Transition Metal Redox Switches for Reversible “On/Off” and “Slow/Fast” Single-Molecule Magnet Behaviour in Dysprosium and Erbium bis-Diamidoferrocene Complexes
Dickie, Courtney M.; Laughlin, Alexander L.; Wofford, Joshua D.; Bhuvanesh, Nattamai; Nippe, Michael; Chem. Sci.  (2017) –; doi:10.1039/C7SC03380J

data_1547517
_publ_section_title
;
 Transition Metal Redox Switches for Reversible &#x201C;On/Off&#x201D; and
 &#x201C;Slow/Fast&#x201D; Single-Molecule Magnet Behaviour in Dysprosium
 and Erbium bis-Diamidoferrocene Complexes
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03380J
_journal_year                    2017
_chemical_formula_moiety         'C44 H76 Er Fe2 N4 Si4'
_chemical_formula_sum            'C44 H76 Er Fe2 N4 Si4'
_chemical_formula_weight         1052.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-08-01 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7942(16)
_cell_length_b                   19.8223(16)
_cell_length_c                   24.603(2)
_cell_measurement_reflns_used    5197
_cell_measurement_temperature    110
_cell_measurement_theta_max      19.591
_cell_measurement_theta_min      2.637
_cell_volume                     9653.4(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3290
_diffrn_reflns_av_unetI/netI     0.1513
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            81679
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        19.999
_diffrn_reflns_theta_max         19.999
_diffrn_reflns_theta_min         1.673
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.449
_exptl_absorpt_correction_T_max  0.4028
_exptl_absorpt_correction_T_min  0.2831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.1212 before and 0.0912 after correction. The Ratio of minimum to maximum transmission is 0.7028. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.353
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         4502
_refine_ls_number_restraints     1008
_refine_ls_restrained_S_all      0.860
_refine_ls_R_factor_all          0.1587
_refine_ls_R_factor_gt           0.0742
_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^)+(0.0949P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2105
_reflns_number_total             4502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03380j2.cif
_cod_data_source_block           mo_mn_cmd042_0m
_cod_original_cell_volume        9653.2(15)
_cod_database_code               1547517
_shelx_shelxl_version_number     2014/7
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4.a Ternary CH refined with riding coordinates:
 C33(H33)
4.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34),
 C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              85423
_olex2_submission_special_instructions 'No special instructions were received'