# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_sbd1905
_database_code_depnum_ccdc_archive 'CCDC 1957542'
loop_
_audit_author_name
_audit_author_address
'Adrian C. Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-12-10 downloaded from the CCDC.
;
_audit_creation_date             2019-09-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H48 Ir P3, 0.28(C H4 O)'
_chemical_formula_sum            'C54.28 H49.13 Ir O0.28 P3'
_chemical_formula_weight         991.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54.3 H49.1 Ir1 O0.3 P3'
_chemical_oxdiff_usercomment     'Ben Tickner PPh3'
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'
Ir Ir -4.7710 6.5667 '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 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   17.31801(12)
_cell_length_b                   12.99024(10)
_cell_length_c                   19.71788(16)
_cell_angle_alpha                90
_cell_angle_beta                 94.4442(7)
_cell_angle_gamma                90
_cell_volume                     4422.50(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9261
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      71.0080
_cell_measurement_theta_min      4.9940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.149
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1996.4
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 1 0.0390
0 0 -1 0.0213
0 0 1 0.0161
-1 0 0 0.0447
2 -1 0 0.0635
1 2 -2 0.0643
-2 2 1 0.0763
-1 -2 0 0.0968
1 0 0 0.0543
-2 1 -2 0.0462
1 0 -2 0.0364
-2 -1 1 0.0670

_exptl_crystal_recrystallization_method 'crystallisation from methanol'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.037
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
0.9989 -0.0007 0.9977 0.1098 0.0267 0.0488
0.0006 -0.0000 -0.9992 -0.0722 -0.0069 0.0296
-0.0006 0.0000 0.9992 0.0722 0.0069 -0.0296
-0.9995 0.0007 0.0015 -0.0377 -0.0198 -0.0784
1.9977 -1.0018 -0.0047 0.0561 0.1550 0.1368
1.0030 2.0001 -1.9964 -0.0682 -0.2245 0.1775
-1.9971 2.0023 1.0056 0.0353 -0.2634 -0.1465
-1.0019 -2.0001 -0.0020 -0.0761 0.2108 -0.1183
0.9995 -0.0007 -0.0015 0.0377 0.0198 0.0784
-1.9966 1.0018 -1.9937 -0.2004 -0.1687 -0.0776
1.0006 -0.0007 -1.9999 -0.1066 0.0061 0.1376
-2.0007 -0.9990 1.0004 -0.0224 0.0825 -0.2064

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17542
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         4.079
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      1.00  26.00   1.00    1.00    --    0.00  57.00 150.00   25
  2  ω    -10.00  27.00   1.00    1.00    --    0.00  93.00  61.00   37
  3  ω    -39.00 -13.00   1.00    1.00    --    0.00  93.00  61.00   26
  4  ω    -21.00  45.00   1.00    1.00    --    0.00  57.00-180.00   66
  5  ω     24.00 109.00   1.00    1.25    --   54.00-125.00 -90.00   85
  6  ω     28.00 114.00   1.00    1.25    --   54.00  37.00 -30.00   86
  7  ω     50.00 100.00   1.00    1.25    --   54.00  57.00-180.00   50
  8  ω    -13.00  73.00   1.00    1.25    --   54.00 -57.00   0.00   86
  9  ω    106.00 176.00   1.00    2.50    --  108.00 111.00 150.00   70
 10  ω     47.00 100.00   1.00    2.50    --  108.00-111.00 -60.00   53
 11  ω     55.00 103.00   1.00    2.50    --  108.00 -50.00-120.00   48
 12  ω     39.00 111.00   1.00    2.50    --  108.00-111.00  90.00   72
 13  ω     69.00 125.00   1.00    2.50    --  108.00 -50.00 150.00   56
 14  ω     95.00 162.00   1.00    2.50    --  108.00  63.00 -30.00   67
 15  ω     84.00 150.00   1.00    2.50    --  108.00 178.00 -60.00   66
 16  ω     86.00 163.00   1.00    2.50    --  108.00  50.00 -60.00   77
 17  ω     70.00  95.00   1.00    2.50    --  108.00-111.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0378139000
_diffrn_orient_matrix_UB_12      0.0190542000
_diffrn_orient_matrix_UB_13      0.0722370000
_diffrn_orient_matrix_UB_21      0.0197567000
_diffrn_orient_matrix_UB_22      -0.1153091000
_diffrn_orient_matrix_UB_23      0.0068760000
_diffrn_orient_matrix_UB_31      0.0784119000
_diffrn_orient_matrix_UB_32      0.0199077000
_diffrn_orient_matrix_UB_33      -0.0295763000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7174
_reflns_number_total             7896
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.000059(6)
_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   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         7896
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0199
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0216P)²+0.6768P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0480
_refine_special_details          
'The asymmetric unit contained a partial methanol whose occupancy refined to be 0.283(5)'
_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, All O(H) groups
2. Others
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(O1)=Sof(H1)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
3.b Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C)
3.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   mixed
_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
C1 C 0.64948(12) 0.96767(18) 0.67458(12) 0.0129(5) Uani 1 1 d . . . . .
C2 C 0.68615(14) 1.0340(2) 0.63166(13) 0.0186(5) Uani 1 1 d . . . . .
H2 H 0.701960 1.009582 0.590599 0.022 Uiso 1 1 calc R . . . .
C3 C 0.69931(16) 1.1368(2) 0.64993(14) 0.0249(6) Uani 1 1 d . . . . .
H3 H 0.724145 1.180207 0.621083 0.030 Uiso 1 1 calc R . . . .
C4 C 0.67559(16) 1.1746(2) 0.71082(14) 0.0248(6) Uani 1 1 d . . . . .
H4 H 0.685333 1.242681 0.723272 0.030 Uiso 1 1 calc R . . . .
C5 C 0.63723(14) 1.1098(2) 0.75288(13) 0.0214(6) Uani 1 1 d . . . . .
H5 H 0.620345 1.134781 0.793382 0.026 Uiso 1 1 calc R . . . .
C6 C 0.62393(13) 1.0075(2) 0.73467(13) 0.0175(5) Uani 1 1 d . . . . .
H6 H 0.597591 0.964931 0.762988 0.021 Uiso 1 1 calc R . . . .
C7 C 0.52819(13) 0.84914(19) 0.61556(13) 0.0152(5) Uani 1 1 d . . . . .
C8 C 0.50890(14) 0.8537(2) 0.54587(14) 0.0227(6) Uani 1 1 d . . . . .
H8 H 0.546993 0.843354 0.515821 0.027 Uiso 1 1 calc R . . . .
C9 C 0.43291(16) 0.8738(2) 0.52059(15) 0.0313(7) Uani 1 1 d . . . . .
H9 H 0.420719 0.876647 0.473858 0.038 Uiso 1 1 calc R . . . .
C10 C 0.37556(15) 0.8895(2) 0.56460(16) 0.0278(6) Uani 1 1 d . . . . .
H10 H 0.324839 0.902083 0.547635 0.033 Uiso 1 1 calc R . . . .
C11 C 0.39432(14) 0.8862(2) 0.63414(15) 0.0239(6) Uani 1 1 d . . . . .
H11 H 0.356053 0.896845 0.663979 0.029 Uiso 1 1 calc R . . . .
C12 C 0.47008(14) 0.8672(2) 0.65951(13) 0.0188(5) Uani 1 1 d . . . . .
H12 H 0.482275 0.866547 0.706276 0.023 Uiso 1 1 calc R . . . .
C13 C 0.62356(13) 0.76881(18) 0.73028(12) 0.0118(5) Uani 1 1 d . . . . .
C14 C 0.68051(13) 0.78807(19) 0.78309(12) 0.0138(5) Uani 1 1 d . . . . .
H14 H 0.719416 0.835680 0.776788 0.017 Uiso 1 1 calc R . . . .
C15 C 0.67944(14) 0.73669(19) 0.84489(13) 0.0161(5) Uani 1 1 d . . . . .
H15 H 0.717559 0.750292 0.879574 0.019 Uiso 1 1 calc R . . . .
C16 C 0.62194(14) 0.6653(2) 0.85518(13) 0.0180(5) Uani 1 1 d . . . . .
H16 H 0.620879 0.631884 0.896812 0.022 Uiso 1 1 calc R . . . .
C17 C 0.56593(14) 0.64412(19) 0.80271(13) 0.0180(5) Uani 1 1 d . . . . .
H17 H 0.527686 0.595598 0.809102 0.022 Uiso 1 1 calc R . . . .
C18 C 0.56668(13) 0.69500(19) 0.74069(12) 0.0145(5) Uani 1 1 d . . . . .
H18 H 0.529100 0.679904 0.705834 0.017 Uiso 1 1 calc R . . . .
C19 C 0.62083(13) 0.53220(19) 0.61399(12) 0.0129(5) Uani 1 1 d . . . . .
C20 C 0.55342(13) 0.57646(19) 0.58388(12) 0.0156(5) Uani 1 1 d . . . . .
H20 H 0.555714 0.640549 0.563109 0.019 Uiso 1 1 calc R . . . .
C21 C 0.48256(14) 0.5258(2) 0.58451(13) 0.0203(5) Uani 1 1 d . . . . .
