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_7229672
_publ_section_title
;
 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         '2(C61 H54 Gd2 N6 O11)'
_chemical_formula_sum            'C122 H108 Gd4 N12 O22'
_chemical_formula_weight         2723.20
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-08-25
_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                76.952(4)
_cell_angle_beta                 72.697(4)
_cell_angle_gamma                86.957(4)
_cell_formula_units_Z            2
_cell_length_a                   16.0344(17)
_cell_length_b                   19.862(2)
_cell_length_c                   20.309(2)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.519
_cell_measurement_theta_min      2.857
_cell_volume                     6015.1(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1437
_diffrn_reflns_av_unetI/netI     0.1142
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            114775
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.843
_exptl_absorpt_coefficient_mu    2.248
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1366 before and 0.0783 after correction.
The Ratio of minimum to maximum transmission is 0.7279.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         1.785
_refine_diff_density_min         -1.373
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1463
_refine_ls_number_reflns         21112
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0722P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12600
_reflns_number_total             21112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11750g2.cif
_cod_data_source_block           1
_cod_database_code               7229672
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.603
_olex2_refinement_description
;
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
 H11-O11
 0.85 with sigma of 0.02
 O22-H22
 0.85 with sigma of 0.02
 H20-H18B
 2.2 with sigma of 0.02
 H11_$1-H11
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C19, O3, C20, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C86) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C81)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C84) \\sim Ueq,
Uanis(C79) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C112) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C56) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C122)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C95) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C45(H45), C34(H34), C49(H49), C28(H28), C44(H44), C98(H98), C10(H10),
 C33(H33), C71(H71), C51(H51), C111(H111), C112(H112), C11(H11A), C72(H72),
 C69(H69), C95(H95), C89(H89), C3(H3), C6(H6), C115(H115), C17(H17), C77(H77),
 C88(H88), C41(H41), C93(H93), C54(H54), C50(H50), C106(H106), C27(H27),
 C25(H25), C42(H42), C76(H76), C110(H110), C8(H8), C78(H78), C105(H105),
 C103(H103), C101(H101), C15(H15), C120(H120), C102(H102), C94(H94), C7(H7),
 C99(H99), C59(H59), C32(H32), C16(H16), C40(H40), C65(H65), C38(H38), C86(H86),
  C64(H64), C23(H23), C4(H4), C37(H37), C21(H21), C24(H24), C84(H84), C67(H67),
 C68(H68), C20(H20), C85(H85), C82(H82), C81(H81)
5.b Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C118(H11B,H11C,H11D), C117(H11E,H11F,H11G), C113(H11H,
 H11I,H11J), C57(H57A,H57B,H57C), C52(H52A,H52B,H52C), C56(H56A,H56B,H56C),
 C96(H96A,H96B,H96C), C122(H12A,H12B,H12C), C35(H35A,H35B,H35C), C1(H1A,H1B,
 H1C), C62(H62A,H62B,H62C), C18(H18A,H18B,H18C), C79(H79A,H79B,H79C)
;
_shelx_res_checksum              805
_olex2_submission_special_instructions 'No special instructions were received'