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_1540698
_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         'C63 H75 As3 Dy3, C7 H8'
_chemical_formula_sum            'C70 H83 As3 Dy3'
_chemical_formula_weight         1636.62
_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             2015-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2015-05-28 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.461(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9242(3)
_cell_length_b                   18.6105(4)
_cell_length_c                   23.7155(5)
_cell_measurement_reflns_used    11132
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.1180
_cell_measurement_theta_min      3.4430
_cell_volume                     6406.0(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
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -73.00  -38.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0746  179.0000  -90.0000 35

  2 omega -119.00  -34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0746 -179.0000 -180.0000 85

  3 omega  -13.00   14.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0746  -99.0000  -90.0000 27

  4 omega   40.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4027  179.0000 -180.0000 82

  5 omega  -12.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4027   57.0000  -90.0000 128

  6 omega  -47.00   15.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4027  -77.0000 -120.0000 62
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0332660000
_diffrn_orient_matrix_UB_12      0.0233139000
_diffrn_orient_matrix_UB_13      0.0169251000
_diffrn_orient_matrix_UB_21      0.0338834000
_diffrn_orient_matrix_UB_22      -0.0273011000
_diffrn_orient_matrix_UB_23      0.0024811000
_diffrn_orient_matrix_UB_31      0.0116159000
_diffrn_orient_matrix_UB_32      0.0127819000
_diffrn_orient_matrix_UB_33      -0.0255524000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20817
_diffrn_reflns_point_group_measured_fraction_full 0.875
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.908
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.040
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43461
_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
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.241
_refine_diff_density_min         -1.957
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Flack x determined using 3838 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.026(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         10263
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0493P)^2^+25.6955P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.751
_reflns_friedel_fraction_full    0.753
_reflns_friedel_fraction_max     0.751
_reflns_number_gt                9704
_reflns_number_total             10263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03755g2.cif
_cod_data_source_block           oral247_xprep_shelxl
_cod_depositor_comments
'Adding full bibliography for 1540697--1540701.cif.'
_cod_original_cell_volume        6406.0(3)
_cod_database_code               1540698
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         Dy3As3C70H86
_reflns_odcompleteness_completeness 99.81
_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
 C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C26, C27, C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.08
C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.02
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.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), C64(H64), C65(H65),
  C66(H66), C67(H67), C68(H68)
4.b 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)
;
_shelx_res_checksum              17538
_olex2_submission_special_instructions 'No special instructions were received'