# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mxm542rm_auto
_audit_block_doi                 10.5517/ccdc.csd.cc2dlrb3
_database_code_depnum_ccdc_archive 'CCDC 2222555'
loop_
_audit_author_name
_audit_author_address
'Lee Cameron'
;Curtin University
Australia
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C29 H23 Ir N7, F6 P, C3 H6 O'
_chemical_formula_sum            'C32 H29 F6 Ir N7 O P'
_chemical_formula_weight         864.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_chemical_absolute_configuration .
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'
_exptl_crystal_recrystallization_method 
'grown from the slow evaporation of acetone from an acetone and water solution'
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            orange
_diffrn_ambient_temperature      100.00(10)
_chemical_oxdiff_formula         'C29 H23 Ir1 N7'
_chemical_oxdiff_usercomment     'Lee Cameron'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;

_cell_length_a                   11.67480(10)
_cell_length_b                   13.09290(10)
_cell_length_c                   20.61330(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.9730(10)
_cell_angle_gamma                90
_cell_volume                     3093.28(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    51553
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4390
_cell_measurement_theta_min      3.9970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1696
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.074
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            90926
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.341
_diffrn_reflns_theta_min         4.021
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     24.00 118.00   0.50    0.05    --   46.32  77.00-120.00  188
  2  ω     24.00 118.00   0.50    0.05    --   46.32  77.00 -60.00  188
  3  ω     24.00 118.00   0.50    0.05    --   46.32  77.00 -90.00  188
  4  ω     24.00 118.00   0.50    0.05    --   46.32  77.00   0.00  188
  5  ω     24.00 118.00   0.50    0.05    --   46.32  77.00  60.00  188
  6  ω     24.00 118.00   0.50    0.05    --   46.32  77.00 120.00  188
  7  ω     24.00 118.00   0.50    0.05    --   46.32  77.00 150.00  188
  8  ω     31.00 118.00   0.50    0.05    --   46.32  59.00 148.00  174
  9  ω     34.00 119.00   0.50    0.05    --   46.32  38.00 120.00  170
 10  ω     34.00 119.00   0.50    0.05    --   46.32  38.00  30.00  170
 11  ω     34.00 121.00   0.50    0.05    --   46.32  19.00 -30.00  174
 12  ω     34.00 119.00   0.50    0.05    --   46.32  38.00 -90.00  170
 13  ω     24.00 118.00   0.50    0.05    --   46.32  77.00-180.00  188
 14  ω    -28.00  26.00   0.50    0.05    --   46.32 -19.00  30.00  108
 15  ω    -25.00  62.00   0.50    0.05    --   46.32 -59.00   8.00  174
 16  ω     30.00 105.00   0.50    0.05    --  102.29 -94.00  90.00  150
 17  ω     13.00  94.00   0.50    0.05    --   46.32-125.00  30.00  162
 18  ω     30.00 111.00   0.50    0.05    --  102.29-125.00 -30.00  162
 19  ω    -26.00  43.00   0.50    0.05    --   46.32 -38.00-180.00  138
 20  ω     30.00 105.00   0.50    0.05    --  102.29 -94.00-150.00  150
 21  ω     30.00  68.00   0.50    0.05    --  102.29 -59.00   8.00   76
 22  ω     30.00 105.00   0.50    0.05    --  102.29 -77.00 120.00  150
 23  ω     30.00 105.00   0.50    0.05    --  102.29 -77.00  90.00  150
 24  ω     30.00  71.00   0.50    0.05    --  102.29 -61.00  30.00   82
 25  ω     30.00 105.00   0.50    0.05    --  102.29 -77.00 -30.00  150
 26  ω     90.00 176.00   0.50    0.05    --  102.29  30.00 -60.00  172
 27  ω     86.00 174.00   0.50    0.05    --  102.29  61.00  60.00  176
 28  ω     87.00 174.00   0.50    0.05    --  102.29  59.00 148.00  174
 29  ω    -26.00  29.00   0.50    0.05    --  -46.32  19.00 -90.00  110
 30  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00-180.00   82
 31  ω   -105.00 -30.00   0.50    0.05    -- -102.29  77.00-180.00  150
 32  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 -60.00   82
 33  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 -90.00   82
 34  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 -30.00   82
 35  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00   0.00   82
 36  ω    -62.00  26.00   0.50    0.05    --  -46.32  59.00 148.00  176
 37  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 120.00   82
 38  ω    -68.00 -30.00   0.50    0.05    -- -102.29  59.00 148.00   76
 39  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -77.00 -60.00  188
 40  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -77.00 -90.00  188
 41  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00-120.00  176
 42  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00 -90.00  176
 43  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00 -30.00  176
 44  ω   -174.00 -87.00   0.50    0.05    -- -102.29 -59.00   8.00  174
 45  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00  60.00  176
 46  ω   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00  30.00  168
 47  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00  90.00  176
 48  ω   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00 120.00  168
 49  ω   -118.00 -31.00   0.50    0.05    --  -46.32 -57.00  60.00  174
 50  ω   -118.00 -31.00   0.50    0.05    --  -46.32 -59.00   8.00  174
 51  ω   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00 -60.00  168
 52  ω   -176.00 -89.00   0.50    0.05    -- -102.29 -15.00 -90.00  174
 53  ω   -176.00 -90.00   0.50    0.05    -- -102.29 -30.00-120.00  172
 54  ω   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00-150.00  168
 55  ω   -176.00 -90.00   0.50    0.05    -- -102.29 -30.00-150.00  172
 56  ω   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00-180.00  168
 57  ω   -118.00 -73.00   0.50    0.05    --  -46.32-125.00-180.00   90
 58  ω   -118.00 -73.00   0.50    0.05    --  -46.32-125.00  90.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1010773000
_diffrn_orient_matrix_UB_12      0.0168026000
_diffrn_orient_matrix_UB_13      -0.0372296000
_diffrn_orient_matrix_UB_21      0.0532223000
_diffrn_orient_matrix_UB_22      0.0804583000
_diffrn_orient_matrix_UB_23      0.0516058000
_diffrn_orient_matrix_UB_31      0.0708779000
_diffrn_orient_matrix_UB_32      -0.0841868000
_diffrn_orient_matrix_UB_33      0.0417630000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6033
_reflns_number_total             6336
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL n/a (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.999
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6336
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0214
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0298P)²+3.3763P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0550
_refine_special_details          
;
# start Validation Reply Form

PROBLEM: 244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of P1  
RESPONSE: This a false alert due to the presence of PF6

# end Validation Reply Form
;
_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.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C14(H14), C8(H8), C10(H10), C11(H11), C4(H4), C5(H5), C6(H6),
 C28(H28), C25(H25), C16(H16), C20(H20), C9(H9), C17(H17), C27(H27), C15(H15),
 C26(H26), C21(H21), C7(H7), C22(H22)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.26116(2) 0.39729(2) 0.64034(2) 0.01142(5) Uani 1 1 d . . . . .
P1 P 0.25774(6) 0.05240(5) 0.43834(3) 0.02011(13) Uani 1 1 d . . . . .
F3 F 0.27274(14) 0.16100(13) 0.47454(9) 0.0319(4) Uani 1 1 d . . . . .
F6 F 0.18546(16) 0.01145(14) 0.49187(9) 0.0383(4) Uani 1 1 d . . . . .
F4 F 0.13930(16) 0.09077(13) 0.39345(9) 0.0369(4) Uani 1 1 d . . . . .
F2 F 0.37584(15) 0.01321(15) 0.48369(9) 0.0399(4) Uani 1 1 d . . . . .
F1 F 0.33051(19) 0.09330(14) 0.38529(10) 0.0432(5) Uani 1 1 d . . . . .
F5 F 0.24370(15) -0.05667(13) 0.40226(9) 0.0371(4) Uani 1 1 d . . . . .
N4 N 0.33780(18) 0.38652(15) 0.55413(10) 0.0143(4) Uani 1 1 d . . . . .
N7 N 0.11365(17) 0.32307(15) 0.59260(9) 0.0138(4) Uani 1 1 d . . . . .
N6 N 0.39402(17) 0.48405(15) 0.69181(9) 0.0140(4) Uani 1 1 d . . . . .
N5 N 0.36887(16) 0.26106(15) 0.65617(9) 0.0140(4) Uani 1 1 d . . . . .
N1 N 0.46099(17) 0.31954(16) 0.50154(10) 0.0172(4) Uani 1 1 d . . . . .
N3 N 0.34146(17) 0.44334(16) 0.49949(10) 0.0171(4) Uani 1 1 d . . . . .
N2 N 0.4158(2) 0.40300(16) 0.46741(11) 0.0192(5) Uani 1 1 d . . . . .
O1 O 0.66494(18) 0.35111(18) 0.62687(10) 0.0349(5) Uani 1 1 d . . . . .
C18 C 0.2180(2) 0.39284(17) 0.73012(12) 0.0145(5) Uani 1 1 d . . . . .
C2 C 0.4119(2) 0.30934(19) 0.55446(11) 0.0146(5) Uani 1 1 d . . . . .
C3 C 0.42799(19) 0.23439(18) 0.60787(11) 0.0146(5) Uani 1 1 d . . . . .
C13 C 0.2971(2) 0.44530(18) 0.77979(11) 0.0155(5) Uani 1 1 d . . . . .
C29 C 0.1524(2) 0.51751(18) 0.62039(11) 0.0139(4) Uani 1 1 d . . . . .
C19 C 0.1075(2) 0.22383(19) 0.57595(11) 0.0163(5) Uani 1 1 d . . . . .
H19 H 0.176707 0.184007 0.584853 0.020 Uiso 1 1 calc R U . . .
C14 C 0.2822(2) 0.44646(19) 0.84568(12) 0.0177(5) Uani 1 1 d . . . . .
H14 H 0.336329 0.481818 0.878249 0.021 Uiso 1 1 calc R U . . .
C12 C 0.3938(2) 0.49682(18) 0.75727(12) 0.0158(5) Uani 1 1 d . . . . .
C23 C 0.0154(2) 0.38215(19) 0.57758(12) 0.0157(5) Uani 1 1 d . . . . .
C8 C 0.4759(2) 0.53118(19) 0.66447(12) 0.0170(5) Uani 1 1 d . . . . .
H8 H 0.474965 0.521974 0.618662 0.020 Uiso 1 1 calc R U . . .
C10 C 0.5640(2) 0.60367(19) 0.76817(14) 0.0215(6) Uani 1 1 d . . . . .
H10 H 0.622715 0.644067 0.794514 0.026 Uiso 1 1 calc R U . . .
C11 C 0.4801(2) 0.5551(2) 0.79610(12) 0.0203(5) Uani 1 1 d . . . . .
H11 H 0.481528 0.561534 0.842144 0.024 Uiso 1 1 calc R U . . .
C4 C 0.4928(2) 0.1457(2) 0.61030(12) 0.0198(5) Uani 1 1 d . . . . .
H4 H 0.531413 0.128189 0.575218 0.024 Uiso 1 1 calc R U . . .
C5 C 0.5003(2) 0.0829(2) 0.66493(13) 0.0205(5) Uani 1 1 d . . . . .
H5 H 0.544475 0.021592 0.667877 0.025 Uiso 1 1 calc R U . . .
C6 C 0.4430(2) 0.11007(19) 0.71525(14) 0.0198(5) Uani 1 1 d . . . . .
H6 H 0.448496 0.068503 0.753488 0.024 Uiso 1 1 calc R U . . .
C28 C 0.1755(2) 0.62118(19) 0.63337(12) 0.0174(5) Uani 1 1 d . . . . .
H28 H 0.252963 0.642399 0.651126 0.021 Uiso 1 1 calc R U . . .
C25 C -0.0524(2) 0.5641(2) 0.57908(12) 0.0194(5) Uani 1 1 d . . . . .
H25 H -0.129609 0.544234 0.559728 0.023 Uiso 1 1 calc R U . . .
C16 C 0.1105(2) 0.3429(2) 0.81523(13) 0.0209(5) Uani 1 1 d . . . . .
H16 H 0.046804 0.307267 0.827215 0.025 Uiso 1 1 calc R U . . .
C20 C 0.0047(2) 0.17732(19) 0.54648(12) 0.0191(5) Uani 1 1 d . . . . .
H20 H 0.003310 0.107159 0.534593 0.023 Uiso 1 1 calc R U . . .
C24 C 0.0356(2) 0.49064(19) 0.59247(12) 0.0159(5) Uani 1 1 d . . . . .
C9 C 0.5609(2) 0.59233(19) 0.70074(14) 0.0202(5) Uani 1 1 d . . . . .
H9 H 0.616383 0.626110 0.680041 0.024 Uiso 1 1 calc R U . . .
C17 C 0.1254(2) 0.34178(19) 0.74949(12) 0.0169(5) Uani 1 1 d . . . . .
H17 H 0.071243 0.305479 0.717447 0.020 Uiso 1 1 calc R U . . .
C27 C 0.0865(2) 0.6940(2) 0.62063(12) 0.0207(5) Uani 1 1 d . . . . .
H27 H 0.104192 0.763775 0.630382 0.025 Uiso 1 1 calc R U . . .
C15 C 0.1880(2) 0.39563(19) 0.86321(13) 0.0209(6) Uani 1 1 d . . . . .
H15 H 0.176617 0.396940 0.907636 0.025 Uiso 1 1 calc R U . . .
C26 C -0.0276(2) 0.6658(2) 0.59389(13) 0.0215(5) Uani 1 1 d . . . . .
H26 H -0.087672 0.715664 0.585891 0.026 Uiso 1 1 calc R U . . .
C21 C -0.0967(2) 0.2355(2) 0.53456(12) 0.0213(5) Uani 1 1 d . . . . .
H21 H -0.169178 0.204883 0.515825 0.026 Uiso 1 1 calc R U . . .
C1 C 0.5504(2) 0.2580(2) 0.47850(13) 0.0252(6) Uani 1 1 d . . . . .
H1A H 0.517611 0.191463 0.463195 0.038 Uiso 1 1 calc R U . . .
H1B H 0.616927 0.248167 0.514899 0.038 Uiso 1 1 calc R U . . .
H1C H 0.576547 0.293440 0.442016 0.038 Uiso 1 1 calc R U . . .
C7 C 0.3774(2) 0.19909(19) 0.70884(12) 0.0173(5) Uani 1 1 d . . . . .
H7 H 0.336938 0.216964 0.743058 0.021 Uiso 1 1 calc R U . . .
C30 C 0.7123(2) 0.3667(2) 0.68366(14) 0.0267(6) Uani 1 1 d . . . . .
C22 C -0.0912(2) 0.3380(2) 0.55011(13) 0.0208(5) Uani 1 1 d . . . . .
H22 H -0.160088 0.378418 0.542104 0.025 Uiso 1 1 calc R U . . .
C31 C 0.6816(3) 0.3093(3) 0.74035(16) 0.0398(8) Uani 1 1 d . . . . .
H31A H 0.628375 0.350351 0.761140 0.060 Uiso 1 1 calc R U . . .
H31B H 0.752677 0.294746 0.772765 0.060 Uiso 1 1 calc R U . . .
H31C H 0.643458 0.244886 0.724431 0.060 Uiso 1 1 calc R U . . .
C32 C 0.8051(3) 0.4466(3) 0.70118(18) 0.0384(7) Uani 1 1 d . . . . .
H32A H 0.881827 0.413701 0.711207 0.058 Uiso 1 1 calc R U . . .
H32B H 0.791760 0.484844 0.739937 0.058 Uiso 1 1 calc R U . . .
H32C H 0.802293 0.493481 0.663852 0.058 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 N4 2.141(2) . ?
Ir1 N7 2.0574(19) . ?
Ir1 N6 2.0484(19) . ?
Ir1 N5 2.1709(19) . ?
Ir1 C18 2.009(2) . ?
Ir1 C29 2.015(2) . ?
P1 F3 1.5998(17) . ?
P1 F6 1.6036(18) . ?
P1 F4 1.5917(18) . ?
P1 F2 1.5962(17) . ?
P1 F1 1.599(2) . ?
P1 F5 1.6041(18) . ?
N4 N3 1.357(3) . ?
N4 C2 1.329(3) . ?
N7 C19 1.342(3) . ?
N7 C23 1.369(3) . ?
N6 C12 1.360(3) . ?
N6 C8 1.348(3) . ?
N5 C3 1.361(3) . ?
N5 C7 1.344(3) . ?
N1 N2 1.351(3) . ?
N1 C2 1.332(3) . ?
N1 C1 1.467(3) . ?
N3 N2 1.299(3) . ?
O1 C30 1.213(3) . ?
C18 C13 1.419(3) . ?
C18 C17 1.393(3) . ?
C2 C3 1.460(3) . ?
C3 C4 1.382(3) . ?
C13 C14 1.402(3) . ?
C13 C12 1.464(3) . ?
C29 C28 1.400(3) . ?
C29 C24 1.419(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.379(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.392(4) . ?
C12 C11 1.390(3) . ?
C23 C24 1.463(3) . ?
C23 C22 1.391(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.380(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.382(4) . ?
C10 C9 1.391(4) . ?
C11 H11 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.383(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.387(3) . ?
C28 H28 0.9500 . ?
C28 C27 1.398(4) . ?
C25 H25 0.9500 . ?
C25 C24 1.396(3) . ?
C25 C26 1.384(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.398(3) . ?
C16 C15 1.390(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.390(4) . ?
C9 H9 0.9500 . ?
C17 H17 0.9500 . ?
C27 H27 0.9500 . ?
C27 C26 1.391(4) . ?
C15 H15 0.9500 . ?
C26 H26 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.379(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C7 H7 0.9500 . ?
C30 C31 1.490(4) . ?
C30 C32 1.500(4) . ?
C22 H22 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ir1 N5 75.46(7) . . ?
N7 Ir1 N4 90.91(8) . . ?
N7 Ir1 N5 95.28(7) . . ?
N6 Ir1 N4 94.10(8) . . ?
N6 Ir1 N7 172.77(8) . . ?
N6 Ir1 N5 91.03(7) . . ?
C18 Ir1 N4 168.62(9) . . ?
C18 Ir1 N7 95.33(9) . . ?
C18 Ir1 N6 80.62(9) . . ?
C18 Ir1 N5 94.45(8) . . ?
C18 Ir1 C29 87.23(9) . . ?
C29 Ir1 N4 103.22(8) . . ?
C29 Ir1 N7 80.43(9) . . ?
C29 Ir1 N6 93.34(9) . . ?
C29 Ir1 N5 175.53(8) . . ?
F3 P1 F6 90.08(10) . . ?
F3 P1 F5 179.57(11) . . ?
F6 P1 F5 90.04(10) . . ?
F4 P1 F3 89.79(9) . . ?
F4 P1 F6 89.59(11) . . ?
F4 P1 F2 179.47(13) . . ?
F4 P1 F1 90.72(12) . . ?
F4 P1 F5 90.61(9) . . ?
F2 P1 F3 90.39(10) . . ?
F2 P1 F6 89.92(11) . . ?
F2 P1 F1 89.77(11) . . ?
F2 P1 F5 89.20(10) . . ?
F1 P1 F3 89.77(10) . . ?
F1 P1 F6 179.66(12) . . ?
F1 P1 F5 90.10(10) . . ?
N3 N4 Ir1 137.46(16) . . ?
C2 N4 Ir1 114.83(16) . . ?
C2 N4 N3 107.33(19) . . ?
C19 N7 Ir1 125.37(16) . . ?
C19 N7 C23 119.1(2) . . ?
C23 N7 Ir1 115.49(16) . . ?
C12 N6 Ir1 115.95(16) . . ?
C8 N6 Ir1 124.37(16) . . ?
C8 N6 C12 119.6(2) . . ?
C3 N5 Ir1 117.44(15) . . ?
C7 N5 Ir1 124.70(16) . . ?
C7 N5 C3 117.8(2) . . ?
N2 N1 C1 120.4(2) . . ?
C2 N1 N2 108.7(2) . . ?
C2 N1 C1 130.8(2) . . ?
N2 N3 N4 109.22(19) . . ?
N3 N2 N1 107.24(19) . . ?
C13 C18 Ir1 114.04(17) . . ?
C17 C18 Ir1 128.51(19) . . ?
C17 C18 C13 117.4(2) . . ?
N4 C2 N1 107.5(2) . . ?
N4 C2 C3 120.4(2) . . ?
N1 C2 C3 132.1(2) . . ?
N5 C3 C2 111.6(2) . . ?
N5 C3 C4 122.7(2) . . ?
C4 C3 C2 125.7(2) . . ?
C18 C13 C12 115.4(2) . . ?
C14 C13 C18 121.4(2) . . ?
C14 C13 C12 123.2(2) . . ?
C28 C29 Ir1 128.84(18) . . ?
C28 C29 C24 117.0(2) . . ?
C24 C29 Ir1 114.10(17) . . ?
N7 C19 H19 118.7 . . ?
N7 C19 C20 122.7(2) . . ?
C20 C19 H19 118.7 . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.8(2) . . ?
C15 C14 H14 120.1 . . ?
N6 C12 C13 113.9(2) . . ?
N6 C12 C11 120.0(2) . . ?
C11 C12 C13 126.1(2) . . ?
N7 C23 C24 114.0(2) . . ?
N7 C23 C22 120.2(2) . . ?
C22 C23 C24 125.8(2) . . ?
N6 C8 H8 118.9 . . ?
N6 C8 C9 122.2(2) . . ?
C9 C8 H8 118.9 . . ?
C11 C10 H10 120.6 . . ?
C11 C10 C9 118.8(2) . . ?
C9 C10 H10 120.6 . . ?
C12 C11 H11 119.8 . . ?
C10 C11 C12 120.4(2) . . ?
C10 C11 H11 119.8 . . ?
C3 C4 H4 120.7 . . ?
C3 C4 C5 118.6(2) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.5(2) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 120.6 . . ?
C5 C6 C7 118.8(2) . . ?
C7 C6 H6 120.6 . . ?
C29 C28 H28 119.5 . . ?
C27 C28 C29 121.0(2) . . ?
C27 C28 H28 119.5 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C26 C25 C24 120.2(2) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C15 C16 C17 120.7(2) . . ?
C19 C20 H20 120.8 . . ?
C19 C20 C21 118.4(2) . . ?
C21 C20 H20 120.8 . . ?
C29 C24 C23 115.5(2) . . ?
C25 C24 C29 121.6(2) . . ?
C25 C24 C23 123.0(2) . . ?
C8 C9 C10 118.9(2) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C18 C17 C16 121.3(2) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C28 C27 H27 119.5 . . ?
C26 C27 C28 121.0(2) . . ?
C26 C27 H27 119.5 . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.5(2) . . ?
C16 C15 H15 120.3 . . ?
C25 C26 C27 119.2(2) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.4 . . ?
C20 C21 H21 120.2 . . ?
C22 C21 C20 119.5(2) . . ?
C22 C21 H21 120.2 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N5 C7 C6 122.6(2) . . ?
N5 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
O1 C30 C31 122.6(3) . . ?
O1 C30 C32 121.7(3) . . ?
C31 C30 C32 115.7(3) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 C23 119.8(2) . . ?
C21 C22 H22 120.1 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ir1 N4 N3 N2 171.85(18) . . . . ?
Ir1 N4 C2 N1 -173.42(14) . . . . ?
Ir1 N4 C2 C3 5.4(3) . . . . ?
Ir1 N7 C19 C20 177.13(17) . . . . ?
Ir1 N7 C23 C24 5.7(3) . . . . ?
Ir1 N7 C23 C22 -174.82(18) . . . . ?
Ir1 N6 C12 C13 0.1(3) . . . . ?
Ir1 N6 C12 C11 -179.59(18) . . . . ?
Ir1 N6 C8 C9 177.25(18) . . . . ?
Ir1 N5 C3 C2 3.5(2) . . . . ?
Ir1 N5 C3 C4 -175.47(18) . . . . ?
Ir1 N5 C7 C6 176.75(18) . . . . ?
Ir1 C18 C13 C14 -177.60(18) . . . . ?
Ir1 C18 C13 C12 2.2(3) . . . . ?
Ir1 C18 C17 C16 177.11(19) . . . . ?
Ir1 C29 C28 C27 -174.96(18) . . . . ?
Ir1 C29 C24 C23 -5.0(3) . . . . ?
Ir1 C29 C24 C25 176.37(18) . . . . ?
N4 N3 N2 N1 -0.2(3) . . . . ?
N4 C2 C3 N5 -6.0(3) . . . . ?
N4 C2 C3 C4 173.0(2) . . . . ?
N7 C19 C20 C21 -1.0(4) . . . . ?
N7 C23 C24 C29 -0.5(3) . . . . ?
N7 C23 C24 C25 178.1(2) . . . . ?
N7 C23 C22 C21 -3.7(4) . . . . ?
N6 C12 C11 C10 2.6(4) . . . . ?
N6 C8 C9 C10 1.6(4) . . . . ?
N5 C3 C4 C5 -1.8(4) . . . . ?
N1 C2 C3 N5 172.6(2) . . . . ?
N1 C2 C3 C4 -8.5(4) . . . . ?
N3 N4 C2 N1 0.8(3) . . . . ?
N3 N4 C2 C3 179.7(2) . . . . ?
N2 N1 C2 N4 -0.9(3) . . . . ?
N2 N1 C2 C3 -179.6(2) . . . . ?
C18 C13 C14 C15 -0.2(4) . . . . ?
C18 C13 C12 N6 -1.5(3) . . . . ?
C18 C13 C12 C11 178.2(2) . . . . ?
C2 N4 N3 N2 -0.4(3) . . . . ?
C2 N1 N2 N3 0.7(3) . . . . ?
C2 C3 C4 C5 179.4(2) . . . . ?
C3 N5 C7 C6 -0.3(3) . . . . ?
C3 C4 C5 C6 0.2(4) . . . . ?
C13 C18 C17 C16 0.5(3) . . . . ?
C13 C14 C15 C16 1.0(4) . . . . ?
C13 C12 C11 C10 -177.1(2) . . . . ?
C29 C28 C27 C26 -0.8(4) . . . . ?
C19 N7 C23 C24 -174.5(2) . . . . ?
C19 N7 C23 C22 5.0(3) . . . . ?
C19 C20 C21 C22 2.4(4) . . . . ?
C14 C13 C12 N6 178.3(2) . . . . ?
C14 C13 C12 C11 -2.0(4) . . . . ?
C12 N6 C8 C9 0.3(4) . . . . ?
C12 C13 C14 C15 180.0(2) . . . . ?
C23 N7 C19 C20 -2.6(3) . . . . ?
C8 N6 C12 C13 177.3(2) . . . . ?
C8 N6 C12 C11 -2.4(3) . . . . ?
C11 C10 C9 C8 -1.4(4) . . . . ?
C4 C5 C6 C7 1.2(4) . . . . ?
C5 C6 C7 N5 -1.2(4) . . . . ?
C28 C29 C24 C23 178.1(2) . . . . ?
C28 C29 C24 C25 -0.5(3) . . . . ?
C28 C27 C26 C25 -0.8(4) . . . . ?
C20 C21 C22 C23 -0.1(4) . . . . ?
C24 C29 C28 C27 1.4(3) . . . . ?
C24 C23 C22 C21 175.7(2) . . . . ?
C24 C25 C26 C27 1.6(4) . . . . ?
C9 C10 C11 C12 -0.6(4) . . . . ?
C17 C18 C13 C14 -0.5(3) . . . . ?
C17 C18 C13 C12 179.3(2) . . . . ?
C17 C16 C15 C14 -1.0(4) . . . . ?
C15 C16 C17 C18 0.2(4) . . . . ?
C26 C25 C24 C29 -1.0(4) . . . . ?
C26 C25 C24 C23 -179.5(2) . . . . ?
C1 N1 N2 N3 -178.6(2) . . . . ?
C1 N1 C2 N4 178.3(2) . . . . ?
C1 N1 C2 C3 -0.4(4) . . . . ?
C7 N5 C3 C2 -179.2(2) . . . . ?
C7 N5 C3 C4 1.8(3) . . . . ?
C22 C23 C24 C29 -179.9(2) . . . . ?
C22 C23 C24 C25 -1.3(4) . . . . ?

