Modulation of the magnetic properties of mononuclear Dy(III) complexes by tuning the coordination geometry and local symmetry.
Zhou, Xuejuan; Qin, Huiliang; Zeng, Zhaopeng; Luo, Shuchang; Yang, Tao; Cen, Peipei; Liu, Xiangyu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16219–16228; doi:10.1039/d4dt02135e

data_7717002
_publ_section_title
;
 Modulation of the magnetic properties of mononuclear Dy(III) complexes by
 tuning the coordination geometry and local symmetry.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16219
_journal_page_last               16228
_journal_paper_doi               10.1039/d4dt02135e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C34 H30 Cl4 Dy N8 O6, 2(C H2 Cl2), C24 H20 B'
_chemical_formula_sum            'C60 H54 B Cl8 Dy N8 O6'
_chemical_formula_weight         1440.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-02-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-01 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.964(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.429(5)
_cell_length_b                   16.344(6)
_cell_length_c                   30.943(10)
_cell_measurement_reflns_used    8428
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.34
_cell_volume                     6271(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            132829
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.568
_diffrn_reflns_theta_min         1.410
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.589
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             2900
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.621
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         14346
_refine_ls_number_restraints     584
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+7.1537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12974
_reflns_number_total             14346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02135e2.cif
_cod_data_source_block           xj82
_cod_depositor_comments
'Adding full bibliography for 7717000--7717002.cif.'
_cod_database_code               7717002
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.832
_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
2. Restrained distances
 Cl6-C59 = C59-Cl5
 1.79 with sigma of 0.02
 Cl5A-C59A = C59A-Cl6A
 1.79 with sigma of 0.02
 Cl6-Cl5
 2.924 with sigma of 0.04
 Cl5A-Cl6A
 2.924 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C59, Cl5, Cl6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C59A, Cl6A, Cl5A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C59A)=Sof(H59C)=Sof(H59D)=Sof(Cl5A)=Sof(Cl6A)=1-FVAR(1)
 Sof(Cl5)=Sof(Cl6)=Sof(C59)=Sof(H59A)=Sof(H59B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C31(H31A,H31B), C32(H32A,H32B), C59(H59A,
 H59B), C60(H60A,H60B), C59A(H59C,H59D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C14(H14), C15(H15), C16(H16), C25(H25),
 C26(H26), C27(H27), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
  C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58)
6.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C), C34(H34A,H34B,
 H34C)
;
_olex2_submission_special_instructions 'No special instructions were received'