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_7059332
_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 La2 N11 O18, 4(C2 H3 N)'
_chemical_formula_sum            'C74 H89 La2 N15 O18'
_chemical_formula_weight         1754.42
_chemical_properties_physical    Air-sensitive,Efflorescent,Heat-sensitive
_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
_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                 118.573(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.023(3)
_cell_length_b                   28.059(4)
_cell_length_c                   18.040(3)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      66.551
_cell_measurement_theta_min      3.21
_cell_volume                     8012(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            80136
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.643
_diffrn_reflns_theta_max         66.643
_diffrn_reflns_theta_min         2.792
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.756
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.2516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1558 before and 0.0947 after correction. The Ratio of minimum to maximum transmission is 0.3342. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       block
_exptl_crystal_F_000             3584
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.903
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         14152
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0698P)^2^+14.5331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12071
_reflns_number_total             14152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05831a2.cif
_cod_data_source_block           20180420_wanggang_chonla_0ma_a
_cod_depositor_comments
;Adding full bibliography for 7059332--7059334.cif.

 Adding full bibliography for 7059332--7059334.cif.
;
_cod_database_code               7059332
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.261
_shelx_estimated_absorpt_t_min   0.179
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,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
 C74-N15
 1 with sigma of 0.02
 C73-C74
 1.4 with sigma of 0.02
 C73-N15
 2.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N15) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(O15) \\sim Ueq,
Uanis(C19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H59A(0.5) H59B(0.5) H59C(0.5) H59D(0.5) C60A(0.5) H60A(0.5)
 H60B(0.5) H60C(0.5) C60B(0.5) H60D(0.5) H60E(0.5) H60F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C20(H20A,H20B), C37(H37A,H37B), C39(H39A,
 H39B), C41(H41A,H41B), C59(H59A,H59B), C59(H59C,H59D), C61(H61A,H61B),
 C63(H63A,H63B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), N7(H7), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C13(H13),
 C21(H21), C25(H25), C27(H27), C30(H30), C32(H32), C33(H33), C35(H35), C42(H42),
  C46(H46), C48(H48), C49(H49), C51(H51), C56(H56), C58(H58), C64(H64)
5.c X=CH2 refined with riding coordinates:
 C22(H22A,H22B), C43(H43A,H43B), C65(H65A,H65B)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C44(H44A,H44B,H44C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C),
 C60A(H60A,H60B,H60C), C19(H19A,H19B,H19C), C60B(H60D,H60E,H60F), C67(H67A,H67B,
 H67C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C)
5.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'