Solvent-driven structures and slow magnetic relaxation behaviors of dinuclear dysprosium clusters
Li, Xiu-Hua; Li, Meng; Gao, Ning; Wei, Hai-Ying; Hou, Yin-Ling; Wu, Zhi-Lei; Inorganica Chimica Acta 500 (2020) 119242–; doi:10.1016/j.ica.2019.119242

data_1565646
_publ_section_title
;
 Solvent-driven structures and slow magnetic relaxation behaviors of
 dinuclear dysprosium clusters
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119242
_journal_paper_doi               10.1016/j.ica.2019.119242
_journal_volume                  500
_journal_year                    2020
_chemical_formula_moiety         'C66 H56 Dy2 N6 O13, C H4 O'
_chemical_formula_sum            'C67 H60 Dy2 N6 O14'
_chemical_formula_weight         1498.21
_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
_cell_angle_alpha                71.83
_cell_angle_beta                 86.193(2)
_cell_angle_gamma                86.193(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2737(7)
_cell_length_b                   15.2603(8)
_cell_length_c                   15.2603(8)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.27
_cell_volume                     3147.6(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45199
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         1.431
_exptl_absorpt_coefficient_mu    2.426
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0580 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.8786.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         11072
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0187P)^2^+3.3665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8893
_reflns_number_total             11072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           2
_cod_database_code               1565646
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.484
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O13-H13
 0.85 with sigma of 0.01
 C66-H13
 1.879488 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C49(H49), C57(H57), C52(H52), C62(H62), C33(H33), C31(H31), C45(H45),
 C58(H58), C15(H15), C8(H8), C20(H20), C42(H42), C29(H29), C41(H41), C23(H23),
 C60(H60), C30(H30), C43(H43), C16(H16), C47(H47), C5(H5), C59(H59), C44(H44),
 C32(H32), C48(H48), C50(H50), C34(H34), C18(H18), C17(H17), C13(H13A),
 C14(H14), C35(H35), C38(H38), C1(H1), C2(H2A), C19(H19), C3(H3), C12(H12),
 C11(H11), C28(H28), C26(H26), C27(H27), C4(H4)
4.b Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C55(H55A,H55B,H55C), C66(H66A,H66B,H66C), C67(H67A,H67B,
 H67C)
4.c Idealised tetrahedral OH refined as rotating group:
 O9(H9), O10(H10), O14(H14A)
;