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_7045467
_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         'C75 H47 N9 O8 Tb2, 2(C2 H3 N), 0.5(C2 H5 O)'
_chemical_formula_sum            'C80 H55.5 N11 O8.5 Tb2'
_chemical_formula_weight         1624.69
_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
_audit_creation_date             2018-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-26 deposited with the CCDC.
2018-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.6820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2718(9)
_cell_length_b                   18.6972(9)
_cell_length_c                   22.4643(12)
_cell_measurement_reflns_used    21124
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     7270.1(6)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42'
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113.15
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            72935
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         3.014
_exptl_absorpt_coefficient_mu    1.994
_exptl_absorpt_correction_T_max  0.7958
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       block
_exptl_crystal_F_000             3242
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.951
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         16534
_refine_ls_number_restraints     391
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+14.1501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14015
_reflns_number_total             16534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00063h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7045466--7045470.cif.'
_cod_original_formula_sum        'C80 H55.50 N11 O8.50 Tb2'
_cod_database_code               7045467
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.691
_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
 O9-C82
 1.4 with sigma of 0.01
 N10-C77 = N11-C79 = N12-C81
 2.66 with sigma of 0.01
 N10-C76 = N11-C78 = N12-C80
 1.12 with sigma of 0.01
 C76-C77 = C78-C79 = C80-C81 = C82-C83
 1.54 with sigma of 0.01
 C40-C41 = C40-C41'
 1.48 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N10 \\sim C76 \\sim C77 \\sim N11 \\sim C78 \\sim C79 \\sim N12 \\sim C80 \\sim
C81 \\sim O9 \\sim C82 \\sim C83: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C41 \\sim C42 \\sim C43 \\sim N9 \\sim C44 \\sim C45 \\sim C41' \\sim C42'
\\sim C43' \\sim N9' \\sim C44' \\sim C45': within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N10) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(N11)
\\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(N12) \\sim Ueq,
Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C82)
\\sim Ueq, Uanis(C83) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
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(C41') \\sim Ueq,
Uanis(C42') \\sim Ueq, Uanis(C43') \\sim Ueq, Uanis(N9') \\sim Ueq, Uanis(C44')
\\sim Ueq, Uanis(C45') \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(C41')=Sof(C42')=Sof(C43')=Sof(N9')=Sof(C44')=Sof(C45')=1-FVAR(1)
 Sof(C41)=Sof(C42)=Sof(C43)=Sof(N9)=Sof(C44)=Sof(C45)=FVAR(1)
 Fixed Sof: N11(0.5) C78(0.5) C79(0.5) H79A(0.5) H79B(0.5) H79C(0.5) N12(0.5)
 C80(0.5) C81(0.5) H81A(0.5) H81B(0.5) H81C(0.5) O9(0.5) C82(0.5) H82A(0.5)
 H82B(0.5) C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B)
5.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)
5.c Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C83(H83A,H83B,
 H83C)
;
_shelx_res_checksum              94902
_olex2_submission_special_instructions 'No special instructions were received'