_olex2_exptl_crystal_mounting_method 
'mounted on a glass fibre using silicon oil'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.937
_oxdiff_exptl_absorpt_empirical_full_min 0.702

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mxm547rm_redo
_audit_block_doi                 10.5517/ccdc.csd.cc2dlrkb
_database_code_depnum_ccdc_archive 'CCDC 2222562'
loop_
_audit_author_name
_audit_author_address
'Lee Cameron'
;Curtin University
Australia
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C14 H9 Br N5 O3 Re'
_chemical_formula_sum            'C14 H9 Br N5 O3 Re'
_chemical_formula_weight         561.37
_exptl_crystal_recrystallization_method 
'grown from the slow evaporation of acetone from an acetone and water solution'
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            'clear light yellow'
_diffrn_ambient_temperature      102(3)
_chemical_oxdiff_formula         'Re N6 C30 O3 Br H10'
_chemical_oxdiff_usercomment     'Lee Cameron'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_chemical_absolute_configuration .
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.97900(10)
_cell_length_b                   10.42840(10)
_cell_length_c                   11.24010(10)
_cell_angle_alpha                89.4990(10)
_cell_angle_beta                 89.7010(10)
_cell_angle_gamma                72.3620(10)
_cell_volume                     779.563(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    24385
_cell_measurement_temperature    102(3)
_cell_measurement_theta_max      75.2250
_cell_measurement_theta_min      3.9030
_shelx_estimated_absorpt_T_max   0.319
_shelx_estimated_absorpt_T_min   0.188
_exptl_absorpt_coefficient_mu    18.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             524
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28125
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.517
_diffrn_reflns_theta_min         3.933
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     24.00 118.00   0.50    0.05    --   46.23  77.00 -90.00  188
  2  ω     28.00 122.00   0.50    0.05    --   50.00  76.00-123.93  188
  3  ω     24.00 118.00   0.50    0.05    --   46.23  77.00 -60.00  188
  4  ω     27.00 122.00   0.50    0.05    --   50.00  77.00 166.18  190
  5  ω     83.00 175.00   0.50    0.05    --  102.37  93.00  73.00  184
  6  ω    -23.00   3.00   0.50    0.05    --   14.00 105.00 -42.81   52
  7  ω     -3.00  23.00   0.50    0.05    --   30.00  99.00  76.19   52
  8  ω    -21.00  14.00   0.50    0.05    --   14.00 102.00-164.37   70
  9  ω     37.00 131.00   0.50    0.05    --   58.00  73.00 175.89  188
 10  ω     36.00 131.00   0.50    0.05    --   58.00  76.00  65.66  190
 11  ω     47.00 143.00   0.50    0.05    --   70.00  77.00  10.61  192
 12  ω     36.00 131.00   0.50    0.05    --   58.00  76.00 -14.61  190
 13  ω     35.00 131.00   0.50    0.05    --   58.00  77.00-103.29  192
 14  ω     44.00 139.00   0.50    0.05    --   66.00  75.00-170.08  190
 15  ω     43.00 139.00   0.50    0.05    --   66.00  77.00 -91.74  192
 16  ω     36.00 131.00   0.50    0.05    --   58.00  76.00  86.59  190
 17  ω     40.00 135.00   0.50    0.05    --   62.00  75.00 113.09  190
 18  ω    -27.00  40.00   0.50    0.05    --   46.23 -37.00 -90.00  134
 19  ω     30.00  68.00   0.50    0.05    --  102.37 -61.00-180.00   76
 20  ω     71.00 101.00   0.50    0.05    --  102.37 -77.00 -30.00   60
 21  ω     34.00  65.00   0.50    0.05    --  102.37 -77.00 -30.00   62
 22  ω     31.00  67.00   0.50    0.05    --  102.37 -61.00   0.00   72
 23  ω     30.00  65.00   0.50    0.05    --  102.37 -61.00 150.00   70
 24  ω     13.00  94.00   0.50    0.05    --   46.23-125.00  90.00  162
 25  ω     30.00 104.00   0.50    0.05    --  102.37 -94.00 120.00  148
 26  ω     33.00 100.00   0.50    0.05    --  102.37 -94.00  90.00  134
 27  ω    -25.00  76.00   0.50    0.05    --   46.23 -93.00 -38.00  202
 28  ω     79.00 105.00   0.50    0.05    --  102.37 -94.00-120.00   52
 29  ω     75.00 104.00   0.50    0.05    --  102.37 -98.00-155.25   58
 30  ω     38.00  64.00   0.50    0.05    --  102.37 -98.00-155.25   52
 31  ω     41.00  67.00   0.50    0.05    --  102.37 -94.00-120.00   52
 32  ω     30.00 106.00   0.50    0.05    --  102.37 -93.00 -38.00  152
 33  ω   -118.00 -23.00   0.50    0.05    --  -46.23 -77.00  30.00  190
 34  ω   -118.00 -23.00   0.50    0.05    --  -46.23 -77.00 -30.00  190
 35  ω   -118.00 -23.00   0.50    0.05    --  -46.23 -77.00-180.00  190
 36  ω   -119.00 -34.00   0.50    0.05    --  -46.23 -37.00-180.00  170
 37  ω   -118.00 -23.00   0.50    0.05    --  -46.23 -77.00  90.00  190
 38  ω   -129.00 -81.00   0.50    0.05    -- -102.37 -77.00 127.42   96
 39  ω   -163.00-138.00   0.50    0.05    -- -102.37 -77.00 127.42   50
 40  ω   -145.00-112.00   0.50    0.05    --  -94.00 -76.00  75.75   66
 41  ω   -104.00 -71.00   0.50    0.05    --  -94.00 -76.00  75.75   66
 42  ω   -106.00 -72.00   0.50    0.05    --  -94.00 -76.00 -10.93   68
 43  ω   -144.00-119.00   0.50    0.05    --  -94.00 -76.00  21.02   50
 44  ω   -148.00-121.00   0.50    0.05    --  -90.00 -76.00  60.17   54
 45  ω    -92.00 -67.00   0.50    0.05    --  -90.00 -76.00  60.17   50
 46  ω   -149.00-111.00   0.50    0.05    --  -94.00 -76.00 -10.93   76
 47  ω   -153.00 -82.00   0.50    0.05    -- -102.37 -76.00 -51.29  142
 48  ω   -142.00 -80.00   0.50    0.05    -- -102.37 -77.00-120.00  124
 49  ω   -175.00-149.00   0.50    0.05    -- -102.37 -77.00-120.00   52
 50  ω   -120.00 -81.00   0.50    0.05    -- -102.37 -74.00-151.52   78
 51  ω   -159.00-127.00   0.50    0.05    -- -102.37 -74.00-151.52   64
 52  ω   -108.00 -71.00   0.50    0.05    --  -94.00 -76.00  21.02   74
 53  ω    -87.00 -61.00   0.50    0.05    --  -82.00 -75.00 109.94   52
 54  ω   -159.00 -65.00   0.50    0.05    --  -86.00 -73.00 146.60  188
 55  ω   -117.00 -82.00   0.50    0.05    -- -102.37 -75.00  61.26   70
 56  ω    -99.00 -65.00   0.50    0.05    --  -86.00 -72.00 136.10   68
 57  ω    -94.00 -68.00   0.50    0.05    --  -86.00 -71.00 168.50   52
 58  ω    -95.00 -57.00   0.50    0.05    --  -78.00 -72.00  92.78   76
 59  ω    -94.00 -69.00   0.50    0.05    --  -90.00 -73.00  23.32   50
 60  ω    -89.00 -63.00   0.50    0.05    --  -82.00 -71.00 -17.17   52
 61  ω    -88.00 -53.00   0.50    0.05    --  -74.00 -72.00 -58.07   70
 62  ω    -90.00 -61.00   0.50    0.05    --  -82.00 -73.00-103.09   58
 63  ω    -86.00 -60.00   0.50    0.05    --  -74.00 -70.00-157.64   52
 64  ω   -153.00 -85.00   0.50    0.05    -- -102.37 -68.00 -96.74  136
 65  ω   -111.00 -83.00   0.50    0.05    -- -102.37 -70.00 -50.93   56
 66  ω   -136.00-111.00   0.50    0.05    --  -86.00 -67.00  96.94   50
 67  ω    -93.00 -67.00   0.50    0.05    --  -86.00 -67.00  96.94   52
 68  ω    -79.00 -54.00   0.50    0.05    --  -74.00 -69.00 169.15   50
 69  ω   -139.00 -47.00   0.50    0.05    --  -66.00 -68.00 166.20  184
 70  ω   -167.00-112.00   0.50    0.05    --  -94.00 -66.00  30.89  110
 71  ω   -106.00 -76.00   0.50    0.05    --  -94.00 -66.00  30.89   60
 72  ω    -94.00 -69.00   0.50    0.05    --  -86.00 -62.00 -52.16   50
 73  ω    -90.00 -65.00   0.50    0.05    --  -82.00 -61.00 -82.82   50
 74  ω    -97.00 -67.00   0.50    0.05    --  -82.00 -64.00 -90.83   60
 75  ω   -139.00 -49.00   0.50    0.05    --  -66.00 -63.00-100.70  180
 76  ω   -157.00-119.00   0.50    0.05    --  -86.00 -61.00-147.05   76
 77  ω   -111.00 -69.00   0.50    0.05    --  -86.00 -61.00-147.05   84
 78  ω    -92.00 -66.00   0.50    0.05    --  -82.00 -59.00-140.78   52
 79  ω   -171.00 -87.00   0.50    0.05    -- -102.37 -61.00 -90.00  168
 80  ω   -175.00 -88.00   0.50    0.05    -- -102.37 -61.00  -4.08  174
 81  ω   -112.00 -75.00   0.50    0.05    --  -90.00 -56.00 175.97   74
 82  ω   -158.00-123.00   0.50    0.05    --  -90.00 -56.00 175.97   70
 83  ω   -163.00-126.00   0.50    0.05    --  -94.00 -50.00 159.61   74
 84  ω   -120.00 -80.00   0.50    0.05    --  -94.00 -50.00 159.61   80
 85  ω   -166.00 -79.00   0.50    0.05    --  -94.00 -58.00  85.66  174
 86  ω   -175.00 -83.00   0.50    0.05    -- -102.37 -93.00 -38.00  184
 87  ω   -101.00 -55.00   0.50    0.05    -- -102.37  93.00  73.00   92
 88  ω    -76.00  27.00   0.50    0.05    --  -46.23  93.00  73.00  206
 89  ω   -103.00 -31.00   0.50    0.05    -- -102.37  77.00 -90.00  144
 90  ω    -96.00 -47.00   0.50    0.05    -- -102.37 125.00-120.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0335148000
_diffrn_orient_matrix_UB_12      0.0586349000
_diffrn_orient_matrix_UB_13      0.1206891000
_diffrn_orient_matrix_UB_21      0.1397064000
_diffrn_orient_matrix_UB_22      -0.1388863000
_diffrn_orient_matrix_UB_23      0.0384985000
_diffrn_orient_matrix_UB_31      0.1816929000
_diffrn_orient_matrix_UB_32      0.0361018000
_diffrn_orient_matrix_UB_33      -0.0523357000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3105
_reflns_number_total             3111
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.957
_refine_diff_density_min         -1.662
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3111
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.156
_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)+(0.0275P)²+1.9576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0525
_refine_special_details          ?
_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.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C11(H11), C8(H8), C10(H10), C12(H12)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.31474(2) 0.77404(2) 0.84298(2) 0.00813(6) Uani 1 1 d . . . . .
Br1 Br 0.67729(5) 0.62978(3) 0.77845(3) 0.01345(9) Uani 1 1 d . . . . .
O3 O 0.4460(4) 1.0285(2) 0.8690(2) 0.0155(5) Uani 1 1 d . . . . .
O2 O 0.4064(4) 0.7205(3) 1.1079(2) 0.0163(5) Uani 1 1 d . . . . .
N4 N 0.2331(4) 0.5947(3) 0.8181(3) 0.0126(6) Uani 1 1 d . . . . .
O1 O -0.1135(4) 0.9373(3) 0.9125(2) 0.0199(6) Uani 1 1 d . . . . .
N5 N 0.2554(4) 0.7630(3) 0.6450(2) 0.0102(5) Uani 1 1 d . . . . .
N2 N 0.1562(5) 0.4181(3) 0.8197(3) 0.0144(6) Uani 1 1 d . . . . .
N1 N 0.1725(5) 0.4412(3) 0.7032(3) 0.0148(6) Uani 1 1 d . . . . .
N3 N 0.1915(5) 0.5072(3) 0.8908(3) 0.0137(6) Uani 1 1 d . . . . .
C2 C 0.3740(5) 0.7428(3) 1.0080(3) 0.0127(7) Uani 1 1 d . . . . .
C1 C 0.0463(5) 0.8761(3) 0.8841(3) 0.0127(7) Uani 1 1 d . . . . .
C3 C 0.3982(5) 0.9338(4) 0.8570(3) 0.0125(7) Uani 1 1 d . . . . .
C6 C 0.2453(5) 0.6432(3) 0.6084(3) 0.0115(6) Uani 1 1 d . . . . .
C13 C 0.2390(5) 0.9911(3) 0.5908(3) 0.0125(7) Uani 1 1 d . . . . .
H13 H 0.225117 1.016132 0.672181 0.015 Uiso 1 1 calc R U . . .
C5 C 0.2204(5) 0.5551(3) 0.7059(3) 0.0120(7) Uani 1 1 d . . . . .
C7 C 0.2539(5) 0.6032(3) 0.4895(3) 0.0148(7) Uani 1 1 d . . . . .
H7 H 0.244561 0.517182 0.468976 0.018 Uiso 1 1 calc R U . . .
C9 C 0.2749(5) 0.8220(4) 0.4359(3) 0.0128(7) Uani 1 1 d . . . . .
C11 C 0.2627(5) 1.0499(4) 0.3837(3) 0.0143(7) Uani 1 1 d . . . . .
H11 H 0.266090 1.115566 0.325307 0.017 Uiso 1 1 calc R U . . .
C14 C 0.2588(5) 0.8572(3) 0.5591(3) 0.0103(6) Uani 1 1 d . . . . .
C8 C 0.2762(5) 0.6913(4) 0.4037(3) 0.0152(7) Uani 1 1 d . . . . .
H8 H 0.292510 0.664663 0.322752 0.018 Uiso 1 1 calc R U . . .
C10 C 0.2801(5) 0.9220(4) 0.3501(3) 0.0152(7) Uani 1 1 d . . . . .
H10 H 0.296017 0.899123 0.268247 0.018 Uiso 1 1 calc R U . . .
C12 C 0.2394(5) 1.0857(4) 0.5054(3) 0.0143(7) Uani 1 1 d . . . . .
H12 H 0.224004 1.175848 0.527916 0.017 Uiso 1 1 calc R U . . .
C4 C 0.0877(6) 0.3073(4) 0.8661(3) 0.0195(8) Uani 1 1 d . . . . .
H4A H -0.058748 0.338273 0.875656 0.029 Uiso 1 1 calc R U . . .
H4B H 0.150871 0.277579 0.943308 0.029 Uiso 1 1 calc R U . . .
H4C H 0.125402 0.232082 0.810211 0.029 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 Br1 2.6239(4) . ?
Re1 N4 2.135(3) . ?
Re1 N5 2.276(3) . ?
Re1 C2 1.906(4) . ?
Re1 C1 1.910(4) . ?
Re1 C3 1.932(4) . ?
O3 C3 1.144(4) . ?
O2 C2 1.153(4) . ?
N4 N3 1.316(4) . ?
N4 C5 1.342(4) . ?
O1 C1 1.149(5) . ?
N5 C6 1.341(4) . ?
N5 C14 1.377(4) . ?
N2 N1 1.339(4) . ?
N2 N3 1.311(4) . ?
N2 C4 1.469(5) . ?
N1 C5 1.328(5) . ?
C6 C5 1.467(5) . ?
C6 C7 1.398(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.410(5) . ?
C13 C12 1.371(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.367(5) . ?
C9 C14 1.431(5) . ?
C9 C8 1.410(5) . ?
C9 C10 1.423(5) . ?
C11 H11 0.9500 . ?
C11 C10 1.358(5) . ?
C11 C12 1.416(5) . ?
C8 H8 0.9500 . ?
C10 H10 0.9500 . ?
C12 H12 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Re1 Br1 85.75(8) . . ?
N4 Re1 N5 73.59(11) . . ?
N5 Re1 Br1 81.89(7) . . ?
C2 Re1 Br1 92.83(10) . . ?
C2 Re1 N4 95.07(12) . . ?
C2 Re1 N5 167.75(12) . . ?
C2 Re1 C1 89.17(14) . . ?
C2 Re1 C3 87.29(14) . . ?
C1 Re1 Br1 177.49(10) . . ?
C1 Re1 N4 92.58(13) . . ?
C1 Re1 N5 95.85(12) . . ?
C1 Re1 C3 89.93(14) . . ?
C3 Re1 Br1 91.67(10) . . ?
C3 Re1 N4 176.57(12) . . ?
C3 Re1 N5 103.84(12) . . ?
N3 N4 Re1 134.0(2) . . ?
N3 N4 C5 108.5(3) . . ?
C5 N4 Re1 117.5(2) . . ?
C6 N5 Re1 114.7(2) . . ?
C6 N5 C14 117.5(3) . . ?
C14 N5 Re1 127.0(2) . . ?
N1 N2 C4 123.0(3) . . ?
N3 N2 N1 115.5(3) . . ?
N3 N2 C4 121.3(3) . . ?
C5 N1 N2 100.8(3) . . ?
N2 N3 N4 103.9(3) . . ?
O2 C2 Re1 177.5(3) . . ?
O1 C1 Re1 177.9(3) . . ?
O3 C3 Re1 177.8(3) . . ?
N5 C6 C5 113.5(3) . . ?
N5 C6 C7 124.8(3) . . ?
C7 C6 C5 121.7(3) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C12 C13 C14 120.7(3) . . ?
N4 C5 C6 118.3(3) . . ?
N1 C5 N4 111.3(3) . . ?
N1 C5 C6 130.2(3) . . ?
C6 C7 H7 120.9 . . ?
C8 C7 C6 118.2(3) . . ?
C8 C7 H7 120.9 . . ?
C8 C9 C14 118.8(3) . . ?
C8 C9 C10 122.5(3) . . ?
C10 C9 C14 118.7(3) . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.3(3) . . ?
C12 C11 H11 119.8 . . ?
N5 C14 C13 120.5(3) . . ?
N5 C14 C9 120.5(3) . . ?
C13 C14 C9 118.9(3) . . ?
C7 C8 C9 119.7(3) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.9(3) . . ?
C11 C10 H10 119.6 . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 N4 N3 N2 -178.9(2) . . . . ?
Re1 N4 C5 N1 178.8(2) . . . . ?
Re1 N4 C5 C6 -5.4(4) . . . . ?
Re1 N5 C6 C5 15.5(4) . . . . ?
Re1 N5 C6 C7 -165.5(3) . . . . ?
Re1 N5 C14 C13 -20.1(4) . . . . ?
Re1 N5 C14 C9 162.3(2) . . . . ?
N5 C6 C5 N4 -7.4(5) . . . . ?
N5 C6 C5 N1 167.6(3) . . . . ?
N5 C6 C7 C8 0.7(5) . . . . ?
N2 N1 C5 N4 0.7(4) . . . . ?
N2 N1 C5 C6 -174.6(3) . . . . ?
N1 N2 N3 N4 0.1(4) . . . . ?
N3 N4 C5 N1 -0.6(4) . . . . ?
N3 N4 C5 C6 175.3(3) . . . . ?
N3 N2 N1 C5 -0.5(4) . . . . ?
C6 N5 C14 C13 170.5(3) . . . . ?
C6 N5 C14 C9 -7.2(5) . . . . ?
C6 C7 C8 C9 -4.6(5) . . . . ?
C5 N4 N3 N2 0.3(4) . . . . ?
C5 C6 C7 C8 179.6(3) . . . . ?
C7 C6 C5 N4 173.6(3) . . . . ?
C7 C6 C5 N1 -11.4(6) . . . . ?
C14 N5 C6 C5 -173.7(3) . . . . ?
C14 N5 C6 C7 5.3(5) . . . . ?
C14 C13 C12 C11 -0.9(5) . . . . ?
C14 C9 C8 C7 2.7(5) . . . . ?
C14 C9 C10 C11 -2.4(5) . . . . ?
C8 C9 C14 N5 3.4(5) . . . . ?
C8 C9 C14 C13 -174.3(3) . . . . ?
C8 C9 C10 C11 174.8(3) . . . . ?
C10 C9 C14 N5 -179.3(3) . . . . ?
C10 C9 C14 C13 3.0(5) . . . . ?
C10 C9 C8 C7 -174.5(3) . . . . ?
C10 C11 C12 C13 1.5(5) . . . . ?
C12 C13 C14 N5 -179.1(3) . . . . ?
C12 C13 C14 C9 -1.4(5) . . . . ?
C12 C11 C10 C9 0.2(5) . . . . ?
C4 N2 N1 C5 174.7(3) . . . . ?
C4 N2 N3 N4 -175.1(3) . . . . ?

_olex2_exptl_crystal_mounting_method 
'mounted on a glass fibre using silicon oil'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.867
_oxdiff_exptl_absorpt_empirical_full_min 0.729

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mxm551rm
_audit_block_doi                 10.5517/ccdc.csd.cc2dlrj9
_database_code_depnum_ccdc_archive 'CCDC 2222561'
loop_
_audit_author_name
_audit_author_address
'Lee Cameron'
;Curtin University
Australia
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C14 H9 Br N5 O3 Re'
_chemical_formula_sum            'C14 H9 Br N5 O3 Re'
_chemical_formula_weight         561.37

_exptl_crystal_recrystallization_method 
'grown from the slow evaporation of an acetonitrile solution'
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            'clear light orange'
_diffrn_ambient_temperature      100.00(10)
_chemical_oxdiff_formula         'Re1 C14 H9 O3 N5 Br1'
_chemical_oxdiff_usercomment     'Lee Cameron'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_chemical_absolute_configuration .
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'

_cell_length_a                   6.87749(3)
_cell_length_b                   11.42838(6)
_cell_length_c                   19.41606(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.1110(4)
_cell_angle_gamma                90
_cell_volume                     1525.038(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    30954
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2970
_cell_measurement_theta_min      3.7940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.896
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.445
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1048
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 5 2 0.0243
-3 -5 -4 0.0606
2 4 -9 0.0464
3 6 -2 0.0432
2 3 10 0.0790
-2 -5 7 0.0405
-1 0 -12 0.0643
1 1 12 0.0808
3 -4 5 0.0522
2 -5 -8 0.0474
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.084
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.1988 4.9515 1.5350 0.8572 -0.4822 0.0141
-2.9296 -5.1132 -3.5526 0.4171 0.7665 -0.4883
1.9640 4.2884 -8.8576 -0.4035 -0.7430 -0.5340
2.8995 5.5089 -2.3406 -0.4774 -0.8780 0.0344
2.0337 2.9892 9.7847 -0.2090 -0.3829 0.8998
-2.3265 -4.8273 7.1936 0.4416 0.8129 0.3798
-1.2191 -0.1321 -11.9873 0.0950 -0.0508 -0.9942
0.8376 0.7141 12.2245 0.0077 -0.0051 1.0000
3.2849 -3.9068 5.0251 -0.7550 0.4100 0.5118
2.2931 -4.5060 -7.8738 -0.7352 0.4002 -0.5471

