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_7045337
_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         'C118 H104 F18 Ir2 N6 O6, 2.25(C Cl2 D2)'
_chemical_formula_sum            'C120.25 H104 Cl4.5 D4.5 F18 Ir2 N6 O6'
_chemical_formula_weight         2624.08
_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
_audit_creation_date             2017-06-06
_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                82.3655(16)
_cell_angle_beta                 83.9971(17)
_cell_angle_gamma                89.7030(17)
_cell_formula_units_Z            2
_cell_length_a                   16.5810(8)
_cell_length_b                   17.1571(9)
_cell_length_c                   19.9803(10)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      2.25
_cell_volume                     5602.5(5)
_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 0.999
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            98934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.068
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.568
_exptl_absorpt_correction_T_max  0.9117
_exptl_absorpt_correction_T_min  0.7575
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0759 before and 0.0538 after correction. The Ratio of minimum to maximum transmission is 0.8309. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       prism
_exptl_crystal_F_000             2625
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.967
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1462
_refine_ls_number_reflns         25715
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+17.4410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19552
_reflns_number_total             25715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04201a2.cif
_cod_data_source_block           13_17srv087
_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               7045337
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.672
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl8-C4S \\sim Cl7-C4S
 with sigma of 0.02
3. Others
 Fixed Sof: Cl3(0.6) Cl4(0.6) C2S(0.6) D2SA(0.6) D2SB(0.6) Cl5(0.4) Cl6(0.4)
 C3S(0.4) D3SA(0.4) D3SB(0.4) Cl7(0.25) Cl8(0.25) C4S(0.25) D4SA(0.25)
 D4SB(0.25)
4.a Ternary CH refined with riding coordinates:
 C68(H68), C83(H83), C98(H98), C113(H113)
4.b Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,
 H72B), C73(H73A,H73B), C82(H82A,H82B), C84(H84A,H84B), C85(H85A,H85B),
 C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C97(H97A,H97B), C99(H99A,H99B),
  C100(H10A,H10B), C101(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H), C112(H11G,
 H11H), C114(H11I,H11J), C115(H11K,H11L), C116(H11M,H11N), C117(H11O,H11P),
 C118(H11Q,H11R), C1S(D1SA,D1SB), C2S(D2SA,D2SB), C3S(D3SA,D3SB), C4S(D4SA,D4SB)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C12(H12), C13(H13), C15(H15), C17(H17), C21(H21),
 C23(H23), C24(H24), C26(H26), C28(H28), C32(H32), C34(H34), C35(H35), C37(H37),
  C39(H39), C43(H43), C45(H45), C46(H46), C61(H61), C63(H63), C76(H76),
 C78(H78), C91(H91), C93(H93), C106(H106), C108(H108)
4.d Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C110(H11A,H11B,H11C),
 C111(H11D,H11E,H11F)
;
_shelx_res_checksum              52257
_olex2_submission_special_instructions 'No special instructions were received'