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_7133322
_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 Na2 O8'
_chemical_formula_sum            'C48 H62 Na2 O8'
_chemical_formula_weight         812.95
_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                 105.1460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.09130(10)
_cell_length_b                   13.28180(10)
_cell_length_c                   15.83920(10)
_cell_measurement_reflns_used    25128
_cell_measurement_temperature    199.98(10)
_cell_measurement_theta_max      79.6870
_cell_measurement_theta_min      4.3640
_cell_volume                     2252.26(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      199.98(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 0.998
_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    -42.00  25.00   0.50    0.29    --  -47.94  37.00-180.00  134
  2  \w   -120.00 -35.00   0.50    0.29    --  -47.94 -45.00  49.78  170
  3  \w   -120.00 -35.00   0.50    0.29    --  -47.94 -44.00 106.08  170
  4  \w    -71.00  16.00   0.50    0.29    --  -47.94  77.00-150.00  174
  5  \w    -71.00  16.00   0.50    0.29    --  -47.94  77.00  60.00  174
  6  \w    -42.00  25.00   0.50    0.29    --  -47.94  37.00  90.00  134
  7  \w     34.00  94.00   0.50    0.29    --   47.94-125.00 -30.00  120
  8  \w   -163.00-110.00   0.50    1.15    --  -91.75 -77.00-120.00  106
  9  \w    -85.00 -22.00   0.50    1.15    --  -91.75 125.00 -60.00  126
 10  \w   -154.00-122.00   0.50    1.15    --  -91.75 -48.00 118.65   64
 11  \w    -47.00 -21.00   0.50    1.15    --  -91.75  45.00 -90.00   52
 12  \w     80.00 109.00   0.50    1.15    --  113.25-125.00-150.00   58
 13  \w     42.00  67.00   0.50    1.15    --  113.25 -61.00  30.00   50
 14  \w    104.00 139.00   0.50    1.15    --  113.25  55.00-173.94   70
 15  \w    107.00 141.00   0.50    1.15    --  113.25  39.00 -52.54   68
 16  \w    107.00 172.00   0.50    1.15    --  113.25  61.00 150.00  130
 17  \w     59.00 111.00   0.50    1.15    --  113.25-125.00  60.00  104
 18  \w     85.00 111.00   0.50    1.15    --  113.25 -86.00-168.33   52
 19  \w     46.00  71.00   0.50    1.15    --  113.25 -61.00 -90.00   50
 20  \w    103.00 146.00   0.50    1.15    --  113.25  45.00-120.00   86
 21  \w     42.00  71.00   0.50    1.15    --  113.25 -61.00-180.00   58
 22  \w    102.00 174.00   0.50    1.15    --  113.25  36.00 176.66  144
 23  \w     44.00  69.00   0.50    1.15    --  113.25 -61.00 -30.00   50
 24  \w    142.00 169.00   0.50    1.15    --  113.25  30.00 -90.00   54
 25  \w     81.00 106.00   0.50    1.15    --  113.25 -94.00 -90.00   50
 26  \w     59.00  85.00   0.50    1.15    --  113.25-125.00 150.00   52
 27  \w     47.00  72.00   0.50    1.15    --  113.25-125.00 -30.00   50
 28  \w     42.00  70.00   0.50    1.15    --  113.25 -61.00   0.00   56
 29  \w     99.00 138.00   0.50    1.15    --  113.25 125.00   0.00   78
 30  \w    149.00 175.00   0.50    1.15    --  113.25 125.00   0.00   52
 31  \w    144.00 169.00   0.50    1.15    --  113.25  61.00 -60.00   50
 32  \w     61.00 105.00   0.50    1.15    --  113.25 -94.00-120.00   88
 33  \w     77.00 103.00   0.50    1.15    --  113.25-125.00 120.00   52
 34  \w    108.00 134.00   0.50    1.15    --  113.25 125.00-120.00   52
 35  \w     46.00  74.00   0.50    1.15    --  113.25-125.00 120.00   56
 36  \w     77.00 106.00   0.50    1.15    --  113.25 -94.00 -60.00   58
 37  \w     42.00  67.00   0.50    1.15    --  113.25 -77.00  90.00   50
 38  \w    153.00 178.00   0.50    1.15    --  113.25 125.00-120.00   50
 39  \w    106.00 132.00   0.50    1.15    --  113.25  61.00 -30.00   52
 40  \w     49.00  75.00   0.50    1.15    --  113.25 -94.00  30.00   52
 41  \w     78.00 106.00   0.50    1.15    --  113.25 -94.00  30.00   56
 42  \w    114.00 145.00   0.50    1.15    --  113.25  77.00-180.00   62
 43  \w    151.00 178.00   0.50    1.15    --  113.25  77.00-180.00   54
 44  \w     42.00  79.00   0.50    1.15    --  113.25 -94.00 150.00   74
 45  \w     63.00 113.00   0.50    1.15    --  113.25 -77.00  60.00  100
 46  \w     43.00  74.00   0.50    1.15    --  113.25 -94.00 -60.00   62
 47  \w     58.00 103.00   0.50    1.15    --  113.25 -94.00  60.00   90
 48  \w     42.00 105.00   0.50    1.15    --  113.25 -94.00-150.00  126
 49  \w     58.00 110.00   0.50    1.15    --  113.25-125.00   0.00  104
 50  \w    122.00 162.00   0.50    1.15    --  113.25  77.00-120.00   80
 51  \w     43.00  69.00   0.50    1.15    --  113.25 -77.00  30.00   52
