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_7229680
_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 N6 O11 Yb2), 2.5(C2 H3 N)'
_chemical_formula_sum            'C127 H115.5 N14.5 O22 Yb4'
_chemical_formula_weight         2888.99
_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             2017-08-24
_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                76.9190(10)
_cell_angle_beta                 72.8040(10)
_cell_angle_gamma                87.3730(10)
_cell_formula_units_Z            2
_cell_length_a                   15.9945(6)
_cell_length_b                   19.7881(6)
_cell_length_c                   20.2867(7)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.447
_cell_measurement_theta_min      2.897
_cell_volume                     5973.0(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0643
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            76384
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.897
_exptl_absorpt_coefficient_mu    3.179
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0850 before and 0.0607 after correction.
The Ratio of minimum to maximum transmission is 0.7802.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       block
_exptl_crystal_F_000             2870
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.698
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1547
_refine_ls_number_reflns         20970
_refine_ls_number_restraints     1044
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.009
_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^+36.4214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14201
_reflns_number_total             20970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11750g2.cif
_cod_data_source_block           5
_cod_original_formula_sum        'C127 H115.50 N14.50 O22 Yb4'
_cod_database_code               7229680
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.702
_shelx_estimated_absorpt_t_min   0.504
_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
 N13-C124
 1.1 with sigma of 0.02
 C124-C123
 1.5 with sigma of 0.02
 C128-N14
 1.1 with sigma of 0.02
 C128-C127
 1.5 with sigma of 0.02
 O22-H22
 0.85 with sigma of 0.02
 H11-O11
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N13 \\sim C124 \\sim C123: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C127 \\sim C128 \\sim N14: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Others
 Fixed Sof: C128(0.5) C127(0.5) H12J(0.5) H12K(0.5) H12L(0.5) N14(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C78(H78), C89(H89), C71(H71), C72(H72), C105(H105), C106(H106), C50(H50),
 C88(H88), C95(H95), C33(H33), C11(H11A), C45(H45), C32(H32), C27(H27),
 C110(H110), C77(H77), C34(H34), C51(H51), C49(H49), C93(H93), C111(H111),
 C8(H8), C10(H10), C25(H25), C44(H44), C3(H3), C102(H102), C28(H28), C67(H67),
 C4(H4), C69(H69), C59(H59), C120(H120), C64(H64), C15(H15), C7(H7), C16(H16),
 C94(H94), C42(H42), C112(H112), C101(H101), C76(H76), C115(H115), C65(H65),
 C68(H68), C6(H6), C103(H103), C86(H86), C17(H17), C54(H54), C38(H38), C40(H40),
  C41(H41), C21(H21), C84(H84), C99(H99), C37(H37), C23(H23), C20(H20),
 C85(H85), C98(H98), C82(H82), C81(H81), C24(H24)
5.b Idealised Me refined as rotating group:
 C113(H11B,H11C,H11D), C61(H61A,H61B,H61C), C118(H11E,H11F,H11G), C62(H62A,
 H62B,H62C), C57(H57A,H57B,H57C), C117(H11H,H11I,H11J), C52(H52A,H52B,H52C),
 C122(H12A,H12B,H12C), C56(H56A,H56B,H56C), C1(H1A,H1B,H1C), C35(H35A,H35B,
 H35C), C96(H96A,H96B,H96C), C18(H18A,H18B,H18C), C79(H79A,H79B,H79C),
 C125(H12D,H12E,H12F), C123(H12G,H12H,H12I), C127(H12J,H12K,H12L)
;
_shelx_res_checksum              47207
_olex2_submission_special_instructions 'No special instructions were received'