H21 H 0.437873 0.556350 0.564481 0.024 Uiso 1 1 calc R . . . .
C22 C 0.47857(14) 0.4306(2) 0.61471(13) 0.0226(6) Uani 1 1 d . . . . .
H22 H 0.431335 0.396584 0.614679 0.027 Uiso 1 1 calc R . . . .
C23 C 0.54525(15) 0.3855(2) 0.64526(14) 0.0237(6) Uani 1 1 d . . . . .
H23 H 0.542581 0.321233 0.665711 0.028 Uiso 1 1 calc R . . . .
C24 C 0.61586(14) 0.4362(2) 0.64531(13) 0.0183(5) Uani 1 1 d . . . . .
H24 H 0.660167 0.406091 0.666355 0.022 Uiso 1 1 calc R . . . .
C25 C 0.73896(13) 0.50026(19) 0.53287(12) 0.0145(5) Uani 1 1 d . . . . .
C26 C 0.75924(14) 0.3981(2) 0.54723(14) 0.0209(5) Uani 1 1 d . . . . .
H26 H 0.770773 0.377731 0.592092 0.025 Uiso 1 1 calc R . . . .
C27 C 0.76238(15) 0.3263(2) 0.49505(15) 0.0258(6) Uani 1 1 d . . . . .
H27 H 0.776221 0.258524 0.505146 0.031 Uiso 1 1 calc R . . . .
C28 C 0.74487(14) 0.3558(2) 0.42807(14) 0.0234(6) Uani 1 1 d . . . . .
H28 H 0.745917 0.307726 0.393223 0.028 Uiso 1 1 calc R . . . .
C29 C 0.72586(14) 0.4571(2) 0.41334(14) 0.0214(6) Uani 1 1 d . . . . .
H29 H 0.714791 0.477324 0.368402 0.026 Uiso 1 1 calc R . . . .
C30 C 0.72319(13) 0.5291(2) 0.46563(12) 0.0164(5) Uani 1 1 d . . . . .
H30 H 0.710694 0.597233 0.455189 0.020 Uiso 1 1 calc R . . . .
C31 C 0.77749(13) 0.54635(18) 0.67382(12) 0.0135(5) Uani 1 1 d . . . . .
C32 C 0.75073(14) 0.54883(19) 0.73871(13) 0.0166(5) Uani 1 1 d . . . . .
H32 H 0.700025 0.569030 0.743967 0.020 Uiso 1 1 calc R . . . .
C33 C 0.79861(15) 0.5216(2) 0.79553(13) 0.0219(6) Uani 1 1 d . . . . .
H33 H 0.779804 0.523812 0.838424 0.026 Uiso 1 1 calc R . . . .
C34 C 0.87465(15) 0.4911(2) 0.78871(14) 0.0279(6) Uani 1 1 d . . . . .
H34 H 0.906512 0.471766 0.826723 0.033 Uiso 1 1 calc R . . . .
C35 C 0.90248(14) 0.4897(2) 0.72434(15) 0.0270(6) Uani 1 1 d . . . . .
H35 H 0.953466 0.470440 0.719457 0.032 Uiso 1 1 calc R . . . .
C36 C 0.85467(14) 0.5170(2) 0.66732(13) 0.0186(5) Uani 1 1 d . . . . .
H36 H 0.873881 0.515880 0.624576 0.022 Uiso 1 1 calc R . . . .
C37 C 0.86844(13) 0.94240(19) 0.57312(12) 0.0142(5) Uani 1 1 d . . . . .
C38 C 0.83560(13) 0.97721(19) 0.51076(13) 0.0154(5) Uani 1 1 d . . . . .
H38 H 0.793133 0.942725 0.489825 0.019 Uiso 1 1 calc R . . . .
C39 C 0.86507(14) 1.0625(2) 0.47920(13) 0.0201(5) Uani 1 1 d . . . . .
H39 H 0.842037 1.084807 0.437613 0.024 Uiso 1 1 calc R . . . .
C40 C 0.92861(15) 1.1146(2) 0.50925(14) 0.0228(6) Uani 1 1 d . . . . .
H40 H 0.948107 1.172142 0.488260 0.027 Uiso 1 1 calc R . . . .
C41 C 0.96284(15) 1.0800(2) 0.57114(15) 0.0258(6) Uani 1 1 d . . . . .
H41 H 1.005805 1.114085 0.591502 0.031 Uiso 1 1 calc R . . . .
C42 C 0.93339(14) 0.9950(2) 0.60261(13) 0.0199(5) Uani 1 1 d . . . . .
H42 H 0.956963 0.972434 0.643926 0.024 Uiso 1 1 calc R . . . .
C43 C 0.91808(13) 0.74267(18) 0.59649(13) 0.0136(5) Uani 1 1 d . . . . .
C44 C 0.98739(14) 0.74623(19) 0.63811(13) 0.0175(5) Uani 1 1 d . . . . .
H44 H 0.990602 0.786942 0.677022 0.021 Uiso 1 1 calc R . . . .
C45 C 1.05130(14) 0.6895(2) 0.62175(14) 0.0210(5) Uani 1 1 d . . . . .
H45 H 1.096722 0.691587 0.650154 0.025 Uiso 1 1 calc R . . . .
C46 C 1.04782(14) 0.6299(2) 0.56347(14) 0.0196(5) Uani 1 1 d . . . . .
H46 H 1.090692 0.591893 0.552686 0.024 Uiso 1 1 calc R . . . .
C47 C 0.98000(14) 0.6272(2) 0.52121(13) 0.0191(5) Uani 1 1 d . . . . .
H47 H 0.977592 0.588024 0.481645 0.023 Uiso 1 1 calc R . . . .
C48 C 0.91540(13) 0.68320(19) 0.53787(13) 0.0165(5) Uani 1 1 d . . . . .
H48 H 0.870039 0.680635 0.509400 0.020 Uiso 1 1 calc R . . . .
C49 C 0.85208(12) 0.85135(19) 0.70372(12) 0.0131(5) Uani 1 1 d . . . . .
C50 C 0.86903(13) 0.7709(2) 0.74953(13) 0.0180(5) Uani 1 1 d . . . . .
H50 H 0.874499 0.704353 0.733160 0.022 Uiso 1 1 calc R . . . .
C51 C 0.87782(14) 0.7888(2) 0.81900(14) 0.0236(6) Uani 1 1 d . . . . .
H51 H 0.889674 0.734493 0.848716 0.028 Uiso 1 1 calc R . . . .
C52 C 0.86907(15) 0.8871(2) 0.84440(13) 0.0271(6) Uani 1 1 d . . . . .
H52 H 0.875024 0.899016 0.891011 0.032 Uiso 1 1 calc R . . . .
C53 C 0.85133(14) 0.9676(2) 0.79962(14) 0.0233(6) Uani 1 1 d . . . . .
H53 H 0.844872 1.033717 0.816363 0.028 Uiso 1 1 calc R . . . .
C54 C 0.84317(13) 0.9500(2) 0.73000(13) 0.0176(5) Uani 1 1 d . . . . .
H54 H 0.831612 1.004696 0.700487 0.021 Uiso 1 1 calc R . . . .
Ir1 Ir 0.71281(2) 0.76500(2) 0.57051(2) 0.00947(4) Uani 1 1 d . . . . .
H H 0.6956(16) 0.868(2) 0.5325(15) 0.031(9) Uiso 1 1 d . . . . .
HA H 0.7593(17) 0.743(2) 0.5079(15) 0.024(8) Uiso 1 1 d . . . . .
HB H 0.6422(16) 0.733(2) 0.5222(15) 0.019(8) Uiso 1 1 d . . . . .
P1 P 0.63074(3) 0.83272(5) 0.64784(3) 0.01082(11) Uani 1 1 d . . . . .
P2 P 0.71553(3) 0.59173(5) 0.60036(3) 0.01056(11) Uani 1 1 d . . . . .
P3 P 0.83357(3) 0.82402(5) 0.61283(3) 0.01083(12) Uani 1 1 d . . . . .
C55 C 0.8930(7) 1.2368(9) 0.6889(7) 0.041(3) Uani 0.283(5) 1 d . . P . .
H55A H 0.869970 1.240671 0.643063 0.062 Uiso 0.283(5) 1 calc GR . P . .
H55B H 0.906489 1.166736 0.699640 0.062 Uiso 0.283(5) 1 calc GR . P . .
H55C H 0.938713 1.278797 0.693202 0.062 Uiso 0.283(5) 1 calc GR . P . .
O1 O 0.8391(5) 1.2730(7) 0.7345(6) 0.052(3) Uani 0.283(5) 1 d . . P . .
H1 H 0.795713 1.275687 0.714726 0.078 Uiso 0.283(5) 1 calc GR . P . .


_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
C1 C2 1.394(3) . ?
C1 C6 1.396(3) . ?
C1 P1 1.852(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.397(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.388(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.387(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.391(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.390(4) . ?
C7 C12 1.398(3) . ?
C7 P1 1.852(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.395(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.384(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.385(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.390(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.400(3) . ?
C13 C18 1.401(3) . ?
