Lanthanide clusters as highly efficient catalysts regarding carbon dioxide activation
Hou, Wei; Wang, Gang; Wu, Xiaojing; Sun, Shuoyi; Zhao, Chunyang; Liu, Wei-Sheng; Pan, Fuxing; New Journal of Chemistry 44 (2020) 5019–5022; doi:10.1039/C9NJ05831A

data_7059334
_publ_section_title
;
 Lanthanide clusters as highly efficient catalysts regarding carbon
 dioxide activation
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5019
_journal_page_last               5022
_journal_paper_doi               10.1039/C9NJ05831A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C66 H77 N11 O18 Sm2, 4(C2 H3 N)'
_chemical_formula_sum            'C74 H89 N15 O18 Sm2'
_chemical_formula_weight         1777.30
_chemical_properties_physical    Air-sensitive,Efflorescent
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-06-11 deposited with the CCDC.	2020-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.089(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8528(8)
_cell_length_b                   27.9296(11)
_cell_length_c                   17.8740(8)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.359
_cell_measurement_theta_min      2.394
_cell_volume                     7862.6(6)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            94748
_diffrn_reflns_point_group_measured_fraction_full 0.997
_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         2.280
_exptl_absorpt_coefficient_mu    1.556
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6719
_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 0.0682 after correction. The Ratio of minimum to maximum transmission is 0.9014. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.561
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         15426
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0549P)^2^+17.9858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11273
_reflns_number_total             15426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05831a2.cif
_cod_data_source_block           p21ccc
_cod_depositor_comments
;Adding full bibliography for 7059332--7059334.cif.

 Adding full bibliography for 7059332--7059334.cif.
;
_cod_database_code               7059334
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.679
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C37B-N6
 1.45 with sigma of 0.02
 N6-C37B
 1.45 with sigma of 0.02
 C61B-N9
 1.45 with sigma of 0.02
 N9-C61B
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C62A) \\sim Ueq, Uanis(C61A) \\sim Ueq, Uanis(C38A) \\sim Ueq,
Uanis(C37A) \\sim Ueq, Uanis(C38B) \\sim Ueq, Uanis(C37B) \\sim Ueq,
Uanis(C61B) \\sim Ueq, Uanis(C62B) \\sim Ueq, Uanis(N14) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C61A(0.5) H61A(0.5) H61B(0.5) C37A(0.5) H37A(0.5) H37B(0.5)
 C38A(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C62A(0.5) H62A(0.5) H62B(0.5)
 H62C(0.5) C61B(0.5) H61C(0.5) H61D(0.5) C62B(0.5) H62D(0.5) H62E(0.5)
 H62F(0.5) C38B(0.5) H38D(0.5) H38E(0.5) H38F(0.5) C37B(0.5) H37C(0.5) H37D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C61A(H61A,H61B), C59(H59A,H59B), C37A(H37A,H37B), C15(H15A,
 H15B), C39(H39A,H39B), C20(H20A,H20B), C63(H63A,H63B), C41(H41A,H41B),
 C61B(H61C,H61D), C37B(H37C,H37D)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), N1(H1), C51(H51), C32(H32), N4(H4), N7(H7), C35(H35), C8(H8),
 C27(H27), C58(H58), C5(H5), C46(H46), C33(H33), C30(H30), C3(H3), C49(H49),
 C10(H10), C25(H25), C11(H11), C56(H56), C48(H48), C42(H42), C64(H64), C21(H21)
5.c X=CH2 refined with riding coordinates:
 C65(H65A,H65B), C43(H43A,H43B), C22(H22A,H22B)
5.d Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C44(H44A,H44B,H44C), C40(H40A,H40B,H40C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C66(H66A,H66B,H66C), C18(H18A,H18B,H18C), C72(H72A,
 H72B,H72C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C38A(H38A,H38B,H38C),
 C74(H74A,H74B,H74C), C62A(H62A,H62B,H62C), C62B(H62D,H62E,H62F), C38B(H38D,
 H38E,H38F)
5.e Idealised tetrahedral OH refined as rotating group:
 O6(H6), O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'