#------------------------------------------------------------------------------
#$Date: 2019-11-24 13:37:25 +0200 (Sun, 24 Nov 2019) $
#$Revision: 238030 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/91/4089194.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4089194
loop_
_publ_author_name
'Congrave, Daniel G.'
'Hsu, Yu-ting'
'Batsanov, Andrei S.'
'Beeby, Andrew'
'Bryce, Martin R.'
_publ_section_title
;
 Synthesis, Diastereomer Separation, and Optoelectronic and Structural
 Properties of Dinuclear Cyclometalated Iridium(III) Complexes with
 Bridging Diarylhydrazide Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              981
_journal_paper_doi               10.1021/acs.organomet.6b00887
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety
'C58 H46 F8 Ir2 N10 O2,2(C H2 Cl2),0.5(C6 H14)'
_chemical_formula_sum            'C63 H57 Cl4 F8 Ir2 N10 O2'
_chemical_formula_weight         1664.38
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.3803(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2699(6)
_cell_length_b                   28.0760(12)
_cell_length_c                   16.8768(7)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    120
_cell_measurement_theta_max      34.02
_cell_measurement_theta_min      2.45
_cell_volume                     6296.2(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
'SHELXL 2014/7 multi-CPU version (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_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  'D8 Venture'
_diffrn_measurement_method       'φ and ω 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  0.0502
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            101443
_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         2.110
_diffrn_source                   'I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.469
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.4085
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1069 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.4119.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.676
_refine_diff_density_min         -2.782
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         18347
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0379
_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/[σ²(Fo²)+(0.0110P)²+24.7450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14811
_reflns_number_total             18347
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00887_si_002.cif
_cod_data_source_block           14b-DCM-hexane
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4089194
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.289
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_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
 Cl2B-C59B \\sim Cl1B-C59B \\sim Cl1-C59A \\sim Cl2A-C59A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C59A) = Uiso(C59B)
Uiso(C60A) = Uiso(C60B)
4. Others
 Fixed Sof: Cl1B(0.15) Cl2B(0.15) C59B(0.15) H59C(0.15) H59D(0.15) Cl4A(0.55)
 C60A(0.55) H60A(0.55) H60B(0.55) Cl4B(0.45) C60B(0.45) H60C(0.45) H60D(0.45)
 Cl1(0.85) Cl2A(0.85) C59A(0.85) H59A(0.85) H59B(0.85)
5.a Secondary CH2 refined with riding coordinates:
 C59B(H59C,H59D), C60A(H60A,H60B), C60B(H60C,H60D), C59A(H59A,H59B), C62(H62A,
 H62B), C63(H63A,H63B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C15(H15), C17(H17), C18(H18), C19(H19),
 C20(H20), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33),
  C35(H35), C36(H36), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49),
 C53(H53), C55(H55), C56(H56), C57(H57), C58(H58)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C61(H61A,H61B,H61C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.71077(2) 0.22905(2) 0.37811(2) 0.01387(3) Uani 1 1 d . . . .
Ir2 Ir 0.37499(2) 0.16497(2) 0.36179(2) 0.01520(4) Uani 1 1 d . . . .
F1 F 1.01137(19) 0.11003(10) 0.49425(16) 0.0328(6) Uani 1 1 d . . . .
F2 F 0.95582(19) 0.16515(10) 0.21823(16) 0.0309(6) Uani 1 1 d . . . .
F3 F 0.8654(2) 0.37445(10) 0.27575(19) 0.0394(7) Uani 1 1 d . . . .
F4 F 1.0249(2) 0.33948(10) 0.56606(18) 0.0387(7) Uani 1 1 d . . . .
F5 F 0.2569(2) 0.26053(10) 0.57389(16) 0.0316(6) Uani 1 1 d . . . .
F6 F 0.02970(17) 0.26734(9) 0.29173(16) 0.0288(6) Uani 1 1 d . . . .
F7 F 0.1041(2) 0.05274(11) 0.15543(18) 0.0436(8) Uani 1 1 d . . . .
F8 F 0.1923(3) 0.01239(13) 0.4425(2) 0.0593(10) Uani 1 1 d . . . .
