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_1544645
_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 Dy3 Sb4, C7 H8'
_chemical_formula_sum            'C70 H83 Dy3 Sb4'
_chemical_formula_weight         1898.86
_chemical_name_systematic        2-Dy
_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             2015-07-17
_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                 106.568(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8968(3)
_cell_length_b                   19.3308(4)
_cell_length_c                   24.2616(5)
_cell_measurement_reflns_used    19363
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      27.6610
_cell_measurement_theta_min      3.6750
_cell_volume                     6696.5(2)
_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      150.02(10)
_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   -7.00   91.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   37.0000    0.0000 98

  2 omega   13.00   61.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000  -60.0000 48

  3 omega  -20.00   61.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000  120.0000 81

  4 omega  -49.00   40.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000    0.0000 89

  5 omega  -16.00   51.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663   57.0000  -90.0000 67

  6 omega   35.00   95.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  178.0000  -60.0000 60

  7 omega  -87.00   -4.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -57.0000  120.0000 83

  8 omega  -88.00   10.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000   30.0000 98

  9 omega  -86.00   10.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000 -120.0000 96
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0302894000
_diffrn_orient_matrix_UB_12      -0.0265648000
_diffrn_orient_matrix_UB_13      0.0041131000
_diffrn_orient_matrix_UB_21      0.0393802000
_diffrn_orient_matrix_UB_22      -0.0200542000
_diffrn_orient_matrix_UB_23      0.0148310000
_diffrn_orient_matrix_UB_31      -0.0010029000
_diffrn_orient_matrix_UB_32      0.0154182000
_diffrn_orient_matrix_UB_33      0.0263399000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            46304
_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         3.369
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.930
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78068
_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 dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_description       block
_exptl_crystal_F_000             3620
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 5503 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.015(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         13695
_refine_ls_number_restraints     455
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0156P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0615
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12454
_reflns_number_total             13695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04465d2.cif
_cod_data_source_block           aral306_rered_xprep
_cod_depositor_comments
;Adding full bibliography for 1544644--1544648.cif.

 Adding full bibliography for 1544644--1544648.cif.
;
_cod_database_code               1544645
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         Dy3Sb4C70H83
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 C64A, C65A, C66A, C67A, C68A, C69A, C70A
 with sigma of 0.1
3. Rigid bond restraints
 C64A, C65A, C66A, C67A, C68A, C69A, C70A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C64, C65, C66, C67, C68, C69, C70
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C20, C19, C23, C22, C21, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C34, C33, C32, C31, C35, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C64A \\sim C65A \\sim C66A \\sim C67A \\sim C68A \\sim C69A \\sim C70A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C20 \\sim C19 \\sim C23 \\sim C22 \\sim C21 \\sim C24: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C36 \\sim C35 \\sim C34 \\sim C33 \\sim C32 \\sim C31: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C66A) \\sim Ueq, Uanis(C64A) \\sim Ueq, Uanis(C65A) \\sim Ueq,
Uanis(C69A) \\sim Ueq, Uanis(C70A) \\sim Ueq, Uanis(C68A) \\sim Ueq,
Uanis(C67A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C70) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. 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
6. Others
 Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66A)=Sof(C67A)=Sof(H67A)=Sof(C68A)=
 Sof(H68A)=Sof(C69A)=Sof(C64A)=Sof(H64A)=Sof(C70A)=Sof(H70A)=Sof(H70B)=
 Sof(H70C)=1-FVAR(1)
 Sof(C65)=Sof(H65)=Sof(C64)=Sof(H64)=Sof(C69)=Sof(C68)=Sof(H68)=Sof(C67)=
 Sof(H67)=Sof(C66)=Sof(H66)=Sof(C70)=Sof(H70D)=Sof(H70E)=Sof(H70F)=FVAR(1)
7.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), C59(H59), C65(H65), C64(H64),
  C68(H68), C67(H67), C66(H66), C65A(H65A), C66A(H66A), C67A(H67A), C68A(H68A),
 C64A(H64A)
7.b Fitted hexagon refined as free rotating group:
 C65(C64,C69,C68,C67,C66), C65A(C66A,C67A,C68A,C69A,C64A)
7.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), C70A(H70A,H70B,H70C), C70(H70D,H70E,H70F)
;
_shelx_res_checksum              6391
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Toluene