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_1540565
_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 H76 N4 P4 Si4 Y, C20 H40 K O8, 2(C4 H8 O)'
_chemical_formula_sum            'C90 H132 K N4 O10 P4 Si4 Y'
_chemical_formula_weight         1794.24
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-03-13 deposited with the CCDC.
2015-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                98.667(2)
_cell_angle_beta                 94.975(2)
_cell_angle_gamma                93.716(3)
_cell_formula_units_Z            2
_cell_length_a                   15.1169(5)
_cell_length_b                   15.2820(5)
_cell_length_c                   21.1716(5)
_cell_measurement_reflns_used    13871
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.3650
_cell_measurement_theta_min      3.9690
_cell_volume                     4801.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0889456000
_diffrn_orient_matrix_UB_12      -0.0320098000
_diffrn_orient_matrix_UB_13      -0.0405903000
_diffrn_orient_matrix_UB_21      0.0027254000
_diffrn_orient_matrix_UB_22      0.0865765000
_diffrn_orient_matrix_UB_23      -0.0290588000
_diffrn_orient_matrix_UB_31      0.0511024000
_diffrn_orient_matrix_UB_32      -0.0440899000
_diffrn_orient_matrix_UB_33      -0.0545729000
_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  0.0610
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37308
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.771
_diffrn_reflns_theta_min         3.340
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    2.791
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.1625
_exptl_crystal_size_mid          0.1166
_exptl_crystal_size_min          0.073
_refine_diff_density_max         2.069
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         19007
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1365P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.2045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15405
_reflns_number_total             19007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03111g2.cif
_cod_data_source_block           2Y
_cod_depositor_comments
'Adding full bibliography for 1540562--1540566.cif.'
_cod_original_cell_volume        4801.8(2)
_cod_database_code               1540565
_nottingham_internal_coll_name   YMGALA
_nottingham_internal_coll_number 13410
_nottingham_internal_coll_client MG/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '72.0000, 18.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_user   MG
_nottingham_internal_coll_date   27/03/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user MG
_nottingham_internal_process_date 28/03/2014
_nottingham_internal_solution_user MG
_nottingham_internal_solution_date 28/03/2014
_nottingham_internal_refinement_user MG
_nottingham_internal_refinement_date 28/04/2014
_nottingham_internal_validation_user pczwl
_nottingham_internal_validation_date 16/1/2015
_nottingham_internal_archive_date 16/1/2015
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C90 H132 K1 N4 O10 P4 Si4 Y1'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-C86 \\sim O9-C83 \\sim O9-C83A \\sim O10-C90 \\sim O10-C87A \\sim O10-C87
 with sigma of 0.02
 C84-C83 \\sim C86-C85 \\sim C84-C83A \\sim C90-C89 \\sim C88A-C87A \\sim
C88-C87
 with sigma of 0.02
 C89-C88A \\sim C89-C88 \\sim C85-C84
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C90 \\sim C89 \\sim C87A \\sim O10 \\sim C88A \\sim C88 \\sim C87: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 O10, C90, C89, C87A, C88A, C87, C88
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C85, C86, O9, C83A, C83, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(H84C)=Sof(H84D)=1-FVAR(1)
 Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H84A)=Sof(H84B)=FVAR(1)
 Sof(H89C)=Sof(H89D)=Sof(C87)=Sof(H87C)=Sof(H87D)=Sof(C88)=Sof(H88C)=Sof(H88D)=
 1-FVAR(2)
 Sof(C87A)=Sof(H87A)=Sof(H87B)=Sof(C88A)=Sof(H88A)=Sof(H88B)=Sof(H89A)=
 Sof(H89B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,
 H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
 C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B),
  C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,
 H81B), C82(H82A,H82B), C83(H83A,H83B), C83A(H83C,H83D), C84(H84A,H84B),
 C84(H84C,H84D), C85(H85A,H85B), C86(H86A,H86B), C87A(H87A,H87B), C88A(H88A,
 H88B), C90(H90A,H90B), C89(H89A,H89B), C89(H89C,H89D), C87(H87C,H87D),
 C88(H88C,H88D)
6.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)
6.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              75755