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_7048014
_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 H60 F18 Ir2 N10 O2, 2(C H4 O)'
_chemical_formula_sum            'C88 H68 F18 Ir2 N10 O4'
_chemical_formula_weight         2055.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0605(10)
_cell_length_b                   13.1557(6)
_cell_length_c                   30.6755(15)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.82
_cell_measurement_theta_min      2.43
_cell_volume                     8095.6(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 2014/7 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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            175372
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        32.000
_diffrn_reflns_theta_max         32.575
_diffrn_reflns_theta_min         2.278
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.385
_exptl_absorpt_correction_T_max  0.5354
_exptl_absorpt_correction_T_min  0.3021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS-2014/5 (Krause et al., 2015) was used for absorption correction. 
 wR2(int) was 0.1215 before and 0.0583 after correction. The Ratio of 
 minimum to maximum transmission is 0.5643. The \l/2 correction factor 
 is Not present.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       tablet
_exptl_crystal_F_000             4056
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/methanol'
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.116
_refine_diff_density_max         3.658
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         14709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+16.6500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11317
_reflns_number_total             14709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04043e2.cif
_cod_data_source_block           meso8-16s473
_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               7048014
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.695
_shelx_estimated_absorpt_t_min   0.317
_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, All O(H) groups
2. Restrained distances
 O2C-C44C
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2A) = Uanis(O2B)
Uanis(C44B) = Uanis(C44A)
4. Others
 Uiso(H41A)=Uiso(H41B)=Uiso(H41C)=FVAR(1)
 Uiso(H32A)=Uiso(H32B)=Uiso(H32C)=FVAR(2)
 Uiso(H34A)=Uiso(H34B)=Uiso(H34C)=FVAR(3)
 Uiso(H42A)=Uiso(H42B)=Uiso(H42C)=FVAR(4)
 Uiso(H43A)=Uiso(H43B)=Uiso(H43C)=FVAR(5)
 Uiso(H33A)=Uiso(H33B)=Uiso(H33C)=FVAR(6)
 Fixed Sof: O2A(0.45) H2A(0.45) C44A(0.45) H44A(0.45) H44B(0.45) H44C(0.45)
 O2B(0.45) H2B(0.45) C44B(0.45) H44D(0.45) H44E(0.45) H44F(0.45) O2C(0.1)
 H2C(0.1) C44C(0.1) H44G(0.1) H44H(0.1) H44I(0.1)
5.a Riding coordinates:
 O2A(H2A), C44A(H44A,H44B,H44C), O2B(H2B), C44B(H44D,H44E,H44F), O2C(H2C),
 C44C(H44G,H44H,H44I)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C12(H12), C14(H14), C18(H18), C19(H19),
 C28(H28), C30(H30), C37(H37), C39(H39)
5.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              58747
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'