# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_aa96
_database_code_depnum_ccdc_archive 'CCDC 1574807'
_audit_update_record             
;
2017-09-15 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'e{N(CH2CH2)2N}2C60?3I2?CS2?C6H6 '
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C34 H8 N2), 2(I2), 2(C3 H3), 0.5(C S2), 0.5(C S2)'
_chemical_formula_sum            'C72 H19 I4 N4 S2'
_chemical_formula_weight         1511.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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'
I I -0.3071 2.1212 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1430 0.1480 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_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+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   15.4566(7)
_cell_length_b                   10.6707(5)
_cell_length_c                   16.0942(7)
_cell_angle_alpha                90
_cell_angle_beta                 115.744(2)
_cell_angle_gamma                90
_cell_volume                     2390.99(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9966
_cell_measurement_theta_min      2.585
_cell_measurement_theta_max      43.948

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_F_000             1446
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    3.428
_shelx_estimated_absorpt_T_min   0.279
_shelx_estimated_absorpt_T_max   0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3944
_exptl_absorpt_correction_T_max  0.4458
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source, beamline 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with Photon 100 CMOS detector'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            61791
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.584
_diffrn_reflns_theta_max         43.971
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             14780
_reflns_number_gt                12163
_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       'Apex 2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2014)'
_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)+(0.0351P)²+6.1659P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14780
_refine_ls_number_parameters     405
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0927
_refine_ls_wR_factor_gt          0.0869
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.004
_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
I1 I 0.68498(2) 1.12178(2) 0.90842(2) 0.01468(3) Uani 1 1 d . . . . .
I2 I 0.41672(2) 0.7500 0.54063(2) 0.01208(3) Uani 1 2 d S T P . .
I3 I 0.30903(2) 0.7500 0.64092(2) 0.02315(5) Uani 1 2 d S T P . .
N1 N 0.69864(12) 0.86871(16) 0.90060(11) 0.0123(3) Uani 1 1 d . . . . .
N2 N 0.61571(17) 0.7500 0.35415(16) 0.0150(4) Uani 1 2 d S T P . .
N3 N 0.52138(15) 0.7500 0.45150(15) 0.0106(3) Uani 1 2 d S T P . .
C1 C 0.75217(13) 0.82567(18) 0.84698(12) 0.0106(3) Uani 1 1 d . . . . .
C2 C 0.85281(13) 0.88473(18) 0.88555(12) 0.0117(3) Uani 1 1 d . . . . .
C3 C 0.93671(13) 0.81953(19) 0.93149(12) 0.0128(3) Uani 1 1 d . . . . .
C4 C 1.02448(13) 0.8602(2) 0.92759(13) 0.0143(3) Uani 1 1 d . . . . .
C5 C 1.07775(19) 0.7500 0.92501(18) 0.0143(4) Uani 1 2 d S T P . .
C6 C 1.12984(19) 0.7500 0.87242(19) 0.0152(5) Uani 1 2 d S T P . .
C7 C 1.12952(13) 0.8601(2) 0.81950(14) 0.0158(3) Uani 1 1 d . . . . .
C8 C 1.12856(13) 0.8181(2) 0.73341(14) 0.0156(3) Uani 1 1 d . . . . .
C9 C 1.07464(14) 0.8833(2) 0.65212(14) 0.0153(3) Uani 1 1 d . . . . .
C10 C 1.01831(13) 0.8150(2) 0.56784(14) 0.0150(3) Uani 1 1 d . . . . .
C11 C 0.92920(13) 0.8835(2) 0.51811(13) 0.0147(3) Uani 1 1 d . . . . .
C12 C 0.84306(13) 0.8179(2) 0.47090(13) 0.0135(3) Uani 1 1 d . . . . .
C13 C 0.75543(13) 0.86027(19) 0.47219(12) 0.0125(3) Uani 1 1 d . . . . .
C14 C 0.68543(18) 0.7500 0.45275(17) 0.0116(4) Uani 1 2 d S T P . .
C15 C 0.62744(17) 0.7500 0.51581(17) 0.0096(4) Uani 1 2 d S T P . .
C16 C 0.65201(12) 0.85981(17) 0.58345(12) 0.0098(3) Uani 1 1 d . . . . .
C17 C 0.65661(12) 0.81862(17) 0.66996(12) 0.0090(2) Uani 1 1 d . . . . .
C18 C 0.70778(12) 0.88422(17) 0.75048(12) 0.0099(3) Uani 1 1 d . . . . .
C19 C 0.76265(13) 0.99035(17) 0.74755(13) 0.0114(3) Uani 1 1 d . . . . .
C20 C 0.85233(13) 0.99181(18) 0.83090(13) 0.0120(3) Uani 1 1 d . . . . .
C21 C 0.93610(14) 1.03384(19) 0.82727(14) 0.0138(3) Uani 1 1 d . . . . .
C22 C 1.02452(14) 0.9664(2) 0.87711(13) 0.0140(3) Uani 1 1 d . . . . .
C23 C 1.07805(14) 0.9659(2) 0.82178(14) 0.0154(3) Uani 1 1 d . . . . .
C24 C 1.02187(14) 1.0340(2) 0.73706(15) 0.0157(3) Uani 1 1 d . . . . .
C25 C 1.02036(14) 0.9936(2) 0.65388(14) 0.0157(3) Uani 1 1 d . . . . .
C26 C 0.93042(14) 0.9931(2) 0.57057(14) 0.0149(3) Uani 1 1 d . . . . .
C27 C 0.84580(14) 1.03200(19) 0.57412(14) 0.0139(3) Uani 1 1 d . . . . .
C28 C 0.75732(13) 0.96345(19) 0.52352(13) 0.0123(3) Uani 1 1 d . . . . .
C29 C 0.70423(13) 0.96276(18) 0.58099(13) 0.0111(3) Uani 1 1 d . . . . .
C30 C 0.76031(13) 1.03067(17) 0.66396(13) 0.0120(3) Uani 1 1 d . . . . .
C31 C 0.84793(14) 1.07374(18) 0.66044(14) 0.0134(3) Uani 1 1 d . . . . .
C32 C 0.93396(14) 1.07567(19) 0.74042(14) 0.0147(3) Uani 1 1 d . . . . .
C33 C 0.74775(16) 0.8227(2) 0.99639(14) 0.0168(3) Uani 1 1 d . . . . .
H33A H 0.7143 0.8541 1.0326 0.020 Uiso 1 1 calc R U . . .
H33B H 0.8146 0.8541 1.0254 0.020 Uiso 1 1 calc R U . . .
C34 C 0.59921(14) 0.8226(2) 0.85753(14) 0.0153(3) Uani 1 1 d . . . . .
H34A H 0.5662 0.8539 0.7934 0.018 Uiso 1 1 calc R U . . .
H34B H 0.5641 0.8539 0.8922 0.018 Uiso 1 1 calc R U . . .
C35 C 0.49656(13) 0.6368(2) 0.39208(13) 0.0147(3) Uani 1 1 d . . . . .
H35A H 0.4269 0.6361 0.3509 0.018 Uiso 1 1 calc R U . . .
H35B H 0.5122 0.5605 0.4309 0.018 Uiso 1 1 calc R U . . .
C36 C 0.55446(14) 0.6376(2) 0.33354(14) 0.0174(4) Uani 1 1 d . . . . .
H36A H 0.5950 0.5616 0.3473 0.021 Uiso 1 1 calc R U . . .
H36B H 0.5095 0.6365 0.2671 0.021 Uiso 1 1 calc R U . . .
C37 C 0.6125(7) 0.3777(7) 0.1102(6) 0.0192(14) Uiso 0.25 1 d D . P A 1
S1 S 0.61852(13) 0.2500 0.09659(13) 0.0340(5) Uani 0.5 2 d DS T P A 1
S2 S 0.6071(4) 0.5164(4) 0.1282(4) 0.0544(12) Uani 0.25 1 d D . P A 1
C38 C 0.6906(7) 0.6767(11) 0.1864(7) 0.0262(18) Uiso 0.25 1 d D . P B 2
S3 S 0.7915(2) 0.7500 0.23988(15) 0.0392(6) Uani 0.5 2 d DS T P B 2
S4 S 0.5851(3) 0.6244(6) 0.1243(3) 0.0580(14) Uani 0.25 1 d D . P B 2
C39 C 0.5807(6) 0.7551(16) 0.1233(7) 0.061(3) Uiso 0.25 1 d G . P C -3
H39 H 0.5149 0.7657 0.0819 0.073 Uiso 0.25 1 d G U P C -3
C40 C 0.6186(7) 0.6353(13) 0.1478(8) 0.042(4) Uiso 0.25 1 d G . P C -3
H40 H 0.5787 0.5641 0.1232 0.050 Uiso 0.25 1 d G U P C -3
C41 C 0.7149(8) 0.6197(8) 0.2084(8) 0.033(2) Uiso 0.25 1 d G . P C -3
H41 H 0.7408 0.5378 0.2251 0.040 Uiso 0.25 1 d G U P C -3
C42 C 0.7732(5) 0.7239(8) 0.2444(6) 0.028(3) Uiso 0.25 1 d G . P C -3
H42 H 0.8390 0.7132 0.2858 0.034 Uiso 0.25 1 d G U P C -3
C43 C 0.7353(8) 0.8437(7) 0.2199(9) 0.035(2) Uiso 0.25 1 d G . P C -3
H43 H 0.7752 0.9149 0.2445 0.042 Uiso 0.25 1 d G U P C -3
C44 C 0.6391(9) 0.8593(12) 0.1593(9) 0.094(10) Uiso 0.25 1 d G . P C -3
H44 H 0.6132 0.9412 0.1426 0.112 Uiso 0.25 1 d G U P C -3


_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 I1 2.7363(3) 4_585 ?
I2 I3 2.7766(3) . ?
N1 C34 1.469(3) . ?
N1 C33 1.476(3) . ?
N1 C1 1.504(2) . ?
N2 C36 1.474(3) . ?
N2 C36 1.474(3) 4_575 ?
N2 C14 1.481(3) . ?
N3 C35 1.484(2) . ?
N3 C35 1.484(2) 4_575 ?
