Dinuclear Ln(iii) complexes constructed from an 8-hydroxyquinoline Schiff base derivative with different terminal groups show differing slow magnetic relaxation
Chang, Yi-Xin; Wang, Wen-Min; Zhang, Ru-Xia; Shen, Hai-Yun; Zhou, Xiao-Pu; Wang, Ni-Ni; Cui, Jian-Zhong; Gao, Hong-Ling; New J. Chem. 41 (2017) 6251–6261; doi:10.1039/C6NJ04035G

data_7056333
_publ_section_title
;
 Dinuclear Ln(iii) complexes constructed from an 8-hydroxyquinoline Schiff
 base derivative with different terminal groups show differing slow
 magnetic relaxation
;
_journal_issue                   14
_journal_name_full               'New J. Chem.'
_journal_page_first              6251
_journal_page_last               6261
_journal_paper_doi               10.1039/C6NJ04035G
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C56 H40.34 Er2 F12 N4 O10'
_chemical_formula_sum            'C56 H46 Er2 F12 N4 O10'
_chemical_formula_weight         1497.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-04-28 deposited with the CCDC.
2017-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.753(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2757(11)
_cell_length_b                   22.0146(18)
_cell_length_c                   11.4203(11)
_cell_measurement_reflns_used    7871
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     2802.7(4)
_computing_cell_refinement
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  "'Rigaku Xtalab P200"
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28004
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.532
_diffrn_reflns_theta_min         3.324
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.075
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.044
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.441
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6362
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.440
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+10.8620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5708
_reflns_number_total             6362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj04035g2.cif
_cod_data_source_block           10
_cod_database_code               7056333
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.673
_shelx_estimated_absorpt_t_min   0.578
_olex2_refinement_description
;There are disorders in the -CF3 and -CH3 groups of the ligand
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
 C24-C25 = C24A-C25
 1.5 with sigma of 0.01
 C19-F1' = C19-F2' = C19-F3' = C19A-F1'A = C19A-F2'A = C19A-F3'A
 1.35 with sigma of 0.01
 C24-F4 = C24-F5 = C24-F6 = C24A-F4A = C24A-F5A = C24A-F6A
 1.35 with sigma of 0.01
 C14-C17 = C14'-C17'
 1.5 with sigma of 0.01
 C17'-C18' = C17-C18
 1.54 with sigma of 0.01
 F1'-F2' \\sim F1'-F3' \\sim F2'-F3' \\sim F1'A-F2'A \\sim F1'A-F3'A \\sim
F2'A-F3'A
 with sigma of 0.01
 N2-C11 \\sim N2-C11'
 with sigma of 0.01
 F4-F5 \\sim F4-F6 \\sim F5-F6 \\sim F4A-F5A \\sim F4A-F6A \\sim F5A-F6A
 with sigma of 0.01
 F1-F2 \\sim F1-F3 \\sim F2-F3
 with sigma of 0.01
3. Restrained planarity
 N2, C11', C12', C13', C14', C15', C16', C17'
 with sigma of 0.01
 N2, C11, C12, C13, C14, C15, C16, C17
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17') \\sim Ueq, Uanis(C18')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(C24A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5A) \\sim Ueq,
Uanis(F6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F1') \\sim Ueq, Uanis(F2') \\sim Ueq, Uanis(F3') \\sim Ueq, Uanis(F1'A)
\\sim Ueq, Uanis(F2'A) \\sim Ueq, Uanis(F3'A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C24) = Uanis(C24A)
Uanis(C17) = Uanis(C17')
Uanis(C16) = Uanis(C16')
Uanis(C15) = Uanis(C15')
Uanis(C14) = Uanis(C14')
Uanis(C13) = Uanis(C13')
Uanis(C12) = Uanis(C12')
Uanis(C11) = Uanis(C11')
Uanis(F1') = Uanis(F1'A)
Uanis(C19) = Uanis(C19A)
5. Others
 Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(F4A)=Sof(F5A)=Sof(F6A)=0.5*FVAR(2)
 Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(2)
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(F1'A)=Sof(F2'A)=Sof(F3'A)=0.5*(1-FVAR(3))
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
 Sof(C11')=Sof(C12')=Sof(H12')=Sof(C13')=Sof(H13')=Sof(C14')=Sof(C15')=
 Sof(H15')=Sof(C16')=Sof(H16')=Sof(C17')=Sof(H17C)=Sof(H17D)=Sof(C18')=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(3)
 Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(C15)=Sof(H15)=
 Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=FVAR(3)
 Fixed Sof: C24(0.5) C24A(0.5) C19(0.5) C19A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C17'(H17C,H17D)
6.b Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C28(H28A,H28B,H28C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C21(H21), C26(H26),
 C12(H12), C13(H13), C15(H15), C16(H16), C12'(H12'), C13'(H13'), C15'(H15'),
 C16'(H16')
6.d Fitted hexagon refined as free rotating group:
 C11(C12,C13,C14,C15,C16), C11'(C12',C13',C14',C15',C16')
6.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C18'(H18D,H18E,H18F)
;
_shelx_res_checksum              39452
_olex2_submission_special_instructions 'No special instructions were received'