C13 P1 1.838(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.391(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.387(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.390(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.391(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.392(3) . ?
C19 C24 1.397(3) . ?
C19 P2 1.852(2) . ?
C20 H20 0.9300 . ?
C20 C21 1.393(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.376(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.390(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.389(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.397(4) . ?
C25 C30 1.385(3) . ?
C25 P2 1.852(2) . ?
C26 H26 0.9300 . ?
C26 C27 1.393(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.386(4) . ?
C28 H28 0.9300 . ?
C28 C29 1.381(4) . ?
C29 H29 0.9300 . ?
C29 C30 1.396(3) . ?
C30 H30 0.9300 . ?
C31 C32 1.395(3) . ?
C31 C36 1.405(3) . ?
C31 P2 1.832(2) . ?
C32 H32 0.9300 . ?
C32 C33 1.387(3) . ?
C33 H33 0.9300 . ?
C33 C34 1.392(4) . ?
C34 H34 0.9300 . ?
C34 C35 1.392(4) . ?
C35 H35 0.9300 . ?
C35 C36 1.390(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.390(3) . ?
C37 C42 1.403(3) . ?
C37 P3 1.848(2) . ?
C38 H38 0.9300 . ?
C38 C39 1.387(3) . ?
C39 H39 0.9300 . ?
C39 C40 1.385(4) . ?
C40 H40 0.9300 . ?
C40 C41 1.390(4) . ?
C41 H41 0.9300 . ?
C41 C42 1.383(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.401(3) . ?
C43 C48 1.388(3) . ?
C43 P3 1.854(2) . ?
C44 H44 0.9300 . ?
C44 C45 1.388(3) . ?
C45 H45 0.9300 . ?
C45 C46 1.383(4) . ?
C46 H46 0.9300 . ?
C46 C47 1.387(3) . ?
C47 H47 0.9300 . ?
C47 C48 1.394(3) . ?
C48 H48 0.9300 . ?
C49 C50 1.398(3) . ?
C49 C54 1.396(3) . ?
C49 P3 1.831(2) . ?
C50 H50 0.9300 . ?
C50 C51 1.386(4) . ?
C51 H51 0.9300 . ?
C51 C52 1.383(4) . ?
C52 H52 0.9300 . ?
C52 C53 1.388(4) . ?
C53 H53 0.9300 . ?
C53 C54 1.388(4) . ?
C54 H54 0.9300 . ?
Ir1 H 1.55(3) . ?
Ir1 HA 1.55(3) . ?
Ir1 HB 1.55(3) . ?
Ir1 P1 2.3354(6) . ?
Ir1 P2 2.3261(6) . ?
Ir1 P3 2.3211(6) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C55 O1 1.425(14) . ?
O1 H1 0.8200 . ?

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
C2 C1 C6 118.4(2) . . ?
C2 C1 P1 119.32(19) . . ?
C6 C1 P1 122.16(19) . . ?
C1 C2 H2 119.8 . . ?
C1 C2 C3 120.4(2) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.2(2) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 H6 119.5 . . ?
C5 C6 C1 121.1(2) . . ?
C5 C6 H6 119.5 . . ?
C8 C7 C12 118.4(2) . . ?
C8 C7 P1 119.69(18) . . ?
C12 C7 P1 121.57(19) . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.6(3) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 120.3 . . ?
C9 C10 C11 119.5(2) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.3(2) . . ?
C12 C11 H11 119.9 . . ?
C7 C12 H12 119.6 . . ?
C11 C12 C7 120.8(2) . . ?
C11 C12 H12 119.6 . . ?
C14 C13 C18 118.4(2) . . ?
C14 C13 P1 119.02(17) . . ?
C18 C13 P1 122.34(18) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.6(2) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.5(2) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 120.3 . . ?
C15 C16 C17 119.4(2) . . ?
C17 C16 H16 120.3 . . ?
C16 C17 H17 119.8 . . ?
C16 C17 C18 120.5(2) . . ?
C18 C17 H17 119.8 . . ?
C13 C18 H18 119.7 . . ?
C17 C18 C13 120.6(2) . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C24 118.6(2) . . ?
C20 C19 P2 119.24(18) . . ?
C24 C19 P2 121.50(18) . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.7(2) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.1(2) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 120.0 . . ?
C21 C22 C23 119.9(2) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.1(2) . . ?
C24 C23 H23 119.9 . . ?
C19 C24 H24 119.8 . . ?
C23 C24 C19 120.5(2) . . ?
C23 C24 H24 119.8 . . ?
C26 C25 P2 122.0(2) . . ?
C30 C25 C26 118.6(2) . . ?
C30 C25 P2 118.44(19) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.7(3) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0(3) . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.2 . . ?
C29 C28 C27 119.7(3) . . ?
C29 C28 H28 120.2 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.3(3) . . ?
C30 C29 H29 119.9 . . ?
C25 C30 C29 120.7(2) . . ?
C25 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C32 C31 C36 118.4(2) . . ?
C32 C31 P2 120.14(18) . . ?
C36 C31 P2 121.21(19) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 C31 121.0(2) . . ?
C33 C32 H32 119.5 . . ?
C32 C33 H33 119.8 . . ?
C32 C33 C34 120.4(2) . . ?
C34 C33 H33 119.8 . . ?
C33 C34 H34 120.4 . . ?
C33 C34 C35 119.2(2) . . ?
C35 C34 H34 120.4 . . ?
C34 C35 H35 119.7 . . ?
C36 C35 C34 120.5(2) . . ?
C36 C35 H35 119.7 . . ?
C31 C36 H36 119.8 . . ?
C35 C36 C31 120.5(2) . . ?
C35 C36 H36 119.8 . . ?
C38 C37 C42 117.9(2) . . ?
C38 C37 P3 121.39(18) . . ?
C42 C37 P3 120.49(19) . . ?
C37 C38 H38 119.4 . . ?
C39 C38 C37 121.1(2) . . ?
C39 C38 H38 119.4 . . ?
C38 C39 H39 119.8 . . ?
C40 C39 C38 120.4(2) . . ?
C40 C39 H39 119.8 . . ?
C39 C40 H40 120.4 . . ?
C39 C40 C41 119.2(2) . . ?
C41 C40 H40 120.4 . . ?
C40 C41 H41 119.8 . . ?
C42 C41 C40 120.4(2) . . ?
C42 C41 H41 119.8 . . ?
C37 C42 H42 119.5 . . ?
C41 C42 C37 121.0(2) . . ?
C41 C42 H42 119.5 . . ?
C44 C43 P3 122.10(19) . . ?
C48 C43 C44 118.6(2) . . ?
C48 C43 P3 119.09(18) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 C43 120.6(2) . . ?
C45 C44 H44 119.7 . . ?
C44 C45 H45 119.8 . . ?
C46 C45 C44 120.4(2) . . ?
C46 C45 H45 119.8 . . ?
C45 C46 H46 120.2 . . ?
C45 C46 C47 119.6(2) . . ?
C47 C46 H46 120.2 . . ?
C46 C47 H47 119.9 . . ?
C46 C47 C48 120.2(2) . . ?
C48 C47 H47 119.9 . . ?
C43 C48 C47 120.7(2) . . ?
C43 C48 H48 119.7 . . ?
C47 C48 H48 119.7 . . ?
C50 C49 P3 119.98(19) . . ?
C54 C49 C50 118.1(2) . . ?
C54 C49 P3 121.71(19) . . ?
C49 C50 H50 119.5 . . ?
C51 C50 C49 121.0(3) . . ?
C51 C50 H50 119.5 . . ?
C50 C51 H51 119.8 . . ?
C52 C51 C50 120.4(3) . . ?
C52 C51 H51 119.8 . . ?
C51 C52 H52 120.3 . . ?
C51 C52 C53 119.3(2) . . ?
C53 C52 H52 120.3 . . ?
C52 C53 H53 119.8 . . ?
C54 C53 C52 120.4(3) . . ?
C54 C53 H53 119.8 . . ?
C49 C54 H54 119.6 . . ?
C53 C54 C49 120.8(3) . . ?
C53 C54 H54 119.6 . . ?
H Ir1 HA 82.3(14) . . ?
H Ir1 HB 79.4(14) . . ?
HA Ir1 HB 84.0(15) . . ?
P1 Ir1 H 83.5(11) . . ?
P1 Ir1 HA 165.5(11) . . ?
P1 Ir1 HB 90.6(10) . . ?
P2 Ir1 H 162.9(11) . . ?
P2 Ir1 HA 91.2(10) . . ?
P2 Ir1 HB 84.2(10) . . ?
P2 Ir1 P1 101.58(2) . . ?
P3 Ir1 H 91.4(11) . . ?
P3 Ir1 HA 80.7(11) . . ?
P3 Ir1 HB 163.1(10) . . ?
P3 Ir1 P1 102.58(2) . . ?
P3 Ir1 P2 103.22(2) . . ?
C1 P1 Ir1 116.13(8) . . ?
C7 P1 C1 97.53(10) . . ?
C7 P1 Ir1 115.78(8) . . ?
C13 P1 C1 101.42(11) . . ?