O1 O 0.61038(19) 0.27230(10) 0.41231(17) 0.0179(5) Uani 1 1 d . . . .
O2 O 0.4869(2) 0.11862(10) 0.35259(17) 0.0189(6) Uani 1 1 d . . . .
N1 N 0.5767(2) 0.18619(12) 0.3499(2) 0.0160(6) Uani 1 1 d . . . .
N2 N 0.4958(2) 0.21174(12) 0.36352(19) 0.0146(6) Uani 1 1 d . . . .
N3 N 0.7675(2) 0.19398(12) 0.4895(2) 0.0176(7) Uani 1 1 d . . . .
N4 N 0.8424(2) 0.16244(12) 0.4963(2) 0.0175(7) Uani 1 1 d . . . .
N5 N 0.6662(2) 0.26289(12) 0.2653(2) 0.0187(7) Uani 1 1 d . . . .
N6 N 0.7246(3) 0.29990(12) 0.2593(2) 0.0205(7) Uani 1 1 d . . . .
N7 N 0.4304(2) 0.16731(13) 0.4900(2) 0.0201(7) Uani 1 1 d . . . .
N8 N 0.3823(3) 0.19854(13) 0.5247(2) 0.0215(7) Uani 1 1 d . . . .
N9 N 0.3101(2) 0.16481(12) 0.2346(2) 0.0152(6) Uani 1 1 d . . . .
N10 N 0.2369(2) 0.13150(12) 0.2014(2) 0.0189(7) Uani 1 1 d . . . .
C1 C 0.5631(3) 0.14002(14) 0.3458(2) 0.0158(7) Uani 1 1 d . . . .
C2 C 0.6401(3) 0.10841(14) 0.3340(2) 0.0164(7) Uani 1 1 d . . . .
C3 C 0.6659(3) 0.11160(14) 0.2629(2) 0.0192(8) Uani 1 1 d . . . .
H3 H 0.6384 0.1363 0.2227 0.023 Uiso 1 1 calc R . . .
C4 C 0.7318(3) 0.07901(14) 0.2497(3) 0.0199(8) Uani 1 1 d . . . .
H4 H 0.7480 0.0815 0.2001 0.024 Uiso 1 1 calc R . . .
C5 C 0.7746(3) 0.04259(14) 0.3079(3) 0.0188(8) Uani 1 1 d . . . .
C6 C 0.7490(3) 0.04069(15) 0.3804(3) 0.0254(9) Uani 1 1 d . . . .
H6 H 0.7785 0.0169 0.4220 0.031 Uiso 1 1 calc R . . .
C7 C 0.6820(3) 0.07245(15) 0.3929(3) 0.0222(9) Uani 1 1 d . . . .
H7 H 0.6645 0.0698 0.4419 0.027 Uiso 1 1 calc R . . .
C8 C 0.8412(3) 0.00400(15) 0.2928(3) 0.0258(9) Uani 1 1 d . . . .
C9 C 0.8715(4) 0.01576(18) 0.2171(3) 0.0333(11) Uani 1 1 d . . . .
H9A H 0.8111 0.0177 0.1653 0.050 Uiso 1 1 calc GR . . .
H9B H 0.9159 -0.0093 0.2104 0.050 Uiso 1 1 calc GR . . .
H9C H 0.9069 0.0464 0.2269 0.050 Uiso 1 1 calc GR . . .
C10 C 0.9374(4) -0.00225(18) 0.3715(3) 0.0343(11) Uani 1 1 d . . . .
H10A H 0.9753 0.0277 0.3836 0.051 Uiso 1 1 calc GR . . .
H10B H 0.9788 -0.0275 0.3609 0.051 Uiso 1 1 calc GR . . .
H10C H 0.9195 -0.0110 0.4204 0.051 Uiso 1 1 calc GR . . .
C11 C 0.7812(4) -0.04266(17) 0.2743(4) 0.0441(14) Uani 1 1 d . . . .
H11A H 0.7636 -0.0512 0.3235 0.066 Uiso 1 1 calc GR . . .
H11B H 0.8221 -0.0681 0.2636 0.066 Uiso 1 1 calc GR . . .
