# Electronic Supplementary Material (ESI) for RSC Chemical Biology.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_tcd2011
_database_code_depnum_ccdc_archive 'CCDC 2256792'
loop_
_audit_author_name
_audit_author_address
'Brendan Twamley'
;TCD
Ireland
;
_audit_update_record             
;
2023-04-17 deposited with the CCDC.	2023-08-16 downloaded from the CCDC.
;
_audit_creation_date             2023-02-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C7 H15 I2 N5 Pt, C3 H7 N O'
_chemical_formula_sum            'C10 H22 I2 N6 O Pt'
_chemical_formula_weight         691.22
_chemical_absolute_configuration rmad
_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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   8.4825(4)
_cell_length_b                   10.3937(5)
_cell_length_c                   11.4784(5)
_cell_angle_alpha                112.2786(14)
_cell_angle_beta                 91.4077(16)
_cell_angle_gamma                108.8135(14)
_cell_volume                     873.87(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2439
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.363
_shelx_estimated_absorpt_T_min   0.183
_exptl_absorpt_coefficient_mu    11.567
_exptl_absorpt_correction_T_max  0.1617
_exptl_absorpt_correction_T_min  0.0518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Krause, 2015) was used for absorption correction.
wR2(int) was 0.0471 before and 0.0396 after correction.
The Ratio of minimum to maximum transmission is 0.5195.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.627
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             632
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3.00 2.00 0.00 0.0540
-2.00 0.00 3.00 0.1100
-2.00 3.00 0.00 0.0490
-2.00 -1.00 0.00 0.0570
0.00 1.00 0.00 0.0550
0.00 -1.00 0.00 0.0300
0.00 1.00 -3.00 0.0880
0.00 -1.00 3.00 0.1120
0.00 1.00 -1.00 0.0530
1.00 -1.00 3.00 0.0900
1.00 -3.00 3.00 0.0910
2.00 0.00 3.00 0.0820
2.00 2.00 -3.00 0.0570
2.00 3.00 0.00 0.0640
3.00 -1.00 -1.00 0.0540

_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36469
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.748
_diffrn_reflns_theta_min         2.268
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CMOS area detector'
_diffrn_detector_area_resol_mean 5.12
_diffrn_detector_type            'Bruker PHOTON 50'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       'ω only'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_detector       'Bruker PHOTON 50'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_source_voltage           50.0
_diffrn_special_details          ?
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.978
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                9805
_reflns_number_total             10735
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'APEX 4 (Bruker, 2021) '
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         1.862
_refine_diff_density_min         -2.078
_refine_diff_density_rms         0.200
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.031(12)
_refine_ls_extinction_coef       0.0025(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         10735
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      1.077
_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)+(0.0170P)²+8.9575P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0745
_refine_special_details          
'Two independent molecules in the asymmetric unit. One azide group was disordered over two locations (68:32% occupied) and modelled using a rigid group and geometrical (SADI) and displacment (SIMU, ISOR) restraints. Carbon C21A/C21B was constrained to have the same anisotropic displacement parameters (EADP). The large residual density is located near the heavy Pt atom, and the intensity (1.86 eA^-3) is smaller than the 0.1*Z eA^-3 (Z = 78 for Pt). This originates from absorption or is a Fourier truncation error. The error in the Flack parameter was such that it required refinement, resulting in a Flack of 0.031(12). The Pt1-Pt2 distance is 3.6321(6) Å.'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.969(12)
 0.031(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C21B-C17 \\sim C17-C21A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N22B \\sim N23B \\sim N24B \\sim C21B \\sim N22A \\sim N23A \\sim N24A \\sim
C21A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.04 within
2A
Uanis(N22A) \\sim Ueq, Uanis(N23A) \\sim Ueq, Uanis(N24A) \\sim Ueq,
Uanis(N22B) \\sim Ueq, Uanis(N23B) \\sim Ueq, Uanis(N24B) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.02
Uanis(C21B) = Uanis(C21A)
5. Others
 Sof(H17)=Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(N22B)=Sof(N23B)=Sof(N24B)=1-FVAR(1)
 Sof(H17A)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(N22A)=Sof(N23A)=Sof(N24A)=FVAR(1)
6.a Free rotating group:
 C21B(N22B,N23B,N24B), C21A(N22A,N23A,N24A)
6.b Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C7(H7), C14(H14), C17(H17A), C17(H17), C19(H19)
6.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N8(H8A,H8B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C9(H9A,H9B),
 N13(H13A,H13B), N20(H20A,H20B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B),
  C21B(H21A,H21B), C21A(H21C,H21D)
6.d Aromatic/amide H refined with riding coordinates:
 C31(H31), C26(H26)
6.e Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C)
;
_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
Pt1 Pt 0.31725(5) 0.23617(4) 0.68728(4) 0.01721(14) Uani 1 1 d . . . . .
I1 I 0.32372(15) 0.11516(16) 0.44554(13) 0.0295(3) Uani 1 1 d . . . . .
I2 I 0.27628(14) -0.00150(14) 0.72625(12) 0.0266(3) Uani 1 1 d . . . . .
N1 N 0.3279(17) 0.4346(17) 0.6764(14) 0.019(3) Uani 1 1 d . . . . .
H1A H 0.434842 0.487121 0.671887 0.022 Uiso 1 1 calc R U . . .
H1B H 0.257490 0.415480 0.605886 0.022 Uiso 1 1 calc R U . . .
N8 N 0.3283(18) 0.3524(17) 0.8796(16) 0.022(3) Uani 1 1 d . . . . .
H8A H 0.229650 0.311835 0.903789 0.027 Uiso 1 1 calc R U . . .
H8B H 0.413595 0.346748 0.924835 0.027 Uiso 1 1 calc R U . . .