N3 C15 1.511(3) . ?
C1 C18 1.532(3) . ?
C1 C2 1.537(3) . ?
C1 C1 1.615(4) 4_575 ?
C2 C3 1.371(3) . ?
C2 C20 1.440(3) . ?
C3 C4 1.452(3) . ?
C3 C3 1.484(4) 4_575 ?
C4 C22 1.395(3) . ?
C4 C5 1.446(3) . ?
C5 C6 1.399(4) . ?
C5 C4 1.446(3) 4_575 ?
C6 C7 1.450(3) . ?
C6 C7 1.450(3) 4_575 ?
C7 C23 1.390(3) . ?
C7 C8 1.450(3) . ?
C8 C9 1.394(3) . ?
C8 C8 1.454(5) 4_575 ?
C9 C10 1.450(3) . ?
C9 C25 1.453(3) . ?
C10 C10 1.387(5) 4_575 ?
C10 C11 1.454(3) . ?
C11 C12 1.400(3) . ?
C11 C26 1.438(3) . ?
C12 C13 1.437(3) . ?
C12 C12 1.449(4) 4_575 ?
C13 C28 1.369(3) . ?
C13 C14 1.536(3) . ?
C14 C13 1.536(3) 4_575 ?
C14 C15 1.620(4) . ?
C15 C16 1.531(2) . ?
C15 C16 1.531(2) 4_575 ?
C16 C29 1.374(3) . ?
C16 C17 1.432(2) . ?
C17 C18 1.380(2) . ?
C17 C17 1.465(4) 4_575 ?
C18 C19 1.428(3) . ?
C19 C30 1.398(3) . ?
C19 C20 1.451(3) . ?
C20 C21 1.395(3) . ?
C21 C22 1.441(3) . ?
C21 C32 1.454(3) . ?
C22 C23 1.455(3) . ?
C23 C24 1.454(3) . ?
C24 C25 1.397(3) . ?
C24 C32 1.453(3) . ?
C25 C26 1.453(3) . ?
C26 C27 1.397(3) . ?
C27 C31 1.446(3) . ?
C27 C28 1.449(3) . ?
C28 C29 1.479(3) . ?
C29 C30 1.433(3) . ?
C30 C31 1.454(3) . ?
C31 C32 1.392(3) . ?
C33 C33 1.551(5) 4_575 ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C34 1.549(4) 4_575 ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.556(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 S1 1.390(8) . ?
C37 S2 1.518(9) . ?
S1 C37 1.390(8) 4_565 ?
C38 C38 1.56(2) 4_575 ?
C38 S4 1.598(10) . ?
C38 S3 1.618(9) . ?
S3 C38 1.618(9) 4_575 ?
C39 C40 1.3900 . ?
C39 C44 1.3900 . ?
C39 H39 0.9500 . ?
C40 C41 1.3900 . ?
C40 H40 0.9500 . ?
C41 C42 1.3900 . ?
C41 H41 0.9500 . ?
C42 C43 1.3900 . ?
C42 H42 0.9500 . ?
C43 C44 1.3900 . ?
C43 H43 0.9500 . ?
C44 H44 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
C34 N1 C33 109.83(16) . . ?
C34 N1 C1 110.51(15) . . ?
C33 N1 C1 109.66(15) . . ?
C36 N2 C36 108.9(2) . 4_575 ?
C36 N2 C14 109.79(14) . . ?
C36 N2 C14 109.79(14) 4_575 . ?
C35 N3 C35 109.0(2) . 4_575 ?
C35 N3 C15 109.95(13) . . ?
C35 N3 C15 109.95(13) 4_575 . ?
N1 C1 C18 109.97(14) . . ?
N1 C1 C2 110.83(14) . . ?
C18 C1 C2 99.86(15) . . ?
N1 C1 C1 107.78(10) . 4_575 ?
C18 C1 C1 114.06(10) . 4_575 ?
C2 C1 C1 114.20(10) . 4_575 ?
C3 C2 C20 119.00(17) . . ?
C3 C2 C1 124.33(18) . . ?
C20 C2 C1 110.05(15) . . ?
C2 C3 C4 120.53(18) . . ?
C2 C3 C3 120.50(12) . 4_575 ?
C4 C3 C3 107.39(12) . 4_575 ?
C22 C4 C5 119.98(19) . . ?
C22 C4 C3 120.33(18) . . ?
C5 C4 C3 108.22(19) . . ?
C6 C5 C4 120.12(15) . . ?
C6 C5 C4 120.12(15) . 4_575 ?
C4 C5 C4 108.8(2) . 4_575 ?
C5 C6 C7 119.96(15) . . ?
C5 C6 C7 119.96(15) . 4_575 ?
C7 C6 C7 108.3(3) . 4_575 ?
C23 C7 C6 119.9(2) . . ?
C23 C7 C8 120.50(19) . . ?
C6 C7 C8 107.9(2) . . ?
C9 C8 C7 119.8(2) . . ?
C9 C8 C8 119.92(13) . 4_575 ?
C7 C8 C8 107.99(13) . 4_575 ?
C8 C9 C10 119.9(2) . . ?
C8 C9 C25 120.05(19) . . ?
C10 C9 C25 107.95(17) . . ?
C10 C10 C9 120.17(12) 4_575 . ?
C10 C10 C11 120.19(12) 4_575 . ?
C9 C10 C11 107.61(19) . . ?
C12 C11 C26 119.48(18) . . ?
C12 C11 C10 119.8(2) . . ?
C26 C11 C10 108.55(17) . . ?
C11 C12 C13 121.00(19) . . ?
C11 C12 C12 119.99(12) . 4_575 ?
C13 C12 C12 108.34(12) . 4_575 ?
C28 C13 C12 119.24(17) . . ?
C28 C13 C14 124.58(17) . . ?
C12 C13 C14 109.94(18) . . ?
N2 C14 C13 109.79(15) . . ?
N2 C14 C13 109.80(15) . 4_575 ?
C13 C14 C13 100.0(2) . 4_575 ?
N2 C14 C15 109.2(2) . . ?
C13 C14 C15 113.88(14) . . ?
C13 C14 C15 113.88(14) 4_575 . ?
N3 C15 C16 110.32(14) . . ?
N3 C15 C16 110.32(14) . 4_575 ?
C16 C15 C16 99.90(19) . 4_575 ?
N3 C15 C14 107.56(19) . . ?
C16 C15 C14 114.31(13) . . ?
C16 C15 C14 114.31(13) 4_575 . ?
C29 C16 C17 119.45(16) . . ?
C29 C16 C15 123.99(17) . . ?
C17 C16 C15 110.41(15) . . ?
C18 C17 C16 121.57(16) . . ?
C18 C17 C17 120.48(10) . 4_575 ?
C16 C17 C17 107.87(10) . 4_575 ?
C17 C18 C19 118.53(16) . . ?
C17 C18 C1 124.52(16) . . ?
C19 C18 C1 110.24(15) . . ?
C30 C19 C18 120.56(17) . . ?
C30 C19 C20 120.09(17) . . ?
C18 C19 C20 108.70(16) . . ?
C21 C20 C2 121.47(18) . . ?
C21 C20 C19 119.74(18) . . ?
C2 C20 C19 107.79(16) . . ?
C20 C21 C22 119.29(18) . . ?
C20 C21 C32 120.32(17) . . ?
C22 C21 C32 107.97(17) . . ?
C4 C22 C21 119.32(18) . . ?
C4 C22 C23 119.83(19) . . ?
C21 C22 C23 108.38(18) . . ?
C7 C23 C24 119.79(19) . . ?
C7 C23 C22 120.2(2) . . ?
C24 C23 C22 107.77(18) . . ?
C25 C24 C32 120.23(18) . . ?
C25 C24 C23 119.9(2) . . ?
C32 C24 C23 107.78(18) . . ?
C24 C25 C26 119.77(19) . . ?
C24 C25 C9 119.95(19) . . ?
C26 C25 C9 107.95(19) . . ?
C27 C26 C11 119.46(18) . . ?
C27 C26 C25 119.92(19) . . ?
C11 C26 C25 107.95(18) . . ?
C26 C27 C31 119.99(18) . . ?
C26 C27 C28 119.92(19) . . ?
C31 C27 C28 108.52(17) . . ?
C13 C28 C27 120.84(18) . . ?
C13 C28 C29 120.07(17) . . ?
C27 C28 C29 107.18(16) . . ?
C16 C29 C30 120.17(17) . . ?
C16 C29 C28 120.95(17) . . ?
C30 C29 C28 107.75(16) . . ?
C19 C30 C29 119.56(17) . . ?
C19 C30 C31 119.97(17) . . ?
C29 C30 C31 108.66(16) . . ?
C32 C31 C27 120.47(19) . . ?
C32 C31 C30 120.01(18) . . ?
C27 C31 C30 107.89(16) . . ?
C31 C32 C24 119.62(19) . . ?
C31 C32 C21 119.87(18) . . ?
C24 C32 C21 108.11(18) . . ?
N1 C33 C33 109.44(11) . 4_575 ?
N1 C33 H33A 109.8 . . ?
C33 C33 H33A 109.8 4_575 . ?
N1 C33 H33B 109.8 . . ?
C33 C33 H33B 109.8 4_575 . ?
H33A C33 H33B 108.2 . . ?
N1 C34 C34 109.57(11) . 4_575 ?
N1 C34 H34A 109.8 . . ?
C34 C34 H34A 109.8 4_575 . ?
N1 C34 H34B 109.8 . . ?
C34 C34 H34B 109.8 4_575 . ?
H34A C34 H34B 108.2 . . ?
N3 C35 C36 109.27(17) . . ?
N3 C35 H35A 109.8 . . ?
C36 C35 H35A 109.8 . . ?
N3 C35 H35B 109.8 . . ?
C36 C35 H35B 109.8 . . ?
H35A C35 H35B 108.3 . . ?
N2 C36 C35 110.51(18) . . ?
N2 C36 H36A 109.5 . . ?
C35 C36 H36A 109.5 . . ?
N2 C36 H36B 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
S1 C37 S2 178.3(8) . . ?
C37 S1 C37 157.3(8) 4_565 . ?