H11C H 0.7196 -0.0385 0.2242 0.066 Uiso 1 1 calc GR . . .
C12 C 0.8166(3) 0.18972(14) 0.3561(2) 0.0164(8) Uani 1 1 d . . . .
C13 C 0.8742(3) 0.16147(14) 0.4259(2) 0.0175(8) Uani 1 1 d . . . .
C14 C 0.9568(3) 0.13615(15) 0.4246(3) 0.0226(9) Uani 1 1 d . . . .
C15 C 0.9865(3) 0.13685(16) 0.3559(3) 0.0248(9) Uani 1 1 d . . . .
H15 H 1.0436 0.1196 0.3553 0.030 Uiso 1 1 calc R . . .
C16 C 0.9283(3) 0.16415(15) 0.2877(3) 0.0208(8) Uani 1 1 d . . . .
C17 C 0.8462(3) 0.19025(14) 0.2858(2) 0.0181(8) Uani 1 1 d . . . .
H17 H 0.8097 0.2086 0.2369 0.022 Uiso 1 1 calc R . . .
C18 C 0.8672(3) 0.13758(16) 0.5698(3) 0.0270(9) Uani 1 1 d . . . .
H18 H 0.9170 0.1134 0.5889 0.032 Uiso 1 1 calc R . . .
C19 C 0.8070(3) 0.15376(17) 0.6116(3) 0.0296(10) Uani 1 1 d . . . .
H19 H 0.8069 0.1432 0.6651 0.036 Uiso 1 1 calc R . . .
C20 C 0.7458(3) 0.18891(16) 0.5595(2) 0.0233(9) Uani 1 1 d . . . .
H20 H 0.6961 0.2066 0.5720 0.028 Uiso 1 1 calc R . . .
C21 C 0.8148(3) 0.28059(14) 0.4050(3) 0.0176(8) Uani 1 1 d . . . .
C22 C 0.8058(3) 0.31076(14) 0.3356(3) 0.0192(8) Uani 1 1 d . . . .
C23 C 0.8715(3) 0.34808(15) 0.3445(3) 0.0276(10) Uani 1 1 d . . . .
C24 C 0.9463(3) 0.35866(16) 0.4219(3) 0.0301(10) Uani 1 1 d . . . .
H24 H 0.9912 0.3846 0.4280 0.036 Uiso 1 1 calc R . . .
C25 C 0.9524(3) 0.32975(16) 0.4893(3) 0.0270(10) Uani 1 1 d . . . .
C26 C 0.8911(3) 0.29078(15) 0.4824(3) 0.0203(8) Uani 1 1 d . . . .
H26 H 0.9010 0.2709 0.5304 0.024 Uiso 1 1 calc R . . .
C27 C 0.6872(3) 0.31875(16) 0.1798(3) 0.0267(10) Uani 1 1 d . . . .
H27 H 0.7141 0.3451 0.1597 0.032 Uiso 1 1 calc R . . .
C28 C 0.6042(4) 0.29297(17) 0.1341(3) 0.0308(10) Uani 1 1 d . . . .
H28 H 0.5623 0.2977 0.0763 0.037 Uiso 1 1 calc R . . .
C29 C 0.5928(3) 0.25829(16) 0.1889(3) 0.0220(9) Uani 1 1 d . . . .
H29 H 0.5410 0.2350 0.1743 0.026 Uiso 1 1 calc R . . .
C30 C 0.5214(3) 0.25453(14) 0.3934(2) 0.0155(7) Uani 1 1 d . . . .
C31 C 0.4482(3) 0.28710(14) 0.4088(2) 0.0164(8) Uani 1 1 d . . . .
C32 C 0.4707(3) 0.30709(15) 0.4889(3) 0.0194(8) Uani 1 1 d . . . .
H32 H 0.5285 0.2966 0.5348 0.023 Uiso 1 1 calc R . . .
C33 C 0.4103(3) 0.34193(15) 0.5028(3) 0.0213(8) Uani 1 1 d . . . .
H33 H 0.4266 0.3545 0.5585 0.026 Uiso 1 1 calc R . . .
