Approaching the 1000 K energy barrier in high coordinate lanthanide single-ion magnets: Increasing <i>U</i><sub>eff</sub> in the [Dy(Tp<sup>2-py</sup>)F]<sup>+</sup> moiety with tetrahydrofuran.
Thomas, Jarrod R.; Giansiracusa, Marcus J.; Sulway, Scott A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9252–9256; doi:10.1039/d4dt01194e

data_7716080
_publ_section_title
;
 Approaching the 1000 K energy barrier in high coordinate lanthanide
 single-ion magnets: Increasing <i>U</i><sub>eff</sub> in the
 [Dy(Tp<sup>2-py</sup>)F]<sup>+</sup> moiety with tetrahydrofuran.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9252
_journal_page_last               9256
_journal_paper_doi               10.1039/d4dt01194e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H35 B Dy F N9 O2, F6 P'
_chemical_formula_sum            'C32 H35 B Dy F7 N9 O2 P'
_chemical_formula_weight         914.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.2830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.5818(13)
_cell_length_b                   12.2694(5)
_cell_length_c                   22.8942(9)
_cell_measurement_reflns_used    9401
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      33.194
_cell_measurement_theta_min      2.179
_cell_volume                     7241.7(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            92218
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.358
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.188
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1339 before and 0.0790 after correction.
The Ratio of minimum to maximum transmission is 0.6012.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       block
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.432
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0048P)^2^+84.8420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7382
_reflns_number_total             8994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01194e2.cif
_cod_data_source_block           jrt204_240111_a
_cod_depositor_comments
'Adding full bibliography for 7716079--7716080.cif.'
_cod_database_code               7716080
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.408
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C29(H29A,H29B), C26(H26A,H26B), C28(H28A,H28B), C32(H32A,
 H32B), C31(H31A,H31B), C27(H27A,H27B), C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C2(H2), C1(H1), C23(H23), C9(H9), C16(H16), C24(H24), C22(H22),
 C8(H8), C10(H10), C17(H17), C21(H21), C7(H7), C6(H6), C15(H15), C5(H5),
 C13(H13), C14(H14)
;
_shelx_res_checksum              31833
_olex2_submission_special_instructions 'No special instructions were received'