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_7056334
_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         'C54 H42 F12 Ho2 N4 O10'
_chemical_formula_sum            'C54 H42 F12 Ho2 N4 O10'
_chemical_formula_weight         1464.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                62.77(2)
_cell_angle_beta                 87.11(3)
_cell_angle_gamma                74.71(3)
_cell_formula_units_Z            1
_cell_length_a                   11.174(3)
_cell_length_b                   11.8895(13)
_cell_length_c                   12.008(3)
_cell_measurement_reflns_used    4402
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1363.7(6)
_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 0.988
_diffrn_measured_fraction_theta_max 0.973
_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  0.0559
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17056
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         3.032
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.982
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.721
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6128
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0806P)^2^+3.7155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5534
_reflns_number_total             6128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj04035g2.cif
_cod_data_source_block           4
_cod_database_code               7056334
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.587
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-F1 = C18-F2 = C18-F3 = C22-F1' = C22-F2' = C22-F3'
 1.36 with sigma of 0.01
 C23-F4 = C23-F5 = C23-F6 = C27-F4' = C27-F5' = C27-F6'
 1.36 with sigma of 0.01
3. Others
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
 Sof(F4')=Sof(F5')=Sof(F6')=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(2)
4.a Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C27(H27A,H27B,
 H27C)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C20(H20), C25(H25)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              47639
_olex2_submission_special_instructions 'No special instructions were received'