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44552
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.491
_diffrn_reflns_theta_min         4.490
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     24.00 119.00   0.50    0.05    --   46.07  77.00  60.00  190
  2  ω     24.00 119.00   0.50    0.05    --   46.07  77.00 120.00  190
  3  ω     24.00 119.00   0.50    0.05    --   46.07  77.00 150.00  190
  4  ω     24.00 119.00   0.50    0.05    --   46.07  77.00 -30.00  190
  5  ω     24.00 119.00   0.50    0.05    --   46.07  77.00-150.00  190
  6  ω     24.00 119.00   0.50    0.05    --   46.07  77.00 -90.00  190
  7  ω     31.00 119.00   0.50    0.05    --   46.07  57.00-150.00  176
  8  ω     34.00 119.00   0.50    0.05    --   46.07  38.00 -60.00  170
  9  ω     31.00 119.00   0.50    0.05    --   46.07  57.00 -60.00  176
 10  ω     31.00 119.00   0.50    0.05    --   46.07  57.00  60.00  176
 11  ω     24.00 119.00   0.50    0.05    --   46.07  77.00   0.00  190
 12  ω     34.00 119.00   0.50    0.05    --   46.07  38.00-180.00  170
 13  ω    -28.00  26.00   0.50    0.05    --   46.07 -19.00-150.00  108
 14  ω    -28.00  26.00   0.50    0.05    --   46.07 -19.00 -90.00  108
 15  ω     30.00  71.00   0.50    0.05    --  102.29 -61.00-150.00   82
 16  ω     30.00  71.00   0.50    0.05    --  102.29 -61.00-120.00   82
 17  ω    -28.00  26.00   0.50    0.05    --   46.07 -19.00   0.00  108
 18  ω     30.00 105.00   0.50    0.05    --  102.29 -77.00  90.00  150
 19  ω     30.00  71.00   0.50    0.05    --  102.29 -61.00  30.00   82
 20  ω     26.00 108.00   0.50    0.05    --   46.07-149.00-100.00  164
 21  ω     30.00 105.00   0.50    0.05    --  102.29 -94.00 -90.00  150
 22  ω     30.00 129.00   0.50    0.05    --  102.29-149.00-100.00  198
 23  ω     30.00 111.00   0.50    0.05    --  102.29-125.00  30.00  162
 24  ω     30.00 110.00   0.50    0.05    --  102.29-123.00  63.00  160
 25  ω     12.00  93.00   0.50    0.05    --   46.07-123.00  63.00  162
 26  ω   -110.00 -30.00   0.50    0.05    -- -102.29 123.00 143.00  160
 27  ω   -121.00 -30.00   0.50    0.05    -- -102.29 138.00  83.96  182
 28  ω   -111.00 -30.00   0.50    0.05    -- -102.29 125.00  60.00  162
 29  ω   -128.00 -30.00   0.50    0.05    -- -102.29 149.00 -52.00  196
 30  ω   -111.00 -30.00   0.50    0.05    -- -102.29 125.00 -60.00  162
 31  ω   -111.00 -30.00   0.50    0.05    -- -102.29 125.00-120.00  162
 32  ω   -107.00 -25.00   0.50    0.05    --  -46.07 149.00 -52.00  164
 33  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00-180.00   82
 34  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00  90.00   82
 35  ω    -92.00 -11.00   0.50    0.05    --  -46.07 123.00 143.00  162
 36  ω     90.00 174.00   0.50    0.05    --  102.29  45.00-120.00  168
 37  ω     74.00 119.00   0.50    0.05    --   46.07 125.00-180.00   90
 38  ω     57.00 119.00   0.50    0.05    --   46.07 149.00 -52.00  124
 39  ω     57.00 166.00   0.50    0.05    --  102.29 149.00 -52.00  218
 40  ω     75.00 174.00   0.50    0.05    --  102.29 123.00 143.00  198
 41  ω     90.00 174.00   0.50    0.05    --  102.29  45.00 -60.00  168
 42  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -75.00  40.95  188
 43  ω   -174.00-109.00   0.50    0.05    -- -102.29 -70.00  68.39  130
 44  ω   -174.00 -85.00   0.50    0.05    -- -102.29 -63.00 150.52  178
 45  ω   -174.00 -88.00   0.50    0.05    -- -102.29 -48.00  98.74  172
 46  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -60.00  85.78  176
 47  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00 -12.12  176
 48  ω   -174.00 -87.00   0.50    0.05    -- -102.29 -59.00 -28.46  174
 49  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00 -90.00  176
 50  ω   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00-150.00  168
 51  ω   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00-180.00  168
 52  ω   -119.00 -57.00   0.50    0.05    --  -46.07-149.00-100.00  124
 53  ω   -166.00 -57.00   0.50    0.05    -- -102.29-149.00-100.00  218
 54  ω   -174.00 -75.00   0.50    0.05    -- -102.29-123.00  63.00  198
 55  ω   -119.00 -73.00   0.50    0.05    --  -46.07-125.00  90.00   92
 56  ω   -119.00 -73.00   0.50    0.05    --  -46.07-125.00 120.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2131846000
_diffrn_orient_matrix_UB_12      0.0312468000
_diffrn_orient_matrix_UB_13      0.0134090000
_diffrn_orient_matrix_UB_21      -0.0463662000
_diffrn_orient_matrix_UB_22      -0.1305654000
_diffrn_orient_matrix_UB_23      0.0103892000
_diffrn_orient_matrix_UB_31      0.0515159000
_diffrn_orient_matrix_UB_32      0.0120890000
_diffrn_orient_matrix_UB_33      0.0775634000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3102
_reflns_number_total             3118
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3118
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.150
_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)+(0.0253P)²+4.6815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0527
_refine_special_details          ?
_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.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C7(H7), C12(H12), C13(H13), C8(H8)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.69282(2) 0.16484(2) 0.38354(2) 0.00932(6) Uani 1 1 d . . . . .
Br1 Br 0.99658(5) 0.24129(3) 0.31861(2) 0.01465(9) Uani 1 1 d . . . . .
O2 O 0.9339(4) 0.1311(2) 0.51853(13) 0.0183(5) Uani 1 1 d . . . . .
O1 O 0.7534(4) -0.0949(2) 0.35423(13) 0.0190(5) Uani 1 1 d . . . . .
O3 O 0.3383(4) 0.0882(2) 0.46170(14) 0.0219(6) Uani 1 1 d . . . . .
N4 N 0.5340(4) 0.1954(3) 0.28829(15) 0.0126(5) Uani 1 1 d . . . . .
N2 N 0.3641(4) 0.1909(3) 0.19245(15) 0.0156(6) Uani 1 1 d . . . . .
N1 N 0.3787(4) 0.3031(3) 0.21432(15) 0.0131(6) Uani 1 1 d . . . . .
N3 N 0.4584(4) 0.1266(3) 0.23723(15) 0.0145(6) Uani 1 1 d . . . . .
N5 N 0.6226(4) 0.3593(2) 0.38100(14) 0.0097(5) Uani 1 1 d . . . . .
C3 C 0.4648(5) 0.1187(3) 0.43240(17) 0.0142(7) Uani 1 1 d . . . . .
C5 C 0.4854(5) 0.3044(3) 0.27349(17) 0.0122(6) Uani 1 1 d . . . . .
C1 C 0.7359(5) 0.0029(3) 0.36601(18) 0.0148(7) Uani 1 1 d . . . . .
C2 C 0.8455(5) 0.1458(3) 0.46823(17) 0.0111(6) Uani 1 1 d . . . . .
C9 C 0.6809(5) 0.5648(3) 0.41129(17) 0.0120(6) Uani 1 1 d . . . . .
C10 C 0.7443(5) 0.6481(3) 0.46108(19) 0.0148(7) Uani 1 1 d . . . . .
H10 H 0.751214 0.728385 0.448813 0.018 Uiso 1 1 calc R U . . .
C6 C 0.5481(5) 0.3984(3) 0.32022(17) 0.0117(6) Uani 1 1 d . . . . .
C11 C 0.7957(5) 0.6140(3) 0.52651(18) 0.0144(7) Uani 1 1 d . . . . .
H11 H 0.837364 0.670496 0.559786 0.017 Uiso 1 1 calc R U . . .
C7 C 0.5385(5) 0.5162(3) 0.30061(18) 0.0143(7) Uani 1 1 d . . . . .
H7 H 0.481971 0.538299 0.257153 0.017 Uiso 1 1 calc R U . . .
C12 C 0.7868(5) 0.4940(3) 0.54480(17) 0.0144(7) Uani 1 1 d . . . . .
H12 H 0.819606 0.471046 0.590797 0.017 Uiso 1 1 calc R U . . .
C13 C 0.7319(5) 0.4109(3) 0.49750(17) 0.0130(6) Uani 1 1 d . . . . .
H13 H 0.728608 0.330856 0.510705 0.016 Uiso 1 1 calc R U . . .
C4 C 0.2691(5) 0.3954(3) 0.17724(18) 0.0174(7) Uani 1 1 d . . . . .
H4A H 0.360072 0.449285 0.155991 0.026 Uiso 1 1 calc R U . . .
H4B H 0.189851 0.438430 0.209647 0.026 Uiso 1 1 calc R U . . .
H4C H 0.184227 0.359922 0.141351 0.026 Uiso 1 1 calc R U . . .
C14 C 0.6799(5) 0.4431(3) 0.42896(17) 0.0115(6) Uani 1 1 d . . . . .
C8 C 0.6117(5) 0.5983(3) 0.34501(18) 0.0144(7) Uani 1 1 d . . . . .
H8 H 0.616231 0.678079 0.331409 0.017 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 Br1 2.6289(4) . ?
Re1 N4 2.142(3) . ?
Re1 N5 2.275(3) . ?
Re1 C3 1.936(4) . ?
Re1 C1 1.907(4) . ?
Re1 C2 1.930(3) . ?
O2 C2 1.144(4) . ?
O1 C1 1.148(4) . ?
O3 C3 1.113(4) . ?
N4 N3 1.354(4) . ?
N4 C5 1.319(5) . ?
N2 N1 1.354(4) . ?
N2 N3 1.294(4) . ?
N1 C5 1.340(4) . ?
N1 C4 1.469(4) . ?
N5 C6 1.345(4) . ?
N5 C14 1.383(4) . ?
C5 C6 1.461(5) . ?
C9 C10 1.414(5) . ?
C9 C14 1.432(5) . ?
C9 C8 1.409(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.363(5) . ?
C6 C7 1.400(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.419(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.358(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.365(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.414(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C8 H8 0.9500 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Re1 Br1 85.45(8) . . ?
N4 Re1 N5 73.78(11) . . ?
N5 Re1 Br1 80.60(7) . . ?
C3 Re1 Br1 176.40(10) . . ?
C3 Re1 N4 94.07(12) . . ?
C3 Re1 N5 95.83(12) . . ?
C1 Re1 Br1 96.06(10) . . ?
C1 Re1 N4 94.69(13) . . ?
C1 Re1 N5 168.17(12) . . ?
C1 Re1 C3 87.53(14) . . ?
C1 Re1 C2 87.69(14) . . ?
C2 Re1 Br1 91.65(10) . . ?
C2 Re1 N4 176.42(12) . . ?
C2 Re1 N5 103.70(12) . . ?
C2 Re1 C3 88.69(14) . . ?
N3 N4 Re1 135.0(2) . . ?
C5 N4 Re1 117.3(2) . . ?
C5 N4 N3 107.6(3) . . ?
N3 N2 N1 107.3(3) . . ?
N2 N1 C4 119.7(3) . . ?
C5 N1 N2 108.1(3) . . ?
C5 N1 C4 131.8(3) . . ?
N2 N3 N4 109.4(3) . . ?
C6 N5 Re1 114.6(2) . . ?
C6 N5 C14 116.8(3) . . ?
C14 N5 Re1 127.4(2) . . ?
O3 C3 Re1 176.9(3) . . ?
N4 C5 N1 107.6(3) . . ?
N4 C5 C6 119.5(3) . . ?
N1 C5 C6 132.9(3) . . ?
O1 C1 Re1 176.9(3) . . ?
O2 C2 Re1 177.8(3) . . ?
C10 C9 C14 119.6(3) . . ?
C8 C9 C10 121.8(3) . . ?
C8 C9 C14 118.6(3) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.5(3) . . ?
C11 C10 H10 119.7 . . ?
N5 C6 C5 113.3(3) . . ?
N5 C6 C7 124.8(3) . . ?
C7 C6 C5 121.9(3) . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.8(3) . . ?
C12 C11 H11 120.1 . . ?
C6 C7 H7 120.7 . . ?
C8 C7 C6 118.6(3) . . ?
C8 C7 H7 120.7 . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.2(3) . . ?
C13 C12 H12 119.4 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.4(3) . . ?
C14 C13 H13 119.8 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N5 C14 C9 121.0(3) . . ?
N5 C14 C13 120.6(3) . . ?
C13 C14 C9 118.4(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 C9 119.8(3) . . ?
C7 C8 H8 120.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 N4 N3 N2 176.0(2) . . . . ?
Re1 N4 C5 N1 -176.6(2) . . . . ?
Re1 N4 C5 C6 2.7(4) . . . . ?
Re1 N5 C6 C5 13.4(3) . . . . ?
Re1 N5 C6 C7 -163.4(3) . . . . ?
Re1 N5 C14 C9 159.6(2) . . . . ?
Re1 N5 C14 C13 -22.9(4) . . . . ?
N4 C5 C6 N5 -11.1(4) . . . . ?
N4 C5 C6 C7 165.8(3) . . . . ?
N2 N1 C5 N4 -0.6(4) . . . . ?
N2 N1 C5 C6 -179.7(3) . . . . ?
N1 N2 N3 N4 0.2(4) . . . . ?
N1 C5 C6 N5 167.9(3) . . . . ?
N1 C5 C6 C7 -15.2(6) . . . . ?
N3 N4 C5 N1 0.7(4) . . . . ?
N3 N4 C5 C6 180.0(3) . . . . ?
N3 N2 N1 C5 0.3(4) . . . . ?
N3 N2 N1 C4 -173.9(3) . . . . ?
N5 C6 C7 C8 1.1(5) . . . . ?
C5 N4 N3 N2 -0.6(4) . . . . ?
C5 C6 C7 C8 -175.5(3) . . . . ?
C9 C10 C11 C12 0.4(5) . . . . ?
C10 C9 C14 N5 -178.6(3) . . . . ?
C10 C9 C14 C13 3.7(5) . . . . ?
C10 C9 C8 C7 -175.0(3) . . . . ?
C10 C11 C12 C13 1.6(5) . . . . ?
C6 N5 C14 C9 -7.2(4) . . . . ?
C6 N5 C14 C13 170.4(3) . . . . ?
C6 C7 C8 C9 -5.0(5) . . . . ?
C11 C12 C13 C14 -0.8(5) . . . . ?
C12 C13 C14 N5 -179.4(3) . . . . ?
C12 C13 C14 C9 -1.8(5) . . . . ?
C4 N1 C5 N4 172.6(3) . . . . ?
C4 N1 C5 C6 -6.5(6) . . . . ?
C14 N5 C6 C5 -178.1(3) . . . . ?
C14 N5 C6 C7 5.0(5) . . . . ?
C14 C9 C10 C11 -3.1(5) . . . . ?
C14 C9 C8 C7 2.8(5) . . . . ?
C8 C9 C10 C11 174.7(3) . . . . ?
C8 C9 C14 N5 3.5(5) . . . . ?
C8 C9 C14 C13 -174.1(3) . . . . ?

_olex2_exptl_crystal_mounting_method 
'mounted on a glass fibre using silicon oil'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.634
_oxdiff_exptl_absorpt_empirical_full_min 0.757

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mxm545rm
_audit_block_doi                 10.5517/ccdc.csd.cc2dlrh8
_database_code_depnum_ccdc_archive 'CCDC 2222560'
loop_
_audit_author_name
_audit_author_address
'Lee Cameron'
;Curtin University
Australia
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C10 H7 Br N5 O3 Re'
_chemical_formula_sum            'C10 H7 Br N5 O3 Re'
_chemical_formula_weight         511.32
_exptl_crystal_recrystallization_method 
'grown from the slow evaporation of acetone from an acetone and water solution'
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            'clear light yellow'
_diffrn_ambient_temperature      100.00(10)
_chemical_oxdiff_formula         'C10 H7 O3 N5 Br Re'
_chemical_oxdiff_usercomment     'Lee Cameron'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_chemical_absolute_configuration .
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.52910(10)
_cell_length_b                   8.4564(2)
_cell_length_c                   13.0106(2)
_cell_angle_alpha                85.7280(10)
_cell_angle_beta                 75.6990(10)
_cell_angle_gamma                76.0190(10)
_cell_volume                     675.38(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17079
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0970
_cell_measurement_theta_min      3.4780
_shelx_estimated_absorpt_T_max   0.568
_shelx_estimated_absorpt_T_min   0.123
_exptl_absorpt_coefficient_mu    21.227
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    2.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             472
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 -11 -5 0.0500
-10 6 -5 0.0500
-6 -1 18 0.0500
0 -3 -21 0.0010
0 -13 13 0.0190
0 14 12 0.0180
1 2 21 0.0320
11 -3 5 0.0940

_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-9.9806 -10.9772 -4.9408 -0.7138 0.7212 2.5867
-9.9880 5.9964 -5.0105 -1.0746 2.7055 0.1183
-5.9996 -0.9673 17.5008 1.7646 1.9563 1.1521
0.2103 -3.1245 -21.4252 -2.3454 -1.3165 -0.0040
0.0003 -12.9629 12.5461 1.6855 -0.9869 2.1396
-0.0115 13.8954 12.4358 1.1146 2.1529 -1.7663
1.3882 2.0239 21.1780 2.4019 0.8227 -0.0157
11.0851 -2.7027 5.0957 1.0580 -2.5599 -0.7153

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24085
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.845
_diffrn_reflns_theta_min         3.506
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     29.00 122.00   0.50    0.05    --   50.00  74.00 -30.70  186
  2  ω     23.00 119.00   0.50    0.05    --   45.98  77.00-120.00  192
  3  ω     27.00 122.00   0.50    0.05    --   50.00  77.00 -80.00  190
  4  ω     28.00 122.00   0.50    0.05    --   50.00  75.00  85.40  188
  5  ω     23.00 119.00   0.50    0.05    --   45.98  77.00 150.00  192
  6  ω     10.00  43.00   0.50    0.05    --   38.00  89.00 -16.32   66
  7  ω     -8.00  18.00   0.50    0.05    --   26.00 101.00 -30.36   52
  8  ω    -15.00  27.00   0.50    0.05    --   18.00  98.00 110.22   84
  9  ω     46.00 118.00   0.50    0.05    --   45.98 168.00  29.00  144
 10  ω     86.00 118.00   0.50    0.14    --  102.37  61.00-150.00   64
 11  ω     82.00 109.00   0.50    0.05    --   62.00  77.00-128.93   54
 12  ω     39.00  65.00   0.50    0.05    --   62.00  77.00-128.93   52
 13  ω     39.00  65.00   0.50    0.05    --   62.00  77.00   9.61   52
 14  ω     43.00  69.00   0.50    0.05    --   66.00  77.00  48.84   52
 15  ω     77.00 104.00   0.50    0.05    --   54.00  76.00 117.63   54
 16  ω     36.00  69.00   0.50    0.05    --   58.00  77.00 178.47   66
 17  ω     32.00  58.00   0.50    0.05    --   54.00  76.00 117.63   52
 18  ω     37.00  71.00   0.50    0.05    --   54.00  71.00 -14.93   68
 19  ω    135.00 168.00   0.50    0.14    --  102.37  61.00-150.00   66
 20  ω     46.00 152.00   0.50    0.14    --  102.37 168.00  29.00  212
 21  ω     80.00 175.00   0.50    0.14    --  102.37 115.00-114.00  190
 22  ω     30.00  66.00   0.50    0.14    --  102.37 -61.00 150.00   72
 23  ω     40.00 102.00   0.50    0.14    --  102.37 -77.00  30.00  124
 24  ω     31.00  68.00   0.50    0.14    --  102.37 -61.00 -60.00   74
 25  ω     34.00 103.00   0.50    0.14    --  102.37 -94.00 -60.00  138
 26  ω     36.00 103.00   0.50    0.14    --  102.37 -94.00   0.00  134
 27  ω     35.00 120.00   0.50    0.05    --   45.98-168.00  11.00  170
 28  ω     35.00 142.00   0.50    0.14    --  102.37-168.00  11.00  214
 29  ω     30.00 108.00   0.50    0.14    --  102.37-115.00 155.00  156
 30  ω      6.00  89.00   0.50    0.05    --   45.98-115.00 155.00  166
 31  ω    -77.00 -51.00   0.50    0.05    --  -74.00 -76.00-130.66   52
 32  ω    -98.00 -71.00   0.50    0.14    --  -94.00 -76.00-166.92   54
 33  ω    -78.00 -52.00   0.50    0.05    --  -74.00 -75.00 -75.64   52
 34  ω    -82.00 -56.00   0.50    0.14    --  -78.00 -74.00  14.22   52
 35  ω   -101.00 -72.00   0.50    0.14    --  -94.00 -75.00  51.18   58
 36  ω   -145.00-119.00   0.50    0.14    --  -94.00 -75.00  51.18   52
 37  ω    -95.00 -60.00   0.50    0.14    --  -82.00 -74.00 149.46   70
 38  ω   -160.00 -75.00   0.50    0.14    --  -98.00 -76.00 146.50  170
 39  ω   -161.00 -99.00   0.50    0.14    --  -90.00 -74.00 125.96  124
 40  ω    -93.00 -68.00   0.50    0.14    --  -90.00 -74.00 125.96   50
 41  ω   -104.00 -69.00   0.50    0.14    --  -90.00 -72.00 159.80   70
 42  ω   -155.00-108.00   0.50    0.14    --  -90.00 -72.00 159.80   94
 43  ω    -83.00 -57.00   0.50    0.14    --  -78.00 -73.00  72.71   52
 44  ω    -88.00 -54.00   0.50    0.05    --  -74.00 -71.00  89.35   68
 45  ω    -88.00 -62.00   0.50    0.14    --  -82.00 -71.00  40.03   52
 46  ω    -93.00 -67.00   0.50    0.14    --  -86.00 -72.00 -21.27   52
 47  ω    -88.00 -62.00   0.50    0.14    --  -82.00 -71.00 -24.47   52
 48  ω    -93.00 -67.00   0.50    0.14    --  -86.00 -70.00   1.14   52
 49  ω    -97.00 -66.00   0.50    0.14    --  -86.00 -71.00 -52.69   62
 50  ω    -87.00 -61.00   0.50    0.14    --  -82.00 -73.00-134.68   52
 51  ω    -92.00 -66.00   0.50    0.14    --  -86.00 -71.00-142.97   52
 52  ω    -76.00 -50.00   0.50    0.05    --  -70.00 -69.00-118.19   52
 53  ω    -82.00 -48.00   0.50    0.05    --  -66.00 -67.00 -59.87   68
 54  ω   -100.00 -74.00   0.50    0.14    --  -94.00 -69.00 -46.94   52
 55  ω   -159.00-114.00   0.50    0.14    --  -86.00 -70.00   1.14   90
 56  ω   -170.00 -88.00   0.50    0.14    -- -102.37 -66.00 -58.54  164
 57  ω    -84.00 -57.00   0.50    0.05    --  -74.00 -65.00-177.19   54
 58  ω   -159.00 -77.00   0.50    0.14    --  -94.00 -65.00  22.45  164
 59  ω    -84.00 -47.00   0.50    0.05    --  -66.00 -68.00  92.23   74
 60  ω    -83.00 -48.00   0.50    0.05    --  -66.00 -67.00 102.39   70
 61  ω    -75.00 -49.00   0.50    0.05    --  -66.00 -66.00 142.82   52
 62  ω   -160.00 -73.00   0.50    0.14    --  -90.00 -65.00  96.55  174
 63  ω   -147.00-121.00   0.50    0.14    --  -90.00 -64.00  86.06   52
 64  ω   -105.00 -72.00   0.50    0.14    --  -90.00 -64.00  86.06   66
 65  ω    -86.00 -60.00   0.50    0.14    --  -78.00 -64.00 -11.54   52
 66  ω   -110.00 -84.00   0.50    0.14    -- -102.37 -65.00  -5.13   52
 67  ω   -175.00-141.00   0.50    0.14    -- -102.37 -65.00  -5.13   68
 68  ω   -149.00-123.00   0.50    0.14    --  -90.00 -63.00-166.73   52
 69  ω   -104.00 -73.00   0.50    0.14    --  -90.00 -63.00-166.73   62
 70  ω    -92.00 -57.00   0.50    0.05    --  -74.00 -64.00-134.46   70
 71  ω   -167.00 -80.00   0.50    0.14    --  -94.00 -61.00-131.07  174
 72  ω   -158.00-122.00   0.50    0.14    --  -86.00 -61.00  55.60   72
 73  ω    -97.00 -70.00   0.50    0.14    --  -86.00 -61.00  55.60   54
 74  ω   -101.00 -74.00   0.50    0.14    --  -90.00 -59.00  43.82   54
 75  ω   -160.00-105.00   0.50    0.14    --  -90.00 -59.00  43.82  110
 76  ω   -104.00 -69.00   0.50    0.14    --  -86.00 -62.00  93.33   70
 77  ω    -86.00 -59.00   0.50    0.05    --  -74.00 -63.00 154.43   54
 78  ω    -76.00 -50.00   0.50    0.05    --  -66.00 -60.00 167.38   52
 79  ω   -160.00-108.00   0.50    0.14    --  -90.00 -46.00 175.23  104
 80  ω   -116.00 -84.00   0.50    0.14    --  -98.00 -54.00 -47.64   64
 81  ω   -108.00 -67.00   0.50    0.14    --  -82.00 -59.00-107.11   82
 82  ω   -166.00 -79.00   0.50    0.14    --  -94.00 -57.00-114.52  174
 83  ω   -117.00 -46.00   0.50    0.05    --  -45.98-168.00  11.00  142
 84  ω   -152.00 -46.00   0.50    0.14    -- -102.37-168.00  11.00  212
 85  ω   -175.00 -80.00   0.50    0.14    -- -102.37-115.00 155.00  190
 86  ω   -117.00 -31.00   0.50    0.05    --  -45.98 -57.00 120.00  172
 87  ω   -118.00 -23.00   0.50    0.05    --  -45.98 -77.00 -60.00  190
 88  ω   -118.00 -23.00   0.50    0.05    --  -45.98 -77.00-150.00  190
 89  ω   -119.00 -33.00   0.50    0.05    --  -45.98 -37.00 -60.00  172
 90  ω   -120.00 -33.00   0.50    0.05    --  -45.98 -19.00 -30.00  174
 91  ω    -69.00 -38.00   0.50    0.14    -- -102.37  61.00 -90.00   62
 92  ω    -98.00 -32.00   0.50    0.14    -- -102.37 125.00-180.00  132
 93  ω    -72.00 -30.00   0.50    0.14    -- -102.37  61.00  30.00   84
 94  ω    -70.00 -32.00   0.50    0.14    -- -102.37  61.00  90.00   76
 95  ω   -120.00 -34.00   0.50    0.05    --  -45.98 168.00  29.00  172
 96  ω   -107.00 -75.00   0.50    0.14    -- -102.37 108.00 153.99   64
 97  ω    -65.00 -31.00   0.50    0.14    -- -102.37 108.00 153.99   68
 98  ω   -141.00 -34.00   0.50    0.14    -- -102.37 168.00  29.00  214
 99  ω   -108.00 -30.00   0.50    0.14    -- -102.37 115.00-114.00  156
100  ω    -89.00  -6.00   0.50    0.05    --  -45.98 115.00-114.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0384910000
_diffrn_orient_matrix_UB_12      -0.0207748000
_diffrn_orient_matrix_UB_13      0.1128758000
_diffrn_orient_matrix_UB_21      -0.2218133000
_diffrn_orient_matrix_UB_22      0.1169808000
_diffrn_orient_matrix_UB_23      0.0422073000
_diffrn_orient_matrix_UB_31      -0.1093196000
_diffrn_orient_matrix_UB_32      -0.1453904000
_diffrn_orient_matrix_UB_33      0.0203185000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2643
_reflns_number_total             2669
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.125
_refine_diff_density_min         -1.781
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.00077(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2669
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0278
_refine_ls_restrained_S_all      1.144
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0378P)²+3.0325P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0727
_refine_special_details          ?
_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.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C8(H8), C9(H9)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.38312(3) 0.70067(2) 0.73157(2) 0.01733(11) Uani 1 1 d . . . . .
Br1 Br 0.49876(8) 0.71830(7) 0.90721(4) 0.02287(14) Uani 1 1 d . . . . .
O2 O 0.5919(6) 0.9814(4) 0.6303(3) 0.0274(8) Uani 1 1 d . . . . .
O3 O 0.2676(7) 0.6820(5) 0.5224(4) 0.0327(9) Uani 1 1 d . . . . .
O1 O -0.0585(6) 0.9295(5) 0.8259(3) 0.0308(9) Uani 1 1 d . . . . .
N5 N 0.2876(7) 0.4755(5) 0.8044(3) 0.0180(8) Uani 1 1 d . . . . .
N4 N 0.6719(6) 0.5092(5) 0.6934(3) 0.0184(8) Uani 1 1 d . . . . .
N2 N 0.9682(6) 0.3428(5) 0.6438(3) 0.0185(8) Uani 1 1 d . . . . .
N3 N 0.8722(7) 0.4982(5) 0.6353(3) 0.0188(8) Uani 1 1 d . . . . .
N1 N 0.8433(7) 0.2515(5) 0.7034(3) 0.0201(8) Uani 1 1 d . . . . .
C3 C 0.3067(7) 0.6806(6) 0.5940(5) 0.0206(10) Uani 1 1 d . . . . .
C5 C 0.6577(8) 0.3592(6) 0.7345(4) 0.0188(9) Uani 1 1 d . . . . .
C7 C 0.4176(8) 0.1929(6) 0.8489(4) 0.0227(10) Uani 1 1 d . . . . .
H7 H 0.535252 0.100156 0.844679 0.027 Uiso 1 1 calc R U . . .
C10 C 0.0881(8) 0.4657(6) 0.8585(4) 0.0212(10) Uani 1 1 d . . . . .
H10 H -0.027172 0.560045 0.862272 0.025 Uiso 1 1 calc R U . . .
C6 C 0.4492(8) 0.3377(6) 0.7992(4) 0.0176(9) Uani 1 1 d . . . . .
C2 C 0.5094(8) 0.8788(7) 0.6697(4) 0.0238(11) Uani 1 1 d . . . . .
C8 C 0.2094(9) 0.1860(7) 0.9051(4) 0.0261(11) Uani 1 1 d . . . . .
H8 H 0.181834 0.088099 0.940365 0.031 Uiso 1 1 calc R U . . .
C9 C 0.0423(9) 0.3242(7) 0.9091(4) 0.0241(11) Uani 1 1 d . . . . .
H9 H -0.101829 0.321774 0.946231 0.029 Uiso 1 1 calc R U . . .
C4 C 1.1923(8) 0.2751(7) 0.5875(4) 0.0251(11) Uani 1 1 d . . . . .
H4A H 1.248889 0.359332 0.541177 0.038 Uiso 1 1 calc R U . . .
H4B H 1.196834 0.183275 0.544636 0.038 Uiso 1 1 calc R U . . .
H4C H 1.281494 0.237294 0.638965 0.038 Uiso 1 1 calc R U . . .
C1 C 0.1065(8) 0.8461(7) 0.7880(4) 0.0239(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 Br1 2.6023(6) . ?
Re1 N5 2.219(4) . ?
Re1 N4 2.146(4) . ?
Re1 C3 2.003(6) . ?
Re1 C2 1.920(6) . ?
Re1 C1 1.929(5) . ?
O2 C2 1.153(7) . ?
O3 C3 1.022(7) . ?
O1 C1 1.150(7) . ?
N5 C10 1.338(6) . ?
N5 C6 1.364(6) . ?
N4 N3 1.324(6) . ?
N4 C5 1.355(6) . ?
N2 N3 1.321(6) . ?
N2 N1 1.329(6) . ?
N2 C4 1.461(6) . ?
N1 C5 1.319(6) . ?
C5 C6 1.458(7) . ?
C7 H7 0.9500 . ?
C7 C6 1.377(7) . ?
C7 C8 1.388(8) . ?
C10 H10 0.9500 . ?
C10 C9 1.383(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.387(8) . ?
C9 H9 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Re1 Br1 84.52(10) . . ?
N4 Re1 Br1 84.77(11) . . ?
N4 Re1 N5 74.34(15) . . ?
C3 Re1 Br1 177.51(13) . . ?
C3 Re1 N5 95.25(17) . . ?
C3 Re1 N4 92.78(17) . . ?
C2 Re1 Br1 91.45(15) . . ?
C2 Re1 N5 171.37(18) . . ?
C2 Re1 N4 97.74(18) . . ?
C2 Re1 C3 88.5(2) . . ?
C2 Re1 C1 91.9(2) . . ?
C1 Re1 Br1 90.10(16) . . ?
C1 Re1 N5 95.72(19) . . ?
C1 Re1 N4 169.18(19) . . ?
C1 Re1 C3 92.4(2) . . ?
C10 N5 Re1 125.7(3) . . ?
C10 N5 C6 117.2(4) . . ?
C6 N5 Re1 117.0(3) . . ?
N3 N4 Re1 135.3(3) . . ?
N3 N4 C5 107.8(4) . . ?
C5 N4 Re1 116.9(3) . . ?
N3 N2 N1 115.2(4) . . ?
N3 N2 C4 122.3(4) . . ?
N1 N2 C4 122.5(4) . . ?
N2 N3 N4 104.0(4) . . ?
C5 N1 N2 101.9(4) . . ?
O3 C3 Re1 174.5(5) . . ?
N4 C5 C6 118.5(4) . . ?
N1 C5 N4 111.2(4) . . ?
N1 C5 C6 130.2(5) . . ?
C6 C7 H7 120.9 . . ?
C6 C7 C8 118.3(5) . . ?
C8 C7 H7 120.9 . . ?
N5 C10 H10 118.6 . . ?
N5 C10 C9 122.9(5) . . ?
C9 C10 H10 118.6 . . ?
N5 C6 C5 112.9(4) . . ?
N5 C6 C7 123.4(5) . . ?
C7 C6 C5 123.7(4) . . ?
O2 C2 Re1 177.4(4) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 C7 119.0(5) . . ?
C9 C8 H8 120.5 . . ?
C10 C9 C8 119.2(5) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O1 C1 Re1 177.0(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 N5 C10 C9 -174.8(4) . . . . ?
Re1 N5 C6 C5 -6.7(5) . . . . ?
Re1 N5 C6 C7 174.1(4) . . . . ?
Re1 N4 N3 N2 -178.6(3) . . . . ?
Re1 N4 C5 N1 178.5(3) . . . . ?
Re1 N4 C5 C6 1.2(6) . . . . ?
N5 C10 C9 C8 0.6(8) . . . . ?
N4 C5 C6 N5 3.8(6) . . . . ?
N4 C5 C6 C7 -177.1(5) . . . . ?
N2 N1 C5 N4 0.7(5) . . . . ?
N2 N1 C5 C6 177.6(5) . . . . ?
N3 N4 C5 N1 -0.6(5) . . . . ?
N3 N4 C5 C6 -178.0(4) . . . . ?
N3 N2 N1 C5 -0.6(5) . . . . ?
N1 N2 N3 N4 0.2(5) . . . . ?
N1 C5 C6 N5 -173.0(5) . . . . ?
N1 C5 C6 C7 6.2(8) . . . . ?
C5 N4 N3 N2 0.2(5) . . . . ?
C7 C8 C9 C10 -1.0(8) . . . . ?
C10 N5 C6 C5 177.3(4) . . . . ?
C10 N5 C6 C7 -1.9(7) . . . . ?
C6 N5 C10 C9 0.8(7) . . . . ?
C6 C7 C8 C9 0.0(8) . . . . ?
C8 C7 C6 N5 1.5(8) . . . . ?
C8 C7 C6 C5 -177.6(5) . . . . ?
C4 N2 N3 N4 177.4(4) . . . . ?
C4 N2 N1 C5 -177.7(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.783
_oxdiff_exptl_absorpt_empirical_full_min 0.743

