# Electronic Supplementary Material (ESI) for Materials Advances.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_gaoxphf
_database_code_depnum_ccdc_archive 'CCDC 2163082'
loop_
_audit_author_name
_audit_author_address
'Toby Blundell'
;Nottingham Trent University
United Kingdom
;
_audit_update_record             
;
2022-03-29 deposited with the CCDC.	2022-04-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_gaoxphf             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note
RESPONSE: Due to reflections being hidden behind large beamstop overlay
;
# Added during the CSD deposition process: Tuesday 29 March 2022 03:41 PM
# end Validation Reply Form

_audit_creation_date             2022-03-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ga O12, 4(C10 H8 S8), C6 H5 F, 0.5(H6 O2)'
_chemical_formula_sum            'C52 H40 F Ga O13 S32'
_chemical_formula_weight         1987.48
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ga1 C20 S4 H27 N4 O12 F'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   10.2801(4)
_cell_length_b                   19.8975(10)
_cell_length_c                   35.2455(13)
_cell_angle_alpha                90
_cell_angle_beta                 92.680(3)
_cell_angle_gamma                90
_cell_volume                     7201.5(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6022
_cell_measurement_temperature    292.1(9)
_cell_measurement_theta_max      28.8450
_cell_measurement_theta_min      3.5610
_shelx_estimated_absorpt_T_max   0.935
_shelx_estimated_absorpt_T_min   0.821
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            19058
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.399
_diffrn_reflns_theta_min         2.884
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.1(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -76.00   43.00   1.0000   21.3850
omega____ theta____ kappa____ phi______ frames
    -      -16.0792    0.0000  -60.0000 119

#__ type_ start__ end____ width___ exp.time_
  2 omega  -72.00    1.00   1.0000   21.3850
omega____ theta____ kappa____ phi______ frames
    -      -16.0792  -57.0000  -60.0000 73

#__ type_ start__ end____ width___ exp.time_
  3 omega  -31.00    4.00   1.0000   21.3850
omega____ theta____ kappa____ phi______ frames
    -       16.2354  -37.0000   90.0000 35

#__ type_ start__ end____ width___ exp.time_
  4 omega   -6.00   20.00   1.0000   21.3850
omega____ theta____ kappa____ phi______ frames
    -       16.2354  -57.0000 -150.0000 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0087484000
_diffrn_orient_matrix_UB_12      0.0072110000
_diffrn_orient_matrix_UB_13      0.0196510000
_diffrn_orient_matrix_UB_21      0.0514183000
_diffrn_orient_matrix_UB_22      0.0224126000
_diffrn_orient_matrix_UB_23      -0.0038597000
_diffrn_orient_matrix_UB_31      -0.0452694000
_diffrn_orient_matrix_UB_32      0.0268146000
_diffrn_orient_matrix_UB_33      -0.0020561000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6975
_reflns_number_total             8480
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8480
_refine_ls_number_restraints     417
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0725
_refine_ls_restrained_S_all      11.200
_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)+(0.0347P)²+52.1914P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1542
_refine_special_details          
'Positional disorder was found for 2 terminal ethyl groups on the BEDT-TTF molecule (C1, C2 and C9 C10). The disorder was modelled, and the occupancy of the major and minor components competitively refined to 63:37 (C1, C2) and 55:45 (C9, C10) respectively. Relevant 1,2- bond distances were restrained to be approximately equal. Oxygen-hydrogen 1,2- distances for O1W were restrained to be aproximatley equal. Positional disorder was found for the fluorine atom of the Ph-F moiety (which lies on a special position) and competatively refined to a ratio of 69.4:15.3:15.3 (F1 : F2 : F2(1-X, Y, 0.5-Z)) . 1,2- bond distances were restrained to be aproximatley equal and the molecule was refined to be aproximatley flat. Enhanced rigid bond restraints were applied to all atoms.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1 times of:
  All O(H,H,H) groups
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O1W-H1Wa_$2 = O1W-H1Wc_$2 = O1W-H1Wb_$2
 0.83 with sigma of 0.02
 S8-C10 \\sim S8-C10A
 with sigma of 0.02
 F1-C24 \\sim F2-C26
 with sigma of 0.02
 F2-C25 \\sim F2-C27
 with sigma of 0.02
 S1-C1A \\sim S1-C1
 with sigma of 0.02
 S2-C2 \\sim S2-C2A
 with sigma of 0.02
 S7-C9A \\sim S7-C9
 with sigma of 0.02
 C2-C1 \\sim C2A-C1A
 with sigma of 0.02
 C9-C10 \\sim C10A-C9A
 with sigma of 0.02
 C2A-C1A \\sim C2-C1 \\sim C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 S1-C1 \\sim S1-C1A \\sim S2-C2A \\sim S2-C2 \\sim S8-C10A \\sim S8-C10 \\sim
S7-C9 \\sim S7-C9A
 with sigma of 0.02
3. Restrained planarity
 C25, C26, C27, F2, C26_$7, C24, C25_$7, F2_$7, F1
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C9A)=Sof(H9Aa)=Sof(H9Ab)=Sof(C10A)=Sof(H10c)=Sof(H10d)=1-FVAR(1)
 Sof(C10)=Sof(H10a)=Sof(H10b)=Sof(C9)=Sof(H9a)=Sof(H9b)=FVAR(1)
 Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=1-FVAR(2)
 Sof(C1)=Sof(H1a)=Sof(H1b)=Sof(C2)=Sof(H2a)=Sof(H2b)=FVAR(2)
 Sof(H24)=1-FVAR(3)
 Sof(F2)=0.5*(1-FVAR(4))
 Sof(F1)=0.5*FVAR(4)
 Sof(H26)=FVAR(3)
 Fixed Sof: H1Wa(0.5) H1Wb(0.5) H1Wc(0.5)
6.a Free rotating group:
 O1W(H1Wa,H1Wb,H1Wc)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C20(H20a,H20b), C1(H1a,H1b), C12(H12a,H12b), C2(H2a,H2b),
 C10(H10a,H10b), C9(H9a,H9b), C19(H19a,H19b), C9A(H9Aa,H9Ab), C10A(H10c,H10d),
 C1A(H1Aa,H1Ab), C2A(H2Aa,H2Ab)
6.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C26(H26), C25(H25), C24(H24)
;
_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
Ga1 Ga 0.500000 0.58317(4) 0.750000 0.03143(19) Uani 1 2 d S T P . .
S4 S 0.97393(12) 0.41125(7) 0.48076(3) 0.0353(3) Uani 1 1 d . . . . .
S3 S 0.74000(12) 0.48705(7) 0.45644(3) 0.0332(3) Uani 1 1 d . . . . .
S6 S 0.85225(12) 0.38234(7) 0.56127(3) 0.0352(3) Uani 1 1 d . . . . .
S11 S 0.33650(12) 0.35679(7) 0.46861(3) 0.0327(3) Uani 1 1 d . . . . .
S5 S 0.61615(12) 0.45682(7) 0.53709(4) 0.0338(3) Uani 1 1 d . . . . .
S14 S 0.45937(13) 0.25380(7) 0.57298(4) 0.0360(3) Uani 1 1 d . . . . .
S12 S 0.57697(12) 0.28538(7) 0.49113(4) 0.0355(3) Uani 1 1 d . . . . .
S13 S 0.22071(12) 0.32620(7) 0.54959(4) 0.0343(3) Uani 1 1 d . . . . .
S1 S 0.82732(13) 0.51723(8) 0.37960(4) 0.0432(4) Uani 1 1 d D . . . .
S7 S 0.47845(13) 0.42801(7) 0.60687(4) 0.0403(3) Uani 1 1 d D . . . .
S2 S 1.10769(14) 0.42982(9) 0.41017(4) 0.0502(4) Uani 1 1 d D . . . .
S10 S 0.70351(13) 0.30568(8) 0.41945(4) 0.0419(3) Uani 1 1 d . . . . .
S9 S 0.41307(13) 0.38903(8) 0.39128(4) 0.0390(3) Uani 1 1 d . . . . .
S8 S 0.75528(16) 0.34389(8) 0.63620(4) 0.0483(4) Uani 1 1 d D . . . .
S15 S 0.09311(15) 0.30645(8) 0.62162(5) 0.0476(4) Uani 1 1 d . . . . .
S16 S 0.38266(18) 0.22481(9) 0.65001(4) 0.0554(4) Uani 1 1 d . . . . .
C14 C 0.5665(5) 0.3193(2) 0.44527(13) 0.0298(10) Uani 1 1 d . . . . .
C7 C 0.6160(5) 0.4167(2) 0.58111(13) 0.0286(10) Uani 1 1 d . . . . .
C8 C 0.7251(5) 0.3831(3) 0.59248(13) 0.0304(10) Uani 1 1 d . . . . .
C18 C 0.3380(5) 0.2593(2) 0.60616(13) 0.0324(11) Uani 1 1 d . . . . .
C15 C 0.4237(5) 0.3121(2) 0.50341(13) 0.0287(10) Uani 1 1 d . . . . .
C13 C 0.4549(5) 0.3516(2) 0.43497(13) 0.0293(10) Uani 1 1 d . . . . .
O3 O 0.6515(3) 0.57182(19) 0.71817(10) 0.0372(8) Uani 1 1 d . . . . .
C4 C 0.9697(5) 0.4456(3) 0.43525(13) 0.0297(10) Uani 1 1 d . . . . .
C6 C 0.7684(4) 0.4274(2) 0.52565(13) 0.0278(10) Uani 1 1 d . . . . .
C17 C 0.2282(5) 0.2922(3) 0.59507(14) 0.0317(10) Uani 1 1 d . . . . .
C16 C 0.3745(5) 0.2985(2) 0.53776(13) 0.0284(10) Uani 1 1 d . . . . .
C3 C 0.8623(5) 0.4801(3) 0.42387(13) 0.0298(10) Uani 1 1 d . . . . .
C5 C 0.8201(5) 0.4399(2) 0.49169(13) 0.0288(10) Uani 1 1 d . . . . .
O5 O 0.5938(4) 0.51706(19) 0.78257(10) 0.0382(8) Uani 1 1 d . . . . .
O2 O 0.4275(4) 0.65785(19) 0.71891(10) 0.0435(9) Uani 1 1 d . . . . .
C22 C 0.6983(5) 0.4946(3) 0.76893(14) 0.0354(11) Uani 1 1 d . . . . .
C21 C 0.7308(5) 0.5260(3) 0.72985(14) 0.0354(11) Uani 1 1 d . . . . .
O4 O 0.8241(4) 0.5054(2) 0.71397(12) 0.0565(12) Uani 1 1 d . . . . .
C11 C 0.5680(5) 0.3935(3) 0.37029(15) 0.0379(12) Uani 1 1 d . . . . .
H11A H 0.554364 0.406418 0.343864 0.046 Uiso 1 1 calc R U . . .
H11B H 0.619017 0.428694 0.382937 0.046 Uiso 1 1 calc R U . . .
C23 C 0.4531(6) 0.7162(3) 0.73187(16) 0.0413(13) Uani 1 1 d . . . . .
O6 O 0.7698(4) 0.4525(2) 0.78361(12) 0.0537(11) Uani 1 1 d . . . . .
O1 O 0.4150(5) 0.7694(2) 0.71824(14) 0.0617(12) Uani 1 1 d . . . . .
C20 C 0.2392(7) 0.2377(4) 0.67614(17) 0.0653(19) Uani 1 1 d . . . . .
H20A H 0.178847 0.201247 0.670367 0.078 Uiso 1 1 calc R U . . .
H20B H 0.263136 0.235486 0.703059 0.078 Uiso 1 1 calc R U . . .
C1 C 0.9773(8) 0.5120(5) 0.3566(3) 0.037(3) Uani 0.631(17) 1 d D . P A 1
H1A H 0.961666 0.519710 0.329585 0.045 Uiso 0.631(17) 1 calc R U P A 1
H1B H 1.035701 0.546834 0.366410 0.045 Uiso 0.631(17) 1 calc R U P A 1
C12 C 0.6452(6) 0.3296(3) 0.37214(15) 0.0408(13) Uani 1 1 d . . . . .
H12A H 0.719460 0.334475 0.356350 0.049 Uiso 1 1 calc R U . . .
H12B H 0.591436 0.293566 0.361514 0.049 Uiso 1 1 calc R U . . .
C2 C 1.0402(14) 0.4447(6) 0.3627(3) 0.047(3) Uani 0.631(17) 1 d D . P A 1
H2A H 1.109363 0.440091 0.345019 0.057 Uiso 0.631(17) 1 calc R U P A 1
H2B H 0.976113 0.410129 0.356525 0.057 Uiso 0.631(17) 1 calc R U P A 1
C10 C 0.6371(14) 0.3784(7) 0.6670(4) 0.044(4) Uani 0.547(18) 1 d D . P B 1
H10A H 0.573491 0.343782 0.671811 0.053 Uiso 0.547(18) 1 calc R U P B 1
H10B H 0.681260 0.389370 0.691155 0.053 Uiso 0.547(18) 1 calc R U P B 1
C9 C 0.5658(12) 0.4398(6) 0.6526(3) 0.043(3) Uani 0.547(18) 1 d D . P B 1
H9A H 0.627881 0.476147 0.650343 0.052 Uiso 0.547(18) 1 calc R U P B 1
H9B H 0.504099 0.453310 0.671179 0.052 Uiso 0.547(18) 1 calc R U P B 1
C19 C 0.1697(8) 0.3039(4) 0.66807(18) 0.068(2) Uani 1 1 d . . . . .
H19A H 0.232042 0.340338 0.670715 0.082 Uiso 1 1 calc R U . . .
H19B H 0.104394 0.310599 0.686705 0.082 Uiso 1 1 calc R U . . .
C27 C 1.000000 0.3641(8) 0.250000 0.112(5) Uani 1 2 d DS T P C .
H27 H 0.999998 0.410803 0.249999 0.134 Uiso 1 2 calc R U P . .
C26 C 0.9127(10) 0.3236(6) 0.26353(19) 0.115(4) Uani 1 1 d D . . . .
H26 H 0.838042 0.346786 0.269680 0.138 Uiso 0.63(2) 1 calc R U P C 1
C25 C 0.9032(9) 0.2617(6) 0.2704(2) 0.096(3) Uani 1 1 d D . . . .
H25 H 0.843346 0.242337 0.286118 0.115 Uiso 1 1 calc R U . . .
C9A C 0.5194(13) 0.4020(8) 0.6544(3) 0.046(4) Uani 0.453(18) 1 d D . P B 2
H9AA H 0.475825 0.430933 0.671950 0.055 Uiso 0.453(18) 1 calc R U P B 2
H9AB H 0.488708 0.356432 0.658017 0.055 Uiso 0.453(18) 1 calc R U P B 2
C10A C 0.6638(13) 0.4047(9) 0.6630(5) 0.052(5) Uani 0.453(18) 1 d D . P B 2
H10C H 0.680829 0.396555 0.689945 0.062 Uiso 0.453(18) 1 calc R U P B 2
H10D H 0.694866 0.449494 0.657493 0.062 Uiso 0.453(18) 1 calc R U P B 2
C1A C 0.9402(14) 0.4672(10) 0.3528(4) 0.050(6) Uani 0.369(17) 1 d D . P A 2
H1AA H 0.911290 0.420819 0.353447 0.061 Uiso 0.369(17) 1 calc R U P A 2
H1AB H 0.932208 0.481731 0.326526 0.061 Uiso 0.369(17) 1 calc R U P A 2
C2A C 1.0817(15) 0.4684(14) 0.3648(5) 0.048(7) Uani 0.369(17) 1 d D . P A 2
H2AA H 1.112098 0.514542 0.366019 0.057 Uiso 0.369(17) 1 calc R U P A 2
H2AB H 1.131194 0.444724 0.346255 0.057 Uiso 0.369(17) 1 calc R U P A 2
F1 F 1.000000 0.1587(7) 0.250000 0.142(7) Uani 0.63(2) 2 d DS T P C 1
C24 C 1.000000 0.2254(8) 0.250000 0.098(4) Uani 1 2 d DS T P . .
H24 H 1.000000 0.178669 0.249999 0.117 Uiso 0.73(4) 2 calc R U P C 2
F2 F 0.848(2) 0.3592(11) 0.2873(7) 0.128(10) Uani 0.183(10) 1 d D . P C 2
O1W O 1.000000 0.4037(4) 0.750000 0.082(2) Uani 1 2 d DGS T P . .
H1WA H 1.072832 0.427116 0.750526 0.082 Uiso 0.5 1 d G U P D -1
H1WB H 0.942480 0.412077 0.766787 0.082 Uiso 0.5 1 d G U P E -1
H1WC H 0.982484 0.362976 0.740114 0.082 Uiso 0.5 1 d G U P F -1


_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
Ga1 O3 1.974(3) . ?
Ga1 O3 1.974(3) 2_656 ?
Ga1 O5 1.969(4) 2_656 ?
Ga1 O5 1.968(4) . ?
Ga1 O2 1.972(4) . ?
Ga1 O2 1.972(4) 2_656 ?
S4 C4 1.743(5) . ?
S4 C5 1.741(5) . ?
S3 C3 1.747(5) . ?
S3 C5 1.733(5) . ?
S6 C8 1.747(5) . ?
S6 C6 1.739(5) . ?
S11 C15 1.731(5) . ?
S11 C13 1.741(5) . ?
S5 C7 1.745(5) . ?
S5 C6 1.736(5) . ?
S14 C18 1.753(5) . ?
S14 C16 1.729(5) . ?
S12 C14 1.751(5) . ?
S12 C15 1.737(5) . ?
S13 C17 1.739(5) . ?
S13 C16 1.743(5) . ?
S1 C3 1.748(5) . ?
S1 C1 1.778(7) . ?
S1 C1A 1.826(12) . ?
S7 C7 1.730(5) . ?
S7 C9 1.824(9) . ?
S7 C9A 1.785(10) . ?
S2 C4 1.735(5) . ?
S2 C2 1.807(9) . ?
S2 C2A 1.782(12) . ?
S10 C14 1.734(5) . ?
S10 C12 1.809(6) . ?
S9 C13 1.746(5) . ?
S9 C11 1.790(5) . ?
S8 C8 1.742(5) . ?
S8 C10 1.803(10) . ?
S8 C10A 1.823(12) . ?
S15 C17 1.734(5) . ?
S15 C19 1.784(7) . ?
S16 C18 1.733(5) . ?
S16 C20 1.793(7) . ?
C14 C13 1.349(7) . ?
C7 C8 1.351(7) . ?
C18 C17 1.346(7) . ?
C15 C16 1.361(7) . ?
O3 C21 1.278(6) . ?
C4 C3 1.345(7) . ?
C6 C5 1.355(7) . ?
O5 C22 1.277(6) . ?
O2 C23 1.271(7) . ?
C22 C21 1.563(7) . ?
C22 O6 1.214(6) . ?
C21 O4 1.205(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.499(7) . ?
C23 C23 1.565(12) 2_656 ?
C23 O1 1.218(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C19 1.518(11) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.499(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.502(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C27 H27 0.9300 . ?
C27 C26 1.311(14) 2_755 ?
C27 C26 1.311(14) . ?
C26 H26 0.9300 . ?
C26 C25 1.261(14) . ?
C26 F2 1.31(2) . ?
C25 H25 0.9300 . ?
C25 C24 1.448(12) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C10A 1.503(14) . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C1A C2A 1.496(15) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
F1 C24 1.327(17) . ?
C24 H24 0.9300 . ?
O1W H1WA 0.8818 . ?
O1W H1WB 0.8721 . ?
O1W H1WC 0.8962 . ?

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
O3 Ga1 O3 166.9(2) 2_656 . ?
O5 Ga1 O3 82.93(15) . . ?
O5 Ga1 O3 88.30(15) 2_656 . ?
O5 Ga1 O3 88.30(15) . 2_656 ?
O5 Ga1 O3 82.93(15) 2_656 2_656 ?
O5 Ga1 O5 96.1(2) . 2_656 ?
O5 Ga1 O2 171.82(17) . . ?
O5 Ga1 O2 171.82(17) 2_656 2_656 ?
O5 Ga1 O2 91.00(16) . 2_656 ?
O5 Ga1 O2 91.00(16) 2_656 . ?
O2 Ga1 O3 93.32(16) . . ?
O2 Ga1 O3 93.32(16) 2_656 2_656 ?
O2 Ga1 O3 96.57(16) . 2_656 ?
O2 Ga1 O3 96.56(16) 2_656 . ?
O2 Ga1 O2 82.2(2) . 2_656 ?
C5 S4 C4 95.2(2) . . ?
C5 S3 C3 95.5(2) . . ?
C6 S6 C8 95.1(2) . . ?
C15 S11 C13 95.6(2) . . ?
C6 S5 C7 95.2(2) . . ?
C16 S14 C18 95.5(2) . . ?
C15 S12 C14 95.4(2) . . ?
C17 S13 C16 95.5(2) . . ?
C3 S1 C1 103.6(3) . . ?
C3 S1 C1A 97.0(6) . . ?
C7 S7 C9 95.7(4) . . ?
C7 S7 C9A 107.0(4) . . ?
C4 S2 C2 98.9(5) . . ?
C4 S2 C2A 106.7(7) . . ?
C14 S10 C12 101.6(2) . . ?
C13 S9 C11 101.5(2) . . ?
C8 S8 C10 105.4(4) . . ?
C8 S8 C10A 95.0(7) . . ?
C17 S15 C19 99.2(3) . . ?
C18 S16 C20 102.2(3) . . ?
S10 C14 S12 114.0(3) . . ?
C13 C14 S12 116.6(4) . . ?
C13 C14 S10 129.4(4) . . ?
S7 C7 S5 116.3(3) . . ?
C8 C7 S5 117.0(4) . . ?
C8 C7 S7 126.6(4) . . ?
S8 C8 S6 116.5(3) . . ?
C7 C8 S6 116.9(4) . . ?
C7 C8 S8 126.5(4) . . ?
S16 C18 S14 113.8(3) . . ?
C17 C18 S14 116.7(4) . . ?
C17 C18 S16 129.4(4) . . ?
S11 C15 S12 115.3(3) . . ?
C16 C15 S11 122.1(4) . . ?
C16 C15 S12 122.7(4) . . ?
S11 C13 S9 115.1(3) . . ?
C14 C13 S11 117.2(4) . . ?
C14 C13 S9 127.7(4) . . ?
C21 O3 Ga1 114.0(3) . . ?
S2 C4 S4 114.3(3) . . ?
C3 C4 S4 117.4(4) . . ?
C3 C4 S2 128.3(4) . . ?
S5 C6 S6 115.4(3) . . ?
C5 C6 S6 122.0(4) . . ?
C5 C6 S5 122.6(4) . . ?
S15 C17 S13 115.6(3) . . ?
C18 C17 S13 117.2(4) . . ?
C18 C17 S15 127.2(4) . . ?
S14 C16 S13 115.1(3) . . ?
C15 C16 S14 123.0(4) . . ?
C15 C16 S13 121.9(4) . . ?
S3 C3 S1 115.4(3) . . ?
C4 C3 S3 116.7(4) . . ?
C4 C3 S1 127.8(4) . . ?
S3 C5 S4 115.1(3) . . ?
C6 C5 S4 122.2(4) . . ?
C6 C5 S3 122.6(4) . . ?
C22 O5 Ga1 114.3(3) . . ?
C23 O2 Ga1 115.0(4) . . ?
O5 C22 C21 114.2(5) . . ?
O6 C22 O5 125.7(5) . . ?
O6 C22 C21 120.1(5) . . ?
O3 C21 C22 114.2(4) . . ?
O4 C21 O3 127.0(5) . . ?
O4 C21 C22 118.8(5) . . ?
S9 C11 H11A 108.6 . . ?
S9 C11 H11B 108.6 . . ?
H11A C11 H11B 107.5 . . ?
C12 C11 S9 114.8(4) . . ?
C12 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
O2 C23 C23 113.7(3) . 2_656 ?
O1 C23 O2 126.4(6) . . ?
O1 C23 C23 119.8(4) . 2_656 ?
S16 C20 H20A 108.6 . . ?
S16 C20 H20B 108.6 . . ?
H20A C20 H20B 107.5 . . ?
C19 C20 S16 114.8(5) . . ?
C19 C20 H20A 108.6 . . ?
C19 C20 H20B 108.6 . . ?
S1 C1 H1A 109.3 . . ?
S1 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 S1 111.4(8) . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
S10 C12 H12A 108.6 . . ?
S10 C12 H12B 108.6 . . ?
C11 C12 S10 114.5(4) . . ?
C11 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
S2 C2 H2A 108.5 . . ?
S2 C2 H2B 108.5 . . ?
C1 C2 S2 115.0(8) . . ?
C1 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
S8 C10 H10A 108.3 . . ?
S8 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C9 C10 S8 116.0(8) . . ?
C9 C10 H10A 108.3 . . ?
C9 C10 H10B 108.3 . . ?
S7 C9 H9A 108.8 . . ?
S7 C9 H9B 108.8 . . ?
C10 C9 S7 114.0(10) . . ?
C10 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
S15 C19 H19A 109.1 . . ?
S15 C19 H19B 109.1 . . ?
C20 C19 S15 112.4(5) . . ?
C20 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
C26 C27 H27 127.9 . . ?
C26 C27 H27 127.9 2_755 . ?
C26 C27 C26 104.3(15) 2_755 . ?
C27 C26 H26 111.5 . . ?
C25 C26 C27 136.9(12) . . ?
C25 C26 H26 111.5 . . ?
C25 C26 F2 111.1(12) . . ?
F2 C26 C27 106.3(12) . . ?
C26 C25 H25 125.4 . . ?
C26 C25 C24 109.3(11) . . ?
C24 C25 H25 125.4 . . ?
S7 C9A H9AA 109.3 . . ?
S7 C9A H9AB 109.3 . . ?
H9AA C9A H9AB 108.0 . . ?
C10A C9A S7 111.5(11) . . ?
C10A C9A H9AA 109.3 . . ?
C10A C9A H9AB 109.3 . . ?
S8 C10A H10C 108.9 . . ?
S8 C10A H10D 108.9 . . ?
C9A C10A S8 113.6(10) . . ?
C9A C10A H10C 108.9 . . ?
C9A C10A H10D 108.9 . . ?
H10C C10A H10D 107.7 . . ?
S1 C1A H1AA 107.7 . . ?
S1 C1A H1AB 107.7 . . ?
H1AA C1A H1AB 107.1 . . ?
C2A C1A S1 118.5(16) . . ?
C2A C1A H1AA 107.7 . . ?
C2A C1A H1AB 107.7 . . ?
S2 C2A H2AA 109.5 . . ?
S2 C2A H2AB 109.5 . . ?
C1A C2A S2 110.5(11) . . ?
C1A C2A H2AA 109.5 . . ?
C1A C2A H2AB 109.5 . . ?
H2AA C2A H2AB 108.1 . . ?
C25 C24 C25 120.2(14) 2_755 . ?
C25 C24 H24 119.9 2_755 . ?
C25 C24 H24 119.9 . . ?
F1 C24 C25 119.9(7) . . ?
F1 C24 C25 119.9(7) . 2_755 ?
H1WA O1W H1WB 119.1 . . ?
H1WA O1W H1WC 129.9 . . ?
H1WB O1W H1WC 107.9 . . ?

