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_1565711
_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 Er2 O14, 1.25(C H2 Cl2)'
_chemical_formula_sum            'C77.25 H60.5 Cl2.5 Er2 O14'
_chemical_formula_weight         1635.90
_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     dual
_cell_angle_alpha                108.54(3)
_cell_angle_beta                 113.32(3)
_cell_angle_gamma                90.32(3)
_cell_formula_units_Z            2
_cell_length_a                   13.749(3)
_cell_length_b                   17.078(3)
_cell_length_c                   17.150(3)
_cell_measurement_reflns_used    10170
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9024
_cell_measurement_theta_min      1.2722
_cell_volume                     3465.8(17)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        crystalclear
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.996
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34771
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         1.911
_exptl_absorpt_coefficient_mu    2.566
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1629
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.444
_refine_diff_density_min         -1.915
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         16389
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0489P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12895
_reflns_number_total             16389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-499-119203.cif
_cod_data_source_block           4
_cod_original_cell_volume        3466.0(15)
_cod_original_formula_sum        'C77.25 H60.50 Cl2.50 Er2 O14'
_cod_database_code               1565711
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.628
_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
2. Restrained distances
 Cl3-C78 = Cl4-C78
 1.72 with sigma of 0.01
 Cl3-Cl4
 2.82 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl3) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(C78) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl3(0.25) Cl4(0.25) C78(0.25) H78A(0.25) H78B(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C77(H77A,H77B), C78(H78A,H78B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6), C7(H7), C9(H9), C13(H13), C14(H14), C15(H15),
 C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C33(H33), C36(H36), C37(H37), C38(H38),
 C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48),
  C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C57(H57), C58(H58),
 C59(H59), C60(H60), C61(H61), C63(H63), C66(H66), C67(H67), C68(H68), C69(H69),
  C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C)
;