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_7045341
_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         'C60 H38 F8 Ir2 N6 O4'
_chemical_formula_sum            'C60 H38 F8 Ir2 N6 O4'
_chemical_formula_weight         1443.36
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-09-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-22 deposited with the CCDC.
2017-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1365(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7982(5)
_cell_length_b                   23.4916(10)
_cell_length_c                   19.1919(8)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.24
_cell_measurement_theta_min      2.33
_cell_volume                     5219.0(4)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2016/6 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  0.0660
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            108935
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.163
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.179
_exptl_absorpt_correction_T_max  0.6963
_exptl_absorpt_correction_T_min  0.6318
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1033 before and 0.0617 after correction. The Ratio of minimum to maximum transmission is 0.9074. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       prism
_exptl_crystal_F_000             2792
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.093
_refine_diff_density_max         1.452
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         15211
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+8.4630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11519
_reflns_number_total             15211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04201a2.cif
_cod_data_source_block           beta-10_17srv057
_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               7045341
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.582
_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. Uiso/Uaniso restraints and constraints
Uanis(O4A) = Uanis(O4B)
3. Rigid body (RIGU) restrains
 C57, O4B, C60B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C57, O4A, C60A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O4B)=Sof(C60B)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(1)
 Sof(O4A)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
5.a Riding coordinates:
 C60A(H60A,H60B,H60C), C60B(H60D,H60E,H60F)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44), C45(H45),
  C46(H46)
5.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C)
;
_shelx_res_checksum              80416
_olex2_submission_special_instructions 'No special instructions were received'