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_7045339
_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         'C94 H72 F10 Ir2 N6 O2, 2(C H2 Cl2)'
_chemical_formula_sum            'C96 H76 Cl4 F10 Ir2 N6 O2'
_chemical_formula_weight         2061.82
_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   mixed
_atom_sites_solution_primary     heavy
_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
;
2017-09-22 deposited with the CCDC.
2017-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                101.8809(19)
_cell_angle_beta                 93.1589(19)
_cell_angle_gamma                109.7449(19)
_cell_formula_units_Z            2
_cell_length_a                   12.8310(8)
_cell_length_b                   13.3678(8)
_cell_length_c                   27.8367(16)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.83
_cell_measurement_theta_min      2.33
_cell_volume                     4357.2(5)
_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 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  0.0432
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            84964
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.999
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.114
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.248
_exptl_absorpt_correction_T_max  0.8595
_exptl_absorpt_correction_T_min  0.5267
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
 wR2(int) was 0.1284 before and 0.0562 after correction. The Ratio of 
 minimum to maximum transmission is 0.6128. The \l/2 correction factor 
 is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       needle
_exptl_crystal_F_000             2044
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.059
_refine_diff_density_max         3.223
_refine_diff_density_min         -7.359
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         25354
_refine_ls_number_restraints     1090
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+44.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19773
_reflns_number_total             25354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04201a2.cif
_cod_data_source_block           11_16srv477
_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               7045339
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.447
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl3-C96 \\sim Cl4-C96 \\sim Cl5-C96 \\sim Cl6-C97 \\sim Cl7-C97
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Uiso(H65A)=Uiso(H65B)=Uiso(H65C)=FVAR(1)
 Uiso(H66A)=Uiso(H66B)=Uiso(H66C)=FVAR(2)
 Uiso(H67A)=Uiso(H67B)=Uiso(H67C)=FVAR(3)
 Uiso(H74A)=Uiso(H74B)=Uiso(H74C)=FVAR(4)
 Uiso(H75A)=Uiso(H75B)=Uiso(H75C)=FVAR(5)
 Uiso(H76A)=Uiso(H76B)=Uiso(H76C)=FVAR(6)
 Uiso(H83A)=Uiso(H83B)=Uiso(H83C)=FVAR(7)
 Uiso(H84A)=Uiso(H84B)=Uiso(H84C)=FVAR(8)
 Uiso(H85A)=Uiso(H85B)=Uiso(H85C)=FVAR(9)
 Uiso(H92A)=Uiso(H92B)=Uiso(H92C)=FVAR(10)
 Uiso(H93A)=Uiso(H93B)=Uiso(H93C)=FVAR(11)
 Uiso(H94A)=Uiso(H94B)=Uiso(H94C)=FVAR(12)
 Fixed Sof: Cl6(0.5) Cl7(0.5) Cl3(0.4) Cl4(0.27) Cl5(0.13) Cl8(0.1) Cl9(0.1)
 C97(0.5) H97A(0.5) H97B(0.5) C96(0.4) H96A(0.4) H96B(0.4)
5.a Riding coordinates:
 C97(H97A,H97B), C96(H96A,H96B)
5.b Secondary CH2 refined with riding coordinates:
 C95(H95A,H95B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38),
 C39(H39), C40(H40), C43(H43), C45(H45), C46(H46), C61(H61), C63(H63), C70(H70),
  C72(H72), C79(H79), C81(H81), C88(H88), C90(H90)
5.d Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C74(H74A,H74B,
 H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C83(H83A,H83B,H83C), C84(H84A,
 H84B,H84C), C85(H85A,H85B,H85C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C),
 C94(H94A,H94B,H94C)
;
_shelx_res_checksum              3259
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'