A series of planar tetranuclear lanthanide complexes: axial ligand modulated magnetic dynamics in Dy4 species
Zhang, Ya-Xin; Li, Meng; Liu, Bi-Ying; Wu, Zhi-Lei; Wei, Hai-Ying; Wang, Wen-Min; RSC Advances 7 (2017) 55523–; doi:10.1039/C7RA11750G

data_7229673
_publ_section_title
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 A series of planar tetranuclear lanthanide complexes: axial ligand
 modulated magnetic dynamics in Dy4 species
;
_journal_issue                   87
_journal_name_full               'RSC Advances'
_journal_page_first              55523
_journal_paper_doi               10.1039/C7RA11750G
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C146 H156 Gd4 N12 O22, 2(C2 H3 N), 2(C2 H6 O)'
_chemical_formula_sum            'C154 H174 Gd4 N14 O24'
_chemical_formula_weight         3234.06
_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   mixed
_audit_creation_date             2017-08-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-03 deposited with the CCDC.
2017-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                67.916(8)
_cell_angle_beta                 74.027(10)
_cell_angle_gamma                71.695(9)
_cell_formula_units_Z            1
_cell_length_a                   14.9356(12)
_cell_length_b                   15.9841(9)
_cell_length_c                   17.9763(12)
_cell_measurement_reflns_used    8974
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3714.8(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40809
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.019
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         3.100
_exptl_absorpt_coefficient_mu    1.834
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.799
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         12981
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0234P)^2^+9.9161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10981
_reflns_number_total             12981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11750g2.cif
_cod_data_source_block           7
_cod_database_code               7229673
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.711
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H8 of O8, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H12A of O12
2. Restrained distances
 C59-C60 = C59-C61 = C59-C62 = C59-C60' = C59-C61' = C59-C62'
 1.54 with sigma of 0.01
 O12-C77
 2.6 with sigma of 0.02
 C76-O12
 1.1 with sigma of 0.02
 H77B-H61F
 2.2 with sigma of 0.02
 H61D-H77B
 2.2 with sigma of 0.02
 H61D-H77C
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C60 \\sim C61 \\sim C62 \\sim C60' \\sim C61' \\sim C62': within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C60')
\\sim Ueq, Uanis(C61') \\sim Ueq, Uanis(C62') \\sim Ueq, Uanis(N7) \\sim Ueq,
Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C76) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C60')=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C61')=Sof(H61D)=Sof(H61E)=
 Sof(H61F)=Sof(C62')=Sof(H62D)=Sof(H62E)=Sof(H62F)=1-FVAR(1)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(1)
5.a Riding coordinates:
 C75(H75A,H75B,H75C)
5.b Ternary CH refined with riding coordinates:
 O8(H8)
5.c Secondary CH2 refined with riding coordinates:
 C76(H76A,H76B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8A), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C32(H32), C33(H33), C37(H37), C38(H38), C41(H41),
 C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C49(H49), C50(H50), C57(H57),
  C68(H68)
5.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C34(H34A,H34B,H34C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C62(H62A,H62B,H62C), C60'(H60D,H60E,H60F), C61'(H61D,H61E,H61F),
 C62'(H62D,H62E,H62F), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,
 H65C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C77(H77A,
 H77B,H77C)
5.f Idealised tetrahedral OH refined as rotating group:
 O12(H12A)
;
_shelx_res_checksum              37384
_olex2_submission_special_instructions 'No special instructions were received'