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_7045340
_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           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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-06-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-09-22 deposited with the CCDC.
2017-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.6047(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.6611(12)
_cell_length_b                   13.3724(6)
_cell_length_c                   15.0140(7)
_cell_measurement_reflns_used    9650
_cell_measurement_temperature    120
_cell_measurement_theta_max      35.24
_cell_measurement_theta_min      2.24
_cell_volume                     4935.3(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2016)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2016)'
_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 0.935
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66493
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        32.500
_diffrn_reflns_theta_max         35.637
_diffrn_reflns_theta_min         2.245
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.477
_exptl_absorpt_correction_T_max  0.6709
_exptl_absorpt_correction_T_min  0.4400
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0702 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.6558. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.136
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.000061(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         10647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+10.4440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9317
_reflns_number_total             10647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04201a2.cif
_cod_data_source_block           alpha-10_17srv056
_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               7045340
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.523
_shelx_estimated_absorpt_t_min   0.379
_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(C30A) = Uanis(C30B)
3. Others
 Fixed Sof: C30A(0.43) H30A(0.43) H30B(0.43) H30C(0.43) C30B(0.57) H30D(0.57)
 H30E(0.57) H30F(0.57)
4.a Riding coordinates:
 C30A(H30A,H30B,H30C), C30B(H30D,H30E,H30F)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23)
;
_shelx_res_checksum              78937
_olex2_submission_special_instructions 'No special instructions were received'