C38 C38 S4 110.4(5) 4_575 . ?
C38 C38 S3 61.1(4) 4_575 . ?
S4 C38 S3 170.9(9) . . ?
C38 S3 C38 57.8(8) 4_575 . ?
C40 C39 C44 120.0 . . ?
C40 C39 H39 120.0 . . ?
C44 C39 H39 120.0 . . ?
C41 C40 C39 120.0 . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 C42 120.0 . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 120.0 . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C44 C43 C42 120.0 . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C39 120.0 . . ?
C43 C44 H44 120.0 . . ?
C39 C44 H44 120.0 . . ?

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
C34 N1 C1 C18 64.6(2) . . . . ?
C33 N1 C1 C18 -174.16(16) . . . . ?
C34 N1 C1 C2 174.08(16) . . . . ?
C33 N1 C1 C2 -64.7(2) . . . . ?
C34 N1 C1 C1 -60.28(15) . . . 4_575 ?
C33 N1 C1 C1 60.94(15) . . . 4_575 ?
N1 C1 C2 C3 110.7(2) . . . . ?
C18 C1 C2 C3 -133.42(19) . . . . ?
C1 C1 C2 C3 -11.3(2) 4_575 . . . ?
N1 C1 C2 C20 -98.40(18) . . . . ?
C18 C1 C2 C20 17.51(19) . . . . ?
C1 C1 C2 C20 139.65(12) 4_575 . . . ?
C20 C2 C3 C4 2.0(3) . . . . ?
C1 C2 C3 C4 150.55(18) . . . . ?
C20 C2 C3 C3 -136.59(13) . . . 4_575 ?
C1 C2 C3 C3 12.0(2) . . . 4_575 ?
C2 C3 C4 C22 0.1(3) . . . . ?
C3 C3 C4 C22 143.46(16) 4_575 . . . ?
C2 C3 C4 C5 -143.2(2) . . . . ?
C3 C3 C4 C5 0.12(17) 4_575 . . . ?
C22 C4 C5 C6 0.4(3) . . . . ?
C3 C4 C5 C6 143.9(2) . . . . ?
C22 C4 C5 C4 -143.69(16) . . . 4_575 ?
C3 C4 C5 C4 -0.2(3) . . . 4_575 ?
C4 C5 C6 C7 -0.7(3) . . . . ?
C4 C5 C6 C7 139.3(2) 4_575 . . . ?
C4 C5 C6 C7 -139.3(2) . . . 4_575 ?
C4 C5 C6 C7 0.7(3) 4_575 . . 4_575 ?
C5 C6 C7 C23 0.5(3) . . . . ?
C7 C6 C7 C23 143.41(17) 4_575 . . . ?
C5 C6 C7 C8 -142.6(2) . . . . ?
C7 C6 C7 C8 0.3(3) 4_575 . . . ?
C23 C7 C8 C9 -0.8(3) . . . . ?
C6 C7 C8 C9 142.0(2) . . . . ?
C23 C7 C8 C8 -143.04(16) . . . 4_575 ?
C6 C7 C8 C8 -0.16(17) . . . 4_575 ?
C7 C8 C9 C10 -137.4(2) . . . . ?
C8 C8 C9 C10 0.3(2) 4_575 . . . ?
C7 C8 C9 C25 0.6(3) . . . . ?
C8 C8 C9 C25 138.33(15) 4_575 . . . ?
C8 C9 C10 C10 -0.3(2) . . . 4_575 ?
C25 C9 C10 C10 -142.83(12) . . . 4_575 ?
C8 C9 C10 C11 142.32(19) . . . . ?
C25 C9 C10 C11 -0.2(2) . . . . ?
C10 C10 C11 C12 0.7(2) 4_575 . . . ?
C9 C10 C11 C12 -141.96(19) . . . . ?
C10 C10 C11 C26 142.89(12) 4_575 . . . ?
C9 C10 C11 C26 0.3(2) . . . . ?
C26 C11 C12 C13 1.6(3) . . . . ?
C10 C11 C12 C13 139.77(19) . . . . ?
C26 C11 C12 C12 -138.82(15) . . . 4_575 ?
C10 C11 C12 C12 -0.7(2) . . . 4_575 ?
C11 C12 C13 C28 -2.7(3) . . . . ?
C12 C12 C13 C28 141.75(15) 4_575 . . . ?
C11 C12 C13 C14 -156.23(19) . . . . ?
C12 C12 C13 C14 -11.78(16) 4_575 . . . ?
C36 N2 C14 C13 174.65(17) . . . . ?
C36 N2 C14 C13 -65.6(2) 4_575 . . . ?
C36 N2 C14 C13 65.6(2) . . . 4_575 ?
C36 N2 C14 C13 -174.65(17) 4_575 . . 4_575 ?
C36 N2 C14 C15 -59.87(15) . . . . ?
C36 N2 C14 C15 59.87(15) 4_575 . . . ?
C28 C13 C14 N2 110.3(2) . . . . ?
C12 C13 C14 N2 -97.86(19) . . . . ?
C28 C13 C14 C13 -134.26(16) . . . 4_575 ?
C12 C13 C14 C13 17.6(2) . . . 4_575 ?
C28 C13 C14 C15 -12.4(3) . . . . ?
C12 C13 C14 C15 139.41(16) . . . . ?
C35 N3 C15 C16 -174.73(16) . . . . ?
C35 N3 C15 C16 65.3(2) 4_575 . . . ?
C35 N3 C15 C16 -65.3(2) . . . 4_575 ?
C35 N3 C15 C16 174.73(16) 4_575 . . 4_575 ?
C35 N3 C15 C14 59.99(14) . . . . ?
C35 N3 C15 C14 -59.99(14) 4_575 . . . ?
N2 C14 C15 N3 0.000(1) . . . . ?
C13 C14 C15 N3 123.08(14) . . . . ?
C13 C14 C15 N3 -123.08(14) 4_575 . . . ?
N2 C14 C15 C16 -122.86(14) . . . . ?
C13 C14 C15 C16 0.2(2) . . . . ?
C13 C14 C15 C16 114.05(16) 4_575 . . . ?
N2 C14 C15 C16 122.87(14) . . . 4_575 ?
C13 C14 C15 C16 -114.05(16) . . . 4_575 ?
C13 C14 C15 C16 -0.2(2) 4_575 . . 4_575 ?
N3 C15 C16 C29 -109.7(2) . . . . ?
C16 C15 C16 C29 134.16(15) 4_575 . . . ?
C14 C15 C16 C29 11.7(3) . . . . ?
N3 C15 C16 C17 98.22(17) . . . . ?
C16 C15 C16 C17 -17.9(2) 4_575 . . . ?
C14 C15 C16 C17 -140.43(16) . . . . ?
C29 C16 C17 C18 3.9(3) . . . . ?
C15 C16 C17 C18 157.45(17) . . . . ?
C29 C16 C17 C17 -141.52(14) . . . 4_575 ?
C15 C16 C17 C17 12.00(16) . . . 4_575 ?
C16 C17 C18 C19 -4.5(3) . . . . ?
C17 C17 C18 C19 136.68(13) 4_575 . . . ?
C16 C17 C18 C1 -152.96(17) . . . . ?
C17 C17 C18 C1 -11.7(2) 4_575 . . . ?
N1 C1 C18 C17 -110.13(19) . . . . ?
C2 C1 C18 C17 133.31(18) . . . . ?
C1 C1 C18 C17 11.1(2) 4_575 . . . ?
N1 C1 C18 C19 99.23(17) . . . . ?
C2 C1 C18 C19 -17.34(18) . . . . ?
C1 C1 C18 C19 -139.57(11) 4_575 . . . ?
C17 C18 C19 C30 3.4(3) . . . . ?
C1 C18 C19 C30 156.02(17) . . . . ?
C17 C18 C19 C20 -141.15(17) . . . . ?
C1 C18 C19 C20 11.5(2) . . . . ?
C3 C2 C20 C21 -3.1(3) . . . . ?
C1 C2 C20 C21 -155.75(17) . . . . ?
C3 C2 C20 C19 140.75(18) . . . . ?
C1 C2 C20 C19 -11.9(2) . . . . ?
C30 C19 C20 C21 0.1(3) . . . . ?
C18 C19 C20 C21 144.87(18) . . . . ?
C30 C19 C20 C2 -144.42(18) . . . . ?
C18 C19 C20 C2 0.3(2) . . . . ?
C2 C20 C21 C22 1.9(3) . . . . ?
C19 C20 C21 C22 -137.76(19) . . . . ?
C2 C20 C21 C32 139.4(2) . . . . ?
C19 C20 C21 C32 -0.2(3) . . . . ?
C5 C4 C22 C21 137.8(2) . . . . ?
C3 C4 C22 C21 -1.3(3) . . . . ?
C5 C4 C22 C23 0.1(3) . . . . ?
C3 C4 C22 C23 -138.94(19) . . . . ?
C20 C21 C22 C4 0.3(3) . . . . ?
C32 C21 C22 C4 -141.92(19) . . . . ?
C20 C21 C22 C23 142.28(19) . . . . ?
C32 C21 C22 C23 0.1(2) . . . . ?
C6 C7 C23 C24 -137.8(2) . . . . ?
C8 C7 C23 C24 0.8(3) . . . . ?
C6 C7 C23 C22 0.0(3) . . . . ?
C8 C7 C23 C22 138.5(2) . . . . ?
C4 C22 C23 C7 -0.4(3) . . . . ?
C21 C22 C23 C7 -142.10(19) . . . . ?
C4 C22 C23 C24 141.88(19) . . . . ?
C21 C22 C23 C24 0.1(2) . . . . ?
C7 C23 C24 C25 -0.5(3) . . . . ?
C22 C23 C24 C25 -142.88(19) . . . . ?
C7 C23 C24 C32 142.17(19) . . . . ?
C22 C23 C24 C32 -0.3(2) . . . . ?
C32 C24 C25 C26 -0.1(3) . . . . ?
C23 C24 C25 C26 137.9(2) . . . . ?
C32 C24 C25 C9 -137.8(2) . . . . ?
C23 C24 C25 C9 0.2(3) . . . . ?