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
Ga1 O3 C21 C22 -6.2(5) . . . . ?
Ga1 O3 C21 O4 173.3(5) . . . . ?
Ga1 O5 C22 C21 1.6(6) . . . . ?
Ga1 O5 C22 O6 -178.2(5) . . . . ?
Ga1 O2 C23 C23 4.9(7) . . . 2_656 ?
Ga1 O2 C23 O1 -177.2(5) . . . . ?
S4 C4 C3 S3 0.6(6) . . . . ?
S4 C4 C3 S1 -177.3(3) . . . . ?
S6 C6 C5 S4 0.6(7) . . . . ?
S6 C6 C5 S3 -177.9(3) . . . . ?
S11 C15 C16 S14 179.9(3) . . . . ?
S11 C15 C16 S13 -1.1(6) . . . . ?
S5 C7 C8 S6 -1.3(6) . . . . ?
S5 C7 C8 S8 175.2(3) . . . . ?
S5 C6 C5 S4 179.0(3) . . . . ?
S5 C6 C5 S3 0.6(7) . . . . ?
S14 C18 C17 S13 -0.9(6) . . . . ?
S14 C18 C17 S15 -179.2(3) . . . . ?
S12 C14 C13 S11 1.0(6) . . . . ?
S12 C14 C13 S9 -178.5(3) . . . . ?
S12 C15 C16 S14 0.6(7) . . . . ?
S12 C15 C16 S13 179.6(3) . . . . ?
S1 C1 C2 S2 -71.7(12) . . . . ?
S1 C1A C2A S2 67(2) . . . . ?
S7 C7 C8 S6 -177.6(3) . . . . ?
S7 C7 C8 S8 -1.0(7) . . . . ?
S7 C9A C10A S8 -66.8(18) . . . . ?
S2 C4 C3 S3 -179.8(3) . . . . ?
S2 C4 C3 S1 2.3(8) . . . . ?
S10 C14 C13 S11 -179.4(3) . . . . ?
S10 C14 C13 S9 1.2(8) . . . . ?
S9 C11 C12 S10 -68.3(5) . . . . ?
S8 C10 C9 S7 57.4(17) . . . . ?
S16 C18 C17 S13 175.0(3) . . . . ?
S16 C18 C17 S15 -3.3(8) . . . . ?
S16 C20 C19 S15 69.9(6) . . . . ?
C14 S12 C15 S11 -0.4(3) . . . . ?
C14 S12 C15 C16 178.9(4) . . . . ?
C14 S10 C12 C11 44.6(5) . . . . ?
C7 S5 C6 S6 -5.4(3) . . . . ?
C7 S5 C6 C5 176.0(5) . . . . ?
C7 S7 C9 C10 -66.2(11) . . . . ?
C7 S7 C9A C10A 22.7(13) . . . . ?
C8 S6 C6 S5 4.9(3) . . . . ?
C8 S6 C6 C5 -176.5(4) . . . . ?
C8 S8 C10 C9 -13.1(15) . . . . ?
C8 S8 C10A C9A 68.7(14) . . . . ?
C18 S14 C16 S13 -0.2(3) . . . . ?
C18 S14 C16 C15 178.9(4) . . . . ?
C18 S16 C20 C19 -37.8(6) . . . . ?
C15 S11 C13 S9 178.4(3) . . . . ?
C15 S11 C13 C14 -1.1(4) . . . . ?
C15 S12 C14 S10 180.0(3) . . . . ?
C15 S12 C14 C13 -0.3(4) . . . . ?
C13 S11 C15 S12 0.9(3) . . . . ?
C13 S11 C15 C16 -178.5(4) . . . . ?
C13 S9 C11 C12 48.4(5) . . . . ?
C4 S4 C5 S3 -1.3(3) . . . . ?
C4 S4 C5 C6 -179.9(5) . . . . ?
C4 S2 C2 C1 55.0(10) . . . . ?
C4 S2 C2A C1A -32(2) . . . . ?
C6 S6 C8 S8 -179.1(3) . . . . ?
C6 S6 C8 C7 -2.1(5) . . . . ?
C6 S5 C7 S7 -179.3(3) . . . . ?
C6 S5 C7 C8 4.0(4) . . . . ?
C17 S13 C16 S14 -0.2(3) . . . . ?
C17 S13 C16 C15 -179.3(4) . . . . ?
C17 S15 C19 C20 -58.0(5) . . . . ?
C16 S14 C18 S16 -175.9(3) . . . . ?
C16 S14 C18 C17 0.6(4) . . . . ?
C16 S13 C17 S15 179.2(3) . . . . ?
C16 S13 C17 C18 0.6(4) . . . . ?
C3 S3 C5 S4 1.6(3) . . . . ?
C3 S3 C5 C6 -179.8(5) . . . . ?
C3 S1 C1 C2 43.1(9) . . . . ?
C3 S1 C1A C2A -58.1(16) . . . . ?
C5 S4 C4 S2 -179.2(3) . . . . ?
C5 S4 C4 C3 0.4(5) . . . . ?
C5 S3 C3 S1 176.9(3) . . . . ?
C5 S3 C3 C4 -1.3(5) . . . . ?
O5 C22 C21 O3 3.1(7) . . . . ?
O5 C22 C21 O4 -176.5(5) . . . . ?
C11 S9 C13 S11 165.2(3) . . . . ?
C11 S9 C13 C14 -15.3(5) . . . . ?
O6 C22 C21 O3 -177.0(5) . . . . ?
O6 C22 C21 O4 3.4(8) . . . . ?
C20 S16 C18 S14 -179.3(3) . . . . ?
C20 S16 C18 C17 4.7(6) . . . . ?
C1 S1 C3 S3 171.8(4) . . . . ?
C1 S1 C3 C4 -10.2(6) . . . . ?
C12 S10 C14 S12 167.8(3) . . . . ?
C12 S10 C14 C13 -11.8(6) . . . . ?
C2 S2 C4 S4 159.9(5) . . . . ?
C2 S2 C4 C3 -19.6(7) . . . . ?
C10 S8 C8 S6 159.7(6) . . . . ?
C10 S8 C8 C7 -16.9(8) . . . . ?
C9 S7 C7 S5 -137.9(5) . . . . ?
C9 S7 C7 C8 38.4(6) . . . . ?
C19 S15 C17 S13 -152.1(3) . . . . ?
C19 S15 C17 C18 26.2(6) . . . . ?
C27 C26 C25 C24 -17.8(4) . . . . ?
C26 C27 C26 C25 11.0(2) 2_755 . . . ?
C26 C27 C26 F2 160.5(13) 2_755 . . . ?
C26 C25 C24 C25 6.6(3) . . . 2_755 ?
C26 C25 C24 F1 -173.4(3) . . . . ?
C9A S7 C7 S5 -164.9(6) . . . . ?
C9A S7 C7 C8 11.4(8) . . . . ?
C10A S8 C8 S6 143.1(6) . . . . ?
C10A S8 C8 C7 -33.5(7) . . . . ?
C1A S1 C3 S3 -156.9(7) . . . . ?
C1A S1 C3 C4 21.0(8) . . . . ?
C2A S2 C4 S4 179.4(9) . . . . ?
C2A S2 C4 C3 -0.2(11) . . . . ?
F2 C26 C25 C24 -166.3(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 2163083'
loop_
_audit_author_name
_audit_author_address
'Toby Blundell'
;Nottingham Trent University
United Kingdom
;
_audit_update_record             
;
2022-03-29 deposited with the CCDC.	2022-04-25 downloaded from the CCDC.
;
_audit_creation_date             2022-03-16
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ga O12, C6 H5 Cl, 4(C10 H8 S8), 0.5(H6 O2)'
_chemical_formula_sum            'C52 H40 Cl Ga O13 S32'
_chemical_formula_weight         2003.93
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   10.2964(7)
_cell_length_b                   19.9923(14)
_cell_length_c                   35.4235(25)
_cell_angle_alpha                90
_cell_angle_beta                 93.0804(31)
_cell_angle_gamma                90
_cell_volume                     7281.3
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4717
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      29.0441
_cell_measurement_theta_min      2.1172
_shelx_estimated_absorpt_T_max   0.934
_shelx_estimated_absorpt_T_min   0.768
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  0.9585
_exptl_absorpt_correction_T_min  0.7873
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.1370
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21117
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.193
_diffrn_reflns_theta_min         2.274
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device_type  'AFC10: Fixed Chi 2 circle'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4946
_reflns_number_total             9327
_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_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         9327
_refine_ls_number_restraints     375
_refine_ls_R_factor_all          0.1483
_refine_ls_R_factor_gt           0.0745
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.198
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0251P)²+11.3723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1447
_refine_special_details          
'Positional disorder was found for 2 terminal ethyl groups on the BEDT-TTF molecule (C1, C2 and C9 C10). The disorder was modelled, and the occupancy of the major and minor components competitively refined to 69:31 (C1, C2) and 32:68 (C9, C10) respectively. Relevant 1,2- bond distances were restrained to be approximately equal. Oxygen-hydrogen 1,2- distances for O1W were restrained to be aproximatley equal. Enhanced rigid bond restraints were applied to all atoms.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O7-H7C = O7-H7B = O7-H7A
 0.83 with sigma of 0.02
 S7-C9 \\sim S7-C9A \\sim S8-C10 \\sim S8-C10A
 with sigma of 0.02
 C2-C1 \\sim C2A-C1A
 with sigma of 0.02
 S2-C2A \\sim S2-C2 \\sim S1-C1A \\sim S1-C1
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(2)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(2)
 Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5)
5.a Free rotating group:
 O7(H7A,H7B,H7C)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C1A(H1AA,H1AB),
 C2A(H2AA,H2AB), C9A(H9AA,H9AB), C10A(H10C,H10D), C11(H11A,H11B), C12(H12A,
 H12B), C19(H19A,H19B), C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Ga1 Ga 0.000000 0.41792(4) 0.750000 0.0365(2) Uani 1 2 d S T P . .
O1 O -0.0844(4) 0.2319(2) 0.71826(13) 0.0643(13) Uani 1 1 d . . . . .
O2 O -0.0743(4) 0.34347(18) 0.71921(10) 0.0467(10) Uani 1 1 d . . . . .
O3 O 0.1482(3) 0.42968(18) 0.71757(10) 0.0435(9) Uani 1 1 d . . . . .
O4 O 0.3204(4) 0.4970(2) 0.71219(11) 0.0590(12) Uani 1 1 d . . . . .
O5 O 0.0972(3) 0.48302(17) 0.78240(10) 0.0399(9) Uani 1 1 d . . . . .
O6 O 0.2777(4) 0.5446(2) 0.78403(11) 0.0562(11) Uani 1 1 d . . . . .
C21 C -0.0460(5) 0.2851(3) 0.73203(16) 0.0449(14) Uani 1 1 d . . . . .
C22 C 0.2291(6) 0.4754(3) 0.72922(15) 0.0422(13) Uani 1 1 d . . . . .
C23 C 0.2012(5) 0.5040(3) 0.76855(15) 0.0403(12) Uani 1 1 d . . . . .
Cl1 Cl 0.500000 0.85127(14) 0.250000 0.1002(11) Uani 1 2 d S T P . .
C24 C 0.500000 0.7642(5) 0.250000 0.060(2) Uani 1 2 d S T P . .
C25 C 0.4047(6) 0.7311(4) 0.26813(18) 0.0652(18) Uani 1 1 d . . . . .
H25 H 0.340440 0.754616 0.279962 0.078 Uiso 1 1 calc R U . . .
C26 C 0.4062(7) 0.6615(4) 0.2685(2) 0.087(3) Uani 1 1 d . . . . .
H26 H 0.343783 0.638195 0.281163 0.104 Uiso 1 1 calc R U . . .
C27 C 0.500000 0.6269(6) 0.250000 0.099(4) Uani 1 2 d S T P . .
H27 H 0.499996 0.580384 0.249999 0.119 Uiso 1 2 calc R U P . .
S1 S 0.32571(14) 0.48343(8) 0.37934(4) 0.0494(4) Uani 1 1 d D . . . .
S2 S 0.60601(15) 0.57145(9) 0.41006(4) 0.0586(5) Uani 1 1 d D . . . .
S3 S 0.24030(13) 0.51209(7) 0.45610(4) 0.0402(3) Uani 1 1 d . . . . .
S4 S 0.47403(13) 0.58853(8) 0.48047(4) 0.0432(4) Uani 1 1 d . . . . .
S5 S 0.11746(13) 0.54255(7) 0.53666(4) 0.0396(3) Uani 1 1 d . . . . .
S6 S 0.35360(13) 0.61752(8) 0.56055(4) 0.0424(4) Uani 1 1 d . . . . .
S7 S -0.01852(14) 0.57208(7) 0.60616(4) 0.0449(4) Uani 1 1 d D . . . .
S8 S 0.25832(16) 0.65708(8) 0.63477(4) 0.0534(4) Uani 1 1 d D . . . .
C3 C 0.3618(5) 0.5200(3) 0.42349(14) 0.0360(12) Uani 1 1 d . . . . .
C4 C 0.4691(5) 0.5551(3) 0.43497(14) 0.0370(12) Uani 1 1 d . . . . .
C5 C 0.3210(5) 0.5600(2) 0.49131(14) 0.0345(12) Uani 1 1 d . . . . .
C6 C 0.2689(5) 0.5721(2) 0.52510(14) 0.0330(11) Uani 1 1 d . . . . .
C7 C 0.1181(5) 0.5832(2) 0.58008(14) 0.0337(11) Uani 1 1 d . . . . .
C8 C 0.2266(5) 0.6168(3) 0.59150(14) 0.0365(12) Uani 1 1 d . . . . .
C1 C 0.4769(8) 0.4869(5) 0.3576(3) 0.048(3) Uani 0.691(14) 1 d D . P A 1
H1A H 0.534343 0.452857 0.368667 0.057 Uiso 0.691(14) 1 calc R U P A 1
H1B H 0.462959 0.477112 0.330896 0.057 Uiso 0.691(14) 1 calc R U P A 1
C2 C 0.5417(12) 0.5550(5) 0.3624(3) 0.053(3) Uani 0.691(14) 1 d D . P A 1
H2A H 0.478735 0.589439 0.355160 0.063 Uiso 0.691(14) 1 calc R U P A 1
H2B H 0.612037 0.557952 0.345298 0.063 Uiso 0.691(14) 1 calc R U P A 1
C9 C 0.0194(18) 0.5973(13) 0.6537(4) 0.047(6) Uani 0.320(19) 1 d D . P B 1
H9A H -0.015185 0.641634 0.657937 0.056 Uiso 0.320(19) 1 calc R U P B 1
H9B H -0.019380 0.566519 0.671011 0.056 Uiso 0.320(19) 1 calc R U P B 1
C10 C 0.1652(19) 0.5977(12) 0.6606(8) 0.050(8) Uani 0.320(19) 1 d D . P B 1
H10A H 0.196941 0.553285 0.655070 0.060 Uiso 0.320(19) 1 calc R U P B 1
H10B H 0.184094 0.605556 0.687382 0.060 Uiso 0.320(19) 1 calc R U P B 1
C1A C 0.4367(15) 0.5328(11) 0.3528(5) 0.046(6) Uani 0.309(14) 1 d D . P A 2
H1AA H 0.428980 0.518269 0.326624 0.056 Uiso 0.309(14) 1 calc R U P A 2
H1AB H 0.408666 0.579089 0.353388 0.056 Uiso 0.309(14) 1 calc R U P A 2
C2A C 0.5801(18) 0.5300(13) 0.3661(6) 0.046(7) Uani 0.309(14) 1 d D . P A 2
H2AA H 0.632101 0.551070 0.347383 0.056 Uiso 0.309(14) 1 calc R U P A 2
H2AB H 0.607334 0.483716 0.368642 0.056 Uiso 0.309(14) 1 calc R U P A 2
C9A C 0.0712(12) 0.5631(6) 0.6520(2) 0.050(3) Uani 0.680(19) 1 d D . P B 2
H9AA H 0.010213 0.550278 0.670664 0.060 Uiso 0.680(19) 1 calc R U P B 2
H9AB H 0.133184 0.526908 0.650183 0.060 Uiso 0.680(19) 1 calc R U P B 2
C10A C 0.1430(14) 0.6243(7) 0.6660(4) 0.059(4) Uani 0.680(19) 1 d D . P B 2
H10C H 0.188436 0.613691 0.689998 0.071 Uiso 0.680(19) 1 calc R U P B 2
H10D H 0.080042 0.658987 0.670772 0.071 Uiso 0.680(19) 1 calc R U P B 2
S9 S -0.08974(14) 0.61113(8) 0.39174(4) 0.0453(4) Uani 1 1 d . . . . .
S10 S 0.20227(14) 0.69346(8) 0.42015(4) 0.0491(4) Uani 1 1 d . . . . .
S11 S -0.16504(13) 0.64340(7) 0.46872(4) 0.0401(3) Uani 1 1 d . . . . .
S12 S 0.07677(13) 0.71411(7) 0.49143(4) 0.0429(4) Uani 1 1 d . . . . .
S13 S -0.27880(13) 0.67398(7) 0.54946(4) 0.0418(4) Uani 1 1 d . . . . .
S14 S -0.03958(14) 0.74568(7) 0.57302(4) 0.0435(4) Uani 1 1 d . . . . .
S15 S -0.40527(16) 0.69288(8) 0.62122(5) 0.0538(4) Uani 1 1 d . . . . .
S16 S -0.11369(18) 0.77350(9) 0.65002(4) 0.0610(5) Uani 1 1 d . . . . .
C11 C 0.0648(5) 0.6059(3) 0.37078(15) 0.0431(13) Uani 1 1 d . . . . .
H11A H 0.115444 0.570637 0.383306 0.052 Uiso 1 1 calc R U . . .
H11B H 0.050420 0.593335 0.344443 0.052 Uiso 1 1 calc R U . . .
C12 C 0.1438(6) 0.6702(3) 0.37286(16) 0.0491(15) Uani 1 1 d . . . . .
H12A H 0.090531 0.706304 0.362264 0.059 Uiso 1 1 calc R U . . .
H12B H 0.217900 0.665201 0.357297 0.059 Uiso 1 1 calc R U . . .
C13 C -0.0463(5) 0.6480(3) 0.43537(14) 0.0356(12) Uani 1 1 d . . . . .
C14 C 0.0654(5) 0.6800(3) 0.44582(14) 0.0354(12) Uani 1 1 d . . . . .
C15 C -0.0770(5) 0.6880(2) 0.50373(14) 0.0326(11) Uani 1 1 d . . . . .
C16 C -0.1260(5) 0.7007(2) 0.53782(14) 0.0345(12) Uani 1 1 d . . . . .
C17 C -0.2703(5) 0.7072(3) 0.59481(15) 0.0393(13) Uani 1 1 d . . . . .
C18 C -0.1594(5) 0.7398(3) 0.60589(14) 0.0386(13) Uani 1 1 d . . . . .
C19 C -0.3293(7) 0.6964(3) 0.66753(19) 0.073(2) Uani 1 1 d . . . . .
H19A H -0.394899 0.690072 0.685868 0.087 Uiso 1 1 calc R U . . .
H19B H -0.267469 0.659943 0.670542 0.087 Uiso 1 1 calc R U . . .
C20 C -0.2591(7) 0.7620(4) 0.67582(17) 0.0679(19) Uani 1 1 d . . . . .
H20A H -0.235664 0.764251 0.702681 0.082 Uiso 1 1 calc R U . . .
H20B H -0.318451 0.798583 0.669753 0.082 Uiso 1 1 calc R U . . .
O7 O 0.500000 0.5980(4) 0.750000 0.096(2) Uani 1 2 d DGS T P . .
H7A H 0.575791 0.581658 0.748825 0.115 Uiso 0.5 1 d DG U P C -1
H7B H 0.512928 0.639002 0.755592 0.115 Uiso 0.5 1 d DG U P D -1
H7C H 0.437737 0.573309 0.758036 0.115 Uiso 0.5 1 d DG U P E -1


_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
Ga1 O2 1.975(4) . ?
Ga1 O2 1.975(4) 2_556 ?
Ga1 O3 1.973(3) . ?
Ga1 O3 1.973(3) 2_556 ?
Ga1 O5 1.972(3) 2_556 ?
Ga1 O5 1.972(4) . ?
O1 C21 1.227(6) . ?
O2 C21 1.280(6) . ?
O3 C22 1.289(6) . ?
O4 C22 1.222(6) . ?
O5 C23 1.272(6) . ?
O6 C23 1.239(6) . ?
C21 C21 1.546(11) 2_556 ?
C22 C23 1.547(7) . ?
Cl1 C24 1.740(9) . ?
C24 C25 1.372(7) 2_655 ?
C24 C25 1.372(7) . ?
C25 H25 0.9300 . ?
C25 C26 1.391(9) . ?
C26 H26 0.9300 . ?
C26 C27 1.380(9) . ?
C27 H27 0.9300 . ?
S1 C3 1.748(5) . ?
S1 C1 1.774(7) . ?
S1 C1A 1.811(13) . ?
S2 C4 1.734(5) . ?
S2 C2 1.811(9) . ?
S2 C2A 1.772(13) . ?
S3 C3 1.755(5) . ?
S3 C5 1.746(5) . ?
S4 C4 1.743(5) . ?
S4 C5 1.739(5) . ?
S5 C6 1.737(5) . ?
S5 C7 1.739(5) . ?
S6 C6 1.745(5) . ?
S6 C8 1.751(5) . ?
S7 C7 1.738(5) . ?
S7 C9 1.781(12) . ?
S7 C9A 1.833(8) . ?
S8 C8 1.747(5) . ?
S8 C10 1.806(14) . ?
S8 C10A 1.791(9) . ?
C3 C4 1.352(7) . ?
C5 C6 1.360(7) . ?
C7 C8 1.348(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.523(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.508(17) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C1A C2A 1.526(16) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C10A 1.501(12) . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
S9 C11 1.795(5) . ?
S9 C13 1.749(5) . ?
S10 C12 1.810(6) . ?
S10 C14 1.739(5) . ?
S11 C13 1.748(5) . ?
S11 C15 1.742(5) . ?
S12 C14 1.752(5) . ?
S12 C15 1.744(5) . ?
S13 C16 1.732(5) . ?
S13 C17 1.736(5) . ?
S14 C16 1.742(5) . ?
S14 C18 1.745(5) . ?
S15 C17 1.740(6) . ?
S15 C19 1.781(7) . ?
S16 C18 1.744(5) . ?
S16 C20 1.810(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.521(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.350(7) . ?
C15 C16 1.357(7) . ?
C17 C18 1.354(7) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.518(9) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
O7 H7A 0.8493 . ?
O7 H7B 0.8516 . ?
O7 H7C 0.8693 . ?

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
O2 Ga1 O2 82.2(2) . 2_556 ?
O3 Ga1 O2 97.05(15) . 2_556 ?
O3 Ga1 O2 93.26(16) 2_556 2_556 ?
O3 Ga1 O2 93.27(16) . . ?
O3 Ga1 O2 97.05(16) 2_556 . ?
O3 Ga1 O3 166.3(2) . 2_556 ?
O5 Ga1 O2 90.38(15) 2_556 . ?
O5 Ga1 O2 171.16(16) . . ?
O5 Ga1 O2 90.38(15) . 2_556 ?
O5 Ga1 O2 171.16(16) 2_556 2_556 ?
O5 Ga1 O3 88.09(14) . 2_556 ?
O5 Ga1 O3 88.09(14) 2_556 . ?
O5 Ga1 O3 82.88(15) 2_556 2_556 ?
O5 Ga1 O3 82.88(15) . . ?
O5 Ga1 O5 97.4(2) 2_556 . ?
C21 O2 Ga1 114.7(4) . . ?
C22 O3 Ga1 113.9(3) . . ?
C23 O5 Ga1 113.8(3) . . ?
O1 C21 O2 126.0(6) . . ?
O1 C21 C21 119.8(4) . 2_556 ?
O2 C21 C21 114.2(3) . 2_556 ?
O3 C22 C23 113.7(5) . . ?
O4 C22 O3 126.3(5) . . ?
O4 C22 C23 119.9(5) . . ?
O5 C23 C22 115.3(5) . . ?
O6 C23 O5 125.0(5) . . ?
O6 C23 C22 119.7(5) . . ?
C25 C24 Cl1 118.9(5) . . ?
C25 C24 Cl1 118.9(5) 2_655 . ?
C25 C24 C25 122.2(10) 2_655 . ?
C24 C25 H25 120.7 . . ?
C24 C25 C26 118.6(8) . . ?
C26 C25 H25 120.7 . . ?
C25 C26 H26 119.8 . . ?
C27 C26 C25 120.4(9) . . ?
C27 C26 H26 119.8 . . ?
C26 C27 C26 119.8(11) 2_655 . ?
C26 C27 H27 120.1 2_655 . ?
C26 C27 H27 120.1 . . ?
C3 S1 C1 102.8(3) . . ?
C3 S1 C1A 97.3(6) . . ?
C4 S2 C2 100.0(4) . . ?
C4 S2 C2A 105.7(8) . . ?
C5 S3 C3 95.3(2) . . ?
C5 S4 C4 95.5(2) . . ?
C6 S5 C7 95.1(2) . . ?
C6 S6 C8 94.9(2) . . ?
C7 S7 C9 108.9(6) . . ?
C7 S7 C9A 95.7(4) . . ?
C8 S8 C10 93.6(11) . . ?
C8 S8 C10A 106.0(4) . . ?
S1 C3 S3 115.2(3) . . ?
C4 C3 S1 128.1(4) . . ?
C4 C3 S3 116.6(4) . . ?
S2 C4 S4 114.5(3) . . ?
C3 C4 S2 128.1(4) . . ?
C3 C4 S4 117.4(4) . . ?
S4 C5 S3 115.1(3) . . ?
C6 C5 S3 122.1(4) . . ?
C6 C5 S4 122.7(4) . . ?
S5 C6 S6 115.3(3) . . ?
C5 C6 S5 123.2(4) . . ?
C5 C6 S6 121.4(4) . . ?
S7 C7 S5 116.5(3) . . ?
C8 C7 S5 117.6(4) . . ?
C8 C7 S7 125.8(4) . . ?
S8 C8 S6 115.8(3) . . ?
C7 C8 S6 116.8(4) . . ?
C7 C8 S8 127.3(4) . . ?
S1 C1 H1A 109.2 . . ?
S1 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C2 C1 S1 112.1(8) . . ?
C2 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
S2 C2 H2A 108.8 . . ?
S2 C2 H2B 108.8 . . ?
C1 C2 S2 113.7(7) . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
S7 C9 H9A 109.9 . . ?
S7 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 S7 108.7(18) . . ?
C10 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
S8 C10 H10A 107.8 . . ?
S8 C10 H10B 107.8 . . ?
C9 C10 S8 118.2(15) . . ?
C9 C10 H10A 107.8 . . ?
C9 C10 H10B 107.8 . . ?
H10A C10 H10B 107.1 . . ?
S1 C1A H1AA 108.2 . . ?
S1 C1A H1AB 108.2 . . ?
H1AA C1A H1AB 107.3 . . ?
C2A C1A S1 116.5(17) . . ?
C2A C1A H1AA 108.2 . . ?
C2A C1A H1AB 108.2 . . ?
S2 C2A H2AA 109.5 . . ?
S2 C2A H2AB 109.5 . . ?
C1A C2A S2 110.6(13) . . ?
C1A C2A H2AA 109.5 . . ?
C1A C2A H2AB 109.5 . . ?
H2AA C2A H2AB 108.1 . . ?
S7 C9A H9AA 108.4 . . ?
S7 C9A H9AB 108.4 . . ?
H9AA C9A H9AB 107.5 . . ?
C10A C9A S7 115.5(10) . . ?
C10A C9A H9AA 108.4 . . ?
C10A C9A H9AB 108.4 . . ?
S8 C10A H10C 108.5 . . ?
S8 C10A H10D 108.5 . . ?
C9A C10A S8 115.1(8) . . ?
C9A C10A H10C 108.5 . . ?
C9A C10A H10D 108.5 . . ?
H10C C10A H10D 107.5 . . ?
C13 S9 C11 101.5(3) . . ?
C14 S10 C12 101.9(3) . . ?
C15 S11 C13 95.6(2) . . ?
C15 S12 C14 95.6(2) . . ?
C16 S13 C17 95.8(3) . . ?
C16 S14 C18 95.2(2) . . ?
C17 S15 C19 99.5(3) . . ?
C18 S16 C20 102.3(3) . . ?
S9 C11 H11A 108.6 . . ?
S9 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 S9 114.5(4) . . ?
C12 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
S10 C12 H12A 108.7 . . ?
S10 C12 H12B 108.7 . . ?
C11 C12 S10 114.4(4) . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
S11 C13 S9 114.9(3) . . ?
C14 C13 S9 128.0(4) . . ?
C14 C13 S11 117.1(4) . . ?
S10 C14 S12 113.9(3) . . ?
C13 C14 S10 129.2(4) . . ?
C13 C14 S12 116.8(4) . . ?
S11 C15 S12 114.8(3) . . ?
C16 C15 S11 121.7(4) . . ?
C16 C15 S12 123.5(4) . . ?
S13 C16 S14 115.1(3) . . ?
C15 C16 S13 122.7(4) . . ?
C15 C16 S14 122.2(4) . . ?
S13 C17 S15 115.6(3) . . ?
C18 C17 S13 116.9(4) . . ?
C18 C17 S15 127.5(4) . . ?
S16 C18 S14 113.9(3) . . ?
C17 C18 S14 117.0(4) . . ?
C17 C18 S16 129.0(4) . . ?
S15 C19 H19A 108.9 . . ?
S15 C19 H19B 108.9 . . ?
H19A C19 H19B 107.8 . . ?
C20 C19 S15 113.2(4) . . ?
C20 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
S16 C20 H20A 108.7 . . ?
S16 C20 H20B 108.7 . . ?
C19 C20 S16 114.2(5) . . ?
C19 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
H7A O7 H7B 104.4 . . ?
H7A O7 H7C 119.5 . . ?
H7B O7 H7C 125.4 . . ?

