Linear hexanuclear helical dysprosium single-molecule magnets: the effect of axial substitution on magnetic interactions and relaxation dynamics.
Lu, Jingjing; Li, Xiao-Lei; Zhu, Zhenhua; Liu, Shuting; Yang, Qianqian; Tang, Jinkui; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14062–14068; doi:10.1039/c9dt03101d

data_7701602
_publ_section_title
;
 Linear hexanuclear helical dysprosium single-molecule magnets: the effect
 of axial substitution on magnetic interactions and relaxation dynamics.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14062
_journal_page_last               14068
_journal_paper_doi               10.1039/c9dt03101d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C78 H80 Dy6 N28 O42'
_chemical_formula_sum            'C78 H80 Dy6 N28 O42'
_chemical_formula_weight         3056.70
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-28 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   55.955(4)
_cell_length_b                   55.955(4)
_cell_length_c                   20.8428(17)
_cell_measurement_reflns_used    9754
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.18
_cell_volume                     56515(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2081
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -69
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            116093
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.262
_diffrn_reflns_theta_min         0.728
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    3.607
_exptl_absorpt_correction_T_max  0.436
_exptl_absorpt_correction_T_min  0.365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       Needlelike
_exptl_crystal_F_000             26568
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.966
_refine_diff_density_min         -2.055
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         12660
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+5837.3667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6965
_reflns_number_total             12660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03101d2.cif
_cod_data_source_block           Dy6-NO3
_cod_original_cell_volume        56515(9)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7701602
_shelx_shelxl_version_number     2018/3
_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, All O(H,H) groups
2. Restrained distances
 N10-O12
 1.24 with sigma of 0.01
 N14-O21
 1.25 with sigma of 0.02
 N14-O19
 1.25 with sigma of 0.02
 N14-O20
 1.25 with sigma of 0.02
 N12-O17
 1.24 with sigma of 0.04
 N12-O16
 1.24 with sigma of 0.04
 N12-O15
 1.24 with sigma of 0.04
 O16-O17
 2.16 with sigma of 0.04
 O16-O15
 2.16 with sigma of 0.04
 O17-O15
 2.16 with sigma of 0.04
 O19-O19_$1
 2.2 with sigma of 0.04
 N13-C38 \\sim N13-C39
 with sigma of 0.02
 N14-O19 \\sim N14-O20 \\sim N14-O21
 with sigma of 0.02
 O19-O20 \\sim O20-O21 \\sim O21-O19
 with sigma of 0.04
3. Restrained planarity
 C37, O18, N13, C38, C39
 with sigma of 0.1
 N14, O19, O20, O21
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C37 \\sim O18 \\sim N13 \\sim C38 \\sim C39: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N14 \\sim O19 \\sim O20 \\sim O21: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O16) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O12) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N13) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C37)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O19) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(O21) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O20) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 N12, O17, O16, O15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, O18, N13, C38, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N14, O19, O20, O21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 C36(H36A,H36B,H36C)
6.b Rotating group:
 O13(H13A,H13B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C9(H9), C12(H12), C16(H16), C17(H17), C18(H18),
 C19(H19), C23(H23), C27(H27), C28(H28), C29(H29), C32(H32), C34(H34), C35(H35),
  C37(H37)
6.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,
 H33C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;