C8 C9 C25 C24 -0.3(3) . . . . ?
C10 C9 C25 C24 142.16(19) . . . . ?
C8 C9 C25 C26 -142.41(19) . . . . ?
C10 C9 C25 C26 0.1(2) . . . . ?
C12 C11 C26 C27 0.4(3) . . . . ?
C10 C11 C26 C27 -141.98(19) . . . . ?
C12 C11 C26 C25 142.14(19) . . . . ?
C10 C11 C26 C25 -0.2(2) . . . . ?
C24 C25 C26 C27 -0.5(3) . . . . ?
C9 C25 C26 C27 141.6(2) . . . . ?
C24 C25 C26 C11 -142.1(2) . . . . ?
C9 C25 C26 C11 0.1(2) . . . . ?
C11 C26 C27 C31 137.7(2) . . . . ?
C25 C26 C27 C31 0.6(3) . . . . ?
C11 C26 C27 C28 -1.3(3) . . . . ?
C25 C26 C27 C28 -138.5(2) . . . . ?
C12 C13 C28 C27 1.8(3) . . . . ?
C14 C13 C28 C27 151.18(19) . . . . ?
C12 C13 C28 C29 -136.22(18) . . . . ?
C14 C13 C28 C29 13.2(3) . . . . ?
C26 C27 C28 C13 0.2(3) . . . . ?
C31 C27 C28 C13 -143.03(18) . . . . ?
C26 C27 C28 C29 142.89(18) . . . . ?
C31 C27 C28 C29 -0.3(2) . . . . ?
C17 C16 C29 C30 -2.0(3) . . . . ?
C15 C16 C29 C30 -151.77(18) . . . . ?
C17 C16 C29 C28 137.41(18) . . . . ?
C15 C16 C29 C28 -12.3(3) . . . . ?
C13 C28 C29 C16 -0.4(3) . . . . ?
C27 C28 C29 C16 -143.44(18) . . . . ?
C13 C28 C29 C30 143.42(18) . . . . ?
C27 C28 C29 C30 0.4(2) . . . . ?
C18 C19 C30 C29 -1.6(3) . . . . ?
C20 C19 C30 C29 138.96(19) . . . . ?
C18 C19 C30 C31 -140.36(19) . . . . ?
C20 C19 C30 C31 0.2(3) . . . . ?
C16 C29 C30 C19 1.0(3) . . . . ?
C28 C29 C30 C19 -143.20(18) . . . . ?
C16 C29 C30 C31 143.87(18) . . . . ?
C28 C29 C30 C31 -0.3(2) . . . . ?
C26 C27 C31 C32 0.1(3) . . . . ?
C28 C27 C31 C32 143.26(19) . . . . ?
C26 C27 C31 C30 -143.04(19) . . . . ?
C28 C27 C31 C30 0.2(2) . . . . ?
C19 C30 C31 C32 -0.5(3) . . . . ?
C29 C30 C31 C32 -143.21(19) . . . . ?
C19 C30 C31 C27 142.82(18) . . . . ?
C29 C30 C31 C27 0.1(2) . . . . ?
C27 C31 C32 C24 -0.7(3) . . . . ?
C30 C31 C32 C24 138.0(2) . . . . ?
C27 C31 C32 C21 -138.3(2) . . . . ?
C30 C31 C32 C21 0.4(3) . . . . ?
C25 C24 C32 C31 0.7(3) . . . . ?
C23 C24 C32 C31 -141.76(19) . . . . ?
C25 C24 C32 C21 142.8(2) . . . . ?
C23 C24 C32 C21 0.3(2) . . . . ?
C20 C21 C32 C31 0.0(3) . . . . ?
C22 C21 C32 C31 141.73(19) . . . . ?
C20 C21 C32 C24 -141.98(19) . . . . ?
C22 C21 C32 C24 -0.2(2) . . . . ?
C34 N1 C33 C33 59.67(15) . . . 4_575 ?
C1 N1 C33 C33 -61.96(14) . . . 4_575 ?
C33 N1 C34 C34 -59.75(15) . . . 4_575 ?
C1 N1 C34 C34 61.37(14) . . . 4_575 ?
C35 N3 C35 C36 60.0(2) 4_575 . . . ?
C15 N3 C35 C36 -60.6(2) . . . . ?
C36 N2 C36 C35 -59.1(3) 4_575 . . . ?
C14 N2 C36 C35 61.2(2) . . . . ?
N3 C35 C36 N2 -0.3(2) . . . . ?
C44 C39 C40 C41 0.0 . . . . ?
C39 C40 C41 C42 0.0 . . . . ?
C40 C41 C42 C43 0.0 . . . . ?
C41 C42 C43 C44 0.0 . . . . ?
C42 C43 C44 C39 0.0 . . . . ?
C40 C39 C44 C43 0.0 . . . . ?

_refine_diff_density_max         3.182
_refine_diff_density_min         -2.267
_refine_diff_density_rms         0.171


# start Validation Reply Form
_vrf_PLAT431_aa96                
;
PROBLEM: Short Inter HL..A  Contact I2..N3  .. 2.59 Ang. 
RESPONSE: I2 is acting as a mild Lewis acid and there is a 
lewis acid-base interaction between I2 and N3.
;

_vrf_PLAT971_aa96                
;
PROBLEM: Check Calcd Residual Density  0.73A From I1 .. 2.92 eA-3.  
RESPONSE: This Alert is due to presence of residual density in the
presence of heavy atom (I).
;
_exptl_crystal_recrystallization_method 
'diffusion of a CS2 solution of the fullerene with a solution of I2 in benzene'
_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# 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_aa97
_database_code_depnum_ccdc_archive 'CCDC 1574808'
_audit_update_record             
;
2017-11-03 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            '{(e(N2C4H8)2C60)(Rh2(O2CCH3)4)2}n 0.5CS2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H34 N4 O12 Rh3, 0.5(C S2)'
_chemical_formula_sum            'C80.50 H34 N4 O12 Rh3 S'
_chemical_formula_weight         1589.91

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'
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'
Rh Rh 0.0927 3.6045 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 2/m'
_space_group_name_Hall           '-I 2y'

_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'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   15.8849(8)
_cell_length_b                   18.9471(10)
_cell_length_c                   19.6812(18)
_cell_angle_alpha                90
_cell_angle_beta                 90.063(2)
_cell_angle_gamma                90
_cell_volume                     5923.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    9829
_cell_measurement_theta_min      3.58
_cell_measurement_theta_max      71.32

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_F_000             3168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.079
_exptl_absorpt_coefficient_mu    7.662
_shelx_estimated_absorpt_T_min   0.514
_shelx_estimated_absorpt_T_max   0.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5158
_exptl_absorpt_correction_T_max  0.7537
_exptl_absorpt_process_details   SADABS-2014/3
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-DUO'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            33873
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.238
_diffrn_reflns_theta_max         63.722
_diffrn_reflns_theta_full        63.722
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4926
_reflns_number_gt                4699
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       'Apex2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0950P)²+137.7951P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4926
_refine_ls_number_parameters     500
_refine_ls_number_restraints     473
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0762
_refine_ls_wR_factor_ref         0.2055
_refine_ls_wR_factor_gt          0.2016
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.000
_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
Rh1 Rh 0.72152(4) 0.30874(3) 0.74860(6) 0.0330(3) Uani 1 1 d . . . . .
Rh2 Rh 0.07342(9) 0.500000 0.98501(10) 0.0503(5) Uani 1 2 d S TU P . .
O1 O 0.6143(10) 0.2687(9) 0.7896(9) 0.035(2) Uani 0.5 1 d . U P A 1
O2 O 0.6626(11) 0.1586(9) 0.7795(10) 0.033(2) Uani 0.5 1 d . U P A 1
O3 O 0.7693(13) 0.3142(9) 0.8452(9) 0.042(3) Uani 0.5 1 d . U P A 1
O4 O 0.8190(13) 0.1998(9) 0.8422(9) 0.039(3) Uani 0.5 1 d . U P A 1
O5 O 0.7027(11) 0.3034(9) 0.8506(9) 0.036(2) Uani 0.5 1 d . U P A 2
O6 O 0.7605(12) 0.1957(9) 0.8571(9) 0.036(3) Uani 0.5 1 d . U P A 2
O7 O 0.6055(9) 0.2605(7) 0.7320(8) 0.027(2) Uani 0.5 1 d . U P A 2
O8 O 0.6634(9) 0.1521(8) 0.7378(9) 0.027(2) Uani 0.5 1 d . U P A 2
O9 O 0.0343(11) 0.500000 0.8860(10) 0.077(4) Uani 1 2 d S TU P . .
O10 O -0.1019(12) 0.500000 0.9138(10) 0.084(4) Uani 1 2 d S TU P . .
O12 O 0.0698(9) 0.3962(6) 0.9864(8) 0.078(3) Uani 1 1 d . U . . .
N1 N 0.6737(5) 0.4309(4) 0.7423(6) 0.0306(17) Uani 1 1 d . U . . .
N2 N 0.2284(13) 0.500000 0.9631(11) 0.072(3) Uani 1 2 d S TU P . .
N3 N 0.3903(13) 0.500000 0.9770(13) 0.080(4) Uani 1 2 d S TU P . .
C1 C 0.3697(14) 0.500000 0.9021(13) 0.063(3) Uani 1 2 d S TU P . .
C2 C 0.2676(13) 0.500000 0.8960(12) 0.059(3) Uani 1 2 d S TU P . .
C3 C 0.2330(7) 0.4381(7) 0.8527(8) 0.048(2) Uani 1 1 d . U . . .
C4 C 0.1686(8) 0.4625(7) 0.8067(9) 0.047(2) Uani 1 1 d . U . . .
C5 C 0.1487(7) 0.4247(6) 0.7478(11) 0.051(2) Uani 1 1 d . U . . .
C6 C 0.1302(9) 0.4636(8) 0.6854(10) 0.057(3) Uani 1 1 d . U . . .
C7 C 0.1654(10) 0.4269(10) 0.6301(11) 0.068(3) Uani 1 1 d . U . . .
