Geometry and magnetic interaction modulations in dinuclear Dy2 single-molecule magnets
Guo, Mei; Xu, Yonghui; Wu, Jianfeng; Zhao, Lang; Tang, Jinkui; Dalton Trans.  (2017) –; doi:10.1039/C7DT01121K

data_7043330
_publ_section_title
;
 Geometry and magnetic interaction modulations in dinuclear Dy2
 single-molecule magnets
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01121K
_journal_year                    2017
_chemical_formula_moiety         'C58 H46 Dy2 N12 O12, 2(C2 H3 N)'
_chemical_formula_sum            'C62 H52 Dy2 N14 O12'
_chemical_formula_weight         1510.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1j3ym6
_audit_creation_date             2017-04-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2017-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                73.8570(10)
_cell_angle_beta                 77.6560(10)
_cell_angle_gamma                83.6090(10)
_cell_formula_units_Z            1
_cell_length_a                   10.3827(6)
_cell_length_b                   11.6579(7)
_cell_length_c                   13.2869(8)
_cell_measurement_reflns_used    3160
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.22
_cell_measurement_theta_min      2.64
_cell_volume                     1506.82(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9592
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.079
_diffrn_reflns_theta_min         1.821
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.536
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       block
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.153
_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     358
_refine_ls_number_reflns         5939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4646
_reflns_number_total             5939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01121k2.cif
_cod_data_source_block           2
_cod_database_code               7043330
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H25A)=Sof(H26A)=Sof(C24A)=Sof(C29A)=Sof(H29A)=Sof(C28A)=Sof(H28A)=
 Sof(C27A)=Sof(H27A)=1-FVAR(1)
 Sof(C24)=Sof(H25)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=
 Sof(H29)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
 C25(H25A), C26(H26), C26(H26A), C27(H27), C28(H28), C29(H29), C29A(H29A),
 C28A(H28A), C27A(H27A)
3.b Fitted hexagon refined as free rotating group:
 C10(C11,C12,C13,C14,C15), C17(C18,C19,C20,C21,C22), C24(C25,C26,C27,C28,C29)
3.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N5(H5A,H5B)
3.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'