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_7060989
_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         'C46 H46 La2 N10 O14'
_chemical_formula_sum            'C46 H46 La2 N10 O14'
_chemical_formula_weight         1240.75
_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   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                 97.637(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.973(3)
_cell_length_b                   14.747(2)
_cell_length_c                   27.502(4)
_cell_measurement_reflns_used    2764
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.03
_cell_measurement_theta_min      2.23
_cell_volume                     7224.7(19)
_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      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEX II DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1133
_diffrn_reflns_av_unetI/netI     0.1767
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41713
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.528
_diffrn_reflns_theta_min         1.793
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  0.8776
_exptl_absorpt_correction_T_min  0.8105
_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    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.687
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         14852
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7410
_reflns_number_total             14852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03652a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7060989--7060993.cif.'
_cod_original_cell_volume        7224.5(19)
_cod_database_code               7060989
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.868
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{O14, O14'}
3. Restrained distances
 O14-C46 = O14'-C46'
 1.43 with sigma of 0.02
 O14'-H14'
 0.87 with sigma of 0.01
 O14-H14
 0.87 with sigma of 0.01
 La2-H14'
 3.063243 with sigma of 0.02
 C46'-H14'
 1.923724 with sigma of 0.02
 La2-H14
 3.164955 with sigma of 0.02
 C46-H14
 1.910504 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O14 \\sim C46' \\sim C46: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 3A
Uanis(O14) = Uanis(O14')
5. Others
 Sof(O14')=Sof(H14')=Sof(C46')=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(O14)=Sof(H14)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
6.a Riding coordinates:
 O13(H13A,H13B)
6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C30(H30A,H30B), C45(H45A,H45B)
6.c Me refined with riding coordinates:
 C46(H46A,H46B,H46C), C46'(H46D,H46E,H46F), C14(H14A,H14B,H14C), C29(H29A,H29B,
 H29C), C44(H44A,H44B,H44C)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C12(H12), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C25(H25), C27(H27), C32(H32), C33(H33),
  C34(H34), C36(H36), C37(H37), C40(H40), C42(H42), N1(H1), N4(H4A), N7(H7A)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64588
_shelx_fab_checksum              7878
_olex2_submission_special_instructions 'No special instructions were received'