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_1571611
_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         'C53 H67 N2 Sm'
_chemical_formula_sum            'C53 H67 N2 Sm'
_chemical_formula_weight         882.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-04
_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                98.600(4)
_cell_angle_beta                 93.568(3)
_cell_angle_gamma                92.844(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8737(4)
_cell_length_b                   11.7593(5)
_cell_length_c                   18.5401(8)
_cell_measurement_reflns_used    19909
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.8240
_cell_measurement_theta_min      1.7500
_cell_volume                     2335.30(17)
_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 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31410
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.716
_diffrn_reflns_theta_min         1.755
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'orange red'
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.393
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         12197
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0482P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10567
_reflns_number_total             12197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02491e3.cif
_cod_data_source_block           3_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1571610--1571617.cif.'
_cod_database_code               1571611
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C01G \\sim C01K \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C54 \\sim C55:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
2. Others
 Sof(C01G)=Sof(H01A)=Sof(H01B)=Sof(C01K)=Sof(H01C)=Sof(H01D)=Sof(H01E)=
 Sof(H12A)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C55)=Sof(H55A)=Sof(H55B)=
 1-FVAR(1)
 Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C12(H12A), C12(H12), C17(H17), C28(H28), C33(H33)
3.b Secondary CH2 refined with riding coordinates:
 C01G(H01A,H01B), C13(H13A,H13B), C15(H15A,H15B), C18(H18A,H18B), C20(H20A,
 H20B), C29(H29A,H29B), C31(H31A,H31B), C34(H34A,H34B), C36(H36A,H36B),
 C55(H55A,H55B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C24(H24), C25(H25), C26(H26), C39(H39), C40(H40),
 C41(H41), C42(H42), C43(H43), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C01K(H01C,H01D,H01E), 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), C54(H54A,
 H54B,H54C)
;
_shelx_res_checksum              55067
_olex2_submission_special_instructions 'No special instructions were received'