N10 N 0.569(2) 1.0067(17) 1.1532(14) 0.038(4) Uani 1 1 d . . . . .
N11 N 0.5878(16) 1.0639(14) 1.0806(13) 0.033(3) Uani 1 1 d . . . . .
N12 N 0.612(2) 1.1340(16) 1.0217(14) 0.052(4) Uani 1 1 d . . . . .
C2 C 0.2736(15) 0.5208(12) 0.7952(10) 0.0191(19) Uani 1 1 d . . . . .
H2 H 0.148749 0.472525 0.787195 0.023 Uiso 1 1 calc R U . . .
C3 C 0.313(2) 0.6822(19) 0.8183(18) 0.021(3) Uani 1 1 d . . . . .
H3A H 0.251873 0.687129 0.746367 0.025 Uiso 1 1 calc R U . . .
H3B H 0.435476 0.730567 0.822057 0.025 Uiso 1 1 calc R U . . .
C4 C 0.2611(17) 0.7657(14) 0.9426(11) 0.025(2) Uani 1 1 d . . . . .
H4A H 0.136484 0.725597 0.934051 0.030 Uiso 1 1 calc R U . . .
H4B H 0.295967 0.872171 0.958152 0.030 Uiso 1 1 calc R U . . .
C5 C 0.3396(19) 0.7530(16) 1.0572(13) 0.028(3) Uani 1 1 d . . . . .
H5 H 0.282971 0.793766 1.130639 0.034 Uiso 1 1 calc R U . . .
C6 C 0.305(2) 0.590(2) 1.0316(16) 0.021(3) Uani 1 1 d . . . . .
H6A H 0.368005 0.584484 1.102432 0.025 Uiso 1 1 calc R U . . .
H6B H 0.182911 0.538261 1.027491 0.025 Uiso 1 1 calc R U . . .
C7 C 0.3582(14) 0.5122(12) 0.9071(10) 0.0182(19) Uani 1 1 d . . . . .
H7 H 0.482560 0.564055 0.915920 0.022 Uiso 1 1 calc R U . . .
C9 C 0.5300(17) 0.8444(13) 1.0982(13) 0.033(3) Uani 1 1 d . . . . .
H9A H 0.576482 0.817705 1.162007 0.040 Uiso 1 1 calc R U . . .
H9B H 0.586756 0.817352 1.022965 0.040 Uiso 1 1 calc R U . . .
Pt2 Pt 0.77308(5) 0.41236(4) 0.78035(4) 0.01701(14) Uani 1 1 d . . . . .
I3 I 0.77888(14) 0.53514(14) 1.02506(12) 0.0258(3) Uani 1 1 d . . . . .
I4 I 0.79724(15) 0.64750(14) 0.74203(12) 0.0277(3) Uani 1 1 d . . . . .
O30 O 1.0216(14) 1.2086(16) 0.9494(13) 0.024(2) Uani 1 1 d . . . . .
N13 N 0.7827(17) 0.2987(18) 0.5916(14) 0.018(3) Uani 1 1 d . . . . .
H13A H 0.680981 0.269548 0.542850 0.022 Uiso 1 1 calc R U . . .
H13B H 0.862351 0.359006 0.564808 0.022 Uiso 1 1 calc R U . . .
N20 N 0.7481(18) 0.2145(17) 0.7888(15) 0.020(3) Uani 1 1 d . . . . .
H20A H 0.843275 0.224452 0.835154 0.024 Uiso 1 1 calc R U . . .
H20B H 0.659530 0.188114 0.828719 0.024 Uiso 1 1 calc R U . . .
N32 N 1.0711(17) 1.0996(17) 1.0763(13) 0.024(3) Uani 1 1 d . . . . .
C14 C 0.8250(15) 0.1663(12) 0.5772(11) 0.0191(19) Uani 1 1 d . . . . .
H14 H 0.947196 0.200276 0.612834 0.023 Uiso 1 1 calc R U . . .
C15 C 0.793(3) 0.054(3) 0.440(2) 0.031(4) Uani 1 1 d . . . . .
H15A H 0.674290 0.025804 0.401586 0.038 Uiso 1 1 calc R U . . .
H15B H 0.867548 0.100185 0.390736 0.038 Uiso 1 1 calc R U . . .
C16 C 0.8246(17) -0.0836(15) 0.4322(13) 0.027(3) Uani 1 1 d . . . . .
H16A H 0.947127 -0.057281 0.457102 0.032 Uiso 1 1 calc R U . . .
H16B H 0.791048 -0.158224 0.342480 0.032 Uiso 1 1 calc R U . . .
C17 C 0.7288(17) -0.1539(13) 0.5172(12) 0.027(2) Uani 1 1 d D . . . .
H17A H 0.775652 -0.230141 0.518947 0.032 Uiso 0.69(11) 1 calc R U P A -1
H17 H 0.774442 -0.230973 0.518557 0.032 Uiso 0.31(11) 1 calc R U P A -2
C18 C 0.759(2) -0.038(2) 0.6562(18) 0.024(3) Uani 1 1 d . . . . .
H18A H 0.686316 -0.083619 0.706646 0.029 Uiso 1 1 calc R U . . .
H18B H 0.878450 -0.004998 0.695417 0.029 Uiso 1 1 calc R U . . .
C19 C 0.7194(13) 0.0960(11) 0.6581(10) 0.0182(19) Uani 1 1 d . . . . .
H19 H 0.597529 0.060247 0.620699 0.022 Uiso 1 1 calc R U . . .
C31 C 0.985(2) 1.104(2) 0.9823(17) 0.020(3) Uani 1 1 d . . . . .
H31 H 0.886653 1.019656 0.935647 0.025 Uiso 1 1 calc R U . . .
C33 C 1.230(2) 1.218(3) 1.151(2) 0.065(6) Uani 1 1 d . . . . .
