An air stable radical-bridged dysprosium single molecule magnet and its neutral counterpart: redox switching of magnetic relaxation dynamics.
Dolinar, Brian S.; Gómez-Coca, Silvia; Alexandropoulos, Dimitris I.; Dunbar, Kim R.; Chemical communications (Cambridge, England) 53 (2017) 2283–2286; doi:10.1039/c6cc09824j

data_7119437
_publ_section_title
;
 An air stable radical-bridged dysprosium single molecule magnet and its
 neutral counterpart: redox switching of magnetic relaxation dynamics.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2283
_journal_page_last               2286
_journal_paper_doi               10.1039/c6cc09824j
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety
'C78 H122 Dy2 N6 O12, C10 H10 Co, 2.5(C5 H12)'
_chemical_formula_sum            'C100.5 H162 Co Dy2 N6 O12'
_chemical_formula_weight         2030.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-09-27 deposited with the CCDC.
2017-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4756(6)
_cell_length_b                   22.8962(8)
_cell_length_c                   25.6356(9)
_cell_measurement_reflns_used    9057
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.33
_cell_volume                     10629.0(6)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            203756
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.742
_diffrn_reflns_theta_min         2.405
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.7782
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1108 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.8042.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.034
_refine_diff_density_max         2.819
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1229
_refine_ls_number_reflns         20253
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+16.9414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16801
_reflns_number_total             20253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09824j2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7119436--7119437.cif.'
_cod_original_formula_sum        'C100.50 H162 Co Dy2 N6 O12'
_cod_database_code               7119437
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.673
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C19-C20A \\sim C20-C19 \\sim C22A-C19 \\sim C22-C19 \\sim C21A-C19 \\sim
C21-C19
 with sigma of 0.01
 C8T-C8S \\sim C9S-C8S \\sim C8T-C10S \\sim C9S-C10S \\sim C8S-C7T \\sim
C8S-C7S \\sim C7S-C6S \\sim C7T-C6S
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C11T \\sim C12T \\sim C13T \\sim C14T \\sim C15T \\sim C11S \\sim C12S \\sim
C13S \\sim C14S \\sim C15S \\sim C11U \\sim C12U \\sim C13U \\sim C14U \\sim
C15U: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C20A \\sim C21A \\sim C22A: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C9S \\sim C8T \\sim C7T \\sim C7S: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Same fragment restrains
{C11S, C12S, C13S, C14S, C15S} sigma for 1-2: 0.01, 1-3: 0.02
{C11T, C12T, C13T, C14T, C15T} sigma for 1-2: 0.01, 1-3: 0.02
{C11U, C12U, C13U, C14U, C15U} sigma for 1-2: 0.01, 1-3: 0.02
as
{C1S, C2S, C3S, C4S, C5S}
5. Others
 1*[Sof(C11S)+Sof(H11D)+Sof(H11E)+Sof(H11F)+Sof(C12S)+Sof(H12D)+Sof(H12E)+
 Sof(C13S)+Sof(H13D)+Sof(H13E)+Sof(C14S)+Sof(H14D)+Sof(H14E)+Sof(C15S)+
 Sof(H15A)+Sof(H15B)+Sof(H15C)]+1*[Sof(C11T)+Sof(H11G)+Sof(H11H)+Sof(H11I)+
 Sof(C12T)+Sof(H12F)+Sof(H12G)+Sof(C13T)+Sof(H13F)+Sof(H13G)+Sof(C14T)+
 Sof(H14F)+Sof(H14G)+Sof(C15T)+Sof(H15D)+Sof(H15E)+Sof(H15F)]+1*[Sof(C11U)+
 Sof(H11J)+Sof(H11K)+Sof(H11L)+Sof(C12U)+Sof(H12H)+Sof(H12I)+Sof(C13U)+
 Sof(H13H)+Sof(H13I)+Sof(C14U)+Sof(H14H)+Sof(H14I)+Sof(C15U)+Sof(H15G)+
 Sof(H15H)+Sof(H15I)]=1 with esd of 0
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21A)=Sof(H21D)=Sof(H21E)=
 Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
 Sof(C11S)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12S)=Sof(H12D)=Sof(H12E)=
 Sof(C13S)=Sof(H13D)=Sof(H13E)=Sof(C14S)=Sof(H14D)=Sof(H14E)=Sof(C15S)=
 Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(2)
 Sof(C11T)=Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(C12T)=Sof(H12F)=Sof(H12G)=
 Sof(C13T)=Sof(H13F)=Sof(H13G)=Sof(C14T)=Sof(H14F)=Sof(H14G)=Sof(C15T)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=FVAR(3)
 Sof(C11U)=Sof(H11J)=Sof(H11K)=Sof(H11L)=Sof(C12U)=Sof(H12H)=Sof(H12I)=
 Sof(C13U)=Sof(H13H)=Sof(H13I)=Sof(C14U)=Sof(H14H)=Sof(H14I)=Sof(C15U)=
 Sof(H15G)=Sof(H15H)=Sof(H15I)=FVAR(4)
 Sof(H6SD)=Sof(H6SE)=Sof(H6SF)=Sof(H8SC)=Sof(H8SD)=Sof(H10G)=Sof(H10H)=
 Sof(H10I)=Sof(C7T)=Sof(H7TA)=Sof(H7TB)=Sof(C8T)=Sof(H8TA)=Sof(H8TB)=1-FVAR(5)
 Sof(H6SA)=Sof(H6SB)=Sof(H6SC)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H8SA)=
 Sof(H8SB)=Sof(C9S)=Sof(H9SA)=Sof(H9SB)=Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(5)
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) C5S(0.5)
 H5SA(0.5) H5SB(0.5) H5SC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C12S(H12D,H12E), C13S(H13D,H13E), C14S(H14D,H14E), C12T(H12F,H12G), C13T(H13F,
 H13G), C14T(H14F,H14G), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB),
 C12U(H12H,H12I), C13U(H13H,H13I), C14U(H14H,H14I), C7S(H7SA,H7SB), C8S(H8SA,
 H8SB), C8S(H8SC,H8SD), C9S(H9SA,H9SB), C7T(H7TA,H7TB), C8T(H8TA,H8TB)
6.b Me refined with riding coordinates:
 C6S(H6SA,H6SB,H6SC), C6S(H6SD,H6SE,H6SF), C10S(H10D,H10E,H10F), C10S(H10G,
 H10H,H10I)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C28(H28), C39(H39), C50(H50), C61(H61), C67(H67), C68(H68),
 C69(H69), C70(H70), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80),
  C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C),
 C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C20A(H20D,H20E,H20F),
 C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F), C11S(H11D,H11E,H11F), C15S(H15A,
 H15B,H15C), C11T(H11G,H11H,H11I), C15T(H15D,H15E,H15F), C1S(H1SA,H1SB,H1SC),
 C5S(H5SA,H5SB,H5SC), C11U(H11J,H11K,H11L), C15U(H15G,H15H,H15I)
;
_shelx_res_checksum              72350
_shelx_hkl_checksum              30408
_olex2_submission_special_instructions 'No special instructions were received'