Bis-cyclometalated iridium(iii) complexes with terpyridine analogues: syntheses, structures, spectroscopy and computational studies
Otaif, Haleema Y.; Adams, Samuel J.; Horton, Peter N.; Coles, Simon J.; Beames, Joseph M.; Pope, Simon J. A.; RSC Advances 11 (2021) 39718–39727; doi:10.1039/D1RA07213G

data_7244050
_publ_section_title
;
 Bis-cyclometalated iridium(iii) complexes with terpyridine analogues:
 syntheses, structures, spectroscopy and computational studies
;
_journal_issue                   63
_journal_name_full               'RSC Advances'
_journal_page_first              39718
_journal_page_last               39727
_journal_paper_doi               10.1039/D1RA07213G
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C50 H40 Ir N10, F6 P, 0.5[CH2Cl2]'
_chemical_formula_sum            'C50.5 H41 Cl F6 Ir N10 P'
_chemical_formula_weight         1160.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-04 deposited with the CCDC.	2021-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.009(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0555(5)
_cell_length_b                   17.4269(3)
_cell_length_c                   29.5696(14)
_cell_measurement_reflns_used    13496
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.6720
_cell_measurement_theta_min      2.9890
_cell_volume                     9828.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -55.00  16.00   0.50    3.00    --    0.00   0.00-180.00  142
  2  \w    -72.00  88.00   0.50    3.00    --    5.00  49.00-120.00  320
  3  \w   -132.00 -84.00   0.50   18.00    --  -90.00  59.00-174.53   96
  4  \w   -161.00-112.00   0.50   18.00    --  -90.00  59.00  84.70   98
  5  \w   -108.00 -34.00   0.50   18.00    --  -90.00  59.00  84.70  148
  6  \w   -179.00-117.00   0.50   18.00    --  -90.00  57.00 -83.31  124
  7  \w    -70.00 -29.00   0.50   18.00    --  -90.00  57.00 -83.31   82
  8  \w   -178.00 -78.00   0.50   18.00    --  -90.00  59.00 -31.67  200
  9  \w   -175.00-148.00   0.50   18.00    --  -90.00  59.00  55.72   54
 10  \w   -139.00-111.00   0.50   18.00    --  -90.00  59.00  18.06   56
 11  \w    -59.00 -24.00   0.50   18.00    --  -90.00  59.00  18.06   70
 12  \w   -178.00  -3.00   0.50   18.00    --  -90.00  58.00 136.08  350
 13  \w   -175.00-150.00   0.50   18.00    --  -90.00  56.00-128.56   50
 14  \w    -81.00 -55.00   0.50   18.00    --  -90.00  56.00-128.56   52
 15  \w    -35.00  -9.00   0.50   18.00    --  -90.00  56.00-128.56   52
 16  \w   -106.00 -80.00   0.50   18.00    --  -90.00  57.00 -83.31   52
 17  \w    -69.00 -38.00   0.50   18.00    --  -90.00  59.00-174.53   62
 18  \w   -178.00  -2.00   0.50   18.00    --  -90.00  10.00 150.00  352
 19  \w    -79.00  -2.00   0.50   18.00    --  -90.00  20.00   0.00  154
 20  \w   -144.00  -2.00   0.50   18.00    --  -90.00  59.00  55.72  284
 21  \w   -177.00 -27.00   0.50   18.00    --  -90.00  59.00 164.27  300
 22  \w   -179.00-110.00   0.50   18.00    --  -90.00  59.00  -5.56  138
 23  \w   -146.00-120.00   0.50   18.00    --  -90.00  39.00-120.00   52
 24  \w    -47.00 -20.00   0.50   18.00    --  -90.00  39.00-120.00   54
 25  \w   -158.00-131.00   0.50   18.00    --  -90.00  55.00 -70.74   54
 26  \w   -176.00-133.00   0.50   18.00    --  -90.00  59.00-131.77   86
 27  \w   -131.00 -97.00   0.50   18.00    --  -90.00  59.00-131.77   68
 28  \w   -177.00 -99.00   0.50   18.00    --  -90.00  20.00   0.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0742230500
_diffrn_orient_matrix_UB_12      -0.0060955500
_diffrn_orient_matrix_UB_13      -0.0046478500
_diffrn_orient_matrix_UB_21      0.0314652500
_diffrn_orient_matrix_UB_22      0.0009126500
_diffrn_orient_matrix_UB_23      0.0546064500
_diffrn_orient_matrix_UB_31      -0.0047846000
_diffrn_orient_matrix_UB_32      -0.0881624000
_diffrn_orient_matrix_UB_33      0.0008796000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            60261
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.233
_diffrn_reflns_theta_min         2.983
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    6.659
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.18b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       plate
_exptl_crystal_F_000             4616
_exptl_crystal_recrystallization_method
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.863
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         8958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0842P)^2^+16.5597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6008
_reflns_number_total             8958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra07213g2.cif
_cod_data_source_block           Irdqxp2
_cod_original_formula_sum        'C50.50 H41 Cl F6 Ir N10 P'
_cod_database_code               7244050
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50H40F6 Ir N10 P'
_chemical_oxdiff_usercomment     Irdqxp31
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.691
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C9(H9), C12(H12), C15(H15), C20(H20), C23(H23),
 C34(H34), C35(H35), C36(H36), C39(H39), C42(H42), C45(H45), C50(H50), C53(H53)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C)
;
_shelx_res_checksum              78001
_shelx_fab_checksum              65676
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id Irdqxp31
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.971
_oxdiff_exptl_absorpt_empirical_full_min 0.662