H33A H 1.324511 1.183690 1.127024 0.098 Uiso 1 1 calc R U . . .
H33B H 1.227974 1.243554 1.242101 0.098 Uiso 1 1 calc R U . . .
H33C H 1.245350 1.306257 1.133569 0.098 Uiso 1 1 calc R U . . .
C34 C 1.011(3) 0.973(2) 1.115(2) 0.031(4) Uani 1 1 d . . . . .
H34A H 0.955277 0.880452 1.039352 0.046 Uiso 1 1 calc R U . . .
H34B H 0.930577 0.989847 1.173943 0.046 Uiso 1 1 calc R U . . .
H34C H 1.107395 0.966210 1.157799 0.046 Uiso 1 1 calc R U . . .
C21B C 0.538(4) -0.229(7) 0.478(12) 0.036(5) Uani 0.31(11) 1 d DG U P A -2
H21A H 0.488069 -0.251430 0.547995 0.043 Uiso 0.31(11) 1 calc R U P A -2
H21B H 0.490972 -0.160759 0.461518 0.043 Uiso 0.31(11) 1 calc R U P A -2
N22B N 0.495(12) -0.367(8) 0.362(8) 0.045(13) Uani 0.31(11) 1 d G U P A -2
N23B N 0.531(7) -0.464(6) 0.372(7) 0.056(13) Uani 0.31(11) 1 d G U P A -2
N24B N 0.559(10) -0.567(7) 0.366(9) 0.060(14) Uani 0.31(11) 1 d G U P A -2
C21A C 0.542(2) -0.235(3) 0.461(4) 0.036(5) Uani 0.69(11) 1 d DG U P A -1
H21C H 0.482534 -0.267645 0.523610 0.043 Uiso 0.69(11) 1 calc R U P A -1
H21D H 0.496475 -0.164417 0.447939 0.043 Uiso 0.69(11) 1 calc R U P A -1
N22A N 0.503(5) -0.366(4) 0.339(3) 0.043(8) Uani 0.69(11) 1 d G U P A -1
N23A N 0.554(4) -0.460(3) 0.338(3) 0.050(7) Uani 0.69(11) 1 d G U P A -1
N24A N 0.597(5) -0.558(3) 0.322(4) 0.072(9) Uani 0.69(11) 1 d G U P A -1
O25 O 0.0800(17) 0.4303(18) 0.4989(14) 0.031(3) Uani 1 1 d . . . . .
N27 N 0.042(2) 0.5358(18) 0.3641(13) 0.028(3) Uani 1 1 d . . . . .
C26 C 0.098(2) 0.536(3) 0.471(2) 0.031(4) Uani 1 1 d . . . . .
H26 H 0.160046 0.631667 0.536576 0.037 Uiso 1 1 calc R U . . .
C28 C -0.051(4) 0.3964(19) 0.2586(17) 0.067(7) Uani 1 1 d . . . . .
H28A H -0.023913 0.316010 0.268643 0.100 Uiso 1 1 calc R U . . .
H28B H -0.020633 0.402055 0.178408 0.100 Uiso 1 1 calc R U . . .
H28C H -0.172487 0.376168 0.256919 0.100 Uiso 1 1 calc R U . . .
C29 C 0.074(3) 0.670(3) 0.347(2) 0.040(5) Uani 1 1 d . . . . .
H29A H 0.166144 0.750471 0.413586 0.061 Uiso 1 1 calc R U . . .
H29B H -0.028393 0.694932 0.353369 0.061 Uiso 1 1 calc R U . . .
H29C H 0.105334 0.656241 0.262957 0.061 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 I1 2.5865(15) . ?
Pt1 I2 2.5914(14) . ?
Pt1 N1 2.087(16) . ?
Pt1 N8 2.058(17) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C2 1.498(19) . ?
N8 H8A 0.9100 . ?
N8 H8B 0.9100 . ?
N8 C7 1.499(18) . ?
N10 N11 1.182(19) . ?
N10 C9 1.475(19) . ?
N11 N12 1.146(19) . ?
C2 H2 1.0000 . ?
C2 C3 1.51(2) . ?
C2 C7 1.502(14) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.52(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.529(17) . ?
C5 H5 1.0000 . ?
C5 C6 1.53(2) . ?
C5 C9 1.538(19) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.51(2) . ?
C7 H7 1.0000 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
Pt2 I3 2.5992(14) . ?
Pt2 I4 2.5894(14) . ?
Pt2 N13 2.056(15) . ?
Pt2 N20 2.039(15) . ?
O30 C31 1.23(2) . ?
N13 H13A 0.9100 . ?
N13 H13B 0.9100 . ?
N13 C14 1.483(18) . ?
N20 H20A 0.9100 . ?
N20 H20B 0.9100 . ?
N20 C19 1.488(19) . ?
N32 C31 1.31(2) . ?
N32 C33 1.47(2) . ?
N32 C34 1.49(2) . ?
C14 H14 1.0000 . ?
C14 C15 1.51(2) . ?
C14 C19 1.527(15) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.51(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.531(19) . ?
C17 H17A 1.0000 . ?
C17 H17 1.0000 . ?
C17 C18 1.54(2) . ?
C17 C21B 1.52(3) . ?
C17 C21A 1.52(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.53(2) . ?
C19 H19 1.0000 . ?
C31 H31 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C21B H21A 0.9900 . ?
C21B H21B 0.9900 . ?
C21B N22B 1.4671 . ?
N22B N23B 1.1816 . ?
N23B N24B 1.1461 . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C21A N22A 1.4669 . ?
N22A N23A 1.1818 . ?
N23A N24A 1.1464 . ?
O25 C26 1.22(3) . ?
N27 C26 1.30(2) . ?
N27 C28 1.44(2) . ?
