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_1540563
_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         'C62 H77 N4 P4 Si4 Y'
_chemical_formula_sum            'C62 H77 N4 P4 Si4 Y'
_chemical_formula_weight         1203.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 132.786(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.667(3)
_cell_length_b                   25.7439(13)
_cell_length_c                   20.938(2)
_cell_measurement_reflns_used    21220
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.5220
_cell_measurement_theta_min      3.8330
_cell_volume                     12527(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      N~2~
_diffrn_ambient_temperature      90(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega   25.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7877   38.0000 -180.0000 90

  2 omega   12.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7877  -38.0000 -150.0000 32

  3 omega   11.00   97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7877 -125.0000   30.0000 86

  4 omega   41.00   77.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  120.0000 36

  5 omega   30.00   93.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -104.0000   54.0000 63

  6 omega   36.00  122.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -77.0000   60.0000 86

  7 omega   84.00  158.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000  150.0000 74

  8 omega   40.00   72.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -150.0000 32

  9 omega  122.00  158.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000 -180.0000 36

 10 omega   37.00   70.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -120.0000 33

 11 omega   37.00   70.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -90.0000 33

 12 omega   44.00   71.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   30.0000 27

 13 omega   37.00   68.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   60.0000 31

 14 omega   83.00  137.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000   60.0000 54

 15 omega  -98.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877  125.0000  150.0000 96

 16 omega -115.00  -23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877  -38.0000 -120.0000 92

 17 omega -115.00  -14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877  -77.0000    0.0000 101

 18 omega   23.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7877   38.0000   90.0000 92

 19 omega   76.00  158.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   77.0000 -150.0000 82

 20 omega   76.00  158.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   77.0000    0.0000 82

 21 omega   83.00  158.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000  -60.0000 75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.0642496000
_diffrn_orient_matrix_UB_12      0.0147014000
_diffrn_orient_matrix_UB_13      -0.0683994000
_diffrn_orient_matrix_UB_21      -0.0163729000
_diffrn_orient_matrix_UB_22      -0.0556578000
_diffrn_orient_matrix_UB_23      0.0032724000
_diffrn_orient_matrix_UB_31      0.0023900000
_diffrn_orient_matrix_UB_32      0.0163049000
_diffrn_orient_matrix_UB_33      0.0731080000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44828
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         74.772
_diffrn_reflns_theta_min         3.434
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.322
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.2019
_exptl_crystal_size_mid          0.1667
_exptl_crystal_size_min          0.0897
_refine_diff_density_max         1.914
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         12547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0600
_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^)+(0.1169P)^2^+44.6698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10860
_reflns_number_total             12547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03111g2.cif
_cod_data_source_block           1Y
_cod_depositor_comments
'Adding full bibliography for 1540562--1540566.cif.'
_cod_original_cell_volume        12527(3)
_cod_database_code               1540563
_nottingham_internal_coll_name   YLSSIG
_nottingham_internal_coll_number 9254
_nottingham_internal_coll_client LS/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '20.0000, 80.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pczwl
_nottingham_internal_coll_date   17/03/2010
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 16/01/2015
_nottingham_internal_process_user pczwl
_nottingham_internal_solution_date 16/01/2015
_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         'C62 H77 N4 P4 Si4 Y'
_chemical_oxdiff_usercomment
'YLSSIG #9254 IN FOMBLIN FILM ON MICROMOUNT FOR LS/STL'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Ternary CH refined with riding coordinates:
 C32(H32)
2.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), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C49(H49), C50(H50),
  C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C)
;
_shelx_res_checksum              10290
_shelx_shelxl_version_number     2014/7
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'