Synthesis, photophysical characterisation, quantum-chemical study and <i>in vitro</i> antiproliferative activity of cyclometalated Ir(III) complexes based on 3,5-dimethyl-1-phenyl-1<i>H</i>-pyrazole and N,N-donor ligands.
Masternak, Joanna; Okła, Karol; Kubas, Adam; Voller, Jiří; Kozlanská, Karolína; Zienkiewicz-Machnik, Małgorzata; Gilewska, Agnieszka; Sitkowski, Jerzy; Kamecka, Anna; Kazimierczuk, Katarzyna; Barszcz, Barbara; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14438–14450; doi:10.1039/d4dt01796j

data_7716808
_publ_section_title
;
 Synthesis, photophysical characterisation, quantum-chemical study and
 <i>in vitro</i> antiproliferative activity of cyclometalated Ir(III)
 complexes based on 3,5-dimethyl-1-phenyl-1<i>H</i>-pyrazole and N,N-donor
 ligands.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14438
_journal_page_last               14450
_journal_paper_doi               10.1039/d4dt01796j
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C28 H27 Ir N8, F6 P, H2 O'
_chemical_formula_sum            'C28 H29 F6 Ir N8 O P'
_chemical_formula_weight         830.76
_chemical_name_systematic
'[Ir(biim)(dmfp)~2~]PF~6~ \\cdot H~2~O -[(2,2?-biimidazole-\k^2^N,N?)-bis(3,5-dimethyl-1-phenyl-1H-pyrazole-\k^2^N,C)iridium(III)] hexafluorophosphate monohydrate'
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2024-07-18
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2024-07-18 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.228(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1393(10)
_cell_length_b                   10.3689(10)
_cell_length_c                   12.5880(11)
_cell_measurement_reflns_used    25370
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.64
_cell_measurement_theta_min      2.20
_cell_volume                     1571.9(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12977
_diffrn_reflns_point_group_measured_fraction_full 0.889
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.197
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.37
_exptl_absorpt_correction_T_max  0.7013
_exptl_absorpt_correction_T_min  0.5936
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
        Numerical  absorption  correction was  performed
        after the  optimization of  the  crystal-shape
        description due to Herrendorf?s method
        [Herrendorf, 1994]
        Herrendorf,  W. (1994).HABITUS, a program for the
        optimization  of  the  crystal description for
 the numerical absorption correction by means of
        suitable, psi scanned reflections;dissertation
        1994,Karlsruhe;extension 1998,Gie\&sen
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.938
_refine_diff_density_min         -1.695
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.173(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7412
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.7759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.781
_reflns_Friedel_fraction_max     0.755
_reflns_number_gt                7160
_reflns_number_total             7412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01796j2.cif
_cod_data_source_block           b6c_2020
_cod_depositor_comments
'Adding full bibliography for 7716806--7716809.cif.'
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               7716808
_shelx_shelxl_version_number     2018/3