N27 C29 1.42(3) . ?
C26 H26 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pt1 I2 95.65(5) . . ?
N1 Pt1 I1 91.3(4) . . ?
N1 Pt1 I2 171.5(4) . . ?
N8 Pt1 I1 174.2(4) . . ?
N8 Pt1 I2 89.3(4) . . ?
N8 Pt1 N1 83.9(6) . . ?
Pt1 N1 H1A 110.4 . . ?
Pt1 N1 H1B 110.4 . . ?
H1A N1 H1B 108.6 . . ?
C2 N1 Pt1 106.5(9) . . ?
C2 N1 H1A 110.4 . . ?
C2 N1 H1B 110.4 . . ?
Pt1 N8 H8A 109.8 . . ?
Pt1 N8 H8B 109.8 . . ?
H8A N8 H8B 108.2 . . ?
C7 N8 Pt1 109.5(10) . . ?
C7 N8 H8A 109.8 . . ?
C7 N8 H8B 109.8 . . ?
N11 N10 C9 116.4(15) . . ?
N12 N11 N10 172.4(17) . . ?
N1 C2 H2 108.3 . . ?
N1 C2 C3 113.3(11) . . ?
N1 C2 C7 108.7(10) . . ?
C3 C2 H2 108.3 . . ?
C7 C2 H2 108.3 . . ?
C7 C2 C3 109.8(10) . . ?
C2 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
C2 C3 C4 111.1(13) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
C3 C4 C5 112.6(11) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C4 C5 H5 107.3 . . ?
C4 C5 C6 111.0(12) . . ?
C4 C5 C9 113.1(12) . . ?
C6 C5 H5 107.3 . . ?
C6 C5 C9 110.5(12) . . ?
C9 C5 H5 107.3 . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
C7 C6 C5 110.4(13) . . ?
C7 C6 H6A 109.6 . . ?
C7 C6 H6B 109.6 . . ?
N8 C7 C2 109.4(10) . . ?
N8 C7 C6 111.9(11) . . ?
N8 C7 H7 107.4 . . ?
C2 C7 C6 112.9(11) . . ?
C2 C7 H7 107.4 . . ?
C6 C7 H7 107.4 . . ?
N10 C9 C5 113.3(12) . . ?
N10 C9 H9A 108.9 . . ?
N10 C9 H9B 108.9 . . ?
C5 C9 H9A 108.9 . . ?
C5 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
I4 Pt2 I3 95.40(5) . . ?
N13 Pt2 I3 172.8(4) . . ?
N13 Pt2 I4 90.9(4) . . ?
N20 Pt2 I3 90.9(4) . . ?
N20 Pt2 I4 173.6(4) . . ?
N20 Pt2 N13 82.9(6) . . ?
Pt2 N13 H13A 109.8 . . ?
Pt2 N13 H13B 109.8 . . ?
H13A N13 H13B 108.3 . . ?
C14 N13 Pt2 109.2(9) . . ?
C14 N13 H13A 109.8 . . ?
C14 N13 H13B 109.8 . . ?
Pt2 N20 H20A 109.6 . . ?
Pt2 N20 H20B 109.6 . . ?
H20A N20 H20B 108.1 . . ?
C19 N20 Pt2 110.5(9) . . ?
C19 N20 H20A 109.6 . . ?
C19 N20 H20B 109.6 . . ?
C31 N32 C33 122.9(15) . . ?
C31 N32 C34 121.6(16) . . ?
C33 N32 C34 115.4(14) . . ?
N13 C14 H14 108.6 . . ?
N13 C14 C15 113.5(12) . . ?
N13 C14 C19 106.5(10) . . ?
C15 C14 H14 108.6 . . ?
C15 C14 C19 110.8(12) . . ?
C19 C14 H14 108.6 . . ?
C14 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C16 C15 C14 111.2(15) . . ?
C16 C15 H15A 109.4 . . ?
C16 C15 H15B 109.4 . . ?
C15 C16 H16A 108.9 . . ?
C15 C16 H16B 108.9 . . ?
C15 C16 C17 113.5(12) . . ?
H16A C16 H16B 107.7 . . ?
C17 C16 H16A 108.9 . . ?
C17 C16 H16B 108.9 . . ?
C16 C17 H17A 107.1 . . ?
C16 C17 H17 107.4 . . ?
C16 C17 C18 111.5(12) . . ?
C18 C17 H17A 107.1 . . ?
C18 C17 H17 107.4 . . ?
C21B C17 C16 117(5) . . ?
C21B C17 H17 107.4 . . ?
C21B C17 C18 106(4) . . ?
C21A C17 C16 111(2) . . ?
C21A C17 H17A 107.1 . . ?
C21A C17 C18 112.6(17) . . ?
C17 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C19 C18 C17 109.9(13) . . ?
C19 C18 H18A 109.7 . . ?
C19 C18 H18B 109.7 . . ?
N20 C19 C14 107.9(9) . . ?
N20 C19 C18 113.3(11) . . ?
N20 C19 H19 108.1 . . ?
C14 C19 C18 111.3(11) . . ?
C14 C19 H19 108.1 . . ?
C18 C19 H19 108.1 . . ?
O30 C31 N32 125.3(16) . . ?
O30 C31 H31 117.3 . . ?
N32 C31 H31 117.3 . . ?
N32 C33 H33A 109.5 . . ?
N32 C33 H33B 109.5 . . ?
N32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N32 C34 H34A 109.5 . . ?
N32 C34 H34B 109.5 . . ?
N32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C17 C21B H21A 109.6 . . ?
C17 C21B H21B 109.6 . . ?
H21A C21B H21B 108.1 . . ?
N22B C21B C17 110(6) . . ?
N22B C21B H21A 109.6 . . ?
