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_1565647
_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         'C54 H52 Dy2 N6 O12'
_chemical_formula_sum            'C54 H52 Dy2 N6 O12'
_chemical_formula_weight         1302.01
_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
_cell_angle_alpha                90
_cell_angle_beta                 90.3810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.0340(8)
_cell_length_b                   9.2730(4)
_cell_length_c                   19.0118(9)
_cell_measurement_reflns_used    6698
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.99
_cell_measurement_theta_min      2.39
_cell_volume                     3003.0(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0688
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26962
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.391
_exptl_absorpt_coefficient_mu    2.528
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0684 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.8583.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.707
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.201
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5246
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0856
_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^)+(0.1275P)^2^+70.0674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2398
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4090
_reflns_number_total             5246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3.cif
_cod_data_source_block           3
_cod_database_code               1565647
_shelx_estimated_absorpt_t_max   0.719
_shelx_estimated_absorpt_t_min   0.571
_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, All O(H) groups
2. Restrained distances
 O4-H4
 0.85 with sigma of 0.01
 H15A-H28
 2.2 with sigma of 0.02
 C0AA-H4
 1.87375 with sigma of 0.02
 Dy1-H4
 2.909506 with sigma of 0.02
3. Rigid bond restraints
 O4, C0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C38, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C1AA \\sim C0AA \\sim O4: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C1B) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB)
5.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C22(H22), C19(H19), C1A(H1A), C17(H17), C13(H13), C20(H20),
 C25(H25), C26(H26), C27(H27), C8(H8), C38(H38), C10(H10), C1B(H1B), C2(H2),
 C9(H9)
5.c Fitted hexagon refined as free rotating group:
 C12(C16,C22,C19,C1A,C17), C29(C38,C10,C1B,C2,C9)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C1AA(H1AA,H1AB,H1AC)
5.e Idealised tetrahedral OH refined as rotating group:
 O28(H28)
;