C34 C 0.3257(3) 0.35913(14) 0.4368(3) 0.0191(8) Uani 1 1 d . . . .
C35 C 0.3026(3) 0.33817(15) 0.3568(3) 0.0203(8) Uani 1 1 d . . . .
H35 H 0.2448 0.3485 0.3107 0.024 Uiso 1 1 calc R . . .
C36 C 0.3636(3) 0.30206(14) 0.3435(2) 0.0180(8) Uani 1 1 d . . . .
H36 H 0.3461 0.2879 0.2888 0.022 Uiso 1 1 calc R . . .
C37 C 0.2638(3) 0.39999(15) 0.4531(3) 0.0259(9) Uani 1 1 d . . . .
C38 C 0.2327(4) 0.38734(18) 0.5283(3) 0.0311(10) Uani 1 1 d . . . .
H38A H 0.1941 0.3576 0.5161 0.047 Uiso 1 1 calc GR . . .
H38B H 0.1912 0.4130 0.5374 0.047 Uiso 1 1 calc GR . . .
H38C H 0.2931 0.3833 0.5796 0.047 Uiso 1 1 calc GR . . .
C39 C 0.1691(4) 0.41000(19) 0.3753(3) 0.0377(12) Uani 1 1 d . . . .
H39A H 0.1284 0.3810 0.3594 0.056 Uiso 1 1 calc GR . . .
H39B H 0.1883 0.4203 0.3278 0.056 Uiso 1 1 calc GR . . .
H39C H 0.1299 0.4352 0.3890 0.056 Uiso 1 1 calc GR . . .
C40 C 0.3292(4) 0.44531(18) 0.4744(4) 0.0440(14) Uani 1 1 d . . . .
H40A H 0.2909 0.4716 0.4860 0.066 Uiso 1 1 calc GR . . .
H40B H 0.3485 0.4537 0.4261 0.066 Uiso 1 1 calc GR . . .
H40C H 0.3898 0.4395 0.5247 0.066 Uiso 1 1 calc GR . . .
C41 C 0.2711(3) 0.20685(14) 0.3808(2) 0.0170(8) Uani 1 1 d . . . .
C42 C 0.2933(3) 0.21871(14) 0.4662(2) 0.0188(8) Uani 1 1 d . . . .
C43 C 0.2301(3) 0.24738(15) 0.4911(3) 0.0218(8) Uani 1 1 d . . . .
C44 C 0.1404(3) 0.26376(15) 0.4335(3) 0.0239(9) Uani 1 1 d . . . .
H44 H 0.0960 0.2829 0.4505 0.029 Uiso 1 1 calc R . . .
C45 C 0.1182(3) 0.25104(15) 0.3501(3) 0.0206(8) Uani 1 1 d . . . .
C46 C 0.1796(3) 0.22356(15) 0.3217(2) 0.0184(8) Uani 1 1 d . . . .
H46 H 0.1603 0.2160 0.2630 0.022 Uiso 1 1 calc R . . .
C47 C 0.4306(3) 0.20037(19) 0.6099(3) 0.0322(11) Uani 1 1 d . . . .
H47 H 0.4125 0.2194 0.6485 0.039 Uiso 1 1 calc R . . .
C48 C 0.5108(4) 0.1697(2) 0.6304(3) 0.0410(13) Uani 1 1 d . . . .
H48 H 0.5585 0.1632 0.6856 0.049 Uiso 1 1 calc R . . .
C49 C 0.5080(3) 0.14980(18) 0.5536(3) 0.0306(10) Uani 1 1 d . . . .
H49 H 0.5546 0.1272 0.5479 0.037 Uiso 1 1 calc R . . .
C50 C 0.2784(3) 0.11069(15) 0.3468(3) 0.0198(8) Uani 1 1 d . . . .
C51 C 0.2207(3) 0.10037(15) 0.2618(3) 0.0200(8) Uani 1 1 d . . . .
C52 C 0.1577(3) 0.06185(17) 0.2390(3) 0.0298(10) Uani 1 1 d . . . .
C53 C 0.1468(4) 0.03170(19) 0.2998(3) 0.0401(13) Uani 1 1 d . . . .