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_mxm544vm
_audit_block_doi                 10.5517/ccdc.csd.cc2dlrg7
_database_code_depnum_ccdc_archive 'CCDC 2222559'
loop_
_audit_author_name
_audit_author_address
'Lee Cameron'
;Curtin University
Australia
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_mxm544vm            
;
PROBLEM: Short Inter D...A Contact  O2       ..O3       .       2.81 Ang.
RESPONSE: Due to the crystal packing, O2 and O3 display a slight overlap at the edge of their orbitals. No hydrogen bonding is present due to O2 and O3 being carbonyls bound to C2 and C3 respectively.
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C10 H7 Br N5 O3 Re'
_chemical_formula_sum            'C10 H7 Br N5 O3 Re'
_chemical_formula_weight         511.32
_exptl_crystal_recrystallization_method 
'grown from the slow evaporation of acetone from an acetone and water solution'
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            'clear light yellow'
_diffrn_ambient_temperature      100.00(10)
_chemical_oxdiff_formula         'H7 C10 O3 N5 Br1 Re1'
_chemical_oxdiff_usercomment     'Lee Cameron'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_chemical_absolute_configuration .
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'

_cell_length_a                   6.92166(4)
_cell_length_b                   11.90491(10)
_cell_length_c                   16.62188(11)
_cell_angle_alpha                90
_cell_angle_beta                 100.1458(6)
_cell_angle_gamma                90
_cell_volume                     1348.253(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    29702
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.9960
_cell_measurement_theta_min      3.6820
_shelx_estimated_absorpt_T_max   0.186
_shelx_estimated_absorpt_T_min   0.073
_exptl_absorpt_coefficient_mu    21.266
_exptl_absorpt_correction_T_max  0.321
_exptl_absorpt_correction_T_min  0.053
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.519
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             944
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 2 10 0.1273
3 1 -8 0.0980
-3 -4 7 0.0741
2 -4 -8 0.0828
3 -3 -8 0.0750
-4 -2 5 0.0649
3 -4 -6 0.0622
-4 4 0 0.0642
4 -4 0 0.0499
1 0 -11 0.0981
-1 -6 6 0.0751
-3 3 8 0.1005
-4 1 6 0.0732
4 2 -5 0.0941
-4 1 3 0.0601
-4 4 3 0.0725
4 2 -2 0.0883
4 -4 -3 0.0530
-4 -2 2 0.0631
-4 0 -1 0.0648
-3 2 -7 0.0827
3 -3 6 0.0976
-3 0 -7 0.0825
1 7 1 0.0808
0 -7 5 0.0678
0 -3 10 0.1112
0 -1 -10 0.0929

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.119
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.7073 2.0287 10.4155 -0.8796 -0.3106 -0.3603
3.4980 1.2545 -7.9239 0.5528 0.8038 -0.2198
-3.3487 -3.5168 6.5916 -0.4855 -0.7065 0.5149
2.4052 -4.3670 -7.6933 0.4788 0.6949 0.5365
2.8424 -3.1316 -8.2207 0.5275 0.7661 0.3672
-4.1108 -2.0226 5.0013 -0.2623 -0.8850 0.3848
3.3755 -3.9638 -5.8492 0.2593 0.8723 0.4146
-3.9176 3.5375 -0.1851 0.3221 -0.9119 -0.2544
3.7539 -4.0674 0.0858 -0.3143 0.8900 0.3302
0.9938 -0.0659 -10.7830 0.9376 0.3316 0.1046
-1.3348 -6.4040 5.5977 -0.5727 -0.2018 0.7946
-2.8520 3.1063 8.2243 -0.5278 -0.7676 -0.3636
-4.0902 1.0048 5.9108 -0.2845 -0.9586 -0.0090
4.0643 2.3904 -4.8323 0.2570 0.8649 -0.4311
-4.3938 1.4459 2.8516 0.0256 -0.9996 -0.0091
-3.7720 4.0635 3.0618 0.0241 -0.9284 -0.3709
4.2681 2.4051 -1.9416 -0.0221 0.8763 -0.4813
3.6993 -4.2513 -3.0606 -0.0238 0.9171 0.3980
-4.3967 -1.5645 2.1987 0.0235 -0.9254 0.3783
-4.3418 -0.4954 -0.7968 0.3196 -0.9048 0.2813
-2.7676 2.1943 -6.6311 0.8226 -0.5660 -0.0545
2.5886 -3.2624 6.3362 -0.8070 0.5551 0.2014
-2.9311 0.2828 -6.7972 0.8078 -0.5560 0.1959
0.8699 7.4898 1.2256 -0.0086 0.0034 -1.0000
0.4287 -6.6901 5.0332 -0.6305 0.1865 0.7535
0.0356 -3.2548 9.6193 -0.9599 -0.0249 0.2791
-0.4775 -0.5781 -10.3315 0.9720 0.0247 0.2336

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38508
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.509
_diffrn_reflns_theta_min         4.593
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     24.00  68.00   0.50    0.05    --   46.32  77.00 -60.00   88
  2  ω     24.00 118.00   0.50    0.05    --   46.32  77.00 120.00  188
  3  ω     32.00 118.00   0.50    0.05    --   46.32  57.00  90.00  172
  4  ω     34.00 121.00   0.50    0.05    --   46.32  18.00  36.00  174
  5  ω     24.00 118.00   0.50    0.05    --   46.32  77.00  90.00  188
  6  ω     24.00 118.00   0.50    0.05    --   46.32  77.00 150.00  188
  7  ω   -105.00 -30.00   0.50    0.05    -- -102.29  77.00 150.00  150
  8  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 150.00   82
  9  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 120.00   82
 10  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 -30.00   82
 11  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00-120.00   82
 12  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00-180.00   82
 13  ω     80.00 174.00   0.50    0.05    --  102.29  77.00 150.00  188
 14  ω     86.00 174.00   0.50    0.05    --  102.29  61.00 120.00  176
 15  ω     90.00 174.00   0.50    0.05    --  102.29  45.00 150.00  168
 16  ω     80.00 174.00   0.50    0.05    --  102.29  77.00 120.00  188
 17  ω     80.00 174.00   0.50    0.05    --  102.29  77.00  60.00  188
 18  ω     80.00 174.00   0.50    0.05    --  102.29  77.00  30.00  188
 19  ω     89.00 177.00   0.50    0.05    --  102.29  18.00  36.00  176
 20  ω     90.00 174.00   0.50    0.05    --  102.29  45.00-150.00  168
 21  ω    -28.00  26.00   0.50    0.05    --   46.32 -18.00-131.00  108
 22  ω    -26.00  43.00   0.50    0.05    --   46.32 -38.00  90.00  138
 23  ω     30.00 105.00   0.50    0.05    --  102.29 -77.00  60.00  150
 24  ω     30.00  71.00   0.50    0.05    --  102.29 -61.00-150.00   82
 25  ω     13.00  94.00   0.50    0.05    --   46.32-125.00-180.00  162
 26  ω     30.00 111.00   0.50    0.05    --  102.29-125.00-150.00  162
 27  ω    -26.00  29.00   0.50    0.05    --  -46.32  18.00  36.00  110
 28  ω    -43.00  27.00   0.50    0.05    --  -46.32  38.00 -30.00  140
 29  ω   -121.00 -33.00   0.50    0.05    --  -46.32 -18.00-131.00  176
 30  ω   -119.00 -33.00   0.50    0.05    --  -46.32 -38.00-180.00  172
 31  ω   -174.00 -79.00   0.50    0.05    -- -102.29 -78.00-152.37  190
 32  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -77.00 120.00  188
 33  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -77.00 122.94  188
 34  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -75.00  89.57  188
 35  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -76.00 139.99  188
 36  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -75.00 148.98  188
 37  ω   -174.00 -82.00   0.50    0.05    -- -102.29 -70.00 178.81  184
 38  ω   -174.00 -84.00   0.50    0.05    -- -102.29 -67.00 154.95  180
 39  ω   -174.00 -83.00   0.50    0.05    -- -102.29 -69.00 119.48  182
 40  ω   -174.00 -84.00   0.50    0.05    -- -102.29 -67.00 164.37  180
 41  ω   -174.00 -82.00   0.50    0.05    -- -102.29 -70.00  70.52  184
 42  ω   -174.00 -85.00   0.50    0.05    -- -102.29 -63.00  85.75  178
 43  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00  90.00  176
 44  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00 124.85  176
 45  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00-164.12  176
 46  ω   -174.00 -84.00   0.50    0.05    -- -102.29 -66.00-177.27  180
 47  ω   -174.00 -83.00   0.50    0.05    -- -102.29 -68.00-140.33  182
 48  ω   -111.00 -30.00   0.50    0.05    -- -102.29 125.00 150.00  162
 49  ω   -174.00 -89.00   0.50    0.05    -- -102.29 -52.00 136.41  170
 50  ω   -174.00 -89.00   0.50    0.05    -- -102.29 -52.00 129.41  170
 51  ω   -174.00 -88.00   0.50    0.05    -- -102.29 -53.00 105.83  172
 52  ω   -177.00 -89.00   0.50    0.05    -- -102.29 -18.00-131.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0590219000
_diffrn_orient_matrix_UB_12      0.0208523000
_diffrn_orient_matrix_UB_13      -0.0925206000
_diffrn_orient_matrix_UB_21      0.2129815000
_diffrn_orient_matrix_UB_22      -0.0224863000
_diffrn_orient_matrix_UB_23      -0.0109805000
_diffrn_orient_matrix_UB_31      -0.0479857000
_diffrn_orient_matrix_UB_32      -0.1257505000
_diffrn_orient_matrix_UB_33      -0.0133593000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2750
_reflns_number_total             2757
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.400
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2757
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0270
_refine_ls_restrained_S_all      1.209
_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)+(0.0294P)²+4.8808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0705
_refine_special_details          ?
_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.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C7(H7), C8(H8)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.72815(3) 0.78694(2) 0.39337(2) 0.02475(10) Uani 1 1 d . . . . .
Br02 Br 1.00509(7) 0.70884(4) 0.31927(3) 0.03100(14) Uani 1 1 d . . . . .
O1 O 0.4209(5) 0.8724(3) 0.4895(2) 0.0316(7) Uani 1 1 d . . . . .
O3 O 0.7837(6) 1.0262(3) 0.3331(2) 0.0398(8) Uani 1 1 d . . . . .
N3 N 0.4254(6) 0.7943(3) 0.2209(3) 0.0288(9) Uani 1 1 d . . . . .
N4 N 0.5246(5) 0.7389(3) 0.2862(2) 0.0237(7) Uani 1 1 d . . . . .
O2 O 1.0442(6) 0.8216(4) 0.5461(2) 0.0444(10) Uani 1 1 d . . . . .
N5 N 0.6663(5) 0.6069(3) 0.4088(2) 0.0252(8) Uani 1 1 d . . . . .
N1 N 0.3417(5) 0.6217(3) 0.2109(2) 0.0250(8) Uani 1 1 d . . . . .
N2 N 0.3135(6) 0.7238(3) 0.1749(3) 0.0276(8) Uani 1 1 d . . . . .
C1 C 0.5301(7) 0.8391(4) 0.4529(3) 0.0271(9) Uani 1 1 d . . . . .
C3 C 0.7646(7) 0.9374(5) 0.3580(3) 0.0332(11) Uani 1 1 d . . . . .
C5 C 0.4730(6) 0.6322(4) 0.2797(3) 0.0251(9) Uani 1 1 d . . . . .
C10 C 0.7448(7) 0.5442(4) 0.4733(3) 0.0306(10) Uani 1 1 d . . . . .
H10 H 0.818906 0.580358 0.519645 0.037 Uiso 1 1 calc R U . . .
C4 C 0.2274(7) 0.5254(4) 0.1744(3) 0.0306(10) Uani 1 1 d . . . . .
H4A H 0.135686 0.549934 0.125802 0.046 Uiso 1 1 calc R U . . .
H4B H 0.153719 0.493356 0.214147 0.046 Uiso 1 1 calc R U . . .
H4C H 0.316177 0.468480 0.158852 0.046 Uiso 1 1 calc R U . . .
C2 C 0.9243(7) 0.8094(5) 0.4899(3) 0.0344(11) Uani 1 1 d . . . . .
C6 C 0.5544(6) 0.5534(4) 0.3442(3) 0.0255(9) Uani 1 1 d . . . . .
C9 C 0.7220(7) 0.4285(5) 0.4751(3) 0.0333(11) Uani 1 1 d . . . . .
H9 H 0.779643 0.386885 0.521923 0.040 Uiso 1 1 calc R U . . .
C7 C 0.5269(7) 0.4380(4) 0.3413(3) 0.0312(10) Uani 1 1 d . . . . .
H7 H 0.450108 0.403516 0.294872 0.037 Uiso 1 1 calc R U . . .
C8 C 0.6142(7) 0.3738(5) 0.4078(3) 0.0345(11) Uani 1 1 d . . . . .
H8 H 0.600516 0.294408 0.407350 0.041 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 Br02 2.6245(5) . ?
Re1 N4 2.145(4) . ?
Re1 N5 2.209(4) . ?
Re1 C1 1.929(5) . ?
Re1 C3 1.915(6) . ?
Re1 C2 1.929(5) . ?
O1 C1 1.123(6) . ?
O3 C3 1.152(7) . ?
N3 N4 1.350(6) . ?
N3 N2 1.297(6) . ?
N4 C5 1.320(6) . ?
O2 C2 1.145(6) . ?
N5 C10 1.341(6) . ?
N5 C6 1.367(6) . ?
N1 N2 1.353(5) . ?
N1 C5 1.335(6) . ?
N1 C4 1.462(6) . ?
C5 C6 1.460(6) . ?
C10 H10 0.9500 . ?
C10 C9 1.387(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 C7 1.386(7) . ?
C9 H9 0.9500 . ?
C9 C8 1.391(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.392(7) . ?
C8 H8 0.9500 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Re1 Br02 86.72(10) . . ?
N4 Re1 N5 74.07(15) . . ?
N5 Re1 Br02 83.30(10) . . ?
C1 Re1 Br02 176.85(14) . . ?
C1 Re1 N4 95.15(16) . . ?
C1 Re1 N5 94.76(17) . . ?
C3 Re1 Br02 92.34(15) . . ?
C3 Re1 N4 95.56(18) . . ?
C3 Re1 N5 168.92(18) . . ?
C3 Re1 C1 90.0(2) . . ?
C3 Re1 C2 90.8(2) . . ?
C2 Re1 Br02 88.52(15) . . ?
C2 Re1 N4 172.2(2) . . ?
C2 Re1 N5 99.2(2) . . ?
C2 Re1 C1 89.3(2) . . ?
N2 N3 N4 108.9(4) . . ?
N3 N4 Re1 134.8(3) . . ?
C5 N4 Re1 117.0(3) . . ?
C5 N4 N3 108.2(4) . . ?
C10 N5 Re1 125.0(3) . . ?
C10 N5 C6 117.5(4) . . ?
C6 N5 Re1 117.1(3) . . ?
N2 N1 C4 119.7(4) . . ?
C5 N1 N2 108.6(4) . . ?
C5 N1 C4 131.7(4) . . ?
N3 N2 N1 107.2(4) . . ?
O1 C1 Re1 177.0(4) . . ?
O3 C3 Re1 176.9(4) . . ?
N4 C5 N1 107.1(4) . . ?
N4 C5 C6 119.6(4) . . ?
N1 C5 C6 133.2(4) . . ?
N5 C10 H10 118.7 . . ?
N5 C10 C9 122.6(5) . . ?
C9 C10 H10 118.7 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O2 C2 Re1 178.2(5) . . ?
N5 C6 C5 111.7(4) . . ?
N5 C6 C7 123.0(4) . . ?
C7 C6 C5 125.3(4) . . ?
C10 C9 H9 120.2 . . ?
C10 C9 C8 119.7(5) . . ?
C8 C9 H9 120.2 . . ?
C6 C7 H7 120.7 . . ?
C6 C7 C8 118.6(5) . . ?
C8 C7 H7 120.7 . . ?
C9 C8 C7 118.5(5) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 N4 C5 N1 177.7(3) . . . . ?
Re1 N4 C5 C6 0.0(5) . . . . ?
Re1 N5 C10 C9 -171.0(3) . . . . ?
Re1 N5 C6 C5 -8.1(5) . . . . ?
Re1 N5 C6 C7 170.9(3) . . . . ?
N3 N4 C5 N1 -0.3(5) . . . . ?
N3 N4 C5 C6 -178.0(4) . . . . ?
N4 N3 N2 N1 -0.2(5) . . . . ?
N4 C5 C6 N5 5.4(6) . . . . ?
N4 C5 C6 C7 -173.6(4) . . . . ?
N5 C10 C9 C8 0.1(7) . . . . ?
N5 C6 C7 C8 1.2(7) . . . . ?
N1 C5 C6 N5 -171.6(4) . . . . ?
N1 C5 C6 C7 9.4(8) . . . . ?
N2 N3 N4 Re1 -177.2(3) . . . . ?
N2 N3 N4 C5 0.3(5) . . . . ?
N2 N1 C5 N4 0.2(5) . . . . ?
N2 N1 C5 C6 177.4(4) . . . . ?
C5 N1 N2 N3 0.0(5) . . . . ?
C5 C6 C7 C8 -179.9(4) . . . . ?
C10 N5 C6 C5 178.0(4) . . . . ?
C10 N5 C6 C7 -3.0(6) . . . . ?
C10 C9 C8 C7 -1.9(7) . . . . ?
C4 N1 N2 N3 177.3(4) . . . . ?
C4 N1 C5 N4 -176.7(4) . . . . ?
C4 N1 C5 C6 0.6(8) . . . . ?
C6 N5 C10 C9 2.3(7) . . . . ?
C6 C7 C8 C9 1.3(7) . . . . ?

_olex2_exptl_crystal_mounting_method 
'mounted on a glass fibre using silicon oil'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.603
_oxdiff_exptl_absorpt_empirical_full_min 0.724

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mxm548rm
_audit_block_doi                 10.5517/ccdc.csd.cc2dlrd5
_database_code_depnum_ccdc_archive 'CCDC 2222557'
loop_
_audit_author_name
_audit_author_address
'Lee Cameron'
;Curtin University
Australia
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
;
_audit_creation_date             2022-11-28
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C33 H25 Ir N7, F6 P'
_chemical_formula_sum            'C33 H25 F6 Ir N7 P'
_chemical_formula_weight         856.77
_exptl_crystal_recrystallization_method 
'grown from the slow evaporation of acetone from an acetone and water solution'
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            'clear orange'
_diffrn_ambient_temperature      99.9(3)
_chemical_oxdiff_formula         'C33 H25 F6 Ir1 N7 P1'
_chemical_oxdiff_usercomment     'Lee for Max/Mark'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.39052(9)
_cell_length_b                   34.3744(4)
_cell_length_c                   11.32559(12)
_cell_angle_alpha                90
_cell_angle_beta                 109.5770(12)
_cell_angle_gamma                90
_cell_volume                     3077.68(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    37341
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      74.9560
_cell_measurement_theta_min      2.5620
_shelx_estimated_absorpt_T_max   0.273
_shelx_estimated_absorpt_T_min   0.185
_exptl_absorpt_coefficient_mu    9.548
_exptl_absorpt_correction_T_max  0.518
_exptl_absorpt_correction_T_min  0.095
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -3 -6 0.1169
0 20 -3 0.0901
-2 20 0 0.0894
-4 1 6 0.1312
-4 -8 6 0.1277
0 -20 3 0.1010
2 -20 -1 0.0968
5 3 -4 0.1224
-1 -7 -6 0.0799
-3 -8 -3 0.0745
-5 -1 5 0.1338
-1 4 5 0.1277
2 6 2 0.1002

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.184
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.4477 -3.0559 -5.8910 -0.0316 0.1354 -0.9903
0.3357 19.6765 -3.4044 0.2206 -0.9197 -0.3248
-1.9911 20.4541 -0.2005 0.2279 -0.9522 0.2036
-4.3858 1.2524 6.0708 0.0114 -0.0512 0.9986
-3.5816 -7.7460 6.2614 -0.0889 0.3678 0.9257
0.1713 -20.3331 2.7788 -0.2276 0.9495 0.2158
2.4806 -19.7756 -0.5986 -0.2200 0.9197 -0.3253
5.2564 3.3503 -3.8568 -0.4309 -0.1025 -0.8966
-0.8901 -7.1878 -6.0566 0.8750 0.2100 -0.4362
-3.4811 -7.8563 -3.1592 0.9683 0.2319 0.0930
-4.8832 -1.4772 5.2404 0.2022 0.0476 0.9782
-1.3215 3.9741 5.2047 -0.4016 -0.1242 0.5969
1.7878 5.6405 2.1385 -0.5653 -0.1827 -0.0021