C13 P1 C7 103.13(11) . . ?
C13 P1 Ir1 119.57(7) . . ?
C19 P2 C25 94.72(10) . . ?
C19 P2 Ir1 116.11(8) . . ?
C25 P2 Ir1 116.12(8) . . ?
C31 P2 C19 102.83(11) . . ?
C31 P2 C25 102.36(11) . . ?
C31 P2 Ir1 120.70(8) . . ?
C37 P3 C43 96.45(10) . . ?
C37 P3 Ir1 115.94(8) . . ?
C43 P3 Ir1 116.79(8) . . ?
C49 P3 C37 102.43(11) . . ?
C49 P3 C43 101.54(11) . . ?
C49 P3 Ir1 120.03(7) . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
O1 C55 H55A 109.5 . . ?
O1 C55 H55B 109.5 . . ?
O1 C55 H55C 109.5 . . ?
C55 O1 H1 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
C1 C2 C3 C4 -0.5(4) . . . . ?
C2 C1 C6 C5 -2.5(3) . . . . ?
C2 C1 P1 C7 -98.4(2) . . . . ?
C2 C1 P1 C13 156.52(19) . . . . ?
C2 C1 P1 Ir1 25.2(2) . . . . ?
C2 C3 C4 C5 -1.3(4) . . . . ?
C3 C4 C5 C6 1.1(4) . . . . ?
C4 C5 C6 C1 0.8(4) . . . . ?
C6 C1 C2 C3 2.3(4) . . . . ?
C6 C1 P1 C7 77.7(2) . . . . ?
C6 C1 P1 C13 -27.4(2) . . . . ?
C6 C1 P1 Ir1 -158.73(16) . . . . ?
C7 C8 C9 C10 0.0(5) . . . . ?
C8 C7 C12 C11 1.9(4) . . . . ?
C8 C7 P1 C1 103.4(2) . . . . ?
C8 C7 P1 C13 -153.0(2) . . . . ?
C8 C7 P1 Ir1 -20.5(2) . . . . ?
C8 C9 C10 C11 0.7(5) . . . . ?
C9 C10 C11 C12 -0.1(4) . . . . ?
C10 C11 C12 C7 -1.2(4) . . . . ?
C12 C7 C8 C9 -1.3(4) . . . . ?
C12 C7 P1 C1 -70.2(2) . . . . ?
C12 C7 P1 C13 33.4(2) . . . . ?
C12 C7 P1 Ir1 165.91(18) . . . . ?
C13 C14 C15 C16 0.1(4) . . . . ?
C14 C13 C18 C17 1.6(3) . . . . ?
C14 C13 P1 C1 -47.9(2) . . . . ?
C14 C13 P1 C7 -148.52(19) . . . . ?
C14 C13 P1 Ir1 81.2(2) . . . . ?
C14 C15 C16 C17 1.1(4) . . . . ?
C15 C16 C17 C18 -0.9(4) . . . . ?
C16 C17 C18 C13 -0.4(4) . . . . ?
C18 C13 C14 C15 -1.4(3) . . . . ?
C18 C13 P1 C1 137.4(2) . . . . ?
C18 C13 P1 C7 36.8(2) . . . . ?
C18 C13 P1 Ir1 -93.45(19) . . . . ?
C19 C20 C21 C22 -0.4(4) . . . . ?
C20 C19 C24 C23 1.1(4) . . . . ?
C20 C19 P2 C25 -99.4(2) . . . . ?
C20 C19 P2 C31 156.80(19) . . . . ?
C20 C19 P2 Ir1 22.8(2) . . . . ?
C20 C21 C22 C23 0.7(4) . . . . ?
C21 C22 C23 C24 0.0(4) . . . . ?
C22 C23 C24 C19 -0.9(4) . . . . ?
C24 C19 C20 C21 -0.5(4) . . . . ?
C24 C19 P2 C25 71.2(2) . . . . ?
C24 C19 P2 C31 -32.6(2) . . . . ?
C24 C19 P2 Ir1 -166.60(17) . . . . ?
C25 C26 C27 C28 -0.4(4) . . . . ?
C26 C25 C30 C29 1.4(3) . . . . ?
C26 C25 P2 C19 -72.2(2) . . . . ?
C26 C25 P2 C31 32.0(2) . . . . ?
C26 C25 P2 Ir1 165.64(17) . . . . ?
C26 C27 C28 C29 1.3(4) . . . . ?
C27 C28 C29 C30 -0.9(4) . . . . ?
C28 C29 C30 C25 -0.5(4) . . . . ?
C30 C25 C26 C27 -1.0(4) . . . . ?
C30 C25 P2 C19 96.67(19) . . . . ?
C30 C25 P2 C31 -159.08(18) . . . . ?
C30 C25 P2 Ir1 -25.5(2) . . . . ?
C31 C32 C33 C34 -0.1(4) . . . . ?
C32 C31 C36 C35 1.0(4) . . . . ?
C32 C31 P2 C19 -45.0(2) . . . . ?
C32 C31 P2 C25 -142.9(2) . . . . ?
C32 C31 P2 Ir1 86.3(2) . . . . ?
C32 C33 C34 C35 1.0(5) . . . . ?
C33 C34 C35 C36 -1.0(5) . . . . ?
C34 C35 C36 C31 0.0(5) . . . . ?
C36 C31 C32 C33 -0.9(4) . . . . ?
C36 C31 P2 C19 140.6(2) . . . . ?
C36 C31 P2 C25 42.8(2) . . . . ?
C36 C31 P2 Ir1 -88.1(2) . . . . ?
C37 C38 C39 C40 0.4(4) . . . . ?
C38 C37 C42 C41 1.2(4) . . . . ?
C38 C37 P3 C43 107.0(2) . . . . ?
C38 C37 P3 C49 -149.7(2) . . . . ?
C38 C37 P3 Ir1 -17.0(2) . . . . ?
C38 C39 C40 C41 0.5(4) . . . . ?
C39 C40 C41 C42 -0.6(4) . . . . ?
C40 C41 C42 C37 -0.3(4) . . . . ?
C42 C37 C38 C39 -1.2(4) . . . . ?
C42 C37 P3 C43 -67.7(2) . . . . ?
C42 C37 P3 C49 35.7(2) . . . . ?
C42 C37 P3 Ir1 168.33(17) . . . . ?
C43 C44 C45 C46 1.1(4) . . . . ?
C44 C43 C48 C47 0.8(4) . . . . ?
C44 C43 P3 C37 81.0(2) . . . . ?
C44 C43 P3 C49 -23.2(2) . . . . ?
C44 C43 P3 Ir1 -155.65(17) . . . . ?
C44 C45 C46 C47 0.1(4) . . . . ?
C45 C46 C47 C48 -0.9(4) . . . . ?
C46 C47 C48 C43 0.4(4) . . . . ?
C48 C43 C44 C45 -1.5(4) . . . . ?
C48 C43 P3 C37 -93.1(2) . . . . ?
C48 C43 P3 C49 162.79(19) . . . . ?
C48 C43 P3 Ir1 30.3(2) . . . . ?
C49 C50 C51 C52 0.7(4) . . . . ?
C50 C49 C54 C53 0.3(3) . . . . ?
C50 C49 P3 C37 -149.56(18) . . . . ?
C50 C49 P3 C43 -50.2(2) . . . . ?
C50 C49 P3 Ir1 80.29(19) . . . . ?
C50 C51 C52 C53 0.1(4) . . . . ?
C51 C52 C53 C54 -0.6(4) . . . . ?
C52 C53 C54 C49 0.4(4) . . . . ?
C54 C49 C50 C51 -0.9(3) . . . . ?
C54 C49 P3 C37 36.2(2) . . . . ?
C54 C49 P3 C43 135.51(19) . . . . ?
C54 C49 P3 Ir1 -93.99(19) . . . . ?
P1 C1 C2 C3 178.48(19) . . . . ?
P1 C1 C6 C5 -178.54(18) . . . . ?
P1 C7 C8 C9 -175.2(2) . . . . ?
P1 C7 C12 C11 175.6(2) . . . . ?
P1 C13 C14 C15 -176.32(18) . . . . ?
P1 C13 C18 C17 176.28(18) . . . . ?
P2 C19 C20 C21 170.40(19) . . . . ?
P2 C19 C24 C23 -169.6(2) . . . . ?
P2 C25 C26 C27 167.87(19) . . . . ?
P2 C25 C30 C29 -167.88(18) . . . . ?
P2 C31 C32 C33 -175.5(2) . . . . ?
P2 C31 C36 C35 175.4(2) . . . . ?
P3 C37 C38 C39 -176.00(18) . . . . ?
P3 C37 C42 C41 176.0(2) . . . . ?
P3 C43 C44 C45 -175.56(19) . . . . ?
P3 C43 C48 C47 175.01(19) . . . . ?
P3 C49 C50 C51 -175.38(18) . . . . ?
P3 C49 C54 C53 174.71(18) . . . . ?

