Magneto-structural correlations in arsenic- and selenium-ligated dysprosium single-molecule magnets
Pugh, Thomas; Vieru, Veacheslav; Chibotaru, Liviu F.; Layfield, Richard A.; Chem. Sci. 7 (2016) 2128–; doi:10.1039/C5SC03755G

data_1540697
_publ_section_title
;
 Magneto-structural correlations in arsenic- and selenium-ligated
 dysprosium single-molecule magnets
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2128
_journal_paper_doi               10.1039/C5SC03755G
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C18 H21 Dy, C9 H13 As'
_chemical_formula_sum            'C27 H34 As Dy'
_chemical_formula_weight         595.96
_chemical_name_systematic        1-Dy
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-02-04
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-28 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.354(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1717(3)
_cell_length_b                   24.8088(10)
_cell_length_c                   11.6477(5)
_cell_measurement_reflns_used    7897
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.4530
_cell_measurement_theta_min      3.2710
_cell_volume                     2354.52(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   33.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590  -99.0000   30.0000 36

  2 omega  -62.00   36.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590  -57.0000   90.0000 98

  3 omega  -11.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590   57.0000  -30.0000 124

  4 omega   10.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590   57.0000 -150.0000 88

  5 omega  -10.00   64.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590  -99.0000 -150.0000 74
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0104371000
_diffrn_orient_matrix_UB_12      -0.0283563000
_diffrn_orient_matrix_UB_13      0.0024771000
_diffrn_orient_matrix_UB_21      0.0750645000
_diffrn_orient_matrix_UB_22      -0.0036948000
_diffrn_orient_matrix_UB_23      -0.0257693000
_diffrn_orient_matrix_UB_31      0.0426785000
_diffrn_orient_matrix_UB_32      -0.0004652000
_diffrn_orient_matrix_UB_33      0.0553480000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14983
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.943
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.579
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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    1.681
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluebe'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4163
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+4.4081P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3728
_reflns_number_total             4163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03755g2.cif
_cod_data_source_block           oral271
_cod_depositor_comments
'Adding full bibliography for 1540697--1540701.cif.'
_cod_original_cell_volume        2354.53(17)
_cod_database_code               1540697
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         Dy1C27H60As1
_reflns_odcompleteness_completeness 99.84
_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
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 1.7A with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C14A, C15A, C16A, C17A, C18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C13A)=Sof(H13A)=Sof(C16A)=
 Sof(H16A)=Sof(C17A)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C13)=Sof(H13)=Sof(C16)=Sof(H16)=
 Sof(C17)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C14A(H14A), C15(H15), C15A(H15A), C23(H23), C13(H13), C13A(H13A),
 C16(H16), C16A(H16A), C21(H21), C1(H1), C2(H2), C3(H3), C4(H4), C10(H10),
 C9(H9), C8(H8), C7(H7)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              58919
_olex2_date_sample_data_collection 2014-07-29
_olex2_submission_special_instructions 'No special instructions were received'