Magnetic properties and structure of tetranuclear lanthanide complexes based on 8-hydroxylquinoline Schiff base derivative and β-diketone coligand.
Gao, Hong-Ling; Huang, Shao-Xia; Zhou, Xiao-Pu; Liu, Zhen; Cui, Jian-Zhong; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3503–3511; doi:10.1039/c8dt00063h

data_7045468
_publ_section_title
;
 Magnetic properties and structure of tetranuclear lanthanide complexes
 based on 8-hydroxylquinoline Schiff base derivative and \b-diketone
 coligand.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3503
_journal_page_last               3511
_journal_paper_doi               10.1039/c8dt00063h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C150 H106 Er4 N18 O16'
_chemical_formula_sum            'C150 H106 Er4 N18 O16'
_chemical_formula_weight         3085.56
_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             2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-01-26 deposited with the CCDC.
2018-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.743(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.2768(14)
_cell_length_b                   18.6343(13)
_cell_length_c                   22.4288(18)
_cell_measurement_reflns_used    20490
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     7233.6(10)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_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_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9859
              2theta: -15.0721
scan:
    Number of images: 300
               Slice: -105.0000 - 45.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9859
              2theta: -15.0721
scan:
    Number of images: 200
               Slice: -105.0000 - -5.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9859
              2theta: -15.0721
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            71788
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         3.018
_exptl_absorpt_coefficient_mu    2.363
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB(Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3064
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.554
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         16373
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+13.4039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13817
_reflns_number_total             16373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00063h2.cif
_cod_data_source_block           shelx_sq_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7045466--7045470.cif.'
_cod_database_code               7045468
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.649
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Restrained distances
 N8-C40 \\sim N8-C40A
 with sigma of 0.02
 C40-C41 \\sim C40A-C41A
 with sigma of 0.01
 N8-C41 \\sim N8-C41A
 with sigma of 0.01
 C40-C42 \\sim C40-C45 \\sim C40A-C42A \\sim C40A-C45A
 with sigma of 0.01
3. Restrained planarity
 C40, C41, C42, C43, N9, C44, C45
 with sigma of 0.01
 C40A, C41A, C42A, C43A, N9A, C44A, C45A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(N9)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C41A) \\sim Ueq,
Uanis(C42A) \\sim Ueq, Uanis(C43A) \\sim Ueq, Uanis(N9A) \\sim Ueq, Uanis(C44A)
\\sim Ueq, Uanis(C45A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C41) = Uanis(C41A)
Uanis(C42) = Uanis(C42A)
Uanis(C43) = Uanis(C43A)
Uanis(N9) = Uanis(N9A)
Uanis(C45) = Uanis(C45A)
Uanis(C44) = Uanis(C44A)
Uanis(C40) = Uanis(C40A)
5. Others
 Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(H43A)=
 Sof(N9A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=1-FVAR(1)
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=Sof(N9)=
 Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 O8(H8)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C25(H25),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C36(H36), C37(H37), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C53(H53),
  C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62),
 C63(H63), C64(H64), C65(H65), C68(H68), C71(H71), C72(H72), C73(H73), C74(H74),
  C75(H75), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C40A(H40A),
 C42A(H42A), C43A(H43A), C44A(H44A), C45A(H45A)
6.c Fitted hexagon refined as free rotating group:
 C41(C42,C43,N9,C44,C45), C41A(C42A,C43A,N9A,C44A,C45A)
;
_shelx_res_checksum              53333
_shelx_fab_checksum              67805
_olex2_submission_special_instructions 'No special instructions were received'