C8 C 0.1991(10) 0.4626(11) 0.5746(11) 0.076(3) Uani 1 1 d . U . . .
C9 C 0.2774(11) 0.4382(11) 0.5459(10) 0.076(3) Uani 1 1 d . U . . .
C10 C 0.3245(15) 0.500000 0.5305(15) 0.072(4) Uani 1 2 d S TU P . .
C11 C 0.4148(14) 0.500000 0.5411(14) 0.068(4) Uani 1 2 d S TU P . .
C12 C 0.4559(9) 0.4381(9) 0.5699(9) 0.060(3) Uani 1 1 d . U . . .
C13 C 0.5254(8) 0.4621(8) 0.6115(8) 0.050(3) Uani 1 1 d . U . . .
C14 C 0.5458(7) 0.4247(6) 0.6706(8) 0.042(2) Uani 1 1 d . U . . .
C15 C 0.5843(6) 0.4570(5) 0.7337(7) 0.034(2) Uani 1 1 d . U . . .
C16 C 0.5283(7) 0.4244(6) 0.7888(7) 0.038(2) Uani 1 1 d . U . . .
C17 C 0.4917(8) 0.4605(6) 0.8410(8) 0.044(2) Uani 1 1 d . U . . .
C18 C 0.4137(8) 0.4392(8) 0.8689(8) 0.051(2) Uani 1 1 d . U . . .
C19 C 0.3728(8) 0.3805(7) 0.8450(8) 0.051(2) Uani 1 1 d . U . . .
C20 C 0.2789(8) 0.3798(7) 0.8336(8) 0.050(2) Uani 1 1 d . U . . .
C21 C 0.2608(7) 0.3410(6) 0.7737(8) 0.050(2) Uani 1 1 d . U . . .
C22 C 0.1978(7) 0.3632(6) 0.7317(9) 0.052(2) Uani 1 1 d . U . . .
C23 C 0.2054(9) 0.3621(8) 0.6572(10) 0.061(3) Uani 1 1 d . U . . .
C24 C 0.2822(10) 0.3414(8) 0.6283(10) 0.063(2) Uani 1 1 d . U . . .
C25 C 0.3162(10) 0.3791(10) 0.5741(10) 0.069(3) Uani 1 1 d . U . . .
C26 C 0.4105(9) 0.3807(10) 0.5839(10) 0.064(3) Uani 1 1 d . U . . .
C27 C 0.4291(9) 0.3403(7) 0.6449(10) 0.058(2) Uani 1 1 d . U . . .
C28 C 0.4955(8) 0.3648(6) 0.6899(9) 0.045(2) Uani 1 1 d . U . . .
C29 C 0.4863(7) 0.3652(5) 0.7620(8) 0.041(2) Uani 1 1 d . U . . .
C30 C 0.4094(8) 0.3426(6) 0.7886(9) 0.049(2) Uani 1 1 d . U . . .
C31 C 0.3409(7) 0.3184(5) 0.7446(11) 0.051(2) Uani 1 1 d . U . . .
C32 C 0.3505(9) 0.3171(7) 0.6762(10) 0.057(2) Uani 1 1 d . U . . .
C33 C 0.3522(11) 0.4355(12) 1.0081(11) 0.086(4) Uani 1 1 d . U . . .
H33A H 0.368160 0.432922 1.056647 0.104 Uiso 1 1 calc R U . . .
H33B H 0.374452 0.392988 0.985056 0.104 Uiso 1 1 calc R U . . .
C34 C 0.2584(10) 0.4370(12) 1.0018(10) 0.084(4) Uani 1 1 d . U . . .
H34A H 0.239142 0.393623 0.978538 0.101 Uiso 1 1 calc R U . . .
H34B H 0.233175 0.437614 1.047814 0.101 Uiso 1 1 calc R U . . .
C35 C 0.7107(7) 0.4595(6) 0.8098(7) 0.032(2) Uani 1 1 d . U . . .
H35A H 0.676657 0.442029 0.848434 0.039 Uiso 1 1 calc R U . . .
H35B H 0.768968 0.442033 0.815615 0.039 Uiso 1 1 calc R U . . .
C36 C 0.7243(8) 0.4599(5) 0.6872(7) 0.033(2) Uani 1 1 d . U . . .
H36A H 0.701930 0.442764 0.643209 0.040 Uiso 1 1 calc R U . . .
H36B H 0.782912 0.442765 0.691684 0.040 Uiso 1 1 calc R U . . .
C37 C 0.6071(16) 0.2088(14) 0.8000(13) 0.035(2) Uiso 0.5 1 d . U P A 1
C38 C 0.519(3) 0.176(2) 0.818(2) 0.079(7) Uiso 0.5 1 d . U P A 1
H38A H 0.517570 0.126256 0.804376 0.118 Uiso 0.5 1 calc R U P A 1
H38B H 0.474432 0.201761 0.793569 0.118 Uiso 0.5 1 calc R U P A 1
H38C H 0.508989 0.179686 0.866963 0.118 Uiso 0.5 1 calc R U P A 1
C39 C 0.8094(16) 0.2567(14) 0.8748(13) 0.042(3) Uiso 0.5 1 d D U P A 1
C40 C 0.866(2) 0.269(2) 0.9388(16) 0.086(10) Uiso 0.5 1 d D U P A 1
H40A H 0.851741 0.314832 0.959094 0.129 Uiso 0.5 1 calc R U P A 1
H40B H 0.855176 0.231494 0.972034 0.129 Uiso 0.5 1 calc R U P A 1
H40C H 0.925000 0.268526 0.925568 0.129 Uiso 0.5 1 calc R U P A 1
C41 C 0.7245(15) 0.2508(13) 0.8815(9) 0.036(2) Uiso 0.5 1 d D U P A 2
C42 C 0.7103(16) 0.2520(13) 0.9597(9) 0.037(5) Uiso 0.5 1 d D U P A 2
H42A H 0.692906 0.205016 0.975020 0.056 Uiso 0.5 1 calc R U P A 2
H42B H 0.666335 0.286368 0.970727 0.056 Uiso 0.5 1 calc R U P A 2
H42C H 0.762831 0.265334 0.982475 0.056 Uiso 0.5 1 calc R U P A 2
C43 C 0.5984(15) 0.1946(12) 0.7284(11) 0.030(2) Uiso 0.5 1 d . U P A 2
C44 C 0.5170(19) 0.1642(16) 0.7171(16) 0.049(6) Uiso 0.5 1 d . U P A 2
H44A H 0.521945 0.124695 0.685287 0.074 Uiso 0.5 1 calc R U P A 2
H44B H 0.479281 0.200050 0.698030 0.074 Uiso 0.5 1 calc R U P A 2
H44C H 0.494091 0.147207 0.760341 0.074 Uiso 0.5 1 calc R U P A 2
C45 C -0.040(2) 0.500000 0.8776(15) 0.085(4) Uiso 1 2 d DS U P . .
C46 C -0.068(3) 0.500000 0.8013(16) 0.139(11) Uiso 1 2 d DS U P . .
H46A H -0.016620 0.500000 0.770170 0.208 Uiso 1 2 d S U P . .
H46B H -0.098970 0.458630 0.788560 0.208 Uiso 1 1 d . U . . .
C47 C 0.000000 0.3627(16) 1.000000 0.088(5) Uiso 1 2 d DS U P . .
C48 C 0.000000 0.2800(16) 1.000000 0.164(13) Uiso 1 2 d DS U P . .
H48A H 0.056515 0.262796 0.988948 0.245 Uiso 0.5 1 calc R U P . .
H48B H -0.016345 0.262796 1.045040 0.245 Uiso 0.5 1 calc R U P . .
H48C H -0.040171 0.262795 0.966013 0.245 Uiso 0.5 1 calc R U P . .
C49 C 0.538(7) 0.146(6) 0.894(5) 0.104(10) Uiso 0.25 1 d . U P B -2
S1 S 0.501(2) 0.2183(18) 0.9027(18) 0.122(8) Uiso 0.25 1 d . U P B -2
S2 S 0.573(2) 0.0622(19) 0.9193(18) 0.128(9) Uiso 0.25 1 d . U P B -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
Rh1 O4 1.91(2) 7_656 ?
Rh1 O8 1.991(15) 7_656 ?
Rh1 O2 2.020(17) 7_656 ?
Rh1 O5 2.032(17) . ?
Rh1 O1 2.033(16) . ?
Rh1 O3 2.049(19) . ?
Rh1 O7 2.083(15) . ?
Rh1 O6 2.101(17) 7_656 ?
Rh1 Rh1 2.4034(13) 7_656 ?
Rh1 N1 2.440(8) . ?
Rh2 O12 1.967(11) . ?
Rh2 O12 1.968(11) 6_565 ?
Rh2 O10 2.04(2) 5_567 ?
Rh2 O9 2.04(2) . ?
Rh2 Rh2 2.407(3) 5_567 ?
Rh2 N2 2.500(19) . ?
O1 C37 1.16(3) . ?
O2 C37 1.36(3) . ?
O3 C39 1.39(3) . ?
O4 C39 1.26(3) . ?
O5 C41 1.22(3) . ?
O6 C41 1.28(3) . ?
O7 C43 1.26(3) . ?
O8 C43 1.32(3) . ?
O9 C45 1.20(3) . ?
O10 C45 1.21(3) . ?
O12 C47 1.306(18) . ?
N1 C36 1.458(15) . ?
N1 C15 1.513(13) . ?
N1 C35 1.551(17) . ?
N2 C2 1.46(3) . ?
N2 C34 1.49(2) 6_565 ?
N2 C34 1.49(2) . ?
N3 C33 1.49(2) . ?
N3 C33 1.49(2) 6_565 ?
N3 C1 1.51(4) . ?
C1 C18 1.497(18) 6_565 ?
C1 C18 1.498(18) . ?
C1 C2 1.63(3) . ?
C2 C3 1.55(2) . ?
C2 C3 1.55(2) 6_565 ?
C3 C20 1.377(18) . ?
C3 C4 1.44(2) . ?
C4 C5 1.40(2) . ?
C4 C4 1.42(3) 6_565 ?
C5 C22 1.437(17) . ?
