Neutral inverse-sandwich rare-earth metal complexes of the benzene tetraanion.
Wang, Yi; Zhang, Yurou; Liang, Jiefeng; Tan, Bowen; Deng, Chong; Huang, Wenliang; Chemical science 15 (2024) 8740–8749; doi:10.1039/d4sc02491e

data_1571617
_publ_section_title
;
 Neutral inverse-sandwich rare-earth metal complexes of the benzene
 tetraanion.
;
_journal_issue                   23
_journal_name_full               'Chemical science'
_journal_page_first              8740
_journal_page_last               8749
_journal_paper_doi               10.1039/d4sc02491e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C80 H120 N4 Y2'
_chemical_formula_sum            'C80 H120 N4 Y2'
_chemical_formula_weight         1315.61
_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             2023-03-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-04-04 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.683(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.8724(5)
_cell_length_b                   21.9655(2)
_cell_length_c                   25.9782(4)
_cell_measurement_reflns_used    96428
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.2590
_cell_measurement_theta_min      2.0840
_cell_volume                     14720.7(4)
_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_temperature      179.99(10)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            189297
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.550
_diffrn_reflns_theta_min         2.015
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.22a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             5648
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.991
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1588
_refine_ls_number_reflns         38188
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1634
_refine_ls_R_factor_gt           0.0833
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+61.3981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21582
_reflns_number_total             38188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02491e3.cif
_cod_data_source_block           3_CCDC7
_cod_depositor_comments
'Adding full bibliography for 1571610--1571617.cif.'
_cod_database_code               1571617
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 C13-C12 \\sim C15-C12
 with sigma of 0.02
 C14-C13 \\sim C16-C15
 with sigma of 0.02
3. Rigid bond restraints
 C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C57, C58
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
C56 \\sim C55 \\sim C54 \\sim C57 \\sim C58: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
5.a Riding coordinates:
 C1(H1A,H1B,H1C)
5.b Ternary CH refined with riding coordinates:
 C12(H12), C17(H17), C28(H28), C33(H33), C49(H49), C54(H54), C65(H65),
 C70(H70), C92(H92), C97(H97), C108(H108), C113(H113), C129(H129), C134(H134),
 C145(H145), C150(H150)
5.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C18(H18A,H18B), C20(H20A,H20B), C29(H29A,
 H29B), C31(H31A,H31B), C34(H34A,H34B), C36(H36A,H36B), C50(H50A,H50B),
 C52(H52A,H52B), C55(H55A,H55B), C57(H57A,H57B), C66(H66A,H66B), C68(H68A,H68B),
  C71(H71A,H71B), C73(H73A,H73B), C93(H93A,H93B), C95(H95A,H95B), C98(H98A,
 H98B), C100(H10A,H10B), C109(H10F,H10G), C111(H11D,H11E), C114(H11I,H11J),
 C116(H11N,H11O), C130(H13C,H13D), C132(H13H,H13I), C135(H13M,H13N), C137(H13R,
 H13S), C146(H14D,H14E), C148(H14I,H14J), C151(H15C,H15D), C153(H15H,H15I)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C24(H24), C25(H25), C26(H26), C40(H40),
 C45(H45), C46(H46), C47(H47), C61(H61), C62(H62), C63(H63), C75(H75), C76(H76),
  C77(H77), C78(H78), C79(H79), C80(H80), C83(H83), C88(H88), C89(H89),
 C90(H90), C104(H104), C105(H105), C106(H106), C120(H120), C125(H125),
 C126(H126), C127(H127), C141(H141), C142(H142), C143(H143), C155(H155),
 C156(H156), C157(H157), C158(H158), C159(H159), C160(H160)
5.e Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C35(H35A,
 H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C),
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C72(H72A,H72B,H72C), C74(H74A,
 H74B,H74C), C81(H81A,H81B,H81C), C85(H85A,H85B,H85C), C94(H94A,H94B,H94C),
 C96(H96A,H96B,H96C), C99(H99A,H99B,H99C), C101(H10C,H10D,H10E), C110(H11A,H11B,
 H11C), C112(H11F,H11G,H11H), C115(H11K,H11L,H11M), C117(H11P,H11Q,H11R),
 C118(H11S,H11T,H11U), C122(H12A,H12B,H12C), C131(H13E,H13F,H13G), C133(H13J,
 H13K,H13L), C136(H13O,H13P,H13Q), C138(H13T,H13U,H13V), C147(H14F,H14G,H14H),
 C149(H14K,H14L,H14M), C152(H15E,H15F,H15G), C154(H15J,H15K,H15L)
;
_shelx_res_checksum              35045
_olex2_submission_special_instructions 'No special instructions were received'