Spectroscopic, structural and photophysical characterization of chloro-bridged iridium(III) and rhodium(III) dinuclear complexes with 1-phenyl-1<i>H</i>-pyrazole and their analogues with 1-(2,4-difluorophenyl)-1<i>H</i>-pyrazole.
Wójcik, Patryk; Latouche, Camille; Suwińska, Kinga; Kamecka, Anna; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12018–12029; doi:10.1039/d5dt01156f

data_1575081
_publ_section_title
;
 Spectroscopic, structural and photophysical characterization of
 chloro-bridged iridium(III) and rhodium(III) dinuclear complexes with
 1-phenyl-1<i>H</i>-pyrazole and their analogues with
 1-(2,4-difluorophenyl)-1<i>H</i>-pyrazole.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12018
_journal_page_last               12029
_journal_paper_doi               10.1039/d5dt01156f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C36 H28 Cl2 Ir2 N8'
_chemical_formula_sum            'C36 H28 Cl2 Ir2 N8'
_chemical_formula_weight         1027.96
_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
_atom_sites_solution_primary     'Intrinsic Phasing'
_audit_creation_method
;FinalCif 2024.9-0 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-03-14 deposited with the CCDC.	2025-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.266(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2164(9)
_cell_length_b                   11.4613(10)
_cell_length_c                   29.273(3)
_cell_measurement_reflns_used    9513
_cell_measurement_temperature    297.15
_cell_measurement_theta_max      25.3484
_cell_measurement_theta_min      2.6708
_cell_measurement_wavelength     0.71073
_cell_volume                     3427.6(6)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'Bruker Instrument Service v8.5.5.6'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.391
_diffrn_detector_type            PhotonII_7
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;<Phi   scan: start=   0.0; len= 180.0; end= 180.0 at [Counterclockwise Eulerian 
angles: dx= 58.82 mm theta=   0.000 deg omega=   0.000 deg chi=  54.739 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Omega scan: start= 187.9; len= 199.0; end= 386.9 at [Counterclockwise Eulerian 
angles: dx= 58.82 mm theta=   8.899 deg phi=  50.999 deg chi=  54.739 deg] 
measure for 15.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Omega scan: start= 187.9; len= 199.0; end= 386.9 at [Counterclockwise Eulerian 
angles: dx= 58.82 mm theta=   8.899 deg phi= 203.999 deg chi=  54.739 deg] 
measure for 15.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Omega scan: start= 187.9; len= 199.0; end= 386.9 at [Counterclockwise Eulerian 
angles: dx= 58.82 mm theta=   8.899 deg phi= 255.001 deg chi=  54.739 deg] 
measure for 15.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Omega scan: start= 195.8; len= 201.0; end= 396.8 at [Counterclockwise Eulerian 
angles: dx= 58.82 mm theta=  13.348 deg phi=   0.000 deg chi=  54.739 deg] 
measure for 15.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Omega scan: start= 187.9; len= 199.0; end= 386.9 at [Counterclockwise Eulerian 
angles: dx= 58.82 mm theta=   8.899 deg phi= 102.001 deg chi=  54.739 deg] 
measure for 15.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Omega scan: start= 187.9; len= 199.0; end= 386.9 at [Counterclockwise Eulerian 
angles: dx= 58.82 mm theta=   8.899 deg phi= 153.000 deg chi=  54.739 deg] 
measure for 15.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Omega scan: start= 187.9; len= 199.0; end= 386.9 at [Counterclockwise Eulerian 
angles: dx= 58.82 mm theta=   8.899 deg phi= 306.000 deg chi=  54.739 deg] 
measure for 15.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Omega scan: start= 187.9; len= 199.0; end= 386.9 at [Counterclockwise Eulerian 
angles: dx= 58.82 mm theta=   8.899 deg phi=   0.000 deg chi=  54.739 deg] 
measure for 15.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 255.7; len= 232.0; end= 487.7 at [Counterclockwise Eulerian 
angles: dx= 58.82 mm theta=   8.899 deg omega= 186.923 deg chi=  54.739 deg] 
measure for 15.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
;
_diffrn_measurement_device       'FIXEDCHI diffractometer'
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            96689
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.358
_diffrn_reflns_theta_min         2.108
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_target            Mo
_diffrn_source_type              'INCOATEC I\mS'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.952
_exptl_absorpt_correction_T_max  0.606
_exptl_absorpt_correction_T_min  0.112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.155
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+10.2075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5582
_reflns_number_total             6218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01156f2.cif
_cod_data_source_block           mo_S306a_1_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1575081--1575082.cif.
;
_cod_original_cell_volume        3427.7(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1575081
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.6311
_shelx_estimated_absorpt_t_min   0.112
_shelx_estimated_absorpt_t_max   0.606
_bruker_diffrn_measurement_temperature_device Cryostream
_diffrn_measurement_bruker_total_exposure_time 27570.0
_diffrn_reflns_bruker_av_norm_i  3873.029
_diffrn_reflns_bruker_number_gt  92426
_computing_bruker_data_scaling
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_geom_details
; All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_shelx_res_checksum              77000
_shelx_hkl_checksum              75706