C5 C6 1.46(3) . ?
C6 C6 1.38(3) 6_565 ?
C6 C7 1.41(2) . ?
C7 C8 1.39(3) . ?
C7 C23 1.48(3) . ?
C8 C8 1.42(4) 6_565 ?
C8 C9 1.44(2) . ?
C9 C25 1.39(3) . ?
C9 C10 1.42(2) . ?
C10 C11 1.45(3) . ?
C11 C12 1.46(2) . ?
C11 C12 1.46(2) 6_565 ?
C12 C26 1.33(2) . ?
C12 C13 1.45(2) . ?
C13 C14 1.40(2) . ?
C13 C13 1.44(3) 6_565 ?
C14 C28 1.439(17) . ?
C14 C15 1.514(19) . ?
C15 C16 1.533(16) . ?
C15 C15 1.629(18) 6_565 ?
C16 C17 1.366(18) . ?
C16 C29 1.407(17) . ?
C17 C18 1.414(16) . ?
C17 C17 1.50(2) 6_565 ?
C18 C19 1.37(2) . ?
C19 C30 1.44(2) . ?
C19 C20 1.510(19) . ?
C20 C21 1.42(2) . ?
C21 C22 1.36(2) . ?
C21 C31 1.461(17) . ?
C22 C23 1.47(2) . ?
C23 C24 1.40(2) . ?
C24 C25 1.39(3) . ?
C24 C32 1.51(3) . ?
C25 C26 1.51(2) . ?
C26 C27 1.45(3) . ?
C27 C28 1.45(2) . ?
C27 C32 1.462(19) . ?
C28 C29 1.43(2) . ?
C29 C30 1.397(15) . ?
C30 C31 1.46(2) . ?
C31 C32 1.36(3) . ?
C33 C34 1.50(2) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C35 1.53(2) 6_565 ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C36 1.52(2) 6_565 ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.58(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.560(10) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.554(10) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.43(4) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.562(10) . ?
C46 H46A 1.0169 . ?
C46 H46B 0.9617 . ?
C47 C48 1.566(10) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 S1 1.49(11) . ?
C49 S2 1.76(11) . ?

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
O4 Rh1 O8 117.8(8) 7_656 7_656 ?
O4 Rh1 O2 94.4(8) 7_656 7_656 ?
O8 Rh1 O5 91.3(7) 7_656 . ?
O4 Rh1 O1 93.3(8) 7_656 . ?
O2 Rh1 O1 170.9(7) 7_656 . ?
O4 Rh1 O3 177.2(7) 7_656 . ?
O2 Rh1 O3 84.3(8) 7_656 . ?
O1 Rh1 O3 87.8(8) . . ?
O8 Rh1 O7 175.6(6) 7_656 . ?
O5 Rh1 O7 90.1(7) . . ?
O4 Rh1 O6 27.7(7) 7_656 7_656 ?
O2 Rh1 O6 67.4(8) 7_656 7_656 ?
O1 Rh1 O6 119.5(7) . 7_656 ?
O3 Rh1 O6 150.4(8) . 7_656 ?
O4 Rh1 Rh1 94.0(5) 7_656 7_656 ?
O2 Rh1 Rh1 86.9(5) 7_656 7_656 ?
O1 Rh1 Rh1 87.7(5) . 7_656 ?
O3 Rh1 Rh1 83.5(5) . 7_656 ?
O4 Rh1 N1 85.9(6) 7_656 . ?
O8 Rh1 N1 86.5(5) 7_656 . ?
O2 Rh1 N1 88.8(5) 7_656 . ?
O5 Rh1 N1 92.9(5) . . ?
O1 Rh1 N1 96.5(5) . . ?
O3 Rh1 N1 96.6(6) . . ?
O7 Rh1 N1 97.6(4) . . ?
O6 Rh1 N1 91.7(5) 7_656 . ?
Rh1 Rh1 N1 175.72(19) 7_656 . ?
O12 Rh2 O12 176.3(7) . 6_565 ?
O12 Rh2 O10 89.6(5) . 5_567 ?
O12 Rh2 O10 89.6(5) 6_565 5_567 ?
O12 Rh2 O9 90.2(5) . . ?
O12 Rh2 O9 90.2(5) 6_565 . ?
O10 Rh2 O9 175.1(7) 5_567 . ?
O12 Rh2 Rh2 88.2(4) . 5_567 ?
O12 Rh2 Rh2 88.2(4) 6_565 5_567 ?
O10 Rh2 Rh2 88.5(5) 5_567 5_567 ?
O9 Rh2 Rh2 86.6(5) . 5_567 ?
O12 Rh2 N2 91.8(4) . . ?
O12 Rh2 N2 91.8(4) 6_565 . ?
O10 Rh2 N2 87.2(7) 5_567 . ?
O9 Rh2 N2 97.7(7) . . ?
Rh2 Rh2 N2 175.7(6) 5_567 . ?
C37 O1 Rh1 121.3(17) . . ?
C37 O2 Rh1 117.4(15) . 7_656 ?
C39 O3 Rh1 121.3(15) . . ?
C39 O4 Rh1 120.5(17) . 7_656 ?
C41 O5 Rh1 119.5(14) . . ?
C43 O7 Rh1 121.6(14) . . ?
C45 O9 Rh2 115.6(18) . . ?
C45 O10 Rh2 113(2) . 5_567 ?
C47 O12 Rh2 120.9(14) . . ?
C36 N1 C15 108.2(10) . . ?
C36 N1 C35 107.3(8) . . ?
C15 N1 C35 109.6(9) . . ?
C36 N1 Rh1 102.9(6) . . ?
C15 N1 Rh1 127.4(6) . . ?
C35 N1 Rh1 99.8(6) . . ?
C2 N2 C34 109.0(12) . 6_565 ?
C2 N2 C34 109.0(12) . . ?
C34 N2 C34 106(2) 6_565 . ?
C2 N2 Rh2 125.2(16) . . ?
C34 N2 Rh2 103.0(9) 6_565 . ?
C34 N2 Rh2 103.0(9) . . ?
C33 N3 C33 110(2) . 6_565 ?
C33 N3 C1 108.2(16) . . ?
C33 N3 C1 108.2(16) 6_565 . ?
C18 C1 C18 100.5(14) 6_565 . ?
C18 C1 N3 108.9(15) 6_565 . ?
C18 C1 N3 108.9(15) . . ?
C18 C1 C2 115.7(14) 6_565 . ?
C18 C1 C2 115.7(14) . . ?
N3 C1 C2 106.8(16) . . ?
N2 C2 C3 110.3(11) . . ?
N2 C2 C3 110.3(11) . 6_565 ?
C3 C2 C3 98.3(18) . 6_565 ?
N2 C2 C1 111(2) . . ?
C3 C2 C1 113.2(10) . . ?
C3 C2 C1 113.2(10) 6_565 . ?
C20 C3 C4 117.5(14) . . ?
C20 C3 C2 124.7(13) . . ?
C4 C3 C2 110.7(13) . . ?
C5 C4 C4 120.8(9) . 6_565 ?
C5 C4 C3 121.0(12) . . ?
C4 C4 C3 108.7(7) 6_565 . ?
C4 C5 C22 118.4(15) . . ?
C4 C5 C6 118.9(12) . . ?
C22 C5 C6 109.4(15) . . ?
C6 C6 C7 119.7(10) 6_565 . ?
C6 C6 C5 120.3(8) 6_565 . ?
C7 C6 C5 108.7(15) . . ?
C8 C7 C6 121.2(17) . . ?
C8 C7 C23 121.3(15) . . ?
C6 C7 C23 107.6(18) . . ?
C7 C8 C8 119.1(11) . 6_565 ?
C7 C8 C9 119.0(19) . . ?
C8 C8 C9 108.7(12) 6_565 . ?
C25 C9 C10 121.0(18) . . ?
C25 C9 C8 118.8(18) . . ?
C10 C9 C8 105.9(17) . . ?
C9 C10 C9 111(2) . 6_565 ?
C9 C10 C11 119.4(15) . . ?
C9 C10 C11 119.4(15) 6_565 . ?
C10 C11 C12 119.9(11) . . ?
C10 C11 C12 119.9(11) . 6_565 ?
C12 C11 C12 107(2) . 6_565 ?
C26 C12 C13 123.5(18) . . ?
C26 C12 C11 119.7(15) . . ?
C13 C12 C11 108.0(16) . . ?
C14 C13 C13 120.5(8) . 6_565 ?
C14 C13 C12 119.1(13) . . ?
C13 C13 C12 108.3(10) 6_565 . ?
C13 C14 C28 119.4(14) . . ?
C13 C14 C15 124.7(11) . . ?
C28 C14 C15 109.1(13) . . ?
N1 C15 C14 109.8(9) . . ?
N1 C15 C16 109.6(10) . . ?
C14 C15 C16 100.5(9) . . ?
N1 C15 C15 109.0(5) . 6_565 ?
C14 C15 C15 113.9(6) . 6_565 ?
C16 C15 C15 113.8(6) . 6_565 ?
C17 C16 C29 118.5(10) . . ?
C17 C16 C15 125.3(10) . . ?
C29 C16 C15 109.4(12) . . ?
C16 C17 C18 121.7(13) . . ?
C16 C17 C17 120.0(7) . 6_565 ?
C18 C17 C17 106.5(8) . 6_565 ?
C19 C18 C17 120.8(13) . . ?
C19 C18 C1 123.6(12) . . ?
C17 C18 C1 111.2(12) . . ?
C18 C19 C30 118.5(11) . . ?
C18 C19 C20 121.7(12) . . ?
C30 C19 C20 106.2(14) . . ?
C3 C20 C21 122.4(14) . . ?
C3 C20 C19 118.5(13) . . ?
C21 C20 C19 109.1(12) . . ?
C22 C21 C20 119.5(12) . . ?
C22 C21 C31 119.5(15) . . ?
C20 C21 C31 107.6(12) . . ?
C21 C22 C5 120.9(15) . . ?
C21 C22 C23 122.6(12) . . ?
C5 C22 C23 106.1(15) . . ?
C24 C23 C22 118.8(16) . . ?
C24 C23 C7 117.3(16) . . ?
