# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_msb457_0m
_database_code_depnum_ccdc_archive 'CCDC 1023322'
_audit_update_record             
;
2014-09-08 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H59 I N6 O2 P4 Pd, 2(C H Cl3)'
_chemical_formula_sum            'C32 H61 Cl6 I N6 O2 P4 Pd'
_chemical_formula_weight         1131.74

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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   15.3398(15)
_cell_length_b                   16.6898(17)
_cell_length_c                   18.9655(19)
_cell_angle_alpha                90
_cell_angle_beta                 94.375(2)
_cell_angle_gamma                90
_cell_volume                     4841.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4782
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      28.30

_exptl_crystal_description       column
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_F_000             2288
_exptl_transmission_factor_min   0.758
_exptl_transmission_factor_max   0.863
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.519
_shelx_estimated_absorpt_T_min   0.753
_shelx_estimated_absorpt_T_max   0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick 2008b)'
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_T_max  0.89

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, collected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 20 sec/frame. From 2203 reflections 
chosen from the full data set and having I/σ(I) > 15.0 it was 
determined that the crystal adopted a primitive monoclinic unit 
cell and was twinned via a 180 deg. rotation about the c* 
axis (CELL_NOW (Sheldrick, 2008a)). Integration of the 2-component 
raw data was accomplished with the multi-component version of 
SAINT under control of the 2-component orientation file generated 
by CELL_NOW.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3660

_diffrn_reflns_number            106951
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.050
_diffrn_reflns_theta_max         28.341
_diffrn_reflns_theta_full        28.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             19796
_reflns_number_gt                17097
_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, 2009)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_structure_solution    'SHELXS (Bruker, 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2009)'

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. H-atoms attached to carbon 
were placed in calculated positions (C---H = 0.95 - 0.98 Å) while those 
attached to nitrogen were placed in locations derived from a difference 
map and their coordinates adjusted to give N---H = 0.91 Å. All were 
included as riding contributions with isotropic displacement parameters 
1.2 - 1.5 times those of the attached atoms. The structure was 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)+(0.0248P)²+12.6312P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     hesvy
_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         19796
_refine_ls_number_parameters     488
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1020
_refine_ls_wR_factor_gt          0.0973
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_restrained_S_all      1.169
_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
I1 I 0.75376(2) -0.00425(2) 0.24668(2) 0.02551(8) Uani 1 1 d . . . . .
Pd1 Pd 0.74195(2) 0.01590(2) 0.10711(2) 0.01481(7) Uani 1 1 d . . . . .
P1 P 0.86276(8) -0.22779(7) 0.15448(7) 0.0184(2) Uani 1 1 d . . . . .
P2 P 0.79911(8) -0.10670(7) 0.08545(6) 0.0154(2) Uani 1 1 d . . . . .
P3 P 0.68095(8) 0.14054(7) 0.09145(6) 0.0156(2) Uani 1 1 d . . . . .
P4 P 0.62992(8) 0.25817(7) 0.16502(7) 0.0166(2) Uani 1 1 d . . . . .
O1 O 0.7957(2) -0.11154(18) -0.00148(17) 0.0196(7) Uani 1 1 d . . . . .
O2 O 0.6694(2) 0.15016(18) 0.00474(17) 0.0193(7) Uani 1 1 d . . . . .
N1 N 0.8889(3) -0.3024(2) 0.1026(2) 0.0255(9) Uani 1 1 d . . . . .
H1N H 0.8674 -0.3003 0.0521 0.031 Uiso 1 1 d R U . . .
N2 N 0.8967(2) -0.1390(2) 0.1149(2) 0.0171(8) Uani 1 1 d . . . . .
N3 N 0.7637(2) -0.1932(2) 0.1153(2) 0.0172(8) Uani 1 1 d . . . . .
N4 N 0.5938(3) 0.3347(2) 0.1154(2) 0.0202(8) Uani 1 1 d . . . . .
H4N H 0.5903 0.3309 0.0598 0.024 Uiso 1 1 d R U . . .
N5 N 0.5883(2) 0.1720(2) 0.1219(2) 0.0168(8) Uani 1 1 d . . . . .
