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_7060993
_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
'2(C92 H84 N19 O23 Tb5), 5(C6 H15 N), 14(H2 O)'
_chemical_formula_sum            'C214 H271 N43 O60 Tb10'
_chemical_formula_weight         5994.92
_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                 101.087(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   36.9338(14)
_cell_length_b                   20.8248(13)
_cell_length_c                   21.7478(13)
_cell_measurement_reflns_used    6888
_cell_measurement_temperature    291.15
_cell_measurement_theta_max      20.45
_cell_measurement_theta_min      2.18
_cell_volume                     16414.9(16)
_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      291.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX II DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            108533
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.463
_diffrn_reflns_theta_min         1.124
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.186
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6783
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             5972
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1832
_refine_ls_number_reflns         37300
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22442
_reflns_number_total             37300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03652a2.cif
_cod_data_source_block           201312277aa
_cod_depositor_comments
'Adding full bibliography for 7060989--7060993.cif.'
_cod_database_code               7060993
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.779
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H14D,H14E} of O14W, {H15C,H15D} of O15W, {H12H,H12I} of
  O12W, {H17B,H17C} of O17W, {H19A,H19B} of O19W, {H11Z,HB} of O11W, {H18A,
  H18B} of O18W, {H16A,H16B} of O16W, {H20A,H20B} of O20W, {H22A,H22B} of O22W,
  {H23A,H23B} of O23W, {H8WA,H8WB} of O8W, {H21A,H21B} of O21W, {H7WA,H7WB} of
  O7W, {H9WA,H9WB} of O9W, {H13A,H13B} of O13W, {H1WA,H1WB} of O1W, {H6WA,H6WB}
  of O6W, {H2WA,H2WB} of O2W, {H4WA,H4WB} of O4W, {H3WA,H3WB} of O3W, {H5WA,
  H5WB} of O5W, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H10Z,HA} of O10W
2. Shared sites
{O6, O6A}
{N7, N7A}
{O22, O22A}
{N4, N4A}
{O23, O23A}
{N1, N1A}
3. Uiso/Uaniso restraints and constraints
Uanis(O16W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: N1(0.5) N4(0.5) N7(0.5) O6(0.5) O22(0.5) O23(0.5) C93(0.5)
 H93A(0.5) H93B(0.5) H93C(0.5) C94(0.5) H94A(0.5) H94B(0.5) C95(0.5) H95A(0.5)
 H95B(0.5) H95C(0.5) C96(0.5) H96A(0.5) H96B(0.5) C97(0.5) H97A(0.5) H97B(0.5)
 H97C(0.5) C98(0.5) H98A(0.5) H98B(0.5) C99(0.5) H99A(0.5) H99B(0.5) H99C(0.5)
 C100(0.5) H10A(0.5) H10B(0.5) C101(0.5) H10C(0.5) H10D(0.5) H10E(0.5)
 C102(0.5) H10F(0.5) H10G(0.5) C103(0.5) H10H(0.5) H10I(0.5) H10J(0.5)
 C104(0.5) H10K(0.5) H10L(0.5) C105(0.5) H10M(0.5) H10N(0.5) H10O(0.5)
 C106(0.5) H10P(0.5) H10Q(0.5) C107(0.5) H10R(0.5) H10S(0.5) H10T(0.5)
 C108(0.5) H10U(0.5) H10V(0.5) C109(0.5) H10W(0.5) H10X(0.5) H10Y(0.5)
 C110(0.5) H11B(0.5) H11C(0.5) C111(0.5) H11D(0.5) H11E(0.5) H11F(0.5)
