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_7704739
_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 Er N9 O15 Zn3, 2(C2 H3 N)'
_chemical_formula_sum            'C100 H126 Er N11 O15 Zn3'
_chemical_formula_weight         2085.48
_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
_atom_sites_solution_primary     iterative
_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                72.372(7)
_cell_angle_beta                 85.842(6)
_cell_angle_gamma                89.624(7)
_cell_formula_units_Z            2
_cell_length_a                   15.1548(12)
_cell_length_b                   19.2532(17)
_cell_length_c                   19.4848(13)
_cell_measurement_reflns_used    7043
_cell_measurement_temperature    239(2)
_cell_measurement_theta_max      25.3960
_cell_measurement_theta_min      3.6460
_cell_volume                     5403.3(8)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      239(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_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  0.0637
_diffrn_reflns_av_unetI/netI     0.1214
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       -24
_diffrn_reflns_number            39555
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.300
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.488
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_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    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             2162
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.695
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1206
_refine_ls_number_reflns         21211
_refine_ls_number_restraints     516
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0526P)^2^+3.6302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13263
_reflns_number_total             21211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01743d2.cif
_cod_data_source_block           zner
_cod_depositor_comments
'Adding full bibliography for 7704739--7704741.cif.'
_cod_database_code               7704739
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.755
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H99A,H99B,H99C} of C99, {H94A,H94B,H94C} of C94, {H96A,
  H96B,H96C} of C96, {H97A,H97B,H97C} of C97, {H95A,H95B,H95C} of C95, All C(H,
  H) groups, All N(H) groups
 At 1.5 times of:
  {H67A,H67B,H67C} of C67, {H92A,H92B,H92C} of C92, {H72A,H72B,H72C} of C72,
  {H19A,H19B,H19C} of C19, {H18A,H18B,H18C} of C18, {H71A,H71B,H71C} of C71,
  {H66A,H66B,H66C} of C66, {H47A,H47B,H47C} of C47, {H70A,H70B,H70C} of C70,
  {H23A,H23B,H23C} of C23, {H91A,H91B,H91C} of C91, {H46A,H46B,H46C} of C46,
  {H22A,H22B,H22C} of C22, {H48A,H48B,H48C} of C48, {H20A,H20B,H20C} of C20,
  {H24A,H24B,H24C} of C24, {H68A,H68B,H68C} of C68, {H43A,H43B,H43C} of C43,
  {H3BA,H3BB,H3BC} of C3B, {H44A,H44B,H44C} of C44, {H42D,H42E,H42F} of C42A,
  {H90A,H90B,H90C} of C90, {H42A,H42B,H42C} of C42
2. Restrained distances
 C43-C41 \\sim C41-C42A
 with sigma of 0.02
 C3B-C41 \\sim C41-C44
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C90) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C95) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(N11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.015
Uanis(C96) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C44) \\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C43) = Uanis(C42A)
Uanis(C3B) = Uanis(C44)
5. Others
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=
 1-FVAR(1)
 Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(H44C)=FVAR(1)
6.a Riding coordinates:
 N1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C80(H80A,H80B), C57(H57A,H57B), C81(H81A,H81B), C32(H32A,
 H32B), C33(H33A,H33B), C9(H9A,H9B), C8(H8A,H8B)
6.c Aromatic/amide H refined with riding coordinates:
 C82(H82), N8(H8), C14(H14), N3(H3), C58(H58), N5(H5), C74(H74), C62(H62),
 C75(H75), C53(H53), C77(H77), C76(H76), C60(H60), C12(H12), C26(H26), C10(H10),
  C38(H38), C34(H34), C50(H50), C27(H27), C2(H2), C29(H29), C28(H28), C52(H52),
 C5(H5A), C4(H4), C84(H84), C36(H36), C51(H51), C3(H3A), C86(H86)
6.d Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C), C24(H24A,H24B,H24C), C20(H20A,H20B,H20C), C48(H48A,H48B,
 H48C), C70(H70A,H70B,H70C), C23(H23A,H23B,H23C), C47(H47A,H47B,H47C), C46(H46A,
 H46B,H46C), C91(H91A,H91B,H91C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C),
 C71(H71A,H71B,H71C), C92(H92A,H92B,H92C), C66(H66A,H66B,H66C), C72(H72A,H72B,
 H72C), C67(H67A,H67B,H67C), C19(H19A,H19B,H19C), C90(H90A,H90B,H90C), C99(H99A,
 H99B,H99C), C94(H94A,H94B,H94C), C96(H96A,H96B,H96C), C95(H95A,H95B,H95C),
 C97(H97A,H97B,H97C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C3B(H3BA,H3BB,
 H3BC), C42A(H42D,H42E,H42F), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              3620
_shelx_fab_checksum              2421
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'