Highly luminescent 2-phenylpyridine-free diiridium complexes with bulky 1,2-diarylimidazole cyclometalating ligands.
Congrave, Daniel G.; Batsanov, Andrei S.; Bryce, Martin R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16524–16533; doi:10.1039/c8dt04043e

data_7048013
_publ_section_title
;
 Highly luminescent 2-phenylpyridine-free diiridium complexes with bulky
 1,2-diarylimidazole cyclometalating ligands.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16524
_journal_page_last               16533
_journal_paper_doi               10.1039/c8dt04043e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C86 H64 F14 Ir2 N10 O2, 6(C H2 Cl2)'
_chemical_formula_sum            'C92 H76 Cl12 F14 Ir2 N10 O2'
_chemical_formula_weight         2429.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-01-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2018-10-02 deposited with the CCDC.
2018-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.2650(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2045(10)
_cell_length_b                   14.8901(6)
_cell_length_c                   27.9788(12)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.46
_cell_volume                     9459.6(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 multi-CPU (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            101919
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.459
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.232
_exptl_absorpt_correction_T_max  0.9000
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; SADABS-2014/5 (Krause et al., 2015) was used for absorption correction. 
 wR2(int) was 0.1104 before and 0.0597 after correction. The Ratio of 
 minimum to maximum transmission is 0.7140. The \l/2 correction factor 
 is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       trapetsoid
_exptl_crystal_F_000             4792
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.055
_refine_diff_density_max         3.041
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         13754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+41.4830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11072
_reflns_number_total             13754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04043e2.cif
_cod_data_source_block           meso7-16s481
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048013--7048014.cif.
;
_cod_database_code               7048013
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.498
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Uiso(H32A)=Uiso(H32B)=Uiso(H32C)=FVAR(1)
 Uiso(H33A)=Uiso(H33B)=Uiso(H33C)=FVAR(2)
 Uiso(H34A)=Uiso(H34B)=Uiso(H34C)=FVAR(3)
 Uiso(H41A)=Uiso(H41B)=Uiso(H41C)=FVAR(4)
 Uiso(H42A)=Uiso(H42B)=Uiso(H42C)=FVAR(5)
 Uiso(H43A)=Uiso(H43B)=Uiso(H43C)=FVAR(6)
 Fixed Sof: Cl4A(0.75) Cl4B(0.25) H45A(0.75) H45B(0.75) H45D(0.25) H45C(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C45(H45D,H45C), C44(H44A,H44B), C46(H46A,H46B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C14(H14), C15(H15),
 C18(H18), C19(H19), C28(H28), C30(H30), C37(H37), C39(H39)
3.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              68420
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'