H53 H 0.1034 0.0048 0.2846 0.048 Uiso 1 1 calc R . . .
C54 C 0.2014(4) 0.04248(19) 0.3826(3) 0.0373(12) Uani 1 1 d . . . .
C55 C 0.2656(3) 0.08043(17) 0.4081(3) 0.0278(10) Uani 1 1 d . . . .
H55 H 0.3013 0.0862 0.4669 0.033 Uiso 1 1 calc R . . .
C56 C 0.1927(3) 0.13760(16) 0.1162(3) 0.0250(9) Uani 1 1 d . . . .
H56 H 0.1394 0.1190 0.0785 0.030 Uiso 1 1 calc R . . .
C57 C 0.2386(3) 0.17529(16) 0.0941(3) 0.0254(9) Uani 1 1 d . . . .
H57 H 0.2238 0.1881 0.0387 0.030 Uiso 1 1 calc R . . .
C58 C 0.3120(3) 0.19105(15) 0.1699(2) 0.0191(8) Uani 1 1 d . . . .
H58 H 0.3568 0.2168 0.1744 0.023 Uiso 1 1 calc R . . .
Cl1B Cl 0.4709(12) 0.4090(6) 0.2848(9) 0.107(7) Uani 0.15 1 d D P A 2
Cl2B Cl 0.6784(9) 0.4112(5) 0.4179(7) 0.068(3) Uani 0.15 1 d D P A 2
C59B C 0.5621(15) 0.3827(10) 0.3737(17) 0.0386(14) Uiso 0.15 1 d D P A 2
H59C H 0.5333 0.3797 0.4187 0.046 Uiso 0.15 1 calc R P A 2
H59D H 0.5743 0.3500 0.3576 0.046 Uiso 0.15 1 calc R P A 2
Cl3 Cl 0.52112(17) -0.03635(8) 0.31448(15) 0.0891(6) Uani 1 1 d . . . .
Cl4A Cl 0.3440(4) -0.04568(17) 0.3547(3) 0.1131(17) Uani 0.55 1 d . P B 1
C60A C 0.4144(12) -0.0049(6) 0.3227(11) 0.081(3) Uiso 0.55 1 d . P B 1
H60A H 0.4376 0.0212 0.3649 0.097 Uiso 0.55 1 calc R P B 1
H60B H 0.3731 0.0090 0.2670 0.097 Uiso 0.55 1 calc R P B 1
Cl4B Cl 0.4572(6) -0.0148(2) 0.4535(3) 0.129(3) Uani 0.45 1 d . P B -2
C60B C 0.4600(15) 0.0001(8) 0.3556(13) 0.081(3) Uiso 0.45 1 d . P B -2
H60C H 0.3897 0.0027 0.3150 0.097 Uiso 0.45 1 calc R P B -2
H60D H 0.4907 0.0321 0.3603 0.097 Uiso 0.45 1 calc R P B -2
Cl1 Cl 0.53141(12) 0.37549(6) 0.27558(9) 0.0374(3) Uani 0.85 1 d D P C 1
Cl2A Cl 0.56088(16) 0.43206(6) 0.42752(11) 0.0540(5) Uani 0.85 1 d D P C 1
C59A C 0.6105(5) 0.3871(2) 0.3815(4) 0.0386(14) Uiso 0.85 1 d D P C 1
H59A H 0.6191 0.3576 0.4154 0.046 Uiso 0.85 1 calc R P C 1
H59B H 0.6776 0.3970 0.3827 0.046 Uiso 0.85 1 calc R P C 1
C61 C 0.3941(6) 0.0600(2) 0.1117(5) 0.077(2) Uani 1 1 d . . . .
H61A H 0.3619 0.0834 0.0670 0.116 Uiso 1 1 calc GR . . .
H61B H 0.4189 0.0760 0.1672 0.116 Uiso 1 1 calc GR . . .
H61C H 0.3451 0.0355 0.1115 0.116 Uiso 1 1 calc GR . . .
C62 C 0.4875(5) 0.0354(3) 0.0944(4) 0.069(2) Uani 1 1 d . . . .
H62A H 0.5388 0.0600 0.0990 0.082 Uiso 1 1 calc R . . .
