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_7704740
_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 Dy N9 O15 Zn3, 3(C2 H3 N)'
_chemical_formula_sum            'C101 H130 Dy N11 O17 Zn3'
_chemical_formula_weight         2128.76
_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   geom
_atom_sites_solution_primary     direct
_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                70.729(2)
_cell_angle_beta                 87.962(3)
_cell_angle_gamma                85.124(2)
_cell_formula_units_Z            2
_cell_length_a                   15.2010(6)
_cell_length_b                   19.7221(4)
_cell_length_c                   19.7307(5)
_cell_measurement_reflns_used    6276
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      3.6320
_cell_measurement_theta_min      23.7270
_cell_volume                     5563.4(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.73(10)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.1186
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35643
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.273
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
_cell_measurement_temperature   291.73(10) 
_cell_measurement_reflns_used   6276
_cell_measurement_theta_min     3.6320
_cell_measurement_theta_max     23.7270
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             2210
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.407
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1222
_refine_ls_number_reflns         19490
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0470P)^2^+9.2182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13310
_reflns_number_total             19490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01743d2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7704739--7704741.cif.'
_cod_database_code               7704740
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.772
_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
2. Restrained distances
 N7-C101
 1.1 with sigma of 0.01
 C101-C102
 1.53 with sigma of 0.01
 H10B-H32A
 2.8 with sigma of 0.02
 C2AA-C1AA \\sim C1AA-C96A
 with sigma of 0.02
 C1AA-C96A \\sim C96A-C2AA
 with sigma of 0.02
 C96A-C2AA \\sim C2AA-C1AA
 with sigma of 0.02
 C95A-C94A \\sim C94A-C0AA
 with sigma of 0.02
 C0AA-C95A \\sim C95A-C94A
 with sigma of 0.02
3. Rigid bond restraints
 O44, N193
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C102 \\sim C101 \\sim N7: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O44 \\sim N193: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C8A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(C93) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C95A)
\\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C84) \\sim Ueq,
Uanis(C93A) \\sim Ueq, Uanis(C94A) \\sim Ueq, Uanis(C86A) \\sim Ueq,
Uanis(C85A) \\sim Ueq, Uanis(C84A) \\sim Ueq, Uanis(C2AA) \\sim Ueq,
Uanis(C96A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C46) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O44) \\sim Ueq, Uanis(O33) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1A) = Uanis(N1)
Uanis(C9A) = Uanis(C9)
Uanis(C8A) = Uanis(C8)
Uanis(C93) = Uanis(C86A)
Uanis(C1AA) = Uanis(C85A)
Uanis(C86) = Uanis(C84A)
Uanis(C0AA) = Uanis(C93A) = Uanis(C96A)
Uanis(C2AA) = Uanis(C95A)
5. Others
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(N1A)=Sof(H1A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-
 FVAR(1)
 Sof(N1)=Sof(H1)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(1)
 Sof(C93A)=Sof(C94A)=Sof(H94A)=Sof(H94B)=Sof(H94C)=Sof(C86A)=Sof(H86A)=
 Sof(C85A)=Sof(C84A)=Sof(H84A)=1-FVAR(2)
 Sof(C93)=Sof(C1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H1AD)=Sof(C86)=Sof(H86)=Sof(C85)=
 Sof(C84)=Sof(H84)=FVAR(2)
 Sof(C95A)=Sof(H95A)=Sof(H95B)=Sof(H95C)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=
 Sof(H0AC)=1-FVAR(3)
 Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C96A)=Sof(H96A)=Sof(H96B)=
 Sof(H96C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C57(H57A,H57B), C81(H81A,H81B), C33(H33A,H33B), C8A(H8AA,
 H8AB), C80(H80A,H80B), C32(H32A,H32B), C9A(H9AA,H9AB), C8(H8A,H8B), C9(H9A,H9B)
6.b Aromatic/amide H refined with riding coordinates:
 C74(H74), N3(H3), C28(H28), N5(H5), C29(H29), C36(H36), C12(H12), C51(H51),
 C77(H77), C27(H27), C82(H82), N1AA(H1AA), C75(H75), C2(H2), C5(H5A), C76(H76),
 C14(H14), C52(H52), C53(H53), C4(H4), C3(H3A), C34(H34), C38(H38), C50(H50),
 C26(H26), C60(H60), C62(H62), N1A(H1A), C10(H10), C58(H58), C86(H86), N1(H1),
 C84(H84), C86A(H86A), C84A(H84A)
6.c Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C42(H42A,H42B,
 H42C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C66(H66A,H66B,H66C), C24(H24A,
 H24B,H24C), C44(H44A,H44B,H44C), C92(H92A,H92B,H92C), C23(H23A,H23B,H23C),
 C72(H72A,H72B,H72C), C91(H91A,H91B,H91C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C99(H99A,H99B,H99C), C47(H47A,
 H47B,H47C), C70(H70A,H70B,H70C), C90(H90A,H90B,H90C), C48(H48A,H48B,H48C),
 C1AA(H1AB,H1AC,H1AD), C95A(H95A,H95B,H95C), C0AA(H0AA,H0AB,H0AC), C94A(H94A,
 H94B,H94C), C2AA(H2AA,H2AB,H2AC), C96A(H96A,H96B,H96C), C97(H97A,H97B,H97C),
 C102(H10A,H10B,H10C)
;
_shelx_res_checksum              47766
_shelx_fab_checksum              99631
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'