Antimony-ligated dysprosium single-molecule magnets as catalysts for stibine dehydrocoupling.
Pugh, Thomas; Chilton, Nicholas F.; Layfield, Richard A.; Chemical science 8 (2017) 2073–2080; doi:10.1039/c6sc04465d

data_1544647
_publ_section_title
;
 Antimony-ligated dysprosium single-molecule magnets as catalysts for
 stibine dehydrocoupling.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              2073
_journal_page_last               2080
_journal_paper_doi               10.1039/c6sc04465d
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C63 H75 Sb3 Y3, C7 H8'
_chemical_formula_sum            'C70 H83 Sb3 Y3'
_chemical_formula_weight         1556.34
_chemical_name_systematic        1-Y
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-06-10 deposited with the CCDC.
2016-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.4370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1052(2)
_cell_length_b                   18.7715(2)
_cell_length_c                   24.1263(3)
_cell_measurement_reflns_used    50976
_cell_measurement_temperature    150.02(11)
_cell_measurement_theta_max      28.2270
_cell_measurement_theta_min      3.3850
_cell_volume                     6653.68(14)
_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)'
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_diffrn_ambient_temperature      150.02(11)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -3.00   88.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000  150.0000 91

  2 omega   -3.00   88.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000  -60.0000 91

  3 omega  -20.00   61.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000    0.0000 81

  4 omega  -11.00   89.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000   30.0000 100

  5 omega  -20.00   61.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000 -120.0000 81

  6 omega  -50.00   40.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000  150.0000 90

  7 omega  -20.00   61.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000   90.0000 81

  8 omega  -50.00   40.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000 -120.0000 90

  9 omega  -11.00   89.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000 -150.0000 100

 10 omega  -94.00  -35.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663 -178.0000  -30.0000 59

 11 omega  -94.00  -35.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663 -178.0000   60.0000 59

 12 omega  -94.00  -35.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663 -178.0000  -60.0000 59

 13 omega  -20.00   61.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000  150.0000 81

 14 omega  -20.00   61.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000  -60.0000 81

 15 omega  -11.00   89.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000  -30.0000 100

 16 omega  -50.00   40.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000    0.0000 90

 17 omega  -94.00  -34.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  178.0000   30.0000 60

 18 omega  -54.00   92.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601    0.0000 -150.0000 146

 19 omega  -54.00   92.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601    0.0000 -120.0000 146

 20 omega  -54.00   92.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601    0.0000  -90.0000 146

 21 omega  -54.00   58.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601    0.0000  -60.0000 112

 22 omega  -54.00   92.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601    0.0000 -180.0000 146
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0000037000
_diffrn_orient_matrix_UB_12      -0.0348225000
_diffrn_orient_matrix_UB_13      -0.0114229000
_diffrn_orient_matrix_UB_21      0.0482758000
_diffrn_orient_matrix_UB_22      0.0000123000
_diffrn_orient_matrix_UB_23      0.0069926000
_diffrn_orient_matrix_UB_31      0.0000480000
_diffrn_orient_matrix_UB_32      -0.0146895000
_diffrn_orient_matrix_UB_33      0.0270920000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_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       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            135283
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.390
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83551
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             3092
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 6090 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.0240(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         13580
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+5.1206P]
 where P=(Fo^2^+2Fc^2^)/3
;
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_refine_ls_wR_factor_gt          0.0445
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_reflns_number_gt                12910
_reflns_number_total             13580
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_cod_data_source_block           aral270_rered_xprep
_cod_depositor_comments
;Adding full bibliography for 1544644--1544648.cif.

 Adding full bibliography for 1544644--1544648.cif.
;
_cod_database_code               1544647
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C9N3H12O2Na1.H2O2
_reflns_odcompleteness_completeness 99.77
_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
 C37A-C43A
 2.66 with sigma of 0.02
 C41A-C45A
 2.5 with sigma of 0.02
 C37A-C45A
 2.54 with sigma of 0.02
 C53A-C48A = C39A-C44A
 2.52 with sigma of 0.02
 C41A-C44A
 2.52 with sigma of 0.02
 C43A-C39A
 2.52 with sigma of 0.02
 C37A-C43A
 2.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C63A) \\sim Ueq, Uanis(C61A) \\sim Ueq, Uanis(C62A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C55A) \\sim Ueq, Uanis(C56A) \\sim Ueq, Uanis(C60A) \\sim Ueq,
Uanis(C59A) \\sim Ueq, Uanis(C58A) \\sim Ueq, Uanis(C57A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C45A) = Uanis(C42A) = Uanis(C37A) = Uanis(C38A) = Uanis(C43A) =
Uanis(C39A) = Uanis(C41A) = Uanis(C40A) = Uanis(C44A)
4. Rigid body (RIGU) restrains
 C46, C47, C48, C49, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Sb1, C37, C38, C39, C40, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46A, C51A, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Sb1A, C37A, C42A, C43A, C44A, C45A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59A, C55A, C56A, C57A, C58A, C60A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Sb2A)=Sof(C50A)=Sof(H50A)=Sof(C49A)=Sof(C48A)=Sof(H48A)=Sof(C47A)=
 Sof(C46A)=Sof(C51A)=Sof(C52A)=Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C53A)=
 Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(1)
 Sof(Sb2)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(C50)=Sof(H50)=
 Sof(C51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(1)
 Sof(Sb3A)=Sof(C57A)=Sof(H57A)=Sof(C58A)=Sof(H59B)=Sof(C60A)=Sof(C55A)=
 Sof(C56A)=Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=Sof(C62A)=Sof(H62D)=
 Sof(H62E)=Sof(H62F)=Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=1-FVAR(2)
 Sof(Sb3)=Sof(C55)=Sof(C56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(C60)=Sof(C61)=
 Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63)=
 Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(H59A)=FVAR(2)
 Sof(Sb1A)=Sof(C41A)=Sof(H41A)=Sof(C40A)=Sof(C39A)=Sof(H39A)=Sof(C38A)=
 Sof(C37A)=Sof(C42A)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44A)=
 Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(3)
 Sof(Sb1)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(C41)=Sof(H41)=
 Sof(C42)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), 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), C41A(H41A), C39A(H39A),
 C50A(H50A), C48A(H48A), C57A(H57A), C59A(H59A), C59A(H59B), C67(H67), C68(H68),
  C64(H64), C65(H65), C66(H66)
6.b Fitted hexagon refined as free rotating group:
 C41A(C40A,C39A,C38A,C37A,C42A), C50A(C49A,C48A,C47A,C46A,C51A), C57A(C58A,
 C59A,C60A,C55A,C56A), C67(C68,C69,C64,C65,C66)
6.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), 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), C43A(H43D,H43E,H43F), C44A(H44D,H44E,H44F), C45A(H45D,H45E,H45F),
 C52A(H52D,H52E,H52F), C53A(H53D,H53E,H53F), C54A(H54D,H54E,H54F), C61A(H61D,
 H61E,H61F), C62A(H62D,H62E,H62F), C63A(H63D,H63E,H63F), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              94394
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Toluene