165.77   64
 21  \w     48.00 107.00   0.50    5.89    --  113.25-105.00 -84.56  118
 22  \w    102.00 136.00   0.50    5.89    --  113.25  30.00  30.00   68
 23  \w    132.00 158.00   0.50    5.89    --  113.25  15.00  30.00   52
 24  \w     42.00  74.00   0.50    5.89    --  113.25 -94.00 -60.00   64
 25  \w     79.00 106.00   0.50    5.89    --  113.25 -94.00 -60.00   54
 26  \w    127.00 165.00   0.50    5.89    --  113.25 125.00 -90.00   76
 27  \w     43.00  71.00   0.50    5.89    --  113.25 -77.00-180.00   56
 28  \w    103.00 129.00   0.50    5.89    --  113.25 -77.00-180.00   52
 29  \w     42.00  67.00   0.50    5.89    --  113.25 -61.00 -60.00   50
 30  \w     85.00 111.00   0.50    5.89    --  113.25-125.00 -30.00   52
 31  \w     42.00 104.00   0.50    5.89    --  113.25 -94.00-120.00  124
 32  \w     43.00  68.00   0.50    5.89    --  113.25 -61.00   0.00   50
 33  \w    134.00 163.00   0.50    5.89    --  113.25  15.00-120.00   58
 34  \w     48.00  84.00   0.50    5.89    --  113.25-125.00 -60.00   72
 35  \w     71.00 106.00   0.50    5.89    --  113.25 -94.00-180.00   70
 36  \w    109.00 139.00   0.50    5.89    --  113.25 -86.00  94.10   60
 37  \w     42.00  67.00   0.50    5.89    --  113.25 -94.00-180.00   50
 38  \w    111.00 141.00   0.50    5.89    --  113.25  77.00-180.00   60
 39  \w    110.00 139.00   0.50    5.89    --  113.25  77.00-120.00   58
 40  \w    114.00 139.00   0.50    5.89    --  113.25  61.00-180.00   50
 41  \w    101.00 166.00   0.50    5.89    --  113.25  45.00  60.00  130
 42  \w    123.00 149.00   0.50    5.89    --  113.25  30.00 150.00   52
 43  \w     49.00 106.00   0.50    5.89    --  113.25 -94.00  90.00  114
 44  \w     56.00  82.00   0.50    5.89    --  113.25 -77.00 -60.00   52
 45  \w    120.00 168.00   0.50    5.89    --  113.25  77.00 -90.00   96
 46  \w     91.00 131.00   0.50    5.89    --  113.25 -77.00  60.00   80
 47  \w    148.00 174.00   0.50    5.89    --  113.25  30.00  30.00   52
 48  \w     42.00  70.00   0.50    5.89    --  113.25 -61.00-150.00   56
 49  \w     81.00 106.00   0.50    5.89    --  113.25 -94.00  30.00   50
 50  \w     43.00  68.00   0.50    5.89    --  113.25 -77.00 -90.00   50
 51  \w    100.00 126.00   0.50    5.89    --  113.25 -77.00 -90.00   52
 52  \w     43.00  73.00   0.50    5.89    --  113.25 -77.00 -30.00   60
 53  \w     92.00 121.00   0.50    5.89    --  113.25 -77.00 -30.00   58
 54  \w     76.00 106.00   0.50    5.89    --  113.25 -94.00 150.00   60
 55  \w    105.00 145.00   0.50    5.89    --  113.25  45.00-120.00   80
 56  \w     42.00  71.00   0.50    5.89    --  113.25 -61.00  90.00   58
 57  \w    141.00 167.00   0.50    5.89    --  113.25 125.00-120.00   52
 58  \w    145.00 177.00   0.50    5.89    --  113.25  77.00-150.00   64
 59  \w    123.00 157.00   0.50    5.89    --  113.25  45.00 -30.00   68
 60  \w     53.00 110.00   0.50    5.89    --  113.25-125.00 120.00  114
 61  \w     46.00  73.00   0.50    5.89    --  113.25 -77.00   0.00   54
 62  \w     42.00  67.00   0.50    5.89    --  113.25 -61.00 150.00   50
 63  \w     44.00  85.00   0.50    5.89    --  113.25-125.00 150.00   82
 64  \w     98.00 123.00   0.50    5.89    --  113.25 125.00-150.00   50
 65  \w    103.00 159.00   0.50    5.89    --  113.25  45.00 150.00  112
 66  \w    108.00 134.00   0.50    5.89    --  113.25  61.00  30.00   52
 67  \w     64.00 105.00   0.50    5.89    --  113.25 -94.00   0.00   82
 68  \w    135.00 161.00   0.50    5.89    --  113.25 125.00-150.00   52
 69  \w    102.00 170.00   0.50    5.89    --  113.25 125.00   0.00  136
 70  \w    102.00 151.00   0.50    5.89    --  113.25  15.00 -30.00   98
 71  \w    110.00 160.00   0.50    5.89    --  113.25  77.00 -30.00  100
 72  \w    142.00 168.00   0.50    5.89    --  113.25  30.00  90.00   52
