Di- and octa-nuclear dysprosium clusters derived from pyridyl-triazole based ligand: {Dy2} showing single molecule magnetic behaviour.
Akhtar, Muhammad Nadeem; Liao, Xiao-Fen; Chen, Yan-Cong; Liu, Jun-Liang; Tong, Ming-Liang; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2981–2987; doi:10.1039/c7dt00047b

data_7041964
_publ_section_title
;
 Di- and octa-nuclear dysprosium clusters derived from pyridyl-triazole
 based ligand: {Dy2} showing single molecule magnetic behaviour.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2981
_journal_page_last               2987
_journal_paper_doi               10.1039/c7dt00047b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C128 H104 Dy8 N64 O8, 6(O)'
_chemical_formula_sum            'C128 H152 Dy8 N64 O32'
_chemical_formula_weight         4399.13
_chemical_name_systematic        '{Dy8} (2)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2017-01-30 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.674(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.003(2)
_cell_length_b                   30.483(3)
_cell_length_c                   24.946(2)
_cell_measurement_reflns_used    38656
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.375
_cell_measurement_theta_min      3.025
_cell_volume                     15851(2)
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1663
_diffrn_reflns_av_unetI/netI     0.2357
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            84103
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.590
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.812
_exptl_absorpt_correction_T_max  0.6792
_exptl_absorpt_correction_T_min  0.18
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             8608
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         4.039
_refine_diff_density_min         -2.884
_refine_diff_density_rms         0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1927
_refine_ls_number_reflns         33757
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.2193
_refine_ls_R_factor_gt           0.1108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1445P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2430
_refine_ls_wR_factor_ref         0.3112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14528
_reflns_number_total             33757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00047b2.cif
_cod_data_source_block           Dy8_2
_cod_depositor_comments
'Adding full bibliography for 7041963--7041964.cif.'
_cod_database_code               7041964
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.679
_shelx_estimated_absorpt_t_min   0.547
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H5 of O5, H1 of O1, H2 of O2, H3 of O3, H4 of O4, H7 of O7,
   H8 of O8, All C(H,H) groups
 At 1.5 times of:
  H6 of O6
2. Rigid bond restraints
 C98, C99
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C35, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C93, C94
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N43, C87
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C66, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C94, C95
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N11) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(N23) \\sim Ueq, Uanis(N34)
\\sim Ueq, Uanis(N35) \\sim Ueq, Uanis(N41) \\sim Ueq, Uanis(N48) \\sim Ueq,
Uanis(N51) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O3W) \\sim Ueq, Uanis(O5W)
\\sim Ueq, Uanis(O6W) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C56) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C115) \\sim Ueq,
Uanis(C126) \\sim Ueq, Uanis(C127) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N19) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C80) \\sim Ueq,
Uanis(C95) \\sim Ueq, Uanis(C103) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(N38)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C86) \\sim Ueq,
Uanis(C88) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C121) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 O1(H1), O2(H2), O3(H3), O4(H4), O5(H5), O6(H6), O7(H7), O8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C24(H24A,H24B), C25(H25A,H25B), C40(H40A,H40B),
 C41(H41A,H41B), C56(H56A,H56B), C57(H57A,H57B), C72(H72A,H72B), C73(H73A,H73B),
  C88(H88A,H88B), C89(H89A,H89B), C104(H10A,H10B), C105(H10C,H10D), C120(H12A,
 H12B), C121(H12C,H12D)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C45(H45), C46(H46), C47(H47),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C61(H61), C62(H62), C63(H63),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C77(H77), C78(H78),
 C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C93(H93), C94(H94),
  C95(H95), C96(H96), C97(H97), C98(H98), C99(H99), C100(H100), C109(H109),
 C110(H110), C111(H111), C112(H112), C113(H113), C114(H114), C115(H115),
 C116(H116), C125(H125), C126(H126), C127(H127), C128(H128)
;
_olex2_date_sample_data_collection 2011-10-10
_olex2_submission_special_instructions 'No special instructions were received'