N6 N 0.7214(2) 0.2270(2) 0.1230(2) 0.0164(8) Uani 1 1 d . . . . .
C1 C 0.9294(4) -0.3807(3) 0.1225(3) 0.0310(13) Uani 1 1 d . . . . .
C2 C 0.9256(7) -0.3960(4) 0.2002(4) 0.073(3) Uani 1 1 d . . . . .
H2A H 0.9598 -0.4439 0.2137 0.109 Uiso 1 1 calc R U . . .
H2B H 0.8647 -0.4042 0.2108 0.109 Uiso 1 1 calc R U . . .
H2C H 0.9497 -0.3498 0.2270 0.109 Uiso 1 1 calc R U . . .
C3 C 1.0247(4) -0.3790(4) 0.1044(6) 0.080(3) Uani 1 1 d . . . . .
H3A H 1.0514 -0.4316 0.1139 0.120 Uiso 1 1 calc R U . . .
H3B H 1.0567 -0.3383 0.1333 0.120 Uiso 1 1 calc R U . . .
H3C H 1.0273 -0.3659 0.0542 0.120 Uiso 1 1 calc R U . . .
C4 C 0.8807(4) -0.4458(3) 0.0799(4) 0.0399(15) Uani 1 1 d . . . . .
H4A H 0.9080 -0.4978 0.0912 0.060 Uiso 1 1 calc R U . . .
H4B H 0.8830 -0.4348 0.0293 0.060 Uiso 1 1 calc R U . . .
H4C H 0.8196 -0.4469 0.0917 0.060 Uiso 1 1 calc R U . . .
C5 C 0.9840(3) -0.1013(3) 0.1189(3) 0.0192(10) Uani 1 1 d . . . . .
C6 C 0.9737(4) -0.0103(3) 0.1088(4) 0.0420(16) Uani 1 1 d . . . . .
H6A H 0.9404 0.0006 0.0637 0.063 Uiso 1 1 calc R U . . .
H6B H 1.0316 0.0145 0.1088 0.063 Uiso 1 1 calc R U . . .
H6C H 0.9425 0.0119 0.1476 0.063 Uiso 1 1 calc R U . . .
C7 C 1.0319(4) -0.1184(5) 0.1893(3) 0.0516(19) Uani 1 1 d . . . . .
H7A H 0.9984 -0.0971 0.2271 0.077 Uiso 1 1 calc R U . . .
H7B H 1.0895 -0.0929 0.1915 0.077 Uiso 1 1 calc R U . . .
H7C H 1.0389 -0.1764 0.1954 0.077 Uiso 1 1 calc R U . . .
C8 C 1.0350(4) -0.1356(4) 0.0596(4) 0.0429(16) Uani 1 1 d . . . . .
H8A H 1.0412 -0.1937 0.0657 0.064 Uiso 1 1 calc R U . . .
H8B H 1.0930 -0.1108 0.0612 0.064 Uiso 1 1 calc R U . . .
H8C H 1.0034 -0.1243 0.0138 0.064 Uiso 1 1 calc R U . . .
C9 C 0.6748(3) -0.2250(3) 0.1235(3) 0.0223(10) Uani 1 1 d . . . . .
C10 C 0.6669(4) -0.2504(4) 0.2003(3) 0.0382(14) Uani 1 1 d . . . . .
H10A H 0.7078 -0.2943 0.2123 0.057 Uiso 1 1 calc R U . . .
H10B H 0.6070 -0.2685 0.2060 0.057 Uiso 1 1 calc R U . . .
H10C H 0.6807 -0.2048 0.2317 0.057 Uiso 1 1 calc R U . . .
C11 C 0.6598(3) -0.2972(3) 0.0734(3) 0.0312(12) Uani 1 1 d . . . . .
H11A H 0.6670 -0.2802 0.0247 0.047 Uiso 1 1 calc R U . . .
H11B H 0.6005 -0.3180 0.0767 0.047 Uiso 1 1 calc R U . . .
H11C H 0.7024 -0.3392 0.0870 0.047 Uiso 1 1 calc R U . . .
C12 C 0.6066(3) -0.1600(3) 0.1041(3) 0.0303(12) Uani 1 1 d . . . . .
H12A H 0.6134 -0.1162 0.1385 0.045 Uiso 1 1 calc R U . . .
