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_7712915
_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
'C20.17 H20.33 Dy N4 Na O6 S4, 1.23(H2 O), 0.77(C H4 O)'
_chemical_formula_sum            'C20.93 H25.87 Dy N4 Na O8 S4'
_chemical_formula_weight         775.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 91.676(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7198(11)
_cell_length_b                   13.9626(11)
_cell_length_c                   15.8515(13)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.96
_cell_volume                     2814.0(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39350
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_min         1.944
_exptl_absorpt_coefficient_mu    3.019
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1112 before and 0.0524 after correction. The Ratio of minimum to maximum transmission is 0.8621. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       block
_exptl_crystal_F_000             1538
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6464
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+3.0328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5879
_reflns_number_total             6464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00714f2.cif
_cod_data_source_block           2b
_cod_database_code               7712915
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.660
_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,H) groups, All O(H,H,H) groups
2. Restrained distances
 O8-H8A
 0.86 with sigma of 0.02
3. Rigid bond restraints
 C22, O9, O8
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
4. Uiso/Uaniso restraints and constraints
O5 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C22, O9, O8
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
6. Others
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(1)
 Sof(H5B)=FVAR(1)
 Sof(O9)=Sof(H9A)=Sof(H9B)=1-FVAR(2)
 Sof(O8)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(H8A)=FVAR(2)
7.a Free rotating group:
 O9(H8A,H9A,H9B)
7.b Rotating group:
 O5(H5B,H5A), O6(H6A,H6B)
7.c Me refined with riding coordinates:
 C21(H21A,H21B,H21C)
7.d 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)
7.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              8174
_shelx_hkl_checksum              65820
_olex2_submission_special_instructions 'No special instructions were received'