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_1571612
_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         'C41 H65 I2 N2 O Y'
_chemical_formula_sum            'C41 H65 I2 N2 O Y'
_chemical_formula_weight         944.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-25
_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                 99.436(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5793(4)
_cell_length_b                   21.9106(6)
_cell_length_c                   15.8022(4)
_cell_measurement_reflns_used    7825
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.3980
_cell_measurement_theta_min      2.4950
_cell_volume                     4296.5(2)
_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      180.00
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24757
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.492
_diffrn_reflns_theta_min         2.480
_exptl_absorpt_coefficient_mu    2.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43607
_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            colorless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.722
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         10611
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0951P)^2^+8.4916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7074
_reflns_number_total             10611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02491e3.cif
_cod_data_source_block           3_CCDC2
_cod_depositor_comments
'Adding full bibliography for 1571610--1571617.cif.'
_cod_database_code               1571612
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C15-C12
 1.5 with sigma of 0.02
 C39-C38 \\sim C38-C39A
 with sigma of 0.02
 C39A-C40A \\sim C40-C39
 with sigma of 0.02
 C41-C40A \\sim C40-C41
 with sigma of 0.02
2. Rigid bond restraints
 C7, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C17, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C33, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 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
Uanis(C39A) = Uanis(C39)
Uanis(C40A) = Uanis(C40)
Uanis(C34) = Uanis(C36)
4. Others
 Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)=
 Sof(H40D)=Sof(H41C)=Sof(H41D)=1-FVAR(1)
 Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(H41A)=Sof(H41B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C17(H17), C28(H28), C33(H33)
5.b 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), C38(H38A,H38B),
 C38(H38C,H38D), C39(H39A,H39B), C39A(H39C,H39D), C40(H40A,H40B), C40A(H40C,
 H40D), C41(H41A,H41B), C41(H41C,H41D)
5.c Me refined with riding coordinates:
 C19(H19A,H19B,H19C)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C24(H24), C25(H25), C26(H26)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              80121
_olex2_submission_special_instructions 'No special instructions were received'