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            57719
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.453
_diffrn_reflns_theta_min         2.571
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     68.00 118.00   0.50    0.05    --   46.38 134.00 116.00  100
  2  ω     97.00 122.00   0.50    0.05    --  102.22 134.00 116.00   50
  3  ω     66.00 118.00   0.50    0.05    --   46.38 136.00 -64.00  104
  4  ω     74.00 119.00   0.50    0.05    --  102.22 125.00 -30.00   90
  5  ω     66.00 175.00   0.50    0.05    --  102.22 136.00 -64.00  218
  6  ω    126.00 173.00   0.50    0.05    --  102.22 125.00 -30.00   94
  7  ω     70.00 105.00   0.50    0.05    --  102.22 -94.00  60.00   70
  8  ω     30.00 118.00   0.50    0.05    --  102.22-134.00  49.00  176
  9  ω     18.00  99.00   0.50    0.05    --   46.38-134.00  49.00  162
 10  ω     63.00 108.00   0.50    0.05    --  102.22-110.00 -60.51   90
 11  ω     30.00 120.00   0.50    0.05    --  102.22-136.00-129.00  180
 12  ω     19.00 100.00   0.50    0.05    --   46.38-136.00-129.00  162
 13  ω     35.00 108.00   0.50    0.05    --  102.22-108.00  58.47  146
 14  ω     32.00  61.00   0.50    0.05    --  102.22 -77.00  60.00   58
 15  ω     66.00  99.00   0.50    0.05    --  102.22 -77.00  60.00   66
 16  ω     37.00  62.00   0.50    0.05    --  102.22 -61.00 120.00   50
 17  ω     31.00  64.00   0.50    0.05    --  102.22 -61.00  90.00   66
 18  ω     32.00  65.00   0.50    0.05    --  102.22 -77.00  30.00   66
 19  ω     55.00  81.00   0.50    0.05    --  102.22 -77.00   0.00   52
 20  ω    -28.00  26.00   0.50    0.05    --   46.38 -19.00  30.00  108
 21  ω     35.00  71.00   0.50    0.05    --  102.22 -61.00 -90.00   72
 22  ω     43.00  69.00   0.50    0.05    --  102.22 -61.00-150.00   52
 23  ω   -100.00 -19.00   0.50    0.05    --  -46.38 136.00 -64.00  162
 24  ω   -120.00 -29.00   0.50    0.05    -- -102.22 136.00 -64.00  182
 25  ω    -99.00 -18.00   0.50    0.05    --  -46.38 134.00 116.00  162
 26  ω   -118.00 -29.00   0.50    0.05    -- -102.22 134.00 116.00  178
 27  ω   -112.00 -29.00   0.50    0.05    -- -102.22 125.00 -90.00  166
 28  ω   -106.00 -56.00   0.50    0.05    -- -102.22 107.00 -82.02  100
 29  ω    -71.00 -29.00   0.50    0.05    -- -102.22  61.00  90.00   84
 30  ω    -57.00 -32.00   0.50    0.05    -- -102.22  61.00 150.00   50
 31  ω    -67.00 -32.00   0.50    0.05    -- -102.22  61.00 -60.00   70
 32  ω    -64.00 -31.00   0.50    0.05    -- -102.22  61.00 -90.00   66
 33  ω    -26.00  29.00   0.50    0.05    --  -46.38  19.00  90.00  110
 34  ω    -26.00  29.00   0.50    0.05    --  -46.38  19.00 -90.00  110
 35  ω   -118.00 -24.00   0.50    0.05    --  -46.38 -77.00 150.00  188
 36  ω   -174.00 -94.00   0.50    0.05    -- -102.22 -60.00  59.67  160
 37  ω   -175.00 -86.00   0.50    0.05    -- -102.22 -59.00 -99.43  178
 38  ω   -174.00 -97.00   0.50    0.05    -- -102.22 -52.00-136.91  154
 39  ω   -174.00 -89.00   0.50    0.05    -- -102.22 -51.00 -49.26  170
 40  ω   -173.00 -90.00   0.50    0.05    -- -102.22 -44.00 121.94  166
 41  ω   -175.00 -68.00   0.50    0.05    -- -102.22-134.00  49.00  214
 42  ω   -175.00 -66.00   0.50    0.05    -- -102.22-136.00-129.00  218
 43  ω   -118.00 -66.00   0.50    0.05    --  -46.38-136.00-129.00  104
 44  ω   -118.00 -68.00   0.50    0.05    --  -46.38-134.00  49.00  100
 45  ω   -118.00 -73.00   0.50    0.05    --  -46.38-125.00-120.00   90
 46  ω   -118.00 -73.00   0.50    0.05    --  -46.38-125.00-180.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1618748000
_diffrn_orient_matrix_UB_12      -0.0057309000
_diffrn_orient_matrix_UB_13      -0.1138782000
_diffrn_orient_matrix_UB_21      0.0199662000
_diffrn_orient_matrix_UB_22      -0.0444587000
_diffrn_orient_matrix_UB_23      0.0151598000
_diffrn_orient_matrix_UB_31      -0.1068197000
_diffrn_orient_matrix_UB_32      0.0004099000
_diffrn_orient_matrix_UB_33      0.0872406000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6149
_reflns_number_total             6259
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0384
_refine_ls_restrained_S_all      1.207
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²+10.7695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0941
_refine_special_details          ?
_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.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C4(H4), C10(H10), C12(H12), C32(H32), C29(H29), C18(H18),
 C25(H25), C5(H5), C7(H7), C26(H26), C30(H30), C13(H13), C8(H8), C9(H9),
 C31(H31), C15(H15), C21(H21), C19(H19), C20(H20), C14(H14)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.04888(2) 0.35503(2) 0.62328(2) 0.02871(8) Uani 1 1 d . . . . .
P1 P 0.70340(17) 0.44124(4) 0.92727(12) 0.0390(3) Uani 1 1 d . . . . .
F6 F 0.6869(4) 0.43921(10) 0.7823(3) 0.0495(8) Uani 1 1 d . . . . .
F3 F 0.8656(4) 0.41309(12) 0.9607(3) 0.0575(9) Uani 1 1 d . . . . .
F4 F 0.5831(5) 0.40442(11) 0.9079(4) 0.0564(9) Uani 1 1 d . . . . .
F1 F 0.5417(5) 0.46899(12) 0.8937(4) 0.0642(10) Uani 1 1 d . . . . .
F5 F 0.7193(5) 0.44323(13) 1.0713(3) 0.0613(10) Uani 1 1 d . . . . .
N6 N 0.1980(5) 0.37541(12) 0.5264(4) 0.0312(8) Uani 1 1 d . . . . .
F2 F 0.8252(6) 0.47789(12) 0.9456(4) 0.0687(11) Uani 1 1 d . . . . .
N5 N -0.0080(5) 0.41980(11) 0.6531(3) 0.0268(8) Uani 1 1 d . . . . .
N7 N -0.0996(5) 0.32725(12) 0.7116(4) 0.0339(9) Uani 1 1 d . . . . .
N4 N 0.2056(5) 0.36926(12) 0.8090(4) 0.0319(8) Uani 1 1 d . . . . .
N1 N 0.2670(5) 0.40445(13) 0.9741(4) 0.0378(9) Uani 1 1 d . . . . .
N2 N 0.3349(6) 0.36906(15) 1.0082(4) 0.0459(11) Uani 1 1 d . . . . .
C16 C -0.0678(7) 0.28871(15) 0.7310(5) 0.0387(11) Uani 1 1 d . . . . .
C33 C -0.1048(6) 0.34347(14) 0.4465(5) 0.0330(10) Uani 1 1 d . . . . .
C23 C 0.3555(6) 0.38924(14) 0.5804(5) 0.0335(10) Uani 1 1 d . . . . .
H23 H 0.396171 0.393294 0.668472 0.040 Uiso 1 1 calc R U . . .
N3 N 0.2968(5) 0.34738(14) 0.9080(4) 0.0415(10) Uani 1 1 d . . . . .
C28 C -0.0373(7) 0.35426(14) 0.3532(5) 0.0361(11) Uani 1 1 d . . . . .
C24 C 0.4594(7) 0.39767(16) 0.5132(5) 0.0405(12) Uani 1 1 d . . . . .
H24 H 0.569838 0.407673 0.553690 0.049 Uiso 1 1 calc R U . . .
C11 C -0.1065(5) 0.44665(14) 0.5690(4) 0.0279(9) Uani 1 1 d . . . . .
C6 C -0.1162(6) 0.48616(14) 0.6034(5) 0.0320(10) Uani 1 1 d . . . . .
C3 C 0.0863(6) 0.43368(14) 0.7664(4) 0.0301(9) Uani 1 1 d . . . . .
C4 C 0.0888(7) 0.47288(15) 0.8033(5) 0.0367(11) Uani 1 1 d . . . . .
H4 H 0.162448 0.481061 0.883016 0.044 Uiso 1 1 calc R U . . .
C22 C 0.1291(6) 0.29997(14) 0.6203(5) 0.0357(10) Uani 1 1 d . . . . .
C17 C 0.0546(7) 0.27261(15) 0.6787(5) 0.0383(11) Uani 1 1 d . . . . .
C10 C -0.2001(6) 0.43536(15) 0.4451(4) 0.0322(10) Uani 1 1 d . . . . .
H10 H -0.193720 0.409336 0.418845 0.039 Uiso 1 1 calc R U . . .
C12 C -0.2099(7) 0.34525(16) 0.7548(5) 0.0383(11) Uani 1 1 d . . . . .
H12 H -0.225819 0.372522 0.742977 0.046 Uiso 1 1 calc R U . . .
C2 C 0.1866(6) 0.40410(15) 0.8496(4) 0.0339(10) Uani 1 1 d . . . . .
C32 C -0.2657(7) 0.32750(16) 0.4094(5) 0.0408(12) Uani 1 1 d . . . . .
H32 H -0.313315 0.319295 0.470429 0.049 Uiso 1 1 calc R U . . .
C29 C -0.1316(7) 0.35069(17) 0.2255(5) 0.0432(13) Uani 1 1 d . . . . .
H29 H -0.086037 0.358914 0.163320 0.052 Uiso 1 1 calc R U . . .
C27 C 0.1335(6) 0.37022(15) 0.3989(4) 0.0336(10) Uani 1 1 d . . . . .
C18 C 0.0955(7) 0.23339(16) 0.6805(6) 0.0475(13) Uani 1 1 d . . . . .
H18 H 0.046162 0.215305 0.721459 0.057 Uiso 1 1 calc R U . . .
C25 C 0.4005(7) 0.39135(16) 0.3849(5) 0.0410(12) Uani 1 1 d . . . . .
H25 H 0.471740 0.396132 0.336578 0.049 Uiso 1 1 calc R U . . .
C5 C -0.0153(7) 0.49885(16) 0.7236(5) 0.0390(11) Uani 1 1 d . . . . .
H5 H -0.020028 0.525105 0.748417 0.047 Uiso 1 1 calc R U . . .
C7 C -0.2259(7) 0.51200(15) 0.5162(5) 0.0393(11) Uani 1 1 d . . . . .
H7 H -0.236073 0.538067 0.540552 0.047 Uiso 1 1 calc R U . . .
C26 C 0.2375(7) 0.37805(16) 0.3279(5) 0.0398(11) Uani 1 1 d . . . . .
H26 H 0.195729 0.374193 0.239744 0.048 Uiso 1 1 calc R U . . .
C30 C -0.2926(7) 0.33492(19) 0.1918(6) 0.0500(14) Uani 1 1 d . . . . .
H30 H -0.357873 0.332030 0.105763 0.060 Uiso 1 1 calc R U . . .
C13 C -0.3019(8) 0.32500(18) 0.8166(6) 0.0520(15) Uani 1 1 d . . . . .
H13 H -0.384461 0.337858 0.842930 0.062 Uiso 1 1 calc R U . . .
C8 C -0.3165(7) 0.50035(16) 0.3988(5) 0.0400(12) Uani 1 1 d . . . . .
H8 H -0.390405 0.517944 0.341420 0.048 Uiso 1 1 calc R U . . .
C9 C -0.2999(6) 0.46182(15) 0.3630(5) 0.0364(11) Uani 1 1 d . . . . .
H9 H -0.359562 0.453942 0.279408 0.044 Uiso 1 1 calc R U . . .
C31 C -0.3579(7) 0.32349(18) 0.2818(6) 0.0486(14) Uani 1 1 d . . . . .
H31 H -0.468283 0.312585 0.257107 0.058 Uiso 1 1 calc R U . . .
C15 C -0.1535(9) 0.26763(18) 0.7974(7) 0.0555(16) Uani 1 1 d . . . . .
H15 H -0.130521 0.240733 0.813681 0.067 Uiso 1 1 calc R U . . .
C21 C 0.2439(7) 0.28614(16) 0.5646(6) 0.0424(12) Uani 1 1 d . . . . .
H21 H 0.297813 0.303968 0.526147 0.051 Uiso 1 1 calc R U . . .
C19 C 0.2070(8) 0.22051(17) 0.6233(6) 0.0501(14) Uani 1 1 d . . . . .
H19 H 0.233698 0.193630 0.624243 0.060 Uiso 1 1 calc R U . . .
C1 C 0.2932(8) 0.43511(19) 1.0670(5) 0.0521(15) Uani 1 1 d . . . . .
H1A H 0.344512 0.424076 1.151062 0.078 Uiso 1 1 calc R U . . .
H1B H 0.184311 0.446998 1.060089 0.078 Uiso 1 1 calc R U . . .
H1C H 0.368613 0.454931 1.052578 0.078 Uiso 1 1 calc R U . . .
C20 C 0.2798(8) 0.24686(17) 0.5647(6) 0.0493(14) Uani 1 1 d . . . . .
H20 H 0.355273 0.237931 0.524100 0.059 Uiso 1 1 calc R U . . .
C14 C -0.2706(9) 0.28582(19) 0.8387(7) 0.0616(18) Uani 1 1 d . . . . .
H14 H -0.329854 0.271454 0.882490 0.074 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 N6 2.045(4) . ?
Ir1 N5 2.325(4) . ?
Ir1 N7 2.074(4) . ?
Ir1 N4 2.131(4) . ?
Ir1 C33 2.025(5) . ?
Ir1 C22 2.013(5) . ?
P1 F6 1.602(3) . ?
P1 F3 1.609(4) . ?
P1 F4 1.588(4) . ?
P1 F1 1.596(4) . ?
P1 F5 1.593(3) . ?
P1 F2 1.592(4) . ?
N6 C23 1.344(6) . ?
N6 C27 1.373(6) . ?
N5 C11 1.384(6) . ?
N5 C3 1.349(6) . ?
N7 C16 1.354(6) . ?
N7 C12 1.334(7) . ?
N4 N3 1.354(6) . ?
N4 C2 1.312(7) . ?
N1 N2 1.344(7) . ?
N1 C2 1.344(6) . ?
N1 C1 1.453(8) . ?
N2 N3 1.305(7) . ?
C16 C17 1.456(7) . ?
C16 C15 1.403(8) . ?
C33 C28 1.406(7) . ?
C33 C32 1.386(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.366(7) . ?
C28 C29 1.402(7) . ?
C28 C27 1.458(7) . ?
C24 H24 0.9500 . ?
C24 C25 1.387(8) . ?
C11 C6 1.423(7) . ?
C11 C10 1.413(7) . ?
C6 C5 1.410(7) . ?
C6 C7 1.415(7) . ?
C3 C4 1.408(7) . ?
C3 C2 1.449(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.359(8) . ?
C22 C17 1.410(7) . ?
C22 C21 1.400(7) . ?
C17 C18 1.390(7) . ?
C10 H10 0.9500 . ?
C10 C9 1.368(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.390(8) . ?
C32 H32 0.9500 . ?
C32 C31 1.399(8) . ?
C29 H29 0.9500 . ?
C29 C30 1.385(9) . ?
C27 C26 1.397(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.376(9) . ?
C25 H25 0.9500 . ?
C25 C26 1.380(8) . ?
C5 H5 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.352(8) . ?
C26 H26 0.9500 . ?
C30 H30 0.9500 . ?
C30 C31 1.366(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.379(9) . ?
C8 H8 0.9500 . ?
C8 C9 1.406(8) . ?
C9 H9 0.9500 . ?
C31 H31 0.9500 . ?
C15 H15 0.9500 . ?
C15 C14 1.372(9) . ?
C21 H21 0.9500 . ?
C21 C20 1.383(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.380(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C20 H20 0.9500 . ?
C14 H14 0.9500 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Ir1 N5 86.67(14) . . ?
N6 Ir1 N7 172.45(16) . . ?
N6 Ir1 N4 99.48(16) . . ?
N7 Ir1 N5 100.68(14) . . ?
N7 Ir1 N4 84.34(16) . . ?
N4 Ir1 N5 74.07(14) . . ?
C33 Ir1 N6 80.69(19) . . ?
C33 Ir1 N5 103.75(16) . . ?
C33 Ir1 N7 95.75(19) . . ?
C33 Ir1 N4 177.79(17) . . ?
C22 Ir1 N6 92.59(19) . . ?
C22 Ir1 N5 171.42(17) . . ?
C22 Ir1 N7 80.40(19) . . ?
C22 Ir1 N4 97.65(18) . . ?
C22 Ir1 C33 84.5(2) . . ?
F6 P1 F3 89.46(19) . . ?
F4 P1 F6 89.5(2) . . ?
F4 P1 F3 90.1(2) . . ?
F4 P1 F1 89.6(2) . . ?
F4 P1 F5 90.4(2) . . ?
F4 P1 F2 179.3(2) . . ?
F1 P1 F6 90.4(2) . . ?
F1 P1 F3 179.7(3) . . ?
F5 P1 F6 179.9(3) . . ?
F5 P1 F3 90.6(2) . . ?
F5 P1 F1 89.5(2) . . ?
F2 P1 F6 89.9(2) . . ?
F2 P1 F3 89.4(2) . . ?
F2 P1 F1 90.9(3) . . ?
F2 P1 F5 90.2(2) . . ?
C23 N6 Ir1 124.2(3) . . ?
C23 N6 C27 120.4(4) . . ?
C27 N6 Ir1 115.0(3) . . ?
C11 N5 Ir1 130.0(3) . . ?
C3 N5 Ir1 113.2(3) . . ?
C3 N5 C11 116.3(4) . . ?
C16 N7 Ir1 114.3(3) . . ?
C12 N7 Ir1 124.4(3) . . ?
C12 N7 C16 121.2(4) . . ?
N3 N4 Ir1 132.9(3) . . ?
C2 N4 Ir1 116.6(3) . . ?
C2 N4 N3 108.6(4) . . ?
N2 N1 C1 120.1(4) . . ?
C2 N1 N2 108.0(5) . . ?
C2 N1 C1 131.9(5) . . ?
N3 N2 N1 108.1(4) . . ?
N7 C16 C17 115.7(4) . . ?
N7 C16 C15 118.9(5) . . ?
C15 C16 C17 125.4(5) . . ?
C28 C33 Ir1 114.1(4) . . ?
C32 C33 Ir1 127.7(4) . . ?
C32 C33 C28 118.3(5) . . ?
N6 C23 H23 118.8 . . ?
N6 C23 C24 122.4(5) . . ?
C24 C23 H23 118.8 . . ?
N2 N3 N4 108.0(4) . . ?
C33 C28 C27 115.4(4) . . ?
C29 C28 C33 121.4(5) . . ?
C29 C28 C27 123.2(5) . . ?
C23 C24 H24 120.6 . . ?
C23 C24 C25 118.7(5) . . ?
C25 C24 H24 120.6 . . ?
N5 C11 C6 121.6(4) . . ?
N5 C11 C10 120.4(4) . . ?
C10 C11 C6 118.1(4) . . ?
C5 C6 C11 119.3(4) . . ?
C5 C6 C7 121.3(5) . . ?
C7 C6 C11 119.4(5) . . ?
N5 C3 C4 124.5(4) . . ?
N5 C3 C2 113.5(4) . . ?
C4 C3 C2 122.1(4) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.3(5) . . ?
C5 C4 H4 120.4 . . ?
C17 C22 Ir1 114.6(4) . . ?
C21 C22 Ir1 127.7(4) . . ?
C21 C22 C17 117.7(5) . . ?
C22 C17 C16 114.9(4) . . ?
C18 C17 C16 124.6(5) . . ?
C18 C17 C22 120.5(5) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 C11 120.2(5) . . ?
C9 C10 H10 119.9 . . ?
N7 C12 H12 119.3 . . ?
N7 C12 C13 121.5(5) . . ?
C13 C12 H12 119.3 . . ?
N4 C2 N1 107.4(4) . . ?
N4 C2 C3 121.7(4) . . ?
N1 C2 C3 130.9(5) . . ?
C33 C32 H32 120.1 . . ?
C33 C32 C31 119.9(5) . . ?
C31 C32 H32 120.1 . . ?
C28 C29 H29 120.7 . . ?
C30 C29 C28 118.7(6) . . ?
C30 C29 H29 120.7 . . ?
N6 C27 C28 114.6(4) . . ?
N6 C27 C26 118.6(5) . . ?
C26 C27 C28 126.7(5) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.6(5) . . ?
C19 C18 H18 119.7 . . ?
C24 C25 H25 120.3 . . ?
C26 C25 C24 119.4(5) . . ?
C26 C25 H25 120.3 . . ?
C6 C5 H5 120.6 . . ?
C4 C5 C6 118.8(5) . . ?
C4 C5 H5 120.6 . . ?
C6 C7 H7 119.3 . . ?
C8 C7 C6 121.4(5) . . ?
C8 C7 H7 119.3 . . ?
C27 C26 H26 119.8 . . ?
C25 C26 C27 120.5(5) . . ?
C25 C26 H26 119.8 . . ?
C29 C30 H30 119.8 . . ?
C31 C30 C29 120.4(5) . . ?
C31 C30 H30 119.8 . . ?
C12 C13 H13 120.8 . . ?
C14 C13 C12 118.4(6) . . ?
C14 C13 H13 120.8 . . ?
C7 C8 H8 120.5 . . ?
C7 C8 C9 119.0(5) . . ?
C9 C8 H8 120.5 . . ?
C10 C9 C8 121.8(5) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C32 C31 H31 119.3 . . ?
C30 C31 C32 121.4(6) . . ?
C30 C31 H31 119.3 . . ?
C16 C15 H15 120.0 . . ?
C14 C15 C16 120.1(6) . . ?
C14 C15 H15 120.0 . . ?
C22 C21 H21 119.5 . . ?
C20 C21 C22 120.9(5) . . ?
C20 C21 H21 119.5 . . ?
C18 C19 H19 120.2 . . ?
C18 C19 C20 119.7(5) . . ?
C20 C19 H19 120.2 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C21 C20 H20 119.7 . . ?
C19 C20 C21 120.6(5) . . ?
C19 C20 H20 119.7 . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.9(6) . . ?
C15 C14 H14 120.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ir1 N6 C23 C24 171.0(4) . . . . ?
Ir1 N6 C27 C28 5.3(5) . . . . ?
Ir1 N6 C27 C26 -170.7(4) . . . . ?
Ir1 N5 C11 C6 -175.4(3) . . . . ?
Ir1 N5 C11 C10 4.1(6) . . . . ?
Ir1 N5 C3 C4 173.4(4) . . . . ?
Ir1 N5 C3 C2 -7.0(5) . . . . ?
Ir1 N7 C16 C17 -4.5(6) . . . . ?
Ir1 N7 C16 C15 175.9(5) . . . . ?
Ir1 N7 C12 C13 -178.0(5) . . . . ?
Ir1 N4 N3 N2 -164.0(4) . . . . ?
Ir1 N4 C2 N1 166.9(3) . . . . ?
Ir1 N4 C2 C3 -10.3(6) . . . . ?
Ir1 C33 C28 C29 -175.7(4) . . . . ?
Ir1 C33 C28 C27 2.6(6) . . . . ?
Ir1 C33 C32 C31 176.5(4) . . . . ?
Ir1 C22 C17 C16 0.1(6) . . . . ?
Ir1 C22 C17 C18 178.3(5) . . . . ?
Ir1 C22 C21 C20 -176.5(5) . . . . ?
N6 C23 C24 C25 -0.7(8) . . . . ?
N6 C27 C26 C25 -1.1(8) . . . . ?
N5 C11 C6 C5 3.9(7) . . . . ?
N5 C11 C6 C7 -176.6(4) . . . . ?
N5 C11 C10 C9 178.8(4) . . . . ?
N5 C3 C4 C5 3.3(8) . . . . ?
N5 C3 C2 N4 11.8(6) . . . . ?
N5 C3 C2 N1 -164.6(5) . . . . ?
N7 C16 C17 C22 3.0(7) . . . . ?
N7 C16 C17 C18 -175.2(6) . . . . ?
N7 C16 C15 C14 1.7(10) . . . . ?
N7 C12 C13 C14 3.4(10) . . . . ?
N1 N2 N3 N4 0.7(5) . . . . ?
N2 N1 C2 N4 -0.1(5) . . . . ?
N2 N1 C2 C3 176.7(5) . . . . ?
C16 N7 C12 C13 -2.8(8) . . . . ?
C16 C17 C18 C19 176.9(6) . . . . ?
C16 C15 C14 C13 -1.0(12) . . . . ?
C33 C28 C29 C30 -2.2(8) . . . . ?
C33 C28 C27 N6 -5.2(6) . . . . ?
C33 C28 C27 C26 170.5(5) . . . . ?
C33 C32 C31 C30 0.2(8) . . . . ?
C23 N6 C27 C28 178.7(4) . . . . ?
C23 N6 C27 C26 2.7(7) . . . . ?
C23 C24 C25 C26 2.2(8) . . . . ?
N3 N4 C2 N1 0.6(5) . . . . ?
N3 N4 C2 C3 -176.6(4) . . . . ?
C28 C33 C32 C31 -1.7(7) . . . . ?
C28 C29 C30 C31 0.6(8) . . . . ?
C28 C27 C26 C25 -176.7(5) . . . . ?
C24 C25 C26 C27 -1.3(8) . . . . ?
C11 N5 C3 C4 0.5(7) . . . . ?
C11 N5 C3 C2 -179.8(4) . . . . ?
C11 C6 C5 C4 0.1(7) . . . . ?
C11 C6 C7 C8 -2.8(8) . . . . ?
C11 C10 C9 C8 -1.7(8) . . . . ?
C6 C11 C10 C9 -1.6(7) . . . . ?
C6 C7 C8 C9 -0.5(8) . . . . ?
C3 N5 C11 C6 -4.1(6) . . . . ?
C3 N5 C11 C10 175.5(4) . . . . ?
C3 C4 C5 C6 -3.4(8) . . . . ?
C4 C3 C2 N4 -168.6(5) . . . . ?
C4 C3 C2 N1 15.0(8) . . . . ?
C22 C17 C18 C19 -1.2(9) . . . . ?
C22 C21 C20 C19 -2.0(9) . . . . ?
C17 C16 C15 C14 -177.9(6) . . . . ?
C17 C22 C21 C20 1.3(8) . . . . ?
C17 C18 C19 C20 0.5(10) . . . . ?
C10 C11 C6 C5 -175.7(4) . . . . ?
C10 C11 C6 C7 3.8(7) . . . . ?
C12 N7 C16 C17 179.8(5) . . . . ?
C12 N7 C16 C15 0.2(8) . . . . ?
C12 C13 C14 C15 -1.5(11) . . . . ?
C2 N4 N3 N2 -0.8(5) . . . . ?
C2 N1 N2 N3 -0.4(5) . . . . ?
C2 C3 C4 C5 -176.3(5) . . . . ?
C32 C33 C28 C29 2.7(7) . . . . ?
C32 C33 C28 C27 -179.0(4) . . . . ?
C29 C28 C27 N6 173.1(5) . . . . ?
C29 C28 C27 C26 -11.2(8) . . . . ?
C29 C30 C31 C32 0.4(9) . . . . ?
C27 N6 C23 C24 -1.8(7) . . . . ?
C27 C28 C29 C30 179.6(5) . . . . ?
C18 C19 C20 C21 1.0(10) . . . . ?
C5 C6 C7 C8 176.7(5) . . . . ?
C7 C6 C5 C4 -179.5(5) . . . . ?
C7 C8 C9 C10 2.8(8) . . . . ?
C15 C16 C17 C22 -177.5(6) . . . . ?
C15 C16 C17 C18 4.4(10) . . . . ?
C21 C22 C17 C16 -178.0(5) . . . . ?
C21 C22 C17 C18 0.2(8) . . . . ?
C1 N1 N2 N3 -178.3(5) . . . . ?
C1 N1 C2 N4 177.5(5) . . . . ?
C1 N1 C2 C3 -5.7(9) . . . . ?

