Radii-dependent self-assembly polynuclear lanthanide complexes as catalysts for CO2 transformation into cyclic carbonates
Chen, Changjuan; Zhang, Aijiang; New Journal of Chemistry 45 (2021) 20155–20163; doi:10.1039/D1NJ03652A

data_7060992
_publ_section_title
;
 Radii-dependent self-assembly polynuclear lanthanide complexes as
 catalysts for CO2 transformation into cyclic carbonates
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20155
_journal_page_last               20163
_journal_paper_doi               10.1039/D1NJ03652A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C45 H46 Eu2 N9 O12, N O3'
_chemical_formula_sum            'C45 H46 Eu2 N10 O15'
_chemical_formula_weight         1270.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-08-31
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2021-09-25 deposited with the CCDC.	2021-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.611(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.693(6)
_cell_length_b                   16.389(5)
_cell_length_c                   24.679(8)
_cell_measurement_reflns_used    2764
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.03
_cell_measurement_theta_min      2.23
_cell_volume                     6821(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_av_unetI/netI     0.1316
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49840
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.730
_diffrn_reflns_theta_min         1.514
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  0.8136
_exptl_absorpt_correction_T_min  0.6851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.996
_refine_diff_density_min         -1.478
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         14822
_refine_ls_number_restraints     1103
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1484
_refine_ls_R_factor_gt           0.0895
_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^)+(0.1225P)^2^+5.1844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2188
_refine_ls_wR_factor_ref         0.2422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8487
_reflns_number_total             14822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03652a2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7060989--7060993.cif.'
_cod_database_code               7060992
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.806
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Shared sites
{O2, O2A}
{N12, N12A}
{O8, O8A}
3. Restrained distances
 O9B-N14B \\sim O11B-N14B \\sim O12B-N14B \\sim O12A-N14A \\sim O11A-N14A \\sim
O9A-N14A
 with sigma of 0.02
 O12B-O11B \\sim O9B-O12B \\sim O9B-O11B
 with sigma of 0.02
4. Restrained planarity
 N14B, O9B, O11B, O12B
 with sigma of 0.1
 N14A, O12A, O11A, O9A
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
N14A \\sim O11A \\sim O12A \\sim O9A \\sim O11B \\sim O9B \\sim N14B \\sim
O12B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
Uanis(C23) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C38) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O11A) \\sim Ueq, Uanis(N14A) \\sim Ueq, Uanis(O12A) \\sim Ueq, Uanis(O9A)
\\sim Ueq, Uanis(O12B) \\sim Ueq, Uanis(N14B) \\sim Ueq, Uanis(O9B) \\sim Ueq,
Uanis(O11B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) = Uanis(O8A)
Uanis(N12) = Uanis(N12A)
Uanis(O2) = Uanis(O2A)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Sof(N14B)=Sof(O9B)=Sof(O11B)=Sof(O12B)=1-FVAR(1)
 Sof(O11A)=Sof(N14A)=Sof(O12A)=Sof(O9A)=FVAR(1)
 Fixed Sof: N12(0.5) O2(0.5) O8(0.5) O2A(0.5) N12A(0.5) O8A(0.5)
8.a Riding coordinates:
 O4(H4B), O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
8.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C37(H37A,H37B), C22(H22A,H22B)
8.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C32(H32),
 C34(H34), C39(H39), C42(H42), C43(H43), C44(H44), C45(H45), C16(H16), C18(H18),
  C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), N4(H4A), N11(H11), N8(H8)
8.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C38(H38A,H38B,H38C), C23(H23A,H23B,H23C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48253
_shelx_fab_checksum              69451
_olex2_submission_special_instructions 'No special instructions were received'