H62B H 0.5186 0.0114 0.1394 0.082 Uiso 1 1 calc R . . .
C63 C 0.4594(5) 0.0118(2) 0.0102(4) 0.0555(17) Uani 1 1 d . . . .
H63A H 0.4071 -0.0123 0.0059 0.067 Uiso 1 1 calc R . . .
H63B H 0.4281 0.0361 -0.0342 0.067 Uiso 1 1 calc R . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2.00 -1.00 -2.00 0.0580
-2.00 1.00 2.00 0.1040
0.00 -1.00 0.00 0.0260
0.00 1.00 0.00 0.0030
0.00 -1.00 2.00 0.0570
-1.00 0.00 -2.00 0.1790
0.00 -1.00 -1.00 0.1450
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
O1 Ir1 N1 75.30(11) .
N3 Ir1 O1 96.19(12) .
N3 Ir1 N1 87.44(13) .
N3 Ir1 N5 174.68(13) .
N3 Ir1 C12 80.25(14) .
N5 Ir1 O1 88.58(12) .
N5 Ir1 N1 96.07(13) .
N5 Ir1 C12 94.82(14) .
C12 Ir1 O1 174.53(13) .
C12 Ir1 N1 108.52(14) .
C21 Ir1 O1 92.47(13) .
C21 Ir1 N1 167.30(14) .
C21 Ir1 N3 97.45(15) .
C21 Ir1 N5 79.96(15) .
C21 Ir1 C12 83.92(15) .
O2 Ir2 N2 75.75(11) .
N7 Ir2 O2 95.05(12) .
N7 Ir2 N2 88.11(13) .
N9 Ir2 O2 89.21(12) .
N9 Ir2 N2 94.05(12) .
N9 Ir2 N7 175.59(13) .
N9 Ir2 C41 95.31(14) .
N9 Ir2 C50 80.55(14) .
C41 Ir2 O2 175.03(13) .
C41 Ir2 N2 105.92(14) .
C41 Ir2 N7 80.40(14) .
C41 Ir2 C50 87.23(16) .
C50 Ir2 O2 91.48(14) .
C50 Ir2 N2 166.28(14) .
C50 Ir2 N7 98.18(15) .
C30 O1 Ir1 114.4(2) .
C1 O2 Ir2 114.0(2) .
N2 N1 Ir1 112.5(2) .
C1 N1 Ir1 131.7(3) .
C1 N1 N2 112.8(3) .
N1 N2 Ir2 112.1(2) .
C30 N2 Ir2 132.5(3) .
C30 N2 N1 113.0(3) .
N4 N3 Ir1 115.7(2) .
C20 N3 Ir1 137.4(3) .
C20 N3 N4 106.5(3) .
N3 N4 C13 115.0(3) .
C18 N4 N3 110.4(3) .
C18 N4 C13 134.5(4) .
N6 N5 Ir1 116.2(2) .
C29 N5 Ir1 137.1(3) .
C29 N5 N6 106.7(3) .
N5 N6 C22 114.7(3) .
N5 N6 C27 109.9(3) .
C27 N6 C22 135.3(4) .
N8 N7 Ir2 114.7(2) .
C49 N7 Ir2 138.0(3) .
C49 N7 N8 107.0(3) .
N7 N8 C42 114.9(3) .
C47 N8 N7 109.8(3) .
C47 N8 C42 135.2(4) .
N10 N9 Ir2 115.3(2) .
C58 N9 Ir2 137.8(3) .
C58 N9 N10 106.6(3) .
N9 N10 C51 115.3(3) .
C56 N10 N9 109.9(3) .
C56 N10 C51 134.7(4) .
O2 C1 N1 125.0(4) .
O2 C1 C2 115.2(3) .
N1 C1 C2 119.8(3) .
C3 C2 C1 121.6(4) .
C3 C2 C7 119.2(4) .
C7 C2 C1 119.0(3) .
C2 C3 C4 120.5(4) .
C3 C4 C5 121.3(4) .
C4 C5 C6 117.2(4) .
C4 C5 C8 122.9(4) .
C6 C5 C8 119.9(4) .