_olex2_date_sample_data_collection 2019-09-06
_olex2_date_sample_submission    2019-09-03
_olex2_exptl_crystal_mounting_method 'oil on micromount'
_olex2_submission_original_sample_id 'BT PPh3'
_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 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.794
####################################################################### 
# 
# 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_sbd1906
_database_code_depnum_ccdc_archive 'CCDC 1957543'
loop_
_audit_author_name
_audit_author_address
'Adrian C. Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2019-10-04 deposited with the CCDC.	2019-12-10 downloaded from the CCDC.
;
_audit_creation_date             2019-09-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H64 Cl2 Ir2 N4 S2, C H4 O'
_chemical_formula_sum            'C57 H68 Cl2 Ir2 N4 O S2'
_chemical_formula_weight         1344.57
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C57 H64 Cl2 Ir2 N4 O S2'
_chemical_oxdiff_usercomment     'Ben Tickner BT Ma1'
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'
Cl Cl 0.3639 0.7018 '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'
S S 0.3331 0.5567 '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 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   12.9317(2)
_cell_length_b                   16.6000(3)
_cell_length_c                   25.5365(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.2757(13)
_cell_angle_gamma                90
_cell_volume                     5481.76(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9511
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.9880
_cell_measurement_theta_min      6.5490
_shelx_estimated_absorpt_T_max   0.476
_shelx_estimated_absorpt_T_min   0.286
_exptl_absorpt_coefficient_mu    11.192
_exptl_absorpt_correction_T_max  0.674
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0444
-1 1 2 0.0518
1 1 -5 0.0332
-1 -1 0 0.0661
-2 -1 -2 0.0572
-1 0 -2 0.0535
0 1 -2 0.0254
2 1 -1 0.0654
-1 0 1 0.0657
1 -2 -1 0.0426
2 -2 -1 0.0549
-1 2 1 0.0476
0 2 1 0.0427
0 -2 -1 0.0355
1 1 2 0.0587
0 0 1 0.0395

_exptl_crystal_recrystallization_method 'crystallisation from methanol'
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.078
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
-0.0002 -0.0010 -1.0002 -0.0284 -0.0531 0.0048
-0.9972 1.0043 2.0004 -0.0674 0.1764 0.0393
0.9993 0.9957 -5.0009 -0.1588 -0.2688 -0.1260
-1.0001 -1.0007 -0.0002 0.0169 0.0035 0.1501
-1.9993 -1.0020 -2.0008 -0.0935 -0.0657 0.2592
-0.9992 -0.0013 -2.0006 -0.1104 -0.0692 0.1092
0.0009 0.9995 -2.0004 -0.1273 -0.0727 -0.0409
1.9988 0.9990 -0.9999 0.0084 -0.0935 -0.2448
-0.9987 0.0018 1.0001 -0.0253 0.0899 0.0947
0.9961 -2.0048 -1.0003 0.1663 -0.1567 0.0064
1.9949 -2.0055 -1.0001 0.2200 -0.1936 -0.0931
-0.9961 2.0048 1.0003 -0.1663 0.1567 -0.0064
0.0027 2.0040 1.0004 -0.1127 0.1198 -0.1059
-0.0027 -2.0040 -1.0004 0.1127 -0.1198 0.1059
1.0005 1.0028 2.0007 0.0399 0.1026 -0.1597
0.0002 0.0010 1.0002 0.0284 0.0531 -0.0048

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20688
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         3.462
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -13.00  52.00   1.00    1.00    --    0.00  57.00 -60.00   65
  2  ω    -51.00 -20.00   1.00    1.00    --    0.00 124.00 101.00   31
  3  ω    -13.00  13.00   1.00    3.00    --   54.00 -57.00-150.00   26
  4  ω     27.00 105.00   1.00    3.00    --   54.00-125.00 120.00   78
  5  ω    -19.00  98.00   1.00    3.00    --   54.00 -19.00 -60.00  117
  6  ω     40.00  74.00   1.00    3.00    --   54.00 -57.00 120.00   34
  7  ω     92.00 119.00   1.00    3.00    --   54.00  77.00 -90.00   27
  8  ω     39.00  97.00   1.00    3.00    --  108.00-111.00-120.00   58
  9  ω    124.00 176.00   1.00    3.00    --  108.00  50.00-150.00   52
 10  ω     38.00  92.00   1.00    3.00    --  108.00-111.00 120.00   54
 11  ω     77.00 103.00   1.00    3.00    --  108.00 -50.00 -30.00   26
 12  ω     36.00  88.00   1.00    3.00    --  108.00-111.00-180.00   52
 13  ω     38.00  73.00   1.00    3.00    --  108.00 -50.00 -30.00   35
 14  ω    106.00 171.00   1.00    3.00    --  108.00  63.00   0.00   65
 15  ω     77.00 113.00   1.00    3.00    --  108.00-111.00 -90.00   36
 16  ω     90.00 176.00   1.00    3.00    --  108.00  63.00 120.00   86
 17  ω    113.00 139.00   1.00    3.00    --  108.00 -12.00-150.00   26
 18  ω     36.00  73.00   1.00    3.00    --  108.00 -12.00-150.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0536477000
_diffrn_orient_matrix_UB_12      -0.0704874000
_diffrn_orient_matrix_UB_13      0.0284325000
_diffrn_orient_matrix_UB_21      -0.0369154000
_diffrn_orient_matrix_UB_22      0.0333776000
_diffrn_orient_matrix_UB_23      0.0530168000
_diffrn_orient_matrix_UB_31      -0.0996791000
_diffrn_orient_matrix_UB_32      -0.0503459000
_diffrn_orient_matrix_UB_33      -0.0047444000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8700
_reflns_number_total             9782
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.916
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         9782
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0299
_refine_ls_restrained_S_all      1.036
_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)+(0.0265P)²+13.1045P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0712
_refine_special_details          
;
The crystal showed evidence of minor twinning with two residual density 
peaks close to the iridiums.  This could not be resolved as either 
merohedral or non-merohedral twinning methods.

One of the 4-chlorobenzyl groups was disordered and modelled in
two positions with refined occupancies of 0.803:0.197(10). pairs of 
disordered carbons were constrained to have the same ADP (e.g. C43, & C43a,
C44 & C44a etc.).  The S-CH2 bond-lengths were restrained to be equal as were 
the CH2-C(ipso) bond-lengths and the C-Cl bond-lengths.  The phenyl ring
of the minor form was constrained to be a regular hexagon with a C-C bond
length of 1.39 angstroms.  For the minor form the CH2-C(ortho) distances were 
restrained to be equal as were the C(meta)-Cl distances.

The hydrides were initially located by difference map, the Ir-H bond-length
was then adjusted to be 1.65 angstroms and then the location fixed to ride
on the iridium.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C46A-Cl1A \\sim Cl1A-C48A
 with sigma of 0.02
 C43A-C44A \\sim C44-C43
 with sigma of 0.02
 S1-C43 \\sim S1-C43A
 with sigma of 0.02
 C49A-C43A \\sim C43A-C45A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C49A) = Uanis(C49)
Uanis(C48) = Uanis(C48A)
Uanis(C47A) = Uanis(C47)
Uanis(C46A) = Uanis(C46)
Uanis(C45A) = Uanis(C45)
Uanis(C44A) = Uanis(C44)
Uanis(C43A) = Uanis(C43)
4. Others
 Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=
 Sof(H46A)=Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(Cl1A)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=
 Sof(C47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(Cl1)=FVAR(1)
5.a Riding coordinates:
 Ir1(H,HA), Ir2(HB,HC)
5.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C43A(H43C,H43D), C50(H50A,H50B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C23(H23), C24(H24),
 C27(H27), C29(H29), C36(H36), C38(H38), C45A(H45A), C46A(H46A), C48A(H48A),
 C49A(H49A), C45(H45), C46(H46), C48(H48), C49(H49), C52(H52), C53(H53),
 C55(H55), C56(H56)
5.d Fitted hexagon refined as free rotating group:
 C44A(C45A,C46A,C47A,C48A,C49A)
5.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C57(H57A,H57B,H57C)
5.f Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   mixed
_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
C0AA C 0.2422(4) 0.3839(3) 0.26156(17) 0.0310(10) Uani 1 1 d . . . . .
C2 C 0.2507(5) 0.4054(4) 0.17344(19) 0.0579(18) Uani 1 1 d . . . . .
H2 H 0.277677 0.408767 0.138962 0.070 Uiso 1 1 calc R . . . .
C3 C 0.1544(5) 0.4221(5) 0.1878(2) 0.068(2) Uani 1 1 d . . . . .
H3 H 0.100011 0.440039 0.165607 0.082 Uiso 1 1 calc R . . . .
C4 C 0.4124(4) 0.3623(3) 0.21638(16) 0.0304(10) Uani 1 1 d . . . . .
C5 C 0.4406(4) 0.2822(3) 0.20970(15) 0.0298(10) Uani 1 1 d . . . . .
C6 C 0.5454(4) 0.2640(3) 0.20476(17) 0.0372(11) Uani 1 1 d . . . . .
H6 H 0.566074 0.209398 0.201231 0.045 Uiso 1 1 calc R . . . .
C7 C 0.6198(4) 0.3238(4) 0.20487(17) 0.0409(12) Uani 1 1 d . . . . .
