Dy<sup>III</sup> single-molecule magnets from ligands incorporating both amine and acylhydrazine Schiff base groups: the centrosymmetric {Dy<sub>2</sub>} displaying dual magnetic relaxation behaviors.
Su, Sen-Da; Li, Jia-Xin; Xu, Fan; Wang, Chen-Xiao; Wang, Kai; Li, Yan; Zhang, Shu-Hua; Zhang, Xiu-Qing; Zhang, Yi-Quan; Liang, Fu-Pei; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15739–15749; doi:10.1039/c9dt04434e

data_7705724
_publ_section_title
;
 Dy<sup>III</sup> single-molecule magnets from ligands incorporating both
 amine and acylhydrazine Schiff base groups: the centrosymmetric
 {Dy<sub>2</sub>} displaying dual magnetic relaxation behaviors.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15739
_journal_page_last               15749
_journal_paper_doi               10.1039/c9dt04434e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'2(C88 H76 Dy6 N12 O21), 17.5(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C193.5 H226 Dy12 N24 O61.5'
_chemical_formula_weight         5821.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-10-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-15 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.804(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8663(14)
_cell_length_b                   25.6934(13)
_cell_length_c                   33.2952(17)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.49
_cell_volume                     21197.6(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            232949
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.107
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.258
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5973
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       block
_exptl_crystal_F_000             11354
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.478
_refine_diff_density_min         -2.328
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2633
_refine_ls_number_reflns         37614
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0614P)^2^+230.0560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25050
_reflns_number_total             37614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04434e2.cif
_cod_data_source_block           3-dy6
_cod_depositor_comments
'Adding full bibliography for 7705722--7705724.cif.'
_cod_original_formula_sum        'C193.50 H226 Dy12 N24 O61.50'
_cod_database_code               7705724
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.727
_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, All C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Restrained distances
 O61-C195
 1.45 with sigma of 0.01
 O47-C181 = O47A-C181
 1.46 with sigma of 0.01
 O51-C185
 1.46 with sigma of 0.01
 O20-C87
 1.46 with sigma of 0.01
 O64-C196
 1.48 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C181) \\sim Ueq, Uanis(O47) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O47A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O61) \\sim Ueq, Uanis(C195) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C164) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C100) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C175) \\sim Ueq, Uanis(O41) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O64) \\sim Ueq, Uanis(C196) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O47) = Uanis(O47A)
Uanis(C110) = Uanis(O28)
Uanis(O20) = Uanis(C87)
4. Others
 Fixed Sof: O43(0.5) H43(0.5) C177(0.5) H17M(0.5) H17N(0.5) H17O(0.5) O44(0.5)
 H44(0.5) C178(0.5) H17P(0.5) H17Q(0.5) H17R(0.5) O47(0.75) H47(0.75)
 O47A(0.25) H47A(0.25) H18B(0.75) H18C(0.75) H18D(0.75) H18E(0.25) H18F(0.25)