C7 C6 C5 121.8(4) .
C6 C7 C2 120.1(4) .
C5 C8 C9 111.8(4) .
C5 C8 C10 110.6(4) .
C5 C8 C11 107.8(4) .
C9 C8 C10 108.2(4) .
C9 C8 C11 108.8(4) .
C10 C8 C11 109.6(4) .
C13 C12 Ir1 113.8(3) .
C17 C12 Ir1 129.1(3) .
C17 C12 C13 116.8(3) .
C12 C13 N4 115.0(3) .
C14 C13 N4 123.9(4) .
C14 C13 C12 121.1(4) .
F1 C14 C13 119.0(4) .
F1 C14 C15 118.8(4) .
C15 C14 C13 122.2(4) .
C14 C15 C16 115.8(4) .
F2 C16 C15 116.9(4) .
F2 C16 C17 118.6(4) .
C17 C16 C15 124.4(4) .
C16 C17 C12 119.6(4) .
N4 C18 C19 107.3(4) .
C18 C19 C20 105.9(4) .
N3 C20 C19 109.9(4) .
C22 C21 Ir1 114.2(3) .
C26 C21 Ir1 128.5(3) .
C26 C21 C22 117.3(4) .
C21 C22 N6 114.9(3) .
C23 C22 N6 124.2(4) .
C23 C22 C21 120.8(4) .
F3 C23 C22 119.6(4) .
F3 C23 C24 118.6(4) .
C22 C23 C24 121.8(4) .
C25 C24 C23 116.6(4) .
F4 C25 C24 117.8(4) .
F4 C25 C26 118.6(4) .
C24 C25 C26 123.5(4) .
C25 C26 C21 119.8(4) .
N6 C27 C28 107.4(4) .
C27 C28 C29 106.5(4) .
N5 C29 C28 109.4(4) .
O1 C30 N2 124.3(3) .
O1 C30 C31 114.3(3) .
N2 C30 C31 121.4(3) .
C32 C31 C30 119.5(3) .
C36 C31 C30 121.3(3) .
C36 C31 C32 118.8(4) .
C33 C32 C31 121.0(4) .
C32 C33 C34 121.4(4) .
C33 C34 C37 120.2(4) .
C35 C34 C33 117.1(4) .
C35 C34 C37 122.7(4) .
C34 C35 C36 121.1(4) .
C31 C36 C35 120.5(3) .
C34 C37 C40 108.7(4) .
C38 C37 C34 109.6(4) .
C38 C37 C40 109.4(4) .
C39 C37 C34 111.8(4) .
C39 C37 C38 108.8(4) .
C39 C37 C40 108.6(4) .
C42 C41 Ir2 113.6(3) .
C42 C41 C46 117.0(4) .
C46 C41 Ir2 129.3(3) .
C41 C42 N8 115.7(3) .
C43 C42 N8 122.7(4) .
C43 C42 C41 121.6(4) .
F5 C43 C42 120.0(4) .
F5 C43 C44 118.5(4) .
C44 C43 C42 121.5(4) .
C45 C44 C43 116.4(4) .
F6 C45 C44 117.3(4) .
F6 C45 C46 118.4(4) .
C44 C45 C46 124.3(4) .
C45 C46 C41 119.1(4) .
N8 C47 C48 107.5(4) .
C47 C48 C49 106.1(4) .
N7 C49 C48 109.7(4) .
C51 C50 Ir2 114.0(3) .
C55 C50 Ir2 129.5(3) .
C55 C50 C51 116.4(4) .
C50 C51 N10 114.8(3) .
C52 C51 N10 123.0(4) .
C52 C51 C50 122.2(4) .
F7 C52 C51 120.3(4) .
F7 C52 C53 118.7(4) .
C51 C52 C53 121.0(4) .
C54 C53 C52 116.6(5) .
F8 C54 C53 116.8(5) .
F8 C54 C55 119.0(5) .
C53 C54 C55 124.2(4) .
C54 C55 C50 119.5(4) .
N10 C56 C57 107.7(4) .
C56 C57 C58 105.6(4) .
N9 C58 C57 110.2(4) .
Cl2B C59B Cl1B 117.9(15) .
