Modulation of the magnetic dynamics in two air-stable sulfur-ligated dysprosium complexes via polymerization
Han, Tian; Wang, Xiao-Qin; Guo, Tong; Cao, Hong-Sheng; Chen, Wei-Peng; He, Ling; Dalton Transactions  (2023) –; doi:10.1039/D3DT00714F

data_7712914
_publ_section_title
;
 Modulation of the magnetic dynamics in two air-stable sulfur-ligated
 dysprosium complexes via polymerization
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00714F
_journal_year                    2023
_chemical_formula_moiety         'C21.29 H22.57 Dy N4 Na O6 S4, 0.74(C H4 O)'
_chemical_formula_sum            'C22.02 H25.52 Dy N4 Na O6.74 S4'
_chemical_formula_weight         767.79
_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
_audit_creation_date             2023-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-04-14 deposited with the CCDC.	2023-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.591(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0840(8)
_cell_length_b                   13.8668(10)
_cell_length_c                   20.6024(14)
_cell_measurement_reflns_used    7351
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.48
_cell_volume                     2855.6(4)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0558
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_number            5013
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.994
_exptl_absorpt_coefficient_mu    2.971
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 28104 reflections, Rint = 0.0558
 (14403 with I > 3sig(I), Rint = 0.0409)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       plate
_exptl_crystal_F_000             1522
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.879
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5013
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+32.8390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4102
_reflns_number_total             5013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00714f2.cif
_cod_data_source_block           2a
_cod_database_code               7712914
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.576
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5B = O5-H5A
 0.87 with sigma of 0.02
 H5B-H5A
 1.38 with sigma of 0.04
 O7-C22 \\sim O7A-C22A
 with sigma of 0.02
 Na1-H5B \\sim Na1-H5A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O7 \\sim C22: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
O7 \\sim C22 \\sim C22A \\sim O7A: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C23 \\sim O5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H5B)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Sof(O7)=Sof(H7A)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(O7A)=Sof(H7AA)=FVAR(3)
5.a Me refined with riding coordinates:
 C23(H23A,H23B,H23C)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C22A(H22D,H22E,H22F)
5.d Idealised tetrahedral OH refined as rotating group:
 O7(H7A), O7A(H7AA)
;
_shelx_res_checksum              39909
_shelx_hkl_checksum              7826
_olex2_submission_special_instructions 'No special instructions were received'