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_7060467
_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         'C76 H86 Dy6 N32 O17, O2'
_chemical_formula_sum            'C76 H86 Dy6 N32 O19'
_chemical_formula_weight         2726.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2021-02-19
_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                90
_cell_angle_beta                 105.045(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8929(15)
_cell_length_b                   18.115(2)
_cell_length_c                   21.769(3)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.45
_cell_volume                     4529.2(10)
_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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44636
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.434
_diffrn_reflns_theta_min         1.484
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.971
_exptl_absorpt_correction_T_max  0.4512
_exptl_absorpt_correction_T_min  0.4253
_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    1.999
_exptl_crystal_description       block
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.810
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9296
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+17.9863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7420
_reflns_number_total             9296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00140j2.cif
_cod_data_source_block           aaaa_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7060465--7060467.cif.'
_cod_original_cell_volume        4529.1(10)
_cod_database_code               7060467
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.503
_shelx_estimated_absorpt_t_min   0.468
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H1A of O1, H2A of O2, H3A of O10A, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H6 of O6, H9 of O9
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 O4_$1-H3A
 2.5 with sigma of 0.02
 H3A-H15
 2.5 with sigma of 0.02
 H3A-Dy1_$1
 2.7 with sigma of 0.02
 O9-H9
 0.85 with sigma of 0.01
 O3-H3A
 0.85 with sigma of 0.02
 C33-H6
 1.897229 with sigma of 0.02
 C37-H9
 1.88308 with sigma of 0.02
3. Rigid bond restraints
 O6, C33, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim
O8: within -3.9A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
-3.9A
Uanis(O10) = Uanis(O10A)
5. Others
 Sof(O10A)=1-FVAR(1)
 Sof(O10)=FVAR(1)
 Fixed Sof: O8(0.5)
6.a Riding coordinates:
 O1(H1A), O2(H2A)
6.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C23(H23A,H23B), C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B)
6.c 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)
6.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C)
;
_shelx_res_checksum              37125
_olex2_submission_special_instructions 'No special instructions were received'