 C112(0.5) H11G(0.5) H11H(0.5) C113(0.5) H11I(0.5) H11J(0.5) H11K(0.5)
 C114(0.5) H11L(0.5) H11M(0.5) C115(0.5) H11N(0.5) H11O(0.5) H11P(0.5)
 C116(0.5) H11Q(0.5) H11R(0.5) C117(0.5) H11S(0.5) H11T(0.5) H11U(0.5)
 C118(0.5) H11V(0.5) H11W(0.5) C119(0.5) H11X(0.5) H11Y(0.5) H(0.5) C120(0.5)
 H12A(0.5) H12B(0.5) C121(0.5) H12C(0.5) H12D(0.5) H12E(0.5) C122(0.5)
 H12F(0.5) H12G(0.5) N20(0.5) N21(0.5) N22(0.5) N23(0.5) N24(0.5) O1W(0.4)
 H1WA(0.4) H1WB(0.4) O2W(0.3) H2WA(0.3) H2WB(0.3) O3W(0.3) H3WA(0.3) H3WB(0.3)
 O4W(0.3) H4WA(0.3) H4WB(0.3) O5W(0.3) H5WA(0.3) H5WB(0.3) O6W(0.3) H6WA(0.3)
 H6WB(0.3) O7W(0.3) H7WA(0.3) H7WB(0.3) O8W(0.3) H8WA(0.3) H8WB(0.3) O9W(0.3)
 H9WA(0.3) H9WB(0.3) O10W(0.3) H10Z(0.3) HA(0.3) O11W(0.3) H11Z(0.3) HB(0.3)
 O12W(0.3) H12H(0.3) H12I(0.3) O13W(0.3) H13A(0.3) H13B(0.3) O14W(0.3)
 H14D(0.3) H14E(0.3) O15W(0.3) H15C(0.3) H15D(0.3) O16W(0.3) H16A(0.3)
 H16B(0.3) O17W(0.3) H17B(0.3) H17C(0.3) O18W(0.3) H18A(0.3) H18B(0.3)
 O19W(0.3) H19A(0.3) H19B(0.3) O20W(0.3) H20A(0.3) H20B(0.3) O21W(0.3)
 H21A(0.3) H21B(0.3) O22W(0.3) H22A(0.3) H22B(0.3) O23W(0.3) H23A(0.3)
 H23B(0.3) O6A(0.5) N7A(0.5) O22A(0.5) N4A(0.5) O23A(0.5) N1A(0.5)
5.a Riding coordinates:
 C111(H11D,H11E,H11F), O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB),
 O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB), O8W(H8WA,H8WB),
  O9W(H9WA,H9WB), O10W(H10Z,HA), O11W(H11Z,HB), O12W(H12H,H12I), O13W(H13A,
 H13B), O14W(H14D,H14E), O15W(H15C,H15D), O16W(H16A,H16B), O17W(H17B,H17C),
 O18W(H18A,H18B), O19W(H19A,H19B), O20W(H20A,H20B), O21W(H21A,H21B), O22W(H22A,
 H22B), O23W(H23A,H23B)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C30(H30A,H30B), C45(H45A,H45B), C60(H60A,H60B), C75(H75A,
 H75B), C90(H90A,H90B), C94(H94A,H94B), C96(H96A,H96B), C98(H98A,H98B),
 C100(H10A,H10B), C102(H10F,H10G), C104(H10K,H10L), C106(H10P,H10Q), C108(H10U,
 H10V), C110(H11B,H11C), C112(H11G,H11H), C114(H11L,H11M), C116(H11Q,H11R),
 C118(H11V,H11W), C120(H12A,H12B), C122(H12F,H12G)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C11(H11), C16(H16), C17(H17),
 C19(H19), C20(H20), C22(H22), C24(H24), C26(H26), C31(H31), C32(H32), C34(H34),
  C35(H35), C37(H37), C39(H39), C41(H41), C46(H46), C47(H47), C49(H49),
 C50(H50), C52(H52), C54(H54), C56(H56), C61(H61), C62(H62), C64(H64), C65(H65),
  C67(H67), C69(H69), C71(H71), C76(H76), C77(H77), C79(H79), C80(H80),
 C82(H82), C86(H86), C88(H88), N2(H2A), N5(H5A), N8(H8), N11(H11A), N14(H14),
 N17(H17A)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C29(H29A,H29B,H29C), C44(H44A,H44B,H44C), C59(H59A,H59B,
 H59C), C74(H74A,H74B,H74C), C89(H89A,H89B,H89C), C91(H91A,H91B,H91C), C92(H92A,
 H92B,H92C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C97(H97A,H97B,H97C),
 C99(H99A,H99B,H99C), C101(H10C,H10D,H10E), C103(H10H,H10I,H10J), C105(H10M,
 H10N,H10O), C107(H10R,H10S,H10T), C109(H10W,H10X,H10Y), C113(H11I,H11J,H11K),
 C115(H11N,H11O,H11P), C117(H11S,H11T,H11U), C119(H11X,H11Y,H), C121(H12C,H12D,
 H12E)
;
_shelx_res_checksum              46674
_olex2_submission_special_instructions 'No special instructions were received'