Regulating the solution structural integrity and slow magnetic relaxation behavior of two Dy6 clusters with a pyridine‒triazole ligand
Li, Hai-Ye; Pang, Xu-Hong; Tao, Ye; Huang, Fu-Ping; Zou, Hua-Hong; Liang, Fu-Pei; New Journal of Chemistry 45 (2021) 7096–7102; doi:10.1039/D1NJ00140J

data_7060465
_publ_section_title
;
 Regulating the solution structural integrity and slow magnetic relaxation
 behavior of two Dy6 clusters with a pyridine--triazole ligand
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7096
_journal_page_last               7102
_journal_paper_doi               10.1039/D1NJ00140J
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety
'C78 H72 Dy6 N36 O20, 2(C0.4 H1.2 N O2), 0.4(N)'
_chemical_formula_sum            'C78.8 H74.4 Dy6 N38.4 O24'
_chemical_formula_weight         2918.36
_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     heavy
_audit_creation_date             2021-02-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-02-28 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                83.756(5)
_cell_angle_beta                 75.623(4)
_cell_angle_gamma                88.170(5)
_cell_formula_units_Z            1
_cell_length_a                   12.446(4)
_cell_length_b                   13.401(5)
_cell_length_c                   15.377(5)
_cell_measurement_reflns_used    9587
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.495
_cell_measurement_theta_min      2.426
_cell_volume                     2469.6(15)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30325
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.521
_diffrn_reflns_theta_min         1.529
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.571
_exptl_absorpt_correction_T_max  0.4603
_exptl_absorpt_correction_T_min  0.3871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.439
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10172
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0294P)^2^+5.5339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9216
_reflns_number_total             10172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00140j2.cif
_cod_data_source_block           aaaa
_cod_depositor_comments
'Adding full bibliography for 7060465--7060467.cif.'
_cod_original_cell_volume        2469.5(15)
_cod_original_formula_sum        'C78.80 H74.40 Dy6 N38.40 O24'
_cod_database_code               7060465
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.7788
_shelx_estimated_absorpt_t_min   0.4545
_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,H,H) groups
2. Restrained distances
 N19-C40
 2 with sigma of 0.02
 C40-N19
 1.55 with sigma of 0.02
 C36A-N18
 1.6 with sigma of 0.02
 O12-N19
 1.4 with sigma of 0.02
 N17A-O8 = N17A-O7 = N17A-O6A
 1.34 with sigma of 0.02
 C36-N18 = C37A-N18
 1.6 with sigma of 0.02
3. Restrained planarity
 O7, O8, O6A, N17A
 with sigma of 0.1
4. Rigid bond restraints
 O5, C35
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O7, O8, N17, N17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(N21) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(N19)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C36A) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C37)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) = Uanis(C36A)
Uanis(O6) = Uanis(O6A)
Uanis(N17) = Uanis(N17A)
Uanis(C37) = Uanis(C37A)
6. Others
 Sof(O6A)=1-FVAR(1)
 Sof(O6)=FVAR(1)
 Sof(N17A)=1-FVAR(2)
 Sof(N17)=FVAR(2)
 Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C37A)=Sof(H37D)=Sof(H37E)=
 Sof(H37F)=1-FVAR(3)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=
 FVAR(3)
 Fixed Sof: O11(0.8) O12(0.4) O13(0.8) H12A(0.4) H40A(0.4) H40B(0.4) C40(0.4)
 N21(0.2)
 Fixed X: H36D(0.965489) H36E(1.086849) H36F(1.03725) H12A(0.49358)
 H40A(0.42948) H40B(0.39848)
 Fixed Y: H36D(0.60145) H36E(0.55877) H36F(0.597569) H12A(0.589509)
 H40A(0.64845) H40B(0.66471)
 Fixed Z: H36D(0.363891) H36E(0.3467) H36F(0.26487) H12A(0.09556)
 H40A(0.17558) H40B(0.08224)
7.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C23(H23A,H23B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C27(H27), C28(H28), C29(H29), C30(H30),
  C35(H35)
7.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C39(H39A,H39B,H39C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C37A(H37D,H37E,H37F)
;
_shelx_res_checksum              49787
_olex2_submission_special_instructions 'No special instructions were received'