Two novel Ln8 clusters bridged by CO32−: effectively converting CO2 into oxazolidinones and cyclic carbonates
Qiao, Na; Xin, Xiao-Yan; Wang, Wen-Min; Wu, Zhi-Lei; Cui, Jian-Zhong; Dalton Transactions  (2023) –; doi:10.1039/D3DT01465G

data_7713425
_publ_section_title
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 Two novel Ln8 clusters bridged by CO32&#x2212;: effectively converting
 CO2 into oxazolidinones and cyclic carbonates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01465G
_journal_year                    2023
_chemical_formula_moiety         'C50 H106 N14 O48 Sm8, 2(N O3), 2(C2 H3 N)'
_chemical_formula_sum            'C54 H112 N18 O54 Sm8'
_chemical_formula_weight         3080.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-17 deposited with the CCDC.	2023-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1190(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.6072(16)
_cell_length_b                   12.0967(8)
_cell_length_c                   30.3098(15)
_cell_measurement_reflns_used    9202
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.22
_cell_volume                     9212.6(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0882
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            73995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.222
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.123
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0879 before and 0.0680 after correction.
The Ratio of minimum to maximum transmission is 0.8724.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.221
_exptl_crystal_description       block
_exptl_crystal_F_000             5960
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.082
_refine_diff_density_min         -2.403
_refine_diff_density_rms         0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9065
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+99.1813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6607
_reflns_number_total             9065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01465g2.cif
_cod_data_source_block           mo_1211_6_0m
_cod_database_code               7713425
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.556
_shelx_estimated_absorpt_t_min   0.349
_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, All O(H) groups
2. Restrained distances
 O9-H9
 0.87 with sigma of 0.01
 O6-H6
 0.87 with sigma of 0.01
 O11-H11
 0.87 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O3-H3
 0.87 with sigma of 0.01
 O1-H1
 0.87 with sigma of 0.01
 C16-H9
 1.919649 with sigma of 0.02
 Sm3-H9
 3.110247 with sigma of 0.02
 C10-H6
 1.903494 with sigma of 0.02
 Sm2-H6
 3.236959 with sigma of 0.02
 C22-H11
 1.930019 with sigma of 0.02
 Sm4-H11
 3.212096 with sigma of 0.02
 C24-H12
 1.946888 with sigma of 0.02
 Sm4-H12
 3.109042 with sigma of 0.02
 C6-H3
 1.894017 with sigma of 0.02
 Sm1-H3
 3.118951 with sigma of 0.02
 C2-H1
 1.975072 with sigma of 0.02
 Sm1-H1
 3.283265 with sigma of 0.02
3. Rigid bond restraints
 C5, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C4(H4A,H4B), C10(H10A,H10B), C24(H24A,H24B), C12(H12A,H12B),
 C7(H7A,H7B), C9(H9A,H9B), C3(H3A,H3B), C1(H1A,H1B), C17(H17A,H17B), C23(H23A,
 H23B), C16(H16A,H16B), C2(H2A,H2B), C19(H19A,H19B), C22(H22A,H22B), C15(H15A,
 H15B), C14(H14A,H14B), C18(H18A,H18B), C13(H13A,H13B), C21(H21A,H21B), C5(H5A,
 H5B), C6(H6A,H6B), C11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              99657
_olex2_submission_special_instructions 'No special instructions were received'