Two novel tetranuclear Yb(iii)-based compounds for highly efficient conversion of CO2 to cyclic carbonates
Sun, Yining; Liu, Guoguo; Xiong, Gang; Xu, Guangwen; CrystEngComm 27 (2025) 2148–2153; doi:10.1039/D4CE00662C

data_7249924
_publ_section_title
;
 Two novel tetranuclear Yb(iii)-based compounds for highly efficient
 conversion of CO2 to cyclic carbonates
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2148
_journal_page_last               2153
_journal_paper_doi               10.1039/D4CE00662C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C78 H55 N6 O8 Yb2'
_chemical_formula_sum            'C78 H55 N6 O8 Yb2'
_chemical_formula_weight         1550.36
_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             2023-11-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-02 deposited with the CCDC.	2025-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                76.367(2)
_cell_angle_beta                 85.738(2)
_cell_angle_gamma                66.875(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8563(9)
_cell_length_b                   15.2810(8)
_cell_length_c                   16.5287(12)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.54
_cell_volume                     3352.9(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1026
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            183131
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.464
_diffrn_reflns_theta_min         2.258
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.834
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0795 after correction.
The Ratio of minimum to maximum transmission is 0.3406.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             1538
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.266
_refine_diff_density_min         -2.624
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         13817
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+13.4577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10085
_reflns_number_total             13817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00662c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7249924--7249925.cif.'
_cod_database_code               7249924
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.601
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N15-C00Z \\sim N01C-C00Z
 with sigma of 0.00001
 N01C-C020 \\sim N15-C14
 with sigma of 0.00001
 C020-C01T \\sim C14-C01T
 with sigma of 0.00001
3. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C028) = Uanis(C13) = Uanis(C02I) = Uanis(C02A) = Uanis(C02K) = Uanis(C025)
Uanis(C7) = Uanis(C02C) = Uanis(C41) = Uanis(C2) = Uanis(C5) = Uanis(C02E) =
Uanis(C1) = Uanis(C01L) = Uanis(C42) = Uanis(C4) = Uanis(C0) = Uanis(C3)
Uanis(N15) = Uanis(N01C)
4. Rigid body (RIGU) restrains
 C4, C42, C1, C5, C41, C7
 with sigma for 1-2 distances of 0.00001 and sigma for 1-3 distances of 0.00001
 C0, C01L, C02E, C2, C02C, C3
 with sigma for 1-2 distances of 0.00001 and sigma for 1-3 distances of 0.00001
 C01L, C0, C02C, C02E, C3, C2, C42, C1, C5, C41, C7, C4
 with sigma for 1-2 distances of 0.00001 and sigma for 1-3 distances of 0.00001
5. Others
 Sof(C42)=Sof(C1)=Sof(H1)=Sof(C5)=Sof(H5)=Sof(C41)=Sof(H41)=Sof(C7)=Sof(H7)=
 Sof(C4)=Sof(H4)=1-FVAR(1)
 Sof(C01L)=Sof(C0)=Sof(H0)=Sof(C02C)=Sof(H02C)=Sof(C02E)=Sof(H02E)=Sof(C3)=
 Sof(H3)=Sof(C2)=Sof(H2)=FVAR(1)
 Sof(C14)=Sof(H14)=Sof(N15)=1-FVAR(2)
 Sof(N01C)=Sof(C020)=Sof(H020)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00L(H00L), C00R(H00R), C00U(H00U), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C012(H012), C013(H013), C015(H015), C017(H017),
 C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01D(H01D), C01F(H01F),
 C01G(H01G), C01I(H01I), C01J(H01J), C01K(H01K), C01N(H01N), C0(H0), C01Q(H01Q),
  C01R(H01R), C01S(H01S), C024(H024), C022(H022), C02B(H02B), C027(H027),
 C01V(H01V), C01U(H01U), C01W(H01W), C01X(H01X), C01Y(H01Y), C01Z(H01Z),
 C020(H020), C021(H021), C023(H023), C026(H026), C025(H025), C02K(H02K),
 C02A(H02A), C02I(H02I), C13(H13), C029(H029), C02C(H02C), C02E(H02E), C3(H3),
 C02G(H02G), C02H(H02H), C02J(H02J), C6(H6), C2(H2), C1(H1), C5(H5), C41(H41),
 C7(H7), C4(H4), C14(H14)
6.b Fitted hexagon refined as free rotating group:
 C01T(C024,C022,C02B,C027,C01V), C028(C025,C02K,C02A,C02I,C13), C42(C1,C5,C41,
 C7,C4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              89847
_shelx_fab_checksum              41329
_olex2_submission_special_instructions 'No special instructions were received'