2-Phenylbenzothiazolyl iridium complexes as inhibitors and probes of amyloid β aggregation.
Terpstra, Karna; Huang, Yiran; Na, Hanah; Sun, Liang; Gutierrez, Citlali; Yu, Zhengxin; Mirica, Liviu M.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14258–14264; doi:10.1039/d4dt01691b

data_7716822
_publ_section_title
;
 2-Phenylbenzothiazolyl iridium complexes as inhibitors and probes of
 amyloid &#x3b2; aggregation.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14258
_journal_page_last               14264
_journal_paper_doi               10.1039/d4dt01691b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C30 H22 Ir N4 S2, C H Cl3, B F4'
_chemical_formula_sum            'C31 H23 B Cl3 F4 Ir N4 S2'
_chemical_formula_weight         901.01
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-19 deposited with the CCDC.	2024-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                94.55
_cell_angle_beta                 92.96
_cell_angle_gamma                93.46
_cell_formula_units_Z            2
_cell_length_a                   8.7808(2)
_cell_length_b                   11.9226(3)
_cell_length_c                   15.5911(4)
_cell_measurement_reflns_used    92764
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.296
_cell_measurement_theta_min      2.607
_cell_volume                     1621.51(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker D8 Venture'
_diffrn_detector_type            'CPAD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa/PhotonII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  multi-mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            119223
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_min         2.246
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Ius microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.546
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1001 before and 0.0498 after correction. The Ratio of minimum to maximum transmission is 0.6739. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.299
_exptl_crystal_size_min          0.206
_refine_diff_density_max         1.238
_refine_diff_density_min         -1.683
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         8069
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0363P)^2^+5.6485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7935
_reflns_number_total             8069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01691b2.cif
_cod_data_source_block           1_a
_cod_depositor_comments          'Adding full bibliography for 7716822.cif.'
_cod_database_code               7716822
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.454
_shelx_estimated_absorpt_t_min   0.308
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-F1 \\sim B1-F3
 with sigma of 0.02
 F1A-B1 \\sim F1-B1 \\sim F3A-B1 \\sim F3-B1 \\sim F4A-B1 \\sim F4-B1 \\sim
F2A-B1 \\sim F2-B1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F2A \\sim F2 \\sim F3 \\sim F3A \\sim F1A \\sim F1 \\sim F4A \\sim F4: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F4A)=Sof(F2A)=Sof(F1A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F3)=Sof(F2)=Sof(F4)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C31(H31)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C2(H2), C5(H5), C18(H18), C25(H25), C3(H3),
 C4(H4), C24(H24), C22(H22), C23(H23), C12(H12), C10(H10), C9(H9), C11(H11)
5.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              23409
_shelx_hkl_checksum              17778
_olex2_submission_special_instructions 'No special instructions were received'