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
Ga1 O2 C21 O1 177.7(5) . . . . ?
Ga1 O2 C21 C21 -2.8(8) . . . 2_556 ?
Ga1 O3 C22 O4 -171.8(5) . . . . ?
Ga1 O3 C22 C23 7.6(6) . . . . ?
Ga1 O5 C23 O6 -179.5(4) . . . . ?
Ga1 O5 C23 C22 1.0(6) . . . . ?
O3 C22 C23 O5 -5.8(7) . . . . ?
O3 C22 C23 O6 174.6(5) . . . . ?
O4 C22 C23 O5 173.6(5) . . . . ?
O4 C22 C23 O6 -6.0(8) . . . . ?
Cl1 C24 C25 C26 -179.2(4) . . . . ?
C24 C25 C26 C27 -1.7(9) . . . . ?
C25 C24 C25 C26 0.8(4) 2_655 . . . ?
C25 C26 C27 C26 0.9(5) . . . 2_655 ?
S1 C3 C4 S2 -3.0(8) . . . . ?
S1 C3 C4 S4 177.4(3) . . . . ?
S1 C1 C2 S2 71.9(11) . . . . ?
S1 C1A C2A S2 -70(2) . . . . ?
S3 C3 C4 S2 179.4(3) . . . . ?
S3 C3 C4 S4 -0.2(6) . . . . ?
S3 C5 C6 S5 -0.7(7) . . . . ?
S3 C5 C6 S6 177.6(3) . . . . ?
S4 C5 C6 S5 -178.7(3) . . . . ?
S4 C5 C6 S6 -0.4(6) . . . . ?
S5 C7 C8 S6 1.5(6) . . . . ?
S5 C7 C8 S8 -175.4(3) . . . . ?
S7 C7 C8 S6 177.3(3) . . . . ?
S7 C7 C8 S8 0.4(8) . . . . ?
S7 C9 C10 S8 65(3) . . . . ?
S7 C9A C10A S8 -56.8(19) . . . . ?
C3 S1 C1 C2 -46.0(8) . . . . ?
C3 S1 C1A C2A 57.8(16) . . . . ?
C3 S3 C5 S4 -2.4(3) . . . . ?
C3 S3 C5 C6 179.4(4) . . . . ?
C4 S2 C2 C1 -52.7(9) . . . . ?
C4 S2 C2A C1A 36(2) . . . . ?
C4 S4 C5 S3 2.3(3) . . . . ?
C4 S4 C5 C6 -179.5(5) . . . . ?
C5 S3 C3 S1 -176.3(3) . . . . ?
C5 S3 C3 C4 1.6(5) . . . . ?
C5 S4 C4 S2 179.0(3) . . . . ?
C5 S4 C4 C3 -1.3(5) . . . . ?
C6 S5 C7 S7 179.4(3) . . . . ?
C6 S5 C7 C8 -4.5(5) . . . . ?
C6 S6 C8 S8 179.5(3) . . . . ?
C6 S6 C8 C7 2.3(5) . . . . ?
C7 S5 C6 S6 5.9(3) . . . . ?
C7 S5 C6 C5 -175.7(4) . . . . ?
C7 S7 C9 C10 -19(2) . . . . ?
C7 S7 C9A C10A 65.7(12) . . . . ?
C8 S6 C6 S5 -5.3(3) . . . . ?
C8 S6 C6 C5 176.3(4) . . . . ?
C8 S8 C10 C9 -69(3) . . . . ?
C8 S8 C10A C9A 12.7(16) . . . . ?
C1 S1 C3 S3 -169.5(4) . . . . ?
C1 S1 C3 C4 12.9(7) . . . . ?
C2 S2 C4 S4 -161.7(4) . . . . ?
C2 S2 C4 C3 18.6(7) . . . . ?
C9 S7 C7 S5 164.1(10) . . . . ?
C9 S7 C7 C8 -11.7(11) . . . . ?
C10 S8 C8 S6 -144.3(8) . . . . ?
C10 S8 C8 C7 32.6(9) . . . . ?
C1A S1 C3 S3 157.5(7) . . . . ?
C1A S1 C3 C4 -20.2(8) . . . . ?
C2A S2 C4 S4 177.8(9) . . . . ?
C2A S2 C4 C3 -1.9(10) . . . . ?
C9A S7 C7 S5 138.9(5) . . . . ?
C9A S7 C7 C8 -36.9(6) . . . . ?
C10A S8 C8 S6 -159.8(7) . . . . ?
C10A S8 C8 C7 17.1(8) . . . . ?
S9 C11 C12 S10 68.0(5) . . . . ?
S9 C13 C14 S10 -1.4(8) . . . . ?
S9 C13 C14 S12 177.9(3) . . . . ?
S11 C13 C14 S10 179.8(3) . . . . ?
S11 C13 C14 S12 -0.9(6) . . . . ?
S11 C15 C16 S13 0.0(6) . . . . ?
S11 C15 C16 S14 -179.6(3) . . . . ?
S12 C15 C16 S13 -179.7(3) . . . . ?
S12 C15 C16 S14 0.6(7) . . . . ?
S13 C17 C18 S14 1.0(6) . . . . ?
S13 C17 C18 S16 -174.9(3) . . . . ?
S15 C17 C18 S14 179.5(3) . . . . ?
S15 C17 C18 S16 3.5(8) . . . . ?
S15 C19 C20 S16 -69.9(6) . . . . ?
C11 S9 C13 S11 -165.4(3) . . . . ?
C11 S9 C13 C14 15.7(6) . . . . ?
C12 S10 C14 S12 -167.3(3) . . . . ?
C12 S10 C14 C13 12.0(6) . . . . ?
C13 S9 C11 C12 -48.3(5) . . . . ?
C13 S11 C15 S12 -0.7(3) . . . . ?
C13 S11 C15 C16 179.5(4) . . . . ?
C14 S10 C12 C11 -44.4(5) . . . . ?
C14 S12 C15 S11 0.4(3) . . . . ?
C14 S12 C15 C16 -179.9(5) . . . . ?
C15 S11 C13 S9 -178.0(3) . . . . ?
C15 S11 C13 C14 1.0(5) . . . . ?
C15 S12 C14 S10 179.7(3) . . . . ?
C15 S12 C14 C13 0.3(4) . . . . ?
C16 S13 C17 S15 -178.9(3) . . . . ?
C16 S13 C17 C18 -0.2(5) . . . . ?
C16 S14 C18 S16 175.3(3) . . . . ?
C16 S14 C18 C17 -1.2(5) . . . . ?
C17 S13 C16 S14 -0.6(3) . . . . ?
C17 S13 C16 C15 179.7(5) . . . . ?
C17 S15 C19 C20 57.4(5) . . . . ?
C18 S14 C16 S13 1.0(3) . . . . ?
C18 S14 C16 C15 -179.3(5) . . . . ?
C18 S16 C20 C19 38.5(5) . . . . ?
C19 S15 C17 S13 153.3(3) . . . . ?
C19 S15 C17 C18 -25.2(6) . . . . ?
C20 S16 C18 S14 178.0(3) . . . . ?
C20 S16 C18 C17 -5.9(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT080_shelxl              
;
PROBLEM: Maximum Shift/Error ............................       0.20 Why ? 
RESPONSE: Due to solvent hydronium ion on special position
;
_vrf_SHFSU01_shelxl              
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.10
RESPONSE: Due to solvent hydronium ion on special position
;
####################################################################### 
# 
# 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_ekr_4_03_b_ir0601
_database_code_depnum_ccdc_archive 'CCDC 2163086'
loop_
_audit_author_name
_audit_author_address
'Toby Blundell'
;Nottingham Trent University
United Kingdom
;
_audit_update_record             
;
2022-03-29 deposited with the CCDC.	2022-04-25 downloaded from the CCDC.
;
_audit_creation_date             2022-03-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ir O12, 4(C10 H8 S8), 0.5(H6 O2), C7 H5 N'
_chemical_formula_sum            'C53 H40 Ir N O13 S32'
_chemical_formula_weight         2116.98
_chemical_melting_point          ?
_chemical_oxdiff_formula         C53H38IrNO13S32
_chemical_oxdiff_usercomment     'Ir C2O4 Benzonitrile block'
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'
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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   10.38140(14)
_cell_length_b                   19.6057(3)
_cell_length_c                   35.5790(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7241.56(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13083
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.8480
_cell_measurement_theta_min      3.7620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.724
_exptl_absorpt_correction_T_max  0.446
_exptl_absorpt_correction_T_min  0.252
_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 black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4232
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 8 3 0.0426
0 0 23 0.0904
-6 -7 0 0.0445
-6 6 2 0.0452
5 -8 0 0.0546
3 -2 -20 0.0521
0 13 3 0.0374
0 -13 -2 0.0636
0 1 -23 0.0628
-4 5 17 0.0781

_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.093
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
5.3755 7.5357 2.6062 0.9583 0.2842 -0.0294
0.4521 0.0750 23.0405 -0.0562 0.7112 -0.7007
-5.7462 -6.6416 -0.3898 -0.9538 -0.2828 -0.1015
-5.8861 6.1403 1.7377 -0.2398 -0.6776 -0.6953
5.4104 -7.5952 0.4356 0.0985 0.7502 0.6538
3.4882 -1.6494 -19.5395 0.3418 -0.2094 0.9162
0.0469 12.6032 3.1612 0.7175 -0.3420 -0.6068
-0.2727 -12.6613 -2.0518 -0.7485 0.3567 0.5591
-0.3204 1.1038 -22.9769 0.1371 -0.7389 0.6597
-3.8340 4.8987 16.8034 -0.1761 -0.0140 -0.9843

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            30911
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.969
_diffrn_reflns_theta_min         4.511
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -103.00  36.00   1.00   10.00    --  -33.50   0.00 -90.00  139
  2  ω    -33.00 106.00   1.00   10.00    --   36.58   0.00  30.00  139
  3  ω    -31.00  53.00   1.00   10.00    --   36.58 -57.00 -30.00   84
  4  ω     22.00  77.00   1.00   10.00    --   36.58-125.00   0.00   55
  5  ω    -18.00  61.00   1.00   10.00    --   36.58 -77.00-150.00   79
  6  ω    112.00 139.00   1.00   40.00    --  108.00 -15.00-120.00   27
  7  ω     64.00 125.00   1.00   40.00    --  108.00 -61.00 -60.00   61
  8  ω    131.00 176.00   1.00   40.00    --  108.00  77.00   0.00   45
  9  ω     40.00 103.00   1.00   40.00    --  108.00 -94.00 -90.00   63
 10  ω    101.00 165.00   1.00   40.00    --  108.00  77.00 -30.00   64
 11  ω     48.00  74.00   1.00   40.00    --  108.00 -15.00-120.00   26
 12  ω    102.00 169.00   1.00   40.00    --  108.00  77.00 -90.00   67
 13  ω    101.00 159.00   1.00   40.00    --  108.00  77.00  30.00   58
 14  ω     73.00 125.00   1.00   40.00    --  108.00 -45.00-120.00   52
 15  ω     59.00 108.00   1.00   40.00    --  108.00-111.00 150.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0995935000
_diffrn_orient_matrix_UB_12      0.0577122000
_diffrn_orient_matrix_UB_13      -0.0045828000
_diffrn_orient_matrix_UB_21      0.0874533000
_diffrn_orient_matrix_UB_22      -0.0347983000
_diffrn_orient_matrix_UB_23      0.0292662000
_diffrn_orient_matrix_UB_31      0.0665759000
_diffrn_orient_matrix_UB_32      -0.0404710000
_diffrn_orient_matrix_UB_33      -0.0315862000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6344
_reflns_number_total             7048
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.627
_refine_diff_density_min         -1.917
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         7048
_refine_ls_number_restraints     345
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0455
_refine_ls_restrained_S_all      1.075
_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)+(0.0480P)²+36.3402P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1201
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O7-H7C = O7-H7A = O7-H7B
 0.83 with sigma of 0.02
 O7-H7C_$1 \\sim O7-H7B_$1 \\sim O7-H7A_$1
 with sigma of 0.01
 H7A-H7B \\sim H7B-H7C \\sim H7A-H7C
 with sigma of 0.01
3. Restrained planarity
 O7, H7A_$1, H7B_$1, H7C_$1
 with sigma of 0.001
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5) N1(0.5) H25(0.5) C28(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C19(H19A,H19B), C20(H20A,H20B)
6.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C26(H26), C27(H27)
;
_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
Ir1 Ir 0.000000 0.69425(2) 0.250000 0.03183(11) Uani 1 2 d S T P . .
O1 O -0.0698(4) 0.6159(2) 0.21840(11) 0.0364(8) Uani 1 1 d . . . . .
O2 O -0.0681(6) 0.5037(2) 0.21605(14) 0.0644(15) Uani 1 1 d . . . . .
O3 O 0.1755(4) 0.69699(19) 0.22253(11) 0.0368(9) Uani 1 1 d . . . . .
O4 O 0.3492(4) 0.7591(2) 0.22258(13) 0.0517(11) Uani 1 1 d . . . . .
O5 O 0.0772(4) 0.7728(2) 0.28139(11) 0.0368(9) Uani 1 1 d . . . . .
O6 O 0.2443(5) 0.8412(3) 0.27684(14) 0.0591(13) Uani 1 1 d . . . . .
C21 C -0.0410(6) 0.5570(3) 0.23131(17) 0.0397(13) Uani 1 1 d . . . . .
C22 C 0.2412(6) 0.7456(3) 0.23447(16) 0.0366(11) Uani 1 1 d . . . . .
C23 C 0.1828(6) 0.7913(3) 0.26638(16) 0.0352(11) Uani 1 1 d . . . . .
S1 S 0.22008(12) 0.87896(8) 0.60805(4) 0.0345(3) Uani 1 1 d . . . . .
S2 S 0.48144(12) 0.97328(7) 0.58896(4) 0.0333(3) Uani 1 1 d . . . . .
S3 S 0.27880(12) 0.80418(6) 0.53784(4) 0.0281(3) Uani 1 1 d . . . . .
S4 S 0.50904(11) 0.88684(7) 0.51968(4) 0.0280(3) Uani 1 1 d . . . . .
S5 S 0.28928(12) 0.73270(6) 0.45774(4) 0.0292(3) Uani 1 1 d . . . . .
S6 S 0.51797(11) 0.81366(7) 0.43644(4) 0.0272(3) Uani 1 1 d . . . . .
S7 S 0.24782(12) 0.67287(7) 0.38306(4) 0.0314(3) Uani 1 1 d . . . . .
S8 S 0.51075(12) 0.77671(7) 0.35613(4) 0.0318(3) Uani 1 1 d . . . . .
C1 C 0.3217(6) 0.9154(3) 0.64416(15) 0.0377(12) Uani 1 1 d . . . . .
H1A H 0.284183 0.959592 0.651943 0.045 Uiso 1 1 calc R U . . .
H1B H 0.319815 0.884805 0.666301 0.045 Uiso 1 1 calc R U . . .
C2 C 0.4600(6) 0.9269(4) 0.63325(17) 0.0429(14) Uani 1 1 d . . . . .
H2A H 0.503426 0.882155 0.631173 0.052 Uiso 1 1 calc R U . . .
H2B H 0.503088 0.952772 0.653591 0.052 Uiso 1 1 calc R U . . .
C3 C 0.3176(4) 0.8715(2) 0.56836(14) 0.0245(10) Uani 1 1 d . . . . .
C4 C 0.4207(5) 0.9094(3) 0.55982(14) 0.0249(10) Uani 1 1 d . . . . .
C5 C 0.3951(4) 0.8266(2) 0.50423(14) 0.0249(10) Uani 1 1 d . . . . .
C6 C 0.3995(5) 0.7965(2) 0.47035(15) 0.0263(10) Uani 1 1 d . . . . .
C7 C 0.3386(5) 0.7293(2) 0.41054(14) 0.0256(10) Uani 1 1 d . . . . .
C8 C 0.4404(5) 0.7673(3) 0.40045(14) 0.0263(10) Uani 1 1 d . . . . .
C9 C 0.2921(6) 0.7016(3) 0.33745(16) 0.0445(15) Uani 1 1 d . . . . .
H9A H 0.255914 0.669785 0.318586 0.053 Uiso 1 1 calc R U . . .
H9B H 0.253019 0.746925 0.333083 0.053 Uiso 1 1 calc R U . . .
C10 C 0.4349(7) 0.7068(3) 0.33142(17) 0.0441(14) Uani 1 1 d . . . . .
H10A H 0.451658 0.712084 0.304182 0.053 Uiso 1 1 calc R U . . .
H10B H 0.475562 0.663589 0.339595 0.053 Uiso 1 1 calc R U . . .
S9 S 0.75089(13) 0.89875(7) 0.37520(4) 0.0310(3) Uani 1 1 d . . . . .
S10 S 1.00556(12) 0.78821(7) 0.40047(4) 0.0332(3) Uani 1 1 d . . . . .
S11 S 0.78351(11) 0.95178(6) 0.45141(3) 0.0251(2) Uani 1 1 d . . . . .
S12 S 0.98621(11) 0.85731(6) 0.47368(4) 0.0263(2) Uani 1 1 d . . . . .
S13 S 0.77538(11) 1.01848(6) 0.53137(4) 0.0265(3) Uani 1 1 d . . . . .
S14 S 0.97791(11) 0.92727(6) 0.55821(3) 0.0233(2) Uani 1 1 d . . . . .
S15 S 0.73508(13) 1.08991(7) 0.60178(4) 0.0364(3) Uani 1 1 d . . . . .
S16 S 0.96998(12) 0.98143(7) 0.63711(3) 0.0284(3) Uani 1 1 d . . . . .
C11 C 0.8490(6) 0.8448(3) 0.34525(16) 0.0365(12) Uani 1 1 d . . . . .
H11A H 0.800151 0.834520 0.322025 0.044 Uiso 1 1 calc R U . . .
H11B H 0.927311 0.870309 0.337901 0.044 Uiso 1 1 calc R U . . .
C12 C 0.8890(6) 0.7787(3) 0.36320(16) 0.0367(12) Uani 1 1 d . . . . .
H12A H 0.925791 0.748553 0.343596 0.044 Uiso 1 1 calc R U . . .
H12B H 0.811544 0.755830 0.373436 0.044 Uiso 1 1 calc R U . . .
C13 C 0.8344(5) 0.8942(2) 0.41742(14) 0.0251(10) Uani 1 1 d . . . . .
C14 C 0.9312(5) 0.8511(2) 0.42759(14) 0.0262(10) Uani 1 1 d . . . . .
C15 C 0.8859(4) 0.9236(2) 0.48619(14) 0.0230(9) Uani 1 1 d . . . . .
C16 C 0.8824(4) 0.9536(2) 0.52129(14) 0.0224(9) Uani 1 1 d . . . . .
C17 C 0.8205(4) 1.0266(2) 0.57838(14) 0.0253(10) Uani 1 1 d . . . . .
C18 C 0.9141(4) 0.9852(2) 0.59063(13) 0.0225(9) Uani 1 1 d . . . . .
C19 C 0.7783(6) 1.0768(3) 0.65063(18) 0.0465(15) Uani 1 1 d . . . . .
H19A H 0.848825 1.108630 0.657215 0.056 Uiso 1 1 calc R U . . .
H19B H 0.703175 1.088414 0.666539 0.056 Uiso 1 1 calc R U . . .
C20 C 0.8206(6) 1.0051(3) 0.65977(16) 0.0397(13) Uani 1 1 d . . . . .
H20A H 0.752312 0.972921 0.651923 0.048 Uiso 1 1 calc R U . . .
H20B H 0.831233 1.000862 0.687326 0.048 Uiso 1 1 calc R U . . .
O7 O 0.500000 0.8753(4) 0.250000 0.0597(19) Uani 1 2 d DS T P . .
H7A H 0.491(6) 0.900(3) 0.2693(10) 0.072 Uiso 0.5 1 d D U P A -1
H7B H 0.441(5) 0.873(3) 0.2336(16) 0.072 Uiso 0.5 1 d D U P B -1
H7C H 0.569(3) 0.853(3) 0.2470(19) 0.072 Uiso 0.5 1 d D U P C -1
N1 N 0.7973(11) 0.4471(6) 0.2945(3) 0.050(3) Uani 0.5 1 d . . P D 1
C24 C 0.500000 0.4579(5) 0.250000 0.045(2) Uani 1 2 d S T P . .
H24 H 0.500000 0.409415 0.250000 0.054 Uiso 1 2 calc R U P . .
C25 C 0.6037(7) 0.4950(4) 0.26445(19) 0.0527(15) Uani 1 1 d . . . . .
H25 H 0.675926 0.471617 0.274621 0.063 Uiso 0.5 1 calc R U P E 2
C26 C 0.6019(10) 0.5649(4) 0.2640(2) 0.074(2) Uani 1 1 d . . . . .
H26 H 0.673831 0.589093 0.273828 0.089 Uiso 1 1 calc R U . . .
C27 C 0.500000 0.6011(6) 0.250000 0.087(4) Uani 1 2 d S T P . .
H27 H 0.500000 0.649548 0.249999 0.105 Uiso 1 2 calc R U P . .
C28 C 0.7065(12) 0.4697(7) 0.2795(3) 0.041(2) Uani 0.5 1 d . . P D 1


_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 O1 2.038(4) . ?
Ir1 O1 2.038(4) 3 ?
Ir1 O3 2.069(4) 3 ?
Ir1 O3 2.069(4) . ?
Ir1 O5 2.065(4) 3 ?
Ir1 O5 2.065(4) . ?
O1 C21 1.278(7) . ?
O2 C21 1.211(7) . ?
O3 C22 1.247(7) . ?
O4 C22 1.227(7) . ?
O5 C23 1.272(7) . ?
O6 C23 1.226(7) . ?
C21 C21 1.579(12) 3 ?
C22 C23 1.568(8) . ?
S1 C1 1.809(6) . ?
S1 C3 1.743(5) . ?
S2 C2 1.833(6) . ?
S2 C4 1.744(5) . ?
S3 C3 1.756(5) . ?
S3 C5 1.755(5) . ?
S4 C4 1.754(5) . ?
S4 C5 1.759(5) . ?
S5 C6 1.754(5) . ?
S5 C7 1.757(5) . ?
S6 C6 1.755(5) . ?
S6 C8 1.765(5) . ?
S7 C7 1.752(5) . ?
S7 C9 1.778(6) . ?
S8 C8 1.748(5) . ?
S8 C10 1.809(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.505(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.338(7) . ?
C5 C6 1.343(7) . ?
C7 C8 1.341(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.501(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
S9 C11 1.815(6) . ?
S9 C13 1.736(5) . ?
S10 C12 1.805(6) . ?
S10 C14 1.746(5) . ?
S11 C13 1.737(5) . ?
S11 C15 1.722(5) . ?
S12 C14 1.740(5) . ?
S12 C15 1.724(5) . ?
S13 C16 1.727(5) . ?
S13 C17 1.744(5) . ?
S14 C16 1.724(5) . ?
S14 C18 1.749(5) . ?
S15 C17 1.738(5) . ?
S15 C19 1.813(7) . ?
S16 C18 1.754(5) . ?
S16 C20 1.808(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.504(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.362(7) . ?
C15 C16 1.380(7) . ?
C17 C18 1.339(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.508(9) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
O7 H7A 0.848(13) . ?
O7 H7A 0.848(13) 3_655 ?
O7 H7B 0.848(13) 3_655 ?
O7 H7B 0.848(13) . ?
O7 H7C 0.849(13) . ?
O7 H7C 0.849(13) 3_655 ?
N1 C28 1.170(17) . ?
C24 H24 0.9500 . ?
C24 C25 1.398(8) 3_655 ?
C24 C25 1.398(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.372(11) . ?
C25 C28 1.293(15) . ?
C26 H26 0.9500 . ?
C26 C27 1.368(12) . ?
C27 H27 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
O1 Ir1 O1 82.1(2) . 3 ?
O1 Ir1 O3 88.11(16) 3 . ?
O1 Ir1 O3 94.14(15) . . ?
O1 Ir1 O3 94.14(15) 3 3 ?
O1 Ir1 O3 88.11(16) . 3 ?
O1 Ir1 O5 97.26(15) . 3 ?
O1 Ir1 O5 177.99(16) . . ?
O1 Ir1 O5 97.26(15) 3 . ?
O1 Ir1 O5 177.99(16) 3 3 ?
O3 Ir1 O3 177.0(2) . 3 ?
O5 Ir1 O3 83.94(15) 3 3 ?
O5 Ir1 O3 93.83(15) . 3 ?
O5 Ir1 O3 93.84(15) 3 . ?
O5 Ir1 O3 83.94(15) . . ?
O5 Ir1 O5 83.5(2) 3 . ?
C21 O1 Ir1 113.5(4) . . ?
C22 O3 Ir1 109.9(4) . . ?
C23 O5 Ir1 108.6(4) . . ?
O1 C21 C21 115.4(3) . 3 ?
O2 C21 O1 124.3(6) . . ?
O2 C21 C21 120.2(4) . 3 ?
O3 C22 C23 118.1(5) . . ?
O4 C22 O3 123.2(6) . . ?
O4 C22 C23 118.7(5) . . ?
O5 C23 C22 118.4(5) . . ?
O6 C23 O5 123.2(6) . . ?
O6 C23 C22 118.3(5) . . ?
C3 S1 C1 105.7(3) . . ?
C4 S2 C2 96.4(3) . . ?
C5 S3 C3 94.3(2) . . ?
C4 S4 C5 94.1(2) . . ?
C6 S5 C7 94.6(2) . . ?
C6 S6 C8 94.6(2) . . ?
C7 S7 C9 99.8(3) . . ?
C8 S8 C10 100.2(3) . . ?
S1 C1 H1A 108.4 . . ?
S1 C1 H1B 108.4 . . ?
H1A C1 H1B 107.4 . . ?
C2 C1 S1 115.6(4) . . ?
C2 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
S2 C2 H2A 108.7 . . ?
S2 C2 H2B 108.7 . . ?
C1 C2 S2 114.4(4) . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
S1 C3 S3 115.5(3) . . ?
C4 C3 S1 127.0(4) . . ?
C4 C3 S3 117.4(4) . . ?
S2 C4 S4 118.4(3) . . ?
C3 C4 S2 123.6(4) . . ?
C3 C4 S4 117.6(4) . . ?
S3 C5 S4 114.7(3) . . ?
C6 C5 S3 121.7(4) . . ?
C6 C5 S4 123.5(4) . . ?
S5 C6 S6 114.7(3) . . ?
C5 C6 S5 121.4(4) . . ?
C5 C6 S6 123.9(4) . . ?
S7 C7 S5 113.6(3) . . ?
C8 C7 S5 117.7(4) . . ?
C8 C7 S7 128.7(4) . . ?
S8 C8 S6 114.2(3) . . ?
C7 C8 S6 116.8(4) . . ?
C7 C8 S8 129.0(4) . . ?
S7 C9 H9A 108.7 . . ?
S7 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 S7 114.1(4) . . ?
C10 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
S8 C10 H10A 108.7 . . ?
S8 C10 H10B 108.7 . . ?
C9 C10 S8 114.3(5) . . ?
C9 C10 H10A 108.7 . . ?
C9 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C13 S9 C11 101.4(3) . . ?
C14 S10 C12 100.6(3) . . ?
C15 S11 C13 96.0(2) . . ?
C15 S12 C14 95.6(2) . . ?
C16 S13 C17 95.4(2) . . ?
C16 S14 C18 95.2(2) . . ?
C17 S15 C19 103.4(3) . . ?
C18 S16 C20 97.2(3) . . ?
S9 C11 H11A 108.7 . . ?
S9 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 S9 114.1(4) . . ?
C12 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
S10 C12 H12A 108.7 . . ?
S10 C12 H12B 108.7 . . ?
C11 C12 S10 114.1(4) . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
S9 C13 S11 114.6(3) . . ?
C14 C13 S9 129.1(4) . . ?
C14 C13 S11 116.3(4) . . ?
S12 C14 S10 115.1(3) . . ?
C13 C14 S10 128.1(4) . . ?
C13 C14 S12 116.7(4) . . ?
S11 C15 S12 115.4(3) . . ?
C16 C15 S11 119.9(4) . . ?
C16 C15 S12 124.7(4) . . ?
S14 C16 S13 115.6(3) . . ?
C15 C16 S13 121.2(4) . . ?
C15 C16 S14 123.2(4) . . ?
S15 C17 S13 112.8(3) . . ?
C18 C17 S13 116.9(4) . . ?
C18 C17 S15 130.3(4) . . ?
S14 C18 S16 118.0(3) . . ?
C17 C18 S14 117.0(4) . . ?
C17 C18 S16 124.9(4) . . ?
S15 C19 H19A 108.7 . . ?
S15 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C20 C19 S15 114.3(4) . . ?
C20 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
S16 C20 H20A 108.9 . . ?
S16 C20 H20B 108.9 . . ?
C19 C20 S16 113.2(4) . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.8 . . ?
H7A O7 H7A 110(9) . 3_655 ?
H7A O7 H7B 120.1(10) . . ?
H7A O7 H7B 64(5) . 3_655 ?
H7A O7 H7C 96(7) . 3_655 ?
H7A O7 H7C 119.9(10) . . ?
H7B O7 H7A 64(5) . 3_655 ?
H7B O7 H7A 120.1(11) 3_655 3_655 ?
H7B O7 H7B 174(8) . 3_655 ?
H7B O7 H7C 120.0(10) . . ?
H7B O7 H7C 57(5) . 3_655 ?
H7C O7 H7A 96(7) . 3_655 ?
H7C O7 H7A 119.9(10) 3_655 3_655 ?
H7C O7 H7B 57(5) . 3_655 ?
H7C O7 H7B 120.0(10) 3_655 3_655 ?
H7C O7 H7C 117(9) . 3_655 ?
C25 C24 H24 121.4 3_655 . ?
C25 C24 H24 121.4 . . ?
C25 C24 C25 117.3(10) 3_655 . ?
C24 C25 H25 119.8 . . ?
C26 C25 C24 120.4(8) . . ?
C26 C25 H25 119.8 . . ?
C28 C25 C24 126.1(9) . . ?
C28 C25 C26 113.5(9) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 C25 122.2(9) . . ?
C27 C26 H26 118.9 . . ?
C26 C27 C26 117.6(11) 3_655 . ?
C26 C27 H27 121.2 3_655 . ?
C26 C27 H27 121.2 . . ?
N1 C28 C25 177.4(12) . . ?

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 O1 C21 O2 -176.8(6) . . . . ?
Ir1 O1 C21 C21 0.3(9) . . . 3 ?
Ir1 O3 C22 O4 -179.2(5) . . . . ?
Ir1 O3 C22 C23 1.0(6) . . . . ?
Ir1 O5 C23 O6 172.9(5) . . . . ?
Ir1 O5 C23 C22 -10.7(6) . . . . ?
O3 C22 C23 O5 7.1(8) . . . . ?
O3 C22 C23 O6 -176.3(6) . . . . ?
O4 C22 C23 O5 -172.6(5) . . . . ?
O4 C22 C23 O6 4.0(9) . . . . ?
S1 C1 C2 S2 50.5(6) . . . . ?
S1 C3 C4 S2 2.6(7) . . . . ?
S1 C3 C4 S4 175.3(3) . . . . ?
S3 C3 C4 S2 -174.2(3) . . . . ?
S3 C3 C4 S4 -1.5(6) . . . . ?
S3 C5 C6 S5 -0.1(6) . . . . ?
S3 C5 C6 S6 -176.8(3) . . . . ?
S4 C5 C6 S5 175.7(3) . . . . ?
S4 C5 C6 S6 -0.9(7) . . . . ?
S5 C7 C8 S6 2.7(5) . . . . ?
S5 C7 C8 S8 -178.5(3) . . . . ?
S7 C7 C8 S6 -174.9(3) . . . . ?
S7 C7 C8 S8 3.9(7) . . . . ?
S7 C9 C10 S8 -71.8(6) . . . . ?
C1 S1 C3 S3 150.1(3) . . . . ?
C1 S1 C3 C4 -26.8(5) . . . . ?
C2 S2 C4 S4 -132.1(3) . . . . ?
C2 S2 C4 C3 40.5(5) . . . . ?
C3 S1 C1 C2 -2.8(5) . . . . ?
C3 S3 C5 S4 12.9(3) . . . . ?
C3 S3 C5 C6 -170.9(4) . . . . ?
C4 S2 C2 C1 -67.5(5) . . . . ?
C4 S4 C5 S3 -13.5(3) . . . . ?
C4 S4 C5 C6 170.4(5) . . . . ?
C5 S3 C3 S1 175.9(3) . . . . ?
C5 S3 C3 C4 -6.9(4) . . . . ?
C5 S4 C4 S2 -177.9(3) . . . . ?
C5 S4 C4 C3 9.0(4) . . . . ?
C6 S5 C7 S7 -176.9(3) . . . . ?
C6 S5 C7 C8 5.2(4) . . . . ?
C6 S6 C8 S8 171.9(3) . . . . ?
C6 S6 C8 C7 -9.1(4) . . . . ?
C7 S5 C6 S6 -11.3(3) . . . . ?
C7 S5 C6 C5 171.8(4) . . . . ?
C7 S7 C9 C10 51.2(5) . . . . ?
C8 S6 C6 S5 12.4(3) . . . . ?
C8 S6 C6 C5 -170.8(5) . . . . ?
C8 S8 C10 C9 46.1(5) . . . . ?
C9 S7 C7 S5 163.9(3) . . . . ?
C9 S7 C7 C8 -18.4(5) . . . . ?
C10 S8 C8 S6 165.5(3) . . . . ?
C10 S8 C8 C7 -13.3(6) . . . . ?
S9 C11 C12 S10 -70.2(5) . . . . ?
S9 C13 C14 S10 2.2(7) . . . . ?
S9 C13 C14 S12 -175.9(3) . . . . ?
S11 C13 C14 S10 -179.3(3) . . . . ?
S11 C13 C14 S12 2.5(5) . . . . ?
S11 C15 C16 S13 0.8(6) . . . . ?
S11 C15 C16 S14 178.1(2) . . . . ?
S12 C15 C16 S13 -178.4(3) . . . . ?
S12 C15 C16 S14 -1.1(6) . . . . ?
S13 C17 C18 S14 -1.0(5) . . . . ?
S13 C17 C18 S16 -176.9(3) . . . . ?
S15 C17 C18 S14 -179.8(3) . . . . ?
S15 C17 C18 S16 4.3(7) . . . . ?
S15 C19 C20 S16 66.0(6) . . . . ?
C11 S9 C13 S11 169.6(3) . . . . ?
C11 S9 C13 C14 -12.0(5) . . . . ?
C12 S10 C14 S12 161.0(3) . . . . ?
C12 S10 C14 C13 -17.2(5) . . . . ?
C13 S9 C11 C12 45.2(5) . . . . ?
C13 S11 C15 S12 0.4(3) . . . . ?
C13 S11 C15 C16 -178.8(4) . . . . ?
C14 S10 C12 C11 50.5(5) . . . . ?
C14 S12 C15 S11 0.6(3) . . . . ?
C14 S12 C15 C16 179.8(4) . . . . ?
C15 S11 C13 S9 176.9(3) . . . . ?
C15 S11 C13 C14 -1.7(4) . . . . ?
C15 S12 C14 S10 179.7(3) . . . . ?
C15 S12 C14 C13 -1.9(4) . . . . ?
C16 S13 C17 S15 179.6(3) . . . . ?
C16 S13 C17 C18 0.5(4) . . . . ?
C16 S14 C18 S16 177.1(3) . . . . ?
C16 S14 C18 C17 0.8(4) . . . . ?
C17 S13 C16 S14 0.1(3) . . . . ?
C17 S13 C16 C15 177.6(4) . . . . ?
C17 S15 C19 C20 -24.6(5) . . . . ?
C18 S14 C16 S13 -0.5(3) . . . . ?
C18 S14 C16 C15 -177.9(4) . . . . ?
C18 S16 C20 C19 -64.8(5) . . . . ?
C19 S15 C17 S13 169.9(3) . . . . ?
C19 S15 C17 C18 -11.2(6) . . . . ?
C20 S16 C18 S14 -146.0(3) . . . . ?
C20 S16 C18 C17 29.9(5) . . . . ?
C24 C25 C26 C27 0.5(10) . . . . ?
C25 C24 C25 C26 -0.2(5) 3_655 . . . ?
C25 C24 C25 C28 178.6(10) 3_655 . . . ?
C25 C26 C27 C26 -0.3(5) . . . 3_655 ?
C28 C25 C26 C27 -178.5(7) . . . . ?