H12B H 0.5478 -0.1828 0.1047 0.045 Uiso 1 1 calc R U . . .
H12C H 0.6151 -0.1394 0.0567 0.045 Uiso 1 1 calc R U . . .
C13 C 0.5468(3) 0.4076(3) 0.1382(3) 0.0244(11) Uani 1 1 d . . . . .
C14 C 0.5174(4) 0.3966(3) 0.2124(3) 0.0379(14) Uani 1 1 d . . . . .
H14A H 0.4862 0.3455 0.2150 0.057 Uiso 1 1 calc R U . . .
H14B H 0.4784 0.4406 0.2233 0.057 Uiso 1 1 calc R U . . .
H14C H 0.5686 0.3964 0.2466 0.057 Uiso 1 1 calc R U . . .
C15 C 0.4670(4) 0.4194(3) 0.0858(4) 0.0421(16) Uani 1 1 d . . . . .
H15A H 0.4295 0.3719 0.0861 0.063 Uiso 1 1 calc R U . . .
H15B H 0.4863 0.4274 0.0383 0.063 Uiso 1 1 calc R U . . .
H15C H 0.4341 0.4665 0.0996 0.063 Uiso 1 1 calc R U . . .
C16 C 0.6068(4) 0.4803(3) 0.1360(3) 0.0332(13) Uani 1 1 d . . . . .
H16A H 0.6572 0.4733 0.1704 0.050 Uiso 1 1 calc R U . . .
H16B H 0.5747 0.5287 0.1476 0.050 Uiso 1 1 calc R U . . .
H16C H 0.6272 0.4856 0.0885 0.050 Uiso 1 1 calc R U . . .
C17 C 0.5055(3) 0.1294(3) 0.1304(3) 0.0189(9) Uani 1 1 d . . . . .
C18 C 0.4301(3) 0.1890(3) 0.1127(3) 0.0267(11) Uani 1 1 d . . . . .
H18A H 0.4357 0.2344 0.1455 0.040 Uiso 1 1 calc R U . . .
H18B H 0.3740 0.1621 0.1173 0.040 Uiso 1 1 calc R U . . .
H18C H 0.4327 0.2083 0.0642 0.040 Uiso 1 1 calc R U . . .
C19 C 0.4980(3) 0.0596(3) 0.0783(3) 0.0305(13) Uani 1 1 d . . . . .
H19A H 0.5044 0.0796 0.0304 0.046 Uiso 1 1 calc R U . . .
H19B H 0.4407 0.0341 0.0801 0.046 Uiso 1 1 calc R U . . .
H19C H 0.5441 0.0204 0.0910 0.046 Uiso 1 1 calc R U . . .
C20 C 0.5032(4) 0.1003(3) 0.2058(3) 0.0333(13) Uani 1 1 d . . . . .
H20A H 0.5514 0.0627 0.2167 0.050 Uiso 1 1 calc R U . . .
H20B H 0.4474 0.0734 0.2115 0.050 Uiso 1 1 calc R U . . .
H20C H 0.5093 0.1461 0.2382 0.050 Uiso 1 1 calc R U . . .
C21 C 0.8138(3) 0.2532(3) 0.1342(3) 0.0198(10) Uani 1 1 d . . . . .
C22 C 0.8142(3) 0.3436(3) 0.1484(3) 0.0314(12) Uani 1 1 d . . . . .
H22A H 0.7839 0.3714 0.1081 0.047 Uiso 1 1 calc R U . . .
H22B H 0.8747 0.3627 0.1550 0.047 Uiso 1 1 calc R U . . .
H22C H 0.7842 0.3546 0.1912 0.047 Uiso 1 1 calc R U . . .
C23 C 0.8576(3) 0.2357(4) 0.0674(3) 0.0347(13) Uani 1 1 d . . . . .
H23A H 0.8583 0.1777 0.0593 0.052 Uiso 1 1 calc R U . . .
H23B H 0.9177 0.2560 0.0720 0.052 Uiso 1 1 calc R U . . .
H23C H 0.8252 0.2620 0.0273 0.052 Uiso 1 1 calc R U . . .
C24 C 0.8598(3) 0.2100(3) 0.1970(3) 0.0308(12) Uani 1 1 d . . . . .
