Magneto-structural correlations in arsenic- and selenium-ligated dysprosium single-molecule magnets
Pugh, Thomas; Vieru, Veacheslav; Chibotaru, Liviu F.; Layfield, Richard A.; Chem. Sci. 7 (2016) 2128–; doi:10.1039/C5SC03755G

data_1540699
_publ_section_title
;
 Magneto-structural correlations in arsenic- and selenium-ligated
 dysprosium single-molecule magnets
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2128
_journal_paper_doi               10.1039/C5SC03755G
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety
'C63 H75 As3 Dy3 Li, 2(C16 H32 Li O4), C4 H8 O'
_chemical_formula_sum            'C99 H147 As3 Dy3 Li3 O9'
_chemical_formula_weight         2214.24
_chemical_name_systematic        3-Dy
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_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   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-05-28 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.470(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4510(4)
_cell_length_b                   15.8357(3)
_cell_length_c                   28.0477(5)
_cell_measurement_reflns_used    43655
_cell_measurement_temperature    150.01(11)
_cell_measurement_theta_max      28.5580
_cell_measurement_theta_min      3.5480
_cell_volume                     9926.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(11)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -36.00   47.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663   77.0000    0.0000 83

  2 omega   -3.00   88.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000  150.0000 91

  3 omega  -50.00   38.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000 -120.0000 88

  4 omega  -14.00   61.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000   90.0000 75

  5 omega    6.00   79.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601 -129.0000  -22.0000 73

  6 omega  -20.00   61.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000 -180.0000 81

  7 omega    6.00   88.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000   30.0000 82

  8 omega   18.00   88.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000  -30.0000 70