 73  \w     95.00 121.00   0.50    5.89    --  113.25 125.00 -30.00   52
 74  \w    153.00 178.00   0.50    5.89    --  113.25  61.00   0.00   50
 75  \w     55.00  94.00   0.50    5.89    --  113.25 -94.00-150.00   78
 76  \w     46.00  77.00   0.50    5.89    --  113.25 -94.00 -30.00   62
 77  \w     50.00  82.00   0.50    5.89    --  113.25-125.00-150.00   64
 78  \w    107.00 144.00   0.50    5.89    --  113.25  61.00   0.00   74
 79  \w     55.00  80.00   0.50    5.89    --  113.25 -77.00  30.00   50
 80  \w     42.00  67.00   0.50    5.89    --  113.25 -61.00 -30.00   50
 81  \w    113.00 139.00   0.50    5.89    --  113.25  99.00 -32.56   52
 82  \w     45.00  71.00   0.50    5.89    --  113.25 -61.00 120.00   52
 83  \w    127.00 153.00   0.50    5.89    --  113.25  61.00-120.00   52
 84  \w    103.00 148.00   0.50    5.89    --  113.25  45.00 120.00   90
 85  \w    108.00 152.00   0.50    5.89    --  113.25  30.00 -30.00   88
 86  \w     50.00  76.00   0.50    5.89    --  113.25 -86.00  94.10   52
 87  \w    100.00 125.00   0.50    5.89    --  113.25 125.00  60.00   50
 88  \w    141.00 167.00   0.50    5.89    --  113.25 125.00  60.00   52
 89  \w     65.00  91.00   0.50    5.89    --  113.25 -77.00-150.00   52
 90  \w     73.00 106.00   0.50    5.89    --  113.25 -99.00 -20.49   66
 91  \w    108.00 133.00   0.50    5.89    --  113.25 -77.00  90.00   50
 92  \w     51.00  76.00   0.50    5.89    --  113.25 -77.00 120.00   50
 93  \w     68.00 106.00   0.50    5.89    --  113.25 -97.00 131.03   76
;
_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      0.0877284000
_diffrn_orient_matrix_UB_12      -0.0471973000
_diffrn_orient_matrix_UB_13      0.0263925000
_diffrn_orient_matrix_UB_21      0.0241870000
_diffrn_orient_matrix_UB_22      -0.0308767000
_diffrn_orient_matrix_UB_23      -0.0668321000
_diffrn_orient_matrix_UB_31      0.0347754000
_diffrn_orient_matrix_UB_32      0.1404739000
_diffrn_orient_matrix_UB_33      -0.0057747000
_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  0.0666
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_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            75093
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.960
_diffrn_reflns_theta_min         3.358
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.077
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.342
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.99a (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            gold
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       needle
_exptl_crystal_F_000             1410
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0271P)^2^+4.3944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7284
_reflns_number_total             7501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02570a2.cif
_cod_data_source_block           pla23085_refinalized
_cod_depositor_comments
'Adding full bibliography for 7133320--7133330.cif.'
_cod_database_code               7133324
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ce K O8 C96 H144'
_chemical_oxdiff_usercomment     'NJK-07-051 from DME'
_shelx_estimated_absorpt_t_max   0.839
_shelx_estimated_absorpt_t_min   0.121
_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:
 C34(H34A,H34B), C35(H35A,H35B), C39(H39A,H39B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C5(H5), C2(H2), C22(H22), C20(H20), C11(H11), C26(H26), C14(H14),
 C28(H28), C23(H23), C19(H19), C32(H32), C13(H13), C16(H16), C25(H25), C31(H31),
  C24(H24), C17(H17), C29(H29), C30(H30), C18(H18), C12(H12)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C)
;
_shelx_res_checksum              47341
_shelx_hkl_checksum              9620
_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 1.485
_oxdiff_exptl_absorpt_empirical_full_min 0.741