H24A H 0.8289 0.2207 0.2394 0.046 Uiso 1 1 calc R U . . .
H24B H 0.9201 0.2293 0.2044 0.046 Uiso 1 1 calc R U . . .
H24C H 0.8600 0.1523 0.1878 0.046 Uiso 1 1 calc R U . . .
C25 C 0.7344(3) 0.0202(2) 0.0025(2) 0.0149(8) Uani 1 1 d . . . . .
C26 C 0.6991(3) 0.0867(2) -0.0339(2) 0.0160(9) Uani 1 1 d . . . . .
C27 C 0.6928(3) 0.0902(3) -0.1073(2) 0.0203(10) Uani 1 1 d . . . . .
H27 H 0.6682 0.1357 -0.1315 0.024 Uiso 1 1 calc R U . . .
C28 C 0.7231(3) 0.0262(3) -0.1442(2) 0.0215(9) Uani 1 1 d . . . . .
H28 H 0.7198 0.0287 -0.1943 0.026 Uiso 1 1 calc R U . . .
C29 C 0.7585(3) -0.0423(3) -0.1106(2) 0.0193(9) Uani 1 1 d . . . . .
H29 H 0.7783 -0.0862 -0.1370 0.023 Uiso 1 1 calc R U . . .
C30 C 0.7636(3) -0.0436(2) -0.0367(2) 0.0167(9) Uani 1 1 d . . . . .
C31 C 0.8547(3) 0.8210(3) 0.3564(3) 0.0279(11) Uani 1 1 d . . . . .
H31 H 0.8365 0.8310 0.3054 0.033 Uiso 1 1 calc R U . . .
Cl1 Cl 0.76373(11) 0.83347(11) 0.40475(9) 0.0524(4) Uani 1 1 d . . . . .
Cl2 Cl 0.93717(9) 0.89027(9) 0.38351(9) 0.0383(3) Uani 1 1 d . . . . .
Cl3 Cl 0.89583(11) 0.72298(9) 0.36483(11) 0.0506(4) Uani 1 1 d . . . . .
C32 C 0.6880(4) 0.3705(3) 0.8896(3) 0.0311(12) Uani 1 1 d . . . . .
H32 H 0.6808 0.4007 0.8440 0.037 Uiso 1 1 calc R U . . .
Cl4 Cl 0.73377(11) 0.43511(9) 0.95501(9) 0.0451(4) Uani 1 1 d . . . . .
Cl5 Cl 0.58382(10) 0.33697(11) 0.91098(10) 0.0493(4) Uani 1 1 d . . . . .
Cl6 Cl 0.75706(10) 0.28842(9) 0.87825(8) 0.0407(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Pd1 2.6608(5) . ?
Pd1 C25 1.980(4) . ?
Pd1 P2 2.2758(12) . ?
Pd1 P3 2.2909(12) . ?
P1 N1 1.655(4) . ?
P1 N3 1.739(4) . ?
P1 N2 1.758(4) . ?
P2 O1 1.647(3) . ?
P2 N2 1.649(4) . ?
P2 N3 1.658(4) . ?
P3 O2 1.648(3) . ?
P3 N5 1.660(4) . ?
P3 N6 1.665(4) . ?
P4 N4 1.657(4) . ?
P4 N6 1.746(4) . ?
P4 N5 1.751(4) . ?
O1 C30 1.387(5) . ?
O2 C26 1.385(5) . ?
N1 C1 1.483(6) . ?
N1 H1N 0.9895 . ?
N2 C5 1.476(6) . ?
N3 C9 1.482(6) . ?
N4 C13 1.494(6) . ?
N4 H4N 1.0536 . ?
N5 C17 1.475(6) . ?
N6 C21 1.483(6) . ?
C1 C2 1.502(9) . ?
C1 C4 1.516(8) . ?
C1 C3 1.528(9) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C7 1.502(7) . ?
C5 C8 1.529(7) . ?
C5 C6 1.537(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.530(7) . ?
C9 C12 1.532(7) . ?
C9 C11 1.540(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.520(8) . ?
C13 C16 1.526(7) . ?
C13 C15 1.529(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C20 1.513(7) . ?