_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 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.696
####################################################################### 
# 
# 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_et4nh4gaox3-phi
_database_code_depnum_ccdc_archive 'CCDC 2163085'
loop_
_audit_author_name
_audit_author_address
'Toby Blundell'
;Nottingham Trent University
United Kingdom
;
_audit_update_record             
;
2022-03-29 deposited with the CCDC.	2022-04-25 downloaded from the CCDC.
;
_audit_creation_date             2022-01-27
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H5 I, C6 Ga O12, 4(C10 H8 S8), 0.5(H6 O2)'
_chemical_formula_sum            'C52 H40 Ga I O13 S32'
_chemical_formula_weight         2095.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   10.2593(2)
_cell_length_b                   20.0074(4)
_cell_length_c                   35.5849(7)
_cell_angle_alpha                90
_cell_angle_beta                 93.740(2)
_cell_angle_gamma                90
_cell_volume                     7288.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17279
_cell_measurement_temperature    293.5(3)
_cell_measurement_theta_max      27.7850
_cell_measurement_theta_min      3.4980
_shelx_estimated_absorpt_T_max   0.720
_shelx_estimated_absorpt_T_min   0.533
_exptl_absorpt_coefficient_mu    1.778
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.597
_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 black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4208
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 5 -1 0.1899
0 0 -1 0.1164
5 -4 3 0.1051
3 -2 5 0.0984
0 0 1 0.0821
-3 2 -5 0.1173
5 5 -2 0.1270
4 -5 -1 0.1259
0 -5 1 0.1884
-4 -5 2 0.1359
-5 4 1 0.1279

_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.198
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            35658
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.875
_diffrn_reflns_theta_min         3.068
_diffrn_ambient_temperature      293.5(3)
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  52.00   0.25    7.50    --  -18.35  57.00 150.00  376
  2  ω    -52.00  45.00   0.25    7.50    --   18.35 -64.00 177.28  388
  3  ω    -48.00  94.00   0.25    7.50    --   18.35  19.00   0.00  568
  4  ω     -5.00  89.00   0.25    7.50    --   18.35  57.00  90.00  376
  5  ω     -5.00  31.00   0.25    7.50    --   18.35  57.00-150.00  144
  6  ω    -55.00  51.00   0.25    7.50    --   18.35 -37.00 -60.00  424
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7250
_reflns_number_total             7838
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         7838
_refine_ls_number_restraints     376
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0347
_refine_ls_restrained_S_all      2.529
_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)+(0.0271P)²+16.1615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0819
_refine_special_details          
'Positional disorder was found for 2 terminal ethyl groups on the BEDT-TTF molecule (C1, C2 and C9 C10). The disorder was modelled, and the occupancy of the major and minor components competitively refined to 77:23 (C1, C2) and 69:31 (C9, C10) respectively Relevant 1,2- bond distances were restrained to be approximately equal. Oxygen-hydrogen 1,2- and hydrogen-hydrogen 1,3 distances for O1W were restrained to be approximately equal. Enhanced rigid bond restraints were applied to all atoms.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 H1WA-H1WB \\sim H1WB-H1WC \\sim H1WA-H1WC
 with sigma of 0.001
 S2-C2A \\sim S2-C2
 with sigma of 0.02
 C1A-C2A \\sim C1-C2
 with sigma of 0.02
 C9A-C10A \\sim C9-C10
 with sigma of 0.02
 S7-C9A \\sim S7-C9
 with sigma of 0.02
 S2-C2 \\sim S2A-C2A
 with sigma of 0.02
 S2-C4 \\sim S2A-C4
 with sigma of 0.02
 S8-C10 \\sim S8-C10A
 with sigma of 0.02
 S1-C1 \\sim S1-C1A
 with sigma of 0.02
3. Restrained planarity
 O1W, H1WA, H1WB, H1WC
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(S2A)=1-FVAR(2)
 Sof(S2)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(2)
 Fixed Sof: H1WA(0.5) H1WB(0.5) H1WC(0.5)
6.a Free rotating group:
 O1W(H1WA,H1WB,H1WC)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C19(H19A,H19B), C2(H2A,H2B), C20(H20A,H20B),
 C9(H9A,H9B), C1(H1A,H1B), C10(H10A,H10B), C10A(H10C,H10D), C9A(H9AA,H9AB),
 C1A(H1AA,H1AB), C2A(H2AA,H2AB)
6.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27)
;
_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
I1 I 0.000000 0.14288(2) 0.750000 0.09142(18) Uani 1 2 d S T P . .
Ga1 Ga 0.500000 0.41511(2) 0.750000 0.03063(10) Uani 1 2 d S T P . .
S11 S 0.66692(6) 0.35632(4) 0.53142(2) 0.03508(15) Uani 1 1 d . . . . .
S5 S 0.37999(6) 0.45846(3) 0.46442(2) 0.03528(15) Uani 1 1 d . . . . .
S3 S 0.26001(6) 0.48849(4) 0.54452(2) 0.03604(15) Uani 1 1 d . . . . .
S13 S 0.77839(6) 0.32619(4) 0.45124(2) 0.03631(15) Uani 1 1 d . . . . .
S6 S 0.14293(6) 0.38328(4) 0.44097(2) 0.03744(16) Uani 1 1 d . . . . .
S4 S 0.02559(6) 0.41214(4) 0.52037(2) 0.03743(16) Uani 1 1 d . . . . .
S12 S 0.42347(7) 0.28680(4) 0.50850(2) 0.03819(16) Uani 1 1 d . . . . .
S14 S 0.53738(7) 0.25537(4) 0.42743(2) 0.03742(15) Uani 1 1 d . . . . .
S7 S 0.51282(7) 0.42818(4) 0.39499(2) 0.03940(16) Uani 1 1 d D . . . .
S9 S 0.59362(7) 0.38851(4) 0.60799(2) 0.04113(17) Uani 1 1 d . . . . .
S10 S 0.29952(7) 0.30750(4) 0.57924(2) 0.04421(17) Uani 1 1 d . . . . .
S1 S 0.17885(7) 0.51588(4) 0.62106(2) 0.04483(18) Uani 1 1 d D . . . .
S15 S 0.90316(8) 0.30775(4) 0.38006(2) 0.04570(18) Uani 1 1 d . . . . .
S8 S 0.23605(9) 0.34236(4) 0.36766(2) 0.0498(2) Uani 1 1 d D . . . .
S16 S 0.60863(9) 0.22921(4) 0.35056(2) 0.0527(2) Uani 1 1 d . . . . .
S2 S -0.1065(3) 0.4312(2) 0.58988(11) 0.0446(7) Uani 0.771(9) 1 d D . P A 1
O3 O 0.35572(19) 0.42776(10) 0.78322(5) 0.0386(4) Uani 1 1 d . . . . .
O5 O 0.39964(18) 0.48030(9) 0.71811(5) 0.0374(4) Uani 1 1 d . . . . .
O1 O 0.4239(2) 0.34118(10) 0.71938(5) 0.0423(5) Uani 1 1 d . . . . .
O6 O 0.2150(2) 0.53882(12) 0.71675(6) 0.0535(6) Uani 1 1 d . . . . .
O4 O 0.1880(2) 0.49689(13) 0.78983(6) 0.0551(6) Uani 1 1 d . . . . .
O2 O 0.4162(2) 0.22988(11) 0.71776(7) 0.0602(6) Uani 1 1 d . . . . .
O1W O 0.000000 0.40225(18) 0.250000 0.0784(12) Uani 1 2 d GS T P . .
H1WA H -0.050004 0.425669 0.259831 0.094 Uiso 0.5 1 d DG U P B -1
H1WB H 0.069624 0.426414 0.248753 0.094 Uiso 0.5 1 d DG U P C -1
H1WC H -0.008566 0.366295 0.242269 0.094 Uiso 0.5 1 d DG U P D -1
C6 C 0.2290(2) 0.42834(13) 0.47610(7) 0.0303(5) Uani 1 1 d . . . . .
C5 C 0.1786(2) 0.44111(13) 0.50974(7) 0.0302(5) Uani 1 1 d . . . . .
C4 C 0.0333(2) 0.44505(14) 0.56574(7) 0.0332(5) Uani 1 1 d D . . . .
C16 C 0.6247(2) 0.29932(12) 0.46260(7) 0.0307(5) Uani 1 1 d . . . . .
C3 C 0.1410(2) 0.47993(13) 0.57712(7) 0.0313(5) Uani 1 1 d . . . . .
C7 C 0.3777(2) 0.41723(13) 0.42128(7) 0.0312(5) Uani 1 1 d . . . . .
C15 C 0.5771(2) 0.31270(13) 0.49659(7) 0.0309(5) Uani 1 1 d . . . . .
C8 C 0.2687(2) 0.38329(13) 0.41021(7) 0.0320(5) Uani 1 1 d . . . . .
C21 C 0.2953(3) 0.50081(14) 0.73203(8) 0.0358(6) Uani 1 1 d . . . . .
C13 C 0.5489(2) 0.35213(13) 0.56453(7) 0.0307(5) Uani 1 1 d . . . . .
C14 C 0.4369(2) 0.32037(13) 0.55385(7) 0.0321(5) Uani 1 1 d . . . . .
C17 C 0.7678(3) 0.29333(13) 0.40596(7) 0.0337(5) Uani 1 1 d . . . . .
C22 C 0.2749(3) 0.47350(14) 0.77213(8) 0.0383(6) Uani 1 1 d . . . . .
C18 C 0.6559(3) 0.26210(13) 0.39475(7) 0.0343(6) Uani 1 1 d . . . . .
C23 C 0.4537(3) 0.28280(14) 0.73171(8) 0.0408(6) Uani 1 1 d . . . . .
C11 C 0.4394(3) 0.39335(14) 0.62885(8) 0.0401(6) Uani 1 1 d . . . . .
H11A H 0.454927 0.405490 0.655150 0.048 Uiso 1 1 calc R U . . .
H11B H 0.388221 0.428824 0.616556 0.048 Uiso 1 1 calc R U . . .
C12 C 0.3603(3) 0.32966(15) 0.62647(8) 0.0428(7) Uani 1 1 d . . . . .
H12A H 0.286721 0.334413 0.642045 0.051 Uiso 1 1 calc R U . . .
H12B H 0.414134 0.293331 0.636772 0.051 Uiso 1 1 calc R U . . .
C24 C 0.000000 0.2467(2) 0.750000 0.0502(11) Uani 1 2 d S T P . .
C25 C 0.0927(4) 0.28014(18) 0.73057(10) 0.0564(8) Uani 1 1 d . . . . .
H25 H 0.154130 0.256846 0.717619 0.068 Uiso 1 1 calc R U . . .
C19 C 0.8260(4) 0.30466(19) 0.33359(9) 0.0596(9) Uani 1 1 d . . . . .
H19A H 0.764597 0.341395 0.330443 0.071 Uiso 1 1 calc R U . . .
H19B H 0.891754 0.310552 0.315473 0.071 Uiso 1 1 calc R U . . .
C2 C -0.0392(7) 0.4451(3) 0.63811(17) 0.0473(15) Uani 0.771(9) 1 d D . P A 1
H2A H -0.108839 0.442120 0.655211 0.057 Uiso 0.771(9) 1 calc R U P A 1
H2B H 0.024088 0.410375 0.644920 0.057 Uiso 0.771(9) 1 calc R U P A 1
C20 C 0.7547(4) 0.2398(2) 0.32543(9) 0.0625(10) Uani 1 1 d . . . . .
H20A H 0.813620 0.202988 0.331814 0.075 Uiso 1 1 calc R U . . .
H20B H 0.731167 0.237257 0.298617 0.075 Uiso 1 1 calc R U . . .
C9 C 0.4194(7) 0.4375(3) 0.34919(12) 0.0386(15) Uani 0.693(15) 1 d D . P E 1
H9A H 0.355707 0.473028 0.351086 0.046 Uiso 0.693(15) 1 calc R U P E 1
H9B H 0.478541 0.450598 0.330317 0.046 Uiso 0.693(15) 1 calc R U P E 1
C1 C 0.0258(4) 0.5125(2) 0.64231(11) 0.0397(11) Uani 0.771(9) 1 d D . P A 1
H1A H 0.039716 0.522973 0.668881 0.048 Uiso 0.771(9) 1 calc R U P A 1
H1B H -0.032058 0.546189 0.630873 0.048 Uiso 0.771(9) 1 calc R U P A 1
C26 C 0.0911(4) 0.3491(2) 0.73102(14) 0.0782(13) Uani 1 1 d . . . . .
H26 H 0.152656 0.372732 0.718284 0.094 Uiso 1 1 calc R U . . .
C10 C 0.3497(7) 0.3744(4) 0.33658(14) 0.0416(15) Uani 0.693(15) 1 d D . P E 1
H10A H 0.414700 0.340240 0.332889 0.050 Uiso 0.693(15) 1 calc R U P E 1
H10B H 0.303734 0.382748 0.312346 0.050 Uiso 0.693(15) 1 calc R U P E 1
C27 C 0.000000 0.3831(3) 0.750000 0.091(2) Uani 1 2 d S T P . .
H27 H -0.000002 0.429619 0.749999 0.109 Uiso 1 2 calc R U P . .
C10A C 0.3236(11) 0.4039(9) 0.3410(4) 0.052(4) Uani 0.307(15) 1 d D . P E 2
H10C H 0.306775 0.393621 0.314443 0.062 Uiso 0.307(15) 1 calc R U P E 2
H10D H 0.284857 0.447228 0.345209 0.062 Uiso 0.307(15) 1 calc R U P E 2
C9A C 0.4692(14) 0.4110(11) 0.3483(3) 0.058(4) Uani 0.307(15) 1 d D . P E 2
H9AA H 0.500093 0.446737 0.332740 0.069 Uiso 0.307(15) 1 calc R U P E 2
H9AB H 0.511304 0.369935 0.341156 0.069 Uiso 0.307(15) 1 calc R U P E 2
C1A C 0.0662(13) 0.4658(9) 0.6469(3) 0.050(5) Uani 0.229(9) 1 d D . P A 2
H1AA H 0.095588 0.419737 0.646359 0.060 Uiso 0.229(9) 1 calc R U P A 2
H1AB H 0.073715 0.480195 0.672939 0.060 Uiso 0.229(9) 1 calc R U P A 2
C2A C -0.0762(16) 0.4669(12) 0.6339(7) 0.051(6) Uani 0.229(9) 1 d D . P A 2
H2AA H -0.104462 0.511742 0.626926 0.062 Uiso 0.229(9) 1 calc R U P A 2
H2AB H -0.129771 0.450190 0.653288 0.062 Uiso 0.229(9) 1 calc R U P A 2
S2A S -0.0848(14) 0.4123(6) 0.5935(4) 0.049(3) Uani 0.229(9) 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
I1 C24 2.078(4) . ?
Ga1 O3 1.9700(18) . ?
Ga1 O3 1.9700(19) 2_656 ?
Ga1 O5 1.9741(19) 2_656 ?
Ga1 O5 1.9741(18) . ?
Ga1 O1 1.9681(19) 2_656 ?
Ga1 O1 1.9681(19) . ?
S11 C15 1.732(3) . ?
S11 C13 1.746(3) . ?
S5 C6 1.738(3) . ?
S5 C7 1.741(3) . ?
S3 C5 1.730(2) . ?
S3 C3 1.746(3) . ?
S13 C16 1.739(3) . ?
S13 C17 1.737(3) . ?
S6 C6 1.735(3) . ?
S6 C8 1.746(3) . ?
S4 C5 1.738(3) . ?
S4 C4 1.741(3) . ?
S12 C15 1.737(3) . ?
S12 C14 1.745(3) . ?
S14 C16 1.731(2) . ?
S14 C18 1.742(3) . ?
S7 C7 1.736(3) . ?
S7 C9 1.846(5) . ?
S7 C9A 1.727(11) . ?
S9 C13 1.743(3) . ?
S9 C11 1.793(3) . ?
S10 C14 1.742(3) . ?
S10 C12 1.809(3) . ?
S1 C3 1.742(3) . ?
S1 C1 1.788(4) . ?
S1 C1A 1.822(12) . ?
S15 C17 1.740(3) . ?
S15 C19 1.787(4) . ?
S8 C8 1.735(3) . ?
S8 C10 1.778(5) . ?
S8 C10A 1.827(12) . ?
S16 C18 1.744(3) . ?
S16 C20 1.807(4) . ?
S2 C4 1.741(4) . ?
S2 C2 1.829(6) . ?
O3 C22 1.280(3) . ?
O5 C21 1.276(3) . ?
O1 C23 1.278(3) . ?
O6 C21 1.222(3) . ?
O4 C22 1.219(3) . ?
O2 C23 1.221(3) . ?
O1W H1WA 0.7928 . ?
O1W H1WB 0.8661 . ?
O1W H1WC 0.7731 . ?
C6 C5 1.358(4) . ?
C4 C3 1.347(4) . ?
C4 S2A 1.740(12) . ?
C16 C15 1.360(4) . ?
C7 C8 1.345(4) . ?
C21 C22 1.555(4) . ?
C13 C14 1.346(4) . ?
C17 C18 1.344(4) . ?
C23 C23 1.561(6) 2_656 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.510(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C24 C25 1.384(4) . ?
C24 C25 1.384(4) 2_556 ?
C25 H25 0.9300 . ?
C25 C26 1.380(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.510(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.508(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.505(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C26 H26 0.9300 . ?
C26 C27 1.370(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C27 H27 0.9300 . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C10A C9A 1.506(14) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C1A C2A 1.504(16) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A S2A 1.802(15) . ?

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
O3 Ga1 O3 165.24(12) 2_656 . ?
O3 Ga1 O5 82.87(8) 2_656 2_656 ?
O3 Ga1 O5 87.38(8) . 2_656 ?
O3 Ga1 O5 87.38(8) 2_656 . ?
O3 Ga1 O5 82.87(8) . . ?
O5 Ga1 O5 97.28(12) . 2_656 ?
O1 Ga1 O3 92.90(8) . 2_656 ?
O1 Ga1 O3 92.90(8) 2_656 . ?
O1 Ga1 O3 98.20(8) . . ?
O1 Ga1 O3 98.19(8) 2_656 2_656 ?
O1 Ga1 O5 90.30(8) . . ?
O1 Ga1 O5 171.12(9) 2_656 . ?
O1 Ga1 O5 90.30(8) 2_656 2_656 ?
O1 Ga1 O5 171.12(8) . 2_656 ?
O1 Ga1 O1 82.55(12) 2_656 . ?
C15 S11 C13 95.66(12) . . ?
C6 S5 C7 94.91(12) . . ?
C5 S3 C3 95.51(12) . . ?
C17 S13 C16 95.51(12) . . ?
C6 S6 C8 95.13(12) . . ?
C5 S4 C4 95.09(12) . . ?
C15 S12 C14 95.32(12) . . ?
C16 S14 C18 95.32(12) . . ?
C7 S7 C9 95.8(2) . . ?
C9A S7 C7 109.1(4) . . ?
C13 S9 C11 101.62(13) . . ?
C14 S10 C12 101.77(13) . . ?
C3 S1 C1 102.32(15) . . ?
C3 S1 C1A 96.5(4) . . ?
C17 S15 C19 99.44(15) . . ?
C8 S8 C10 105.99(19) . . ?
C8 S8 C10A 93.6(6) . . ?
C18 S16 C20 102.20(15) . . ?
C4 S2 C2 99.6(3) . . ?
C22 O3 Ga1 113.81(17) . . ?
C21 O5 Ga1 114.12(17) . . ?
C23 O1 Ga1 114.82(18) . . ?
H1WA O1W H1WB 104.6 . . ?
H1WA O1W H1WC 130.2 . . ?
H1WB O1W H1WC 125.2 . . ?
S6 C6 S5 115.30(14) . . ?
C5 C6 S5 122.8(2) . . ?
C5 C6 S6 121.9(2) . . ?
S3 C5 S4 115.31(14) . . ?
C6 C5 S3 122.7(2) . . ?
C6 C5 S4 121.99(19) . . ?
S4 C4 S2 114.1(2) . . ?
C3 C4 S4 117.5(2) . . ?
C3 C4 S2 128.3(2) . . ?
C3 C4 S2A 127.8(5) . . ?
S2A C4 S4 113.1(5) . . ?
S14 C16 S13 115.04(14) . . ?
C15 C16 S13 121.99(19) . . ?
C15 C16 S14 123.0(2) . . ?
S1 C3 S3 115.55(14) . . ?
C4 C3 S3 116.51(19) . . ?
C4 C3 S1 127.9(2) . . ?
S7 C7 S5 116.73(14) . . ?
C8 C7 S5 117.4(2) . . ?
C8 C7 S7 125.7(2) . . ?
S11 C15 S12 115.12(15) . . ?
C16 C15 S11 122.0(2) . . ?
C16 C15 S12 122.8(2) . . ?
S8 C8 S6 116.02(14) . . ?
C7 C8 S6 116.8(2) . . ?
C7 C8 S8 127.1(2) . . ?
O5 C21 C22 114.2(2) . . ?
O6 C21 O5 125.8(3) . . ?
O6 C21 C22 120.0(3) . . ?
S9 C13 S11 115.13(14) . . ?
C14 C13 S11 116.7(2) . . ?
C14 C13 S9 128.2(2) . . ?
S10 C14 S12 113.89(15) . . ?
C13 C14 S12 117.2(2) . . ?
C13 C14 S10 128.9(2) . . ?
S13 C17 S15 115.15(15) . . ?
C18 C17 S13 116.8(2) . . ?
C18 C17 S15 128.0(2) . . ?
O3 C22 C21 114.3(2) . . ?
O4 C22 O3 126.6(3) . . ?
O4 C22 C21 119.1(3) . . ?
S14 C18 S16 114.04(15) . . ?
C17 C18 S14 117.2(2) . . ?
C17 C18 S16 128.7(2) . . ?
O1 C23 C23 113.90(16) . 2_656 ?
O2 C23 O1 126.3(3) . . ?
O2 C23 C23 119.83(19) . 2_656 ?
S9 C11 H11A 108.6 . . ?
S9 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 S9 114.6(2) . . ?
C12 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
S10 C12 H12A 108.7 . . ?
S10 C12 H12B 108.7 . . ?
C11 C12 S10 114.2(2) . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C25 C24 I1 118.9(2) . . ?
C25 C24 I1 118.9(2) 2_556 . ?
C25 C24 C25 122.2(5) 2_556 . ?
C24 C25 H25 121.0 . . ?
C26 C25 C24 117.9(4) . . ?
C26 C25 H25 121.0 . . ?
S15 C19 H19A 109.0 . . ?
S15 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C20 C19 S15 112.8(2) . . ?
C20 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
S2 C2 H2A 109.3 . . ?
S2 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C1 C2 S2 111.5(4) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
S16 C20 H20A 108.7 . . ?
S16 C20 H20B 108.7 . . ?
C19 C20 S16 114.4(2) . . ?
C19 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
S7 C9 H9A 109.0 . . ?
S7 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 S7 112.8(4) . . ?
C10 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
S1 C1 H1A 109.0 . . ?
S1 C1 H1B 109.0 . . ?
C2 C1 S1 112.8(4) . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C25 C26 H26 119.6 . . ?
C27 C26 C25 120.8(5) . . ?
C27 C26 H26 119.6 . . ?
S8 C10 H10A 108.3 . . ?
S8 C10 H10B 108.3 . . ?
C9 C10 S8 115.8(5) . . ?
C9 C10 H10A 108.3 . . ?
C9 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C26 C27 C26 120.4(6) . 2_556 ?
C26 C27 H27 119.8 . . ?
C26 C27 H27 119.8 2_556 . ?
S8 C10A H10C 107.5 . . ?
S8 C10A H10D 107.5 . . ?
H10C C10A H10D 107.0 . . ?
C9A C10A S8 119.3(11) . . ?
C9A C10A H10C 107.5 . . ?
C9A C10A H10D 107.5 . . ?
S7 C9A H9AA 109.2 . . ?
S7 C9A H9AB 109.2 . . ?
C10A C9A S7 112.2(11) . . ?
C10A C9A H9AA 109.2 . . ?
C10A C9A H9AB 109.2 . . ?
H9AA C9A H9AB 107.9 . . ?
S1 C1A H1AA 107.8 . . ?
S1 C1A H1AB 107.8 . . ?
H1AA C1A H1AB 107.1 . . ?
C2A C1A S1 118.2(15) . . ?
C2A C1A H1AA 107.8 . . ?
C2A C1A H1AB 107.8 . . ?
C1A C2A H2AA 111.1 . . ?
C1A C2A H2AB 111.1 . . ?
C1A C2A S2A 103.4(13) . . ?
H2AA C2A H2AB 109.0 . . ?
S2A C2A H2AA 111.1 . . ?
S2A C2A H2AB 111.1 . . ?
C4 S2A C2A 103.0(11) . . ?

