Dramatic impact of auxiliary ligands on the two-step magnetic relaxation process in Dy<sub>4</sub>(iii) single-molecule magnets.
Zhang, Kun; Li, Gao-Peng; Zhang, Cheng; Wang, Yao-Yu; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5793–5799; doi:10.1039/c9dt01076a

data_7049593
_publ_section_title
;
 Dramatic impact of auxiliary ligands on the two-step magnetic relaxation
 process in Dy<sub>4</sub>(iii) single-molecule magnets.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5793
_journal_page_last               5799
_journal_paper_doi               10.1039/c9dt01076a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C76 H70 Dy4 N6 O20, C3 H7 N O'
_chemical_formula_sum            'C79 H77 Dy4 N7 O21'
_chemical_formula_weight         2110.47
_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
_audit_creation_date             2019-03-30
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5716)
;
_audit_update_record
;
2019-04-02 deposited with the CCDC.    2019-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.908(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.120(8)
_cell_length_b                   25.340(17)
_cell_length_c                   12.262(8)
_cell_measurement_reflns_used    2219
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     4003(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19090
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.581
_exptl_absorpt_coefficient_mu    3.766
_exptl_absorpt_correction_T_max  0.8517
_exptl_absorpt_correction_T_min  0.6492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.668
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         6989
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+39.0179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5295
_reflns_number_total             6989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01076a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7049592--7049593.cif.'
_cod_database_code               7049593
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.505
_shelx_estimated_absorpt_t_min   0.379
_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
2. Restrained distances
 N3-C30 \\sim N3-C31
 with sigma of 0.01
 C34-C35 \\sim C35-C34A
 with sigma of 0.02
 C34A-C33 \\sim C33-C34
 with sigma of 0.02
3. Restrained planarity
 C32, C33, C34, C35, C36
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C34A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C28) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C33, C34, C35, C34A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C30, C31, C29, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C39, N4, C41, C40, O11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H33(0.5) H33A(0.5) C34(0.5) H34(0.5) H35(0.5) H35A(0.5) C34A(0.5)
 H34A(0.5) N4(0.5) O11(0.5) C41(0.5) H41(0.5) C39(0.5) H39A(0.5) H39B(0.5)
 H39C(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5)
7.a Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C38(H38A,H38B,H38C)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26),
  C29(H29), C33(H33), C33(H33A), C34(H34), C35(H35), C35(H35A), C34A(H34A),
 C41(H41)
7.c Fitted pentagon refined as free rotating group:
 C32(C33,C34,C35,C36)
7.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              57641
_olex2_submission_special_instructions 'No special instructions were received'