Trinuclear rare earth pyridyl-β-diketonate complexes: developing new methods towards finding lost toroidal spin states.
Mangundu, Patrick; Tanner, Kate E.; Bloomfield, Andrew; Barnard, Peter J.; White, Keith F.; Ho, Curtis C.; Yepuri, Nageshwar R.; Mole, Richard A.; Fuller, Rebecca O.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10455–10466; doi:10.1039/d5dt01067e

data_7718899
_publ_section_title
;
 Trinuclear rare earth pyridyl-&#x3b2;-diketonate complexes: developing
 new methods towards finding lost toroidal spin states.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10455
_journal_page_last               10466
_journal_paper_doi               10.1039/d5dt01067e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'2(C27 H34 Cl Dy3 N3 O13), 6(Cl), 1[Cl2C16H40O2]'
_chemical_formula_sum            'C70 H108 Cl10 Dy6 N6 O28'
_chemical_formula_weight         2811.12
_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             2025-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-05-05 deposited with the CCDC.	2025-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                85.924(3)
_cell_angle_beta                 89.925(2)
_cell_angle_gamma                74.263(3)
_cell_formula_units_Z            2
_cell_length_a                   15.6133(4)
_cell_length_b                   18.1248(6)
_cell_length_c                   18.1431(7)
_cell_measurement_reflns_used    13795
_cell_measurement_temperature    150.1(10)
_cell_measurement_theta_max      70.65
_cell_measurement_theta_min      2.92
_cell_volume                     4928.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.817
_diffrn_measured_fraction_theta_max 0.810
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix3000'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.817
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52996
_diffrn_reflns_point_group_measured_fraction_full 0.817
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.380
_diffrn_reflns_theta_min         2.941
_exptl_absorpt_coefficient_mu    26.966
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_correction_T_min  0.121
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       plate
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.916
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         15548
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0741P)^2^+9.1632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11728
_reflns_number_total             15548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01067e2.cif
_cod_data_source_block           complex_2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_cell_measurement_temperature' value '150.1 (1)' was
changed to '150.1(10)' -- precision was estimated.

data item '_diffrn_ambient_temperature' value '150.0 (1)' was changed
to '150.0(10)' -- precision was estimated.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7718894--7718899.cif.
;
_cod_database_code               7718899
_shelx_shelxl_version_number     2018/3
_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
 Dy6-H26A \\sim Dy6-H26B
 with sigma of 0.02
 Dy1-H11A \\sim Dy1-H11B
 with sigma of 0.02
 Dy4-H24A \\sim Dy4-H24B
 with sigma of 0.02
 Dy3-H12A \\sim Dy3-H12B
 with sigma of 0.02
3. Others
 Fixed Sof: O17B(0.5) N4B(0.5) H37A(0.5) H37(0.5) C44B(0.5) C32B(0.5)
 C38B(0.5) H38B(0.5) H43A(0.5) H43(0.5) C40B(0.5) H40B(0.5) C39B(0.5) H39B(0.5)
 C45B(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C31B(0.5) H31B(0.5) C30B(0.5)
 H30B(0.5) C28B(0.5) H28B(0.5) C29B(0.5) H29B(0.5) C28A(0.5) H28A(0.5)
 C29A(0.5) H29A(0.5) C30A(0.5) H30A(0.5) C31A(0.5) H31A(0.5) C32A(0.5) N4A(0.5)
 C45A(0.5) H45D(0.5) H45E(0.5) H45F(0.5) C44A(0.5) C39A(0.5) H39A(0.5)
 C38A(0.5) H38A(0.5) C40A(0.5) H40A(0.5) O17A(0.5)
4.a Free rotating group:
 O26(H26A,H26B), O11(H11A,H11B), O24(H24A,H24B), O12(H12A,H12B)
4.b Rotating group:
 O23(H23A,H23B), O22(H22A,H22B), O25(H25A,H25B), O9(H9A,H9B), O10(H10A,H10B),
 O13(H13A,H13B)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C25(H25), C16(H16), C13(H13), C52(H52), C49(H49), C11(H11),
 C46(H46), C12(H12), C7(H7), C37(H37A), C37(H37), C4(H4), C22(H22), C19(H19),
 C47(H47), C1(H1), C21(H21), C3(H3), C38B(H38B), C34(H34), C2(H2), C20(H20),
 C48(H48), C43(H43A), C43(H43), C40B(H40B), C39B(H39B), C31B(H31B), C30B(H30B),
 C28B(H28B), C29B(H29B), C28A(H28A), C29A(H29A), C30A(H30A), C31A(H31A),
 C39A(H39A), C38A(H38A), C40A(H40A)
4.d Idealised Me refined as rotating group:
 C9(H9C,H9D,H9E), C27(H27A,H27B,H27C), C18(H18A,H18B,H18C), C54(H54A,H54B,
 H54C), C45B(H45A,H45B,H45C), C36(H36A,H36B,H36C), C45A(H45D,H45E,H45F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 376 electrons were 
found in a volume of 1352\%A^3^ in 1 void per unit cell. 
This is consistent with 2Cl- ions, 2EtOH and 2Hexane 
molecules per Asymmetric Unit which account for 374
electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'