_olex2_date_sample_data_collection 2021-03-19
_olex2_exptl_crystal_mounting_method 'mounted on a glass fibre with silicon oil'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.896
_oxdiff_exptl_absorpt_empirical_full_min 0.697

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mxm543rm_auto
_audit_block_doi                 10.5517/ccdc.csd.cc2dlrc4
_database_code_depnum_ccdc_archive 'CCDC 2222556'
loop_
_audit_author_name
_audit_author_address
'Lee Cameron'
;Curtin University
Australia
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_mxm543rm_auto       
;
PROBLEM: Check Calcd Resid. Dens.  0.55Ang From F4              3.20 eA-3
RESPONSE: This alert is caused by a disordered PF6 counterion
;
_vrf_PLAT972_mxm543rm_auto       
;
PROBLEM: Check Calcd Resid. Dens.  0.32Ang From F5             -2.62 eA-3
RESPONSE: This alert is caused by a disordered PF6 counterion
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C29 H23 Ir N7, C3 H6 O, F6 P'
_chemical_formula_sum            'C32 H29 F6 Ir N7 O P'
_chemical_formula_weight         864.79
_exptl_crystal_recrystallization_method 
'formed from the slow evaporation of acetone from an acetone and water solution.'
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            'clear yellow'
_diffrn_ambient_temperature      100.00(10)
_chemical_oxdiff_formula         'C29 H23 Ir1 N7 P1 F6'
_chemical_oxdiff_usercomment     'Lee Cameron'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_chemical_absolute_configuration .
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.95004(6)
_cell_length_b                   13.30076(5)
_cell_length_c                   17.34384(7)
_cell_angle_alpha                90
_cell_angle_beta                 111.4208(4)
_cell_angle_gamma                90
_cell_volume                     3210.54(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    57718
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2050
_cell_measurement_theta_min      4.2830
_shelx_estimated_absorpt_T_max   0.470
_shelx_estimated_absorpt_T_min   0.329
_exptl_absorpt_coefficient_mu    9.180
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1696
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.097
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            94362
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.334
_diffrn_reflns_theta_min         3.175
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     34.00 119.00   0.50    0.05    --   46.32  41.00 -25.00  170
  2  ω     32.00 118.00   0.50    0.05    --   46.32  57.00  60.00  172
  3  ω     32.00 118.00   0.50    0.05    --   46.32  57.00  90.00  172
  4  ω     34.00 119.00   0.50    0.05    --   46.32  38.00 150.00  170
  5  ω    -46.00  26.00   0.50    0.05    --  -46.32  41.00 -25.00  144
  6  ω    -69.00  26.00   0.50    0.05    --  -46.32  77.00 -90.00  190
  7  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00-180.00   82
  8  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00   0.00   82
  9  ω   -105.00 -30.00   0.50    0.05    -- -102.29  77.00  30.00  150
 10  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00  90.00   82
 11  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 120.00   82
 12  ω    -71.00 -30.00   0.50    0.05    -- -102.29  61.00 150.00   82
 13  ω   -119.00 -33.00   0.50    0.05    --  -46.32 -38.00 150.00  172
 14  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -77.00 120.00  188
 15  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -77.00  90.00  188
 16  ω   -174.00 -79.00   0.50    0.05    -- -102.29 -78.00  72.54  190
 17  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -77.00  60.00  188
 18  ω   -174.00 -81.00   0.50    0.05    -- -102.29 -73.00 102.98  186
 19  ω   -174.00 -80.00   0.50    0.05    -- -102.29 -77.00 138.93  188
 20  ω   -174.00 -83.00   0.50    0.05    -- -102.29 -69.00 123.87  182
 21  ω   -174.00 -83.00   0.50    0.05    -- -102.29 -69.00  91.90  182
 22  ω   -174.00 -83.00   0.50    0.05    -- -102.29 -69.00  44.60  182
 23  ω   -174.00 -83.00   0.50    0.05    -- -102.29 -68.00  75.75  182
 24  ω   -174.00 -85.00   0.50    0.05    -- -102.29 -64.00  94.28  178
 25  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -62.00 123.64  176
 26  ω   -174.00 -84.00   0.50    0.05    -- -102.29 -65.00 148.26  180
 27  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00  60.00  176
 28  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -61.00  46.08  176
 29  ω   -174.00 -86.00   0.50    0.05    -- -102.29 -60.00  62.26  176
 30  ω   -174.00 -88.00   0.50    0.05    -- -102.29 -54.00  86.47  172
 31  ω   -174.00 -88.00   0.50    0.05    -- -102.29 -53.00 117.64  172
 32  ω   -174.00 -88.00   0.50    0.05    -- -102.29 -53.00  67.24  172
 33  ω   -174.00 -88.00   0.50    0.05    -- -102.29 -48.00  67.56  172
 34  ω   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00  60.00  168
 35  ω   -174.00 -89.00   0.50    0.05    -- -102.29 -51.00  11.05  170
 36  ω   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00  30.00  168
 37  ω   -174.00 -88.00   0.50    0.05    -- -102.29 -48.00 -99.61  172
 38  ω   -175.00 -90.00   0.50    0.05    -- -102.29 -41.00-178.00  170
 39  ω   -119.00 -34.00   0.50    0.05    --  -46.32 -41.00-178.00  170
 40  ω   -108.00 -30.00   0.50    0.05    -- -102.29 108.00 -60.75  156
 41  ω   -174.00 -90.00   0.50    0.05    -- -102.29 -45.00  90.00  168
 42  ω   -174.00 -79.00   0.50    0.05    -- -102.29 -82.00 129.39  190
 43  ω   -118.00 -73.00   0.50    0.05    --  -46.32-125.00   0.00   90
 44  ω   -118.00 -73.00   0.50    0.05    --  -46.32-125.00 -90.00   90
 45  ω     33.00  69.00   0.50    0.05    --  102.29 -61.00-180.00   72
 46  ω     30.00 101.00   0.50    0.05    --  102.29-125.00  90.00  142
 47  ω     30.00  71.00   0.50    0.05    --  102.29 -61.00   0.00   82
 48  ω    -28.00  26.00   0.50    0.05    --   46.32 -19.00  30.00  108
 49  ω    -26.00  46.00   0.50    0.05    --   46.32 -41.00-178.00  144
 50  ω    119.00 160.00   0.50    0.05    --  102.29 125.00-150.00   82
 51  ω     75.00 104.00   0.50    0.05    --  102.29 125.00-150.00   58
 52  ω    131.00 177.00   0.50    0.05    --  102.29  15.00-120.00   92
 53  ω    132.00 165.00   0.50    0.05    --  102.29  77.00  90.00   66
 54  ω     80.00 174.00   0.50    0.05    --  102.29  77.00  60.00  188
 55  ω     90.00 175.00   0.50    0.05    --  102.29  41.00 -25.00  170
 56  ω     80.00 106.00   0.50    0.05    --  102.29  77.00  90.00   52
 57  ω     89.00 131.00   0.50    0.05    --  102.29  61.00 120.00   84
 58  ω     86.00 112.00   0.50    0.05    --  102.29  61.00  90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0555032000
_diffrn_orient_matrix_UB_12      0.0127343000
_diffrn_orient_matrix_UB_13      0.0936870000
_diffrn_orient_matrix_UB_21      0.0793465000
_diffrn_orient_matrix_UB_22      0.0582483000
_diffrn_orient_matrix_UB_23      -0.0179393000
_diffrn_orient_matrix_UB_31      -0.0536689000
_diffrn_orient_matrix_UB_32      0.0992959000
_diffrn_orient_matrix_UB_33      -0.0014902000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6366
_reflns_number_total             6566
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.142
_refine_diff_density_min         -2.615
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6566
_refine_ls_number_restraints     179
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0385
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0595P)²+18.4436P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1029
_refine_special_details          ?
_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. Restrained distances
 F6A-F3A
 2.328 with sigma of 0.02
 F3A-F5A
 2.328 with sigma of 0.02
 F5A-F4A
 2.328 with sigma of 0.02
 F6A-F4A
 2.328 with sigma of 0.02
 P1-F6 \\sim P1-F1 \\sim P1-F5 \\sim P1-F2 \\sim P1-F3 \\sim P1-F4
 with sigma of 0.02
 F6-F1 \\sim F6-F2 \\sim F6-F3 \\sim F6-F4 \\sim F5-F1 \\sim F5-F2 \\sim F5-F3
\\sim F5-F4
 with sigma of 0.04
 F6-F5 \\sim F1-F2 \\sim F4-F3
 with sigma of 0.05
 P1-F5 \\sim P1-F5A \\sim P1-F3 \\sim P1-F3A \\sim P1-F6 \\sim P1-F6A \\sim
P1-F4 \\sim P1-F4A \\sim P1-F2 ~
 P1-F1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P1 \\sim F6 \\sim F1 \\sim F5 \\sim F2 \\sim F3 \\sim F4: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(F3) = Uanis(F5A) = Uanis(F3A) = Uanis(F4) = Uanis(F6A) = Uanis(F4A) =
Uanis(F6) = Uanis(F5)
4. Rigid body (RIGU) restrains
 P1, F6, F1, F5, F2, F3, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F6A)=Sof(F5A)=Sof(F3A)=Sof(F4A)=1-FVAR(1)
 Sof(F6)=Sof(F5)=Sof(F3)=Sof(F4)=FVAR(1)
6.a Free rotating group:
 P1(F6,F1,F5,F2,F3,F4)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C5(H5), C27(H27), C17(H17), C8(H8), C6(H6), C22(H22),
 C26(H26), C25(H25), C21(H21), C20(H20), C19(H19), C28(H28), C14(H14), C16(H16),
  C9(H9), C15(H15), C11(H11), C10(H10)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.21579(2) 0.17112(2) 0.36242(2) 0.01453(8) Uani 1 1 d . . . . .
N6 N 0.1078(3) 0.2717(3) 0.3505(2) 0.0211(8) Uani 1 1 d . . . . .
N7 N 0.3077(2) 0.0573(3) 0.3605(2) 0.0168(7) Uani 1 1 d . . . . .
N5 N 0.2762(3) 0.1914(3) 0.4963(2) 0.0163(7) Uani 1 1 d . . . . .
N2 N 0.4350(3) 0.3859(3) 0.3914(2) 0.0247(8) Uani 1 1 d . . . . .
N1 N 0.4473(3) 0.3682(3) 0.4702(2) 0.0215(8) Uani 1 1 d . . . . .
C29 C 0.1763(3) 0.1535(3) 0.2387(3) 0.0191(9) Uani 1 1 d . . . . .
N3 N 0.3632(3) 0.3369(3) 0.3368(2) 0.0231(8) Uani 1 1 d . . . . .
N4 N 0.3256(3) 0.2828(3) 0.3812(2) 0.0178(7) Uani 1 1 d . . . . .
C3 C 0.3498(3) 0.2576(3) 0.5259(3) 0.0161(8) Uani 1 1 d . . . . .
C18 C 0.1144(3) 0.0749(4) 0.3676(3) 0.0182(8) Uani 1 1 d . . . . .
C23 C 0.3010(3) 0.0260(3) 0.2837(3) 0.0214(9) Uani 1 1 d . . . . .
C4 C 0.3938(3) 0.2799(3) 0.6087(3) 0.0188(8) Uani 1 1 d . . . . .
H4 H 0.444277 0.327954 0.626839 0.023 Uiso 1 1 calc R U . . .
C7 C 0.2476(3) 0.1435(4) 0.5517(3) 0.0193(8) Uani 1 1 d . . . . .
H7 H 0.196910 0.095946 0.532291 0.023 Uiso 1 1 calc R U . . .
C5 C 0.3631(3) 0.2307(3) 0.6654(3) 0.0206(9) Uani 1 1 d . . . . .
H5 H 0.392075 0.244694 0.722938 0.025 Uiso 1 1 calc R U . . .
C24 C 0.2319(3) 0.0828(3) 0.2154(3) 0.0202(9) Uani 1 1 d . . . . .
C27 C 0.0888(4) 0.1848(4) 0.0922(3) 0.0303(11) Uani 1 1 d . . . . .
H27 H 0.039008 0.219296 0.050056 0.036 Uiso 1 1 calc R U . . .
C17 C 0.1231(3) -0.0278(4) 0.3829(3) 0.0236(9) Uani 1 1 d . . . . .
H17 H 0.180064 -0.061610 0.385378 0.028 Uiso 1 1 calc R U . . .
C2 C 0.3770(3) 0.3035(3) 0.4618(3) 0.0179(8) Uani 1 1 d . . . . .
C8 C 0.1129(4) 0.3709(4) 0.3362(3) 0.0285(10) Uani 1 1 d . . . . .
H8 H 0.170831 0.397818 0.334164 0.034 Uiso 1 1 calc R U . . .
C6 C 0.2898(3) 0.1613(4) 0.6366(3) 0.0215(10) Uani 1 1 d . . . . .
H6 H 0.268327 0.125956 0.674180 0.026 Uiso 1 1 calc R U . . .
C22 C 0.3519(3) -0.0584(4) 0.2752(3) 0.0293(11) Uani 1 1 d . . . . .
H22 H 0.347573 -0.079682 0.221660 0.035 Uiso 1 1 calc R U . . .
C26 C 0.1461(4) 0.1163(4) 0.0707(3) 0.0298(11) Uani 1 1 d . . . . .
H26 H 0.135866 0.104329 0.014116 0.036 Uiso 1 1 calc R U . . .
C25 C 0.2180(4) 0.0658(4) 0.1323(3) 0.0265(10) Uani 1 1 d . . . . .
H25 H 0.257985 0.019582 0.118111 0.032 Uiso 1 1 calc R U . . .
C21 C 0.4081(4) -0.1104(4) 0.3436(4) 0.0354(12) Uani 1 1 d . . . . .
H21 H 0.441996 -0.168476 0.337668 0.042 Uiso 1 1 calc R U . . .
C20 C 0.4156(3) -0.0779(4) 0.4220(3) 0.0303(11) Uani 1 1 d . . . . .
H20 H 0.454711 -0.112972 0.470299 0.036 Uiso 1 1 calc R U . . .
C19 C 0.3647(3) 0.0064(4) 0.4279(3) 0.0237(9) Uani 1 1 d . . . . .
H19 H 0.369831 0.029375 0.481228 0.028 Uiso 1 1 calc R U . . .
C13 C 0.0279(3) 0.1217(4) 0.3646(3) 0.0253(10) Uani 1 1 d . . . . .
C28 C 0.1042(4) 0.2030(4) 0.1753(3) 0.0249(9) Uani 1 1 d . . . . .
H28 H 0.064577 0.250160 0.188961 0.030 Uiso 1 1 calc R U . . .
C14 C -0.0459(4) 0.0669(5) 0.3755(3) 0.0339(12) Uani 1 1 d . . . . .
H14 H -0.103412 0.099552 0.372884 0.041 Uiso 1 1 calc R U . . .
C12 C 0.0247(3) 0.2317(4) 0.3532(3) 0.0267(10) Uani 1 1 d . . . . .
C16 C 0.0497(4) -0.0818(4) 0.3946(3) 0.0302(11) Uani 1 1 d . . . . .
H16 H 0.057488 -0.151835 0.405911 0.036 Uiso 1 1 calc R U . . .
C9 C 0.0358(4) 0.4340(4) 0.3244(3) 0.0379(13) Uani 1 1 d . . . . .
H9 H 0.040275 0.503346 0.313302 0.045 Uiso 1 1 calc R U . . .
C15 C -0.0351(4) -0.0349(5) 0.3900(3) 0.0357(12) Uani 1 1 d . . . . .
H15 H -0.085469 -0.072941 0.396826 0.043 Uiso 1 1 calc R U . . .
C11 C -0.0536(4) 0.2938(5) 0.3428(4) 0.0419(14) Uani 1 1 d . . . . .
H11 H -0.111204 0.266390 0.345112 0.050 Uiso 1 1 calc R U . . .
C1 C 0.4976(5) 0.4524(5) 0.3674(4) 0.0464(17) Uani 1 1 d . . . . .
H1A H 0.514656 0.510740 0.404438 0.070 Uiso 1 1 calc R U . . .
H1B H 0.464294 0.475106 0.310264 0.070 Uiso 1 1 calc R U . . .
H1C H 0.556192 0.416118 0.371281 0.070 Uiso 1 1 calc R U . . .
O1 O 0.2844(4) 0.5188(4) 0.4533(5) 0.080(2) Uani 1 1 d . . . . .
C10 C -0.0474(5) 0.3956(5) 0.3290(4) 0.0443(15) Uani 1 1 d . . . . .
H10 H -0.100378 0.438642 0.322718 0.053 Uiso 1 1 calc R U . . .
C31 C 0.2497(5) 0.5999(5) 0.4284(5) 0.0537(18) Uani 1 1 d . . . . .
C30 C 0.1755(6) 0.6439(6) 0.4575(6) 0.061(2) Uani 1 1 d . . . . .
H30A H 0.162770 0.597175 0.495947 0.092 Uiso 1 1 calc R U . . .
H30B H 0.116033 0.655509 0.409777 0.092 Uiso 1 1 calc R U . . .
H30C H 0.198937 0.707835 0.485656 0.092 Uiso 1 1 calc R U . . .
C32 C 0.2806(14) 0.6623(11) 0.3727(11) 0.141(7) Uani 1 1 d . . . . .
H32A H 0.248453 0.727745 0.365068 0.212 Uiso 1 1 calc R U . . .
H32B H 0.263636 0.628647 0.318955 0.212 Uiso 1 1 calc R U . . .
H32C H 0.350351 0.671993 0.396920 0.212 Uiso 1 1 calc R U . . .
P1 P 0.36544(12) 0.84450(12) 0.64321(9) 0.0476(4) Uani 1 1 d DG U . . .
F6 F 0.2968(3) 0.9178(4) 0.6747(3) 0.0917(12) Uani 0.594(6) 1 d DG U P A 1
F1 F 0.2947(3) 0.8639(4) 0.54638(13) 0.142(3) Uani 1 1 d DG U . A .
F5 F 0.4340(3) 0.7712(4) 0.6117(3) 0.0917(12) Uani 0.594(6) 1 d DG U P A 1
F2 F 0.4362(3) 0.8251(3) 0.74005(12) 0.098(2) Uani 1 1 d DG U . A .
F3 F 0.4309(3) 0.9423(3) 0.6388(3) 0.0917(12) Uani 0.594(6) 1 d DG U P A 1
F4 F 0.3000(3) 0.7467(3) 0.6476(3) 0.0917(12) Uani 0.594(6) 1 d DG U P A 1
F6A F 0.2697(9) 0.8315(10) 0.6531(10) 0.0917(12) Uani 0.406(6) 1 d D . P A 2
F5A F 0.4750(9) 0.8297(9) 0.6281(11) 0.0917(12) Uani 0.406(6) 1 d D . P A 2
F3A F 0.3912(10) 0.9572(8) 0.6421(10) 0.0917(12) Uani 0.406(6) 1 d D . P A 2
F4A F 0.3693(10) 0.7183(7) 0.6347(9) 0.0917(12) Uani 0.406(6) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 N6 2.048(4) . ?
Ir1 N7 2.053(4) . ?
Ir1 N5 2.179(4) . ?
Ir1 C29 2.020(4) . ?
Ir1 N4 2.149(4) . ?
Ir1 C18 2.010(4) . ?
N6 C8 1.349(7) . ?
N6 C12 1.368(7) . ?
N7 C23 1.363(6) . ?
N7 C19 1.351(6) . ?
N5 C3 1.356(6) . ?
N5 C7 1.346(6) . ?
N2 N1 1.332(5) . ?
N2 N3 1.316(6) . ?
N2 C1 1.455(6) . ?
N1 C2 1.324(6) . ?
C29 C24 1.409(6) . ?
C29 C28 1.392(7) . ?
N3 N4 1.319(5) . ?
N4 C2 1.355(6) . ?
C3 C4 1.377(6) . ?
C3 C2 1.451(6) . ?
C18 C17 1.389(7) . ?
C18 C13 1.420(6) . ?
C23 C24 1.466(7) . ?
C23 C22 1.395(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(6) . ?
C7 H7 0.9500 . ?
C7 C6 1.393(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.380(7) . ?
C24 C25 1.397(6) . ?
C27 H27 0.9500 . ?
C27 C26 1.391(8) . ?
C27 C28 1.396(7) . ?
C17 H17 0.9500 . ?
C17 C16 1.387(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.379(7) . ?
C6 H6 0.9500 . ?
C22 H22 0.9500 . ?
C22 C21 1.365(8) . ?
C26 H26 0.9500 . ?
C26 C25 1.381(8) . ?
C25 H25 0.9500 . ?
C21 H21 0.9500 . ?
C21 C20 1.393(8) . ?
C20 H20 0.9500 . ?
C20 C19 1.380(7) . ?
C19 H19 0.9500 . ?
C13 C14 1.391(7) . ?
C13 C12 1.475(8) . ?
C28 H28 0.9500 . ?
C14 H14 0.9500 . ?
C14 C15 1.375(9) . ?
C12 C11 1.389(7) . ?
C16 H16 0.9500 . ?
C16 C15 1.389(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.374(10) . ?
C15 H15 0.9500 . ?
C11 H11 0.9500 . ?
C11 C10 1.384(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
O1 C31 1.206(9) . ?
C10 H10 0.9500 . ?
C31 C30 1.495(11) . ?
C31 C32 1.471(15) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
P1 F6 1.6462 . ?
P1 F1 1.6457 . ?
P1 F5 1.6459 . ?
P1 F2 1.6457 . ?
P1 F3 1.6463 . ?
P1 F4 1.6459 . ?
P1 F6A 1.513(10) . ?
P1 F5A 1.762(10) . ?
P1 F3A 1.550(10) . ?
P1 F4A 1.688(10) . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Ir1 N7 170.98(14) . . ?
N6 Ir1 N5 91.81(14) . . ?
N6 Ir1 N4 95.41(16) . . ?
N7 Ir1 N5 95.11(14) . . ?
N7 Ir1 N4 91.90(14) . . ?
C29 Ir1 N6 93.14(17) . . ?
C29 Ir1 N7 80.49(17) . . ?
C29 Ir1 N5 173.04(16) . . ?
C29 Ir1 N4 98.72(16) . . ?
N4 Ir1 N5 75.94(14) . . ?
C18 Ir1 N6 80.86(19) . . ?
C18 Ir1 N7 92.94(17) . . ?
C18 Ir1 N5 93.26(15) . . ?
C18 Ir1 C29 92.35(17) . . ?
C18 Ir1 N4 168.52(15) . . ?
C8 N6 Ir1 124.2(3) . . ?
C8 N6 C12 120.0(4) . . ?
C12 N6 Ir1 115.7(3) . . ?
C23 N7 Ir1 115.5(3) . . ?
C19 N7 Ir1 124.7(3) . . ?
C19 N7 C23 119.4(4) . . ?
C3 N5 Ir1 116.5(3) . . ?
C7 N5 Ir1 125.9(3) . . ?
C7 N5 C3 117.6(4) . . ?
N1 N2 C1 122.6(4) . . ?
N3 N2 N1 114.9(4) . . ?
N3 N2 C1 122.4(4) . . ?
C2 N1 N2 101.2(4) . . ?
C24 C29 Ir1 114.1(3) . . ?
C28 C29 Ir1 128.7(4) . . ?
C28 C29 C24 117.2(4) . . ?
N2 N3 N4 105.1(4) . . ?
N3 N4 Ir1 138.9(3) . . ?
N3 N4 C2 106.8(4) . . ?
C2 N4 Ir1 114.2(3) . . ?
N5 C3 C4 123.2(4) . . ?
N5 C3 C2 113.6(4) . . ?
C4 C3 C2 123.3(4) . . ?
C17 C18 Ir1 128.0(3) . . ?
C17 C18 C13 117.2(4) . . ?
C13 C18 Ir1 114.3(4) . . ?
N7 C23 C24 114.3(4) . . ?
N7 C23 C22 120.1(4) . . ?
C22 C23 C24 125.4(4) . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.7(4) . . ?
C5 C4 H4 120.6 . . ?
N5 C7 H7 118.8 . . ?
N5 C7 C6 122.3(4) . . ?
C6 C7 H7 118.8 . . ?
C4 C5 H5 120.6 . . ?
C6 C5 C4 118.8(4) . . ?
C6 C5 H5 120.6 . . ?
C29 C24 C23 115.2(4) . . ?
C25 C24 C29 121.6(4) . . ?
C25 C24 C23 123.1(4) . . ?
C26 C27 H27 119.8 . . ?
C26 C27 C28 120.4(5) . . ?
C28 C27 H27 119.8 . . ?
C18 C17 H17 119.5 . . ?
C16 C17 C18 120.9(5) . . ?
C16 C17 H17 119.5 . . ?
N1 C2 N4 112.0(4) . . ?
N1 C2 C3 128.4(4) . . ?
N4 C2 C3 119.6(4) . . ?
N6 C8 H8 119.3 . . ?
N6 C8 C9 121.5(5) . . ?
C9 C8 H8 119.3 . . ?
C7 C6 H6 120.3 . . ?
C5 C6 C7 119.3(4) . . ?
C5 C6 H6 120.3 . . ?
C23 C22 H22 119.9 . . ?
C21 C22 C23 120.2(5) . . ?
C21 C22 H22 119.9 . . ?
C27 C26 H26 120.2 . . ?
C25 C26 C27 119.5(4) . . ?
C25 C26 H26 120.2 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 119.9(5) . . ?
C26 C25 H25 120.0 . . ?
C22 C21 H21 120.1 . . ?
C22 C21 C20 119.8(5) . . ?
C20 C21 H21 120.1 . . ?
C21 C20 H20 120.8 . . ?
C19 C20 C21 118.3(5) . . ?
C19 C20 H20 120.8 . . ?
N7 C19 C20 122.3(5) . . ?
N7 C19 H19 118.9 . . ?
C20 C19 H19 118.9 . . ?
C18 C13 C12 115.0(4) . . ?
C14 C13 C18 121.5(5) . . ?
C14 C13 C12 123.4(4) . . ?
C29 C28 C27 121.4(5) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.7(5) . . ?
C15 C14 H14 120.2 . . ?
N6 C12 C13 114.0(4) . . ?
N6 C12 C11 119.7(5) . . ?
C11 C12 C13 126.2(5) . . ?
C17 C16 H16 119.6 . . ?
C17 C16 C15 120.9(5) . . ?
C15 C16 H16 119.6 . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.4(6) . . ?
C10 C9 H9 120.3 . . ?
C14 C15 C16 119.8(5) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 C12 119.9(6) . . ?
C10 C11 H11 120.0 . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C9 C10 C11 119.4(5) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
O1 C31 C30 120.4(8) . . ?
O1 C31 C32 122.8(9) . . ?
C32 C31 C30 116.8(8) . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C31 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
F6 P1 F3 90.0 . . ?
F1 P1 F6 90.0 . . ?
F1 P1 F5 90.0 . . ?
F1 P1 F2 180.0 . . ?
F1 P1 F3 90.0 . . ?
F1 P1 F4 90.0 . . ?
F1 P1 F5A 98.7(6) . . ?
F1 P1 F4A 95.5(6) . . ?
F5 P1 F6 180.0 . . ?
F5 P1 F3 90.0 . . ?
F5 P1 F4 90.0 . . ?
F2 P1 F6 90.0 . . ?
F2 P1 F5 90.0 . . ?
F2 P1 F3 90.0 . . ?
F2 P1 F4 90.0 . . ?
F2 P1 F5A 81.3(6) . . ?
F2 P1 F4A 84.5(6) . . ?
F4 P1 F6 90.0 . . ?
F4 P1 F3 180.0 . . ?
F6A P1 F1 81.4(6) . . ?
F6A P1 F2 98.6(6) . . ?
F6A P1 F5A 166.9(6) . . ?
F6A P1 F3A 111.2(7) . . ?
F6A P1 F4A 87.7(6) . . ?
F3A P1 F1 84.6(7) . . ?
F3A P1 F2 95.4(7) . . ?
F3A P1 F5A 81.8(6) . . ?
F3A P1 F4A 160.8(7) . . ?
F4A P1 F5A 79.2(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ir1 N6 C8 C9 176.5(4) . . . . ?
Ir1 N6 C12 C13 0.2(5) . . . . ?
Ir1 N6 C12 C11 -177.8(4) . . . . ?
Ir1 N7 C23 C24 2.8(5) . . . . ?
Ir1 N7 C23 C22 -172.6(3) . . . . ?
Ir1 N7 C19 C20 171.3(4) . . . . ?
Ir1 N5 C3 C4 178.6(3) . . . . ?
Ir1 N5 C3 C2 -0.9(5) . . . . ?
Ir1 N5 C7 C6 -179.6(3) . . . . ?
Ir1 C29 C24 C23 6.7(5) . . . . ?
Ir1 C29 C24 C25 -176.1(3) . . . . ?
Ir1 C29 C28 C27 177.2(4) . . . . ?
Ir1 N4 C2 N1 176.3(3) . . . . ?
Ir1 N4 C2 C3 -5.2(5) . . . . ?
Ir1 C18 C17 C16 171.9(4) . . . . ?
Ir1 C18 C13 C14 -173.8(4) . . . . ?
Ir1 C18 C13 C12 3.5(5) . . . . ?
N6 C8 C9 C10 1.3(7) . . . . ?
N6 C12 C11 C10 0.6(8) . . . . ?
N7 C23 C24 C29 -6.3(6) . . . . ?
N7 C23 C24 C25 176.7(4) . . . . ?
N7 C23 C22 C21 0.5(7) . . . . ?
N5 C3 C4 C5 1.4(6) . . . . ?
N5 C3 C2 N1 -177.8(4) . . . . ?
N5 C3 C2 N4 4.1(6) . . . . ?
N5 C7 C6 C5 0.4(7) . . . . ?
N2 N1 C2 N4 0.6(5) . . . . ?
N2 N1 C2 C3 -177.7(4) . . . . ?
N2 N3 N4 Ir1 -175.4(4) . . . . ?
N2 N3 N4 C2 0.7(5) . . . . ?
N1 N2 N3 N4 -0.4(5) . . . . ?
C29 C24 C25 C26 -2.3(7) . . . . ?
N3 N2 N1 C2 -0.1(5) . . . . ?
N3 N4 C2 N1 -0.8(5) . . . . ?
N3 N4 C2 C3 177.6(4) . . . . ?
C3 N5 C7 C6 1.0(6) . . . . ?
C3 C4 C5 C6 0.2(6) . . . . ?
C18 C17 C16 C15 1.1(7) . . . . ?
C18 C13 C14 C15 0.4(7) . . . . ?
C18 C13 C12 N6 -2.4(6) . . . . ?
C18 C13 C12 C11 175.5(5) . . . . ?
C23 N7 C19 C20 -1.1(7) . . . . ?
C23 C24 C25 C26 174.6(4) . . . . ?
C23 C22 C21 C20 -1.0(8) . . . . ?
C4 C3 C2 N1 2.8(7) . . . . ?
C4 C3 C2 N4 -175.3(4) . . . . ?
C4 C5 C6 C7 -1.0(7) . . . . ?
C7 N5 C3 C4 -2.0(6) . . . . ?
C7 N5 C3 C2 178.5(4) . . . . ?
C24 C29 C28 C27 -1.2(7) . . . . ?
C24 C23 C22 C21 -174.3(5) . . . . ?
C27 C26 C25 C24 0.8(7) . . . . ?
C17 C18 C13 C14 -0.8(7) . . . . ?
C17 C18 C13 C12 176.5(4) . . . . ?
C17 C16 C15 C14 -1.5(8) . . . . ?
C2 C3 C4 C5 -179.2(4) . . . . ?
C8 N6 C12 C13 176.7(4) . . . . ?
C8 N6 C12 C11 -1.3(7) . . . . ?
C8 C9 C10 C11 -2.0(8) . . . . ?
C22 C23 C24 C29 168.8(4) . . . . ?
C22 C23 C24 C25 -8.2(7) . . . . ?
C22 C21 C20 C19 0.5(8) . . . . ?
C26 C27 C28 C29 -0.2(8) . . . . ?
C21 C20 C19 N7 0.6(8) . . . . ?
C19 N7 C23 C24 175.9(4) . . . . ?
C19 N7 C23 C22 0.5(6) . . . . ?
C13 C18 C17 C16 0.0(7) . . . . ?
C13 C14 C15 C16 0.7(8) . . . . ?
C13 C12 C11 C10 -177.1(5) . . . . ?
C28 C29 C24 C23 -174.6(4) . . . . ?
C28 C29 C24 C25 2.5(7) . . . . ?
C28 C27 C26 C25 0.4(8) . . . . ?
C14 C13 C12 N6 174.8(4) . . . . ?
C14 C13 C12 C11 -7.3(8) . . . . ?
C12 N6 C8 C9 0.4(7) . . . . ?
C12 C13 C14 C15 -176.7(5) . . . . ?
C12 C11 C10 C9 1.0(8) . . . . ?
C1 N2 N1 C2 -178.5(5) . . . . ?
C1 N2 N3 N4 178.0(5) . . . . ?

