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_1544644
_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 Sb4 Y3, C7 H8'
_chemical_formula_sum            'C70 H83 Sb4 Y3'
_chemical_formula_weight         1678.09
_chemical_melting_point          ?
_chemical_name_systematic        2-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     heavy
_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                 107.004(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8643(4)
_cell_length_b                   19.3840(3)
_cell_length_c                   24.2728(7)
_cell_measurement_reflns_used    6901
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      22.9400
_cell_measurement_theta_min      3.4440
_cell_volume                     6688.0(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
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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 16.1428
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   25.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663   57.0000  -30.0000 25

  2 omega   -3.00   78.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038   57.0000 -150.0000 81

  3 omega   50.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038 -129.0000 -168.0000 27

  4 omega  -31.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038  -19.0000  120.0000 94

  5 omega  -87.00   -4.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000 -120.0000 83

  6 omega  -88.00    9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000  -30.0000 97

  7 omega  -94.00  -68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  178.0000  120.0000 26
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0356348000
_diffrn_orient_matrix_UB_12      -0.0244594000
_diffrn_orient_matrix_UB_13      -0.0134383000
_diffrn_orient_matrix_UB_21      0.0329417000
_diffrn_orient_matrix_UB_22      -0.0271729000
_diffrn_orient_matrix_UB_23      0.0105531000
_diffrn_orient_matrix_UB_31      -0.0133422000
_diffrn_orient_matrix_UB_32      -0.0016609000
_diffrn_orient_matrix_UB_33      0.0253270000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25440
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.369
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             3296
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Flack x determined using 3244 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.021(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         11082
_refine_ls_number_restraints     394
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0283P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    0.815
_reflns_Friedel_fraction_max     0.811
_reflns_number_gt                8834
_reflns_number_total             11082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04465d2.cif
_cod_data_source_block           aral302_rered_xprep
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'N/A' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1544644--1544648.cif.

 Adding full bibliography for 1544644--1544648.cif.
;
_cod_database_code               1544644
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         Y3Sb3C70H86
_reflns_odcompleteness_completeness 99.79
_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 distances
 C70A-C64A
 2.5 with sigma of 0.02
 C70A-C68A
 2.5 with sigma of 0.02
 C68-C70
 2.5 with sigma of 0.02
 C64-C70
 2.5 with sigma of 0.02
 C70-C64
 2.45 with sigma of 0.02
 C68-C70
 2.45 with sigma of 0.02
 H70B-C64
 2.49 with sigma of 0.02
3. Restrained planarity
 C64, C65, C66, C67, C68, C69, C70
 with sigma of 0.1
4. Rigid bond restraints
 C64A, C65A, C66A, C67A, C68A, C69A, C70A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C25, C26, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C17, C13, C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C35, C34, C33, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C62, C58, C59, C60, C63, C55, C56, C57, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C64A \\sim C65A \\sim C66A \\sim C67A \\sim C68A \\sim C69A \\sim C70A: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C16 \\sim C17 \\sim C13 \\sim C14 \\sim C15: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C34 \\sim C35 \\sim C31 \\sim C32 \\sim C33: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C63 \\sim C60 \\sim C59 \\sim C58 \\sim C57 \\sim C56 \\sim C55 \\sim C61 \\sim
C62: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C65A) \\sim Ueq, Uanis(C66A) \\sim Ueq, Uanis(C64A) \\sim Ueq,
Uanis(C69A) \\sim Ueq, Uanis(C70A) \\sim Ueq, Uanis(C67A) \\sim Ueq,
Uanis(C68A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C70) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
6. Others
 Sof(C69A)=Sof(C68A)=Sof(H68A)=Sof(C67A)=Sof(H67A)=Sof(C66A)=Sof(H66A)=
 Sof(C65A)=Sof(H65A)=Sof(C64A)=Sof(H64A)=Sof(C70A)=Sof(H70D)=Sof(H70E)=
 Sof(H70F)=1-FVAR(1)
 Sof(C68)=Sof(H68)=Sof(C69)=Sof(C64)=Sof(H64)=Sof(C65)=Sof(H65)=Sof(C66)=
 Sof(H66)=Sof(C67)=Sof(H67)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=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), C68(H68), C64(H64),
  C65(H65), C66(H66), C67(H67), C68A(H68A), C67A(H67A), C66A(H66A), C65A(H65A),
 C64A(H64A)
7.b Fitted hexagon refined as free rotating group:
 C68(C69,C64,C65,C66,C67), C69A(C68A,C67A,C66A,C65A,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), C70(H70A,H70B,H70C), C70A(H70D,H70E,H70F)
;
_shelx_res_checksum              30567
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Toluene