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_7716079
_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 F N9 O2 Y, F6 P, C H1.5, 0.5(N)'
_chemical_formula_sum            'C33 H36.5 B F7 N9.5 O2 P Y'
_chemical_formula_weight         861.90
_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             2023-06-21
_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                 125.349(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.635(2)
_cell_length_b                   12.2783(7)
_cell_length_c                   22.9447(14)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      33.154
_cell_measurement_theta_min      2.357
_cell_volume                     7269.2(8)
_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      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            113873
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.356
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.731
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1251 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.8098.
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    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         10604
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+28.6205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9038
_reflns_number_total             10604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01194e2.cif
_cod_data_source_block           jrt199_230508_0m_a
_cod_depositor_comments
'Adding full bibliography for 7716079--7716080.cif.'
_cod_original_cell_volume        7269.1(8)
_cod_original_formula_sum        'C33 H36.50 B F7 N9.50 O2 P Y'
_cod_database_code               7716079
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.625
_shelx_estimated_absorpt_t_min   0.478
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32-C31 \\sim C32-C31A
 with sigma of 0.02
 C30-C31 \\sim C30-C31A
 with sigma of 0.02
3. Others
 Fixed Sof: H32A(0.85) H32B(0.85) H32C(0.15) H32D(0.15) H30A(0.85) H30B(0.85)
 H30C(0.15) H30D(0.15) C31(0.85) H31A(0.85) H31B(0.85) C31A(0.15) H31C(0.15)
 H31D(0.15) H33A(0.5) H33B(0.5) H33C(0.5) N10(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C32(H32A,H32B), C32(H32C,H32D), C28(H28A,H28B), C26(H26A,
 H26B), C25(H25A,H25B), C27(H27A,H27B), C30(H30A,H30B), C30(H30C,H30D),
 C31(H31A,H31B), C31A(H31C,H31D)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C10(H10), C2(H2), C9(H9), C13(H13), C24(H24), C15(H15), C1(H1),
 C17(H17), C14(H14), C8(H8), C18(H18), C21(H21), C23(H23), C22(H22), C6(H6),
 C7(H7), C5(H5)
4.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              96751
_olex2_submission_special_instructions 'No special instructions were received'