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_1540701
_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 Se3 Y3, C7 H8'
_chemical_formula_sum            'C70 H83 Se3 Y3'
_chemical_formula_weight         1427.97
_chemical_name_systematic        4-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             2015-01-21
_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                 103.0350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.90290(10)
_cell_length_b                   18.42530(10)
_cell_length_c                   23.4230(2)
_cell_measurement_reflns_used    21927
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.5770
_cell_measurement_theta_min      3.8300
_cell_volume                     6266.00(8)
_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      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega   67.67  250.67   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       97.4570   73.8672   81.7092 183

  2 omega   80.85  263.85   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      110.6420   73.8672  -77.4991 183

  3 phi   -201.78  158.56   1.0009    2.0000
omega____ theta____ kappa____ phi______ frames
 -50.7813  -39.9910   73.8672     -     360

  4 omega   79.90  262.90   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6940   73.8672   30.2616 183

  5 omega   79.65  262.65   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4400   73.8672 -133.6445 183

  6 omega   79.94  262.94   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7290   73.8672   83.2986 183

  7 omega  -97.16   80.84   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -67.3741   73.8672  117.6319 178

  8 omega   96.85  244.85   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6449   73.8672  123.6078 148
;
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      -0.0361505000
_diffrn_orient_matrix_UB_12      0.0701097000
_diffrn_orient_matrix_UB_13      0.0227809000
_diffrn_orient_matrix_UB_21      0.0967240000
_diffrn_orient_matrix_UB_22      0.0338855000
_diffrn_orient_matrix_UB_23      0.0093618000
_diffrn_orient_matrix_UB_31      -0.0243571000
_diffrn_orient_matrix_UB_32      0.0304379000
_diffrn_orient_matrix_UB_33      -0.0628663000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23361
_diffrn_reflns_point_group_measured_fraction_full 0.730
_diffrn_reflns_point_group_measured_fraction_max 0.711
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.724
_diffrn_reflns_theta_min         3.876
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.921
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33829
_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    1.514
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 2770 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.010(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         9014
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+13.8384P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.450
_reflns_friedel_fraction_full    0.461
_reflns_friedel_fraction_max     0.442
_reflns_number_gt                8997
_reflns_number_total             9014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03755g2.cif
_cod_data_source_block           xral31_rered_xprep
_cod_depositor_comments
'Adding full bibliography for 1540697--1540701.cif.'
_cod_database_code               1540701
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 97.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.57
_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.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)
2.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              81791
_olex2_submission_special_instructions 'No special instructions were received'