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_7060990
_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         'C48 H49 N11 O14 Pr2'
_chemical_formula_sum            'C48 H49 N11 O14 Pr2'
_chemical_formula_weight         1285.80
_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                 106.684(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4217(14)
_cell_length_b                   14.6810(11)
_cell_length_c                   27.191(2)
_cell_measurement_reflns_used    2789
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.855
_cell_measurement_theta_min      1.220
_cell_volume                     6661.8(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            45163
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.855
_diffrn_reflns_theta_min         1.564
_exptl_absorpt_coefficient_mu    1.504
_exptl_absorpt_correction_T_max  0.8456
_exptl_absorpt_correction_T_min  0.6885
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.796
_refine_diff_density_min         -2.453
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         15550
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0622P)^2^+0.3993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12367
_reflns_number_total             15550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03652a2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7060989--7060993.cif.'
_cod_original_cell_volume        6661.9(9)
_cod_database_code               7060990
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.840
_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, All O(H,H) groups
2. Restrained distances
 N11-C45
 1.3 with sigma of 0.002
 O9-H9A
 0.87 with sigma of 0.01
 C45A-C46A
 2.5 with sigma of 0.002
 C48A-C46A
 2.4 with sigma of 0.002
 Pr2-H9A
 3.189366 with sigma of 0.02
 C47-H9A
 1.899329 with sigma of 0.02
 N11-C46 \\sim N11-C48
 with sigma of 0.02
 C46-N11 \\sim C46A-N11A
 with sigma of 0.02
 C48-N11 \\sim C48A-N11A
 with sigma of 0.02
 C48-C46 \\sim C48A-C46A
 with sigma of 0.04
 C45-O13 \\sim C45A-O13
 with sigma of 0.02
 C45-C46 \\sim C45A-C46A
 with sigma of 0.04
 C45-N11 \\sim C45A-N11A
 with sigma of 0.02
 N11-O13 \\sim N11A-O13
 with sigma of 0.04
 C45-C48 \\sim C45A-C48A
 with sigma of 0.04
 N11A-C45A \\sim C12-C11 \\sim N11-C45
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N11A \\sim C46A \\sim C48A \\sim C45A \\sim O13 \\sim C45 \\sim N11 \\sim C46
\\sim C48: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4. Rigid body (RIGU) restrains
 C46, C48, N11, C45, O13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C46A, N11A, C48A, C45A, O13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C45A)=Sof(H45A)=Sof(N11A)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=
 Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(C45)=Sof(H45)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C46)=Sof(H46A)=
 Sof(H46B)=Sof(H46C)=Sof(N11)=FVAR(1)
6.a Everything fixed:
 C48, C46
6.b Fixed occupancy and ADP/Uiso:
 C45
6.c Riding coordinates:
 C46(H46A,H46B,H46C), N1(H1A), N4(H4A), N7(H7A), O14(H14C,H14D), C48A(H48D,
 H48E,H48F)
6.d Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B), C47(H47A,H47B)
6.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C11(H11), C16(H16), C17(H17),
 C18(H18), C20(H20), C22(H22), C24(H24), C26(H26), C31(H31), C32(H32), C34(H34),
  C35(H35), C37(H37), C39(H39), C41(H41), C45(H45), C45A(H45A)
6.f Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C44(H44A,H44B,H44C), C48(H48A,H48B,
 H48C), C46A(H46D,H46E,H46F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82368
_shelx_fab_checksum              2063
_olex2_submission_special_instructions 'No special instructions were received'