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_1571610
_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         'C90 H140 N4 O2 Sm2'
_chemical_formula_sum            'C90 H140 N4 O2 Sm2'
_chemical_formula_weight         1610.75
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-03
_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                64.913(4)
_cell_angle_beta                 70.485(4)
_cell_angle_gamma                61.214(5)
_cell_formula_units_Z            1
_cell_length_a                   12.7862(7)
_cell_length_b                   13.2072(6)
_cell_length_c                   15.4523(6)
_cell_measurement_reflns_used    15829
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.4120
_cell_measurement_theta_min      2.5420
_cell_volume                     2043.3(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      179.99(10)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.912
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26322
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.350
_diffrn_reflns_theta_min         1.913
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.471
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69295
_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    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         10253
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0416P)^2^+0.3700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9022
_reflns_number_total             10253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02491e3.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1571610--1571617.cif.'
_cod_database_code               1571610
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C39, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C38) = Uanis(C40)
4. Others
 Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(H44C)=Sof(H44D)=1-FVAR(1)
 Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H44A)=Sof(H44B)=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), C42(H42A,H42B),
 C42(H42C,H42D), C43(H43A,H43B), C43A(H43C,H43D), C44(H44A,H44B), C44(H44C,
 H44D), C45(H45A,H45B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C24(H24), C25(H25), C26(H26), C38(H38),
 C40(H40)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), 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), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              58934
_olex2_submission_special_instructions 'No special instructions were received'