 52  \w    111.00 136.00   0.50    1.15    --  113.25 -77.00  30.00   50
 53  \w    120.00 146.00   0.50    1.15    --  113.25 125.00 120.00   52
 54  \w    104.00 132.00   0.50    1.15    --  113.25  30.00  90.00   56
 55  \w     77.00 105.00   0.50    1.15    --  113.25 -94.00 -30.00   56
 56  \w     42.00  70.00   0.50    1.15    --  113.25 -61.00-120.00   56
 57  \w     61.00 103.00   0.50    1.15    --  113.25 -77.00-150.00   84
 58  \w     48.00 104.00   0.50    1.15    --  113.25 -94.00   0.00  112
 59  \w     72.00 106.00   0.50    1.15    --  113.25 -94.00  90.00   68
 60  \w     45.00  74.00   0.50    1.15    --  113.25 -94.00 120.00   58
 61  \w     79.00 106.00   0.50    1.15    --  113.25 -94.00 120.00   54
 62  \w    111.00 136.00   0.50    1.15    --  113.25 -77.00 -30.00   50
 63  \w     45.00  70.00   0.50    1.15    --  113.25 -77.00 -30.00   50
 64  \w     47.00  73.00   0.50    1.15    --  113.25 -94.00 -30.00   52
 65  \w    111.00 171.00   0.50    1.15    --  113.25  15.00   0.00  120
 66  \w    134.00 160.00   0.50    1.15    --  113.25  15.00 -30.00   52
 67  \w     64.00  91.00   0.50    1.15    --  113.25-125.00 -60.00   54
 68  \w    111.00 145.00   0.50    1.15    --  113.25  77.00  90.00   68
 69  \w    152.00 177.00   0.50    1.15    --  113.25  77.00  90.00   50
 70  \w    125.00 151.00   0.50    1.15    --  113.25  45.00  30.00   52
 71  \w     45.00  98.00   0.50    1.15    --  113.25 -94.00-180.00  106
 72  \w    153.00 178.00   0.50    1.15    --  113.25  55.00-173.94   50
 73  \w    111.00 136.00   0.50    1.15    --  113.25 -77.00  90.00   50
 74  \w     79.00 105.00   0.50    1.15    --  113.25-125.00-180.00   52
 75  \w     83.00 109.00   0.50    1.15    --  113.25-125.00  90.00   52
 76  \w    129.00 162.00   0.50    1.15    --  113.25  77.00   0.00   66
 77  \w    118.00 144.00   0.50    1.15    --  113.25  77.00  60.00   52
 78  \w    109.00 139.00   0.50    1.15    --  113.25  61.00-120.00   60
 79  \w     43.00  73.00   0.50    1.15    --  113.25 -66.00 113.17   60
 80  \w     43.00  68.00   0.50    1.15    --  113.25 -86.00-168.33   50
 81  \w    111.00 136.00   0.50    1.15    --  113.25  61.00  30.00   50
 82  \w    128.00 171.00   0.50    1.15    --  113.25  15.00 120.00   86
 83  \w    126.00 170.00   0.50    1.15    --  113.25  15.00 150.00   88
 84  \w    108.00 135.00   0.50    1.15    --  113.25  45.00 -90.00   54
 85  \w     47.00  73.00   0.50    1.15    --  113.25 -77.00 -90.00   52
 86  \w    108.00 134.00   0.50    1.15    --  113.25 -77.00 150.00   52
 87  \w    109.00 134.00   0.50    1.15    --  113.25 -88.00 106.08   50
;
_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      0.0405134000
_diffrn_orient_matrix_UB_12      -0.0808845000
_diffrn_orient_matrix_UB_13      -0.0566717000
_diffrn_orient_matrix_UB_21      -0.0646628000
_diffrn_orient_matrix_UB_22      -0.0814986000
_diffrn_orient_matrix_UB_23      0.0418274000
_diffrn_orient_matrix_UB_31      -0.1219927000
_diffrn_orient_matrix_UB_32      0.0163407000
_diffrn_orient_matrix_UB_33      -0.0720827000
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49719
_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         79.947
_diffrn_reflns_theta_min         4.129
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.472
_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    1.199
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.00059(14)
_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   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0465P)^2^+0.9233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4533
_reflns_number_total             4901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02570a2.cif
_cod_data_source_block           pla23075_refinalized
_cod_depositor_comments
'Adding full bibliography for 7133320--7133330.cif.'
_cod_database_code               7133322
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Na2 O8 C60 H70'
_chemical_oxdiff_usercomment     NJK-07-040
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.777
_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:
 C22(H22A,H22B), C23(H23A,H23B), C19(H19A,H19B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C12(H12), C15(H15), C10(H10), C13(H13), C7(H7), C14(H14),
 C9(H9), C8(H8)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C20(H20A,H20B,H20C), C17(H17A,H17B,
 H17C)
;
_shelx_res_checksum              8117
_shelx_hkl_checksum              96074
_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 1.475
_oxdiff_exptl_absorpt_empirical_full_min 0.649