C8 C 0.5885(4) 0.4033(4) 0.21075(18) 0.0431(13) Uani 1 1 d . . . . .
H8 H 0.639251 0.444629 0.211150 0.052 Uiso 1 1 calc R . . . .
C9 C 0.4843(4) 0.4242(3) 0.21610(17) 0.0388(12) Uani 1 1 d . . . . .
C10 C 0.3602(4) 0.2163(3) 0.20645(19) 0.0425(12) Uani 1 1 d . . . . .
H10A H 0.330470 0.214991 0.171092 0.064 Uiso 1 1 calc GR . . . .
H10B H 0.305451 0.226797 0.231924 0.064 Uiso 1 1 calc GR . . . .
H10C H 0.392706 0.164243 0.214207 0.064 Uiso 1 1 calc GR . . . .
C11 C 0.7329(4) 0.3022(5) 0.1986(2) 0.067(2) Uani 1 1 d . . . . .
H11A H 0.751220 0.259435 0.223435 0.100 Uiso 1 1 calc GR . . . .
H11B H 0.775646 0.349802 0.205504 0.100 Uiso 1 1 calc GR . . . .
H11C H 0.745045 0.283305 0.162783 0.100 Uiso 1 1 calc GR . . . .
C12 C 0.4524(5) 0.5105(3) 0.2216(2) 0.0564(16) Uani 1 1 d . . . . .
H12A H 0.402020 0.523950 0.194178 0.085 Uiso 1 1 calc GR . . . .
H12B H 0.513179 0.545289 0.218247 0.085 Uiso 1 1 calc GR . . . .
H12C H 0.420941 0.518706 0.256062 0.085 Uiso 1 1 calc GR . . . .
C13 C 0.0547(4) 0.4278(3) 0.26964(18) 0.0391(12) Uani 1 1 d . . . . .
C14 C 0.0373(4) 0.5087(3) 0.28073(19) 0.0402(12) Uani 1 1 d . . . . .
C15 C -0.0582(4) 0.5291(3) 0.3024(2) 0.0424(12) Uani 1 1 d . . . . .
H15 H -0.072782 0.584114 0.309394 0.051 Uiso 1 1 calc R . . . .
C16 C -0.1323(4) 0.4717(3) 0.3139(2) 0.0417(12) Uani 1 1 d . . . . .
C17 C -0.1104(4) 0.3921(3) 0.3037(2) 0.0457(13) Uani 1 1 d . . . . .
H17 H -0.159562 0.352089 0.313015 0.055 Uiso 1 1 calc R . . . .
C18 C -0.0181(4) 0.3686(3) 0.2802(2) 0.0433(13) Uani 1 1 d . . . . .
C19 C 0.1174(5) 0.5718(4) 0.2705(3) 0.0635(18) Uani 1 1 d . . . . .
H19A H 0.136531 0.570623 0.233387 0.095 Uiso 1 1 calc GR . . . .
H19B H 0.178760 0.561008 0.292065 0.095 Uiso 1 1 calc GR . . . .
H19C H 0.089508 0.624920 0.279257 0.095 Uiso 1 1 calc GR . . . .
C20 C -0.2350(4) 0.4957(4) 0.3380(3) 0.0629(17) Uani 1 1 d . . . . .
H20A H -0.233793 0.483891 0.375618 0.094 Uiso 1 1 calc GR . . . .
H20B H -0.291023 0.465275 0.321248 0.094 Uiso 1 1 calc GR . . . .
H20C H -0.246536 0.553520 0.332726 0.094 Uiso 1 1 calc GR . . . .
C21 C 0.0000(5) 0.2817(4) 0.2657(3) 0.067(2) Uani 1 1 d . . . . .
H21A H -0.030376 0.270932 0.231201 0.101 Uiso 1 1 calc GR . . . .
H21B H -0.032440 0.246763 0.291854 0.101 Uiso 1 1 calc GR . . . .
H21C H 0.074454 0.271042 0.264763 0.101 Uiso 1 1 calc GR . . . .
C22 C 0.2556(3) 0.2869(3) 0.49085(16) 0.0292(10) Uani 1 1 d . . . . .
C23 C 0.1576(4) 0.3373(3) 0.55626(19) 0.0419(12) Uani 1 1 d . . . . .
H23 H 0.115030 0.373239 0.575500 0.050 Uiso 1 1 calc R . . . .
C24 C 0.1889(4) 0.2646(3) 0.57186(18) 0.0411(12) Uani 1 1 d . . . . .
H24 H 0.173285 0.238867 0.604088 0.049 Uiso 1 1 calc R . . . .
C25 C 0.1818(4) 0.4268(3) 0.48070(18) 0.0372(11) Uani 1 1 d . . . . .
C26 C 0.2560(5) 0.4862(3) 0.4874(2) 0.0454(13) Uani 1 1 d . . . . .
C27 C 0.2352(5) 0.5597(4) 0.4629(2) 0.0600(18) Uani 1 1 d . . . . .
H27 H 0.283280 0.602659 0.466369 0.072 Uiso 1 1 calc R . . . .
C28 C 0.1457(6) 0.5715(4) 0.4334(2) 0.0572(16) Uani 1 1 d . . . . .
C29 C 0.0756(5) 0.5107(3) 0.4288(2) 0.0502(14) Uani 1 1 d . . . . .
H29 H 0.014352 0.519570 0.408943 0.060 Uiso 1 1 calc R . . . .
C30 C 0.0909(4) 0.4368(3) 0.45191(19) 0.0417(12) Uani 1 1 d . . . . .
C31 C 0.3538(5) 0.4719(4) 0.5189(2) 0.0590(17) Uani 1 1 d . . . . .
H31A H 0.335789 0.450978 0.553567 0.088 Uiso 1 1 calc GR . . . .
H31B H 0.391540 0.522790 0.522863 0.088 Uiso 1 1 calc GR . . . .
H31C H 0.397494 0.432740 0.500704 0.088 Uiso 1 1 calc GR . . . .
C32 C 0.1283(7) 0.6532(4) 0.4081(3) 0.092(3) Uani 1 1 d . . . . .
H32A H 0.089472 0.646320 0.375320 0.138 Uiso 1 1 calc GR . . . .
H32B H 0.195162 0.678399 0.400638 0.138 Uiso 1 1 calc GR . . . .
H32C H 0.088889 0.687719 0.431914 0.138 Uiso 1 1 calc GR . . . .
C33 C 0.0119(4) 0.3715(4) 0.4457(2) 0.0492(14) Uani 1 1 d . . . . .
H33A H 0.044672 0.323458 0.430845 0.074 Uiso 1 1 calc GR . . . .
H33B H -0.043384 0.389946 0.422206 0.074 Uiso 1 1 calc GR . . . .
H33C H -0.017375 0.358259 0.479971 0.074 Uiso 1 1 calc GR . . . .
C34 C 0.2975(4) 0.1567(3) 0.53664(16) 0.0330(10) Uani 1 1 d . . . . .
C35 C 0.3980(4) 0.1529(3) 0.55631(16) 0.0346(11) Uani 1 1 d . . . . .
C36 C 0.4392(4) 0.0769(3) 0.56540(18) 0.0409(12) Uani 1 1 d . . . . .
H36 H 0.507100 0.072824 0.579524 0.049 Uiso 1 1 calc R . . . .
C37 C 0.3849(4) 0.0065(3) 0.55460(18) 0.0409(12) Uani 1 1 d . . . . .
C38 C 0.2855(4) 0.0132(3) 0.53551(18) 0.0390(11) Uani 1 1 d . . . . .
H38 H 0.247003 -0.034488 0.528664 0.047 Uiso 1 1 calc R . . . .
C39 C 0.2398(4) 0.0874(3) 0.52597(18) 0.0359(11) Uani 1 1 d . . . . .
C40 C 0.4604(4) 0.2273(4) 0.5678(2) 0.0471(13) Uani 1 1 d . . . . .
H40A H 0.490103 0.247913 0.535225 0.071 Uiso 1 1 calc GR . . . .
H40B H 0.516238 0.213974 0.592433 0.071 Uiso 1 1 calc GR . . . .
H40C H 0.415625 0.268410 0.583286 0.071 Uiso 1 1 calc GR . . . .
C41 C 0.4350(5) -0.0742(4) 0.5638(2) 0.0536(15) Uani 1 1 d . . . . .
H41A H 0.502317 -0.075614 0.546333 0.080 Uiso 1 1 calc GR . . . .
H41B H 0.390628 -0.116805 0.549447 0.080 Uiso 1 1 calc GR . . . .
H41C H 0.444611 -0.082727 0.601437 0.080 Uiso 1 1 calc GR . . . .
C42 C 0.1312(4) 0.0937(4) 0.5047(2) 0.0512(14) Uani 1 1 d . . . . .
H42A H 0.088956 0.125724 0.528719 0.077 Uiso 1 1 calc GR . . . .
H42B H 0.101487 0.039661 0.501232 0.077 Uiso 1 1 calc GR . . . .
H42C H 0.132556 0.119865 0.470299 0.077 Uiso 1 1 calc GR . . . .
