A series of salen-type asymmetric dinuclear Dy(iii) complexes: site-resolved two-step magnetic relaxation process
Zhang, Wan-Ying; Chen, Peng; Tian, Yong-Mei; Li, Hong-Feng; Sun, Wen-Bin; Yan, Peng-Fei; CrystEngComm 20 (2018) 777–; doi:10.1039/C7CE01797A

data_7229799
_publ_section_title
;
 A series of salen-type asymmetric dinuclear Dy(iii) complexes:
 site-resolved two-step magnetic relaxation process
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              777
_journal_paper_doi               10.1039/C7CE01797A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C60 H40 Dy2 F12 N2 O11, C4 H9 O'
_chemical_formula_sum            'C64 H49 Dy2 F12 N2 O12'
_chemical_formula_weight         1591.05
_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   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1q14fb
_audit_creation_date             2017-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-06 deposited with the CCDC.
2017-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                94.837(2)
_cell_angle_beta                 90.373(2)
_cell_angle_gamma                95.881(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7743(3)
_cell_length_b                   13.7731(4)
_cell_length_c                   21.4829(6)
_cell_measurement_reflns_used    8318
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3565
_cell_measurement_theta_min      2.9099
_cell_volume                     3159.52(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.831
_diffrn_measurement_details
;
  1 omega    7.00   68.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6223   38.0000  -60.0000 61

  2 omega    1.00   74.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6223   57.0000 -150.0000 73

  3 omega  -33.00   28.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6223  -57.0000   90.0000 61

  4 omega    3.00   80.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6223   57.0000    0.0000 77

  5 omega  -84.00  -21.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.7941  -38.0000    0.0000 63

  6 omega  -19.00    6.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.7941  -99.0000  120.0000 25

  7 omega   -9.00   20.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.7941  -99.0000 -120.0000 29
;
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_UB_11      0.0293265000
_diffrn_orient_matrix_UB_12      0.0486880000
_diffrn_orient_matrix_UB_13      0.0017478000
_diffrn_orient_matrix_UB_21      -0.0204240000
_diffrn_orient_matrix_UB_22      0.0046137000
_diffrn_orient_matrix_UB_23      -0.0309665000
_diffrn_orient_matrix_UB_31      -0.0557113000
_diffrn_orient_matrix_UB_32      0.0175554000
_diffrn_orient_matrix_UB_33      0.0116705000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29005
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.388
_diffrn_reflns_theta_min         2.913
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             1566
_refine_diff_density_max         1.914
_refine_diff_density_min         -2.300
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         14521
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0268P)^2^+16.5563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9788
_reflns_number_total             14521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01797a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7229799--7229802.cif.'
_cod_original_cell_volume        3159.52(15)
_cod_database_code               7229799
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F1' \\sim F2' \\sim F3': within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
F7 \\sim F7' \\sim F8 \\sim F8' \\sim F9 \\sim F9': within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
F10 \\sim F10' \\sim F11 \\sim F11' \\sim F12 \\sim F12': within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(F1) \\sim Ueq, Uanis(F1') \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F2')
\\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3') \\sim Ueq, Uanis(F4) \\sim Ueq,
Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F7') \\sim
Ueq, Uanis(F8) \\sim Ueq, Uanis(F8') \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F9')
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F10') \\sim Ueq, Uanis(F11) \\sim Ueq,
Uanis(F11') \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12') \\sim Ueq: with sigma
of 0.05 and sigma for terminal atoms of 0.1
Uanis(F1) = Uanis(F2) = Uanis(F3) = Uanis(F1') = Uanis(F2') = Uanis(F3')
Uanis(F7) = Uanis(F7') = Uanis(F8) = Uanis(F8') = Uanis(F9) = Uanis(F9')
Uanis(F10) = Uanis(F10') = Uanis(F11) = Uanis(F11') = Uanis(F12) = Uanis(F12')
3. Others
 Sof(F1)=Sof(F2)=Sof(F3)=1-FVAR(1)
 Sof(F1')=Sof(F2')=Sof(F3')=FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=1-FVAR(2)
 Sof(F7')=Sof(F8')=Sof(F9')=FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=1-FVAR(3)
 Sof(F10')=Sof(F11')=Sof(F12')=FVAR(3)
4.a Rotating group:
 O11(H11A,H11B)
4.b Secondary CH2 refined with riding coordinates:
 C63(H63A,H63B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C33(H33), C36(H36), C37(H37), C38(H38),
 C39(H39), C40(H40), C43(H43), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
  C53(H53), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C62(H62)
4.d Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C64(H64A,H64B,H64C)
;
_olex2_submission_special_instructions 'No special instructions were received'