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_7701603
_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         'C96 H104 Dy6 N32 O26 S6, C3 H7 N O'
_chemical_formula_sum            'C99 H111 Dy6 N33 O27 S6'
_chemical_formula_weight         3362.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-28
_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                 96.3550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1621(9)
_cell_length_b                   19.7925(9)
_cell_length_c                   36.6621(17)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      2.32
_cell_volume                     13819.2(11)
_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      153.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0674
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            85352
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.039
_diffrn_reflns_theta_min         1.118
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.367
_exptl_absorpt_correction_T_max  0.493
_exptl_absorpt_correction_T_min  0.379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       Needlelike
_exptl_crystal_F_000             6576
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.778
_refine_diff_density_min         -2.383
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1563
_refine_ls_number_reflns         27222
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0844P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19420
_reflns_number_total             27222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03101d2.cif
_cod_data_source_block           Dy6-SCN
_cod_database_code               7701603
_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
2. Restrained distances
 N33-C99
 1.3 with sigma of 0.01
 O28-C99
 1.21 with sigma of 0.01
 N33-C95 = N33-C97
 1.47 with sigma of 0.01
 C95-C97
 2.5 with sigma of 0.01
3. Restrained planarity
 O28, C95, C99, C97, N33
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C99) \\sim Ueq, Uanis(C94) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O28) \\sim Ueq, Uanis(N33) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C98) \\sim Ueq, Uanis(N31) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C96)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C97) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Riding coordinates:
 C97(H97A,H97B,H97C)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14),
 C22(H22), C27(H27), C30(H30), C33(H33), C36(H36), C37(H37), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C48(H48), C50(H50), C51(H51), C54(H54),
 C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65),
  C66(H66), C68(H68), C69(H69), C71(H71), C73(H73), C74(H74), C98(H98), C99(H99)
5.c Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C3(H3A,H3B,H3C), C70(H70A,H70B,H70C), C72(H72A,H72B,
 H72C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,
 H78B,H78C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C),
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,
 H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C91(H91A,
 H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C),
 C96(H96A,H96B,H96C)
;
_olex2_submission_special_instructions 'No special instructions were received'