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_1565645
_publ_section_title
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 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         '2(C25 H22 Dy N3 O6), C2 H3 N'
_chemical_formula_sum            'C52 H47 Dy2 N7 O12'
_chemical_formula_weight         1286.96
_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
_cell_angle_alpha                68.710(2)
_cell_angle_beta                 86.308(2)
_cell_angle_gamma                66.439(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7237(7)
_cell_length_b                   14.7337(6)
_cell_length_c                   15.8914(8)
_cell_measurement_reflns_used    6828
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.33
_cell_volume                     2533.0(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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0965
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36470
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.333
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.997
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0693 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.8057.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.057
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         8901
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0231P)^2^+19.4335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5796
_reflns_number_total             8901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           1
_cod_database_code               1565645
_shelx_estimated_absorpt_t_max   0.679
_shelx_estimated_absorpt_t_min   0.447
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N7-C51
 1.15 with sigma of 0.02
 C51-C52
 1.35 with sigma of 0.02
 H49_$1-H52A_$2
 2.2 with sigma of 0.02
 H52B-H24
 2.2 with sigma of 0.02
 H30_$3-H52B_$4
 2.2 with sigma of 0.02
 O10_$5-H9
 2.3 with sigma of 0.02
3. Rigid bond restraints
 N7, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N7, C51, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C11)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Riding coordinates:
 C27(H27)
5.b Rotating group:
 O6(H6A,H6B), O12(H12A,H12B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C18(H18), C32(H32), C43(H43), C2(H2), C25(H25), C21(H21), C5(H5),
 C37(H37), C4(H4), C15(H15), C3(H3A), C28(H28), C30(H30), C38(H38), C46(H46),
 C36(H36), C22(H22), C11(H11), C29(H29), C40(H40), C50(H50), C14(H14), C39(H39),
  C47(H47), C23(H23), C49(H49), C24(H24), C48(H48), C13(H13), C12(H12)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C35(H35A,H35B,H35C), C52(H52A,H52B,H52C)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O9(H9)
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