C17 C19 1.526(7) . ?
C17 C18 1.543(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C23 1.507(7) . ?
C21 C24 1.519(7) . ?
C21 C22 1.533(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C30 1.393(6) . ?
C25 C26 1.393(6) . ?
C26 C27 1.389(6) . ?
C27 C28 1.377(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.397(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.398(6) . ?
C29 H29 0.9500 . ?
C31 Cl1 1.739(5) . ?
C31 Cl3 1.757(6) . ?
C31 Cl2 1.762(5) . ?
C31 H31 1.0000 . ?
C32 Cl4 1.750(6) . ?
C32 Cl6 1.755(6) . ?
C32 Cl5 1.769(6) . ?
C32 H32 1.0000 . ?

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
C25 Pd1 P2 81.12(12) . . ?
C25 Pd1 P3 81.08(12) . . ?
P2 Pd1 P3 162.20(4) . . ?
C25 Pd1 I1 174.79(12) . . ?
P2 Pd1 I1 93.90(3) . . ?
P3 Pd1 I1 103.88(3) . . ?
N1 P1 N3 103.9(2) . . ?
N1 P1 N2 106.7(2) . . ?
N3 P1 N2 79.39(18) . . ?
O1 P2 N2 106.37(19) . . ?
O1 P2 N3 108.23(18) . . ?
N2 P2 N3 84.97(18) . . ?
O1 P2 Pd1 103.97(12) . . ?
N2 P2 Pd1 125.84(15) . . ?
N3 P2 Pd1 125.49(14) . . ?
O2 P3 N5 106.67(19) . . ?
O2 P3 N6 106.41(18) . . ?
N5 P3 N6 84.64(18) . . ?
O2 P3 Pd1 103.27(12) . . ?
N5 P3 Pd1 126.45(14) . . ?
N6 P3 Pd1 127.12(14) . . ?
N4 P4 N6 102.5(2) . . ?
N4 P4 N5 105.9(2) . . ?
N6 P4 N5 79.60(18) . . ?
C30 O1 P2 115.2(3) . . ?
C26 O2 P3 116.0(3) . . ?
C1 N1 P1 128.9(4) . . ?
C1 N1 H1N 112.4 . . ?
P1 N1 H1N 118.0 . . ?
C5 N2 P2 132.4(3) . . ?
C5 N2 P1 129.4(3) . . ?
P2 N2 P1 97.43(19) . . ?
C9 N3 P2 132.5(3) . . ?
C9 N3 P1 128.2(3) . . ?
P2 N3 P1 97.83(19) . . ?
C13 N4 P4 127.6(4) . . ?
C13 N4 H4N 110.6 . . ?
P4 N4 H4N 120.7 . . ?
C17 N5 P3 130.8(3) . . ?
C17 N5 P4 129.2(3) . . ?
P3 N5 P4 97.53(19) . . ?
C21 N6 P3 129.3(3) . . ?
C21 N6 P4 129.8(3) . . ?
P3 N6 P4 97.53(19) . . ?
N1 C1 C2 110.6(5) . . ?
N1 C1 C4 108.4(4) . . ?
C2 C1 C4 110.3(5) . . ?
N1 C1 C3 108.4(5) . . ?
C2 C1 C3 109.5(6) . . ?
C4 C1 C3 109.6(6) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C7 110.1(4) . . ?
N2 C5 C8 108.4(4) . . ?
C7 C5 C8 109.9(5) . . ?
N2 C5 C6 109.3(4) . . ?
C7 C5 C6 109.7(5) . . ?
C8 C5 C6 109.4(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 109.8(4) . . ?
N3 C9 C12 109.7(4) . . ?
C10 C9 C12 108.8(4) . . ?
N3 C9 C11 108.1(4) . . ?
C10 C9 C11 110.5(4) . . ?
C12 C9 C11 109.8(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 110.7(4) . . ?
N4 C13 C16 109.5(4) . . ?
C14 C13 C16 110.1(5) . . ?
N4 C13 C15 107.2(4) . . ?
C14 C13 C15 109.7(5) . . ?
C16 C13 C15 109.5(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N5 C17 C20 109.9(4) . . ?
N5 C17 C19 108.7(4) . . ?