_olex2_exptl_crystal_mounting_method 
'mounted on a glass fibre using silicon oil'
_olex2_submission_original_sample_id 'mxm543rm - IrPTzN2'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.240
_oxdiff_exptl_absorpt_empirical_full_min 0.851

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mxm589rm
_audit_block_doi                 10.5517/ccdc.csd.cc2dlrf6
_database_code_depnum_ccdc_archive 'CCDC 2222558'
loop_
_audit_author_name
_audit_author_address
'Lee Cameron'
;Curtin University
Australia
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
;
_audit_creation_date             2022-10-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C33 H25 Ir N7, F6 P, 0.375[CH2Cl2]'
_chemical_formula_sum            'C33.38 H25.75 Cl0.75 F6 Ir N7 P'
_chemical_formula_weight         888.68
_exptl_crystal_recrystallization_method 
'grown from the evaporation of a dichloromethane and ether solution'
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            'clear yellowish orange'
_diffrn_ambient_temperature      100.00(10)
_chemical_oxdiff_formula         'Ir C40 h28 N6 O P6 F12'
_chemical_oxdiff_usercomment     'Lee Cameron for Ryan Morris'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'
Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_chemical_absolute_configuration .
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.48790(10)
_cell_length_b                   18.7654(4)
_cell_length_c                   41.0127(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.8150(10)
_cell_angle_gamma                90
_cell_volume                     6517.98(19)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    28236
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4060
_cell_measurement_theta_min      4.3100
_shelx_estimated_absorpt_T_max   0.570
_shelx_estimated_absorpt_T_min   0.413
_exptl_absorpt_coefficient_mu    9.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3470
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 5 0 0.0785
-2 7 21 0.0541
-5 -6 -3 0.0151
0 -8 -20 0.0133
5 2 -6 0.0621
0 9 -24 0.0388
-5 2 -11 0.0266
-3 -5 21 0.0226
2 -5 23 0.0264

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.066
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.0911 4.6015 0.0649 0.2414 -0.2539 -0.9366
-1.5208 7.0457 20.8702 0.6472 -0.6830 0.3386
-4.7925 -5.6065 -3.2237 -0.3361 0.3539 0.8728
0.4071 -7.8401 -20.3582 -0.6819 0.7194 -0.1323
5.4086 1.5106 -5.6288 -0.0275 -0.0640 -0.9976
0.1092 8.5815 -24.1594 0.6519 0.8928 -0.3159
-4.7242 2.1070 -11.3717 0.2740 0.6589 0.7006
-3.0960 -4.5255 20.6239 -0.2513 -0.6076 0.7535
1.7209 -4.6424 22.5622 -0.3825 -0.9219 -0.0621

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            64395
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.567
_diffrn_reflns_theta_min         2.590
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     49.00 119.00   0.50    0.08    --   45.98 163.00-166.00  140
  2  ω     87.00 116.00   0.50    0.08    --   45.98 125.00 -30.00   58
  3  ω     75.00 118.00   0.50    0.08    --   45.98 125.00   0.00   86
  4  ω    103.00 128.00   0.50    0.28    --  102.69 116.00  44.00   50
  5  ω     91.00 171.00   0.50    0.28    --  102.69  45.00 -30.00  160
  6  ω    -27.00  24.00   0.50    0.08    --   45.98 -19.00 -90.00  102
  7  ω     32.00 118.00   0.50    0.08    --   45.98-163.00 167.00  172
  8  ω     48.00  73.00   0.50    0.08    --   45.98-116.00 -43.00   50
  9  ω     31.00  64.00   0.50    0.28    --  102.69 -61.00  90.00   66
 10  ω     35.00 103.00   0.50    0.28    --  102.69 -94.00 150.00  136
 11  ω     60.00  85.00   0.50    0.28    --  102.69-163.00 167.00   50
 12  ω     82.00 109.00   0.50    0.28    --  102.69-116.00 -43.00   54
 13  ω     30.00  77.00   0.50    0.28    --  102.69-116.00 -43.00   94
 14  ω     52.00  78.00   0.50    0.28    --  102.69 -94.00   0.00   52
 15  ω   -118.00 -32.00   0.50    0.08    --  -45.98 163.00-166.00  172
 16  ω    -72.00 -30.00   0.50    0.28    -- -102.69  61.00   0.00   84
 17  ω    -64.00 -30.00   0.50    0.28    -- -102.69  61.00  30.00   68
 18  ω    -72.00 -32.00   0.50    0.28    -- -102.69  61.00 -30.00   80
 19  ω   -109.00 -50.00   0.50    0.28    -- -102.69 116.00  44.00  118
 20  ω    -89.00  -6.00   0.50    0.08    --  -45.98 116.00  44.00  166
 21  ω   -104.00 -31.00   0.50    0.28    -- -102.69  77.00 120.00  146
 22  ω    -72.00 -34.00   0.50    0.08    --  -45.98 -37.00 -30.00   76
 23  ω   -174.00 -93.00   0.50    0.28    -- -102.69 -45.00 150.00  162
 24  ω   -119.00 -88.00   0.50    0.08    --  -45.98 -37.00 -30.00   62
 25  ω   -127.00 -87.00   0.50    0.28    -- -102.69 -61.00-120.00   80
 26  ω   -140.00 -81.00   0.50    0.28    -- -102.69-116.00 -43.00  118
 27  ω   -118.00 -73.00   0.50    0.08    --  -45.98-125.00   0.00   90
 28  ω   -104.00 -79.00   0.50    0.08    --  -45.98-125.00  30.00   50
 29  ω   -118.00 -48.00   0.50    0.08    --  -45.98-163.00 167.00  140
 30  ω   -126.00-101.00   0.50    0.28    -- -102.69-163.00 167.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0259510000
_diffrn_orient_matrix_UB_12      0.0811479000
_diffrn_orient_matrix_UB_13      0.0017247000
_diffrn_orient_matrix_UB_21      -0.0504273000
_diffrn_orient_matrix_UB_22      0.0011303000
_diffrn_orient_matrix_UB_23      -0.0367808000
_diffrn_orient_matrix_UB_31      -0.1727783000
_diffrn_orient_matrix_UB_32      -0.0124958000
_diffrn_orient_matrix_UB_33      0.0078547000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11849
_reflns_number_total             12976
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.949
_refine_diff_density_min         -2.196
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         12976
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0514
_refine_ls_restrained_S_all      1.159
_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)+(0.0151P)²+58.5742P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1134
_refine_special_details          ?
_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.a Aromatic/amide H refined with riding coordinates:
 C51(H51), C12(H12), C13(H13), C56(H56), C10(H10), C4(H4), C54(H54), C46(H46),
 C42(H42), C64(H64), C43(H43), C24(H24), C57(H57), C23(H23), C21(H21), C32(H32),
  C53(H53), C31(H31), C20(H20), C65(H65), C15(H15), C48(H48), C14(H14),
 C30(H30), C59(H59), C18(H18), C52(H52), C45(H45), C7(H7), C47(H47), C19(H19),
 C29(H29), C38(H38), C41(H41), C26(H26), C62(H62), C25(H25), C5(H5), C63(H63),
 C37(H37), C58(H58), C8(H8), C9(H9), C40(H40)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C34(H34A,H34B,H34C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir2 Ir 0.04751(3) 0.86044(2) 0.60301(2) 0.02405(8) Uani 1 1 d . . . . .
Ir1 Ir -0.00885(3) 0.32819(2) 0.66405(2) 0.02459(8) Uani 1 1 d . . . . .
P1 P 0.5376(2) 0.55194(11) 0.70967(5) 0.0395(4) Uani 1 1 d . . . . .
P2 P -0.4773(2) 0.80537(13) 0.50036(5) 0.0422(5) Uani 1 1 d . . . . .
F3 F 0.4373(6) 0.6228(2) 0.71481(12) 0.0502(12) Uani 1 1 d . . . . .
F6 F 0.6363(6) 0.4796(3) 0.70512(13) 0.0602(14) Uani 1 1 d . . . . .
F2 F 0.5901(6) 0.5506(3) 0.74780(11) 0.0477(11) Uani 1 1 d . . . . .
F4 F 0.3861(6) 0.5049(3) 0.71642(13) 0.0552(13) Uani 1 1 d . . . . .
F12 F -0.4074(6) 0.7433(3) 0.47890(11) 0.0540(13) Uani 1 1 d . . . . .
F8 F -0.5481(6) 0.8665(3) 0.52234(11) 0.0582(14) Uani 1 1 d . . . . .
F7 F -0.3140(6) 0.8471(3) 0.50008(14) 0.0575(13) Uani 1 1 d . . . . .
N13 N -0.1398(7) 0.9303(3) 0.59759(13) 0.0258(11) Uani 1 1 d . . . . .
N11 N 0.1079(7) 0.8905(3) 0.55536(12) 0.0272(12) Uani 1 1 d . . . . .
N4 N -0.0747(7) 0.3892(3) 0.70500(12) 0.0264(12) Uani 1 1 d . . . . .
F9 F -0.4128(6) 0.7649(3) 0.53297(11) 0.0597(14) Uani 1 1 d . . . . .
N6 N 0.1913(7) 0.3019(3) 0.69241(13) 0.0267(12) Uani 1 1 d . . . . .
F11 F -0.5409(7) 0.8463(3) 0.46809(12) 0.0652(15) Uani 1 1 d . . . . .
N14 N 0.2393(7) 0.7982(3) 0.61553(13) 0.0282(12) Uani 1 1 d . . . . .
F1 F 0.6917(6) 0.5988(3) 0.70378(13) 0.0614(14) Uani 1 1 d . . . . .
N7 N -0.2095(6) 0.3395(3) 0.63360(12) 0.0262(12) Uani 1 1 d . . . . .
N9 N 0.1554(7) 0.9372(3) 0.51082(14) 0.0340(13) Uani 1 1 d . . . . .
N8 N 0.0888(7) 0.8757(4) 0.50199(14) 0.0359(14) Uani 1 1 d . . . . .
N2 N -0.1122(7) 0.4326(3) 0.75045(13) 0.0303(13) Uani 1 1 d . . . . .
F5 F 0.4884(6) 0.5531(3) 0.67143(12) 0.0649(16) Uani 1 1 d . . . . .
N5 N 0.0643(7) 0.4421(3) 0.65309(13) 0.0265(12) Uani 1 1 d . . . . .
N12 N -0.0409(7) 0.7687(3) 0.56929(13) 0.0292(12) Uani 1 1 d . . . . .
C33 C 0.0538(9) 0.2697(4) 0.62553(15) 0.0300(15) Uani 1 1 d . . . . .
F10 F -0.6406(6) 0.7627(4) 0.50088(16) 0.0759(18) Uani 1 1 d . . . . .
N3 N -0.1356(7) 0.3733(3) 0.73315(13) 0.0284(12) Uani 1 1 d . . . . .
N10 N 0.1699(7) 0.9484(3) 0.54272(13) 0.0305(13) Uani 1 1 d . . . . .
N1 N -0.0390(7) 0.4855(3) 0.73563(13) 0.0327(13) Uani 1 1 d . . . . .
C66 C -0.0084(8) 0.8285(4) 0.64802(14) 0.0275(14) Uani 1 1 d . . . . .
C60 C 0.2515(9) 0.7752(4) 0.64727(16) 0.0310(15) Uani 1 1 d . . . . .
C28 C -0.0713(8) 0.2565(4) 0.60187(16) 0.0301(15) Uani 1 1 d . . . . .
C17 C 0.0365(8) 0.2018(4) 0.70430(14) 0.0265(14) Uani 1 1 d . . . . .
C22 C -0.0801(8) 0.2351(3) 0.68269(14) 0.0247(13) Uani 1 1 d . . . . .
C11 C 0.1193(8) 0.4709(4) 0.62503(16) 0.0297(15) Uani 1 1 d . . . . .
C2 C -0.0179(8) 0.4554(4) 0.70668(15) 0.0257(13) Uani 1 1 d . . . . .
C55 C 0.1445(8) 0.9471(4) 0.62583(14) 0.0274(14) Uani 1 1 d . . . . .
C49 C -0.1168(8) 0.9955(4) 0.61172(15) 0.0291(14) Uani 1 1 d . . . . .
C16 C 0.1876(8) 0.2387(4) 0.70850(15) 0.0264(14) Uani 1 1 d . . . . .
C51 C 0.0925(9) 1.0683(4) 0.64283(16) 0.0312(15) Uani 1 1 d . . . . .
H51 H 0.022462 1.107636 0.643759 0.037 Uiso 1 1 calc R U . . .
C12 C 0.3250(8) 0.3426(4) 0.69524(16) 0.0292(14) Uani 1 1 d . . . . .
H12 H 0.326219 0.387345 0.684430 0.035 Uiso 1 1 calc R U . . .
C13 C 0.4569(8) 0.3203(4) 0.71327(17) 0.0327(15) Uani 1 1 d . . . . .
H13 H 0.548905 0.349248 0.714805 0.039 Uiso 1 1 calc R U . . .
C35 C 0.0582(8) 0.8471(4) 0.53098(14) 0.0279(14) Uani 1 1 d . . . . .
C56 C 0.3602(8) 0.7861(4) 0.59642(17) 0.0319(15) Uani 1 1 d . . . . .
H56 H 0.352016 0.802453 0.574452 0.038 Uiso 1 1 calc R U . . .
C50 C 0.0424(8) 1.0043(4) 0.62751(15) 0.0300(15) Uani 1 1 d . . . . .
C3 C 0.0483(8) 0.4872(4) 0.67811(17) 0.0297(14) Uani 1 1 d . . . . .
C61 C 0.1110(9) 0.7880(4) 0.66495(15) 0.0304(15) Uani 1 1 d . . . . .
C10 C 0.1283(9) 0.4287(5) 0.59720(17) 0.0390(17) Uani 1 1 d . . . . .
H10 H 0.092868 0.380669 0.597430 0.047 Uiso 1 1 calc R U . . .
C4 C 0.0920(8) 0.5589(4) 0.67870(18) 0.0330(15) Uani 1 1 d . . . . .
H4 H 0.079580 0.587486 0.697464 0.040 Uiso 1 1 calc R U . . .
C54 C 0.2978(8) 0.9524(4) 0.63970(15) 0.0310(15) Uani 1 1 d . . . . .
H54 H 0.368151 0.913144 0.638840 0.037 Uiso 1 1 calc R U . . .
C46 C -0.4054(9) 0.9619(4) 0.58072(16) 0.0336(16) Uani 1 1 d . . . . .
H46 H -0.504446 0.949376 0.570129 0.040 Uiso 1 1 calc R U . . .
C42 C -0.1958(9) 0.6217(4) 0.6174(2) 0.0396(18) Uani 1 1 d . . . . .
H42 H -0.214349 0.611700 0.639571 0.048 Uiso 1 1 calc R U . . .
C64 C -0.1693(9) 0.8146(4) 0.69421(17) 0.0389(18) Uani 1 1 d . . . . .
H64 H -0.264018 0.824113 0.704522 0.047 Uiso 1 1 calc R U . . .
C6 C 0.1684(9) 0.5425(4) 0.62386(18) 0.0351(16) Uani 1 1 d . . . . .
C43 C -0.1327(8) 0.6865(4) 0.60928(18) 0.0321(15) Uani 1 1 d . . . . .
H43 H -0.108443 0.720635 0.625959 0.039 Uiso 1 1 calc R U . . .
C27 C -0.2173(8) 0.2962(4) 0.60672(16) 0.0313(15) Uani 1 1 d . . . . .
C24 C -0.4646(9) 0.3844(4) 0.61913(17) 0.0380(17) Uani 1 1 d . . . . .
H24 H -0.547216 0.416911 0.622990 0.046 Uiso 1 1 calc R U . . .
C57 C 0.4954(9) 0.7506(4) 0.60794(19) 0.0386(17) Uani 1 1 d . . . . .
H57 H 0.576586 0.740237 0.593778 0.046 Uiso 1 1 calc R U . . .
C23 C -0.3301(8) 0.3829(4) 0.63944(16) 0.0294(14) Uani 1 1 d . . . . .
H23 H -0.322001 0.413066 0.658057 0.035 Uiso 1 1 calc R U . . .
C21 C -0.2266(9) 0.2033(4) 0.67818(16) 0.0317(15) Uani 1 1 d . . . . .
H21 H -0.304427 0.223894 0.663344 0.038 Uiso 1 1 calc R U . . .
C32 C 0.2018(8) 0.2405(4) 0.62037(16) 0.0312(15) Uani 1 1 d . . . . .
H32 H 0.288391 0.249068 0.635747 0.037 Uiso 1 1 calc R U . . .
C1 C -0.1676(10) 0.4402(4) 0.78309(16) 0.0379(17) Uani 1 1 d . . . . .
H1A H -0.265004 0.468465 0.781967 0.057 Uiso 1 1 calc R U . . .
H1B H -0.086735 0.464402 0.797227 0.057 Uiso 1 1 calc R U . . .
H1C H -0.188498 0.393021 0.792043 0.057 Uiso 1 1 calc R U . . .
C44 C -0.1037(8) 0.7029(4) 0.57701(18) 0.0329(15) Uani 1 1 d . . . . .
C53 C 0.3477(9) 1.0159(4) 0.65497(16) 0.0342(16) Uani 1 1 d . . . . .
H53 H 0.452767 1.019833 0.664340 0.041 Uiso 1 1 calc R U . . .
C31 C 0.2230(9) 0.1989(4) 0.59284(17) 0.0366(17) Uani 1 1 d . . . . .
H31 H 0.324652 0.180439 0.589222 0.044 Uiso 1 1 calc R U . . .
C20 C -0.2619(9) 0.1417(4) 0.69502(17) 0.0336(15) Uani 1 1 d . . . . .
H20 H -0.364565 0.121598 0.692039 0.040 Uiso 1 1 calc R U . . .
C65 C -0.1479(9) 0.8426(4) 0.66331(16) 0.0317(15) Uani 1 1 d . . . . .
H65 H -0.227862 0.871315 0.652628 0.038 Uiso 1 1 calc R U . . .
C15 C 0.3192(8) 0.2151(4) 0.72699(16) 0.0305(15) Uani 1 1 d . . . . .
H15 H 0.315341 0.170907 0.738183 0.037 Uiso 1 1 calc R U . . .
C36 C -0.0135(8) 0.7799(4) 0.53779(16) 0.0321(16) Uani 1 1 d . . . . .
C48 C -0.2381(9) 1.0454(4) 0.61021(17) 0.0348(16) Uani 1 1 d . . . . .
H48 H -0.221869 1.091205 0.619724 0.042 Uiso 1 1 calc R U . . .
C14 C 0.4560(8) 0.2548(4) 0.72948(16) 0.0348(16) Uani 1 1 d . . . . .
H14 H 0.547164 0.238038 0.741844 0.042 Uiso 1 1 calc R U . . .
C30 C 0.0956(10) 0.1842(4) 0.57059(17) 0.0394(18) Uani 1 1 d . . . . .
H30 H 0.109174 0.153749 0.552485 0.047 Uiso 1 1 calc R U . . .
C59 C 0.3876(9) 0.7426(4) 0.66015(18) 0.0368(17) Uani 1 1 d . . . . .
H59 H 0.396237 0.728645 0.682473 0.044 Uiso 1 1 calc R U . . .
C18 C 0.0008(9) 0.1396(4) 0.72074(16) 0.0312(15) Uani 1 1 d . . . . .
H18 H 0.078928 0.117757 0.735122 0.037 Uiso 1 1 calc R U . . .
C52 C 0.2462(9) 1.0728(4) 0.65656(17) 0.0361(17) Uani 1 1 d . . . . .
H52 H 0.281610 1.115468 0.667129 0.043 Uiso 1 1 calc R U . . .
C45 C -0.2820(7) 0.9141(4) 0.58226(15) 0.0291(15) Uani 1 1 d . . . . .
H45 H -0.296804 0.868641 0.572333 0.035 Uiso 1 1 calc R U . . .
C34 C 0.2226(9) 0.9859(4) 0.48751(17) 0.0400(18) Uani 1 1 d . . . . .
H34A H 0.320219 0.965447 0.480082 0.060 Uiso 1 1 calc R U . . .
H34B H 0.245732 1.031791 0.498149 0.060 Uiso 1 1 calc R U . . .
H34C H 0.146683 0.992910 0.468718 0.060 Uiso 1 1 calc R U . . .
C39 C -0.1374(10) 0.6506(4) 0.5528(2) 0.0443(19) Uani 1 1 d . . . . .
C7 C 0.2304(10) 0.5695(5) 0.5950(2) 0.048(2) Uani 1 1 d . . . . .
H7 H 0.266449 0.617370 0.594423 0.058 Uiso 1 1 calc R U . . .
C47 C -0.3832(9) 1.0277(4) 0.59465(17) 0.0388(18) Uani 1 1 d . . . . .
H47 H -0.467128 1.061272 0.593696 0.047 Uiso 1 1 calc R U . . .
C19 C -0.1486(9) 0.1090(4) 0.71624(17) 0.0346(16) Uani 1 1 d . . . . .
H19 H -0.173083 0.066581 0.727461 0.041 Uiso 1 1 calc R U . . .
C29 C -0.0506(9) 0.2140(4) 0.57494(17) 0.0369(17) Uani 1 1 d . . . . .
H29 H -0.136697 0.205319 0.559444 0.044 Uiso 1 1 calc R U . . .
C38 C -0.1063(12) 0.6656(5) 0.5202(2) 0.057(2) Uani 1 1 d . . . . .
H38 H -0.129689 0.631269 0.503534 0.068 Uiso 1 1 calc R U . . .
C41 C -0.2331(10) 0.5701(5) 0.5931(2) 0.048(2) Uani 1 1 d . . . . .
H41 H -0.278283 0.525784 0.598649 0.058 Uiso 1 1 calc R U . . .
C26 C -0.3539(9) 0.2942(5) 0.58653(18) 0.0410(18) Uani 1 1 d . . . . .
H26 H -0.361933 0.262744 0.568339 0.049 Uiso 1 1 calc R U . . .
C62 C 0.0869(9) 0.7599(4) 0.69583(17) 0.0356(16) Uani 1 1 d . . . . .
H62 H 0.166486 0.731951 0.707041 0.043 Uiso 1 1 calc R U . . .
C25 C -0.4787(9) 0.3379(5) 0.59281(18) 0.046(2) Uani 1 1 d . . . . .
H25 H -0.573664 0.336224 0.579207 0.055 Uiso 1 1 calc R U . . .
C5 C 0.1530(9) 0.5865(4) 0.6515(2) 0.0401(18) Uani 1 1 d . . . . .
H5 H 0.184911 0.635014 0.651139 0.048 Uiso 1 1 calc R U . . .
C63 C -0.0532(10) 0.7731(4) 0.70983(17) 0.0415(19) Uani 1 1 d . . . . .
H63 H -0.070211 0.753301 0.730618 0.050 Uiso 1 1 calc R U . . .
C37 C -0.0428(11) 0.7292(5) 0.5128(2) 0.048(2) Uani 1 1 d . . . . .
H37 H -0.018358 0.739552 0.491018 0.058 Uiso 1 1 calc R U . . .
C58 C 0.5106(9) 0.7302(4) 0.6407(2) 0.0416(18) Uani 1 1 d . . . . .
H58 H 0.604701 0.708002 0.649458 0.050 Uiso 1 1 calc R U . . .
C8 C 0.2386(12) 0.5271(5) 0.5683(2) 0.055(2) Uani 1 1 d . . . . .
H8 H 0.278327 0.545557 0.548899 0.066 Uiso 1 1 calc R U . . .
C9 C 0.1881(11) 0.4559(5) 0.5694(2) 0.049(2) Uani 1 1 d . . . . .
H9 H 0.195347 0.426212 0.550833 0.059 Uiso 1 1 calc R U . . .
C40 C -0.2032(11) 0.5849(5) 0.5617(2) 0.052(2) Uani 1 1 d . . . . .
H40 H -0.227311 0.550148 0.545300 0.062 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir2 N13 2.061(5) . ?
Ir2 N11 2.129(5) . ?
Ir2 N14 2.042(6) . ?
Ir2 N12 2.303(6) . ?
Ir2 C66 2.027(6) . ?
Ir2 C55 2.024(7) . ?
Ir1 N4 2.137(5) . ?
Ir1 N6 2.054(6) . ?
Ir1 N7 2.055(5) . ?
Ir1 N5 2.279(5) . ?
Ir1 C33 2.023(6) . ?
Ir1 C22 2.016(6) . ?
P1 F3 1.600(5) . ?
P1 F6 1.613(5) . ?
P1 F2 1.597(5) . ?
P1 F4 1.599(6) . ?
P1 F1 1.608(6) . ?
P1 F5 1.596(5) . ?
P2 F12 1.598(5) . ?
P2 F8 1.600(5) . ?
P2 F7 1.592(5) . ?
P2 F9 1.602(5) . ?
P2 F11 1.593(6) . ?
P2 F10 1.603(6) . ?
N13 C49 1.363(9) . ?
N13 C45 1.358(9) . ?
N11 N10 1.327(8) . ?
N11 C35 1.336(8) . ?
N4 N3 1.330(7) . ?
N4 C2 1.334(8) . ?
N6 C16 1.360(8) . ?
N6 C12 1.366(8) . ?
N14 C60 1.369(8) . ?
N14 C56 1.351(9) . ?
N7 C27 1.368(8) . ?
N7 C23 1.342(9) . ?
N9 N8 1.324(9) . ?
N9 N10 1.323(8) . ?
N9 C34 1.465(9) . ?
N8 C35 1.346(8) . ?
N2 N3 1.327(8) . ?
N2 N1 1.339(8) . ?
N2 C1 1.455(8) . ?
N5 C11 1.381(8) . ?
N5 C3 1.344(9) . ?
N12 C44 1.390(9) . ?
N12 C36 1.345(9) . ?
C33 C28 1.412(10) . ?
C33 C32 1.399(10) . ?
N1 C2 1.338(8) . ?
C66 C61 1.411(10) . ?
C66 C65 1.402(10) . ?
C60 C61 1.456(10) . ?
C60 C59 1.381(10) . ?
C28 C27 1.470(10) . ?
C28 C29 1.383(9) . ?
C17 C22 1.428(9) . ?
C17 C16 1.457(9) . ?
C17 C18 1.392(9) . ?
C22 C21 1.380(10) . ?
C11 C10 1.396(10) . ?
C11 C6 1.409(10) . ?
C2 C3 1.460(9) . ?
C55 C50 1.383(10) . ?
C55 C54 1.388(10) . ?
C49 C50 1.469(10) . ?
C49 C48 1.390(10) . ?
C16 C15 1.380(10) . ?
C51 H51 0.9500 . ?
C51 C50 1.408(10) . ?
C51 C52 1.389(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.366(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.399(11) . ?
C35 C36 1.436(10) . ?
C56 H56 0.9500 . ?
C56 C57 1.383(10) . ?
C3 C4 1.395(10) . ?
C61 C62 1.399(9) . ?
C10 H10 0.9500 . ?
C10 C9 1.375(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.362(11) . ?
C54 H54 0.9500 . ?
C54 C53 1.400(10) . ?
C46 H46 0.9500 . ?
C46 C45 1.377(10) . ?
C46 C47 1.368(11) . ?
C42 H42 0.9500 . ?
C42 C43 1.379(10) . ?
C42 C41 1.409(12) . ?
C64 H64 0.9500 . ?
C64 C65 1.395(9) . ?
C64 C63 1.380(12) . ?
C6 C7 1.419(11) . ?
C6 C5 1.417(11) . ?
C43 H43 0.9500 . ?
C43 C44 1.397(10) . ?
C27 C26 1.380(10) . ?
C24 H24 0.9500 . ?
C24 C23 1.368(10) . ?
C24 C25 1.387(11) . ?
C57 H57 0.9500 . ?
C57 C58 1.394(10) . ?
C23 H23 0.9500 . ?
C21 H21 0.9500 . ?
C21 C20 1.389(10) . ?
C32 H32 0.9500 . ?
C32 C31 1.395(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C44 C39 1.412(11) . ?
C53 H53 0.9500 . ?
C53 C52 1.375(11) . ?
C31 H31 0.9500 . ?
C31 C30 1.396(11) . ?
C20 H20 0.9500 . ?
C20 C19 1.395(10) . ?
C65 H65 0.9500 . ?
C15 H15 0.9500 . ?
C15 C14 1.377(10) . ?
C36 C37 1.409(10) . ?
C48 H48 0.9500 . ?
C48 C47 1.390(11) . ?
C14 H14 0.9500 . ?
C30 H30 0.9500 . ?
C30 C29 1.384(11) . ?
C59 H59 0.9500 . ?
C59 C58 1.376(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.393(10) . ?
C52 H52 0.9500 . ?
C45 H45 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C39 C38 1.408(12) . ?
C39 C40 1.412(11) . ?
C7 H7 0.9500 . ?
C7 C8 1.361(13) . ?
C47 H47 0.9500 . ?
C19 H19 0.9500 . ?
C29 H29 0.9500 . ?
C38 H38 0.9500 . ?
C38 C37 1.353(12) . ?
C41 H41 0.9500 . ?
C41 C40 1.359(12) . ?
C26 H26 0.9500 . ?
C26 C25 1.377(11) . ?
C62 H62 0.9500 . ?
C62 C63 1.377(11) . ?
C25 H25 0.9500 . ?
C5 H5 0.9500 . ?
C63 H63 0.9500 . ?
C37 H37 0.9500 . ?
C58 H58 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.405(12) . ?
C9 H9 0.9500 . ?
C40 H40 0.9500 . ?