N22B C21B H21B 109.6 . . ?
N23B N22B C21B 116.6 . . ?
N24B N23B N22B 172.0 . . ?
C17 C21A H21C 108.5 . . ?
C17 C21A H21D 108.5 . . ?
H21C C21A H21D 107.5 . . ?
N22A C21A C17 115(2) . . ?
N22A C21A H21C 108.5 . . ?
N22A C21A H21D 108.5 . . ?
N23A N22A C21A 116.6 . . ?
N24A N23A N22A 172.1 . . ?
C26 N27 C28 119.8(18) . . ?
C26 N27 C29 121.7(19) . . ?
C29 N27 C28 118.5(16) . . ?
O25 C26 N27 129(2) . . ?
O25 C26 H26 115.7 . . ?
N27 C26 H26 115.7 . . ?
N27 C28 H28A 109.5 . . ?
N27 C28 H28B 109.5 . . ?
N27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N27 C29 H29A 109.5 . . ?
N27 C29 H29B 109.5 . . ?
N27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1B O25 0.91 2.00 2.87(2) 159 . yes
N8 H8A O30 0.91 1.95 2.85(2) 175 1_445 yes
C4 H4B N11 0.99 2.57 3.212(18) 123 . yes
N13 H13B O25 0.91 2.04 2.894(19) 157 1_655 yes
N20 H20A O30 0.91 2.07 2.958(18) 167 1_545 yes
N20 H20B N12 0.91 2.50 3.23(2) 138 1_545 yes

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
Pt1 N1 C2 C3 166.4(9) . . . . ?
Pt1 N1 C2 C7 43.9(11) . . . . ?
Pt1 N8 C7 C2 33.0(12) . . . . ?
Pt1 N8 C7 C6 159.0(10) . . . . ?
N1 C2 C3 C4 -177.9(11) . . . . ?
N1 C2 C7 N8 -51.7(14) . . . . ?
N1 C2 C7 C6 -177.1(12) . . . . ?
N11 N10 C9 C5 -89.1(19) . . . . ?
C2 C3 C4 C5 54.6(16) . . . . ?
C3 C2 C7 N8 -176.2(12) . . . . ?
C3 C2 C7 C6 58.3(15) . . . . ?
C3 C4 C5 C6 -52.6(16) . . . . ?
C3 C4 C5 C9 72.3(15) . . . . ?
C4 C5 C6 C7 52.5(16) . . . . ?
C4 C5 C9 N10 68.5(16) . . . . ?
C5 C6 C7 N8 179.2(12) . . . . ?
C5 C6 C7 C2 -56.7(15) . . . . ?
C6 C5 C9 N10 -166.4(13) . . . . ?
C7 C2 C3 C4 -56.1(14) . . . . ?
C9 C5 C6 C7 -73.8(16) . . . . ?
Pt2 N13 C14 C15 165.5(11) . . . . ?
Pt2 N13 C14 C19 43.3(11) . . . . ?
Pt2 N20 C19 C14 36.5(11) . . . . ?
Pt2 N20 C19 C18 160.2(10) . . . . ?
N13 C14 C15 C16 -175.4(13) . . . . ?
N13 C14 C19 N20 -52.2(13) . . . . ?
N13 C14 C19 C18 -177.1(11) . . . . ?
C14 C15 C16 C17 52.8(19) . . . . ?
C15 C14 C19 N20 -176.1(12) . . . . ?
C15 C14 C19 C18 59.0(15) . . . . ?
C15 C16 C17 C18 -51.8(17) . . . . ?
C15 C16 C17 C21B 70(3) . . . . ?
C15 C16 C17 C21A 74.6(18) . . . . ?
C16 C17 C18 C19 53.1(16) . . . . ?
C16 C17 C21B N22B 71(5) . . . . ?
C16 C17 C21A N22A 66(3) . . . . ?
C17 C18 C19 N20 -179.1(12) . . . . ?
C17 C18 C19 C14 -57.3(15) . . . . ?
C17 C21B N22B N23B 66(11) . . . . ?
C17 C21A N22A N23A 56(5) . . . . ?
C18 C17 C21B N22B -164(5) . . . . ?
C18 C17 C21A N22A -169(2) . . . . ?
C19 C14 C15 C16 -55.6(17) . . . . ?
C33 N32 C31 O30 -4(3) . . . . ?
C34 N32 C31 O30 175.5(17) . . . . ?
C21B C17 C18 C19 -75(5) . . . . ?
C21A C17 C18 C19 -72(2) . . . . ?
C28 N27 C26 O25 -1(3) . . . . ?
C29 N27 C26 O25 180(2) . . . . ?

_olex2_exptl_crystal_mounting_method 'mounted in oil on a MIteGen microloop'
_olex2_submission_original_sample_id POD74
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.969(12)
2 0.031(12)

_vrf_PLAT342_tcd2011             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.021 Ang.  
RESPONSE: Many heavy atoms in the structure, with disorder present.
;
####################################################################### 
# 
# 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_tcd1762
_database_code_depnum_ccdc_archive 'CCDC 2256793'
loop_
_audit_author_name
_audit_author_address
'Brendan Twamley'
;TCD
Ireland
;
_audit_update_record             
;
2023-04-17 deposited with the CCDC.	2023-08-16 downloaded from the CCDC.
;
_audit_creation_date             2021-06-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C7 H17 N5, C4 H4 O6, 0.5(C H4 O), 1.15(H2 O)'
_chemical_formula_sum            'C11.50 H25.30 N5 O7.65'
_chemical_formula_weight         356.07
_chemical_absolute_configuration ad
_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 0.0181 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'

_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           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   18.1460(8)
_cell_length_b                   6.3721(3)
_cell_length_c                   16.6518(7)
_cell_angle_alpha                90
_cell_angle_beta                 117.203(2)
_cell_angle_gamma                90
_cell_volume                     1712.45(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.40
_cell_measurement_theta_min      2.984
_shelx_estimated_absorpt_T_max   0.952
_shelx_estimated_absorpt_T_min   0.717
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Krause, 2015) was used for absorption correction.
wR2(int) was 0.1347 before and 0.0951 after correction.
