A monometallic lanthanide bis(methanediide) single molecule magnet with a large energy barrier and complex spin relaxation behaviour
Gregson, Matthew; Chilton, Nicholas F.; Ariciu, Ana-Maria; Tuna, Floriana; Crowe, Iain F.; Lewis, William; Blake, Alexander J.; Collison, David; McInnes, Eric J. L.; Winpenny, Richard E. P.; Liddle, Stephen T.; Chem. Sci. 7 (2016) 155–; doi:10.1039/C5SC03111G

data_1540562
_publ_section_title
;
 A monometallic lanthanide bis(methanediide) single molecule magnet with a
 large energy barrier and complex spin relaxation behaviour
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              155
_journal_paper_doi               10.1039/C5SC03111G
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C42 H53 Dy N2 O P2 Si2'
_chemical_formula_sum            'C42 H53 Dy N2 O P2 Si2'
_chemical_formula_weight         882.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-03-13 deposited with the CCDC.
2015-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0778(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.47242(8)
_cell_length_b                   19.20658(14)
_cell_length_c                   10.61743(9)
_cell_measurement_reflns_used    11641
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4780
_cell_measurement_theta_min      4.1550
_cell_volume                     2130.18(3)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction
;
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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega -103.00  -17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000  -90.0000 86

  2 omega  -42.00   -3.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000   60.0000 39

  3 omega  -91.00  -47.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000   60.0000 44

  4 omega  -24.00   10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   90.0000 34

  5 omega   86.00  154.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295   61.0000   30.0000 68

  6 omega   42.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -30.0000   60.0000 30

  7 omega   59.00   99.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -45.0000  120.0000 40

  8 omega   44.00  134.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -77.0000  -90.0000 90

  9 omega   36.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -94.0000 -120.0000 67

 10 omega   93.00  174.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295   45.0000   90.0000 81

 11 omega   35.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -30.0000  -90.0000 55

 12 omega  -90.00  -17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  -60.0000 73

 13 omega -109.00  -19.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000  150.0000 90

 14 omega  -22.00    4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -90.0000 26

 15 omega   36.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -30.0000   90.0000 47

 16 omega   52.00   78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -30.0000 -180.0000 26

 17 omega  102.00  150.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295   45.0000  120.0000 48

 18 omega   26.00  108.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -94.0000  150.0000 82

 19 omega   63.00  120.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295 -125.0000   90.0000 57

 20 omega   83.00  172.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295   45.0000    0.0000 89

 21 omega   42.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -30.0000 -150.0000 34

 22 omega   30.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -94.0000   90.0000 33

 23 omega   60.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  -30.0000  -60.0000 30
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  GV1000
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      0.1001509000
_diffrn_orient_matrix_UB_12      -0.0572649000
_diffrn_orient_matrix_UB_13      0.0318079000
_diffrn_orient_matrix_UB_21      0.1082347000
_diffrn_orient_matrix_UB_22      0.0532157000
_diffrn_orient_matrix_UB_23      -0.0134899000
_diffrn_orient_matrix_UB_31      -0.0013838000
_diffrn_orient_matrix_UB_32      0.0179262000
_diffrn_orient_matrix_UB_33      0.1413301000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17192
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.429
_diffrn_reflns_theta_min         4.174
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    10.878
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.405
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       block
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.2701
_exptl_crystal_size_mid          0.1672
_exptl_crystal_size_min          0.1333
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4419
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0193
_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^)+(0.0301P)^2^+0.6644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4362
_reflns_number_total             4419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03111g2.cif
_cod_data_source_block           '[Dy(BIPMtms)(Bn)(THF)]'
_cod_depositor_comments
'Adding full bibliography for 1540562--1540566.cif.'
_cod_database_code               1540562
_nottingham_internal_coll_name   DYMGLB
_nottingham_internal_coll_number 13153
_nottingham_internal_coll_client MG/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '1.0000, 4.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxmjg
_nottingham_internal_coll_date   16/01/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 17/01/2014
_nottingham_internal_process_user pcxmjg
_nottingham_internal_solution_date 17/01/2014
_nottingham_internal_solution_user pcxmjg
_nottingham_internal_refinement_date 16/01/2015
_nottingham_internal_refinement_user pcxmjg
_nottingham_internal_self_archive_date 16/01/2015
_nottingham_internal_self_validation_date 16/01/2015
_nottingham_internal_self_validation_user pcxmjg
_nottingham_internal_validation_date 19/1/2015
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 19/1/2015
_chemical_oxdiff_formula         'C42 H53 Dy1 N2 O1 P2 Si2'
_chemical_oxdiff_usercomment
'DYMGLB #13153 IN FOMBLIN FILM ON MICROMOUNT FOR MG/STL'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C22 \\sim O1-C25
 with sigma of 0.02
 C23-C22 \\sim C25-C24 \\sim C24-C23
 with sigma of 0.02
 C22-C24 \\sim C23-C25
 with sigma of 0.02
 C23-O1 \\sim O1-C24
 with sigma of 0.02
 C25-Dy1 \\sim Dy1-C22
 with sigma of 0.02
3. Others
 Fixed Sof: O1(0.5) H17A(0.5) H17B(0.5) C22(0.5) H22A(0.5) H22B(0.5) C25(0.5)
 H25A(0.5) H25B(0.5) C23(0.5) H23A(0.5) H23B(0.5) C24(0.5) H24A(0.5) H24B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C22(H22A,H22B), C25(H25A,H25B), C23(H23A,H23B), C24(H24A,H24B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C19(H19), C20(H20), C21(H21)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              27799
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'In fomblin on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'