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_7229681
_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 Tb2), C2 H3 N'
_chemical_formula_sum            'C124 H111 N13 O22 Tb4'
_chemical_formula_weight         2770.93
_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             2017-08-25
_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                76.7080(10)
_cell_angle_beta                 73.0480(10)
_cell_angle_gamma                87.7160(10)
_cell_formula_units_Z            2
_cell_length_a                   16.0380(6)
_cell_length_b                   19.7829(8)
_cell_length_c                   20.3633(8)
_cell_measurement_reflns_used    9098
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      3.1
_cell_volume                     6012.0(4)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0497
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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            255204
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.891
_exptl_absorpt_coefficient_mu    2.397
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       block
_exptl_crystal_F_000             2764
_platon_squeeze_details
;
;
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1491
_refine_ls_number_reflns         21167
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+23.6665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17905
_reflns_number_total             21167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11750g2.cif
_cod_data_source_block           2
_cod_database_code               7229681
_shelx_shelxl_version_number     2016/6
_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. Uiso/Uaniso restraints and constraints
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(O12) \\sim Ueq,
Uanis(C62) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C102) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(O16)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C101(H101), C67(H67), C65(H65), C64(H64), C68(H68), C95(H95), C105(H105),
 C72(H72), C106(H106), C71(H71), C102(H102), C78(H78), C81(H81), C120(H120),
 C115(H115), C110(H110), C94(H94), C111(H111), C93(H93), C82(H82), C86(H86),
 C89(H89), C84(H84), C85(H85), C99(H99), C76(H76), C77(H77), C69(H69), C88(H88),
  C98(H98), C112(H112), C103(H103), C17(H17), C59(H59), C20(H20), C4(H4),
 C40(H40), C38(H38), C41(H41), C6(H6), C45(H45), C16(H16), C37(H37), C51(H51),
 C7(H7), C50(H50), C49(H49), C33(H33), C28(H28), C10(H10), C44(H44), C15(H15),
 C23(H23), C11(H11J), C27(H27), C8(H8), C24(H24), C42(H42), C25(H25), C54(H54),
 C32(H32), C21(H21), C34(H34), C3(H3)
3.b Idealised Me refined as rotating group:
 C117(H11A,H11B,H11C), C113(H11D,H11E,H11F), C122(H12A,H12B,H12C), C118(H11G,
 H11H,H11I), C96(H96A,H96B,H96C), C62(H62A,H62B,H62C), C79(H79A,H79B,H79C),
 C1(H1A,H1B,H1C), C56(H56A,H56B,H56C), C18(H18A,H18B,H18C), C35(H35A,H35B,H35C),
  C52(H52A,H52B,H52C), C61(H61A,H61B,H61C), C57(H57A,H57B,H57C), C123(H12D,H12E,
 H12F)
;
_shelx_res_checksum              14677
_olex2_submission_special_instructions 'No special instructions were received'