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_7244049
_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         'C42 H24 Ir N10, F6 P, C2 H3 N, 1[C4H10O]'
_chemical_formula_sum            'C48 H37 F6 Ir N11 O P'
_chemical_formula_weight         1121.05
_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     dual
_audit_creation_date             2018-11-28
_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                 97.8170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.61910(10)
_cell_length_b                   17.9773(2)
_cell_length_c                   15.73360(10)
_cell_measurement_reflns_used    62142
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.4770
_cell_measurement_theta_min      1.7240
_cell_volume                     4376.77(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -108.00  16.00   0.50    2.00    --  -19.10 -57.00-150.00  248
  2  \w   -108.00  16.00   0.50    2.00    --  -19.10 -57.00  60.00  248
  3  \w   -108.00  19.00   0.50    2.00    --  -19.10 -70.00-150.00  254
  4  \w    -54.00  70.00   0.50    2.00    --  -19.10  57.00 -30.00  248
  5  \w    -57.00  70.00   0.50    2.00    --  -19.10  70.00   0.00  254
  6  \w   -108.00  19.00   0.50    2.00    --  -19.10 -70.00  30.00  254
  7  \w   -108.00  19.00   0.50    2.00    --  -19.10 -70.00 150.00  254
  8  \w    -54.00  70.00   0.50    2.00    --  -19.10  57.00 150.00  248
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0304520000
_diffrn_orient_matrix_UB_12      -0.0121484000
_diffrn_orient_matrix_UB_13      0.0266267000
_diffrn_orient_matrix_UB_21      0.0200777000
_diffrn_orient_matrix_UB_22      -0.0354281000
_diffrn_orient_matrix_UB_23      0.0037377000
_diffrn_orient_matrix_UB_31      0.0277822000
_diffrn_orient_matrix_UB_32      0.0124087000
_diffrn_orient_matrix_UB_33      0.0366964000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            85017
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.701
_diffrn_reflns_theta_min         1.724
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    3.166
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.385
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.701
_exptl_crystal_description       prism
_exptl_crystal_F_000             2224
_exptl_crystal_recrystallization_method
'The material was recrystallised from ether by'
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.024
_refine_diff_density_max         3.846
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         11289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+6.2981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9970
_reflns_number_total             11289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra07213g2.cif
_cod_data_source_block           Irdqxp1
_cod_database_code               7244049
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H24 F6 Ir N10 P C4H10O C2H3N'
_chemical_oxdiff_usercomment     Irdqxp3
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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:
 C10(H10), C34(H34), C12(H12), C11(H11), C37(H37), C2(H2), C7(H7), C40(H40),
 C3(H3), C32(H32), C13(H13), C33(H33), C51(H51), C4(H4), C21(H21), C48(H48),
 C41(H41), C19(H19), C50(H50), C43(H43), C49(H49), C18(H18), C20(H20), C42(H42)
2.b Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C)
;
_shelx_res_checksum              99924
_shelx_fab_checksum              25812
_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 Irdqxp3
_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 2.485
_oxdiff_exptl_absorpt_empirical_full_min 0.624