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_7060991
_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
'C92 H85 Er5 N18 O20, 2(C15 H14 N3 O3), 2(C H4 O), 5(H2 O)'
_chemical_formula_sum            'C124 H131 Er5 N24 O33'
_chemical_formula_weight         3321.82
_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                 100.671(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.3440(16)
_cell_length_b                   20.8374(14)
_cell_length_c                   21.3950(15)
_cell_measurement_reflns_used    8785
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.11
_cell_volume                     15484.4(17)
_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(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            143207
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.609
_diffrn_reflns_theta_min         0.586
_exptl_absorpt_coefficient_mu    2.752
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5881
_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    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6588
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1841
_refine_ls_number_reflns         35297
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0648P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20709
_reflns_number_total             35297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03652a2.cif
_cod_data_source_block           hl2-er
_cod_depositor_comments
'Adding full bibliography for 7060989--7060993.cif.'
_cod_database_code               7060991
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.734
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H12C,H12D,H12E} of C122, All C(H,H) groups, All N(H)
  groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  {H30A,H30B,H30C} of C30, {H15A,H15B,H15C} of C15, {H60A,H60B,H60C} of C60,
  {H75A,H75B,H75C} of C75, {H91A,H91B,H91C} of C91, {H92A,H92B,H92C} of C92,
  {H90A,H90B,H90C} of C90, {H12L,H12M,H12N} of C123, {H12O,H12P,H12Q} of C124,
  {H12R,H12S,H12T} of C125, {H10C,H10D,H10E} of C107, {H12U,H12V,H12W} of C126,
  {H12I,H12J,H12K} of C128, {H12F,H12G,H12H} of C127, {H45A,H45B,H45C} of C45
2. Shared sites
{O16, O16A}
{N9, N9A}
{O19, O19A}
{N18, N18A}
3. Restrained distances
 C126-O30
 1.49 with sigma of 0.001
 O28-C123
 1.5 with sigma of 0.002
 O31-C127 \\sim O31-C128
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C127 \\sim C128: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C124) \\sim Ueq, Uanis(C125) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C128) \\sim Ueq, Uanis(C127) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O5W) \\sim Ueq, Uanis(O13W) \\sim Ueq, Uanis(O3W) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(N18) = Uanis(N18A)
Uanis(O19) = Uanis(O19A)
Uanis(N9) = Uanis(N9A)
Uanis(O16) = Uanis(O16A)
5. Others
 Fixed Sof: C123(0.4) H12L(0.4) H12M(0.4) H12N(0.4) C124(0.4) H12O(0.4)
 H12P(0.4) H12Q(0.4) C125(0.4) H12R(0.4) H12S(0.4) H12T(0.4) C126(0.4)
 H12U(0.4) H12V(0.4) H12W(0.4) C127(0.2) H12F(0.2) H12G(0.2) H12H(0.2)
 C128(0.2) H12I(0.2) H12J(0.2) H12K(0.2) N9(0.5) N18(0.5) O16(0.5) O19(0.5)
 O27(0.4) H27A(0.4) O28(0.4) H28A(0.4) O29(0.4) H29(0.4) O30(0.4) H30(0.4)
 O31(0.4) H31A(0.2) H31B(0.2) O1W(0.3) H1WA(0.3) H1WB(0.3) O2W(0.3) H2WA(0.3)
 H2WB(0.3) O3W(0.4) H3WA(0.4) H3WB(0.4) O4W(0.3) H4WA(0.3) H4WB(0.3) O5W(0.3)
 H5WA(0.3) H5WB(0.3) O6W(0.4) H6WA(0.4) H6WB(0.4) 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) H10F(0.3)
 H10G(0.3) O11W(0.3) H11B(0.3) H11C(0.3) O12W(0.3) H12X(0.3) H12Y(0.3)
 O13W(0.3) H13A(0.3) H13B(0.3) O14W(0.3) H14C(0.3) H14D(0.3) O15W(0.3)
 H15D(0.3) H15E(0.3) O16W(0.3) H16A(0.3) H16B(0.3) O16A(0.5) N9A(0.5) O19A(0.5)
 N18A(0.5)
6.a Riding coordinates:
 C26(H26), C30(H30A,H30B,H30C), C58(H58), C89(H89A,H89B), C118(H118),
 C123(H12L,H12M,H12N), C124(H12O,H12P,H12Q), C125(H12R,H12S,H12T), C126(H12U,
 H12V,H12W), C127(H12F,H12G,H12H), C128(H12I,H12J,H12K), O20(H20A), O22(H22A),
 O25(H25A), O27(H27A), O28(H28A), O29(H29), O30(H30), O31(H31A,H31B), 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(H10F,
 H10G), O11W(H11B,H11C), O12W(H12X,H12Y), O13W(H13A,H13B), O14W(H14C,H14D),
 O15W(H15D,H15E), O16W(H16A,H16B)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B), C44(H44A,H44B), C59(H59A,H59B), C74(H74A,
 H74B), C106(H10A,H10B), C121(H12A,H12B)
6.c Me refined with riding coordinates:
 C45(H45A,H45B,H45C), C122(H12C,H12D,H12E)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C18(H18),
 C20(H20), C22(H22), C25(H25), C27(H27), C28(H28), C33(H33), C35(H35), C37(H37),
  C40(H40), C41(H41), C42(H42), C43(H43), C48(H48), C50(H50), C52(H52),
 C55(H55), C56(H56), C57(H57), C63(H63), C65(H65), C67(H67), C70(H70), C71(H71),
  C72(H72), C73(H73), C78(H78), C80(H80), C82(H82), C85(H85), C86(H86),
 C87(H87), C88(H88), C95(H95), C97(H97), C99(H99), C102(H102), C103(H103),
 C104(H104), C105(H105), C110(H110), C112(H112), C114(H114), C117(H117),
 C119(H119), C120(H120), N2(H2), N5(H5A), N8(H8), N11(H11A), N14(H14), N17(H17),
  N20(H20B), N23(H23)
6.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C60(H60A,H60B,H60C), C75(H75A,H75B,H75C), C90(H90A,H90B,
 H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C107(H10C,H10D,H10E)
;
_shelx_res_checksum              48040
_olex2_submission_special_instructions 'No special instructions were received'