Reduction of hexaazatrinaphthylenes by divalent lanthanocenes leads to ligand-based multiconfigurational properties.
Temple, Siobhan R.; Tang, Jinkui; Tizzard, Graham J.; Mansikkamäki, Akseli; Layfield, Richard A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12460–12464; doi:10.1039/d4dt01835d

data_7716633
_publ_section_title
;
 Reduction of hexaazatrinaphthylenes by divalent lanthanocenes leads to
 ligand-based multiconfigurational properties.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12460
_journal_page_last               12464
_journal_paper_doi               10.1039/d4dt01835d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C84 H102 N6 Yb3, C7 H8'
_chemical_formula_sum            'C91 H110 N6 Yb3'
_chemical_formula_weight         1806.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-01 deposited with the CCDC.	2024-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.65820(10)
_cell_length_b                   23.6916(2)
_cell_length_c                   18.15350(10)
_cell_measurement_reflns_used    19928
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      71.9750
_cell_measurement_theta_min      4.8550
_cell_volume                     7594.54(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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     -1.00 109.00   1.00   50.00    --   37.24  15.00 -23.00  110
  2  \w    -34.00  76.00   1.00   50.00    --   37.24 -15.00 166.00  110
  3  \w     69.00 178.00   1.00  150.00    --  106.94  15.00 -23.00  109
  4  \w     36.00 145.00   1.00  150.00    --  106.94 -15.00 166.00  109
  5  \w      1.00  87.00   1.00   50.00    --   37.24-125.00-150.00   86
  6  \w     39.00 134.00   1.00  150.00    --  106.94 -77.00  30.00   95
  7  \w     37.00 128.00   1.00  150.00    --  106.94 -30.00 -90.00   91
  8  \w     21.00 105.00   1.00   50.00    --   37.24  57.00-180.00   84
  9  \w      1.00  87.00   1.00   50.00    --   37.24-125.00  30.00   86
 10  \w     37.00  84.00   1.00  150.00    --  106.94-111.00-120.00   47
 11  \w     90.00 175.00   1.00  150.00    --  106.94  45.00-120.00   85
 12  \w     37.00  84.00   1.00  150.00    --  106.94-111.00 -30.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37386
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.174
_diffrn_reflns_theta_min         3.492
_exptl_absorpt_coefficient_mu    6.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       block
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.302
_refine_diff_density_min         -1.850
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         7573
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0339P)^2^+54.0940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6860
_reflns_number_total             7573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01835d2.cif
_cod_data_source_block           1Yb_C7H8
_cod_depositor_comments
'Adding full bibliography for 7716633--7716636.cif.'
_cod_database_code               7716633
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C1A-C1B = C1A-C1E = C1B-C1C = C1C-C1D = C1D-C1E
 1.42 with sigma of 0.02
 C1A-C1J = C1E-C1F
 1.5 with sigma of 0.02
 C1B-C1I = C1C-C1H = C1D-C1G
 1.51 with sigma of 0.02
 C1A-C1C = C1A-C1D
 2.29 with sigma of 0.04
 C1A-C1I = C1A-C1F = C1B-C1H
 2.6 with sigma of 0.04
 C1B-C1D = C1C-C1E
 2.3 with sigma of 0.04
 C1C-C1G = C1D-C1F
 2.61 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1A
 with sigma of 0.02
 C1A-C1C \\sim C1B-C1D \\sim C1C-C1E \\sim C1E-C1B \\sim C1A-C1D
 with sigma of 0.04
 C1A-C1J \\sim C1B-C1I \\sim C1C-C1H \\sim C1D-C1G \\sim C1E-C1F
 with sigma of 0.02
 C1J-C1B \\sim C1J-C1E \\sim C1I-C1A \\sim C1I-C1C \\sim C1H-C1B \\sim C1H-C1D
\\sim C1G-C1C \\sim C1G-C1E
 \\sim C1F-C1D \\sim C1F-C1A
 with sigma of 0.04
2. Restrained planarity
 C1A, C1B, C1C, C1D, C1E, C1F, C1G, C1H, C1I, C1J
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C1G \\sim C1H \\sim
C1I \\sim C1J: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
4. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E, C1F, C1G, C1H, C1I, C1J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H34A(0.5) H34B(0.5) H34C(0.5) H51A(0.5) H51B(0.5) H51C(0.5)
 C1A(0.5) C1B(0.5) C1C(0.5) C1D(0.5) C1E(0.5) C1F(0.5) H1FA(0.5) H1FB(0.5)
 H1FC(0.5) C1G(0.5) H1GA(0.5) H1GB(0.5) H1GC(0.5) C1H(0.5) H1HA(0.5) H1HB(0.5)
 H1HC(0.5) C1I(0.5) H1IA(0.5) H1IB(0.5) H1IC(0.5) C1J(0.5) H1JA(0.5) H1JB(0.5)
 H1JC(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C43(H43), C46(H46), C35(H35), C36(H36), C44(H44), C45(H45), C49(H49),
 C47(H47), C48(H48)
6.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C10(H10A,H10B,H10C), C20(H20A,H20B,
 H20C), C6(H6A,H6B,H6C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C34(H34A,
 H34B,H34C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C19(H19A,
 H19B,H19C), C9(H9A,H9B,H9C), C51(H51A,H51B,H51C), C1F(H1FA,H1FB,H1FC),
 C1G(H1GA,H1GB,H1GC), C1H(H1HA,H1HB,H1HC), C1I(H1IA,H1IB,H1IC), C1J(H1JA,H1JB,
 H1JC)
;
_shelx_res_checksum              96567
_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
;