Coordination anion effects on the geometry and magnetic interaction of binuclear Dy2 single-molecule magnets
Wu, Jinjiang; Li, Xiao-Lei; La Droitte, Léo; Cador, Olivier; Le Guennic, Boris; Tang, Jinkui; Dalton Transactions  (2021) –; doi:10.1039/D1DT02071D

data_7708359
_publ_section_title
;
 Coordination anion effects on the geometry and magnetic interaction of
 binuclear Dy2 single-molecule magnets
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02071D
_journal_year                    2021
_chemical_formula_moiety         'C70 H68 Dy2 N10 O12, 2(C2 H3 N), 2(O)'
_chemical_formula_sum            'C74 H74 Dy2 N12 O14'
_chemical_formula_weight         1680.45
_chemical_name_systematic        '[Dy2(HL)2(NO3)2].2CH3CN.2H2O (2)'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-06-06 deposited with the CCDC.	2021-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.585(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6039(9)
_cell_length_b                   15.8167(9)
_cell_length_c                   16.5425(10)
_cell_measurement_reflns_used    9303
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.023
_cell_measurement_theta_min      2.575
_cell_volume                     3642.5(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            74904
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.037
_diffrn_reflns_theta_max         25.037
_diffrn_reflns_theta_min         1.949
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.108
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6430
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.297
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0169P)^2^+6.3464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5760
_reflns_number_total             6430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02071d2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               7708359
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.678
_shelx_estimated_absorpt_t_min   0.364
_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
 O3-H3
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Everything fixed:
 O7
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C12(H12A,H12B), C15(H15A,H15B), C22(H22A,H22B),
 C25(H25A,H25B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C11(H11), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19),
  C21(H21), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34)
4.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              4130
_shelx_hkl_checksum              30547
_olex2_submission_special_instructions 'No special instructions were received'