  9 omega  -11.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000 -120.0000 100
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0048440000
_diffrn_orient_matrix_UB_12      0.0017257000
_diffrn_orient_matrix_UB_13      0.0245977000
_diffrn_orient_matrix_UB_21      0.0313712000
_diffrn_orient_matrix_UB_22      0.0009293000
_diffrn_orient_matrix_UB_23      0.0062232000
_diffrn_orient_matrix_UB_31      -0.0004245000
_diffrn_orient_matrix_UB_32      0.0447523000
_diffrn_orient_matrix_UB_33      -0.0010631000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            128160
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         3.276
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             4476
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: thf'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.235
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1299
_refine_ls_number_reflns         17494
_refine_ls_number_restraints     401
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+22.8744P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15469
_reflns_number_total             17494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03755g2.cif
_cod_data_source_block           aral252_rered_xprep
_cod_depositor_comments
'Adding full bibliography for 1540697--1540701.cif.'
_cod_database_code               1540699
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         Cr7Zn1O32F8N1C200H200
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 O9-C99
 1.48 with sigma of 0.02
 O9-C96
 1.48 with sigma of 0.02
 C96-C97
 1.53 with sigma of 0.02
 C99-C98
 1.53 with sigma of 0.02
 C98-C97
 1.6 with sigma of 0.02
 C99-C97
 2.38 with sigma of 0.02
 C98-C96
 2.38 with sigma of 0.02
 O9-C98
 2.35 with sigma of 0.02
 O9-C97
 2.35 with sigma of 0.02
 C86-C85
 1.6 with sigma of 0.02
 O9A-C99A
 1.48 with sigma of 0.02
 O9A-C96A
 1.48 with sigma of 0.02
 C99A-C98A
 1.53 with sigma of 0.02
 C96A-C97A
 1.53 with sigma of 0.02
 C97A-C98A
 1.6 with sigma of 0.02
 C99A-C97A
 2.38 with sigma of 0.02
 C96A-C98A
 2.38 with sigma of 0.02
 O9A-C98A
 2.35 with sigma of 0.02
 O9A-C97A
 2.35 with sigma of 0.02
 C87A-C85A
 2.4 with sigma of 0.02
 C86A-C84A
 2.4 with sigma of 0.02
 C87A-C86A
 1.5 with sigma of 0.02
 C84A-C85A
 1.5 with sigma of 0.02
 O6A-C85A
 2.4 with sigma of 0.02
 O6A-C86A
 2.4 with sigma of 0.02
3. Rigid bond restraints
 C80, O5, C83, C82, C81
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O8 \\sim C92 \\sim C93 \\sim C94 \\sim C95: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C80 \\sim O5 \\sim C83 \\sim C82 \\sim C81: within 1.7A with sigma of 0.005 and
sigma for terminal atoms of 0.02
C83A \\sim C82A \\sim C81A \\sim C80A \\sim O5A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(C62) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O9, C96, C97, C98, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, C88, C89, C90, C91
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C84, C85, C86, C87
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9A, C96A, C97A, C98A, C99A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8A, C92A, C93A, C94A, C95A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6A, C84A, C85A, C86A, C87A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7A, C88A, C89A, C90A, C91A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C80, O5, C83, C82, C81
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O9A)=Sof(C96A)=Sof(H96C)=Sof(H96D)=Sof(C97A)=Sof(H97C)=Sof(H97D)=
 Sof(C98A)=Sof(H98C)=Sof(H98D)=Sof(C99A)=Sof(H99C)=Sof(H99D)=1-FVAR(1)
 Sof(O9)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(C98)=
 Sof(H98A)=Sof(H98B)=Sof(C99)=Sof(H99A)=Sof(H99B)=FVAR(1)
 Sof(O8A)=Sof(C92A)=Sof(H92C)=Sof(H92D)=Sof(C93A)=Sof(H93C)=Sof(H93D)=
 Sof(C94A)=Sof(H94C)=Sof(H94D)=Sof(C95A)=Sof(H95C)=Sof(H95D)=1-FVAR(2)
 Sof(O8)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C94)=
 Sof(H94A)=Sof(H94B)=Sof(C95)=Sof(H95A)=Sof(H95B)=FVAR(2)
 Sof(O7A)=Sof(C88A)=Sof(H88C)=Sof(H88D)=Sof(C89A)=Sof(H89C)=Sof(H89D)=
 Sof(C90A)=Sof(H90C)=Sof(H90D)=Sof(C91A)=Sof(H91C)=Sof(H91D)=1-FVAR(3)
 Sof(O7)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(C90)=
 Sof(H90A)=Sof(H90B)=Sof(C91)=Sof(H91A)=Sof(H91B)=FVAR(3)
 Sof(O6A)=Sof(C84A)=Sof(H84C)=Sof(H84D)=Sof(C85A)=Sof(H85C)=Sof(H85D)=
 Sof(C86A)=Sof(H86C)=Sof(H86D)=Sof(C87A)=Sof(H87C)=Sof(H87D)=1-FVAR(4)
 Sof(O6)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=
 Sof(H86A)=Sof(H86B)=Sof(C87)=Sof(H87A)=Sof(H87B)=FVAR(4)
 Sof(C80A)=Sof(H80C)=Sof(H80D)=Sof(C81A)=Sof(H81C)=Sof(H81D)=Sof(C82A)=
 Sof(H82C)=Sof(H82D)=Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(O5A)=1-FVAR(5)
 Sof(O5)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C81)=
 Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=FVAR(5)
7.a Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,
 H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B),
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
  C78(H78A,H78B), C79(H79A,H79B), C84(H84A,H84B), C84A(H84C,H84D), C85(H85A,
 H85B), C85A(H85C,H85D), C86(H86A,H86B), C86A(H86C,H86D), C87(H87A,H87B),
 C87A(H87C,H87D), C88(H88A,H88B), C88A(H88C,H88D), C89(H89A,H89B), C89A(H89C,
 H89D), C90(H90A,H90B), C90A(H90C,H90D), C91(H91A,H91B), C91A(H91C,H91D),
 C92(H92A,H92B), C92A(H92C,H92D), C93(H93A,H93B), C93A(H93C,H93D), C94(H94A,
 H94B), C94A(H94C,H94D), C95(H95A,H95B), C95A(H95C,H95D), C96(H96A,H96B),
 C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C96A(H96C,H96D), C97A(H97C,
 H97D), C98A(H98C,H98D), C99A(H99C,H99D), C80(H80A,H80B), C83(H83A,H83B),
 C81(H81A,H81B), C82(H82A,H82B), C80A(H80C,H80D), C81A(H81C,H81D), C82A(H82C,
 H82D), C83A(H83C,H83D)
7.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C2AA(H2AA), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10),
 C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22),
  C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33),
 C34(H34), C39(H39), C41(H41), C48(H48), C50(H50), C57(H57), C59(H59)
7.c Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C24(H24A,H24B,
 H24C), C30(H30A,H30B,H30C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C)
;
_shelx_res_checksum              49730
_olex2_submission_special_instructions 'No special instructions were received'