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_7249925
_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
'C162 H122 N12 O22 Yb4, 2(C H2 Cl2), 6(C2 H3 N)'
_chemical_formula_sum            'C176 H144 Cl4 N18 O22 Yb4'
_chemical_formula_weight         3697.04
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-21
_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                90
_cell_angle_beta                 95.3090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.4927(3)
_cell_length_b                   15.5992(2)
_cell_length_c                   25.5168(4)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      74.54
_cell_measurement_theta_min      3.51
_cell_volume                     8518.3(2)
_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 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            69197
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.918
_diffrn_reflns_theta_min         3.479
_diffrn_source_current           0.95
_diffrn_source_power             0.0475
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.040
_exptl_absorpt_correction_T_max  0.0872
_exptl_absorpt_correction_T_min  0.0090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1075 before and 0.0657 after correction.
The Ratio of minimum to maximum transmission is 0.1032.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             3700
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.591
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         17460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0718
_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^)+(0.1339P)^2^+8.6850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2059
_refine_ls_wR_factor_ref         0.2127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14610
_reflns_number_total             17460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00662c2.cif
_cod_data_source_block           cu_0423_5_0m
_cod_depositor_comments
'Adding full bibliography for 7249924--7249925.cif.'
_cod_database_code               7249925
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.633
_shelx_estimated_absorpt_t_min   0.432
_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.a Secondary CH2 refined with riding coordinates:
 C035(H03D,H03E)
2.b Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00U(H00U), C00W(H00W), C010(H010), C011(H011), C012(H012),
 C013(H013), C015(H015), C016(H016), C017(H017), C018(H018), C019(H019),
 C01A(H01A), C01B(H01B), C01F(H01F), C01G(H01G), C01H(H01H), C01J(H01J),
 C01K(H01K), C01N(H01N), C01O(H01O), C01Q(H01Q), C01S(H01S), C01T(H01T),
 C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X), C01Y(H01Y), C020(H020),
 C021(H021), C022(H022), C023(H023), C024(H024), C028(H028), C029(H029),
 C02A(H02A), C02C(H02C), C02D(H02D), C02F(H02F), C02G(H02G), C02I(H02I),
 C02J(H02J), C02L(H02L), C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R),
 C02S(H02S), C02T(H02T), C02U(H02U), C02W(H02W)
2.c Idealised Me refined as rotating group:
 C02K(H02B,H02E,H02H), C02M(H02K,H02M,H02N), C02V(H02Z,H,HA), C02X(H02V,H02X,
 H02Y), C02Z(H02,HB,HC), C030(H03A,H03B,H03C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96271
_shelx_fab_checksum              3322
_olex2_submission_special_instructions 'No special instructions were received'