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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N13 Ir2 N11 87.9(2) . . ?
N13 Ir2 N12 101.1(2) . . ?
N11 Ir2 N12 74.7(2) . . ?
N14 Ir2 N13 171.0(2) . . ?
N14 Ir2 N11 98.4(2) . . ?
N14 Ir2 N12 86.9(2) . . ?
C66 Ir2 N13 93.5(2) . . ?
C66 Ir2 N11 178.1(3) . . ?
C66 Ir2 N14 80.4(3) . . ?
C66 Ir2 N12 103.8(2) . . ?
C55 Ir2 N13 80.0(3) . . ?
C55 Ir2 N11 95.5(2) . . ?
C55 Ir2 N14 92.9(3) . . ?
C55 Ir2 N12 170.0(2) . . ?
C55 Ir2 C66 86.0(3) . . ?
N4 Ir1 N5 75.0(2) . . ?
N6 Ir1 N4 86.2(2) . . ?
N6 Ir1 N7 171.8(2) . . ?
N6 Ir1 N5 96.4(2) . . ?
N7 Ir1 N4 99.9(2) . . ?
N7 Ir1 N5 90.5(2) . . ?
C33 Ir1 N4 179.5(3) . . ?
C33 Ir1 N6 93.5(3) . . ?
C33 Ir1 N7 80.3(3) . . ?
C33 Ir1 N5 105.4(2) . . ?
C22 Ir1 N4 93.8(2) . . ?
C22 Ir1 N6 80.5(2) . . ?
C22 Ir1 N7 93.6(2) . . ?
C22 Ir1 N5 168.6(2) . . ?
C22 Ir1 C33 85.8(3) . . ?
F3 P1 F6 178.6(3) . . ?
F3 P1 F1 90.6(3) . . ?
F2 P1 F3 90.0(3) . . ?
F2 P1 F6 89.2(3) . . ?
F2 P1 F4 89.8(3) . . ?
F2 P1 F1 88.8(3) . . ?
F4 P1 F3 89.7(3) . . ?
F4 P1 F6 89.2(3) . . ?
F4 P1 F1 178.6(3) . . ?
F1 P1 F6 90.6(3) . . ?
F5 P1 F3 90.6(3) . . ?
F5 P1 F6 90.1(3) . . ?
F5 P1 F2 179.0(3) . . ?
F5 P1 F4 90.9(3) . . ?
F5 P1 F1 90.4(3) . . ?
F12 P2 F8 178.9(3) . . ?
F12 P2 F9 89.7(3) . . ?
F12 P2 F10 89.8(3) . . ?
F8 P2 F9 89.4(3) . . ?
F8 P2 F10 89.6(3) . . ?
F7 P2 F12 90.0(3) . . ?
F7 P2 F8 90.7(3) . . ?
F7 P2 F9 89.4(3) . . ?
F7 P2 F11 90.2(3) . . ?
F7 P2 F10 179.4(4) . . ?
F9 P2 F10 90.0(3) . . ?
F11 P2 F12 90.7(3) . . ?
F11 P2 F8 90.2(3) . . ?
F11 P2 F9 179.5(4) . . ?
F11 P2 F10 90.3(4) . . ?
C49 N13 Ir2 115.9(5) . . ?
C45 N13 Ir2 124.3(5) . . ?
C45 N13 C49 119.7(6) . . ?
N10 N11 Ir2 134.5(4) . . ?
N10 N11 C35 108.7(5) . . ?
C35 N11 Ir2 116.2(5) . . ?
N3 N4 Ir1 134.4(4) . . ?
N3 N4 C2 108.9(5) . . ?
C2 N4 Ir1 115.3(4) . . ?
C16 N6 Ir1 116.0(4) . . ?
C16 N6 C12 119.5(6) . . ?
C12 N6 Ir1 124.4(5) . . ?
C60 N14 Ir2 115.3(5) . . ?
C56 N14 Ir2 125.0(5) . . ?
C56 N14 C60 119.1(6) . . ?
C27 N7 Ir1 115.0(5) . . ?
C23 N7 Ir1 124.5(4) . . ?
C23 N7 C27 120.5(6) . . ?
N8 N9 C34 122.8(6) . . ?
N10 N9 N8 114.7(6) . . ?
N10 N9 C34 122.1(6) . . ?
N9 N8 C35 102.1(6) . . ?
N3 N2 N1 115.9(5) . . ?
N3 N2 C1 121.9(6) . . ?
N1 N2 C1 122.2(6) . . ?
C11 N5 Ir1 130.0(4) . . ?
C3 N5 Ir1 113.4(4) . . ?
C3 N5 C11 116.5(6) . . ?
C44 N12 Ir2 130.0(4) . . ?
C36 N12 Ir2 112.9(5) . . ?
C36 N12 C44 116.8(6) . . ?
C28 C33 Ir1 114.0(5) . . ?
C32 C33 Ir1 128.0(5) . . ?
C32 C33 C28 118.0(6) . . ?
N2 N3 N4 102.9(5) . . ?
N9 N10 N11 104.1(5) . . ?
C2 N1 N2 100.6(6) . . ?
C61 C66 Ir2 113.8(5) . . ?
C65 C66 Ir2 127.4(5) . . ?
C65 C66 C61 118.9(6) . . ?
N14 C60 C61 114.2(6) . . ?
N14 C60 C59 120.8(7) . . ?
C59 C60 C61 125.1(6) . . ?
C33 C28 C27 114.9(6) . . ?
C29 C28 C33 121.3(7) . . ?
C29 C28 C27 123.6(6) . . ?
C22 C17 C16 115.7(6) . . ?
C18 C17 C22 120.2(6) . . ?
C18 C17 C16 124.0(6) . . ?
C17 C22 Ir1 113.7(5) . . ?
C21 C22 Ir1 127.8(5) . . ?
C21 C22 C17 118.4(6) . . ?
N5 C11 C10 120.0(7) . . ?
N5 C11 C6 121.3(6) . . ?
C10 C11 C6 118.8(6) . . ?
N4 C2 N1 111.7(6) . . ?
N4 C2 C3 119.7(6) . . ?
N1 C2 C3 128.4(6) . . ?
C50 C55 Ir2 114.2(5) . . ?
C50 C55 C54 119.8(6) . . ?
C54 C55 Ir2 126.0(5) . . ?
N13 C49 C50 113.0(6) . . ?
N13 C49 C48 120.1(7) . . ?
C48 C49 C50 126.9(7) . . ?
N6 C16 C17 114.0(6) . . ?
N6 C16 C15 120.1(6) . . ?
C15 C16 C17 125.9(6) . . ?
C50 C51 H51 120.7 . . ?
C52 C51 H51 120.7 . . ?
C52 C51 C50 118.7(7) . . ?
N6 C12 H12 119.3 . . ?
C13 C12 N6 121.4(7) . . ?
C13 C12 H12 119.3 . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.8(7) . . ?
C14 C13 H13 120.1 . . ?
N11 C35 N8 110.3(6) . . ?
N11 C35 C36 120.5(6) . . ?
N8 C35 C36 129.2(6) . . ?
N14 C56 H56 119.1 . . ?
N14 C56 C57 121.9(6) . . ?
C57 C56 H56 119.1 . . ?
C55 C50 C49 116.9(6) . . ?
C55 C50 C51 120.8(7) . . ?
C51 C50 C49 122.3(7) . . ?
N5 C3 C2 114.8(6) . . ?
N5 C3 C4 125.5(6) . . ?
C4 C3 C2 119.7(6) . . ?
C66 C61 C60 115.4(6) . . ?
C62 C61 C66 120.2(7) . . ?
C62 C61 C60 124.2(7) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 C11 120.6(8) . . ?
C9 C10 H10 119.7 . . ?
C3 C4 H4 121.0 . . ?
C5 C4 C3 117.9(7) . . ?
C5 C4 H4 121.0 . . ?
C55 C54 H54 120.3 . . ?
C55 C54 C53 119.4(7) . . ?
C53 C54 H54 120.3 . . ?
C45 C46 H46 120.5 . . ?
C47 C46 H46 120.5 . . ?
C47 C46 C45 119.1(7) . . ?
C43 C42 H42 119.8 . . ?
C43 C42 C41 120.4(8) . . ?
C41 C42 H42 119.8 . . ?
C65 C64 H64 119.9 . . ?
C63 C64 H64 119.9 . . ?
C63 C64 C65 120.2(7) . . ?
C11 C6 C7 119.7(7) . . ?
C11 C6 C5 119.1(7) . . ?
C5 C6 C7 121.2(7) . . ?
C42 C43 H43 119.3 . . ?
C42 C43 C44 121.4(7) . . ?
C44 C43 H43 119.3 . . ?
N7 C27 C28 114.4(6) . . ?
N7 C27 C26 119.6(7) . . ?
C26 C27 C28 126.0(6) . . ?
C23 C24 H24 120.5 . . ?
C23 C24 C25 119.0(7) . . ?
C25 C24 H24 120.5 . . ?
C56 C57 H57 120.6 . . ?
C56 C57 C58 118.8(7) . . ?
C58 C57 H57 120.6 . . ?
N7 C23 C24 121.4(7) . . ?
N7 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
C22 C21 H21 119.5 . . ?
C22 C21 C20 121.0(7) . . ?
C20 C21 H21 119.5 . . ?
C33 C32 H32 119.7 . . ?
C31 C32 C33 120.5(7) . . ?
C31 C32 H32 119.7 . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N12 C44 C43 120.4(7) . . ?
N12 C44 C39 121.3(7) . . ?
C43 C44 C39 118.2(7) . . ?
C54 C53 H53 119.7 . . ?
C52 C53 C54 120.7(7) . . ?
C52 C53 H53 119.7 . . ?
C32 C31 H31 119.9 . . ?
C32 C31 C30 120.2(7) . . ?
C30 C31 H31 119.9 . . ?
C21 C20 H20 119.6 . . ?
C21 C20 C19 120.9(7) . . ?
C19 C20 H20 119.6 . . ?
C66 C65 H65 120.0 . . ?
C64 C65 C66 120.0(7) . . ?
C64 C65 H65 120.0 . . ?
C16 C15 H15 119.5 . . ?
C14 C15 C16 121.0(7) . . ?
C14 C15 H15 119.5 . . ?
N12 C36 C35 115.3(6) . . ?
N12 C36 C37 124.1(7) . . ?
C37 C36 C35 120.6(7) . . ?
C49 C48 H48 120.3 . . ?
C47 C48 C49 119.4(7) . . ?
C47 C48 H48 120.3 . . ?
C13 C14 H14 120.9 . . ?
C15 C14 C13 118.1(7) . . ?
C15 C14 H14 120.9 . . ?
C31 C30 H30 120.0 . . ?
C29 C30 C31 119.9(7) . . ?
C29 C30 H30 120.0 . . ?
C60 C59 H59 120.0 . . ?
C58 C59 C60 120.1(7) . . ?
C58 C59 H59 120.0 . . ?
C17 C18 H18 119.8 . . ?
C17 C18 C19 120.4(7) . . ?
C19 C18 H18 119.8 . . ?
C51 C52 H52 119.7 . . ?
C53 C52 C51 120.5(7) . . ?
C53 C52 H52 119.7 . . ?
N13 C45 C46 121.7(7) . . ?
N13 C45 H45 119.2 . . ?
C46 C45 H45 119.2 . . ?
N9 C34 H34A 109.5 . . ?
N9 C34 H34B 109.5 . . ?
N9 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C38 C39 C44 119.2(7) . . ?
C38 C39 C40 121.5(8) . . ?
C40 C39 C44 119.3(8) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.3(8) . . ?
C8 C7 H7 119.9 . . ?
C46 C47 C48 120.1(7) . . ?
C46 C47 H47 120.0 . . ?
C48 C47 H47 120.0 . . ?
C20 C19 H19 120.5 . . ?
C18 C19 C20 119.1(7) . . ?
C18 C19 H19 120.5 . . ?
C28 C29 C30 119.9(7) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C39 C38 H38 120.3 . . ?
C37 C38 C39 119.5(8) . . ?
C37 C38 H38 120.3 . . ?
C42 C41 H41 120.5 . . ?
C40 C41 C42 118.9(8) . . ?
C40 C41 H41 120.5 . . ?
C27 C26 H26 120.1 . . ?
C25 C26 C27 119.8(7) . . ?
C25 C26 H26 120.1 . . ?
C61 C62 H62 120.2 . . ?
C63 C62 C61 119.5(7) . . ?
C63 C62 H62 120.2 . . ?
C24 C25 H25 120.2 . . ?
C26 C25 C24 119.6(7) . . ?
C26 C25 H25 120.2 . . ?
C4 C5 C6 119.6(7) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C64 C63 H63 119.4 . . ?
C62 C63 C64 121.2(7) . . ?
C62 C63 H63 119.4 . . ?
C36 C37 H37 120.4 . . ?
C38 C37 C36 119.1(8) . . ?
C38 C37 H37 120.4 . . ?
C57 C58 H58 120.4 . . ?
C59 C58 C57 119.2(7) . . ?
C59 C58 H58 120.4 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.8(8) . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 120.7(8) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C39 C40 H40 119.1 . . ?
C41 C40 C39 121.8(8) . . ?
C41 C40 H40 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ir2 N13 C49 C50 1.9(7) . . . . ?
Ir2 N13 C49 C48 -178.1(5) . . . . ?
Ir2 N13 C45 C46 176.9(5) . . . . ?
Ir2 N11 N10 N9 -171.0(5) . . . . ?
Ir2 N11 C35 N8 173.4(4) . . . . ?
Ir2 N11 C35 C36 -7.7(8) . . . . ?
Ir2 N14 C60 C61 10.8(8) . . . . ?
Ir2 N14 C60 C59 -169.6(6) . . . . ?
Ir2 N14 C56 C57 171.9(6) . . . . ?
Ir2 N12 C44 C43 5.1(10) . . . . ?
Ir2 N12 C44 C39 -173.8(6) . . . . ?
Ir2 N12 C36 C35 -2.5(8) . . . . ?
Ir2 N12 C36 C37 173.9(6) . . . . ?
Ir2 C66 C61 C60 -1.0(8) . . . . ?
Ir2 C66 C61 C62 -177.5(5) . . . . ?
Ir2 C66 C65 C64 178.1(6) . . . . ?
Ir2 C55 C50 C49 -2.3(7) . . . . ?
Ir2 C55 C50 C51 179.6(5) . . . . ?
Ir2 C55 C54 C53 -179.4(5) . . . . ?
Ir1 N4 N3 N2 165.7(5) . . . . ?
Ir1 N4 C2 N1 -168.5(4) . . . . ?
Ir1 N4 C2 C3 14.8(8) . . . . ?
Ir1 N6 C16 C17 -3.5(7) . . . . ?
Ir1 N6 C16 C15 177.2(5) . . . . ?
Ir1 N6 C12 C13 -176.7(5) . . . . ?
Ir1 N7 C27 C28 -8.3(8) . . . . ?
Ir1 N7 C27 C26 173.3(6) . . . . ?
Ir1 N7 C23 C24 -175.8(5) . . . . ?
Ir1 N5 C11 C10 3.7(10) . . . . ?
Ir1 N5 C11 C6 -175.8(5) . . . . ?
Ir1 N5 C3 C2 -2.3(7) . . . . ?
Ir1 N5 C3 C4 176.4(6) . . . . ?
Ir1 C33 C28 C27 8.9(8) . . . . ?
Ir1 C33 C28 C29 -176.3(6) . . . . ?
Ir1 C33 C32 C31 177.4(6) . . . . ?
Ir1 C22 C21 C20 -174.4(5) . . . . ?
N13 C49 C50 C55 0.3(8) . . . . ?
N13 C49 C50 C51 178.3(6) . . . . ?
N13 C49 C48 C47 1.1(10) . . . . ?
N11 C35 C36 N12 6.9(10) . . . . ?
N11 C35 C36 C37 -169.7(7) . . . . ?
N4 C2 C3 N5 -8.1(9) . . . . ?
N4 C2 C3 C4 173.1(6) . . . . ?
N6 C16 C15 C14 -0.1(10) . . . . ?
N6 C12 C13 C14 -0.5(10) . . . . ?
N14 C60 C61 C66 -6.4(9) . . . . ?
N14 C60 C61 C62 170.0(7) . . . . ?
N14 C60 C59 C58 -2.6(11) . . . . ?
N14 C56 C57 C58 -3.5(12) . . . . ?
N7 C27 C26 C25 2.7(12) . . . . ?
N9 N8 C35 N11 -0.9(8) . . . . ?
N9 N8 C35 C36 -179.6(7) . . . . ?
N8 N9 N10 N11 -0.3(8) . . . . ?
N8 C35 C36 N12 -174.5(7) . . . . ?
N8 C35 C36 C37 8.9(12) . . . . ?
N2 N1 C2 N4 -0.3(7) . . . . ?
N2 N1 C2 C3 176.1(7) . . . . ?
N5 C11 C10 C9 -177.7(8) . . . . ?
N5 C11 C6 C7 177.4(7) . . . . ?
N5 C11 C6 C5 -3.4(11) . . . . ?
N5 C3 C4 C5 1.5(11) . . . . ?
N12 C44 C39 C38 0.1(13) . . . . ?
N12 C44 C39 C40 -179.1(8) . . . . ?
N12 C36 C37 C38 1.8(14) . . . . ?
C33 C28 C27 N7 -0.3(9) . . . . ?
C33 C28 C27 C26 177.9(7) . . . . ?
C33 C28 C29 C30 -0.8(11) . . . . ?
C33 C32 C31 C30 -1.9(11) . . . . ?
N3 N4 C2 N1 -0.1(8) . . . . ?
N3 N4 C2 C3 -176.8(6) . . . . ?
N3 N2 N1 C2 0.7(7) . . . . ?
N10 N11 C35 N8 0.8(8) . . . . ?
N10 N11 C35 C36 179.6(6) . . . . ?
N10 N9 N8 C35 0.8(8) . . . . ?
N1 N2 N3 N4 -0.7(7) . . . . ?
N1 C2 C3 N5 175.8(7) . . . . ?
N1 C2 C3 C4 -3.0(11) . . . . ?
C66 C61 C62 C63 -1.2(11) . . . . ?
C60 N14 C56 C57 0.6(11) . . . . ?
C60 C61 C62 C63 -177.4(7) . . . . ?
C60 C59 C58 C57 -0.4(12) . . . . ?
C28 C33 C32 C31 -0.9(11) . . . . ?
C28 C27 C26 C25 -175.5(8) . . . . ?
C17 C22 C21 C20 2.0(10) . . . . ?
C17 C16 C15 C14 -179.4(6) . . . . ?
C17 C18 C19 C20 0.0(10) . . . . ?
C22 C17 C16 N6 3.6(8) . . . . ?
C22 C17 C16 C15 -177.1(6) . . . . ?
C22 C17 C18 C19 0.1(10) . . . . ?
C22 C21 C20 C19 -1.9(11) . . . . ?
C11 N5 C3 C2 176.9(6) . . . . ?
C11 N5 C3 C4 -4.3(10) . . . . ?
C11 C10 C9 C8 -1.2(14) . . . . ?
C11 C6 C7 C8 1.8(13) . . . . ?
C11 C6 C5 C4 0.4(11) . . . . ?
C2 N4 N3 N2 0.4(7) . . . . ?
C2 C3 C4 C5 -179.8(7) . . . . ?
C55 C54 C53 C52 0.5(10) . . . . ?
C49 N13 C45 C46 -0.4(9) . . . . ?
C49 C48 C47 C46 -0.6(10) . . . . ?
C16 N6 C12 C13 1.7(10) . . . . ?
C16 C17 C22 Ir1 -2.0(7) . . . . ?
C16 C17 C22 C21 -178.8(6) . . . . ?
C16 C17 C18 C19 177.6(6) . . . . ?
C16 C15 C14 C13 1.3(10) . . . . ?
C12 N6 C16 C17 178.0(6) . . . . ?
C12 N6 C16 C15 -1.4(9) . . . . ?
C12 C13 C14 C15 -1.0(10) . . . . ?
C35 N11 N10 N9 -0.3(7) . . . . ?
C35 C36 C37 C38 178.1(8) . . . . ?
C56 N14 C60 C61 -177.0(6) . . . . ?
C56 N14 C60 C59 2.5(10) . . . . ?
C56 C57 C58 C59 3.4(12) . . . . ?
C50 C55 C54 C53 -0.7(9) . . . . ?
C50 C49 C48 C47 -178.9(6) . . . . ?
C50 C51 C52 C53 0.5(10) . . . . ?
C3 N5 C11 C10 -175.4(7) . . . . ?
C3 N5 C11 C6 5.1(10) . . . . ?
C3 C4 C5 C6 0.6(11) . . . . ?
C61 C66 C65 C64 -2.4(10) . . . . ?
C61 C60 C59 C58 176.9(7) . . . . ?
C61 C62 C63 C64 -1.1(12) . . . . ?
C10 C11 C6 C7 -2.1(11) . . . . ?
C10 C11 C6 C5 177.2(7) . . . . ?
C54 C55 C50 C49 178.8(6) . . . . ?
C54 C55 C50 C51 0.8(9) . . . . ?
C54 C53 C52 C51 -0.4(10) . . . . ?
C42 C43 C44 N12 179.6(7) . . . . ?
C42 C43 C44 C39 -1.4(11) . . . . ?
C42 C41 C40 C39 -0.6(14) . . . . ?
C6 C11 C10 C9 1.8(12) . . . . ?
C6 C7 C8 C9 -1.2(15) . . . . ?
C43 C42 C41 C40 1.1(13) . . . . ?
C43 C44 C39 C38 -178.8(8) . . . . ?
C43 C44 C39 C40 1.9(12) . . . . ?
C27 N7 C23 C24 0.9(10) . . . . ?
C27 C28 C29 C30 173.6(7) . . . . ?
C27 C26 C25 C24 1.0(13) . . . . ?
C23 N7 C27 C28 174.7(6) . . . . ?
C23 N7 C27 C26 -3.7(10) . . . . ?
C23 C24 C25 C26 -3.8(12) . . . . ?
C21 C20 C19 C18 0.8(11) . . . . ?
C32 C33 C28 C27 -172.6(6) . . . . ?
C32 C33 C28 C29 2.2(11) . . . . ?
C32 C31 C30 C29 3.3(12) . . . . ?
C1 N2 N3 N4 177.4(6) . . . . ?
C1 N2 N1 C2 -177.4(6) . . . . ?
C44 N12 C36 C35 -177.2(6) . . . . ?
C44 N12 C36 C37 -0.8(11) . . . . ?
C44 C39 C38 C37 0.9(15) . . . . ?
C44 C39 C40 C41 -1.0(14) . . . . ?
C31 C30 C29 C28 -2.0(12) . . . . ?
C65 C66 C61 C60 179.5(6) . . . . ?
C65 C66 C61 C62 2.9(10) . . . . ?
C65 C64 C63 C62 1.6(12) . . . . ?
C36 N12 C44 C43 178.7(7) . . . . ?
C36 N12 C44 C39 -0.2(10) . . . . ?
C48 C49 C50 C55 -179.8(6) . . . . ?
C48 C49 C50 C51 -1.8(10) . . . . ?
C59 C60 C61 C66 174.0(7) . . . . ?
C59 C60 C61 C62 -9.6(12) . . . . ?
C18 C17 C22 Ir1 175.8(5) . . . . ?
C18 C17 C22 C21 -1.1(9) . . . . ?
C18 C17 C16 N6 -174.1(6) . . . . ?
C18 C17 C16 C15 5.3(10) . . . . ?
C52 C51 C50 C55 -0.6(10) . . . . ?
C52 C51 C50 C49 -178.6(6) . . . . ?
C45 N13 C49 C50 179.5(5) . . . . ?
C45 N13 C49 C48 -0.5(9) . . . . ?
C45 C46 C47 C48 -0.3(10) . . . . ?
C34 N9 N8 C35 174.7(7) . . . . ?
C34 N9 N10 N11 -174.4(6) . . . . ?
C39 C38 C37 C36 -1.8(15) . . . . ?
C7 C6 C5 C4 179.6(8) . . . . ?
C7 C8 C9 C10 0.9(15) . . . . ?
C47 C46 C45 N13 0.8(10) . . . . ?
C29 C28 C27 N7 -175.0(7) . . . . ?
C29 C28 C27 C26 3.2(12) . . . . ?
C38 C39 C40 C41 179.8(10) . . . . ?
C41 C42 C43 C44 -0.1(12) . . . . ?
C25 C24 C23 N7 2.9(11) . . . . ?
C5 C6 C7 C8 -177.4(9) . . . . ?
C63 C64 C65 C66 0.2(11) . . . . ?
C40 C39 C38 C37 -179.9(9) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.088 0.000 0.000 200.4 57.8 '1.5 CH2Cl2'
2 -0.002 0.500 0.500 200.4 57.8 '1.5 CH2Cl2'
3 0.393 0.070 0.292 47.6 2.0 ?
4 0.393 0.430 0.792 47.6 2.0 ?
5 0.607 0.570 0.208 47.6 2.0 ?
6 0.607 0.930 0.708 47.6 2.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 
'crystal was mounted on a glass fibre using silicon oil'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.859

