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_7711698
_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         'C48 H54 Dy2 N12 O16.7, 2(C H4 O)'
_chemical_formula_sum            'C50 H62 Dy2 N12 O18.7'
_chemical_formula_weight         1455.31
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                 100.741(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3758(17)
_cell_length_b                   12.797(2)
_cell_length_c                   22.018(3)
_cell_measurement_reflns_used    6859
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.36
_cell_volume                     3149.1(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 0.992
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19190
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.224
_diffrn_reflns_theta_min         1.822
_exptl_absorpt_coefficient_mu    2.430
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0692 before and 0.0544 after correction.
The Ratio of minimum to maximum transmission is 0.8456.
The \l/2 correction factor is Not present.
;
_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    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             1455
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.465
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6284
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.5236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4076
_reflns_number_total             6284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02996k2.cif
_cod_data_source_block           Dy2-2
_cod_original_formula_sum        'C50 H62 Dy2 N12 O18.70'
_cod_database_code               7711698
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.571
_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
 O9-C25A \\sim O9-C25B
 with sigma of 0.001
3. Rigid bond restraints
 C18, O7, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C19 \\sim C20 \\sim C22 \\sim C18 \\sim O7 \\sim C24: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 O9, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C17, C12, C13, C14, C15, C16, O26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, C5, C19, C20, C22, C18, O7, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H9B)=Sof(C25B)=Sof(H25A)=Sof(H25B)=Sof(H25C)=1-FVAR(1)
 Sof(H9A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=FVAR(1)
 Fixed Sof: H16(0.65) O26(0.35) H26(0.35)
 Fixed Uiso: C25B(0.12) C25A(0.12)
7.a Riding coordinates:
 O26(H26)
7.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4A), C1(H1), C11(H11), C10(H10), C6(H6), C13(H13), C14(H14),
 C15(H15), C16(H16), C20(H20), C22(H22), C19(H19)
7.c Tetrahedral OH refined with riding coordinates:
 O9(H9B), O9(H9A)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25B(H25A,H25B,H25C), C25A(H25D,H25E,H25F)
7.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O8(H8)
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_smtbx_masks_special_details
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A solvent mask was calculated and 48 electrons were 
found in a volume of 308\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2.5[H2O] per Formula Unit 
which account for 50 electrons per unit cell.
;
_shelx_res_checksum              94422
_shelx_hkl_checksum              54700
_shelx_fab_checksum              21510
_olex2_submission_special_instructions 'No special instructions were received'