Synthesis of theophylline-based iridium(I) N-heterocyclic carbene complexes including fluorinated-thiophenolate ligands. Preliminary evaluation of their in vitro anticancer activity
Eslava-Gonzalez, Itzel; Valdés, Hugo; Teresa Ramírez-Apan, María; Hernandez-Ortega, Simón; Rosario Zermeño-Ortega, Miriam; Avila-Sorrosa, Alcives; Morales-Morales, David; Inorganica Chimica Acta 507 (2020) 119588–; doi:10.1016/j.ica.2020.119588

data_1564748
_publ_section_title
;
 Synthesis of theophylline-based iridium(I) N-heterocyclic carbene
 complexes including fluorinated-thiophenolate ligands. Preliminary
 evaluation of their in vitro anticancer activity
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119588
_journal_paper_doi               10.1016/j.ica.2020.119588
_journal_volume                  507
_journal_year                    2020
_chemical_formula_moiety         'C29 H28 F4 Ir N4 O2 S'
_chemical_formula_sum            'C29 H28 F4 Ir N4 O2 S'
_chemical_formula_weight         764.81
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                78.7458(14)
_cell_angle_beta                 86.3229(14)
_cell_angle_gamma                77.6856(14)
_cell_formula_units_Z            2
_cell_length_a                   7.3026(4)
_cell_length_b                   9.4501(5)
_cell_length_c                   20.9232(10)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.25
_cell_volume                     1383.19(12)
_computing_cell_refinement       'APEX3 v2016.1 (Bruker, 2014)'
_computing_data_collection       'APEX3 v2016.1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.37A  (Bruker, 2014)'
_computing_molecular_graphics
'Ortep-3 Ver 2.02 L.J. Farrugia (1997) J. Appl. Cryst. 30, 565'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Bruker, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 52.0833
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Bruker D8 Venture \k-geometry diffractometer 208039-01'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15479
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.364
_diffrn_reflns_theta_min         2.245
_diffrn_source                   'micro-focus X-ray source'
_exptl_absorpt_coefficient_mu    4.964
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_description       'Prism from CH2Cl2,'
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.465
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0277P)^2^+0.9266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4578
_reflns_number_total             5059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            499MMD18.cif
_cod_data_source_block           499MMD18
_cod_database_code               1564748
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.304
_shelx_estimated_absorpt_t_max   0.838
_shelx_res_checksum              22056
_shelx_hkl_checksum              47356