Self-assembly of tetranuclear 3d-4f helicates as highly efficient catalysts for CO<sub>2</sub> cycloaddition reactions under mild conditions.
Yang, Huan; Gao, Guoshu; Chen, Wanmin; Wang, Li; Liu, Weisheng; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10270–10277; doi:10.1039/d0dt01743d

data_7704741
_publ_section_title
;
 Self-assembly of tetranuclear 3d-4f helicates as highly efficient
 catalysts for CO<sub>2</sub> cycloaddition reactions under mild
 conditions.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10270
_journal_page_last               10277
_journal_paper_doi               10.1039/d0dt01743d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C96 H120 Gd N9 O15 Zn3, 2(C2 H3 N)'
_chemical_formula_sum            'C100 H126 Gd N11 O15 Zn3'
_chemical_formula_weight         2075.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-26 deposited with the CCDC.	2020-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                70.414(2)
_cell_angle_beta                 87.940(2)
_cell_angle_gamma                85.250(2)
_cell_formula_units_Z            2
_cell_length_a                   15.2301(4)
_cell_length_b                   19.7361(5)
_cell_length_c                   19.7667(6)
_cell_measurement_reflns_used    7736
_cell_measurement_temperature    295.42(10)
_cell_measurement_theta_max      25.3960
_cell_measurement_theta_min      3.6460
_cell_volume                     5578.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.42(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -21.00   40.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000  -60.0000 61

  2 omega  -20.00   23.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000 -180.0000 43

  3 omega  -15.00   25.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000  -60.0000 40

  4 omega  -50.00   81.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854    0.0000 -180.0000 131

  5 omega   18.00   57.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   57.0000  -90.0000 39

  6 omega   42.00   68.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000   90.0000 26

  7 omega   62.00   97.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000 -150.0000 35

  8 omega  -40.00   18.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -38.0000  150.0000 58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0067688000
_diffrn_orient_matrix_UB_12      -0.0239277000
_diffrn_orient_matrix_UB_13      -0.0199542000
_diffrn_orient_matrix_UB_21      -0.0105696000
_diffrn_orient_matrix_UB_22      -0.0291879000
_diffrn_orient_matrix_UB_23      0.0308933000
_diffrn_orient_matrix_UB_31      -0.0450176000
_diffrn_orient_matrix_UB_32      0.0062398000
_diffrn_orient_matrix_UB_33      -0.0099089000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39536
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.321
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_F_000             2154
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1218
_refine_ls_number_reflns         19376
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0451P)^2^+5.6810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13785
_reflns_number_total             19376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01743d2.cif
_cod_data_source_block           wanglil1zngd
_cod_depositor_comments
'Adding full bibliography for 7704739--7704741.cif.'
_cod_database_code               7704741
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 98.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C68 \\sim C65 \\sim C67 \\sim C66 \\sim C61 \\sim C60 \\sim C62: within 3.8A
with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N10) \\sim Ueq, Uanis(N11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C97) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C68) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Others
 Fixed Sof: N1B(0.5) H1B(0.5) C8B(0.5) H8BA(0.5) H8BB(0.5) H9AA(0.5) H9AB(0.5)
 H9BC(0.5) H9BD(0.5) N1A(0.5) H1A(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C80(H80A,H80B), C57(H57A,H57B), C81(H81A,H81B), C33(H33A,H33B), C56(H56A,
 H56B), C8B(H8BA,H8BB), C32(H32A,H32B), C9(H9AA,H9AB), C9(H9BC,H9BD), C8A(H8AA,
 H8AB)
4.b Aromatic/amide H refined with riding coordinates:
 C29(H29), N3(H3), C50(H50), C28(H28), N7(H7), C12(H12), C75(H75), C36(H36),
 C60(H60), C52(H52), C76(H76), C27(H27), C53(H53), C4(H4), N5(H5), C2(H2),
 C14(H14), C51(H51), C5(H5A), C26(H26), C34(H34), C77(H77), C58(H58), C84(H84),
 C38(H38), C3(H3A), C74(H74), C10(H10), C62(H62), C86(H86), N1A(H1A), C82(H82)
4.c Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C96(H96A,H96B,H96C), C23(H23A,H23B,H23C), C18(H18A,H18B,
 H18C), C48(H48A,H48B,H48C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C46(H46A,
 H46B,H46C), C70(H70A,H70B,H70C), C90(H90A,H90B,H90C), C19(H19A,H19B,H19C),
 C24(H24A,H24B,H24C), C94(H94A,H94B,H94C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C47(H47A,H47B,H47C), C22(H22A,H22B,H22C), C100(H10A,H10B,H10C),
 C72(H72A,H72B,H72C), C20(H20A,H20B,H20C), C95(H95A,H95B,H95C), C71(H71A,H71B,
 H71C), C43(H43A,H43B,H43C), C66(H66A,H66B,H66C), C98(H98A,H98B,H98C), C68(H68A,
 H68B,H68C)
;
_shelx_res_checksum              27634
_shelx_fab_checksum              58698
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'