The Ratio of minimum to maximum transmission is 0.7183.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.36
_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  0.0645
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25857
_diffrn_reflns_point_group_measured_fraction_full 0.888
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.060
_diffrn_reflns_theta_min         2.984
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 Kappa Duo'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       APEX2
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.029796
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           49.66
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.626
_reflns_Friedel_fraction_full    0.758
_reflns_Friedel_fraction_max     0.752
_reflns_number_gt                2714
_reflns_number_total             2878
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX 3 (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL  (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         2878
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0678
_refine_ls_restrained_S_all      1.067
_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)+(0.1491P)²+0.7853P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.1863
_refine_special_details          
'The void has solvent molecules. One site is occupied by a fully occupied H2O molecule. The other site consists of 2 x MeOH at 25% occupancy and modelled with restraints (DFIX, ISOR) and constraints (EADP), as well as a partially occupied H2O molecule (15% occupied), modelled with restraints (ISOR).'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9(4)
 0.1(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C27-O26
 1.45 with sigma of 0.01
 O24-C25
 1.45 with sigma of 0.01
 O17-H17 = O19-H19
 0.88 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C27) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(C25)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C25) = Uanis(C27)
Uanis(O24) = Uanis(O26)
5. Others
 Fixed Sof: C25(0.25) H25A(0.25) H25B(0.25) H25C(0.25) O24(0.25) H24(0.25)
 C27(0.25) H27A(0.25) H27B(0.25) H27C(0.25) O26(0.25) H26(0.25) O28(0.15)
 H28A(0.15) H28B(0.15)
6.a Riding coordinates:
 O28(H28A,H28B)
6.b Free rotating group:
 O23(H23A,H23B)
6.c Ternary CH refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C16(H16), C18(H18)
6.d Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C11(H11A,H11B), C12(H12A,H12B)
6.e Idealised Me refined as rotating group:
 N8(H8A,H8B,H8C), N10(H10A,H10B,H10C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
6.f Idealised tetrahedral OH refined as rotating group:
 O24(H24), O26(H26)
;
_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
C4 C 0.4388(3) 0.1354(9) 0.6013(3) 0.0443(11) Uani 1 1 d . . . . .
H4A H 0.474697 0.245541 0.595707 0.053 Uiso 1 1 calc R U . . .
H4B H 0.471304 0.060649 0.659029 0.053 Uiso 1 1 calc R U . . .
C5 C 0.3633(3) 0.2387(8) 0.6030(3) 0.0353(10) Uani 1 1 d . . . . .
H5 H 0.330541 0.307831 0.543076 0.042 Uiso 1 1 calc R U . . .
C6 C 0.3892(3) 0.4096(6) 0.6752(3) 0.0307(8) Uani 1 1 d . . . . .
H6A H 0.340094 0.494378 0.665376 0.037 Uiso 1 1 calc R U . . .
H6B H 0.429784 0.503881 0.669163 0.037 Uiso 1 1 calc R U . . .
C7 C 0.4277(2) 0.3180(6) 0.7706(3) 0.0255(8) Uani 1 1 d . . . . .
H7 H 0.478415 0.237258 0.780373 0.031 Uiso 1 1 calc R U . . .
C9 C 0.3674(2) 0.1679(6) 0.7815(3) 0.0278(8) Uani 1 1 d . . . . .
H9 H 0.316034 0.246796 0.770755 0.033 Uiso 1 1 calc R U . . .
C11 C 0.3445(3) -0.0066(7) 0.7120(3) 0.0337(9) Uani 1 1 d . . . . .
H11A H 0.304274 -0.102174 0.718058 0.040 Uiso 1 1 calc R U . . .
H11B H 0.394672 -0.088892 0.723784 0.040 Uiso 1 1 calc R U . . .
C12 C 0.3066(3) 0.0800(8) 0.6156(3) 0.0371(10) Uani 1 1 d . . . . .
H12A H 0.295601 -0.037519 0.572762 0.045 Uiso 1 1 calc R U . . .
H12B H 0.252980 0.148032 0.601461 0.045 Uiso 1 1 calc R U . . .
N1 N 0.3276(5) 0.1017(15) 0.3778(4) 0.086(2) Uani 1 1 d . . . . .
N2 N 0.3705(4) 0.0590(11) 0.4506(4) 0.0671(16) Uani 1 1 d . . . . .
N3 N 0.4146(4) -0.0156(10) 0.5251(4) 0.0635(14) Uani 1 1 d . . . . .
N8 N 0.4533(2) 0.4942(5) 0.8371(2) 0.0259(7) Uani 1 1 d . . . . .
H8A H 0.479268 0.594779 0.820450 0.031 Uiso 1 1 calc R U . . .
H8B H 0.488579 0.444973 0.892885 0.031 Uiso 1 1 calc R U . . .
H8C H 0.407717 0.550071 0.838306 0.031 Uiso 1 1 calc R U . . .
N10 N 0.4039(2) 0.0745(5) 0.8738(2) 0.0287(7) Uani 1 1 d . . . . .
H10A H 0.365820 -0.009897 0.878915 0.034 Uiso 1 1 calc R U . . .
H10B H 0.418809 0.178923 0.915591 0.034 Uiso 1 1 calc R U . . .
H10C H 0.449393 -0.002442 0.883196 0.034 Uiso 1 1 calc R U . . .
C15 C 0.5895(2) -0.1278(6) 0.8755(3) 0.0277(8) Uani 1 1 d . . . . .
