Sky-blue emitting bridged diiridium complexes: beneficial effects of intramolecular π‒π stacking
Congrave, Daniel G.; Hsu, Yu-Ting; Batsanov, Andrei S.; Beeby, Andrew; Bryce, Martin R.; Dalton Transactions  (2018) –; doi:10.1039/C7DT04201A

data_7045338
_publ_section_title
;
 Sky-blue emitting bridged diiridium complexes: beneficial effects of
 intramolecular \p--\p stacking
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT04201A
_journal_year                    2018
_chemical_formula_moiety         'C84 H72 F6 Ir2 N6 O2, 5(C H2 Cl2)'
_chemical_formula_sum            'C89 H82 Cl10 F6 Ir2 N6 O2'
_chemical_formula_weight         2120.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-12-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_audit_update_record
;
2017-09-22 deposited with the CCDC.
2017-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                66.269(3)
_cell_angle_beta                 77.005(3)
_cell_angle_gamma                64.469(3)
_cell_formula_units_Z            2
_cell_length_a                   16.3594(14)
_cell_length_b                   17.7516(14)
_cell_length_c                   18.4512(15)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.63
_cell_measurement_theta_min      2.55
_cell_volume                     4417.7(6)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (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  0.0382
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            115844
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        32.500
_diffrn_reflns_theta_max         33.142
_diffrn_reflns_theta_min         2.106
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.375
_exptl_absorpt_correction_T_max  0.3856
_exptl_absorpt_correction_T_min  0.2093
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1107 before and 0.0548 after correction. The Ratio of minimum to maximum transmission is 0.5428. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.214
_refine_diff_density_max         4.886
_refine_diff_density_min         -1.519
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         33660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+10.4500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25210
_reflns_number_total             33660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04201a2.cif
_cod_data_source_block           12_16srv475
_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 
;
_cod_database_code               7045338
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.532
_shelx_estimated_absorpt_t_min   0.360
_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(H31A)=Uiso(H31B)=Uiso(H31C)=FVAR(1)
 Uiso(H32A)=Uiso(H32B)=Uiso(H32C)=FVAR(2)
 Uiso(H33A)=Uiso(H33B)=Uiso(H33C)=FVAR(3)
 Uiso(H40A)=Uiso(H40B)=Uiso(H40C)=FVAR(4)
 Uiso(H41A)=Uiso(H41B)=Uiso(H41C)=FVAR(5)
 Uiso(H42A)=Uiso(H42B)=Uiso(H42C)=FVAR(6)
 Uiso(H40D)=Uiso(H40E)=Uiso(H40F)=FVAR(7)
 Uiso(H41D)=Uiso(H41E)=Uiso(H41F)=FVAR(8)
 Uiso(H31D)=Uiso(H31E)=Uiso(H31F)=Uiso(H42D)=Uiso(H42E)=Uiso(H42F)=FVAR(9)
 Uiso(H32D)=Uiso(H32E)=Uiso(H32F)=FVAR(10)
 Uiso(H33D)=Uiso(H33E)=Uiso(H33F)=FVAR(11)
 Fixed Sof: Cl5A(0.5) Cl6A(0.5) Cl5B(0.5) Cl6B(0.5) H3SA(0.5) H3SB(0.5)
 H3SC(0.5) H3SD(0.5) Cl1B(0.5) Cl2B(0.5) Cl1A(0.5) Cl2A(0.5) H1SC(0.5)
 H1SD(0.5) H1SA(0.5) H1SB(0.5) Cl3A(0.85) Cl4A(0.85) C2SA(0.85) H2SA(0.85)
 H2SB(0.85) Cl7A(0.75) Cl8A(0.75) C4SA(0.75) H4SA(0.75) H4SB(0.75) Cl3B(0.15)
 Cl4B(0.15) C2SB(0.15) H2SC(0.15) H2SD(0.15) Cl7B(0.25) Cl8B(0.25) C4SB(0.25)
 H4SC(0.25) H4SD(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C3S(H3SC,H3SD), C1S(H1SC,H1SD), C1S(H1SA,H1SB), C2SA(H2SA,
 H2SB), C4SA(H4SA,H4SB), C2SB(H2SC,H2SD), C5S(H5SA,H5SB), C4SB(H4SC,H4SD)
3.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C9A(H9A), C11A(H11A), C12A(H12A),
 C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C20A(H20A), C22A(H22A),
 C23A(H23A), C27A(H27A), C29A(H29A), C36A(H36A), C38A(H38A), C3B(H3B), C4B(H4B),
  C5B(H5B), C6B(H6B), C9B(H9B), C11B(H11B), C12B(H12B), C14B(H14B), C15B(H15B),
 C16B(H16B), C17B(H17B), C20B(H20B), C22B(H22B), C23B(H23B), C27B(H27B),
 C29B(H29B), C36B(H36B), C38B(H38B)
3.c Idealised Me refined as rotating group:
 C31A(H31A,H31B,H31C), C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C40A(H40A,
 H40B,H40C), C41A(H41A,H41B,H41C), C42A(H42A,H42B,H42C), C31B(H31D,H31E,H31F),
 C32B(H32D,H32E,H32F), C33B(H33D,H33E,H33F), C40B(H40D,H40E,H40F), C41B(H41D,
 H41E,H41F), C42B(H42D,H42E,H42F)
;
_shelx_res_checksum              51079
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'