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_1544648
_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         'C18 H24 Sb2'
_chemical_formula_sum            'C18 H24 Sb2'
_chemical_formula_weight         483.87
_chemical_name_systematic        Dimesityldistibine
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-14
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_audit_update_record
;
2016-06-14 deposited with the CCDC.
2016-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                88.921(4)
_cell_angle_beta                 79.679(4)
_cell_angle_gamma                73.714(4)
_cell_formula_units_Z            1
_cell_length_a                   5.1740(2)
_cell_length_b                   7.9835(4)
_cell_length_c                   11.2694(5)
_cell_measurement_reflns_used    3194
_cell_measurement_temperature    150.01(13)
_cell_measurement_theta_max      28.4150
_cell_measurement_theta_min      4.1600
_cell_volume                     439.35(4)
_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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(13)
_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  -47.00   40.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000    0.0000 87

  2 omega   10.00   43.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601 -125.0000  131.0000 33

  3 omega   48.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601 -125.0000  131.0000 25

  4 omega  -38.00   25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000  -90.0000 63

  5 omega    4.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000 -180.0000 69

  6 omega    6.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000  -90.0000 81

  7 omega   19.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000   90.0000 56

  8 omega  -11.00   89.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000    0.0000 100

  9 omega  -50.00   40.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000  120.0000 90

 10 omega  -84.00  -35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663 -178.0000  120.0000 49

 11 omega  -75.00  -46.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  125.0000 -150.0000 29
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
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_diffrn_orient_matrix_UB_21      -0.0950985000
_diffrn_orient_matrix_UB_22      0.0840820000
_diffrn_orient_matrix_UB_23      0.0099681000
_diffrn_orient_matrix_UB_31      0.1097064000
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_diffrn_orient_matrix_UB_33      -0.0048161000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5797
_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         26.369
_diffrn_reflns_theta_min         3.677
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.064
_exptl_absorpt_correction_T_max  1.00000
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_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 colourless'
_exptl_crystal_colour_lustre     clear
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_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_description       plate
_exptl_crystal_F_000             234
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_refine_diff_density_max         0.373
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_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0308
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+0.1181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                1499
_reflns_number_total             1798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04465d2.cif
_cod_data_source_block           aral256_rered_xprep
_cod_depositor_comments
;Adding full bibliography for 1544644--1544648.cif.

 Adding full bibliography for 1544644--1544648.cif.
;
_cod_database_code               1544648
_chemical_oxdiff_formula         C24H18P1F3
_reflns_odcompleteness_completeness 99.78
_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. Others
 Sof(Sb1A)=Sof(H1A)=1-FVAR(1)
 Sof(Sb1)=Sof(H1)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              52058
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method toluene