C43 C 0.2126(10) 0.1586(4) 0.3268(4) 0.0385(13) Uani 0.802(10) 1 d D . P A 1
H43A H 0.164998 0.159028 0.296303 0.046 Uiso 0.802(10) 1 calc R . P A 1
H43B H 0.283955 0.163214 0.313262 0.046 Uiso 0.802(10) 1 calc R . P A 1
C43A C 0.219(4) 0.1649(13) 0.3227(13) 0.0385(13) Uani 0.198(10) 1 d D . P A 2
H43C H 0.181325 0.170914 0.288969 0.046 Uiso 0.198(10) 1 calc R . P A 2
H43D H 0.293987 0.164602 0.315697 0.046 Uiso 0.198(10) 1 calc R . P A 2
C44 C 0.2022(6) 0.0807(5) 0.3541(4) 0.0329(15) Uani 0.802(10) 1 d D . P A 1
C44A C 0.187(2) 0.0903(17) 0.3493(15) 0.0329(15) Uani 0.198(10) 1 d D . P A 2
C45A C 0.083(2) 0.0707(16) 0.3533(14) 0.051(2) Uani 0.198(10) 1 d DG . P A 2
H45A H 0.032081 0.106502 0.340089 0.062 Uiso 0.198(10) 1 calc R . P A 2
C46A C 0.0538(16) -0.0013(15) 0.3767(11) 0.070(3) Uani 0.198(10) 1 d DG . P A 2
H46A H -0.017423 -0.014744 0.379419 0.084 Uiso 0.198(10) 1 calc R . P A 2
C47A C 0.1285(17) -0.0538(13) 0.3961(11) 0.052(2) Uani 0.198(10) 1 d G . P A 2
C48A C 0.2327(16) -0.0342(15) 0.3921(11) 0.0444(17) Uani 0.198(10) 1 d DG . P A
2
H48A H 0.283790 -0.069991 0.405332 0.053 Uiso 0.198(10) 1 calc R . P A 2
C49A C 0.2621(17) 0.0379(17) 0.3687(13) 0.0372(17) Uani 0.198(10) 1 d DG . P A
2
H49A H 0.333296 0.051255 0.366003 0.045 Uiso 0.198(10) 1 calc R . P A 2
C45 C 0.1070(6) 0.0406(5) 0.3576(4) 0.051(2) Uani 0.802(10) 1 d . . P A 1
H45 H 0.048445 0.063121 0.340373 0.062 Uiso 0.802(10) 1 calc R . P A 1
C46 C 0.0953(7) -0.0292(6) 0.3848(4) 0.070(3) Uani 0.802(10) 1 d . . P A 1
H46 H 0.030027 -0.055345 0.385730 0.084 Uiso 0.802(10) 1 calc R . P A 1
C47 C 0.1776(7) -0.0614(4) 0.4106(3) 0.052(2) Uani 0.802(10) 1 d . . P A 1
C48 C 0.2727(6) -0.0268(4) 0.4077(3) 0.0444(17) Uani 0.802(10) 1 d . . P A 1
H48 H 0.330394 -0.051465 0.424346 0.053 Uiso 0.802(10) 1 calc R . P A 1
C49 C 0.2849(6) 0.0445(5) 0.3803(3) 0.0372(17) Uani 0.802(10) 1 d . . P A 1
H49 H 0.351059 0.069316 0.379339 0.045 Uiso 0.802(10) 1 calc R . P A 1
C50 C 0.5390(3) 0.3273(3) 0.34595(17) 0.0292(9) Uani 1 1 d . . . . .
H50A H 0.555275 0.350275 0.311168 0.035 Uiso 1 1 calc R . . . .
H50B H 0.525970 0.372798 0.370138 0.035 Uiso 1 1 calc R . . . .
C51 C 0.6311(3) 0.2806(3) 0.36543(17) 0.0303(10) Uani 1 1 d . . . . .
C52 C 0.6779(4) 0.3011(3) 0.4130(2) 0.0424(12) Uani 1 1 d . . . . .
H52 H 0.650135 0.343537 0.433497 0.051 Uiso 1 1 calc R . . . .
C53 C 0.7646(5) 0.2600(4) 0.4305(3) 0.0566(16) Uani 1 1 d . . . . .
H53 H 0.796827 0.274239 0.462663 0.068 Uiso 1 1 calc R . . . .
C54 C 0.8032(4) 0.1981(4) 0.4005(3) 0.0567(16) Uani 1 1 d . . . . .
C55 C 0.7566(4) 0.1755(4) 0.3544(2) 0.0538(15) Uani 1 1 d . . . . .
H55 H 0.783271 0.131802 0.334577 0.065 Uiso 1 1 calc R . . . .
C56 C 0.6705(4) 0.2169(3) 0.3371(2) 0.0409(12) Uani 1 1 d . . . . .
H56 H 0.637866 0.201414 0.305233 0.049 Uiso 1 1 calc R . . . .
Cl1 Cl 0.1612(4) -0.14952(16) 0.44671(12) 0.0881(11) Uani 0.802(10) 1 d . . P A
1
Cl1A Cl 0.092(2) -0.1454(7) 0.4150(12) 0.146(14) Uani 0.198(10) 1 d D . P A 2
Cl2 Cl 0.91403(12) 0.14677(13) 0.42033(11) 0.0991(8) Uani 1 1 d . . . . .
Ir1 Ir 0.27973(2) 0.36413(2) 0.33525(2) 0.02535(6) Uani 1 1 d . . . . .
H H 0.358988 0.439517 0.322706 0.068(19) Uiso 1 1 d R . . . .
HA H 0.183988 0.428027 0.344966 0.047(15) Uiso 1 1 d R . . . .
Ir2 Ir 0.33547(2) 0.27300(2) 0.42294(2) 0.02557(6) Uani 1 1 d . . . . .
HB H 0.439088 0.324491 0.440569 0.10(2) Uiso 1 1 d R . . . .
HC H 0.389488 0.193161 0.450159 0.08(2) Uiso 1 1 d R . . . .
N1 N 0.3045(3) 0.3823(3) 0.21792(14) 0.0353(9) Uani 1 1 d . . . . .
N2 N 0.1481(3) 0.4084(3) 0.24140(15) 0.0457(11) Uani 1 1 d . . . . .
N3 N 0.1983(3) 0.3512(2) 0.50698(14) 0.0340(9) Uani 1 1 d . . . . .
N4 N 0.2491(3) 0.2341(2) 0.53133(14) 0.0323(9) Uani 1 1 d . . . . .
S1 S 0.18491(9) 0.24786(7) 0.36789(4) 0.0312(2) Uani 1 1 d D . . . .
S2 S 0.42171(8) 0.26690(6) 0.34048(4) 0.0262(2) Uani 1 1 d . . . . .
C57 C 0.4545(6) 0.5665(4) 0.3773(3) 0.070(2) Uani 1 1 d . . . . .
H57A H 0.501637 0.540637 0.352511 0.105 Uiso 1 1 calc GR . . . .
H57B H 0.441631 0.529931 0.406730 0.105 Uiso 1 1 calc GR . . . .
H57C H 0.485733 0.616383 0.390393 0.105 Uiso 1 1 calc GR . . . .
O1 O 0.3598(4) 0.5844(2) 0.35177(17) 0.0616(11) Uani 1 1 d . . . . .
H1 H 0.331515 0.541376 0.341897 0.092 Uiso 1 1 calc GR . . . .


_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
C0AA Ir1 1.969(4) . ?
C0AA N1 1.379(6) . ?
C0AA N2 1.380(6) . ?
C2 C3 1.329(8) . ?
C2 N1 1.383(6) . ?
C3 N2 1.389(6) . ?
C4 C5 1.390(6) . ?
C4 C9 1.386(7) . ?
C4 N1 1.436(6) . ?
C5 C6 1.395(7) . ?
C5 C10 1.510(7) . ?
C6 C7 1.383(8) . ?
C7 C8 1.388(8) . ?
C7 C11 1.515(7) . ?
C8 C9 1.398(7) . ?
C9 C12 1.497(7) . ?
C13 C14 1.390(7) . ?
C13 C18 1.389(8) . ?
C13 N2 1.446(6) . ?
C14 C15 1.397(7) . ?
C14 C19 1.498(8) . ?
C15 C16 1.383(7) . ?
C16 C17 1.376(8) . ?
C16 C20 1.520(7) . ?
C17 C18 1.396(7) . ?
C18 C21 1.506(7) . ?
C22 Ir2 2.036(4) . ?
C22 N3 1.364(6) . ?
C22 N4 1.359(6) . ?
C23 C24 1.333(7) . ?
C23 N3 1.386(6) . ?
C24 N4 1.394(6) . ?
C25 C26 1.386(8) . ?
C25 C30 1.393(7) . ?
C25 N3 1.439(6) . ?
C26 C27 1.397(8) . ?
C26 C31 1.516(8) . ?
C27 C28 1.390(9) . ?
C28 C29 1.362(9) . ?
C28 C32 1.520(9) . ?
C29 C30 1.375(7) . ?
C30 C33 1.498(8) . ?
C34 C35 1.393(7) . ?
C34 C39 1.398(7) . ?
