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_7716806
_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         'C34  H31  F6  Ir  N7  P'
_chemical_formula_sum            'C34 H31 F6 Ir N7 P'
_chemical_formula_weight         874.83
_chemical_name_systematic
'[Ir(PyBIm)(dmfp)~2~]PF~6~ \\cdot H~2~O -[(2-(2-pyridyl)benzimidazole-\k^2^N,N?)-bis(3,5-dimethyl-1-phenyl-1H-pyrazole-\k^2^N,C)iridium(III)] hexafluorophosphate'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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             2024-07-17
_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                 93.152(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6526(4)
_cell_length_b                   17.3070(3)
_cell_length_c                   27.5369(8)
_cell_measurement_reflns_used    44306
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      2.30
_cell_volume                     7924.3(3)
_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-2016/6 (Sheldrick, 2016)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0577
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            47200
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.298
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.469
_exptl_absorpt_correction_T_max  0.7909
_exptl_absorpt_correction_T_min  0.5680
_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            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.548
_refine_diff_density_min         -2.079
_refine_diff_density_rms         0.284
_refine_ls_extinction_coef       0.00164(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         15532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0851
_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^)+(0.1473P)^2^+84.4243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2545
_refine_ls_wR_factor_ref         0.2711
_reflns_Friedel_coverage         0
_reflns_number_gt                11150
_reflns_number_total             15532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01796j2.cif
_cod_data_source_block           b2_2021
_cod_depositor_comments
'Adding full bibliography for 7716806--7716809.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7716806
_shelx_shelxl_version_number     2018/3
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_smtbx_masks_special_details
;
A solvent mask was calculated and 426 electrons were 
found in a volume of 1984\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C2H6O] per Asymmetric Unit 
which account for 416 electrons 
per unit cell.
;