C22 C23 C7 108.1(13) . . ?
C25 C24 C23 120.4(18) . . ?
C25 C24 C32 110.9(14) . . ?
C23 C24 C32 117.1(17) . . ?
C24 C25 C9 123.1(15) . . ?
C24 C25 C26 107.3(19) . . ?
C9 C25 C26 118.2(17) . . ?
C12 C26 C27 119.4(16) . . ?
C12 C26 C25 121.7(18) . . ?
C27 C26 C25 107.2(16) . . ?
C28 C27 C26 118.9(13) . . ?
C28 C27 C32 117.3(15) . . ?
C26 C27 C32 109.5(15) . . ?
C29 C28 C14 108.4(12) . . ?
C29 C28 C27 122.3(11) . . ?
C14 C28 C27 119.6(15) . . ?
C30 C29 C16 121.3(12) . . ?
C30 C29 C28 117.5(13) . . ?
C16 C29 C28 109.2(11) . . ?
C29 C30 C19 119.2(12) . . ?
C29 C30 C31 121.6(15) . . ?
C19 C30 C31 108.2(11) . . ?
C32 C31 C21 119.6(15) . . ?
C32 C31 C30 120.7(12) . . ?
C21 C31 C30 108.9(14) . . ?
C31 C32 C27 120.6(15) . . ?
C31 C32 C24 122.3(13) . . ?
C27 C32 C24 105.0(15) . . ?
N3 C33 C34 110.8(19) . . ?
N3 C33 H33A 109.5 . . ?
C34 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 108.1 . . ?
N2 C34 C33 112.0(17) . . ?
N2 C34 H34A 109.2 . . ?
C33 C34 H34A 109.2 . . ?
N2 C34 H34B 109.2 . . ?
C33 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
C35 C35 N1 110.4(5) 6_565 . ?
C35 C35 H35A 109.6 6_565 . ?
N1 C35 H35A 109.6 . . ?
C35 C35 H35B 109.6 6_565 . ?
N1 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
N1 C36 C36 112.1(5) . 6_565 ?
N1 C36 H36A 109.2 . . ?
C36 C36 H36A 109.2 6_565 . ?
N1 C36 H36B 109.2 . . ?
C36 C36 H36B 109.2 6_565 . ?
H36A C36 H36B 107.9 . . ?
O1 C37 O2 125(2) . . ?
O1 C37 C38 121(3) . . ?
O2 C37 C38 112(2) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O4 C39 O3 121(2) . . ?
O4 C39 C40 118(3) . . ?
O3 C39 C40 119(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O5 C41 O6 127.2(18) . . ?
O5 C41 C42 116(2) . . ?
O6 C41 C42 117(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O7 C43 O8 122(2) . . ?
O7 C43 C44 119(2) . . ?
O8 C43 C44 119(2) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O9 C45 O10 136(3) . . ?
O9 C45 C46 114(3) . . ?
O10 C45 C46 110(3) . . ?
C45 C46 H46A 111.0 . . ?
C45 C46 H46B 113.2 . . ?
H46A C46 H46B 104.8 . . ?
C45 C46 H46B 113(2) . 6_565 ?
H46A C46 H46B 104.8 . 6_565 ?
H46B C46 H46B 109.2 . 6_565 ?
O12 C47 O12 122(2) 2_557 . ?
O12 C47 C48 119.1(12) 2_557 . ?
O12 C47 C48 119.1(12) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C48 H48A 109.470(6) . 2_557 ?
H48A C48 H48A 141.1 . 2_557 ?
H48B C48 H48A 56.2 . 2_557 ?
H48C C48 H48A 56.3 . 2_557 ?
C47 C48 H48B 109.471(10) . 2_557 ?
H48A C48 H48B 56.3 . 2_557 ?
H48B C48 H48B 141.1 . 2_557 ?
H48C C48 H48B 56.2 . 2_557 ?
H48A C48 H48B 109.5 2_557 2_557 ?
C47 C48 H48C 109.472(14) . 2_557 ?
H48A C48 H48C 56.3 . 2_557 ?
H48B C48 H48C 56.2 . 2_557 ?
H48C C48 H48C 141.1 . 2_557 ?
H48A C48 H48C 109.5 2_557 2_557 ?
H48B C48 H48C 109.5 2_557 2_557 ?
S1 C49 S2 157(8) . . ?

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
C33 N3 C1 C18 -175.0(13) . . . 6_565 ?
C33 N3 C1 C18 66.3(17) 6_565 . . 6_565 ?
C33 N3 C1 C18 -66.3(17) . . . . ?
C33 N3 C1 C18 175.0(13) 6_565 . . . ?
C33 N3 C1 C2 59.3(12) . . . . ?
C33 N3 C1 C2 -59.3(12) 6_565 . . . ?
C34 N2 C2 C3 -176.1(15) 6_565 . . . ?
C34 N2 C2 C3 69(2) . . . . ?
Rh2 N2 C2 C3 -53.7(12) . . . . ?
C34 N2 C2 C3 -69(2) 6_565 . . 6_565 ?
C34 N2 C2 C3 176.1(15) . . . 6_565 ?
Rh2 N2 C2 C3 53.7(12) . . . 6_565 ?
C34 N2 C2 C1 57.6(14) 6_565 . . . ?
C34 N2 C2 C1 -57.6(14) . . . . ?
Rh2 N2 C2 C1 180.000(7) . . . . ?
C18 C1 C2 N2 -121.4(15) 6_565 . . . ?
C18 C1 C2 N2 121.4(15) . . . . ?
N3 C1 C2 N2 0.000(8) . . . . ?
C18 C1 C2 C3 113.9(15) 6_565 . . . ?
C18 C1 C2 C3 -3(2) . . . . ?
N3 C1 C2 C3 -124.6(13) . . . . ?
C18 C1 C2 C3 3(2) 6_565 . . 6_565 ?
C18 C1 C2 C3 -113.9(15) . . . 6_565 ?
N3 C1 C2 C3 124.6(13) . . . 6_565 ?
N2 C2 C3 C20 -111.0(17) . . . . ?
C3 C2 C3 C20 133.8(12) 6_565 . . . ?
C1 C2 C3 C20 14(2) . . . . ?
N2 C2 C3 C4 99.3(16) . . . . ?
C3 C2 C3 C4 -15.9(15) 6_565 . . . ?
C1 C2 C3 C4 -135.6(14) . . . . ?
C20 C3 C4 C5 5.4(17) . . . . ?
C2 C3 C4 C5 157.5(12) . . . . ?
C20 C3 C4 C4 -141.2(8) . . . 6_565 ?
C2 C3 C4 C4 10.9(11) . . . 6_565 ?
C4 C4 C5 C22 138.6(10) 6_565 . . . ?
C3 C4 C5 C22 -4.0(18) . . . . ?
C4 C4 C5 C6 1.7(13) 6_565 . . . ?
C3 C4 C5 C6 -140.9(11) . . . . ?
C4 C5 C6 C6 -1.7(13) . . . 6_565 ?
C22 C5 C6 C6 -142.1(7) . . . 6_565 ?
C4 C5 C6 C7 141.6(12) . . . . ?
C22 C5 C6 C7 1.2(15) . . . . ?
C6 C6 C7 C8 -1(2) 6_565 . . . ?
C5 C6 C7 C8 -144.7(17) . . . . ?
C6 C6 C7 C23 145.0(9) 6_565 . . . ?
C5 C6 C7 C23 1.4(16) . . . . ?
C6 C7 C8 C8 1(2) . . . 6_565 ?
C23 C7 C8 C8 -140.5(13) . . . 6_565 ?
C6 C7 C8 C9 137.7(19) . . . . ?
C23 C7 C8 C9 -4(3) . . . . ?
C7 C8 C9 C25 1(3) . . . . ?
C8 C8 C9 C25 141.5(14) 6_565 . . . ?
C7 C8 C9 C10 -139(2) . . . . ?
C8 C8 C9 C10 1(2) 6_565 . . . ?
C25 C9 C10 C9 -141.4(17) . . . 6_565 ?
C8 C9 C10 C9 -2(3) . . . 6_565 ?
C25 C9 C10 C11 3(4) . . . . ?
C8 C9 C10 C11 142(2) . . . . ?
C9 C10 C11 C12 -3(4) . . . . ?
C9 C10 C11 C12 139(2) 6_565 . . . ?
C9 C10 C11 C12 -139(2) . . . 6_565 ?
C9 C10 C11 C12 3(4) 6_565 . . 6_565 ?
C10 C11 C12 C26 3(3) . . . . ?
C12 C11 C12 C26 144.0(13) 6_565 . . . ?
C10 C11 C12 C13 -146(2) . . . . ?
C12 C11 C12 C13 -5(2) 6_565 . . . ?
C26 C12 C13 C14 -2(2) . . . . ?
C11 C12 C13 C14 145.5(15) . . . . ?
C26 C12 C13 C13 -144.2(12) . . . 6_565 ?
C11 C12 C13 C13 2.8(14) . . . 6_565 ?
C13 C13 C14 C28 135.9(8) 6_565 . . . ?
C12 C13 C14 C28 -2.1(18) . . . . ?
C13 C13 C14 C15 -12.0(13) 6_565 . . . ?
C12 C13 C14 C15 -150.0(12) . . . . ?
C36 N1 C15 C14 67.6(11) . . . . ?
C35 N1 C15 C14 -175.6(9) . . . . ?
Rh1 N1 C15 C14 -55.6(13) . . . . ?
C36 N1 C15 C16 177.1(9) . . . . ?
C35 N1 C15 C16 -66.2(10) . . . . ?
Rh1 N1 C15 C16 53.8(13) . . . . ?
C36 N1 C15 C15 -57.8(9) . . . 6_565 ?
C35 N1 C15 C15 59.0(7) . . . 6_565 ?
Rh1 N1 C15 C15 179.0(6) . . . 6_565 ?
C13 C14 C15 N1 -111.3(12) . . . . ?
C28 C14 C15 N1 98.0(10) . . . . ?
C13 C14 C15 C16 133.3(11) . . . . ?
C28 C14 C15 C16 -17.3(11) . . . . ?
