Enhancing magnetic relaxation through subcomponent self-assembly from a Dy2 to Dy4 grid
Li, Xiao-Lei; Ma, Zhifang; Wu, Jinjiang; Zhou, Quan; Tang, Jinkui; Dalton Transactions  (2022) –; doi:10.1039/D2DT02996K

data_7711697
_publ_section_title
;
 Enhancing magnetic relaxation through subcomponent self-assembly from a
 Dy2 to Dy4 grid
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02996K
_journal_year                    2022
_chemical_formula_moiety         'C32 H46 Dy2 N14 O20, 2(C3 H7 N O)'
_chemical_formula_sum            'C38 H60 Dy2 N16 O22'
_chemical_formula_weight         1418.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-10-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-10-20 deposited with the CCDC.	2022-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.499(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.314(5)
_cell_length_b                   14.009(3)
_cell_length_c                   19.509(4)
_cell_measurement_reflns_used    8607
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.20
_cell_volume                     5613(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(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 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17535
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.186
_diffrn_reflns_theta_min         1.760
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.729
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0650 before and 0.0453 after correction.
The Ratio of minimum to maximum transmission is 0.8013.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5574
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0311P)^2^+3.8673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4497
_reflns_number_total             5574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02996k2.cif
_cod_data_source_block           Dy2
_cod_database_code               7711697
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N7-C16 \\sim N7-C17
 with sigma of 0.02
 C13-O10 \\sim C13A-O10
 with sigma of 0.02
 C13-N7 \\sim C13A-N7
 with sigma of 0.02
 N7-C16 \\sim N7-C16A
 with sigma of 0.02
 N7-C17 \\sim N7-C17A
 with sigma of 0.02
3. Restrained planarity
 C13, O10, N7, C16, C17
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C13 \\sim O10 \\sim N7 \\sim C16 \\sim C17: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C13, O10, N7, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C13A)=Sof(H13A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C16A)=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(C13)=Sof(H13)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=
 Sof(H17B)=Sof(H17C)=FVAR(1)
7.a Riding coordinates:
 N2(H2)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C12(H12), C15(H15), C20(H20),
 C13(H13), C13A(H13A)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C17A(H17D,H17E,H17F), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              66766
_shelx_hkl_checksum              68794
_olex2_submission_special_instructions 'No special instructions were received'