Cl4A C60A Cl3 107.6(9) .
Cl3 C60B Cl4B 116.9(13) .
Cl2A C59A Cl1 111.6(4) .
C63 C62 C61 114.2(6) .
C63 C63 C62 117.5(8) 3_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 O1 2.113(3) .
Ir1 N1 2.161(3) .
Ir1 N3 2.012(3) .
Ir1 N5 2.012(3) .
Ir1 C12 2.012(4) .
Ir1 C21 2.003(4) .
Ir2 O2 2.109(3) .
Ir2 N2 2.159(3) .
Ir2 N7 2.015(3) .
Ir2 N9 2.004(3) .
Ir2 C41 2.007(4) .
Ir2 C50 2.008(4) .
F1 C14 1.364(5) .
F2 C16 1.365(4) .
F3 C23 1.353(5) .
F4 C25 1.359(5) .
F5 C43 1.359(5) .
F6 C45 1.367(4) .
F7 C52 1.361(5) .
F8 C54 1.359(5) .
O1 C30 1.291(4) .
O2 C1 1.284(4) .
N1 N2 1.447(4) .
N1 C1 1.309(5) .
N2 C30 1.303(5) .
N3 N4 1.360(4) .
N3 C20 1.334(5) .
N4 C13 1.418(5) .
N4 C18 1.354(5) .
N5 N6 1.358(5) .
N5 C29 1.339(5) .
N6 C22 1.416(5) .
N6 C27 1.359(5) .
N7 N8 1.370(5) .
N7 C49 1.324(5) .
N8 C42 1.412(5) .
N8 C47 1.350(5) .
N9 N10 1.362(4) .
N9 C58 1.326(5) .
N10 C51 1.424(5) .
N10 C56 1.355(5) .
C1 C2 1.482(5) .
C2 C3 1.380(5) .
C2 C7 1.390(6) .
C3 C4 1.386(5) .
C4 C5 1.395(6) .
C5 C6 1.398(6) .
C5 C8 1.523(5) .
C6 C7 1.378(6) .
C8 C9 1.527(6) .
C8 C10 1.533(6) .
C8 C11 1.533(6) .
C12 C13 1.409(5) .
C12 C17 1.398(5) .
C13 C14 1.384(5) .
C14 C15 1.372(6) .
C15 C16 1.380(6) .
C16 C17 1.372(5) .
C18 C19 1.373(6) .
C19 C20 1.397(6) .
C21 C22 1.413(6) .
C21 C26 1.392(5) .
C22 C23 1.378(6) .
C23 C24 1.384(7) .
C24 C25 1.374(7) .
C25 C26 1.379(6) .
C27 C28 1.362(7) .
C28 C29 1.392(6) .
C30 C31 1.481(5) .
C31 C32 1.389(5) .
C31 C36 1.370(5) .
C32 C33 1.379(5) .
C33 C34 1.397(6) .
C34 C35 1.397(6) .
C34 C37 1.533(6) .
C35 C36 1.407(5) .
C37 C38 1.532(6) .
C37 C39 1.527(6) .
C37 C40 1.541(7) .
C41 C42 1.399(5) .
C41 C46 1.403(5) .
C42 C43 1.384(5) .
C43 C44 1.374(6) .
C44 C45 1.373(6) .
C45 C46 1.378(6) .
C47 C48 1.372(7) .
C48 C49 1.398(7) .
C50 C51 1.400(6) .
C50 C55 1.400(6) .
C51 C52 1.369(6) .
C52 C53 1.383(6) .
C53 C54 1.364(7) .
C54 C55 1.368(7) .
C56 C57 1.366(6) .
C57 C58 1.397(6) .
Cl1B C59B 1.751(15) .
Cl2B C59B 1.746(15) .
Cl3 C60A 1.809(16) .
Cl3 C60B 1.65(2) .
Cl4A C60A 1.732(18) .
Cl4B C60B 1.72(2) .
Cl1 C59A 1.762(6) .
Cl2A C59A 1.761(6) .
C61 C62 1.619(10) .
C62 C63 1.484(9) .
C63 C63 1.482(12) 3_655
