New dinuclear compounds of dysprosium and erbium constructed by an O-vanillin ligand and β-diketonate coligand: Synthesis, near-Infrared luminescent and magnetism
Duan, Yao-Yao; Wu, Dong-Fang; Chen, Huan-Huan; Wang, Yun-Juan; Li, Ling; Gao, Hong-Ling; Cui, Jian-Zhong; Inorganica Chimica Acta 499 (2020) 119203–; doi:10.1016/j.ica.2019.119203

data_1565708
_publ_section_title
;
 New dinuclear compounds of dysprosium and erbium constructed by an
 O-vanillin ligand and \b-diketonate coligand: Synthesis, near-Infrared
 luminescent and magnetism
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119203
_journal_paper_doi               10.1016/j.ica.2019.119203
_journal_volume                  499
_journal_year                    2020
_chemical_formula_moiety         'C76 H58 Dy2 O14, C2 H3 N'
_chemical_formula_sum            'C78 H61 Dy2 N O14'
_chemical_formula_weight         1561.27
_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   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                68.50(3)
_cell_angle_beta                 68.72(3)
_cell_angle_gamma                88.95(3)
_cell_formula_units_Z            2
_cell_length_a                   13.464(3)
_cell_length_b                   17.063(3)
_cell_length_c                   17.642(4)
_cell_measurement_reflns_used    8648
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.8744
_cell_measurement_theta_min      1.4614
_cell_volume                     3483.0(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.1034
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.837
_diffrn_reflns_theta_min         1.294
_exptl_absorpt_coefficient_mu    2.194
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.086
_refine_diff_density_min         -2.279
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       0.0046(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/8 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         16421
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0770
_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^)+(0.0936P)^2^+3.4008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1924
_refine_ls_wR_factor_ref         0.2170
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12326
_reflns_number_total             16421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-499-119203.cif
_cod_data_source_block           1
_cod_original_cell_volume        3483.2(15)
_cod_database_code               1565708
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.668
_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
2. Restrained distances
 C53-C52 = C53-C52'
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C47') \\sim Ueq, Uanis(C48') \\sim Ueq, Uanis(C49') \\sim Ueq,
Uanis(C50') \\sim Ueq, Uanis(C51') \\sim Ueq, Uanis(C51') \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C47')=Sof(H47')=Sof(C48')=Sof(H48')=Sof(C49')=Sof(H49')=Sof(C50')=
 Sof(H50')=Sof(C51')=Sof(H51')=Sof(C52')=1-FVAR(1)
 Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50)=
 Sof(C51)=Sof(H51)=Sof(C52)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C39(H39), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48), C49(H49), C50(H50), C51(H51), C47'(H47'), C48'(H48'), C49'(H49'),
 C50'(H50'), C51'(H51'), C54(H54), C57(H57), C58(H58), C59(H59), C60(H60),
 C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C69(H69), C72(H72),
  C73(H73), C74(H74), C75(H75), C76(H76)
5.b Fitted hexagon refined as free rotating group:
 C47(C48,C49,C50,C51,C52), C47'(C48',C49',C50',C51',C52')
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C78(H78A,H78B,H78C)
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