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_7229675
_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 Dy2 N6 O11), 2.5(C2 H3 N)'
_chemical_formula_sum            'C127 H115.5 Dy4 N14.5 O22'
_chemical_formula_weight         2846.83
_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                76.789(3)
_cell_angle_beta                 73.047(3)
_cell_angle_gamma                87.924(4)
_cell_formula_units_Z            2
_cell_length_a                   15.8898(9)
_cell_length_b                   19.6837(12)
_cell_length_c                   20.3485(9)
_cell_measurement_reflns_used    17272
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5923.6(6)
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_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       -24
_diffrn_reflns_number            65209
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.056
_exptl_absorpt_coefficient_mu    2.570
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2838
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1619
_refine_ls_number_reflns         20695
_refine_ls_number_restraints     904
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17641
_reflns_number_total             20695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra11750g2.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C127 H115.50 Dy4 N14.50 O22'
_cod_database_code               7229675
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.769
_shelx_estimated_absorpt_t_min   0.627
_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
 C88-C89 = C88-C89'
 1.52 with sigma of 0.01
 H22-O22
 0.84 with sigma of 0.02
 H11-O11
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq,
Uanis(C112) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N5)
\\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(N8) \\sim Ueq,
Uanis(N9) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(N12)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq,
Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq,
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq,
Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77)
\\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq,
Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq,
Uanis(C88) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91)
\\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq,
Uanis(O15') \\sim Ueq, Uanis(C89') \\sim Ueq, Uanis(C90') \\sim Ueq,
Uanis(C91') \\sim Ueq, Uanis(C92') \\sim Ueq, Uanis(C93') \\sim Ueq,
Uanis(C94') \\sim Ueq, Uanis(C95') \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C97)
\\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C100) \\sim Ueq,
Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq,
Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C109) \\sim Ueq,
Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C115) \\sim Ueq,
Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C118) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C121) \\sim Ueq,
Uanis(C122) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C124)
\\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq,
Uanis(N15) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H88(0.55) H88A(0.45) O15(0.55) C89(0.55) C90(0.55) H90(0.55)
 C91(0.55) H91(0.55) C92(0.55) C93(0.55) H93(0.55) C94(0.55) H94(0.55)
 C95(0.55) H95A(0.55) H95B(0.55) H95C(0.55) O15'(0.45) C89'(0.45) C90'(0.45)
 H90'(0.45) C91'(0.45) H91'(0.45) C92'(0.45) C93'(0.45) H93'(0.45) C94'(0.45)
 H94'(0.45) C95'(0.45) H95D(0.45) H95E(0.45) H95F(0.45) N15(0.5) C127(0.5)
 C128(0.5) H12J(0.5) H12K(0.5) H12L(0.5)
5.a Riding coordinates:
 C57(H57A,H57B,H57C)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C11(H11M), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C27(H27),
  C29(H29), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37),
 C40(H40), C41(H41), C44(H44), C46(H46), C47(H47), C49(H49), C50(H50), C54(H54),
  C59(H59), C62(H62), C63(H63), C64(H64), C67(H67), C68(H68), C71(H71),
 C73(H73), C74(H74), C76(H76), C77(H77), C79(H79), C80(H80), C81(H81), C84(H84),
  C85(H85), C88(H88), C88(H88A), C90(H90), C91(H91), C93(H93), C94(H94),
 C90'(H90'), C91'(H91'), C93'(H93'), C94'(H94'), C96(H96), C97(H97), C98(H98),
 C101(H101), C102(H102), C105(H105), C107(H107), C108(H108), C110(H110),
 C111(H111), C115(H115), C120(H120)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C34(H34A,H34B,H34C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C56(H56A,H56B,H56C), C61(H61A,H61B,H61C), C78(H78A,H78B,H78C), C95(H95A,
 H95B,H95C), C95'(H95D,H95E,H95F), C112(H11A,H11B,H11C), C113(H11D,H11E,H11F),
 C117(H11G,H11H,H11I), C118(H11J,H11K,H11L), C122(H12A,H12B,H12C), C124(H12D,
 H12E,H12F), C126(H12G,H12H,H12I), C128(H12J,H12K,H12L)
;
_shelx_res_checksum              16467
_olex2_submission_special_instructions 'No special instructions were received'