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
I1 C24 C25 C26 -179.8(2) . . . . ?
Ga1 O3 C22 O4 -169.8(2) . . . . ?
Ga1 O3 C22 C21 9.3(3) . . . . ?
Ga1 O5 C21 O6 -176.7(2) . . . . ?
Ga1 O5 C21 C22 3.8(3) . . . . ?
Ga1 O1 C23 O2 178.7(3) . . . . ?
Ga1 O1 C23 C23 -0.9(4) . . . 2_656 ?
S11 C13 C14 S12 0.4(3) . . . . ?
S11 C13 C14 S10 -179.51(16) . . . . ?
S5 C6 C5 S3 -0.2(3) . . . . ?
S5 C6 C5 S4 178.40(15) . . . . ?
S5 C7 C8 S6 -1.2(3) . . . . ?
S5 C7 C8 S8 175.73(16) . . . . ?
S13 C16 C15 S11 -1.1(3) . . . . ?
S13 C16 C15 S12 179.64(14) . . . . ?
S13 C17 C18 S14 -2.4(3) . . . . ?
S13 C17 C18 S16 174.90(16) . . . . ?
S6 C6 C5 S3 -177.57(15) . . . . ?
S6 C6 C5 S4 1.1(3) . . . . ?
S4 C4 C3 S3 0.5(3) . . . . ?
S4 C4 C3 S1 -177.50(16) . . . . ?
S4 C4 S2A C2A -168.2(9) . . . . ?
S14 C16 C15 S11 179.56(14) . . . . ?
S14 C16 C15 S12 0.3(3) . . . . ?
S7 C7 C8 S6 -176.74(15) . . . . ?
S7 C7 C8 S8 0.2(4) . . . . ?
S7 C9 C10 S8 58.8(9) . . . . ?
S9 C13 C14 S12 -178.00(15) . . . . ?
S9 C13 C14 S10 2.1(4) . . . . ?
S9 C11 C12 S10 -68.2(3) . . . . ?
S1 C1A C2A S2A 78(2) . . . . ?
S15 C17 C18 S14 179.98(16) . . . . ?
S15 C17 C18 S16 -2.7(4) . . . . ?
S15 C19 C20 S16 70.3(3) . . . . ?
S8 C10A C9A S7 -56(3) . . . . ?
S2 C4 C3 S3 -176.1(2) . . . . ?
S2 C4 C3 S1 5.9(4) . . . . ?
S2 C2 C1 S1 -73.4(5) . . . . ?
O5 C21 C22 O3 -8.9(3) . . . . ?
O5 C21 C22 O4 170.3(3) . . . . ?
O6 C21 C22 O3 171.5(3) . . . . ?
O6 C21 C22 O4 -9.3(4) . . . . ?
C6 S5 C7 S7 -179.36(16) . . . . ?
C6 S5 C7 C8 4.7(2) . . . . ?
C6 S6 C8 S8 179.75(16) . . . . ?
C6 S6 C8 C7 -3.0(2) . . . . ?
C5 S3 C3 S1 176.23(16) . . . . ?
C5 S3 C3 C4 -2.0(2) . . . . ?
C5 S4 C4 S2 178.4(2) . . . . ?
C5 S4 C4 C3 1.3(2) . . . . ?
C5 S4 C4 S2A -165.4(5) . . . . ?
C4 S4 C5 S3 -2.66(17) . . . . ?
C4 S4 C5 C6 178.6(2) . . . . ?
C4 S2 C2 C1 54.9(5) . . . . ?
C16 S13 C17 S15 179.08(15) . . . . ?
C16 S13 C17 C18 1.2(2) . . . . ?
C16 S14 C18 S16 -175.41(15) . . . . ?
C16 S14 C18 C17 2.3(2) . . . . ?
C3 S3 C5 S4 2.88(17) . . . . ?
C3 S3 C5 C6 -178.4(2) . . . . ?
C3 S1 C1 C2 47.2(4) . . . . ?
C3 S1 C1A C2A -56.8(13) . . . . ?
C3 C4 S2A C2A 26.8(13) . . . . ?
C7 S5 C6 S6 -6.62(17) . . . . ?
C7 S5 C6 C5 175.9(2) . . . . ?
C7 S7 C9 C10 -66.6(6) . . . . ?
C7 S7 C9A C10A 10.7(19) . . . . ?
C15 S11 C13 S9 178.18(15) . . . . ?
C15 S11 C13 C14 -0.5(2) . . . . ?
C15 S12 C14 S10 179.79(15) . . . . ?
C15 S12 C14 C13 -0.2(2) . . . . ?
C8 S6 C6 S5 6.15(17) . . . . ?
C8 S6 C6 C5 -176.3(2) . . . . ?
C8 S8 C10 C9 -14.7(8) . . . . ?
C8 S8 C10A C9A 65.6(17) . . . . ?
C13 S11 C15 S12 0.34(17) . . . . ?
C13 S11 C15 C16 -179.0(2) . . . . ?
C13 S9 C11 C12 48.1(2) . . . . ?
C14 S12 C15 S11 -0.16(17) . . . . ?
C14 S12 C15 C16 179.2(2) . . . . ?
C14 S10 C12 C11 45.2(2) . . . . ?
C17 S13 C16 S14 0.43(17) . . . . ?
C17 S13 C16 C15 -179.0(2) . . . . ?
C17 S15 C19 C20 -56.8(3) . . . . ?
C18 S14 C16 S13 -1.42(17) . . . . ?
C18 S14 C16 C15 178.0(2) . . . . ?
C18 S16 C20 C19 -39.4(3) . . . . ?
C11 S9 C13 S11 166.05(15) . . . . ?
C11 S9 C13 C14 -15.5(3) . . . . ?
C12 S10 C14 S12 167.05(15) . . . . ?
C12 S10 C14 C13 -13.0(3) . . . . ?
C24 C25 C26 C27 -0.3(5) . . . . ?
C25 C24 C25 C26 0.2(2) 2_556 . . . ?
C25 C26 C27 C26 0.2(2) . . . 2_556 ?
C19 S15 C17 S13 -153.45(18) . . . . ?
C19 S15 C17 C18 24.2(3) . . . . ?
C2 S2 C4 S4 161.1(3) . . . . ?
C2 S2 C4 C3 -22.2(4) . . . . ?
C20 S16 C18 S14 -176.68(17) . . . . ?
C20 S16 C18 C17 5.9(3) . . . . ?
C9 S7 C7 S5 -138.1(2) . . . . ?
C9 S7 C7 C8 37.5(3) . . . . ?
C1 S1 C3 S3 168.5(2) . . . . ?
C1 S1 C3 C4 -13.4(3) . . . . ?
C10 S8 C8 S6 159.8(3) . . . . ?
C10 S8 C8 C7 -17.2(4) . . . . ?
C10A S8 C8 S6 142.1(4) . . . . ?
C10A S8 C8 C7 -34.8(5) . . . . ?
C9A S7 C7 S5 -158.1(8) . . . . ?
C9A S7 C7 C8 17.5(8) . . . . ?
C1A S1 C3 S3 -158.4(6) . . . . ?
C1A S1 C3 C4 19.7(6) . . . . ?
C1A C2A S2A C4 -53(2) . . . . ?
S2A C4 C3 S3 165.0(6) . . . . ?
S2A C4 C3 S1 -13.1(7) . . . . ?

_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
;
_vrf_PLAT910_et4nh4gaox3-phi     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         13 Note  
RESPONSE: Due to reflections being hidden behind large beamstop overlay
;
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2163087'
loop_
_audit_author_name
_audit_author_address
'Toby Blundell'
;Nottingham Trent University
United Kingdom
;
_audit_update_record             
;
2022-03-29 deposited with the CCDC.	2022-04-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Ir O12, 5(C10 H8 S8), C2 H6 O'
_chemical_formula_sum            'C58 H46 Ir O13 S40'
_chemical_formula_weight         2425.56

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'
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'
Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.37840(10)
_cell_length_b                   13.17680(10)
_cell_length_c                   33.6413(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.0750(10)
_cell_angle_gamma                90
_cell_volume                     8126.27(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    26389
_cell_measurement_theta_min      4.0930
_cell_measurement_theta_max      70.2620

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_F_000             4860
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    13.310
_shelx_estimated_absorpt_T_min   0.350
_shelx_estimated_absorpt_T_max   0.556
_exptl_absorpt_correction_T_min  0.63717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.31c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measurement_details      
;
Data collection strategy using shutter-less operation of detector. 
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_radiation_collimation    '0.3 mm, Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_source                   'Rotating anode'
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_source_current           30.0
_diffrn_source_target            Cu
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_number            38584
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         4.132
_diffrn_reflns_theta_max         70.487
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7628
_reflns_number_gt                7466
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
'CrysAlisPro 1.171.39.31c (Rigaku Oxford Diffraction, 2017)'
_computing_cell_refinement       
'CrysAlisPro 1.171.39.31c (Rigaku Oxford Diffraction, 2017)'
_computing_data_reduction        
'CrysAlisPro 1.171.39.31c (Rigaku Oxford Diffraction, 2017)'
_computing_structure_solution    
'SHELXT (G. M. Sheldrick Acta Cryst. (2015). A71, 3-8)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0399P)²+48.0442P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7628
_refine_ls_number_parameters     508
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0824
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Ir01 Ir 0.0000 0.06582(2) 0.7500 0.01944(7) Uani 1 2 d S T P . .
S7 S 0.69440(4) 0.12934(6) 0.50123(2) 0.01684(16) Uani 1 1 d . . . . .
S3 S 0.65109(4) -0.12222(6) 0.58067(2) 0.01661(16) Uani 1 1 d . . . . .
S6 S 0.75044(4) 0.05129(6) 0.58942(2) 0.01690(16) Uani 1 1 d . . . . .
S20 S 0.82822(4) 0.79525(6) 0.54869(2) 0.01652(16) Uani 1 1 d . . . . .
S15 S 0.60339(4) 0.44580(6) 0.48394(2) 0.01735(16) Uani 1 1 d . . . . .
S2 S 0.59272(4) -0.04294(6) 0.49348(2) 0.01694(16) Uani 1 1 d . . . . .
S17 S 0.72657(4) 0.62482(6) 0.53953(2) 0.01722(16) Uani 1 1 d . . . . .
S14 S 0.66251(4) 0.35973(6) 0.56988(2) 0.01649(16) Uani 1 1 d . . . . .
S9 S 0.41605(4) 0.36681(6) 0.40343(2) 0.01797(17) Uani 1 1 d . . . . .
S19 S 0.87969(4) 0.74759(6) 0.63221(2) 0.01739(16) Uani 1 1 d . . . . .
S8 S 0.64610(4) 0.22252(6) 0.42397(2) 0.01843(16) Uani 1 1 d . . . . .
S10 S 0.47910(4) 0.30605(7) 0.48271(2) 0.01983(17) Uani 1 1 d . . . . .
S1 S 0.52202(4) 0.01795(6) 0.41665(2) 0.01946(17) Uani 1 1 d . . . . .
S13 S 0.72753(4) 0.28767(6) 0.64919(2) 0.01926(17) Uani 1 1 d . . . . .
S4 S 0.67737(5) -0.19311(6) 0.66415(2) 0.02015(17) Uani 1 1 d . . . . .
S18 S 0.75635(5) 0.54297(7) 0.62015(2) 0.02084(17) Uani 1 1 d . . . . .
S11 S 0.53488(4) 0.22594(7) 0.57062(2) 0.02024(17) Uani 1 1 d . . . . .
S16 S 0.57036(5) 0.52403(7) 0.40311(2) 0.02384(19) Uani 1 1 d . . . . .
S12 S 0.57987(5) 0.13183(7) 0.64865(2) 0.02450(19) Uani 1 1 d . . . . .
S5 S 0.80508(5) 0.00760(7) 0.67126(3) 0.0284(2) Uani 1 1 d . . . . .
O1 O -0.04394(13) 0.1807(2) 0.71478(7) 0.0247(5) Uani 1 1 d . . . . .
O5 O -0.03835(14) -0.05139(19) 0.71522(7) 0.0236(5) Uani 1 1 d . . . . .
O2 O -0.10260(14) 0.06724(19) 0.77073(7) 0.0240(5) Uani 1 1 d . . . . .
O3 O -0.20764(14) 0.1488(2) 0.76193(8) 0.0293(6) Uani 1 1 d . . . . .
O4 O -0.14216(14) 0.2805(2) 0.71086(7) 0.0263(5) Uani 1 1 d . . . . .
O6 O -0.0393(2) -0.2195(2) 0.71335(10) 0.0525(10) Uani 1 1 d . . . . .
C22 C 0.82289(17) 0.7161(2) 0.59016(9) 0.0151(6) Uani 1 1 d . . . . .
C13 C 0.48634(17) 0.3818(2) 0.44057(9) 0.0153(6) Uani 1 1 d . . . . .
C5 C 0.65967(17) 0.0211(2) 0.52276(9) 0.0150(6) Uani 1 1 d . . . . .
C17 C 0.65837(18) 0.2788(3) 0.61088(9) 0.0173(7) Uani 1 1 d . . . . .
C6 C 0.68387(17) -0.0122(2) 0.55998(9) 0.0139(6) Uani 1 1 d . . . . .
C8 C 0.69863(17) -0.1070(3) 0.62725(9) 0.0169(6) Uani 1 1 d . . . . .
C3 C 0.58881(17) 0.0453(2) 0.45462(9) 0.0151(6) Uani 1 1 d . . . . .
C25 C 0.88175(18) 0.6271(3) 0.65830(10) 0.0189(7) Uani 1 1 d . . . . .
H25A H 0.9082 0.5771 0.6427 0.023 Uiso 1 1 calc R U . . .
H25B H 0.9095 0.6356 0.6844 0.023 Uiso 1 1 calc R U . . .
C18 C 0.59973(18) 0.2173(3) 0.61157(9) 0.0174(7) Uani 1 1 d . . . . .
C4 C 0.63556(17) 0.1244(2) 0.45786(9) 0.0141(6) Uani 1 1 d . . . . .
C16 C 0.58306(17) 0.3144(3) 0.54493(9) 0.0166(6) Uani 1 1 d . . . . .
C23 C 0.77541(17) 0.6372(3) 0.58603(9) 0.0167(6) Uani 1 1 d . . . . .
C14 C 0.54438(18) 0.4450(2) 0.44096(9) 0.0164(6) Uani 1 1 d . . . . .
C7 C 0.74612(18) -0.0282(3) 0.63076(9) 0.0178(7) Uani 1 1 d . . . . .
C21 C 0.76191(18) 0.7328(3) 0.51865(9) 0.0161(6) Uani 1 1 d . . . . .
C15 C 0.55860(17) 0.3499(3) 0.50794(9) 0.0162(6) Uani 1 1 d . . . . .
C12 C 0.4563(2) 0.4239(3) 0.36127(10) 0.0226(7) Uani 1 1 d . . . . .
H12A H 0.4952 0.3787 0.3526 0.027 Uiso 1 1 calc R U . . .
H12B H 0.4185 0.4300 0.3389 0.027 Uiso 1 1 calc R U . . .
C1 C 0.60128(18) 0.1664(3) 0.37946(10) 0.0208(7) Uani 1 1 d . . . . .
H1A H 0.5991 0.2171 0.3577 0.025 Uiso 1 1 calc R U . . .
H1B H 0.6307 0.1082 0.3711 0.025 Uiso 1 1 calc R U . . .
C10 C 0.7890(2) -0.0898(3) 0.70732(10) 0.0233(7) Uani 1 1 d . . . . .
H10A H 0.8183 -0.1503 0.7015 0.028 Uiso 1 1 calc R U . . .
H10B H 0.8061 -0.0651 0.7342 0.028 Uiso 1 1 calc R U . . .
C24 C 0.80711(18) 0.5849(3) 0.66525(10) 0.0196(7) Uani 1 1 d . . . . .
H24A H 0.7786 0.6379 0.6781 0.024 Uiso 1 1 calc R U . . .
H24B H 0.8129 0.5270 0.6839 0.024 Uiso 1 1 calc R U . . .
C26 C -0.10840(19) 0.2067(3) 0.72435(10) 0.0221(7) Uani 1 1 d . . . . .
C11 C 0.48840(19) 0.5277(3) 0.37053(10) 0.0217(7) Uani 1 1 d . . . . .
H11A H 0.4516 0.5696 0.3830 0.026 Uiso 1 1 calc R U . . .
H11B H 0.4993 0.5610 0.3452 0.026 Uiso 1 1 calc R U . . .
C2 C 0.52447(18) 0.1300(3) 0.38566(10) 0.0215(7) Uani 1 1 d . . . . .
H2A H 0.4991 0.1152 0.3594 0.026 Uiso 1 1 calc R U . . .
H2B H 0.4975 0.1853 0.3981 0.026 Uiso 1 1 calc R U . . .
C27 C -0.1433(2) 0.1359(3) 0.75497(10) 0.0230(7) Uani 1 1 d . . . . .
C20 C 0.6703(2) 0.2768(3) 0.69077(10) 0.0258(8) Uani 1 1 d . . . . .
H20A H 0.7008 0.2881 0.7158 0.031 Uiso 1 1 calc R U . . .
H20B H 0.6330 0.3310 0.6885 0.031 Uiso 1 1 calc R U . . .
C28 C -0.0223(2) -0.1404(3) 0.72971(11) 0.0286(8) Uani 1 1 d . . . . .
C9 C 0.7099(2) -0.1207(3) 0.70787(10) 0.0234(7) Uani 1 1 d . . . . .
H9A H 0.6796 -0.0590 0.7096 0.028 Uiso 1 1 calc R U . . .
H9B H 0.7037 -0.1620 0.7320 0.028 Uiso 1 1 calc R U . . .
C19 C 0.6325(2) 0.1765(3) 0.69332(11) 0.0310(9) Uani 1 1 d . . . . .
H19A H 0.5993 0.1804 0.7152 0.037 Uiso 1 1 calc R U . . .
H19B H 0.6699 0.1246 0.7010 0.037 Uiso 1 1 calc R U . . .
C30 C 0.4904(5) 0.0642(8) 0.2733(3) 0.026(2) Uiso 0.5 1 d D U P A -1
H30A H 0.4730 0.1347 0.2764 0.031 Uiso 0.5 1 calc R U P A -1
H30B H 0.4536 0.0179 0.2835 0.031 Uiso 0.5 1 calc R U P A -1
C29 C 0.4977(8) 0.0426(12) 0.2298(4) 0.057(4) Uiso 0.5 1 d D U P A -1
H29A H 0.4504 0.0521 0.2149 0.086 Uiso 0.5 1 calc R U P A -1
H29B H 0.5335 0.0891 0.2195 0.086 Uiso 0.5 1 calc R U P A -1
H29C H 0.5140 -0.0276 0.2266 0.086 Uiso 0.5 1 calc R U P A -1
O7 O 0.5557(3) 0.0517(5) 0.29526(19) 0.0423(15) Uiso 0.5 1 d D U P A -1
H7 H 0.588(6) 0.119(9) 0.290(3) 0.06(3) Uiso 0.5 1 d . . P B -1


_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
Ir01 O5 2.033(2) . ?
Ir01 O5 2.033(2) 2_556 ?
Ir01 O1 2.052(3) . ?
Ir01 O1 2.053(3) 2_556 ?
Ir01 O2 2.056(3) 2_556 ?
Ir01 O2 2.057(2) . ?
S7 C5 1.741(3) . ?
S7 C4 1.755(3) . ?
S3 C6 1.734(3) . ?
S3 C8 1.751(3) . ?
S6 C6 1.734(3) . ?
S6 C7 1.747(3) . ?
S20 C21 1.734(3) . ?
S20 C22 1.750(3) . ?
S15 C15 1.738(3) . ?
S15 C14 1.745(3) . ?
S2 C5 1.739(3) . ?
S2 C3 1.748(3) . ?
S17 C21 1.734(3) . ?
S17 C23 1.755(3) . ?
S14 C16 1.738(3) . ?
S14 C17 1.750(3) . ?
S9 C13 1.743(3) . ?
S9 C12 1.809(3) . ?
S19 C22 1.747(3) . ?
S19 C25 1.814(3) . ?
S8 C4 1.744(3) . ?
S8 C1 1.815(3) . ?
S10 C15 1.736(3) . ?
S10 C13 1.746(3) . ?
S1 C3 1.745(3) . ?
S1 C2 1.810(4) . ?
S13 C17 1.749(3) . ?
S13 C20 1.815(4) . ?
S4 C8 1.747(3) . ?
S4 C9 1.818(4) . ?
S18 C23 1.744(3) . ?
S18 C24 1.810(3) . ?
S11 C16 1.732(3) . ?
S11 C18 1.760(3) . ?
S16 C14 1.738(3) . ?
S16 C11 1.799(3) . ?
S12 C18 1.738(3) . ?
S12 C19 1.826(4) . ?
S5 C7 1.744(3) . ?
S5 C10 1.805(4) . ?
O1 C26 1.296(4) . ?
O5 C28 1.296(5) . ?
O2 C27 1.266(5) . ?
O3 C27 1.233(4) . ?
O4 C26 1.224(4) . ?
O6 C28 1.209(5) . ?
C22 C23 1.358(5) . ?
C13 C14 1.353(5) . ?
C5 C6 1.371(4) . ?
C17 C18 1.350(5) . ?
C8 C7 1.356(5) . ?
C3 C4 1.350(5) . ?
C25 C24 1.513(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C16 C15 1.375(5) . ?
C21 C21 1.376(6) 7_666 ?
C12 C11 1.513(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C1 C2 1.519(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C10 C9 1.510(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 C27 1.561(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C20 C19 1.498(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C28 C28 1.542(7) 2_556 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C30 O7 1.375(10) . ?
C30 C29 1.508(11) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O7 H7 1.09(12) . ?

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
O5 Ir01 O5 81.15(14) . 2_556 ?
O5 Ir01 O1 97.01(10) . . ?
O5 Ir01 O1 177.04(10) 2_556 . ?
O5 Ir01 O1 177.04(10) . 2_556 ?
O5 Ir01 O1 97.01(10) 2_556 2_556 ?
O1 Ir01 O1 84.93(14) . 2_556 ?
O5 Ir01 O2 95.76(10) . 2_556 ?
O5 Ir01 O2 85.03(10) 2_556 2_556 ?
O1 Ir01 O2 97.48(10) . 2_556 ?
O1 Ir01 O2 81.75(10) 2_556 2_556 ?
O5 Ir01 O2 85.03(10) . . ?
O5 Ir01 O2 95.77(10) 2_556 . ?
O1 Ir01 O2 81.74(10) . . ?
O1 Ir01 O2 97.48(10) 2_556 . ?
O2 Ir01 O2 178.95(14) 2_556 . ?
C5 S7 C4 95.32(15) . . ?
C6 S3 C8 95.61(15) . . ?
C6 S6 C7 95.47(15) . . ?
C21 S20 C22 96.04(15) . . ?
C15 S15 C14 95.38(15) . . ?
C5 S2 C3 95.20(16) . . ?
C21 S17 C23 95.85(16) . . ?
C16 S14 C17 95.12(16) . . ?
C13 S9 C12 101.03(16) . . ?
C22 S19 C25 100.07(15) . . ?
C4 S8 C1 99.91(16) . . ?
C15 S10 C13 95.55(16) . . ?
C3 S1 C2 101.99(16) . . ?
C17 S13 C20 97.59(16) . . ?
C8 S4 C9 99.00(16) . . ?
C23 S18 C24 102.62(16) . . ?
C16 S11 C18 95.31(15) . . ?
C14 S16 C11 101.58(16) . . ?
C18 S12 C19 104.82(17) . . ?
C7 S5 C10 102.15(16) . . ?
C26 O1 Ir01 112.4(2) . . ?
C28 O5 Ir01 114.2(2) . . ?
C27 O2 Ir01 113.2(2) . . ?
C23 C22 S19 127.4(3) . . ?
C23 C22 S20 116.5(2) . . ?
S19 C22 S20 116.11(18) . . ?
C14 C13 S9 128.3(3) . . ?
C14 C13 S10 116.7(2) . . ?
S9 C13 S10 114.96(18) . . ?
C6 C5 S2 122.2(3) . . ?
C6 C5 S7 122.5(2) . . ?
S2 C5 S7 115.30(18) . . ?
C18 C17 S13 124.5(3) . . ?
C18 C17 S14 117.3(2) . . ?
S13 C17 S14 118.05(19) . . ?
C5 C6 S6 122.5(2) . . ?
C5 C6 S3 122.3(2) . . ?
S6 C6 S3 115.17(18) . . ?
C7 C8 S4 127.7(3) . . ?
C7 C8 S3 116.3(2) . . ?
S4 C8 S3 116.03(19) . . ?
C4 C3 S1 129.0(3) . . ?
C4 C3 S2 117.5(2) . . ?
S1 C3 S2 113.54(19) . . ?
C24 C25 S19 114.1(2) . . ?
C24 C25 H25A 108.7 . . ?
S19 C25 H25A 108.7 . . ?
C24 C25 H25B 108.7 . . ?
S19 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
C17 C18 S12 127.6(3) . . ?
C17 C18 S11 116.4(2) . . ?
S12 C18 S11 116.01(19) . . ?
C3 C4 S8 128.2(2) . . ?
C3 C4 S7 116.6(2) . . ?
S8 C4 S7 115.18(18) . . ?
C15 C16 S11 122.4(3) . . ?
C15 C16 S14 122.0(3) . . ?
S11 C16 S14 115.60(18) . . ?
C22 C23 S18 129.5(3) . . ?
C22 C23 S17 116.5(2) . . ?
S18 C23 S17 113.98(19) . . ?
C13 C14 S16 128.3(3) . . ?
C13 C14 S15 117.0(2) . . ?
S16 C14 S15 114.64(19) . . ?
C8 C7 S5 129.4(3) . . ?
C8 C7 S6 117.1(2) . . ?
S5 C7 S6 113.52(19) . . ?
C21 C21 S17 122.4(3) 7_666 . ?
C21 C21 S20 122.7(3) 7_666 . ?
S17 C21 S20 114.91(18) . . ?
C16 C15 S10 122.6(3) . . ?
C16 C15 S15 122.2(3) . . ?
S10 C15 S15 115.15(18) . . ?
C11 C12 S9 112.9(2) . . ?
C11 C12 H12A 109.0 . . ?
S9 C12 H12A 109.0 . . ?
C11 C12 H12B 109.0 . . ?
S9 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C2 C1 S8 112.8(2) . . ?
C2 C1 H1A 109.0 . . ?
S8 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
S8 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C9 C10 S5 113.8(2) . . ?
C9 C10 H10A 108.8 . . ?
S5 C10 H10A 108.8 . . ?
C9 C10 H10B 108.8 . . ?
S5 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C25 C24 S18 113.7(2) . . ?
C25 C24 H24A 108.8 . . ?
S18 C24 H24A 108.8 . . ?
C25 C24 H24B 108.8 . . ?
S18 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
O4 C26 O1 124.5(3) . . ?
O4 C26 C27 119.9(3) . . ?
O1 C26 C27 115.6(3) . . ?
C12 C11 S16 113.5(2) . . ?
C12 C11 H11A 108.9 . . ?
S16 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
S16 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C1 C2 S1 113.4(2) . . ?
C1 C2 H2A 108.9 . . ?
S1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
S1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
O3 C27 O2 124.4(3) . . ?
O3 C27 C26 119.2(3) . . ?
O2 C27 C26 116.4(3) . . ?
C19 C20 S13 114.2(3) . . ?
C19 C20 H20A 108.7 . . ?
S13 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
S13 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
O6 C28 O5 124.3(3) . . ?
O6 C28 C28 120.5(2) . 2_556 ?
O5 C28 C28 115.19(19) . 2_556 ?
C10 C9 S4 113.2(2) . . ?
C10 C9 H9A 108.9 . . ?
S4 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
S4 C9 H9B 108.9 . . ?
H9A C9 H9B 107.8 . . ?
C20 C19 S12 117.2(3) . . ?
C20 C19 H19A 108.0 . . ?
S12 C19 H19A 108.0 . . ?
C20 C19 H19B 108.0 . . ?
S12 C19 H19B 108.0 . . ?
H19A C19 H19B 107.2 . . ?
O7 C30 C29 111.4(9) . . ?
O7 C30 H30A 109.4 . . ?
C29 C30 H30A 109.4 . . ?
O7 C30 H30B 109.4 . . ?
C29 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 O7 H7 107(6) . . ?

_refine_diff_density_max         3.714
_refine_diff_density_min         -1.522
_refine_diff_density_rms         0.105

####################################################################### 
# 
# 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_et4h3ogaox3-phbr3
_database_code_depnum_ccdc_archive 'CCDC 2163084'
loop_
_audit_author_name
_audit_author_address
'Toby Blundell'
;Nottingham Trent University
United Kingdom
;
_audit_update_record             
;
2022-03-29 deposited with the CCDC.	2022-04-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_et4h3ogaox3-phbr3   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note
RESPONSE: Due to reflections being hidden behind large beamstop overlay
;
# Added during the CSD deposition process: Tuesday 29 March 2022 03:41 PM
# end Validation Reply Form

_audit_creation_date             2022-01-27
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ga O12, C6 H5 Br, 4(C10 H8 S8), 0.5(H6 O2)'
_chemical_formula_sum            'C52 H40 Br Ga O13 S32'
_chemical_formula_weight         2048.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H40 Ga Br O13 S32'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   10.2760(2)
_cell_length_b                   19.9386(5)
_cell_length_c                   35.4579(8)
_cell_angle_alpha                90
_cell_angle_beta                 93.377(2)
_cell_angle_gamma                90
_cell_volume                     7252.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19529
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      29.0040
_cell_measurement_theta_min      3.5270
_shelx_estimated_absorpt_T_max   0.679
_shelx_estimated_absorpt_T_min   0.503
_exptl_absorpt_coefficient_mu    1.912
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.609
_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 black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4136
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
12 -12 10 0.1006
-1 17 -39 0.0871
2 27 10 0.0675
-1 -27 -12 0.1394
-1 7 -48 0.0829
-13 4 -18 0.1767
-2 -7 48 0.1341
-11 -16 16 0.2415
-11 9 30 0.2310

_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.219
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
12.4904 -12.3148 10.0814 -0.7793 -0.1446 0.6097
-1.3452 17.1730 -38.9700 0.9280 0.1721 0.3303
1.7264 27.2616 10.3836 0.2324 0.9686 0.0882
-0.9362 -27.2109 -12.0077 -0.2332 -0.9721 -0.0263
-0.6752 7.2716 -48.0081 0.8809 -0.2113 0.4235
-13.0372 4.1370 -17.7777 0.7810 -0.1874 -0.5957
-1.9730 -7.0085 48.2477 -0.7910 0.1897 -0.5817
-11.3692 -15.7194 15.6764 -0.1174 -0.4893 -0.8642
-11.1449 8.6213 30.2151 0.0535 0.4069 -0.9119

