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_7713424
_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         'C25 H53 N7 Nd4 O24, N O3, C2 H3 N'
_chemical_formula_sum            'C27 H56 N9 Nd4 O27'
_chemical_formula_weight         1515.76
_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             2022-01-17
_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                 101.200(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.6443(14)
_cell_length_b                   12.1157(6)
_cell_length_c                   30.4747(17)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.40
_cell_volume                     9288.1(9)
_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 0.997
_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  0.0700
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            48344
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.310
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.496
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.8035.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.168
_exptl_crystal_description       block
_exptl_crystal_F_000             5896
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9131
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0506P)^2^+116.4551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6781
_reflns_number_total             9131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01465g2.cif
_cod_data_source_block           mo_1211_7_0m
_cod_database_code               7713424
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.638
_shelx_estimated_absorpt_t_min   0.399
_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
 O6-H6
 0.87 with sigma of 0.01
 O2-H2
 0.87 with sigma of 0.01
 O8-H8
 0.87 with sigma of 0.01
 O11-H11
 0.87 with sigma of 0.01
 O5-H5
 0.87 with sigma of 0.01
 O10-H10
 0.87 with sigma of 0.01
 C12-H6
 1.92004 with sigma of 0.02
 Nd2-H6
 3.213913 with sigma of 0.02
 C4-H2
 1.927393 with sigma of 0.02
 Nd1-H2
 3.128375 with sigma of 0.02
 C16-H8
 1.889918 with sigma of 0.02
 Nd3-H8
 3.257975 with sigma of 0.02
 C22-H11
 1.902698 with sigma of 0.02
 Nd4-H11
 3.153958 with sigma of 0.02
 C10-H5
 1.941023 with sigma of 0.02
 Nd2-H5
 3.121889 with sigma of 0.02
 C20-H10
 1.9765 with sigma of 0.02
 Nd4-H10
 3.336446 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C16(H16A,H16B), C14(H14A,H14B), C8(H8A,H8B), C24(H24A,H24B),
 C23(H23A,H23B), C19(H19A,H19B), C20(H20A,H20B), C10(H10A,H10B), C2(H2A,H2B),
 C17(H17A,H17B), C9(H9A,H9B), C15(H15A,H15B), C7(H7A,H7B), C5(H5A,H5B), C1(H1A,
 H1B), C4(H4A,H4B), C13(H13A,H13B), C22(H22A,H22B), C12(H12A,H12B), C6(H6A,H6B),
  C21(H21A,H21B), C11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C18(H18)
4.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              41458
_olex2_submission_special_instructions 'No special instructions were received'