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_1540564
_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 Dy N4 P4 Si4'
_chemical_formula_sum            'C62 H77 Dy N4 P4 Si4'
_chemical_formula_weight         1277.02
_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             2013-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_audit_update_record
;
2015-03-13 deposited with the CCDC.
2015-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 132.690(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.7145(11)
_cell_length_b                   25.7230(4)
_cell_length_c                   20.9468(7)
_cell_measurement_reflns_used    21121
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4720
_cell_measurement_theta_min      4.2270
_cell_volume                     12560.4(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0653399000
_diffrn_orient_matrix_UB_12      -0.0088132000
_diffrn_orient_matrix_UB_13      0.0688188000
_diffrn_orient_matrix_UB_21      -0.0053739000
_diffrn_orient_matrix_UB_22      -0.0396458000
_diffrn_orient_matrix_UB_23      -0.0603202000
_diffrn_orient_matrix_UB_31      0.0083343000
_diffrn_orient_matrix_UB_32      0.0440496000
_diffrn_orient_matrix_UB_33      -0.0404158000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37587
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.629
_diffrn_reflns_theta_min         3.792
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.370
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.292
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_F_000             5272
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.0393
_refine_diff_density_max         0.656
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         12499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+9.2287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12055
_reflns_number_total             12499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03111g2.cif
_cod_data_source_block           1Dy
_cod_depositor_comments
'Adding full bibliography for 1540562--1540566.cif.'
_cod_original_cell_volume        12560.4(11)
_cod_database_code               1540564
_nottingham_internal_coll_name   DYMGLA
_nottingham_internal_coll_number 13131
_nottingham_internal_coll_client MG/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '15.0000, 60.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_user   Service
_nottingham_internal_coll_date   19/12/2013
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user pczaw
_nottingham_internal_process_date 20/12/2013
_nottingham_internal_solution_user pcxmjg
_nottingham_internal_solution_date 20/12/2013
_nottingham_internal_refinement_user pcxmjg
_nottingham_internal_refinement_date 20/12/2013
_nottingham_internal_validation_date 16/1/2015
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 16/1/2015
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C62 H77 Dy1 N4 P4 Si4'
_chemical_oxdiff_usercomment
'DYMGLA #13131 IN FOMBLIN FILM ON MICROMOUNT FOR MG/STL'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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              29509