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            39761
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.436
_diffrn_reflns_theta_min         2.893
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00   1.00   0.50   16.00    --  -16.16 -57.00-150.00  168
  2  ω    -83.00   3.00   0.50   16.00    --  -16.16 -63.00 136.47  172
  3  ω    -50.00  36.00   0.50   16.00    --   16.24 -65.00 -36.50  172
  4  ω    -51.00  33.00   0.50   16.00    --   16.24 -57.00  90.00  168
  5  ω     -3.00  85.00   0.50   16.00    --   16.24  37.00   0.00  176
  6  ω    -52.00  32.00   0.50   16.00    --   16.24 -44.00-172.72  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0337039000
_diffrn_orient_matrix_UB_12      0.0165134000
_diffrn_orient_matrix_UB_13      -0.0153738000
_diffrn_orient_matrix_UB_21      0.0120780000
_diffrn_orient_matrix_UB_22      0.0313460000
_diffrn_orient_matrix_UB_23      0.0089789000
_diffrn_orient_matrix_UB_31      0.0591887000
_diffrn_orient_matrix_UB_32      0.0029904000
_diffrn_orient_matrix_UB_33      -0.0092014000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7402
_reflns_number_total             8976
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8976
_refine_ls_number_restraints     367
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0425
_refine_ls_restrained_S_all      2.908
_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)+(0.0443P)²+12.0299P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1057
_refine_special_details          
'Positional disorder was found for 2 terminal ethyl groups on the BEDT-TTF molecule (C11, C12 and C19 C20). The disorder was modelled, and the occupancy of the major and minor components competitively refined to 71:29 (C11, C12) and 71:29 (C19, C20) respectively Relevant 1,2- bond distances were restrained to be approximately equal. Oxygen-hydrogen 1,2- and hydrogen-hydrogen 1,3 distances for O1W were restrained to be approximately equal.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 S2-C2A \\sim S2-C2B
 with sigma of 0.02
 H-HA \\sim H-HB \\sim HA-HB
 with sigma of 0.001
 S7-C9B \\sim S7-C9A
 with sigma of 0.02
 S8-C10A \\sim S8-C10B
 with sigma of 0.02
 S1-C1A \\sim S1-C1B
 with sigma of 0.02
 C10A-C9A \\sim C10B-C9B
 with sigma of 0.02
 C2A-C1A \\sim C2B-C1B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(1)
 Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C10B)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(2)
 Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=FVAR(2)
 Fixed Sof: H(0.5) HA(0.5) HB(0.5)
5.a Free rotating group:
 O1W(H,HA,HB)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C20(H20A,H20B), C19(H19A,H19B), C2B(H2BA,
 H2BB), C9B(H9BA,H9BB), C10B(H10A,H10B), C1B(H1BA,H1BB), C10A(H10C,H10D),
 C9A(H9AA,H9AB), C1A(H1AA,H1AB), C2A(H2AA,H2AB)
5.c Aromatic/amide H refined with riding coordinates:
 C25(HG), C26(HT), C27(HU)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Ga1 Ga 0.000000 0.58287(2) 0.250000 0.03078(10) Uani 1 2 d S T P . .
Br1 Br -0.500000 0.85450(3) 0.250000 0.0896(2) Uani 1 2 d S T P . .
S5 S 0.11811(6) 0.54209(4) 0.53623(2) 0.03573(16) Uani 1 1 d . . . . .
S11 S -0.16600(6) 0.64353(4) 0.46870(2) 0.03571(16) Uani 1 1 d . . . . .
S3 S 0.23988(6) 0.51202(4) 0.45579(2) 0.03603(16) Uani 1 1 d . . . . .
S13 S -0.27883(6) 0.67367(4) 0.54921(2) 0.03701(16) Uani 1 1 d . . . . .
S4 S 0.47415(6) 0.58825(4) 0.48014(2) 0.03777(17) Uani 1 1 d . . . . .
S6 S 0.35499(6) 0.61697(4) 0.55995(2) 0.03746(17) Uani 1 1 d . . . . .
S12 S 0.07677(7) 0.71371(4) 0.49145(2) 0.03830(16) Uani 1 1 d . . . . .
S14 S -0.03868(7) 0.74518(4) 0.57294(2) 0.03830(16) Uani 1 1 d . . . . .
S7 S -0.01624(7) 0.57199(4) 0.60589(2) 0.03988(17) Uani 1 1 d D . . . .
S9 S -0.09176(7) 0.61144(4) 0.39174(2) 0.04112(17) Uani 1 1 d . . . . .
S10 S 0.20157(7) 0.69313(4) 0.42034(2) 0.04443(18) Uani 1 1 d . . . . .
S1 S 0.32358(7) 0.48391(4) 0.37904(2) 0.04405(19) Uani 1 1 d D . . . .
S8 S 0.26097(8) 0.65736(4) 0.63384(2) 0.0492(2) Uani 1 1 d D . . . .
S15 S -0.40500(8) 0.69265(4) 0.62071(2) 0.04690(19) Uani 1 1 d . . . . .
S2 S 0.60503(8) 0.57172(5) 0.40992(2) 0.0546(2) Uani 1 1 d D . . . .
S16 S -0.11209(9) 0.77233(5) 0.64991(2) 0.0542(2) Uani 1 1 d . . . . .
O3 O 0.14706(19) 0.57066(10) 0.21724(5) 0.0383(4) Uani 1 1 d . . . . .
O5 O 0.09804(18) 0.51769(10) 0.28226(5) 0.0371(4) Uani 1 1 d . . . . .
O1 O -0.0757(2) 0.65720(10) 0.21925(5) 0.0422(5) Uani 1 1 d . . . . .
O6 O 0.2810(2) 0.45745(12) 0.28392(6) 0.0511(5) Uani 1 1 d . . . . .
O4 O 0.3168(2) 0.50250(13) 0.21152(6) 0.0531(6) Uani 1 1 d . . . . .
O2 O -0.0848(2) 0.76878(12) 0.21804(7) 0.0596(6) Uani 1 1 d . . . . .
O1W O 0.500000 0.40183(19) 0.250000 0.0772(12) Uani 1 2 d GS T P . .
H H 0.499368 0.360716 0.241320 0.093 Uiso 0.5 1 d DG U P A -1
HA H 0.565666 0.430303 0.250668 0.093 Uiso 0.5 1 d DG U P B -1
HB H 0.444319 0.418031 0.263311 0.093 Uiso 0.5 1 d DG U P C -1
C6 C 0.2698(2) 0.57196(13) 0.52455(7) 0.0305(5) Uani 1 1 d . . . . .
C4 C 0.4677(2) 0.55480(14) 0.43463(7) 0.0330(6) Uani 1 1 d . . . . .
C7 C 0.1198(2) 0.58316(13) 0.57968(7) 0.0309(5) Uani 1 1 d . . . . .
C5 C 0.3206(2) 0.55939(14) 0.49078(7) 0.0305(5) Uani 1 1 d . . . . .
C8 C 0.2291(3) 0.61670(14) 0.59090(7) 0.0324(5) Uani 1 1 d . . . . .
C3 C 0.3604(2) 0.52025(14) 0.42320(7) 0.0320(5) Uani 1 1 d . . . . .
C15 C -0.0765(2) 0.68776(13) 0.50360(7) 0.0308(5) Uani 1 1 d . . . . .
C16 C -0.1249(2) 0.70085(13) 0.53766(7) 0.0308(5) Uani 1 1 d . . . . .
C14 C 0.0640(3) 0.68021(14) 0.44585(7) 0.0329(5) Uani 1 1 d . . . . .
C22 C 0.2267(3) 0.52493(15) 0.22868(8) 0.0360(6) Uani 1 1 d . . . . .
C13 C -0.0476(2) 0.64791(13) 0.43535(7) 0.0309(5) Uani 1 1 d . . . . .
C18 C -0.1587(3) 0.73876(14) 0.60577(7) 0.0342(6) Uani 1 1 d . . . . .
C21 C -0.0463(3) 0.71574(15) 0.23191(8) 0.0400(6) Uani 1 1 d . . . . .
C23 C 0.2029(3) 0.49648(14) 0.26852(8) 0.0352(6) Uani 1 1 d . . . . .
C17 C -0.2694(3) 0.70719(14) 0.59461(7) 0.0343(6) Uani 1 1 d . . . . .
C11 C 0.0635(3) 0.60624(15) 0.37100(8) 0.0399(6) Uani 1 1 d . . . . .
H11A H 0.114414 0.571044 0.383678 0.048 Uiso 1 1 calc R U . . .
H11B H 0.049082 0.593402 0.344698 0.048 Uiso 1 1 calc R U . . .
C12 C 0.1415(3) 0.67027(16) 0.37301(8) 0.0420(7) Uani 1 1 d . . . . .
H12A H 0.087515 0.706470 0.362612 0.050 Uiso 1 1 calc R U . . .
H12B H 0.215188 0.665522 0.357324 0.050 Uiso 1 1 calc R U . . .
C24 C -0.500000 0.7597(2) 0.250000 0.0495(11) Uani 1 2 d S T P . .
C25 C -0.4056(4) 0.7265(2) 0.23106(10) 0.0589(9) Uani 1 1 d . . . . .
HG H -0.343156 0.749967 0.218441 0.071 Uiso 1 1 calc R U . . .
C20 C -0.2577(4) 0.7609(2) 0.67542(9) 0.0631(10) Uani 1 1 d . . . . .
H20A H -0.234264 0.763281 0.702292 0.076 Uiso 1 1 calc R U . . .
H20B H -0.317183 0.797561 0.669216 0.076 Uiso 1 1 calc R U . . .
C19 C -0.3276(4) 0.6957(2) 0.66723(10) 0.0612(10) Uani 1 1 d . . . . .
H19A H -0.392890 0.689279 0.685572 0.073 Uiso 1 1 calc R U . . .
H19B H -0.265574 0.659127 0.670138 0.073 Uiso 1 1 calc R U . . .
C2B C 0.5402(7) 0.5548(3) 0.36226(17) 0.0459(16) Uani 0.709(10) 1 d D . P D 1
H2BA H 0.476853 0.589225 0.354969 0.055 Uiso 0.709(10) 1 calc R U P D 1
H2BB H 0.610556 0.557878 0.345263 0.055 Uiso 0.709(10) 1 calc R U P D 1
C9B C 0.0751(7) 0.5624(3) 0.65194(12) 0.0432(15) Uani 0.710(14) 1 d D . P E 1
H9BA H 0.014974 0.549655 0.670786 0.052 Uiso 0.710(14) 1 calc R U P E 1
H9BB H 0.138050 0.526465 0.650165 0.052 Uiso 0.710(14) 1 calc R U P E 1
C10B C 0.1452(7) 0.6253(4) 0.66463(16) 0.0456(16) Uani 0.710(14) 1 d D . P E 1
H10A H 0.189793 0.616734 0.689030 0.055 Uiso 0.710(14) 1 calc R U P E 1
H10B H 0.080662 0.659872 0.668239 0.055 Uiso 0.710(14) 1 calc R U P E 1
C1B C 0.4762(4) 0.4871(3) 0.35745(12) 0.0380(13) Uani 0.709(10) 1 d D . P D 1
H1BA H 0.533792 0.453023 0.368626 0.046 Uiso 0.709(10) 1 calc R U P D 1
H1BB H 0.462403 0.477240 0.330726 0.046 Uiso 0.709(10) 1 calc R U P D 1
C26 C -0.4067(4) 0.6575(2) 0.23144(14) 0.0795(13) Uani 1 1 d . . . . .
HT H -0.343826 0.633915 0.219043 0.095 Uiso 1 1 calc R U . . .
C27 C -0.500000 0.6228(3) 0.250000 0.093(2) Uani 1 2 d S T P . .
HU H -0.500001 0.576125 0.249999 0.112 Uiso 1 2 calc R U P . .
C10A C 0.1710(12) 0.5968(9) 0.6607(5) 0.052(4) Uani 0.290(14) 1 d D . P E 2
H10C H 0.206287 0.552646 0.656071 0.062 Uiso 0.290(14) 1 calc R U P E 2
H10D H 0.188073 0.606516 0.687291 0.062 Uiso 0.290(14) 1 calc R U P E 2
C9A C 0.0256(13) 0.5936(10) 0.6529(3) 0.048(4) Uani 0.290(14) 1 d D . P E 2
H9AA H -0.012153 0.636874 0.658330 0.058 Uiso 0.290(14) 1 calc R U P E 2
H9AB H -0.010621 0.560723 0.669487 0.058 Uiso 0.290(14) 1 calc R U P E 2
C1A C 0.4382(11) 0.5335(8) 0.3532(3) 0.051(4) Uani 0.291(10) 1 d D . P D 2
H1AA H 0.430690 0.518999 0.327090 0.061 Uiso 0.291(10) 1 calc R U P D 2
H1AB H 0.409232 0.579805 0.353670 0.061 Uiso 0.291(10) 1 calc R U P D 2
C2A C 0.5791(12) 0.5327(10) 0.3657(4) 0.049(5) Uani 0.291(10) 1 d D . P D 2
H2AA H 0.628621 0.555835 0.347174 0.059 Uiso 0.291(10) 1 calc R U P D 2
H2AB H 0.609665 0.486653 0.367292 0.059 Uiso 0.291(10) 1 calc R U P D 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
Ga1 O3 1.9746(18) . ?
Ga1 O3 1.9747(18) 2 ?
Ga1 O5 1.9688(19) 2 ?
Ga1 O5 1.9689(19) . ?
Ga1 O1 1.972(2) 2 ?
Ga1 O1 1.9724(19) . ?
Br1 C24 1.889(5) . ?
S5 C6 1.741(3) . ?
S5 C7 1.744(3) . ?
S11 C15 1.738(3) . ?
S11 C13 1.748(3) . ?
S3 C5 1.731(3) . ?
S3 C3 1.751(3) . ?
S13 C16 1.743(3) . ?
S13 C17 1.741(3) . ?
S4 C4 1.744(3) . ?
S4 C5 1.742(3) . ?
S6 C6 1.737(3) . ?
S6 C8 1.745(3) . ?
S12 C15 1.736(3) . ?
S12 C14 1.747(3) . ?
S14 C16 1.732(3) . ?
S14 C18 1.750(3) . ?
S7 C7 1.738(3) . ?
S7 C9B 1.845(5) . ?
S7 C9A 1.750(10) . ?
S9 C13 1.745(3) . ?
S9 C11 1.798(3) . ?
S10 C14 1.742(3) . ?
S10 C12 1.812(3) . ?
S1 C3 1.746(3) . ?
S1 C1B 1.787(4) . ?
S1 C1A 1.825(10) . ?
S8 C8 1.739(3) . ?
S8 C10B 1.780(5) . ?
S8 C10A 1.822(13) . ?
S15 C17 1.742(3) . ?
S15 C19 1.790(4) . ?
S2 C4 1.737(3) . ?
S2 C2B 1.811(6) . ?
S2 C2A 1.758(12) . ?
S16 C18 1.743(3) . ?
S16 C20 1.808(4) . ?
O3 C22 1.275(3) . ?
O5 C23 1.280(3) . ?
O1 C21 1.280(3) . ?
O6 C23 1.224(3) . ?
O4 C22 1.223(3) . ?
O2 C21 1.222(3) . ?
O1W H 0.8754 . ?
O1W HA 0.8811 . ?
O1W HB 0.8285 . ?
C6 C5 1.357(4) . ?
C4 C3 1.342(4) . ?
C7 C8 1.347(4) . ?
C15 C16 1.358(4) . ?
C14 C13 1.348(4) . ?
C22 C23 1.555(4) . ?
C18 C17 1.339(4) . ?
C21 C21 1.551(6) 2 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.507(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C24 C25 1.382(4) . ?
C24 C25 1.382(4) 2_455 ?
C25 HG 0.9300 . ?
C25 C26 1.376(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C19 1.505(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C2B H2BA 0.9700 . ?
C2B H2BB 0.9700 . ?
C2B C1B 1.508(7) . ?
C9B H9BA 0.9700 . ?
C9B H9BB 0.9700 . ?
C9B C10B 1.503(7) . ?
C10B H10A 0.9700 . ?
C10B H10B 0.9700 . ?
C1B H1BA 0.9700 . ?
C1B H1BB 0.9700 . ?
C26 HT 0.9300 . ?
C26 C27 1.380(6) . ?
C27 HU 0.9300 . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C10A C9A 1.504(14) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C1A C2A 1.489(14) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

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
O3 Ga1 O3 165.84(12) . 2 ?
O5 Ga1 O3 87.71(8) . 2 ?
O5 Ga1 O3 87.71(8) 2 . ?
O5 Ga1 O3 82.95(8) 2 2 ?
O5 Ga1 O3 82.95(8) . . ?
O5 Ga1 O5 97.40(12) 2 . ?
O5 Ga1 O1 171.39(9) . . ?
O5 Ga1 O1 90.18(8) 2 . ?
O5 Ga1 O1 171.39(8) 2 2 ?
O5 Ga1 O1 90.18(8) . 2 ?
O1 Ga1 O3 93.32(8) 2 2 ?
O1 Ga1 O3 97.31(8) 2 . ?
O1 Ga1 O3 97.31(8) . 2 ?
O1 Ga1 O3 93.32(8) . . ?
O1 Ga1 O1 82.57(12) 2 . ?
C6 S5 C7 94.98(12) . . ?
C15 S11 C13 95.52(12) . . ?
C5 S3 C3 95.40(12) . . ?
C17 S13 C16 95.50(13) . . ?
C5 S4 C4 95.08(12) . . ?
C6 S6 C8 95.30(12) . . ?
C15 S12 C14 95.50(12) . . ?
C16 S14 C18 95.31(13) . . ?
C7 S7 C9B 95.9(2) . . ?
C7 S7 C9A 108.5(4) . . ?
C13 S9 C11 101.30(13) . . ?
C14 S10 C12 101.61(13) . . ?
C3 S1 C1B 102.70(16) . . ?
C3 S1 C1A 96.4(4) . . ?
C8 S8 C10B 105.8(2) . . ?
C8 S8 C10A 94.2(7) . . ?
C17 S15 C19 99.09(15) . . ?
C4 S2 C2B 99.8(2) . . ?
C4 S2 C2A 106.2(6) . . ?
C18 S16 C20 102.08(15) . . ?
C22 O3 Ga1 113.57(17) . . ?
C23 O5 Ga1 114.21(17) . . ?
C21 O1 Ga1 114.45(18) . . ?
H O1W HA 127.1 . . ?
H O1W HB 125.1 . . ?
HA O1W HB 106.7 . . ?
S6 C6 S5 115.14(14) . . ?
C5 C6 S5 122.9(2) . . ?
C5 C6 S6 122.0(2) . . ?
S2 C4 S4 113.88(15) . . ?
C3 C4 S4 117.5(2) . . ?
C3 C4 S2 128.6(2) . . ?
S7 C7 S5 116.45(15) . . ?
C8 C7 S5 117.3(2) . . ?
C8 C7 S7 126.1(2) . . ?
S3 C5 S4 115.28(14) . . ?
C6 C5 S3 122.7(2) . . ?
C6 C5 S4 122.0(2) . . ?
S8 C8 S6 116.17(15) . . ?
C7 C8 S6 116.9(2) . . ?
C7 C8 S8 126.9(2) . . ?
S1 C3 S3 115.36(15) . . ?
C4 C3 S3 116.7(2) . . ?
C4 C3 S1 127.9(2) . . ?
S12 C15 S11 115.10(14) . . ?
C16 C15 S11 121.6(2) . . ?
C16 C15 S12 123.3(2) . . ?
S14 C16 S13 114.94(15) . . ?
C15 C16 S13 122.3(2) . . ?
C15 C16 S14 122.8(2) . . ?
S10 C14 S12 113.89(15) . . ?
C13 C14 S12 117.0(2) . . ?
C13 C14 S10 129.1(2) . . ?
O3 C22 C23 114.7(2) . . ?
O4 C22 O3 126.4(3) . . ?
O4 C22 C23 118.9(3) . . ?
S9 C13 S11 115.08(15) . . ?
C14 C13 S11 116.8(2) . . ?
C14 C13 S9 128.0(2) . . ?
S16 C18 S14 113.73(15) . . ?
C17 C18 S14 117.2(2) . . ?
C17 C18 S16 129.0(2) . . ?
O1 C21 C21 114.24(16) . 2 ?
O2 C21 O1 125.7(3) . . ?
O2 C21 C21 120.05(19) . 2 ?
O5 C23 C22 114.0(2) . . ?
O6 C23 O5 125.8(3) . . ?
O6 C23 C22 120.2(2) . . ?
S13 C17 S15 115.13(16) . . ?
C18 C17 S13 117.0(2) . . ?
C18 C17 S15 127.8(2) . . ?
S9 C11 H11A 108.6 . . ?
S9 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 S9 114.5(2) . . ?
C12 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
S10 C12 H12A 108.7 . . ?
S10 C12 H12B 108.7 . . ?
C11 C12 S10 114.1(2) . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C25 C24 Br1 118.7(3) 2_455 . ?
C25 C24 Br1 118.7(3) . . ?
C25 C24 C25 122.6(5) 2_455 . ?
C24 C25 HG 121.0 . . ?
C26 C25 C24 118.0(4) . . ?
C26 C25 HG 121.0 . . ?
S16 C20 H20A 108.7 . . ?
S16 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C19 C20 S16 114.3(2) . . ?
C19 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
S15 C19 H19A 109.0 . . ?
S15 C19 H19B 109.0 . . ?
C20 C19 S15 112.9(2) . . ?
C20 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
S2 C2B H2BA 108.8 . . ?
S2 C2B H2BB 108.8 . . ?
H2BA C2B H2BB 107.7 . . ?
C1B C2B S2 114.0(4) . . ?
C1B C2B H2BA 108.8 . . ?
C1B C2B H2BB 108.8 . . ?
S7 C9B H9BA 109.0 . . ?
S7 C9B H9BB 109.0 . . ?
H9BA C9B H9BB 107.8 . . ?
C10B C9B S7 112.9(5) . . ?
C10B C9B H9BA 109.0 . . ?
C10B C9B H9BB 109.0 . . ?
S8 C10B H10A 108.2 . . ?
S8 C10B H10B 108.2 . . ?
C9B C10B S8 116.2(4) . . ?
C9B C10B H10A 108.2 . . ?
C9B C10B H10B 108.2 . . ?
H10A C10B H10B 107.4 . . ?
S1 C1B H1BA 109.3 . . ?
S1 C1B H1BB 109.3 . . ?
C2B C1B S1 111.8(4) . . ?
C2B C1B H1BA 109.3 . . ?
C2B C1B H1BB 109.3 . . ?
H1BA C1B H1BB 107.9 . . ?
C25 C26 HT 119.6 . . ?
C25 C26 C27 120.8(5) . . ?
C27 C26 HT 119.6 . . ?
C26 C27 C26 119.8(6) . 2_455 ?
C26 C27 HU 120.1 2_455 . ?
C26 C27 HU 120.1 . . ?
S8 C10A H10C 107.9 . . ?
S8 C10A H10D 107.9 . . ?
H10C C10A H10D 107.2 . . ?
C9A C10A S8 117.5(10) . . ?
C9A C10A H10C 107.9 . . ?
C9A C10A H10D 107.9 . . ?
S7 C9A H9AA 109.3 . . ?
S7 C9A H9AB 109.3 . . ?
C10A C9A S7 111.7(12) . . ?
C10A C9A H9AA 109.3 . . ?
C10A C9A H9AB 109.3 . . ?
H9AA C9A H9AB 107.9 . . ?
S1 C1A H1AA 107.5 . . ?
S1 C1A H1AB 107.5 . . ?
H1AA C1A H1AB 107.0 . . ?
C2A C1A S1 119.4(12) . . ?
C2A C1A H1AA 107.5 . . ?
C2A C1A H1AB 107.5 . . ?
S2 C2A H2AA 109.5 . . ?
S2 C2A H2AB 109.5 . . ?
C1A C2A S2 110.6(9) . . ?
C1A C2A H2AA 109.5 . . ?
C1A C2A H2AB 109.5 . . ?
H2AA C2A H2AB 108.1 . . ?

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
Ga1 O3 C22 O4 171.3(2) . . . . ?
Ga1 O3 C22 C23 -8.7(3) . . . . ?
Ga1 O5 C23 O6 177.8(2) . . . . ?
Ga1 O5 C23 C22 -2.2(3) . . . . ?
Ga1 O1 C21 O2 -178.0(2) . . . . ?
Ga1 O1 C21 C21 1.9(4) . . . 2 ?
Br1 C24 C25 C26 179.8(2) . . . . ?
S5 C6 C5 S3 -0.2(4) . . . . ?
S5 C6 C5 S4 -178.54(15) . . . . ?
S5 C7 C8 S6 1.7(3) . . . . ?
S5 C7 C8 S8 -175.75(17) . . . . ?
S11 C15 C16 S13 0.8(3) . . . . ?
S11 C15 C16 S14 -179.63(15) . . . . ?
S4 C4 C3 S3 -0.7(3) . . . . ?
S4 C4 C3 S1 177.42(17) . . . . ?
S6 C6 C5 S3 177.54(15) . . . . ?
S6 C6 C5 S4 -0.8(4) . . . . ?
S12 C15 C16 S13 -179.56(15) . . . . ?
S12 C15 C16 S14 0.0(4) . . . . ?
S12 C14 C13 S11 0.0(3) . . . . ?
S12 C14 C13 S9 178.00(16) . . . . ?
S14 C18 C17 S13 2.1(3) . . . . ?
S14 C18 C17 S15 179.66(16) . . . . ?
S7 C7 C8 S6 176.94(16) . . . . ?
S7 C7 C8 S8 -0.5(4) . . . . ?
S7 C9B C10B S8 -58.8(9) . . . . ?
S9 C11 C12 S10 68.8(3) . . . . ?
S10 C14 C13 S11 179.23(17) . . . . ?
S10 C14 C13 S9 -2.8(4) . . . . ?
S1 C1A C2A S2 -67.5(18) . . . . ?
S8 C10A C9A S7 61(2) . . . . ?
S2 C4 C3 S3 179.42(18) . . . . ?
S2 C4 C3 S1 -2.4(4) . . . . ?
S2 C2B C1B S1 72.1(6) . . . . ?
S16 C18 C17 S13 -174.87(17) . . . . ?
S16 C18 C17 S15 2.7(4) . . . . ?
S16 C20 C19 S15 -70.5(3) . . . . ?
O3 C22 C23 O5 7.5(3) . . . . ?
O3 C22 C23 O6 -172.5(3) . . . . ?
O4 C22 C23 O5 -172.6(3) . . . . ?
O4 C22 C23 O6 7.5(4) . . . . ?
C6 S5 C7 S7 179.45(16) . . . . ?
C6 S5 C7 C8 -4.8(2) . . . . ?
C6 S6 C8 S8 -179.87(17) . . . . ?
C6 S6 C8 C7 2.4(2) . . . . ?
C4 S4 C5 S3 2.32(18) . . . . ?
C4 S4 C5 C6 -179.2(2) . . . . ?
C4 S2 C2B C1B -52.6(5) . . . . ?
C4 S2 C2A C1A 33.2(16) . . . . ?
C7 S5 C6 S6 6.35(18) . . . . ?
C7 S5 C6 C5 -175.8(2) . . . . ?
C7 S7 C9B C10B 65.9(6) . . . . ?
C7 S7 C9A C10A -16.1(16) . . . . ?
C5 S3 C3 S1 -176.38(16) . . . . ?
C5 S3 C3 C4 2.0(3) . . . . ?
C5 S4 C4 S2 178.92(17) . . . . ?
C5 S4 C4 C3 -0.9(3) . . . . ?
C8 S6 C6 S5 -5.68(18) . . . . ?
C8 S6 C6 C5 176.4(2) . . . . ?
C8 S8 C10B C9B 15.0(8) . . . . ?
C8 S8 C10A C9A -66.9(17) . . . . ?
C3 S3 C5 S4 -2.62(18) . . . . ?
C3 S3 C5 C6 178.9(2) . . . . ?
C3 S1 C1B C2B -46.4(4) . . . . ?
C3 S1 C1A C2A 57.0(12) . . . . ?
C15 S11 C13 S9 -177.94(15) . . . . ?
C15 S11 C13 C14 0.3(2) . . . . ?
C15 S12 C14 S10 -179.66(16) . . . . ?
C15 S12 C14 C13 -0.3(2) . . . . ?
C16 S13 C17 S15 -179.02(16) . . . . ?
C16 S13 C17 C18 -1.2(2) . . . . ?
C16 S14 C18 S16 175.56(16) . . . . ?
C16 S14 C18 C17 -1.9(2) . . . . ?
C14 S12 C15 S11 0.53(18) . . . . ?
C14 S12 C15 C16 -179.2(2) . . . . ?
C14 S10 C12 C11 -45.3(2) . . . . ?
C13 S11 C15 S12 -0.53(17) . . . . ?
C13 S11 C15 C16 179.2(2) . . . . ?
C13 S9 C11 C12 -49.0(2) . . . . ?
C18 S14 C16 S13 1.03(18) . . . . ?
C18 S14 C16 C15 -178.6(2) . . . . ?
C18 S16 C20 C19 38.9(3) . . . . ?
C17 S13 C16 S14 -0.16(18) . . . . ?
C17 S13 C16 C15 179.5(2) . . . . ?
C17 S15 C19 C20 57.4(3) . . . . ?
C11 S9 C13 S11 -165.57(16) . . . . ?
C11 S9 C13 C14 16.4(3) . . . . ?
C12 S10 C14 S12 -167.61(16) . . . . ?
C12 S10 C14 C13 13.2(3) . . . . ?
C24 C25 C26 C27 0.4(5) . . . . ?
C25 C24 C25 C26 -0.2(2) 2_455 . . . ?
C25 C26 C27 C26 -0.2(2) . . . 2_455 ?
C20 S16 C18 S14 177.59(18) . . . . ?
C20 S16 C18 C17 -5.3(3) . . . . ?
C19 S15 C17 S13 152.93(19) . . . . ?
C19 S15 C17 C18 -24.6(3) . . . . ?
C2B S2 C4 S4 -162.1(3) . . . . ?
C2B S2 C4 C3 17.7(4) . . . . ?
C9B S7 C7 S5 138.4(2) . . . . ?
C9B S7 C7 C8 -37.0(3) . . . . ?
C10B S8 C8 S6 -160.5(3) . . . . ?
C10B S8 C8 C7 17.0(4) . . . . ?
C1B S1 C3 S3 -168.9(2) . . . . ?
C1B S1 C3 C4 12.9(3) . . . . ?
C10A S8 C8 S6 -143.1(5) . . . . ?
C10A S8 C8 C7 34.3(5) . . . . ?
C9A S7 C7 S5 161.4(7) . . . . ?
C9A S7 C7 C8 -13.9(7) . . . . ?
C1A S1 C3 S3 158.6(5) . . . . ?
C1A S1 C3 C4 -19.5(5) . . . . ?
C2A S2 C4 S4 179.1(7) . . . . ?
C2A S2 C4 C3 -1.1(7) . . . . ?