C34 N4 1.435(6) . ?
C35 C36 1.388(7) . ?
C35 C40 1.504(7) . ?
C36 C37 1.390(8) . ?
C37 C38 1.377(7) . ?
C37 C41 1.506(7) . ?
C38 C39 1.388(7) . ?
C39 C42 1.507(7) . ?
C43 C44 1.476(8) . ?
C43 S1 1.851(6) . ?
C43A C44A 1.472(19) . ?
C43A S1 1.851(17) . ?
C44 C45 1.402(9) . ?
C44 C49 1.395(9) . ?
C44A C45A 1.3900 . ?
C44A C49A 1.3900 . ?
C45A C46A 1.3900 . ?
C46A C47A 1.3900 . ?
C47A C48A 1.3900 . ?
C47A Cl1A 1.66(2) . ?
C48A C49A 1.3900 . ?
C45 C46 1.360(10) . ?
C46 C47 1.358(11) . ?
C47 C48 1.359(10) . ?
C47 Cl1 1.743(8) . ?
C48 C49 1.384(10) . ?
C50 C51 1.504(6) . ?
C50 S2 1.823(4) . ?
C51 C52 1.396(7) . ?
C51 C56 1.380(7) . ?
C52 C53 1.384(8) . ?
C53 C54 1.376(9) . ?
C54 C55 1.374(9) . ?
C54 Cl2 1.740(6) . ?
C55 C56 1.379(8) . ?
Ir1 Ir2 2.7941(3) . ?
Ir1 S1 2.4357(12) . ?
Ir1 S2 2.4478(11) . ?
Ir2 S1 2.4321(11) . ?
Ir2 S2 2.3896(9) . ?
C57 O1 1.417(8) . ?

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
N1 C0AA Ir1 128.8(3) . . ?
N1 C0AA N2 102.8(4) . . ?
N2 C0AA Ir1 128.2(3) . . ?
C3 C2 N1 107.4(4) . . ?
C2 C3 N2 107.4(5) . . ?
C5 C4 N1 118.7(4) . . ?
C9 C4 C5 122.3(4) . . ?
C9 C4 N1 118.7(4) . . ?
C4 C5 C6 118.2(4) . . ?
C4 C5 C10 121.3(4) . . ?
C6 C5 C10 120.5(4) . . ?
C7 C6 C5 121.4(5) . . ?
C6 C7 C8 118.6(5) . . ?
C6 C7 C11 120.1(6) . . ?
C8 C7 C11 121.3(6) . . ?
C7 C8 C9 121.9(5) . . ?
C4 C9 C8 117.5(5) . . ?
C4 C9 C12 121.6(5) . . ?
C8 C9 C12 120.9(5) . . ?
C14 C13 N2 117.0(5) . . ?
C18 C13 C14 122.3(5) . . ?
C18 C13 N2 120.5(5) . . ?
C13 C14 C15 117.3(5) . . ?
C13 C14 C19 121.8(5) . . ?
C15 C14 C19 120.9(5) . . ?
C16 C15 C14 122.1(5) . . ?
C15 C16 C20 120.9(5) . . ?
C17 C16 C15 118.5(5) . . ?
C17 C16 C20 120.6(5) . . ?
C16 C17 C18 121.8(5) . . ?
C13 C18 C17 117.8(5) . . ?
C13 C18 C21 121.6(5) . . ?
C17 C18 C21 120.5(5) . . ?
N3 C22 Ir2 128.6(3) . . ?
N4 C22 Ir2 127.5(3) . . ?
N4 C22 N3 103.9(3) . . ?
C24 C23 N3 107.8(4) . . ?
C23 C24 N4 106.1(4) . . ?
C26 C25 C30 124.2(5) . . ?
C26 C25 N3 117.5(5) . . ?
C30 C25 N3 118.2(5) . . ?
C25 C26 C27 115.8(6) . . ?
C25 C26 C31 122.0(5) . . ?
C27 C26 C31 122.2(6) . . ?
C28 C27 C26 121.5(6) . . ?
C27 C28 C32 118.5(7) . . ?
C29 C28 C27 119.6(6) . . ?
C29 C28 C32 121.8(7) . . ?
C28 C29 C30 122.0(6) . . ?
C25 C30 C33 122.9(5) . . ?
C29 C30 C25 116.9(5) . . ?
C29 C30 C33 120.2(5) . . ?
C35 C34 C39 121.9(5) . . ?
C35 C34 N4 118.8(4) . . ?
C39 C34 N4 119.1(4) . . ?
C34 C35 C40 122.1(5) . . ?
C36 C35 C34 117.3(5) . . ?
C36 C35 C40 120.6(5) . . ?
C35 C36 C37 122.5(5) . . ?
C36 C37 C41 120.0(5) . . ?
C38 C37 C36 118.2(5) . . ?
C38 C37 C41 121.8(5) . . ?
C37 C38 C39 121.9(5) . . ?
C34 C39 C42 120.6(5) . . ?
C38 C39 C34 118.1(5) . . ?
C38 C39 C42 121.3(5) . . ?
C44 C43 S1 114.5(6) . . ?
C44A C43A S1 106(2) . . ?
C45 C44 C43 121.9(6) . . ?
C49 C44 C43 122.2(6) . . ?
C49 C44 C45 115.9(6) . . ?
C45A C44A C43A 120.0(8) . . ?
C45A C44A C49A 120.0 . . ?
C49A C44A C43A 119.9(8) . . ?
C44A C45A C46A 120.0 . . ?
C45A C46A C47A 120.0 . . ?
C46A C47A Cl1A 118.7(8) . . ?
C48A C47A C46A 120.0 . . ?
C48A C47A Cl1A 120.6(7) . . ?
C49A C48A C47A 120.0 . . ?
C48A C49A C44A 120.0 . . ?
C46 C45 C44 122.4(7) . . ?
C47 C46 C45 119.6(7) . . ?
C46 C47 C48 121.0(7) . . ?
C46 C47 Cl1 119.3(6) . . ?
C48 C47 Cl1 119.7(6) . . ?
C47 C48 C49 119.6(6) . . ?
C48 C49 C44 121.4(6) . . ?
C51 C50 S2 113.5(3) . . ?
C52 C51 C50 120.1(4) . . ?
C56 C51 C50 121.0(4) . . ?
C56 C51 C52 118.8(5) . . ?
C53 C52 C51 120.5(5) . . ?
C54 C53 C52 119.0(6) . . ?
C53 C54 Cl2 120.4(5) . . ?
C55 C54 C53 121.4(5) . . ?
C55 C54 Cl2 118.2(5) . . ?
C54 C55 C56 119.3(5) . . ?
C55 C56 C51 120.9(5) . . ?
C0AA Ir1 Ir2 156.63(13) . . ?
C0AA Ir1 S1 109.70(14) . . ?
C0AA Ir1 S2 110.11(13) . . ?
S1 Ir1 Ir2 54.91(3) . . ?
S1 Ir1 S2 80.65(4) . . ?
S2 Ir1 Ir2 53.75(2) . . ?
C22 Ir2 Ir1 119.43(13) . . ?
C22 Ir2 S1 95.96(13) . . ?
C22 Ir2 S2 175.02(13) . . ?
S1 Ir2 Ir1 55.03(3) . . ?
S2 Ir2 Ir1 55.70(3) . . ?
S2 Ir2 S1 81.90(4) . . ?
C0AA N1 C2 111.4(4) . . ?
C0AA N1 C4 126.8(4) . . ?
C2 N1 C4 121.8(4) . . ?
C0AA N2 C3 111.0(4) . . ?
C0AA N2 C13 128.1(4) . . ?
C3 N2 C13 120.6(4) . . ?
C22 N3 C23 110.7(4) . . ?
C22 N3 C25 128.4(4) . . ?
C23 N3 C25 120.8(4) . . ?
C22 N4 C24 111.5(4) . . ?
C22 N4 C34 128.4(4) . . ?
C24 N4 C34 120.0(4) . . ?
C43 S1 Ir1 109.9(3) . . ?
C43 S1 Ir2 108.0(4) . . ?
C43A S1 Ir1 104.8(9) . . ?
C43A S1 Ir2 107.3(15) . . ?
Ir2 S1 Ir1 70.06(3) . . ?
C50 S2 Ir1 105.35(15) . . ?
C50 S2 Ir2 107.50(14) . . ?
Ir2 S2 Ir1 70.55(3) . . ?

_olex2_date_sample_data_collection 2019-09-20
_olex2_date_sample_submission    2019-09-19
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id 'BT Ma1'
_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 1.277
_oxdiff_exptl_absorpt_empirical_full_min 0.810
_vrf_PLAT415_sbd1906             
;
PROBLEM: Short Inter D-H..H-X H ..H1 . 1.80 Ang.
RESPONSE: The short-contact would correspond to a dihydrogen bond 
between the electronegative hydride and the protic hydrogen of the 
methanol.  Note that whilst there was evidence of the positions
of both hydrogens in the difference map, they were modelled
using a riding model otherwise their positions changed to unfeasible 
positions due to the minor unresolved twinning.
see e.g. DOI: 10.1021/acs.chemrev.6b00091
;
