Hierarchical Subcomponent Self-assembly of Covalent Triple-stranded Complex with 3d-4f Vertices: Luminescence and Magnetic Property
Zhi, Liu; Fan, Yin; Yang, Jian; Guo, Xiao-Qing; Zhou, Lipeng; Tian, Chong-Bin; Sun, Qing-Fu; Dalton Transactions  (2023) –; doi:10.1039/D3DT01139A

data_7713117
_publ_section_title
;
 Hierarchical Subcomponent Self-assembly of Covalent Triple-stranded
 Complex with 3d-4f Vertices: Luminescence and Magnetic Property
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01139A
_journal_year                    2023
_chemical_formula_moiety         'C107 H104 Lu2 N14 O8 Zn2, 4(C F3 O3 S)'
_chemical_formula_sum            'C111 H104 F12 Lu2 N14 O20 S4 Zn2'
_chemical_formula_weight         2791.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2fr08h
_audit_creation_date             2023-04-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-15 deposited with the CCDC.	2023-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.285(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.602(2)
_cell_length_b                   26.315(2)
_cell_length_c                   28.155(2)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    159.98
_cell_measurement_theta_max      22.05
_cell_measurement_theta_min      2.39
_cell_volume                     15239(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      159.98
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            47081
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        22.002
_diffrn_reflns_theta_max         22.002
_diffrn_reflns_theta_min         2.611
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5204
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       plate
_exptl_crystal_F_000             5608
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.426
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         9273
_refine_ls_number_restraints     787
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0815
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1085P)^2^+266.6213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6334
_reflns_number_total             9273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01139a2.cif
_cod_data_source_block           mo_3b_LuZn
_cod_database_code               7713117
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.673
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 F4A-C56A = F6A-C56A = F5A-C56A
 1.44 with sigma of 0.02
 S2A-O8 = S2A-O10A = S2A-O9A
 1.42 with sigma of 0.02
 S2A-C56A = S2B-C56B = S1-C55
 1.4 with sigma of 0.02
 S1-O7 = S1-O6 = S1-O5
 1.42 with sigma of 0.02
 F1-C55 = F3-C55 = F2-C55
 1.44 with sigma of 0.02
 S1-F1 = S1-F3 = S1-F2
 2.5 with sigma of 0.02
 C55-O5 = C55-O7 = C55-O6
 2.2 with sigma of 0.02
 F4A-F5A \\sim F4A-F6A \\sim F5A-F6A
 with sigma of 0.04
 S2A-F4A \\sim S2A-F6A \\sim S2A-F5A
 with sigma of 0.04
 C56A-O10A \\sim C56A-O9A \\sim C56A-O8
 with sigma of 0.04
 O5-O7 \\sim O7-O6 \\sim O6-O5
 with sigma of 0.04
 F1-F3 \\sim F3-F2 \\sim F2-F1
 with sigma of 0.04
3. Rigid bond restraints
 S1, O5, C55, O7, O6, F1, F3, F2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
Uanis(O5) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O6) \\sim
Ueq, Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(S1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C56B)=Sof(F6B)=Sof(F3A)=Sof(F4B)=Sof(S2B)=Sof(O10B)=Sof(O9B)=Sof(C1)=
 Sof(H1A)=Sof(H1B)=1-FVAR(1)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(F4A)=Sof(S2A)=Sof(O9A)=Sof(O10A)=Sof(F5A)=
 Sof(F6A)=Sof(C56A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C17(H17A,H17B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C18(H18A,H18B), C54(H54A,H54B), C1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C42(H42), C26(H26), C8(H8), C44(H44), C22(H22), C21(H21), C25(H25),
 C3(H3), C12(H12), C10(H10), C4(H4A), C52(H52), C39(H39), C40(H40), C24(H24),
 C16(H16), C34(H34), C48(H48), C46(H46), C28(H28), C30(H30), C7(H7), C6(H6)
6.c Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C33(H33A,H33B,H33C), C51(H51A,H51B,H51C), C15(H15A,H15B,
 H15C)
6.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60606
_shelx_hkl_checksum              1166
_shelx_fab_checksum              54927
_olex2_submission_special_instructions 'No special instructions were received'