C16 C 0.6748(2) -0.0405(6) 0.8954(3) 0.0267(8) Uani 1 1 d . . . . .
H16 H 0.712152 -0.159410 0.899146 0.032 Uiso 1 1 calc R U . . .
C18 C 0.6677(2) 0.1091(6) 0.8211(3) 0.0265(8) Uani 1 1 d . . . . .
H18 H 0.648676 0.028248 0.763521 0.032 Uiso 1 1 calc R U . . .
C20 C 0.7529(2) 0.2041(7) 0.8453(3) 0.0274(8) Uani 1 1 d . . . . .
O13 O 0.56071(18) -0.0891(5) 0.9299(2) 0.0319(7) Uani 1 1 d . . . . .
O14 O 0.55300(19) -0.2342(5) 0.8044(2) 0.0364(8) Uani 1 1 d . . . . .
O17 O 0.71184(19) 0.0765(5) 0.97743(19) 0.0323(7) Uani 1 1 d D . . . .
O19 O 0.60904(18) 0.2675(5) 0.8087(2) 0.0356(7) Uani 1 1 d D . . . .
O21 O 0.75965(18) 0.3992(5) 0.8570(2) 0.0312(7) Uani 1 1 d . . . . .
O22 O 0.80953(18) 0.0815(5) 0.8521(2) 0.0332(7) Uani 1 1 d . . . . .
C25 C 0.6150(12) 0.582(4) 0.6403(17) 0.031(4) Uani 0.25 1 d D U P A -2
H25A H 0.618851 0.603860 0.584040 0.047 Uiso 0.25 1 calc R U P A -2
H25B H 0.604946 0.433686 0.646496 0.047 Uiso 0.25 1 calc R U P A -2
H25C H 0.667048 0.625941 0.691613 0.047 Uiso 0.25 1 calc R U P A -2
O24 O 0.5482(9) 0.705(2) 0.6385(10) 0.046(2) Uani 0.25 1 d D U P A -2
H24 H 0.552385 0.712301 0.690764 0.069 Uiso 0.25 1 calc R U P A -2
C27 C 0.5898(13) 0.613(4) 0.6180(11) 0.031(4) Uani 0.25 1 d D U P B -1
H27A H 0.537977 0.662104 0.616383 0.047 Uiso 0.25 1 calc R U P B -1
H27B H 0.629066 0.729349 0.633831 0.047 Uiso 0.25 1 calc R U P B -1
H27C H 0.613510 0.501227 0.663345 0.047 Uiso 0.25 1 calc R U P B -1
O26 O 0.5731(10) 0.531(2) 0.5300(9) 0.046(2) Uani 0.25 1 d D U P B -1
H26 H 0.523460 0.492307 0.502406 0.069 Uiso 0.25 1 calc R U P B -1
O23 O 0.59285(17) 0.3608(4) 0.99418(19) 0.0292(6) Uani 1 1 d G . . . .
H23A H 0.629009 0.451950 1.029339 0.044 Uiso 1 1 d G U . . .
H23B H 0.619851 0.287457 0.971991 0.044 Uiso 1 1 d G U . . .
H19 H 0.634(4) 0.390(5) 0.822(4) 0.055(18) Uiso 1 1 d D . . . .
H17 H 0.720(4) 0.000(8) 1.025(3) 0.042(15) Uiso 1 1 d D . . . .
O28 O 0.612(2) 0.634(5) 0.676(3) 0.061(8) Uani 0.15 1 d . U P C -3
H28A H 0.555451 0.628065 0.625739 0.092 Uiso 0.15 1 d R U P C -3
H28B H 0.623031 0.545845 0.728359 0.092 Uiso 0.15 1 d R 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
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.533(7) . ?
C4 N3 1.489(7) . ?
C5 H5 1.0000 . ?
C5 C6 1.528(6) . ?
C5 C12 1.524(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.529(5) . ?
C7 H7 1.0000 . ?
C7 C9 1.527(5) . ?
C7 N8 1.493(5) . ?
C9 H9 1.0000 . ?
C9 C11 1.519(5) . ?
C9 N10 1.491(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.531(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N1 N2 1.134(9) . ?
N2 N3 1.224(8) . ?
N8 H8A 0.9100 . ?
N8 H8B 0.9100 . ?
N8 H8C 0.9100 . ?
N10 H10A 0.9100 . ?
N10 H10B 0.9100 . ?
N10 H10C 0.9100 . ?
C15 C16 1.531(5) . ?
C15 O13 1.260(5) . ?
C15 O14 1.258(5) . ?
C16 H16 1.0000 . ?
C16 C18 1.521(5) . ?
C16 O17 1.426(5) . ?
C18 H18 1.0000 . ?
C18 C20 1.532(5) . ?
C18 O19 1.413(5) . ?
C20 O21 1.256(5) . ?
C20 O22 1.254(5) . ?
O17 H17 0.879(14) . ?
O19 H19 0.881(14) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25 O24 1.431(12) . ?
O24 H24 0.8400 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C27 O26 1.451(12) . ?
O26 H26 0.8400 . ?
O23 H23A 0.8715 . ?
O23 H23B 0.8720 . ?
O28 H28A 0.9830 . ?
O28 H28B 0.9830 . ?

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
H4A C4 H4B 107.9 . . ?
C5 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
N3 C4 H4A 109.2 . . ?
N3 C4 H4B 109.2 . . ?
N3 C4 C5 112.0(4) . . ?
C4 C5 H5 107.4 . . ?
C6 C5 C4 111.3(4) . . ?
C6 C5 H5 107.4 . . ?
C12 C5 C4 112.6(4) . . ?
C12 C5 H5 107.4 . . ?
C12 C5 C6 110.4(4) . . ?