C20 C17 C19 111.2(4) . . ?
N5 C17 C18 107.6(4) . . ?
C20 C17 C18 109.9(4) . . ?
C19 C17 C18 109.5(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N6 C21 C23 107.7(4) . . ?
N6 C21 C24 110.8(4) . . ?
C23 C21 C24 111.0(4) . . ?
N6 C21 C22 107.8(4) . . ?
C23 C21 C22 110.0(4) . . ?
C24 C21 C22 109.5(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 118.2(4) . . ?
C30 C25 Pd1 120.7(3) . . ?
C26 C25 Pd1 121.1(3) . . ?
O2 C26 C27 119.8(4) . . ?
O2 C26 C25 118.6(4) . . ?
C27 C26 C25 121.7(4) . . ?
C28 C27 C26 118.4(4) . . ?
C28 C27 H27 120.8 . . ?
C26 C27 H27 120.8 . . ?
C27 C28 C29 122.5(4) . . ?
C27 C28 H28 118.7 . . ?
C29 C28 H28 118.7 . . ?
C28 C29 C30 117.4(4) . . ?
C28 C29 H29 121.3 . . ?
C30 C29 H29 121.3 . . ?
O1 C30 C25 119.0(4) . . ?
O1 C30 C29 119.1(4) . . ?
C25 C30 C29 121.8(4) . . ?
Cl1 C31 Cl3 111.1(3) . . ?
Cl1 C31 Cl2 110.8(3) . . ?
Cl3 C31 Cl2 109.8(3) . . ?
Cl1 C31 H31 108.3 . . ?
Cl3 C31 H31 108.3 . . ?
Cl2 C31 H31 108.3 . . ?
Cl4 C32 Cl6 110.8(3) . . ?
Cl4 C32 Cl5 110.7(3) . . ?
Cl6 C32 Cl5 110.2(3) . . ?
Cl4 C32 H32 108.4 . . ?
Cl6 C32 H32 108.4 . . ?
Cl5 C32 H32 108.4 . . ?

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
N4 H4N Cl5 1.05 2.82 3.868(5) 174 1_554
C3 H3A Cl2 0.98 2.98 3.899(7) 157 2_735
C11 H11A Cl1 0.98 2.95 3.731(6) 138 4_565
C11 H11B Cl5 0.98 2.87 3.830(5) 166 3_656
C20 H20A I1 0.98 3.31 4.238(6) 159 .
C23 H23C Cl6 0.98 2.97 3.895(6) 158 1_554
C24 H24A Cl6 0.98 2.93 3.889(6) 165 4_565
C24 H24C I1 0.98 3.32 4.069(5) 135 .
C27 H27 Cl6 0.95 2.89 3.468(5) 120 1_554
C29 H29 Cl3 0.95 2.91 3.728(5) 145 4_565
C31 H31 I1 1.00 3.19 3.839(5) 124 1_565
C32 H32 I1 1.00 2.82 3.710(5) 148 4_566

_refine_diff_density_max         1.149
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.118

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_msb473_0m
_database_code_depnum_ccdc_archive 'CCDC 1023323'
_audit_update_record             
;
2014-09-08 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H59 I N6 Ni O2 P4, 2(C H Cl3)'
_chemical_formula_sum            'C32 H61 Cl6 I N6 Ni O2 P4'
_chemical_formula_weight         1084.05

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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   16.6214(16)
_cell_length_b                   15.2055(15)
_cell_length_c                   19.0941(19)
_cell_angle_alpha                90
_cell_angle_beta                 91.5300(10)
_cell_angle_gamma                90
_cell_volume                     4824.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4594
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      27.28

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_F_000             2216
_exptl_transmission_factor_min   0.554
_exptl_transmission_factor_max   0.928
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.542
_shelx_estimated_absorpt_T_min   0.738
_shelx_estimated_absorpt_T_max   0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2009)'
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.79

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, collected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 20 sec/frame. Analysis of 2665 reflections 
having I/σ(I) > 15 and chosen from the full data set with 
CELL_NOW (Sheldrick, 2008a) showed the crystal to belong to the 
monoclinic system and to be twinned by a 180 ° rotation about the 
c* axis. The raw data were processed using the multi-component 