_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 1.171
_oxdiff_exptl_absorpt_empirical_full_min 0.755
####################################################################### 
# 
# 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_ekr_4_01_b
_database_code_depnum_ccdc_archive 'CCDC 2163088'
loop_
_audit_author_name
_audit_author_address
'Toby Blundell'
;Nottingham Trent University
United Kingdom
;
_audit_update_record             
;
2022-03-29 deposited with the CCDC.	2022-04-25 downloaded from the CCDC.
;
_audit_creation_date             2022-03-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ir O12, 5(C10 H8 S8), C2 H6 O'
_chemical_formula_sum            'C58 H46 Ir O13 S40'
_chemical_formula_weight         2425.55
_chemical_melting_point          ?
_chemical_oxdiff_formula         C56IrO16S40H20
_chemical_oxdiff_usercomment     'Balck block'
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'
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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.4349(2)
_cell_length_b                   13.18390(10)
_cell_length_c                   33.6063(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.1340(10)
_cell_angle_gamma                90
_cell_volume                     8146.55(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8989
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      71.8890
_cell_measurement_theta_min      4.2970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.277
_exptl_absorpt_correction_T_max  0.441
_exptl_absorpt_correction_T_min  0.182
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4860
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 7 8 0.0311
10 -4 -8 0.0568
-2 -8 0 0.0558
-3 2 -20 0.1013
0 -2 21 0.0509
10 3 -11 0.0653
-10 -3 12 0.0720
-12 -2 2 0.0984
7 -1 17 0.0751
3 8 -2 0.0433
3 -8 1 0.0476

_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.103
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
-5.9605 6.8978 7.7010 0.7233 0.6182 -0.3077
10.0059 -3.9014 -7.9635 -0.4810 -0.5072 0.7151
-2.4742 -8.3638 -0.0570 -0.8385 -0.3475 -0.4198
-2.6978 1.5526 -20.4790 0.5583 -0.8119 -0.1707
0.0689 -2.0100 21.1455 -0.5658 0.8227 -0.0554
10.1965 2.5521 -10.7254 0.2466 -0.3585 0.9004
-9.6828 -2.6170 12.2107 -0.2884 0.4192 -0.8609
-11.6488 -1.9612 2.2641 -0.0146 0.0211 -0.9997
6.8129 -0.5979 16.9383 -0.4798 0.6978 0.5318
2.5371 8.3295 -2.0149 0.8679 0.2573 0.4248
3.3679 -8.1746 1.3102 -0.9570 -0.2838 0.0598

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            15759
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.026
_diffrn_reflns_theta_min         4.126
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     16.00  43.00   1.00    5.00    --   36.58 -99.00 -30.00   27
  2  ω     22.00  96.00   1.00    5.00    --   36.58  57.00 120.00   74
  3  ω     47.00  88.00   1.00    5.00    --   36.58-125.00-150.00   41
  4  ω      1.00  38.00   1.00    5.00    --   36.58 -57.00-120.00   37
  5  ω     32.00 106.00   1.00    5.00    --   36.58  37.00   0.00   74
  6  ω    -33.00  49.00   1.00    5.00    --   36.58 -37.00-180.00   82
  7  ω     94.00 175.00   1.00   20.00    --  108.00  61.00 150.00   81
  8  ω    120.00 175.00   1.00   20.00    --  108.00  45.00 -90.00   55
  9  ω     41.00 122.00   1.00   20.00    --  108.00 -61.00   0.00   81
 10  ω     49.00 123.00   1.00   20.00    --  108.00 -61.00-120.00   74
 11  ω    100.00 167.00   1.00   20.00    --  108.00  61.00  60.00   67
 12  ω     44.00  80.00   1.00   20.00    --  108.00 -94.00   0.00   36
 13  ω     44.00 102.00   1.00   20.00    --  108.00 -94.00-150.00   58
 14  ω     40.00  97.00   1.00   20.00    --  108.00 -77.00 120.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0198544000
_diffrn_orient_matrix_UB_12      0.1062340000
_diffrn_orient_matrix_UB_13      -0.0165928000
_diffrn_orient_matrix_UB_21      -0.0004543000
_diffrn_orient_matrix_UB_22      0.0413931000
_diffrn_orient_matrix_UB_23      0.0428431000
_diffrn_orient_matrix_UB_31      0.0813399000
_diffrn_orient_matrix_UB_32      0.0261317000
_diffrn_orient_matrix_UB_33      -0.0003999000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7137
_reflns_number_total             7803
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.282
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         7803
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0350
_refine_ls_restrained_S_all      1.038
_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)+(0.0578P)²+2.2454P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0899
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
O7 \\sim H7 \\sim C30 \\sim C29 \\sim H30A \\sim H30B \\sim H29A \\sim H29B
\\sim H29C: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Rigid body (RIGU) restrains
 O7, C29, H29A, H29B, H29C, C30, H30A, H30B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O7(0.5) H7(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5)
 H30A(0.5) H30B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C19(H19A,H19B), C20(H20A,H20B), C24(H24A,H24B), C25(H25A,H25B),
  C30(H30A,H30B)
5.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C)
5.c Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_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 1.000000 0.06504(2) 0.750000 0.02248(7) Uani 1 2 d S T P . .
O1 O 0.95583(13) 0.17977(19) 0.71496(7) 0.0271(5) Uani 1 1 d . . . . .
O2 O 0.89869(13) 0.06709(19) 0.77104(7) 0.0253(5) Uani 1 1 d . . . . .
O3 O 0.79375(15) 0.1492(2) 0.76243(8) 0.0362(6) Uani 1 1 d . . . . .
O4 O 0.85823(14) 0.2796(2) 0.71095(7) 0.0312(5) Uani 1 1 d . . . . .
O5 O 0.96103(14) -0.05190(19) 0.71538(7) 0.0275(5) Uani 1 1 d . . . . .
O6 O 0.9589(2) -0.2198(2) 0.71396(11) 0.0640(11) Uani 1 1 d . . . . .
C26 C 0.89146(19) 0.2067(3) 0.72441(9) 0.0257(7) Uani 1 1 d . . . . .
C27 C 0.85714(19) 0.1355(3) 0.75535(9) 0.0260(7) Uani 1 1 d . . . . .
C28 C 0.9768(2) -0.1404(3) 0.72977(10) 0.0325(8) Uani 1 1 d . . . . .
S1 S 0.52251(4) 0.01840(6) 0.41652(2) 0.02507(16) Uani 1 1 d . . . . .
S2 S 0.59268(4) -0.04225(6) 0.49347(2) 0.02281(16) Uani 1 1 d . . . . .
S3 S 0.65063(4) -0.12112(6) 0.58076(2) 0.02163(15) Uani 1 1 d . . . . .
S4 S 0.67716(5) -0.19208(6) 0.66417(2) 0.02527(16) Uani 1 1 d . . . . .
S5 S 0.80498(5) 0.00741(7) 0.67118(2) 0.0342(2) Uani 1 1 d . . . . .
S6 S 0.75018(4) 0.05150(6) 0.58938(2) 0.02208(16) Uani 1 1 d . . . . .
S7 S 0.69447(4) 0.12920(6) 0.50112(2) 0.02226(15) Uani 1 1 d . . . . .
S8 S 0.64653(4) 0.22207(6) 0.42379(2) 0.02414(16) Uani 1 1 d . . . . .
C1 C 0.60163(19) 0.1664(3) 0.37941(9) 0.0281(7) Uani 1 1 d . . . . .
H1A H 0.599540 0.217313 0.357704 0.034 Uiso 1 1 calc R U . . .
H1B H 0.630963 0.108422 0.370931 0.034 Uiso 1 1 calc R U . . .
C2 C 0.52511(18) 0.1298(3) 0.38525(10) 0.0261(7) Uani 1 1 d . . . . .
H2A H 0.500280 0.114322 0.358840 0.031 Uiso 1 1 calc R U . . .
H2B H 0.497811 0.185097 0.397359 0.031 Uiso 1 1 calc R U . . .
C3 C 0.58905(17) 0.0459(2) 0.45448(9) 0.0194(6) Uani 1 1 d . . . . .
C4 C 0.63576(17) 0.1240(2) 0.45779(9) 0.0192(6) Uani 1 1 d . . . . .
C5 C 0.65997(17) 0.0217(2) 0.52284(9) 0.0206(6) Uani 1 1 d . . . . .
C6 C 0.68382(17) -0.0115(2) 0.55980(9) 0.0205(6) Uani 1 1 d . . . . .
C7 C 0.74589(18) -0.0281(2) 0.63095(9) 0.0218(6) Uani 1 1 d . . . . .
C8 C 0.69848(17) -0.1059(2) 0.62710(9) 0.0205(6) Uani 1 1 d . . . . .
C9 C 0.7098(2) -0.1200(3) 0.70780(10) 0.0276(7) Uani 1 1 d . . . . .
H9A H 0.679836 -0.058021 0.709491 0.033 Uiso 1 1 calc R U . . .
H9B H 0.703489 -0.161043 0.731968 0.033 Uiso 1 1 calc R U . . .
C10 C 0.7885(2) -0.0898(3) 0.70728(10) 0.0269(7) Uani 1 1 d . . . . .
H10A H 0.817465 -0.150518 0.701461 0.032 Uiso 1 1 calc R U . . .
H10B H 0.805724 -0.065145 0.734153 0.032 Uiso 1 1 calc R U . . .
S9 S 0.41666(4) 0.36639(6) 0.40355(2) 0.02353(16) Uani 1 1 d . . . . .
S10 S 0.47926(4) 0.30596(6) 0.48294(2) 0.02525(17) Uani 1 1 d . . . . .
S11 S 0.53487(4) 0.22601(6) 0.57085(2) 0.02571(17) Uani 1 1 d . . . . .
S12 S 0.57971(5) 0.13244(7) 0.64900(2) 0.03230(19) Uani 1 1 d . . . . .
S13 S 0.72690(4) 0.28781(6) 0.64945(2) 0.02460(16) Uani 1 1 d . . . . .
S14 S 0.66201(4) 0.35945(6) 0.57015(2) 0.02135(15) Uani 1 1 d . . . . .
S15 S 0.60325(4) 0.44516(6) 0.48410(2) 0.02201(16) Uani 1 1 d . . . . .
S16 S 0.57033(5) 0.52324(7) 0.40325(2) 0.03054(19) Uani 1 1 d . . . . .
C11 C 0.48897(19) 0.5264(3) 0.37054(10) 0.0278(7) Uani 1 1 d . . . . .
H11A H 0.452226 0.568537 0.382907 0.033 Uiso 1 1 calc R U . . .
H11B H 0.499981 0.559377 0.345201 0.033 Uiso 1 1 calc R U . . .
C12 C 0.4569(2) 0.4227(3) 0.36139(10) 0.0295(7) Uani 1 1 d . . . . .
H12A H 0.495632 0.377310 0.352823 0.035 Uiso 1 1 calc R U . . .
H12B H 0.419311 0.428560 0.338937 0.035 Uiso 1 1 calc R U . . .
C13 C 0.48641(17) 0.3811(2) 0.44064(8) 0.0191(6) Uani 1 1 d . . . . .
C14 C 0.54407(17) 0.4444(2) 0.44095(9) 0.0192(6) Uani 1 1 d . . . . .
C15 C 0.55861(17) 0.3497(2) 0.50834(9) 0.0198(6) Uani 1 1 d . . . . .
C16 C 0.58294(17) 0.3140(2) 0.54495(9) 0.0207(6) Uani 1 1 d . . . . .
C17 C 0.65760(17) 0.2792(3) 0.61137(9) 0.0212(6) Uani 1 1 d . . . . .
C18 C 0.59958(17) 0.2177(2) 0.61182(9) 0.0218(6) Uani 1 1 d . . . . .
C19 C 0.6325(2) 0.1767(3) 0.69352(11) 0.0400(9) Uani 1 1 d . . . . .
H19A H 0.599530 0.180609 0.715454 0.048 Uiso 1 1 calc R U . . .
H19B H 0.669683 0.124652 0.701083 0.048 Uiso 1 1 calc R U . . .
C20 C 0.6702(2) 0.2762(3) 0.69116(10) 0.0349(8) Uani 1 1 d . . . . .
H20A H 0.700799 0.286947 0.716228 0.042 Uiso 1 1 calc R U . . .
H20B H 0.633098 0.330651 0.689167 0.042 Uiso 1 1 calc R U . . .
S17 S 0.77353(4) -0.12519(6) 0.46044(2) 0.02222(15) Uani 1 1 d . . . . .
S18 S 0.74402(5) -0.04380(6) 0.37976(2) 0.02674(17) Uani 1 1 d . . . . .
S19 S 0.62094(4) -0.24773(6) 0.36771(2) 0.02203(15) Uani 1 1 d . . . . .
S20 S 0.67210(4) -0.29520(6) 0.45129(2) 0.02166(15) Uani 1 1 d . . . . .
C21 C 0.73849(18) -0.2329(2) 0.48127(9) 0.0206(6) Uani 1 1 d . . . . .
C22 C 0.67767(17) -0.2164(2) 0.40964(8) 0.0191(6) Uani 1 1 d . . . . .
C23 C 0.72484(17) -0.1377(2) 0.41394(9) 0.0202(6) Uani 1 1 d . . . . .
C24 C 0.69338(18) -0.0862(3) 0.33471(9) 0.0235(6) Uani 1 1 d . . . . .
H24A H 0.687870 -0.028706 0.315793 0.028 Uiso 1 1 calc R U . . .
H24B H 0.721572 -0.139786 0.322105 0.028 Uiso 1 1 calc R U . . .
C25 C 0.61896(18) -0.1272(2) 0.34182(9) 0.0225(6) Uani 1 1 d . . . . .
H25A H 0.590834 -0.135214 0.315782 0.027 Uiso 1 1 calc R U . . .
H25B H 0.593190 -0.077070 0.357596 0.027 Uiso 1 1 calc R U . . .
O7 O 0.4429(5) -0.0505(5) 0.7055(2) 0.0587(19) Uani 0.5 1 d . U P A -1
H7 H 0.419219 -0.104856 0.705746 0.088 Uiso 0.5 1 calc R U P A -1
C29 C 0.5016(18) -0.0375(19) 0.7685(7) 0.093(8) Uani 0.5 1 d . U P A -1
H29A H 0.550671 -0.034949 0.781801 0.139 Uiso 0.5 1 calc R U P A -1
H29B H 0.473117 -0.089716 0.781094 0.139 Uiso 0.5 1 calc R U P A -1
H29C H 0.477964 0.028529 0.770857 0.139 Uiso 0.5 1 calc R U P A -1
C30 C 0.5062(11) -0.0620(11) 0.7266(6) 0.037(2) Uani 0.5 1 d . U P A -1
H30A H 0.542996 -0.017710 0.715359 0.044 Uiso 0.5 1 calc R U P A -1
H30B H 0.522660 -0.133138 0.724223 0.044 Uiso 0.5 1 calc R U P A -1


_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 O1 2.049(2) . ?
Ir1 O1 2.049(2) 2_756 ?
Ir1 O2 2.044(2) . ?
Ir1 O2 2.044(2) 2_756 ?
Ir1 O5 2.031(2) . ?
Ir1 O5 2.031(2) 2_756 ?
O1 C26 1.300(4) . ?
O2 C27 1.273(5) . ?
O3 C27 1.223(5) . ?
O4 C26 1.211(4) . ?
O5 C28 1.288(4) . ?
O6 C28 1.209(5) . ?
C26 C27 1.567(5) . ?
C28 C28 1.553(6) 2_756 ?
S1 C2 1.808(3) . ?
S1 C3 1.743(3) . ?
S2 C3 1.749(3) . ?
S2 C5 1.745(3) . ?
S3 C6 1.738(3) . ?
S3 C8 1.745(3) . ?
S4 C8 1.751(3) . ?
S4 C9 1.814(3) . ?
S5 C7 1.738(3) . ?
S5 C10 1.805(3) . ?
S6 C6 1.732(3) . ?
S6 C7 1.754(3) . ?
S7 C4 1.752(3) . ?
S7 C5 1.736(3) . ?
S8 C1 1.808(3) . ?
S8 C4 1.747(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.517(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.342(5) . ?
C5 C6 1.360(4) . ?
C7 C8 1.347(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.506(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
S9 C12 1.805(3) . ?
S9 C13 1.736(3) . ?
S10 C13 1.746(3) . ?
S10 C15 1.738(3) . ?
S11 C16 1.732(3) . ?
S11 C18 1.759(3) . ?
S12 C18 1.739(3) . ?
S12 C19 1.821(4) . ?
S13 C17 1.746(3) . ?
S13 C20 1.815(4) . ?
S14 C16 1.738(3) . ?
S14 C17 1.750(3) . ?
S15 C14 1.751(3) . ?
S15 C15 1.739(3) . ?
S16 C11 1.795(3) . ?
S16 C14 1.734(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.513(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.351(5) . ?
C15 C16 1.362(4) . ?
C17 C18 1.343(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.489(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
S17 C21 1.729(3) . ?
S17 C23 1.753(3) . ?
S18 C23 1.742(3) . ?
S18 C24 1.809(3) . ?
S19 C22 1.743(3) . ?
S19 C25 1.811(3) . ?
S20 C21 1.735(3) . ?
S20 C22 1.752(3) . ?
C21 C21 1.375(6) 7_646 ?
C22 C23 1.355(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.510(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
O7 H7 0.8400 . ?
O7 C30 1.33(2) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C29 C30 1.453(16) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?

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
O1 Ir1 O1 84.86(14) . 2_756 ?
O2 Ir1 O1 97.27(9) . 2_756 ?
O2 Ir1 O1 81.60(10) 2_756 2_756 ?
O2 Ir1 O1 81.60(9) . . ?
O2 Ir1 O1 97.27(9) 2_756 . ?
O2 Ir1 O2 178.48(14) . 2_756 ?
O5 Ir1 O1 96.99(10) . . ?
O5 Ir1 O1 177.23(10) 2_756 . ?
O5 Ir1 O1 177.23(10) . 2_756 ?
O5 Ir1 O1 96.98(10) 2_756 2_756 ?
O5 Ir1 O2 85.07(10) 2_756 2_756 ?
O5 Ir1 O2 96.09(10) . 2_756 ?
O5 Ir1 O2 96.09(10) 2_756 . ?
O5 Ir1 O2 85.06(10) . . ?
O5 Ir1 O5 81.25(14) . 2_756 ?
C26 O1 Ir1 113.1(2) . . ?
C27 O2 Ir1 113.8(2) . . ?
C28 O5 Ir1 114.3(2) . . ?
O1 C26 C27 114.7(3) . . ?
O4 C26 O1 124.9(3) . . ?
O4 C26 C27 120.4(3) . . ?
O2 C27 C26 116.1(3) . . ?
O3 C27 O2 125.4(3) . . ?
O3 C27 C26 118.6(3) . . ?
O5 C28 C28 115.07(18) . 2_756 ?
O6 C28 O5 124.9(3) . . ?
O6 C28 C28 120.0(2) . 2_756 ?
C3 S1 C2 102.11(15) . . ?
C5 S2 C3 95.18(15) . . ?
C6 S3 C8 95.51(15) . . ?
C8 S4 C9 99.00(15) . . ?
C7 S5 C10 101.83(16) . . ?
C6 S6 C7 95.70(15) . . ?
C5 S7 C4 95.40(15) . . ?
C4 S8 C1 99.91(16) . . ?
S8 C1 H1A 108.9 . . ?
S8 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C2 C1 S8 113.4(2) . . ?
C2 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
S1 C2 H2A 108.9 . . ?
S1 C2 H2B 108.9 . . ?
C1 C2 S1 113.4(2) . . ?
C1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
S1 C3 S2 113.40(17) . . ?
C4 C3 S1 129.3(2) . . ?
C4 C3 S2 117.2(2) . . ?
S8 C4 S7 114.96(18) . . ?
C3 C4 S7 117.0(2) . . ?
C3 C4 S8 128.1(2) . . ?
S7 C5 S2 115.06(17) . . ?
C6 C5 S2 122.1(2) . . ?
C6 C5 S7 122.9(3) . . ?
S6 C6 S3 114.90(18) . . ?
C5 C6 S3 122.5(3) . . ?
C5 C6 S6 122.6(2) . . ?
S5 C7 S6 113.35(18) . . ?
C8 C7 S5 130.2(2) . . ?
C8 C7 S6 116.4(2) . . ?
S3 C8 S4 115.79(18) . . ?
C7 C8 S3 117.1(2) . . ?
C7 C8 S4 127.1(2) . . ?
S4 C9 H9A 108.9 . . ?
S4 C9 H9B 108.9 . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 S4 113.2(2) . . ?
C10 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
S5 C10 H10A 108.8 . . ?
S5 C10 H10B 108.8 . . ?
C9 C10 S5 113.9(2) . . ?
C9 C10 H10A 108.8 . . ?
C9 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C13 S9 C12 101.10(16) . . ?
C15 S10 C13 95.83(15) . . ?
C16 S11 C18 95.30(15) . . ?
C18 S12 C19 104.79(17) . . ?
C17 S13 C20 97.39(16) . . ?
C16 S14 C17 95.28(15) . . ?
C15 S15 C14 95.52(15) . . ?
C14 S16 C11 101.33(15) . . ?
S16 C11 H11A 108.8 . . ?
S16 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C12 C11 S16 113.6(2) . . ?
C12 C11 H11A 108.8 . . ?
C12 C11 H11B 108.8 . . ?
S9 C12 H12A 109.0 . . ?
S9 C12 H12B 109.0 . . ?
C11 C12 S9 112.9(2) . . ?
C11 C12 H12A 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
S9 C13 S10 115.21(18) . . ?
C14 C13 S9 128.0(2) . . ?
C14 C13 S10 116.7(2) . . ?
S16 C14 S15 114.30(18) . . ?
C13 C14 S15 116.9(2) . . ?
C13 C14 S16 128.7(2) . . ?
S10 C15 S15 114.84(17) . . ?
C16 C15 S10 122.7(2) . . ?
C16 C15 S15 122.5(2) . . ?
S11 C16 S14 115.30(18) . . ?
C15 C16 S11 122.5(2) . . ?
C15 C16 S14 122.1(2) . . ?
S13 C17 S14 117.87(18) . . ?
C18 C17 S13 124.9(2) . . ?
C18 C17 S14 117.2(2) . . ?
S12 C18 S11 115.89(18) . . ?
C17 C18 S11 116.7(2) . . ?
C17 C18 S12 127.4(2) . . ?
S12 C19 H19A 107.9 . . ?
S12 C19 H19B 107.9 . . ?
H19A C19 H19B 107.2 . . ?
C20 C19 S12 117.5(3) . . ?
C20 C19 H19A 107.9 . . ?
C20 C19 H19B 107.9 . . ?
S13 C20 H20A 108.7 . . ?
S13 C20 H20B 108.7 . . ?
C19 C20 S13 114.4(3) . . ?
C19 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C21 S17 C23 95.83(15) . . ?
C23 S18 C24 102.43(15) . . ?
C22 S19 C25 99.84(15) . . ?
C21 S20 C22 95.97(15) . . ?
S17 C21 S20 114.98(18) . . ?
C21 C21 S17 122.7(3) 7_646 . ?
C21 C21 S20 122.3(3) 7_646 . ?
S19 C22 S20 116.06(18) . . ?
C23 C22 S19 127.6(2) . . ?
C23 C22 S20 116.3(2) . . ?
S18 C23 S17 113.95(18) . . ?
C22 C23 S17 116.8(2) . . ?
C22 C23 S18 129.3(2) . . ?
S18 C24 H24A 108.9 . . ?
S18 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C25 C24 S18 113.5(2) . . ?
C25 C24 H24A 108.9 . . ?
C25 C24 H24B 108.9 . . ?
S19 C25 H25A 108.8 . . ?
S19 C25 H25B 108.8 . . ?
C24 C25 S19 113.8(2) . . ?
C24 C25 H25A 108.8 . . ?
C24 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C30 O7 H7 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
O7 C30 C29 112.4(11) . . ?
O7 C30 H30A 109.1 . . ?
O7 C30 H30B 109.1 . . ?
C29 C30 H30A 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?

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 O1 C26 O4 171.5(3) . . . . ?
Ir1 O1 C26 C27 -9.1(3) . . . . ?
Ir1 O2 C27 O3 177.8(3) . . . . ?
Ir1 O2 C27 C26 -1.9(3) . . . . ?
Ir1 O5 C28 O6 179.9(4) . . . . ?
Ir1 O5 C28 C28 -0.8(5) . . . 2_756 ?
O1 C26 C27 O2 7.7(4) . . . . ?
O1 C26 C27 O3 -172.1(3) . . . . ?
O4 C26 C27 O2 -172.9(3) . . . . ?
O4 C26 C27 O3 7.4(5) . . . . ?
S1 C3 C4 S7 178.52(19) . . . . ?
S1 C3 C4 S8 -2.2(5) . . . . ?
S2 C3 C4 S7 -0.6(3) . . . . ?
S2 C3 C4 S8 178.69(18) . . . . ?
S2 C5 C6 S3 1.0(4) . . . . ?
S2 C5 C6 S6 -179.62(17) . . . . ?
S4 C9 C10 S5 71.4(3) . . . . ?
S5 C7 C8 S3 -177.1(2) . . . . ?
S5 C7 C8 S4 5.0(5) . . . . ?
S6 C7 C8 S3 2.9(4) . . . . ?
S6 C7 C8 S4 -174.98(19) . . . . ?
S7 C5 C6 S3 -178.27(17) . . . . ?
S7 C5 C6 S6 1.1(4) . . . . ?
S8 C1 C2 S1 -70.7(3) . . . . ?
C1 S8 C4 S7 161.61(18) . . . . ?
C1 S8 C4 C3 -17.7(3) . . . . ?
C2 S1 C3 S2 172.84(18) . . . . ?
C2 S1 C3 C4 -6.3(3) . . . . ?
C3 S1 C2 C1 42.0(3) . . . . ?
C3 S2 C5 S7 -3.7(2) . . . . ?
C3 S2 C5 C6 176.9(3) . . . . ?
C4 S7 C5 S2 3.5(2) . . . . ?
C4 S7 C5 C6 -177.2(3) . . . . ?
C4 S8 C1 C2 53.4(3) . . . . ?
C5 S2 C3 S1 -176.65(18) . . . . ?
C5 S2 C3 C4 2.6(3) . . . . ?
C5 S7 C4 S8 178.85(18) . . . . ?
C5 S7 C4 C3 -1.8(3) . . . . ?
C6 S3 C8 S4 172.95(19) . . . . ?
C6 S3 C8 C7 -5.2(3) . . . . ?
C6 S6 C7 S5 -179.01(19) . . . . ?
C6 S6 C7 C8 1.0(3) . . . . ?
C7 S5 C10 C9 -39.0(3) . . . . ?
C7 S6 C6 S3 -4.5(2) . . . . ?
C7 S6 C6 C5 176.1(3) . . . . ?
C8 S3 C6 S6 5.7(2) . . . . ?
C8 S3 C6 C5 -174.9(3) . . . . ?
C8 S4 C9 C10 -56.0(3) . . . . ?
C9 S4 C8 S3 -159.08(19) . . . . ?
C9 S4 C8 C7 18.8(3) . . . . ?
C10 S5 C7 S6 -178.69(19) . . . . ?
C10 S5 C7 C8 1.3(4) . . . . ?
S9 C13 C14 S15 177.26(18) . . . . ?
S9 C13 C14 S16 -5.4(5) . . . . ?
S10 C13 C14 S15 -1.3(3) . . . . ?
S10 C13 C14 S16 175.96(19) . . . . ?
S10 C15 C16 S11 -3.2(4) . . . . ?
S10 C15 C16 S14 -179.38(17) . . . . ?
S12 C19 C20 S13 -52.3(4) . . . . ?
S13 C17 C18 S11 177.47(18) . . . . ?
S13 C17 C18 S12 -0.8(5) . . . . ?
S14 C17 C18 S11 -0.2(4) . . . . ?
S14 C17 C18 S12 -178.55(19) . . . . ?
S15 C15 C16 S11 174.85(17) . . . . ?
S15 C15 C16 S14 -1.3(4) . . . . ?
S16 C11 C12 S9 71.1(3) . . . . ?
C11 S16 C14 S15 -166.65(19) . . . . ?
C11 S16 C14 C13 16.0(3) . . . . ?
C12 S9 C13 S10 -163.17(19) . . . . ?
C12 S9 C13 C14 18.2(3) . . . . ?
C13 S9 C12 C11 -50.1(3) . . . . ?
C13 S10 C15 S15 3.3(2) . . . . ?
C13 S10 C15 C16 -178.6(3) . . . . ?
C14 S15 C15 S10 -3.8(2) . . . . ?
C14 S15 C15 C16 178.0(3) . . . . ?
C14 S16 C11 C12 -48.3(3) . . . . ?
C15 S10 C13 S9 -179.95(18) . . . . ?
C15 S10 C13 C14 -1.2(3) . . . . ?
C15 S15 C14 S16 -174.58(18) . . . . ?
C15 S15 C14 C13 3.1(3) . . . . ?
C16 S11 C18 S12 -178.34(19) . . . . ?
C16 S11 C18 C17 3.1(3) . . . . ?
C16 S14 C17 S13 179.3(2) . . . . ?
C16 S14 C17 C18 -2.8(3) . . . . ?
C17 S13 C20 C19 64.4(3) . . . . ?
C17 S14 C16 S11 4.9(2) . . . . ?
C17 S14 C16 C15 -178.6(3) . . . . ?
C18 S11 C16 S14 -5.0(2) . . . . ?
C18 S11 C16 C15 178.6(3) . . . . ?
C18 S12 C19 C20 8.1(4) . . . . ?
C19 S12 C18 S11 -157.5(2) . . . . ?
C19 S12 C18 C17 20.8(4) . . . . ?
C20 S13 C17 S14 139.3(2) . . . . ?
C20 S13 C17 C18 -38.4(3) . . . . ?
S18 C24 C25 S19 -70.3(3) . . . . ?
S19 C22 C23 S17 178.96(18) . . . . ?
S19 C22 C23 S18 -0.1(5) . . . . ?
S20 C22 C23 S17 -0.1(3) . . . . ?
S20 C22 C23 S18 -179.15(19) . . . . ?
C21 S17 C23 S18 -178.33(18) . . . . ?
C21 S17 C23 C22 2.5(3) . . . . ?
C21 S20 C22 S19 178.49(19) . . . . ?
C21 S20 C22 C23 -2.3(3) . . . . ?
C22 S19 C25 C24 54.4(2) . . . . ?
C22 S20 C21 S17 4.0(2) . . . . ?
C22 S20 C21 C21 -175.8(4) . . . 7_646 ?
C23 S17 C21 S20 -4.0(2) . . . . ?
C23 S17 C21 C21 175.8(4) . . . 7_646 ?
C23 S18 C24 C25 41.2(3) . . . . ?
C24 S18 C23 S17 174.23(18) . . . . ?
C24 S18 C23 C22 -6.7(3) . . . . ?
C25 S19 C22 S20 159.45(18) . . . . ?
C25 S19 C22 C23 -19.6(3) . . . . ?