 H18G(0.25) O51(0.75) H51A(0.75) C185(0.75) H18T(0.75) H18U(0.75) H18V(0.75)
 O58(0.75) H58(0.75) C192(0.75) H19H(0.75) H19I(0.75) H19J(0.75) O60(0.75)
 H60A(0.75) C194(0.75) H19N(0.75) H19O(0.75) H19P(0.75) O61(0.75) H61A(0.75)
 C195(0.75) H19Q(0.75) H19R(0.75) H19S(0.75) O64(0.5) H64A(0.5) C196(0.5)
 H19T(0.5) H19U(0.5) H19V(0.5)
 Fixed U11: C88(0.048273) C173(0.043671) C175(0.041017) O47(0.074928)
 O47A(0.074928) C181(0.074928) O49(0.04816) C183(0.04816) C194(0.074928)
 Fixed U12: C88(0.001288) C173(-0.006109) C175(-0.008599) O47(-0.001808) O47A(-
 0.001808) C181(-0.001808) O49(-0.008687) C183(-0.008687) C194(-0.001808)
 Fixed U13: C88(-0.003012) C173(0.015021) C175(0.025595) O47(0.003155)
 O47A(0.003155) C181(0.003155) O49(-0.009929) C183(-0.009929) C194(0.003155)
 Fixed U22: C88(0.06297) C173(0.05685) C175(0.0645) O47(0.04136) O47A(0.04136)
 C181(0.04136) O49(0.0656) C183(0.0656) C194(0.04136)
 Fixed U23: C88(0.00366) C173(-0.02105) C175(-0.01625) O47(-0.00129) O47A(-
 0.00129) C181(-0.00129) O49(-0.01079) C183(-0.01079) C194(-0.00129)
 Fixed U33: C88(0.04826) C173(0.05674) C175(0.06681) O47(0.08998)
 O47A(0.08998) C181(0.08998) O49(0.06919) C183(0.06919) C194(0.08998)
5.a Riding coordinates:
 O4(H4), O5(H5), O12(H12), O13(H13), O18(H18), O19(H19), O20(H20), O21(H21),
 C87(H87A,H87B,H87C), O23(H23A), O24(H24A), O33(H33A), O34(H34A), O39(H39A),
 O40(H40A), O41(H41A), O42(H42A), O43(H43), O44(H44), O45(H45A), C179(H17S,H17T,
 H17U), O46(H46), O47(H47), O47A(H47A), O48(H48A), O49(H49), O50(H50),
 C184(H18Q,H18R,H18S), O51(H51A), O52(H52A), O53(H53A), O54(H54A), O55(H55),
 O56(H56), O57(H57A), O58(H58), O59(H59), O60(H60A), O61(H61A), O62(H62A,H62B),
 O63(H63A,H63B), O64(H64A)
5.b Me refined with riding coordinates:
 C176(H17J,H17K,H17L)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12A), C15(H15), C18(H18A),
 C19(H19A), C20(H20A), C21(H21A), C22(H22), C23(H23), C24(H24), C25(H25),
 C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
  C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45), C48(H48),
 C51(H51), C52(H52), C53(H53), C54(H54), C57(H57), C60(H60), C61(H61), C62(H62),
  C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C70(H70), C73(H73),
 C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81),
  C82(H82), C83(H83), C84(H84), C90(H90), C93(H93), C94(H94), C95(H95),
 C96(H96), C99(H99), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106),
  C107(H107), C108(H108), C109(H109), C111(H111), C114(H114), C115(H115),
 C116(H116), C117(H117), C120(H120), C123(H123), C124(H124), C125(H125),
 C126(H126), C127(H127), C128(H128), C129(H129), C130(H130), C133(H133),
 C136(H136), C139(H139), C140(H140), C141(H141), C142(H142), C145(H145),
 C148(H148), C149(H149), C150(H150), C151(H151), C152(H152), C153(H153),
 C154(H154), C155(H155), C158(H158), C161(H161), C162(H162), C163(H163),
 C164(H164), C165(H165), C166(H166), C167(H167), C168(H168), C169(H169),
 C170(H170), C171(H171), C172(H172)
5.d Idealised Me refined as rotating group:
 C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C88(H88A,H88B,H88C), C173(H17A,H17B,
 H17C), C174(H17D,H17E,H17F), C175(H17G,H17H,H17I), C177(H17M,H17N,H17O),
 C178(H17P,H17Q,H17R), C180(H18H,H18I,H18J), C181(H18B,H18C,H18D), C181(H18E,
 H18F,H18G), C182(H18K,H18L,H18M), C183(H18N,H18O,H18P), C185(H18T,H18U,H18V),
 C186(H18W,H18X,H18Y), C187(H18Z,H,HA), C188(H1,HB,HC), C189(H2,HD,HE),
 C190(H19B,H19C,H19D), C191(H19E,H19F,H19G), C192(H19H,H19I,H19J), C193(H19K,
 H19L,H19M), C194(H19N,H19O,H19P), C195(H19Q,H19R,H19S), C196(H19T,H19U,H19V)
;
_shelx_res_checksum              66166
_olex2_submission_special_instructions 'No special instructions were received'