C13 C14 C15 C15 11.3(12) . . . 6_565 ?
C28 C14 C15 C15 -139.4(7) . . . 6_565 ?
N1 C15 C16 C17 111.9(14) . . . . ?
C14 C15 C16 C17 -132.6(15) . . . . ?
C15 C15 C16 C17 -10.5(17) 6_565 . . . ?
N1 C15 C16 C29 -97.5(12) . . . . ?
C14 C15 C16 C29 18.0(12) . . . . ?
C15 C15 C16 C29 140.1(7) 6_565 . . . ?
C29 C16 C17 C18 1(2) . . . . ?
C15 C16 C17 C18 149.0(14) . . . . ?
C29 C16 C17 C17 -137.1(10) . . . 6_565 ?
C15 C16 C17 C17 11.1(17) . . . 6_565 ?
C16 C17 C18 C19 1(2) . . . . ?
C17 C17 C18 C19 144.0(13) 6_565 . . . ?
C16 C17 C18 C1 -155.7(17) . . . . ?
C17 C17 C18 C1 -13.0(17) 6_565 . . . ?
C18 C1 C18 C19 -136.5(13) 6_565 . . . ?
N3 C1 C18 C19 109.1(19) . . . . ?
C2 C1 C18 C19 -11(3) . . . . ?
C18 C1 C18 C17 20(3) 6_565 . . . ?
N3 C1 C18 C17 -94.7(16) . . . . ?
C2 C1 C18 C17 145.0(16) . . . . ?
C17 C18 C19 C30 -3(2) . . . . ?
C1 C18 C19 C30 151.2(17) . . . . ?
C17 C18 C19 C20 -137.9(15) . . . . ?
C1 C18 C19 C20 16(3) . . . . ?
C4 C3 C20 C21 -4.6(16) . . . . ?
C2 C3 C20 C21 -152.4(14) . . . . ?
C4 C3 C20 C19 137.2(13) . . . . ?
C2 C3 C20 C19 -11(2) . . . . ?
C18 C19 C20 C3 -5(2) . . . . ?
C30 C19 C20 C3 -144.7(13) . . . . ?
C18 C19 C20 C21 141.5(14) . . . . ?
C30 C19 C20 C21 1.8(15) . . . . ?
C3 C20 C21 C22 2.5(18) . . . . ?
C19 C20 C21 C22 -142.4(12) . . . . ?
C3 C20 C21 C31 143.0(12) . . . . ?
C19 C20 C21 C31 -1.9(15) . . . . ?
C20 C21 C22 C5 -0.9(18) . . . . ?
C31 C21 C22 C5 -136.8(13) . . . . ?
C20 C21 C22 C23 139.0(13) . . . . ?
C31 C21 C22 C23 3.2(18) . . . . ?
C4 C5 C22 C21 1.8(18) . . . . ?
C6 C5 C22 C21 142.4(13) . . . . ?
C4 C5 C22 C23 -143.9(13) . . . . ?
C6 C5 C22 C23 -3.3(14) . . . . ?
C21 C22 C23 C24 -4(2) . . . . ?
C5 C22 C23 C24 141.0(13) . . . . ?
C21 C22 C23 C7 -140.8(13) . . . . ?
C5 C22 C23 C7 4.1(14) . . . . ?
C8 C7 C23 C24 5(3) . . . . ?
C6 C7 C23 C24 -141.1(15) . . . . ?
C8 C7 C23 C22 142.6(17) . . . . ?
C6 C7 C23 C22 -3.5(16) . . . . ?
C22 C23 C24 C25 -136.0(17) . . . . ?
C7 C23 C24 C25 -3(2) . . . . ?
C22 C23 C24 C32 4(2) . . . . ?
C7 C23 C24 C32 136.9(16) . . . . ?
C23 C24 C25 C9 0(3) . . . . ?
C32 C24 C25 C9 -142.0(17) . . . . ?
C23 C24 C25 C26 142.6(16) . . . . ?
C32 C24 C25 C26 0.5(18) . . . . ?
C10 C9 C25 C24 135(2) . . . . ?
C8 C9 C25 C24 1(3) . . . . ?
C10 C9 C25 C26 -4(3) . . . . ?
C8 C9 C25 C26 -137.7(18) . . . . ?
C13 C12 C26 C27 2(2) . . . . ?
C11 C12 C26 C27 -141.6(18) . . . . ?
C13 C12 C26 C25 140.2(17) . . . . ?
C11 C12 C26 C25 -3(3) . . . . ?
C24 C25 C26 C12 -140.8(18) . . . . ?
C9 C25 C26 C12 4(3) . . . . ?
C24 C25 C26 C27 1.8(18) . . . . ?
C9 C25 C26 C27 146.5(16) . . . . ?
C12 C26 C27 C28 2(2) . . . . ?
C25 C26 C27 C28 -142.2(13) . . . . ?
C12 C26 C27 C32 140.2(14) . . . . ?
C25 C26 C27 C32 -3.5(17) . . . . ?
C13 C14 C28 C29 -141.3(12) . . . . ?
C15 C14 C28 C29 11.2(13) . . . . ?
C13 C14 C28 C27 5.4(16) . . . . ?
C15 C14 C28 C27 157.8(10) . . . . ?
C26 C27 C28 C29 136.8(13) . . . . ?
C32 C27 C28 C29 1.2(19) . . . . ?
C26 C27 C28 C14 -5.1(17) . . . . ?
C32 C27 C28 C14 -140.7(13) . . . . ?
C17 C16 C29 C30 -1(2) . . . . ?
C15 C16 C29 C30 -154.0(13) . . . . ?
C17 C16 C29 C28 140.4(13) . . . . ?
C15 C16 C29 C28 -12.5(13) . . . . ?
C14 C28 C29 C30 144.0(11) . . . . ?
C27 C28 C29 C30 -1.5(17) . . . . ?
C14 C28 C29 C16 0.9(14) . . . . ?
C27 C28 C29 C16 -144.7(12) . . . . ?
C16 C29 C30 C19 0(2) . . . . ?
C28 C29 C30 C19 -139.0(14) . . . . ?
C16 C29 C30 C31 139.3(14) . . . . ?
C28 C29 C30 C31 0.8(16) . . . . ?
C18 C19 C30 C29 2(2) . . . . ?
C20 C19 C30 C29 143.7(14) . . . . ?
C18 C19 C30 C31 -142.2(14) . . . . ?
C20 C19 C30 C31 -0.9(15) . . . . ?
C22 C21 C31 C32 -2.7(17) . . . . ?
C20 C21 C31 C32 -143.2(12) . . . . ?
C22 C21 C31 C30 141.8(13) . . . . ?
C20 C21 C31 C30 1.3(15) . . . . ?
C29 C30 C31 C32 0.2(18) . . . . ?
C19 C30 C31 C32 143.8(12) . . . . ?
C29 C30 C31 C21 -143.8(12) . . . . ?
C19 C30 C31 C21 -0.2(15) . . . . ?
C21 C31 C32 C27 139.8(13) . . . . ?
C30 C31 C32 C27 0(2) . . . . ?
C21 C31 C32 C24 2.9(18) . . . . ?
C30 C31 C32 C24 -137.4(13) . . . . ?
C28 C27 C32 C31 0(2) . . . . ?
C26 C27 C32 C31 -139.6(15) . . . . ?
C28 C27 C32 C24 143.1(13) . . . . ?
C26 C27 C32 C24 3.7(16) . . . . ?
C25 C24 C32 C31 139.9(14) . . . . ?
C23 C24 C32 C31 -4(2) . . . . ?
C25 C24 C32 C27 -2.6(16) . . . . ?
C23 C24 C32 C27 -146.1(13) . . . . ?
C33 N3 C33 C34 55(3) 6_565 . . . ?
C1 N3 C33 C34 -63(2) . . . . ?
C2 N2 C34 C33 57(2) . . . . ?
C34 N2 C34 C33 -60(2) 6_565 . . . ?
Rh2 N2 C34 C33 -167.8(15) . . . . ?
N3 C33 C34 N2 3(3) . . . . ?
C36 N1 C35 C35 57.5(7) . . . 6_565 ?
C15 N1 C35 C35 -59.8(7) . . . 6_565 ?
Rh1 N1 C35 C35 164.4(7) . . . 6_565 ?
C15 N1 C36 C36 59.7(9) . . . 6_565 ?
C35 N1 C36 C36 -58.5(7) . . . 6_565 ?
Rh1 N1 C36 C36 -163.3(2) . . . 6_565 ?
Rh1 O1 C37 O2 -8(4) . . . . ?
Rh1 O1 C37 C38 -168(2) . . . . ?
Rh1 O2 C37 O1 17(4) 7_656 . . . ?
Rh1 O2 C37 C38 178(2) 7_656 . . . ?
Rh1 O4 C39 O3 0(3) 7_656 . . . ?
Rh1 O4 C39 C40 -162(2) 7_656 . . . ?
Rh1 O3 C39 O4 2(3) . . . . ?
Rh1 O3 C39 C40 163(2) . . . . ?
Rh1 O5 C41 O6 1(4) . . . . ?
Rh1 O5 C41 C42 178.2(16) . . . . ?
Rh1 O6 C41 O5 -4(4) 7_656 . . . ?
Rh1 O6 C41 C42 178.8(16) 7_656 . . . ?
Rh1 O7 C43 O8 3(3) . . . . ?
Rh1 O7 C43 C44 179.8(18) . . . . ?
Rh1 O8 C43 O7 -5(3) 7_656 . . . ?
Rh1 O8 C43 C44 178.4(18) 7_656 . . . ?
Rh2 O9 C45 O10 0.000(12) . . . . ?
Rh2 O9 C45 C46 180.000(8) . . . . ?
Rh2 O10 C45 O9 0.000(12) 5_567 . . . ?
Rh2 O10 C45 C46 180.000(8) 5_567 . . . ?
Rh2 O12 C47 O12 -0.4(6) . . . 2_557 ?
Rh2 O12 C47 C48 179.6(6) . . . . ?

_refine_diff_density_max         1.759
_refine_diff_density_min         -1.903
_refine_diff_density_rms         0.198

