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_7059333
_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 Nd2 O18, 3(C2 H3 N)'
_chemical_formula_sum            'C72 H86 N14 Nd2 O18'
_chemical_formula_weight         1724.02
_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                 117.705(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7253(15)
_cell_length_b                   27.7358(15)
_cell_length_c                   17.9572(17)
_cell_measurement_reflns_used    7555
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.9460
_cell_measurement_theta_min      2.5430
_cell_volume                     7816.1(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     12.00  81.00   1.00   20.00    --   11.74  57.00  90.00   69
  2  \w    -21.00  86.00   1.00   20.00    --   11.74  77.00-180.00  107
  3  \w    -20.00   5.00   1.00   20.00    --   11.74 -99.00 150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0202460000
_diffrn_orient_matrix_UB_12      -0.0005538000
_diffrn_orient_matrix_UB_13      -0.0446031000
_diffrn_orient_matrix_UB_21      0.0396335000
_diffrn_orient_matrix_UB_22      0.0048086000
_diffrn_orient_matrix_UB_23      0.0007181000
_diffrn_orient_matrix_UB_31      0.0080279000
_diffrn_orient_matrix_UB_32      -0.0251089000
_diffrn_orient_matrix_UB_33      0.0011197000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.1221
_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       34
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37659
_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         1.949
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             3520
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.278
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1025
_refine_ls_number_reflns         15343
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0442P)^2^+7.0873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10961
_reflns_number_total             15343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05831a2.cif
_cod_data_source_block           ndno3
_cod_depositor_comments
;Adding full bibliography for 7059332--7059334.cif.

 Adding full bibliography for 7059332--7059334.cif.
;
_cod_database_code               7059333
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.829
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(C61B) \\sim Ueq, Uanis(C62B) \\sim Ueq, Uanis(C62A) \\sim Ueq,
Uanis(C61A) \\sim Ueq, Uanis(C42A) \\sim Ueq, Uanis(C43A) \\sim Ueq,
Uanis(C38A) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38B) \\sim Ueq,
Uanis(C37B) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C43B) \\sim Ueq, Uanis(C42B) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: C38A(0.5) H38A(0.5) H38B(0.5) H38C(0.5) H41C(0.5) H41D(0.5)
 H41A(0.5) H41B(0.5) C37A(0.5) H37A(0.5) H37B(0.5) C61B(0.5) H61A(0.5)
 H61B(0.5) C42A(0.5) H42A(0.5) C43A(0.5) H43A(0.5) H43B(0.5) C62B(0.5)
 H62A(0.5) H62B(0.5) H62C(0.5) C62A(0.5) H62D(0.5) H62E(0.5) H62F(0.5)
 C61A(0.5) H61C(0.5) H61D(0.5) C38B(0.5) H38D(0.5) H38E(0.5) H38F(0.5)
 C37B(0.5) H37C(0.5) H37D(0.5) C42B(0.5) H42B(0.5) C43B(0.5) H43C(0.5) H43D(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C41(H41C,H41D), C41(H41A,H41B), C39(H39A,H39B), C37A(H37A,
 H37B), C17(H17A,H17B), C15(H15A,H15B), C59(H59A,H59B), C63(H63A,H63B),
 C61B(H61A,H61B), C61A(H61C,H61D), C37B(H37C,H37D)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), C5(H5), C30(H30), C8(H8), C27(H27), C35(H35), C11(H11),
 C10(H10), C3(H3), C33(H33), C25(H25), C21(H21), C32(H32), C46(H46), N7(H7),
 C51(H51), C13(H13), C48(H48), C58(H58), C49(H49), C56(H56), C64(H64),
 C42A(H42A), C42B(H42B)
4.c X=CH2 refined with riding coordinates:
 C65(H65A,H65B), C43A(H43A,H43B), C22(H22A,H22B), C43B(H43C,H43D)
4.d Idealised Me refined as rotating group:
 C38A(H38A,H38B,H38C), C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C60(H60A,H60B,
 H60C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C66(H66A,H66B,H66C), C68(H68A,
 H68B,H68C), C70(H70A,H70B,H70C), C62B(H62A,H62B,H62C), C19(H19A,H19B,H19C),
 C62A(H62D,H62E,H62F), C38B(H38D,H38E,H38F), C72(H72A,H72B,H72C)
4.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.096
_oxdiff_exptl_absorpt_empirical_full_min 0.915