C5 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
C5 C6 C7 112.1(3) . . ?
H6A C6 H6B 107.9 . . ?
C7 C6 H6A 109.2 . . ?
C7 C6 H6B 109.2 . . ?
C6 C7 H7 108.4 . . ?
C9 C7 C6 110.5(3) . . ?
C9 C7 H7 108.4 . . ?
N8 C7 C6 108.8(3) . . ?
N8 C7 H7 108.4 . . ?
N8 C7 C9 112.3(3) . . ?
C7 C9 H9 108.9 . . ?
C11 C9 C7 109.2(3) . . ?
C11 C9 H9 108.9 . . ?
N10 C9 C7 111.5(3) . . ?
N10 C9 H9 108.9 . . ?
N10 C9 C11 109.3(3) . . ?
C9 C11 H11A 109.3 . . ?
C9 C11 H11B 109.3 . . ?
C9 C11 C12 111.7(4) . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C5 C12 C11 112.1(3) . . ?
C5 C12 H12A 109.2 . . ?
C5 C12 H12B 109.2 . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
N1 N2 N3 171.0(8) . . ?
N2 N3 C4 114.5(6) . . ?
C7 N8 H8A 109.5 . . ?
C7 N8 H8B 109.5 . . ?
C7 N8 H8C 109.5 . . ?
H8A N8 H8B 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
C9 N10 H10A 109.5 . . ?
C9 N10 H10B 109.5 . . ?
C9 N10 H10C 109.5 . . ?
H10A N10 H10B 109.5 . . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
O13 C15 C16 118.9(4) . . ?
O14 C15 C16 116.5(3) . . ?
O14 C15 O13 124.7(4) . . ?
C15 C16 H16 109.1 . . ?
C18 C16 C15 110.5(3) . . ?
C18 C16 H16 109.1 . . ?
O17 C16 C15 112.7(3) . . ?
O17 C16 H16 109.1 . . ?
O17 C16 C18 106.2(3) . . ?
C16 C18 H18 108.7 . . ?
C16 C18 C20 109.5(3) . . ?
C20 C18 H18 108.7 . . ?
O19 C18 C16 110.1(3) . . ?
O19 C18 H18 108.7 . . ?
O19 C18 C20 111.0(3) . . ?
O21 C20 C18 116.6(3) . . ?
O22 C20 C18 117.7(4) . . ?
O22 C20 O21 125.8(4) . . ?
C16 O17 H17 112(4) . . ?
C18 O19 H19 109(5) . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O24 C25 H25A 109.5 . . ?
O24 C25 H25B 109.5 . . ?
O24 C25 H25C 109.5 . . ?
C25 O24 H24 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O26 C27 H27A 109.5 . . ?
O26 C27 H27B 109.5 . . ?
O26 C27 H27C 109.5 . . ?
C27 O26 H26 109.5 . . ?
H23A O23 H23B 104.2 . . ?
H28A O28 H28B 116.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C7 H7 O19 1.00 2.20 3.069(5) 144 . yes
N8 H8A O14 0.91 1.84 2.732(4) 167 1_565 yes
N8 H8B O23 0.91 1.95 2.815(4) 159 . yes
N8 H8C O22 0.91 1.91 2.789(4) 162 3_455 yes
N10 H10A O21 0.91 1.88 2.740(4) 157 3_445 yes
N10 H10B O23 0.91 1.98 2.837(4) 155 2_657 yes
N10 H10C O13 0.91 1.89 2.761(5) 161 . yes
O24 H24 O14 0.84 1.92 2.751(15) 172 1_565 yes
O23 H23A O22 0.87 1.95 2.742(4) 150 4_657 yes
O23 H23B O17 0.87 2.11 2.928(4) 155 . yes
O19 H19 O21 0.881(14) 2.07(6) 2.610(4) 119(5) . yes
O17 H17 O21 0.879(14) 1.94(2) 2.800(4) 165(6) 4_647 yes

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
C4 C5 C6 C7 -71.8(5) . . . . ?
C4 C5 C12 C11 72.5(5) . . . . ?
C5 C4 N3 N2 55.4(7) . . . . ?
C5 C6 C7 C9 -57.6(4) . . . . ?
C5 C6 C7 N8 178.6(3) . . . . ?
C6 C5 C12 C11 -52.6(5) . . . . ?
C6 C7 C9 C11 58.4(4) . . . . ?
C6 C7 C9 N10 179.4(3) . . . . ?
C7 C9 C11 C12 -57.6(4) . . . . ?
C9 C11 C12 C5 55.6(5) . . . . ?
C12 C5 C6 C7 54.0(5) . . . . ?
N3 C4 C5 C6 -174.0(4) . . . . ?
N3 C4 C5 C12 61.4(5) . . . . ?
N8 C7 C9 C11 -179.9(3) . . . . ?
N8 C7 C9 N10 -58.9(4) . . . . ?
N10 C9 C11 C12 -179.9(3) . . . . ?
C15 C16 C18 C20 176.7(3) . . . . ?
C15 C16 C18 O19 54.4(4) . . . . ?
C16 C18 C20 O21 -116.7(4) . . . . ?
C16 C18 C20 O22 62.9(5) . . . . ?
O13 C15 C16 C18 -118.0(4) . . . . ?
O13 C15 C16 O17 0.6(5) . . . . ?
O14 C15 C16 C18 61.7(5) . . . . ?
O14 C15 C16 O17 -179.6(3) . . . . ?
O17 C16 C18 C20 54.2(4) . . . . ?
O17 C16 C18 O19 -68.1(4) . . . . ?
O19 C18 C20 O21 5.1(5) . . . . ?
O19 C18 C20 O22 -175.3(3) . . . . ?

_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id POD58R1-2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9(4)
2 0.1(4)

