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_7711699
_publ_section_title
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 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
'C50 H58 Dy2 N12 O18, 2(H2 O), 2(C H4 O), 6[H2O]'
_chemical_formula_sum            'C52 H82 Dy2 N12 O28'
_chemical_formula_weight         1648.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-10-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-20 deposited with the CCDC.	2022-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.776(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4197(13)
_cell_length_b                   15.2284(10)
_cell_length_c                   24.1517(13)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.108
_cell_measurement_theta_min      2.205
_cell_volume                     7110.5(8)
_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      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21851
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.116
_diffrn_reflns_theta_min         1.607
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.171
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0690 before and 0.0477 after correction.
The Ratio of minimum to maximum transmission is 0.8013.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.295
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         7063
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0610P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5895
_reflns_number_total             7063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02996k2.cif
_cod_data_source_block           Dy2-1
_cod_database_code               7711699
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O10-C26
 1.4 with sigma of 0.02
 O4-H4
 0.85 with sigma of 0.01
 Dy1-H4
 2.948477 with sigma of 0.02
 C25-H4
 1.915054 with sigma of 0.02
3. Rigid bond restraints
 O4, C25
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O4 \\sim C25: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
O10 \\sim C26: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
5.a Everything fixed:
 O10, H10A
5.b Free rotating group:
 O9(H9A,H9B)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), C3(H3A), C4(H4A), C5(H5A), C8(H8), C10(H10), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
5.e Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 260 electrons were 
found in a volume of 1370\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
6[H2O] per Asymmetric Unit 
which account for 240 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7632
_shelx_hkl_checksum              19777
_shelx_fab_checksum              21262
_olex2_submission_special_instructions 'No special instructions were received'