_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 2.176
_oxdiff_exptl_absorpt_empirical_full_min 0.704
####################################################################### 
# 
# 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_iret5vt_2_290_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2163089'
loop_
_audit_author_name
_audit_author_address
'Toby Blundell'
;Nottingham Trent University
United Kingdom
;
_audit_update_record             
;
2022-03-29 deposited with the CCDC.	2022-04-25 downloaded from the CCDC.
;
_audit_creation_date             2022-03-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ir O12, 5(C10 H8 S8), C2 H6 O'
_chemical_formula_sum            'C58 H46 Ir O13 S40'
_chemical_formula_weight         2425.55
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 H10 O10 S10 Ir'
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'
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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.6386(15)
_cell_length_b                   13.2500(8)
_cell_length_c                   33.689(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.474(6)
_cell_angle_gamma                90
_cell_volume                     8294.5(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5530
_cell_measurement_temperature    290.03(10)
_cell_measurement_theta_max      71.7950
_cell_measurement_theta_min      4.0950
_shelx_estimated_absorpt_T_max   0.754
_shelx_estimated_absorpt_T_min   0.280
_exptl_absorpt_coefficient_mu    13.040
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             4860
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.023
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            26226
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         4.098
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_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   -100.00  32.00   1.00   30.00    --  -33.50   0.00 150.00  132
  2  ω     -9.00  34.00   1.00   30.00    --  -33.50  37.00   0.00   43
  3  ω    -33.00  14.00   1.00   30.00    --   36.58 -37.00-180.00   47
  4  ω     20.00 103.00   1.00   30.00    --   36.58  57.00 -30.00   83
  5  ω    -25.00  43.00   1.00   30.00    --   36.58 -37.00  90.00   68
  6  ω     27.00  88.00   1.00   30.00    --   36.58-125.00  60.00   61
  7  ω     44.00  71.00   1.00   30.00    --   36.58-125.00 120.00   27
  8  ω     22.00  56.00   1.00   30.00    --   36.58 -37.00-180.00   34
  9  ω     32.00  89.00   1.00   30.00    --   36.58-125.00-120.00   57
 10  ω     54.00 105.00   1.00   30.00    --   36.58  37.00  90.00   51
 11  ω     77.00 106.00   1.00  120.00    --  108.00 -94.00-120.00   29
 12  ω     40.00 124.00   1.00  120.00    --  108.00 -45.00 -60.00   84
 13  ω     76.00 105.00   1.00  120.00    --  108.00 -94.00  60.00   29
 14  ω     64.00 105.00   1.00  120.00    --  108.00 -94.00 -30.00   41
 15  ω     40.00 125.00   1.00  120.00    --  108.00 -45.00 120.00   85
 16  ω     54.00  88.00   1.00  120.00    --  108.00 -77.00 -90.00   34
 17  ω     69.00 108.00   1.00  120.00    --  108.00-111.00-150.00   39
 18  ω    107.00 168.00   1.00  120.00    --  108.00  61.00-120.00   61
 19  ω     40.00 115.00   1.00  120.00    --  108.00 -30.00-150.00   75
 20  ω     78.00 124.00   1.00  120.00    --  108.00 -61.00 150.00   46
 21  ω     69.00 108.00   1.00  120.00    --  108.00-111.00  60.00   39
 22  ω     88.00 125.00   1.00  120.00    --  108.00 178.00-180.00   37
 23  ω    103.00 176.00   1.00  120.00    --  108.00  77.00 -90.00   73
 24  ω     62.00  88.00   1.00  120.00    --  108.00 178.00 -90.00   26
 25  ω    119.00 145.00   1.00  120.00    --  108.00 178.00 -90.00   26
 26  ω     41.00  66.00   1.00  120.00    --  108.00 -94.00-150.00   25
 27  ω     40.00  96.00   1.00  120.00    --  108.00 -94.00 120.00   56
 28  ω     46.00 166.00   1.00  120.00    --  108.00   0.00-120.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0117156000
_diffrn_orient_matrix_UB_12      -0.0471594000
_diffrn_orient_matrix_UB_13      -0.0407889000
_diffrn_orient_matrix_UB_21      -0.0806862000
_diffrn_orient_matrix_UB_22      -0.0261479000
_diffrn_orient_matrix_UB_23      -0.0058363000
_diffrn_orient_matrix_UB_31      -0.0150332000
_diffrn_orient_matrix_UB_32      0.1029988000
_diffrn_orient_matrix_UB_33      -0.0201340000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5332
_reflns_number_total             7329
_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 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         4.205
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         7329
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0964
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1085P)²+97.9948P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2453
_refine_ls_wR_factor_ref         0.2645
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O7-C30
 1.336 with sigma of 0.02
 O7-C29
 2.382 with sigma of 0.02
 C30-C29
 1.489 with sigma of 0.02
3. Rigid bond restraints
 O7, H7, C29, H29A, H29B, H29C, C30, H30A, H30B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Rigid body (RIGU) restrains
 O7, H7, C29, H29A, H29B, H29C, C30, H30A, H30B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O7(0.5) H7(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5)
 H30A(0.5) H30B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C19(H19A,H19B), C20(H20A,H20B), C24(H24A,H24B), C25(H25A,H25B),
  C30(H30A,H30B)
6.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C)
6.c Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_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
Ir Ir 0.500000 0.56643(6) 0.750000 0.0528(3) Uani 1 2 d S T P . .
O1 O 0.4550(5) 0.6815(6) 0.7150(3) 0.054(2) Uani 1 1 d . . . . .
O2 O 0.4000(4) 0.5690(8) 0.7715(3) 0.055(2) Uani 1 1 d . . . . .
O3 O 0.2983(6) 0.6508(9) 0.7641(3) 0.077(3) Uani 1 1 d . . . . .
O4 O 0.3584(6) 0.7799(9) 0.7112(3) 0.072(3) Uani 1 1 d . . . . .
O5 O 0.4600(5) 0.4477(6) 0.7158(3) 0.055(2) Uani 1 1 d . . . . .
O6 O 0.4540(8) 0.2830(9) 0.7164(4) 0.101(5) Uani 1 1 d . . . . .
C26 C 0.3924(8) 0.7063(11) 0.7255(4) 0.058(3) Uani 1 1 d . . . . .
C27 C 0.3590(8) 0.6375(11) 0.7560(4) 0.058(3) Uani 1 1 d . . . . .
C28 C 0.4756(8) 0.3623(9) 0.7308(4) 0.057(3) Uani 1 1 d . . . . .
S1 S 0.0258(2) 0.5181(3) 0.41508(11) 0.0655(9) Uani 1 1 d . . . . .
S2 S 0.0930(2) 0.4600(3) 0.49291(10) 0.0582(8) Uani 1 1 d . . . . .
S3 S 0.14894(19) 0.3835(3) 0.58080(10) 0.0558(8) Uani 1 1 d . . . . .
S4 S 0.1760(2) 0.3142(3) 0.66391(10) 0.0633(9) Uani 1 1 d . . . . .
S5 S 0.3040(3) 0.5093(3) 0.67046(11) 0.0755(12) Uani 1 1 d . . . . .
S6 S 0.2491(2) 0.5527(3) 0.58860(10) 0.0568(8) Uani 1 1 d . . . . .
S7 S 0.1944(2) 0.6284(3) 0.50043(10) 0.0565(8) Uani 1 1 d . . . . .
S8 S 0.1481(2) 0.7193(3) 0.42291(11) 0.0630(9) Uani 1 1 d . . . . .
C1 C 0.1013(8) 0.6662(13) 0.3784(4) 0.065(4) Uani 1 1 d . . . . .
H1A H 0.097250 0.717636 0.357889 0.078 Uiso 1 1 calc R U . . .
H1B H 0.129891 0.611443 0.368889 0.078 Uiso 1 1 calc R U . . .
C2 C 0.0300(9) 0.6284(13) 0.3843(5) 0.074(5) Uani 1 1 d . . . . .
H2A H 0.005960 0.613313 0.358458 0.089 Uiso 1 1 calc R U . . .
H2B H 0.003117 0.681880 0.396057 0.089 Uiso 1 1 calc R U . . .
C3 C 0.0911(7) 0.5445(10) 0.4535(4) 0.052(3) Uani 1 1 d . . . . .
C4 C 0.1371(7) 0.6225(9) 0.4568(4) 0.048(3) Uani 1 1 d . . . . .
C5 C 0.1606(7) 0.5227(9) 0.5225(4) 0.051(3) Uani 1 1 d . . . . .
C6 C 0.1828(8) 0.4913(11) 0.5594(4) 0.057(3) Uani 1 1 d . . . . .
C7 C 0.2435(7) 0.4750(9) 0.6302(4) 0.049(3) Uani 1 1 d . . . . .
C8 C 0.1981(7) 0.3997(9) 0.6269(4) 0.047(3) Uani 1 1 d . . . . .
C9 C 0.2092(10) 0.3852(13) 0.7073(4) 0.073(4) Uani 1 1 d . . . . .
H9A H 0.180074 0.445361 0.709150 0.088 Uiso 1 1 calc R U . . .
H9B H 0.203489 0.344745 0.730848 0.088 Uiso 1 1 calc R U . . .
C10 C 0.2850(8) 0.4152(11) 0.7071(4) 0.065(4) Uani 1 1 d . . . . .
H10A H 0.313364 0.355550 0.702548 0.078 Uiso 1 1 calc R U . . .
H10B H 0.300828 0.441024 0.733277 0.078 Uiso 1 1 calc R U . . .
S9 S -0.08183(19) 0.8636(3) 0.40375(10) 0.0584(8) Uani 1 1 d . . . . .
S10 S -0.0203(2) 0.8047(3) 0.48314(10) 0.0631(9) Uani 1 1 d . . . . .
S11 S 0.0354(2) 0.7256(3) 0.57099(10) 0.0626(9) Uani 1 1 d . . . . .
S12 S 0.0784(2) 0.6375(3) 0.65013(11) 0.0790(13) Uani 1 1 d . . . . .
S13 S 0.2239(2) 0.7921(3) 0.65006(10) 0.0654(10) Uani 1 1 d . . . . .
S14 S 0.16013(19) 0.8596(3) 0.57065(9) 0.0552(8) Uani 1 1 d . . . . .
S15 S 0.10221(19) 0.9431(3) 0.48464(9) 0.0566(8) Uani 1 1 d . . . . .
S16 S 0.0685(2) 1.0209(3) 0.40391(12) 0.0782(12) Uani 1 1 d . . . . .
C11 C -0.0098(9) 1.0210(14) 0.3706(5) 0.076(5) Uani 1 1 d . . . . .
H11A H -0.045784 1.063164 0.381709 0.091 Uiso 1 1 calc R U . . .
H11B H 0.001908 1.051749 0.345776 0.091 Uiso 1 1 calc R U . . .
C12 C -0.0415(10) 0.9225(13) 0.3617(4) 0.077(5) Uani 1 1 d . . . . .
H12A H -0.004465 0.878093 0.352969 0.092 Uiso 1 1 calc R U . . .
H12B H -0.078147 0.929541 0.339831 0.092 Uiso 1 1 calc R U . . .
C13 C -0.0117(6) 0.8798(9) 0.4412(3) 0.044(3) Uani 1 1 d . . . . .
C14 C 0.0431(7) 0.9434(10) 0.4415(3) 0.050(3) Uani 1 1 d . . . . .
C15 C 0.0582(7) 0.8494(10) 0.5086(3) 0.049(3) Uani 1 1 d . . . . .
C16 C 0.0825(7) 0.8139(10) 0.5456(4) 0.052(3) Uani 1 1 d . . . . .
C17 C 0.1548(7) 0.7823(9) 0.6126(4) 0.051(3) Uani 1 1 d . . . . .
C18 C 0.1001(7) 0.7189(10) 0.6123(4) 0.053(3) Uani 1 1 d . . . . .
C19 C 0.1294(12) 0.6862(17) 0.6935(5) 0.103(7) Uani 1 1 d . . . . .
H19A H 0.095212 0.700129 0.713086 0.124 Uiso 1 1 calc R U . . .
H19B H 0.159672 0.631439 0.704142 0.124 Uiso 1 1 calc R U . . .
C20 C 0.1747(12) 0.7734(18) 0.6922(5) 0.101(7) Uani 1 1 d . . . . .
H20A H 0.208926 0.771186 0.715427 0.121 Uiso 1 1 calc R U . . .
H20B H 0.144787 0.832466 0.695000 0.121 Uiso 1 1 calc R U . . .
S17 S 0.27415(19) 0.3731(3) 0.46049(9) 0.0569(8) Uani 1 1 d . . . . .
S18 S 0.2439(2) 0.4536(3) 0.37986(11) 0.0651(10) Uani 1 1 d . . . . .
S19 S 0.1224(2) 0.2506(2) 0.36778(10) 0.0564(8) Uani 1 1 d . . . . .
S20 S 0.17372(19) 0.2042(3) 0.45096(9) 0.0556(8) Uani 1 1 d . . . . .
C21 C 0.2387(8) 0.2657(10) 0.4821(4) 0.054(3) Uani 1 1 d . . . . .
C22 C 0.1797(7) 0.2829(9) 0.4099(4) 0.047(3) Uani 1 1 d . . . . .
C23 C 0.2241(6) 0.3608(9) 0.4142(4) 0.046(3) Uani 1 1 d . . . . .
C24 C 0.1947(8) 0.4089(12) 0.3347(4) 0.060(3) Uani 1 1 d . . . . .
H24A H 0.190324 0.463805 0.315611 0.073 Uiso 1 1 calc R U . . .
H24B H 0.222245 0.355609 0.323278 0.073 Uiso 1 1 calc R U . . .
C25 C 0.1215(8) 0.3699(11) 0.3407(4) 0.063(4) Uani 1 1 d . . . . .
H25A H 0.095318 0.360670 0.314903 0.075 Uiso 1 1 calc R U . . .
H25B H 0.095877 0.419768 0.355211 0.075 Uiso 1 1 calc R U . . .
O7 O -0.064(2) 0.451(2) 0.7106(14) 0.189(17) Uani 0.5 1 d D U P A -1
H7 H -0.059473 0.480190 0.689367 0.283 Uiso 0.5 1 calc R U P A -1
C29 C 0.012(4) 0.493(6) 0.768(2) 0.23(3) Uani 0.5 1 d D U P A -1
H29A H -0.017876 0.551878 0.766387 0.341 Uiso 0.5 1 calc R U P A -1
H29B H 0.061686 0.512885 0.771908 0.341 Uiso 0.5 1 calc R U P A -1
H29C H -0.000312 0.450444 0.789054 0.341 Uiso 0.5 1 calc R U P A -1
C30 C 0.001(3) 0.437(4) 0.7296(18) 0.184(18) Uani 0.5 1 d D U P A -1
H30A H 0.037914 0.457749 0.712255 0.220 Uiso 0.5 1 calc R U P A -1
H30B H 0.008048 0.365417 0.734899 0.220 Uiso 0.5 1 calc R U P A -1


_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
Ir O1 2.064(8) . ?
Ir O1 2.064(8) 2_656 ?
Ir O2 2.052(8) . ?
Ir O2 2.052(8) 2_656 ?
Ir O5 2.056(8) 2_656 ?
Ir O5 2.056(8) . ?
O1 C26 1.288(17) . ?
O2 C27 1.272(17) . ?
O3 C27 1.197(17) . ?
O4 C26 1.240(18) . ?
O5 C28 1.264(15) . ?
O6 C28 1.213(16) . ?
C26 C27 1.54(2) . ?
C28 C28 1.52(3) 2_656 ?
S1 C2 1.797(15) . ?
S1 C3 1.742(13) . ?
S2 C3 1.735(12) . ?
S2 C5 1.754(13) . ?
S3 C6 1.740(15) . ?
S3 C8 1.753(12) . ?
S4 C8 1.758(12) . ?
S4 C9 1.806(16) . ?
S5 C7 1.753(13) . ?
S5 C10 1.808(14) . ?
S6 C6 1.722(14) . ?
S6 C7 1.749(12) . ?
S7 C4 1.750(12) . ?
S7 C5 1.728(12) . ?
S8 C1 1.817(14) . ?
S8 C4 1.739(12) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.45(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.342(18) . ?
C5 C6 1.345(19) . ?
C7 C8 1.308(18) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.47(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
S9 C12 1.830(15) . ?
S9 C13 1.758(11) . ?
S10 C13 1.745(12) . ?
S10 C15 1.742(12) . ?
S11 C16 1.729(13) . ?
S11 C18 1.772(12) . ?
S12 C18 1.740(13) . ?
S12 C19 1.800(18) . ?
S13 C17 1.736(13) . ?
S13 C20 1.77(2) . ?
S14 C16 1.728(13) . ?
S14 C17 1.755(12) . ?
S15 C14 1.753(12) . ?
S15 C15 1.724(13) . ?
S16 C11 1.772(15) . ?
S16 C14 1.727(13) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.45(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.323(18) . ?
C15 C16 1.373(18) . ?
C17 C18 1.320(18) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.43(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
S17 C21 1.750(13) . ?
S17 C23 1.760(11) . ?
S18 C23 1.747(12) . ?
S18 C24 1.814(14) . ?
S19 C22 1.760(12) . ?
S19 C25 1.824(14) . ?
S20 C21 1.742(13) . ?
S20 C22 1.743(12) . ?
C21 C21 1.31(3) 7_556 ?
C22 C23 1.325(17) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.49(2) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
O7 H7 0.8200 . ?
O7 C30 1.34(2) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C29 C30 1.48(2) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?

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
O1 Ir O1 84.7(5) . 2_656 ?
O2 Ir O1 97.2(4) . 2_656 ?
O2 Ir O1 81.4(4) 2_656 2_656 ?
O2 Ir O1 81.4(4) . . ?
O2 Ir O1 97.2(4) 2_656 . ?
O2 Ir O2 178.1(6) . 2_656 ?
O2 Ir O5 96.6(4) . 2_656 ?
O2 Ir O5 96.6(4) 2_656 . ?
O2 Ir O5 84.9(4) . . ?
O2 Ir O5 84.9(4) 2_656 2_656 ?
O5 Ir O1 97.6(4) 2_656 2_656 ?
O5 Ir O1 97.6(4) . . ?
O5 Ir O1 177.1(4) 2_656 . ?
O5 Ir O1 177.1(4) . 2_656 ?
O5 Ir O5 80.2(5) 2_656 . ?
C26 O1 Ir 111.6(8) . . ?
C27 O2 Ir 113.6(9) . . ?
C28 O5 Ir 113.5(8) . . ?
O1 C26 C27 117.0(13) . . ?
O4 C26 O1 122.8(13) . . ?
O4 C26 C27 120.2(14) . . ?
O2 C27 C26 115.8(13) . . ?
O3 C27 O2 124.1(15) . . ?
O3 C27 C26 120.1(14) . . ?
O5 C28 C28 116.3(7) . 2_656 ?
O6 C28 O5 123.8(13) . . ?
O6 C28 C28 119.8(9) . 2_656 ?
C3 S1 C2 101.8(7) . . ?
C3 S2 C5 95.7(6) . . ?
C6 S3 C8 94.9(6) . . ?
C8 S4 C9 98.9(7) . . ?
C7 S5 C10 101.6(6) . . ?
C6 S6 C7 95.5(6) . . ?
C5 S7 C4 96.1(6) . . ?
C4 S8 C1 100.5(7) . . ?
S8 C1 H1A 108.7 . . ?
S8 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C2 C1 S8 114.1(11) . . ?
C2 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
S1 C2 H2A 108.2 . . ?
S1 C2 H2B 108.2 . . ?
C1 C2 S1 116.3(12) . . ?
C1 C2 H2A 108.2 . . ?
C1 C2 H2B 108.2 . . ?
H2A C2 H2B 107.4 . . ?
S2 C3 S1 114.2(7) . . ?
C4 C3 S1 128.4(10) . . ?
C4 C3 S2 117.4(10) . . ?
S8 C4 S7 115.0(7) . . ?
C3 C4 S7 116.5(9) . . ?
C3 C4 S8 128.4(10) . . ?
S7 C5 S2 114.1(7) . . ?
C6 C5 S2 122.3(11) . . ?
C6 C5 S7 123.5(11) . . ?
S6 C6 S3 114.7(8) . . ?
C5 C6 S3 122.8(11) . . ?
C5 C6 S6 122.5(11) . . ?
S6 C7 S5 113.2(7) . . ?
C8 C7 S5 129.6(10) . . ?
C8 C7 S6 117.2(10) . . ?
S3 C8 S4 114.5(7) . . ?
C7 C8 S3 117.4(10) . . ?
C7 C8 S4 128.1(10) . . ?
S4 C9 H9A 108.8 . . ?
S4 C9 H9B 108.8 . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 S4 114.0(11) . . ?
C10 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
S5 C10 H10A 108.4 . . ?
S5 C10 H10B 108.4 . . ?
C9 C10 S5 115.4(11) . . ?
C9 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
C13 S9 C12 100.2(7) . . ?
C15 S10 C13 94.5(6) . . ?
C16 S11 C18 94.8(6) . . ?
C18 S12 C19 103.5(8) . . ?
C17 S13 C20 99.8(8) . . ?
C16 S14 C17 95.3(6) . . ?
C15 S15 C14 95.6(6) . . ?
C14 S16 C11 101.8(7) . . ?
S16 C11 H11A 108.4 . . ?
S16 C11 H11B 108.4 . . ?
H11A C11 H11B 107.5 . . ?
C12 C11 S16 115.5(12) . . ?
C12 C11 H11A 108.4 . . ?
C12 C11 H11B 108.4 . . ?
S9 C12 H12A 108.7 . . ?
S9 C12 H12B 108.7 . . ?
C11 C12 S9 114.1(11) . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
S10 C13 S9 113.7(6) . . ?
C14 C13 S9 127.8(9) . . ?
C14 C13 S10 118.5(9) . . ?
S16 C14 S15 114.7(8) . . ?
C13 C14 S15 116.1(9) . . ?
C13 C14 S16 129.0(10) . . ?
S15 C15 S10 115.2(7) . . ?
C16 C15 S10 122.3(10) . . ?
C16 C15 S15 122.4(10) . . ?
S14 C16 S11 115.6(8) . . ?
C15 C16 S11 122.5(10) . . ?
C15 C16 S14 121.8(10) . . ?
S13 C17 S14 117.1(7) . . ?
C18 C17 S13 125.6(10) . . ?
C18 C17 S14 117.2(10) . . ?
S12 C18 S11 115.1(7) . . ?
C17 C18 S11 116.8(10) . . ?
C17 C18 S12 127.7(10) . . ?
S12 C19 H19A 106.7 . . ?
S12 C19 H19B 106.7 . . ?
H19A C19 H19B 106.6 . . ?
C20 C19 S12 122.6(13) . . ?
C20 C19 H19A 106.7 . . ?
C20 C19 H19B 106.7 . . ?
S13 C20 H20A 107.6 . . ?
S13 C20 H20B 107.6 . . ?
C19 C20 S13 118.8(15) . . ?
C19 C20 H20A 107.6 . . ?
C19 C20 H20B 107.6 . . ?
H20A C20 H20B 107.1 . . ?
C21 S17 C23 95.9(6) . . ?
C23 S18 C24 102.0(6) . . ?
C22 S19 C25 100.0(6) . . ?
C21 S20 C22 96.5(6) . . ?
S20 C21 S17 113.4(7) . . ?
C21 C21 S17 122.4(14) 7_556 . ?
C21 C21 S20 124.2(14) 7_556 . ?
S20 C22 S19 115.0(7) . . ?
C23 C22 S19 127.8(9) . . ?
C23 C22 S20 117.1(9) . . ?
S18 C23 S17 113.4(6) . . ?
C22 C23 S17 117.0(9) . . ?
C22 C23 S18 129.5(10) . . ?
S18 C24 H24A 108.7 . . ?
S18 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 S18 114.1(10) . . ?
C25 C24 H24A 108.7 . . ?
C25 C24 H24B 108.7 . . ?
S19 C25 H25A 108.9 . . ?
S19 C25 H25B 108.9 . . ?
C24 C25 S19 113.3(10) . . ?
C24 C25 H25A 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C30 O7 H7 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
O7 C30 C29 113(2) . . ?
O7 C30 H30A 108.9 . . ?
O7 C30 H30B 108.9 . . ?
C29 C30 H30A 108.9 . . ?
C29 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?

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
Ir O1 C26 O4 172.9(11) . . . . ?
Ir O1 C26 C27 -9.3(14) . . . . ?
Ir O2 C27 O3 178.9(12) . . . . ?
Ir O2 C27 C26 -1.7(14) . . . . ?
Ir O5 C28 O6 175.9(15) . . . . ?
Ir O5 C28 C28 -4(2) . . . 2_656 ?
O1 C26 C27 O2 7.7(17) . . . . ?
O1 C26 C27 O3 -172.8(13) . . . . ?
O4 C26 C27 O2 -174.4(12) . . . . ?
O4 C26 C27 O3 5(2) . . . . ?
S1 C3 C4 S7 178.0(9) . . . . ?
S1 C3 C4 S8 -2(2) . . . . ?
S2 C3 C4 S7 0.7(16) . . . . ?
S2 C3 C4 S8 -179.8(8) . . . . ?
S2 C5 C6 S3 2.3(19) . . . . ?
S2 C5 C6 S6 -179.9(8) . . . . ?
S4 C9 C10 S5 69.0(15) . . . . ?
S5 C7 C8 S3 -176.4(8) . . . . ?
S5 C7 C8 S4 7(2) . . . . ?
S6 C7 C8 S3 1.0(15) . . . . ?
S6 C7 C8 S4 -175.4(8) . . . . ?
S7 C5 C6 S3 -179.1(8) . . . . ?
S7 C5 C6 S6 -1.3(19) . . . . ?
S8 C1 C2 S1 -68.4(17) . . . . ?
C1 S8 C4 S7 163.9(8) . . . . ?
C1 S8 C4 C3 -15.6(15) . . . . ?
C2 S1 C3 S2 171.5(9) . . . . ?
C2 S1 C3 C4 -5.9(16) . . . . ?
C3 S1 C2 C1 41.9(15) . . . . ?
C3 S2 C5 S7 -2.1(9) . . . . ?
C3 S2 C5 C6 176.7(13) . . . . ?
C4 S7 C5 S2 2.3(9) . . . . ?
C4 S7 C5 C6 -176.4(13) . . . . ?
C4 S8 C1 C2 50.1(14) . . . . ?
C5 S2 C3 S1 -176.9(8) . . . . ?
C5 S2 C3 C4 0.8(13) . . . . ?
C5 S7 C4 S8 178.5(8) . . . . ?
C5 S7 C4 C3 -1.8(12) . . . . ?
C6 S3 C8 S4 173.1(8) . . . . ?
C6 S3 C8 C7 -3.8(12) . . . . ?
C6 S6 C7 S5 -179.8(8) . . . . ?
C6 S6 C7 C8 2.4(12) . . . . ?
C7 S5 C10 C9 -36.2(14) . . . . ?
C7 S6 C6 S3 -4.9(9) . . . . ?
C7 S6 C6 C5 177.1(13) . . . . ?
C8 S3 C6 S6 5.3(9) . . . . ?
C8 S3 C6 C5 -176.7(13) . . . . ?
C8 S4 C9 C10 -54.8(13) . . . . ?
C9 S4 C8 S3 -158.8(8) . . . . ?
C9 S4 C8 C7 17.7(15) . . . . ?
C10 S5 C7 S6 -179.4(8) . . . . ?
C10 S5 C7 C8 -1.9(16) . . . . ?
S9 C13 C14 S15 177.9(8) . . . . ?
S9 C13 C14 S16 -7(2) . . . . ?
S10 C13 C14 S15 0.8(15) . . . . ?
S10 C13 C14 S16 175.7(8) . . . . ?
S10 C15 C16 S11 -2.8(18) . . . . ?
S10 C15 C16 S14 -179.6(8) . . . . ?
S12 C19 C20 S13 -37(3) . . . . ?
S13 C17 C18 S11 178.8(8) . . . . ?
S13 C17 C18 S12 6(2) . . . . ?
S14 C17 C18 S11 -4.2(17) . . . . ?
S14 C17 C18 S12 -177.0(9) . . . . ?
S15 C15 C16 S11 175.8(8) . . . . ?
S15 C15 C16 S14 -0.9(18) . . . . ?
S16 C11 C12 S9 68.8(18) . . . . ?
C11 S16 C14 S15 -169.1(9) . . . . ?
C11 S16 C14 C13 15.9(16) . . . . ?
C12 S9 C13 S10 -164.3(8) . . . . ?
C12 S9 C13 C14 18.4(15) . . . . ?
C13 S9 C12 C11 -48.4(15) . . . . ?
C13 S10 C15 S15 3.0(9) . . . . ?
C13 S10 C15 C16 -178.3(12) . . . . ?
C14 S15 C15 S10 -2.7(9) . . . . ?
C14 S15 C15 C16 178.6(12) . . . . ?
C14 S16 C11 C12 -47.1(15) . . . . ?
C15 S10 C13 S9 -179.8(8) . . . . ?
C15 S10 C13 C14 -2.3(12) . . . . ?
C15 S15 C14 S16 -174.5(8) . . . . ?
C15 S15 C14 C13 1.2(12) . . . . ?
C16 S11 C18 S12 178.9(9) . . . . ?
C16 S11 C18 C17 5.2(13) . . . . ?
C16 S14 C17 S13 178.2(8) . . . . ?
C16 S14 C17 C18 0.9(13) . . . . ?
C17 S13 C20 C19 52(2) . . . . ?
C17 S14 C16 S11 2.8(9) . . . . ?
C17 S14 C16 C15 179.8(12) . . . . ?
C18 S11 C16 S14 -4.5(9) . . . . ?
C18 S11 C16 C15 178.5(12) . . . . ?
C18 S12 C19 C20 0(3) . . . . ?
C19 S12 C18 S11 -156.1(11) . . . . ?
C19 S12 C18 C17 16.8(18) . . . . ?
C20 S13 C17 S14 144.9(11) . . . . ?
C20 S13 C17 C18 -38.1(16) . . . . ?
S18 C24 C25 S19 -70.3(13) . . . . ?
S19 C22 C23 S17 179.5(8) . . . . ?
S19 C22 C23 S18 -3(2) . . . . ?
S20 C22 C23 S17 2.1(15) . . . . ?
S20 C22 C23 S18 179.6(8) . . . . ?
C21 S17 C23 S18 -178.0(8) . . . . ?
C21 S17 C23 C22 -0.1(12) . . . . ?
C21 S20 C22 S19 179.3(8) . . . . ?
C21 S20 C22 C23 -2.9(13) . . . . ?
C22 S19 C25 C24 52.6(11) . . . . ?
C22 S20 C21 S17 2.7(10) . . . . ?
C22 S20 C21 C21 -175.4(19) . . . 7_556 ?
C23 S17 C21 S20 -1.8(9) . . . . ?
C23 S17 C21 C21 176.3(19) . . . 7_556 ?
C23 S18 C24 C25 42.1(13) . . . . ?
C24 S18 C23 S17 171.9(8) . . . . ?
C24 S18 C23 C22 -5.6(15) . . . . ?
C25 S19 C22 S20 160.8(8) . . . . ?
C25 S19 C22 C23 -16.7(15) . . . . ?

_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 2.430
_oxdiff_exptl_absorpt_empirical_full_min 0.593
