Modulation of the magnetic properties of mononuclear Dy(III) complexes by tuning the coordination geometry and local symmetry.
Zhou, Xuejuan; Qin, Huiliang; Zeng, Zhaopeng; Luo, Shuchang; Yang, Tao; Cen, Peipei; Liu, Xiangyu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16219–16228; doi:10.1039/d4dt02135e

data_7717001
_publ_section_title
;
 Modulation of the magnetic properties of mononuclear Dy(III) complexes by
 tuning the coordination geometry and local symmetry.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16219
_journal_page_last               16228
_journal_paper_doi               10.1039/d4dt02135e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'2(C28 H32 Cl2 Dy N7 O5), 1.5(C6 H2 Cl2 N O3), 2(F6 P), H2 O, 0.5(C6 Cl2 N O3)'
_chemical_formula_sum            'C68 H69 Cl8 Dy2 F12 N16 O17 P2'
_chemical_formula_weight         2280.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2024-04-01 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                105.480(2)
_cell_angle_beta                 91.339(2)
_cell_angle_gamma                103.205(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6622(7)
_cell_length_b                   18.6466(12)
_cell_length_c                   19.8147(13)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      2.17
_cell_volume                     4371.7(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0441
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            68773
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.709
_diffrn_reflns_theta_max         24.709
_diffrn_reflns_theta_min         1.659
_exptl_absorpt_coefficient_mu    2.075
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6826
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0833 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.9161.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       block
_exptl_crystal_F_000             2262
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.663
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1285
_refine_ls_number_reflns         14798
_refine_ls_number_restraints     411
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0455P)^2^+15.1934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12155
_reflns_number_total             14798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02135e2.cif
_cod_data_source_block           xj6_22
_cod_depositor_comments
'Adding full bibliography for 7717000--7717002.cif.'
_cod_database_code               7717001
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.774
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Cl7B-C58A = Cl8A-C62A
 1.73 with sigma of 0.01
 O16A-C57C
 1.3 with sigma of 0.01
 N15A-C61A \\sim N15A-C59A
 with sigma of 0.02
 O14A-C60A \\sim O15A-C60A
 with sigma of 0.02
 O16A-C62A \\sim O16A-C58A
 with sigma of 0.02
 Cl7B-C57C \\sim Cl7B-C59A
 with sigma of 0.02
 Cl8A-C57C \\sim Cl8A-C61A
 with sigma of 0.02
 O11C-N16A \\sim O11B-N16
 with sigma of 0.02
 N16-C63 \\sim N16A-C63
 with sigma of 0.02
 O12-N16 \\sim O12A-N16A
 with sigma of 0.02
 O12-O11B \\sim O12A-O11C
 with sigma of 0.02
 N3-C8A \\sim N3-C8
 with sigma of 0.02
 C8A-C10 \\sim C8-C10
 with sigma of 0.02
 C9C-C8A \\sim C9B-C8
 with sigma of 0.02
3. Restrained planarity
 O16A, C58A, C57C, C59A, Cl7B, C62A, C60A, C61A, Cl8A, N15A, O14A, O15A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Cl8 \\sim C58 \\sim C59 \\sim C57 \\sim C60 \\sim O16 \\sim C9 \\sim N15 \\sim
C61 \\sim Cl7 \\sim O14 \\sim O15: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O16A \\sim C58A \\sim C57C \\sim C59A \\sim Cl7B \\sim C62A \\sim C60A \\sim
C61A \\sim Cl8A \\sim N15A \\sim O14A \\sim O15A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
N16 \\sim O11B \\sim O12 \\sim N16A \\sim O11C \\sim O12A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C8 \\sim C8A \\sim C9C \\sim C9B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(Cl8) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(N15) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(Cl7) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
5. Rigid body (RIGU) restrains
 C63, N16, O12, O11B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C63, N16A, O11C, O12A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C10, C8, N3, C9B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C10, C8A, N3, C9C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Sof(N16A)=Sof(O11C)=Sof(O12A)=1-FVAR(1)
 Sof(N16)=Sof(O11B)=Sof(O12)=FVAR(1)
 Sof(C8A)=Sof(C9C)=Sof(H9CA)=Sof(H9CB)=Sof(H9CC)=1-FVAR(2)
 Sof(C8)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=FVAR(2)
 Fixed Sof: C57C(0.5) C62A(0.5) C61A(0.5) H61A(0.5) C60A(0.5) C59A(0.5)
 H59A(0.5) C58A(0.5) O16A(0.5) Cl7B(0.5) Cl8A(0.5) N15A(0.5) O14A(0.5)
 O15A(0.5) Cl8(0.5) Cl7(0.5) O14(0.5) O16(0.5) C60(0.5) N15(0.5) O15(0.5)
 C59(0.5) C61(0.5) C58(0.5) C9(0.5) C57(0.5)
7.a Free rotating group:
 O11(H11A,H11B)
7.b Rotating group:
 O4(H4A,H4B), O5(H5D,H5E), O9(H9A,H9B), O10(H10A,H10B)
7.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C17(H17A,H17B), C18(H18A,H18B), C34(H34A,H34B),
 C35(H35A,H35B), C45(H45A,H45B), C46(H46A,H46B)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C11(H11), C12(H12), C13(H13), C22(H22), C25(H25), C27(H27),
 C29(H29), C30(H30), C39(H39), C40(H40), C41(H41), C50(H50), C53(H53), C55(H55),
  C64(H64), C68(H68), C61A(H61A), C59A(H59A)
7.e Fitted hexagon refined as free rotating group:
 C57C(C62A,C61A,C60A,C59A,C58A)
7.f Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C9B(H9BA,H9BB,H9BC), C16(H16A,H16B,H16C), C20(H20A,H20B,
 H20C), C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C), C48(H48A,
 H48B,H48C), C9C(H9CA,H9CB,H9CC)
;
_shelx_res_checksum              33707
_shelx_hkl_checksum              66660
_olex2_submission_special_instructions 'No special instructions were received'