Tuning symmetry and magnetic blocking of an exchange-coupled lanthanide ion in isomeric, tetrametallic complexes: [LnCl<sub>6</sub>(TiCp<sub>2</sub>)<sub>3</sub>].
Jiang, Ningxin; Nakritskaia, Daria D.; Xie, Jiaze; Ramanathan, Arun; Varganov, Sergey A.; La Pierre, Henry S.; Chemical science 14 (2023) 4302–4307; doi:10.1039/d2sc06263a

data_1568696
_publ_section_title
;
 Tuning symmetry and magnetic blocking of an exchange-coupled lanthanide
 ion in isomeric, tetrametallic complexes:
 [LnCl<sub>6</sub>(TiCp<sub>2</sub>)<sub>3</sub>].
;
_journal_issue                   16
_journal_name_full               'Chemical science'
_journal_page_first              4302
_journal_page_last               4307
_journal_paper_doi               10.1039/d2sc06263a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C30 H30 Cl6 Tb Ti3'
_chemical_formula_sum            'C30 H30 Cl6 Tb Ti3'
_chemical_formula_weight         905.86
_chemical_name_systematic        C30H30Cl6TbTi3
_chemical_properties_physical    Air-sensitive
_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   geom
_audit_creation_date             2021-04-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-10 deposited with the CCDC.	2023-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.419(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7966(8)
_cell_length_b                   21.4650(13)
_cell_length_c                   12.9750(7)
_cell_measurement_reflns_used    9034
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.537
_cell_measurement_theta_min      2.580
_cell_volume                     3245.2(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_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  0.0572
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38624
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.545
_diffrn_reflns_theta_min         1.968
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.379
_exptl_absorpt_correction_T_max  0.6385
_exptl_absorpt_correction_T_min  0.4354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1167 before and 0.1066 after correction. The Ratio of minimum to maximum transmission is 0.6914. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       prism
_exptl_crystal_F_000             1772
_exptl_crystal_preparation
'Mix (Cp2TiCl)2 and TbCl3 in toluene, stir overnight,Magnetic properties'
_exptl_crystal_recrystallization_method 'Sovlent diffusion.'
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.156
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         9885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0474P)^2^+3.9597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9261
_reflns_number_total             9885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06263a2.cif
_cod_data_source_block           mo_a737_0m
_cod_depositor_comments
'Adding full bibliography for 1568691--1568696.cif.'
_cod_database_code               1568696
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.621
_shelx_estimated_absorpt_t_min   0.355
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C6(H6), C10(H10), C9(H9), C25(H25), C1(H1), C11(H11),
 C16(H16), C29(H29), C5(H5), C21(H21), C2(H2), C30(H30), C4(H4), C24(H24),
 C22(H22), C3(H3), C26(H26), C27(H27), C15(H15), C17(H17), C23(H23), C20(H20),
 C12(H12), C28(H28), C13(H13), C18(H18), C19(H19), C14(H14)
;
_olex2_exptl_crystal_mounting_method N.A.
_olex2_submission_original_sample_id C30H30Cl6TbTi3
_olex2_submission_special_instructions 'No special instructions were received'