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_7708358
_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         'C72 H68 Dy2 N10 O6 S2, 2(C2 H3 N)'
_chemical_formula_sum            'C76 H74 Dy2 N12 O6 S2'
_chemical_formula_weight         1640.59
_chemical_name_systematic        Dy2(HL)2(SCN)2].2CH3CN-(1)
_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     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                96.5470(10)
_cell_angle_beta                 100.2410(10)
_cell_angle_gamma                113.9310(10)
_cell_formula_units_Z            1
_cell_length_a                   11.6924(4)
_cell_length_b                   12.8898(4)
_cell_length_c                   13.8753(4)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      62.43
_cell_measurement_theta_min      5.28
_cell_volume                     1840.25(10)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20505
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        62.424
_diffrn_reflns_theta_max         62.424
_diffrn_reflns_theta_min         3.308
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    11.744
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.3419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1370 before and 0.0798 after correction.
The Ratio of minimum to maximum transmission is 0.4545.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             826
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.634
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         5779
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0861P)^2^+12.2164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5379
_reflns_number_total             5779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02071d2.cif
_cod_data_source_block           1
_cod_database_code               7708358
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.333
_shelx_estimated_absorpt_t_min   0.157
_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
 N6-C37
 1.1 with sigma of 0.02
 C37-C38
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C34 \\sim C35 \\sim C36: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
N6 \\sim C37 \\sim C38: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
4.a Everything fixed:
 H3
4.b Riding coordinates:
 C38(H38a,H38b,H38c)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C11(H11a,H11b), C15(H15a,H15b), C16(H16a,H16b), C17(H17a,H17b),
 C22(H22a,H22b)
4.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C13(H13), C14(H14), C18(H18), C19(H19), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
  C35(H35), C36(H36)
4.e Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c)
;
_olex2_submission_special_instructions 'No special instructions were received'