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_1544646
_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
'C38.63 H45.88 Dy2 Sb1.63, C24.37 H29.12 Dy Sb1.37, C7 H8'
_chemical_formula_sum            'C70 H83 Dy3 Sb3'
_chemical_formula_weight         1777.11
_chemical_name_systematic        1-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     heavy
_audit_creation_date             2016-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-10 deposited with the CCDC.
2016-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.3390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1130(2)
_cell_length_b                   18.7437(2)
_cell_length_c                   24.0965(3)
_cell_measurement_reflns_used    39107
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.2380
_cell_measurement_theta_min      3.7120
_cell_volume                     6641.75(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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(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  -88.00   12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000 -120.0000 100

  2 omega  -87.00    4.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -57.0000  150.0000 91

  3 omega  -88.00   12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000   60.0000 100

  4 omega  -87.00    4.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -57.0000  -60.0000 91

  5 omega  -50.00   40.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038  -57.0000   90.0000 90

  6 omega  -50.00   40.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038  -57.0000 -180.0000 90

  7 omega  -51.00   49.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038  -77.0000  -60.0000 100

  8 omega  -20.00   61.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038  -99.0000   30.0000 81

  9 omega  -20.00   61.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038  -99.0000 -150.0000 81

 10 omega  -94.00  -35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663 -178.0000  -90.0000 59

 11 omega  -39.00   51.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663   57.0000  -60.0000 90

 12 omega  -54.00   -5.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038    0.0000 -180.0000 49

 13 omega  -20.00   61.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7038  -99.0000   60.0000 81

 14 omega    2.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000 -125.0000  -32.5258 75

 15 omega    6.00   82.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000 -132.0000  114.2750 76
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
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_diffrn_orient_matrix_UB_11      0.0274311000
_diffrn_orient_matrix_UB_12      0.0194972000
_diffrn_orient_matrix_UB_13      0.0228574000
_diffrn_orient_matrix_UB_21      0.0373900000
_diffrn_orient_matrix_UB_22      -0.0225595000
_diffrn_orient_matrix_UB_23      -0.0007538000
_diffrn_orient_matrix_UB_31      0.0132468000
_diffrn_orient_matrix_UB_32      0.0233174000
_diffrn_orient_matrix_UB_33      -0.0197968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0341
_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       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            74897
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.346
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         3.394
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76091
_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    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             3416
_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         3.560
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 5477 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         12154
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0288P)^2^+23.4314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                11677
_reflns_number_total             12154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04465d2.cif
_cod_data_source_block           aral294_rered_xprep
_cod_depositor_comments
;Adding full bibliography for 1544644--1544648.cif.

 Adding full bibliography for 1544644--1544648.cif.
;
_cod_database_code               1544646
_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. Rigid bond restraints
 C37, C38, C39, C40, C41, C42
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C46A, C47A, C48A, C49A, C50A, C51A, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C49, C48, C47, C46, C51, C50, C52, C53, C54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C58A, C59A, C60A, C55A, C56A, C57A, C61A, C62A, C63A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C46A \\sim C47A \\sim C48A \\sim C49A \\sim C50A \\sim C51A \\sim C52A \\sim
C53A \\sim C54A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C49 \\sim C48 \\sim C47 \\sim C46 \\sim C51 \\sim C50 \\sim C52 \\sim C53 \\sim
C54: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C58A \\sim C59A \\sim C60A \\sim C55A \\sim C56A \\sim C57A \\sim C61A \\sim
C62A \\sim C63A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 C55, C56, C57, C58, C59, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, C35, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Others
 Sof(Sb3A)=Sof(C58A)=Sof(C59A)=Sof(H59A)=Sof(C60A)=Sof(C55A)=Sof(C56A)=
 Sof(C57A)=Sof(H57A)=Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62A)=
 Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63A)=Sof(H63A)=Sof(H63B)=Sof(H63C)=1-FVAR(1)
 Sof(Sb3)=Sof(C55)=Sof(C56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(C59)=Sof(H59)=
 Sof(C60)=Sof(C61)=Sof(H61D)=Sof(H61E)=Sof(H61F)=Sof(C62)=Sof(H62D)=Sof(H62E)=
 Sof(H62F)=Sof(C63)=Sof(H63D)=Sof(H63E)=Sof(H63F)=FVAR(1)
 Sof(Sb2A)=Sof(C46A)=Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(C50A)=
 Sof(H50A)=Sof(C51A)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53A)=
 Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54A)=Sof(H54A)=Sof(H54B)=Sof(H54C)=1-FVAR(2)
 Sof(Sb2)=Sof(C49)=Sof(C48)=Sof(H48)=Sof(C47)=Sof(C46)=Sof(C51)=Sof(C50)=
 Sof(H50)=Sof(C52)=Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C53)=Sof(H53D)=Sof(H53E)=
 Sof(H53F)=Sof(C54)=Sof(H54D)=Sof(H54E)=Sof(H54F)=FVAR(2)
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), C59A(H59A),
 C57A(H57A), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20),
 C21(H21), C22(H22), C39(H39), C41(H41), C48A(H48A), C50A(H50A), C25(H25),
 C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C48(H48),
  C50(H50), C57(H57), C59(H59), C64(H64), C68(H68), C67(H67), C66(H66), C65(H65)
6.b Fitted hexagon refined as free rotating group:
 C58A(C59A,C60A,C55A,C56A,C57A), C49(C48,C47,C46,C51,C50), C64(C69,C68,C67,C66,
 C65)
6.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C61A(H61A,H61B,H61C), C62A(H62A,H62B,
 H62C), C63A(H63A,H63B,H63C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C52A(H52A,H52B,
 H52C), C53A(H53A,H53B,H53C), C54A(H54A,H54B,H54C), C30(H30A,H30B,H30C),
 C36(H36A,H36B,H36C), C52(H52D,H52E,H52F), C53(H53D,H53E,H53F), C54(H54D,H54E,
 H54F), C61(H61D,H61E,H61F), C62(H62D,H62E,H62F), C63(H63D,H63E,H63F), C70(H70A,
 H70B,H70C)
;
_shelx_res_checksum              79251
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Toluene