version of SAINT under control of the two-component orientation 
file generated by CELL_NOW.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3660
_diffrn_reflns_number            102296
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.815
_diffrn_reflns_theta_max         27.912
_diffrn_reflns_theta_full        27.900
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             19001
_reflns_number_gt                13299
_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, 2009)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_structure_solution    'SHELXT (Bruker, 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2009)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. H-atoms were placed in
 calculated positions (C---H = 0.95 - 0.98 Å) and included as riding
 contributions with isotropic displacement parameters 1.2 - 1.5 times those
 of the attached carbon atoms. The side of the molecule containing P1, P2
 and their substituents appeared to be affected by positional disorder
 which was most pronounced for the N3/C9/C10/C11/C12 moiety. Two independent
 locations were found for this moiety which were refined subject to
 restraints that the geometry be the same for both. It is apparent, however,
 that the rest of this diphosphazane unit is affected by a smaller degree
 of disorder, particularly P2, but it did not appear fruitful to model
 the disorder further. The structure was 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)+(0.0343P)²+15.7397P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_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         19001
_refine_ls_number_parameters     550
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1428
_refine_ls_wR_factor_gt          0.1199
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.51811(4) 0.76848(5) 0.89766(4) 0.02759(18) Uani 1 1 d . . . . .
I1 I 0.50527(2) 0.77822(3) 0.76700(2) 0.04094(13) Uani 1 1 d . . . . .
P1 P 0.63786(9) 0.82344(13) 0.91060(9) 0.0357(4) Uani 1 1 d . . . . .
P2 P 0.75187(10) 0.87319(17) 0.83267(10) 0.0522(6) Uani 1 1 d D . . . .
P3 P 0.40165(8) 0.70852(10) 0.91144(9) 0.0272(3) Uani 1 1 d . . . . .
P4 P 0.28411(8) 0.65098(10) 0.83494(10) 0.0306(4) Uani 1 1 d . . . . .
O1 O 0.6528(2) 0.8303(4) 0.9962(2) 0.0476(14) Uani 1 1 d . . . . .
O2 O 0.3935(2) 0.6992(3) 0.9972(2) 0.0304(10) Uani 1 1 d . . . . .
N1 N 0.7219(3) 0.7812(4) 0.8792(3) 0.0400(14) Uani 1 1 d . . . . .
N2 N 0.6706(3) 0.9163(4) 0.8773(3) 0.0389(14) Uani 1 1 d . . . . .
N4 N 0.3726(3) 0.6143(3) 0.8765(3) 0.0352(14) Uani 1 1 d . . . . .
N5 N 0.3146(2) 0.7456(3) 0.8793(3) 0.0266(11) Uani 1 1 d . . . . .
N6 N 0.2095(3) 0.6111(3) 0.8807(3) 0.0378(14) Uani 1 1 d . . . . .
H6N H 0.2197 0.6144 0.9261 0.045 Uiso 1 1 d R U . . .
C1 C 0.7467(4) 0.6882(6) 0.8703(4) 0.048(2) Uani 1 1 d . . . . .
C2 C 0.7107(4) 0.6487(6) 0.8035(4) 0.061(2) Uani 1 1 d . . . . .
H2A H 0.6519 0.6537 0.8039 0.091 Uiso 1 1 calc R U . . .
H2B H 0.7258 0.5865 0.8006 0.091 Uiso 1 1 calc R U . . .
H2C H 0.7311 0.6803 0.7629 0.091 Uiso 1 1 calc R U . . .
C3 C 0.7184(4) 0.6358(6) 0.9336(4) 0.053(2) Uani 1 1 d . . . . .
H3A H 0.7413 0.6616 0.9767 0.080 Uiso 1 1 calc R U . . .
H3B H 0.7363 0.5746 0.9296 0.080 Uiso 1 1 calc R U . . .
H3C H 0.6596 0.6375 0.9348 0.080 Uiso 1 1 calc R U . . .
C4 C 0.8386(4) 0.6848(7) 0.8685(4) 0.062(2) Uani 1 1 d . . . . .
H4A H 0.8570 0.7184 0.8282 0.093 Uiso 1 1 calc R U . . .
H4B H 0.8561 0.6235 0.8643 0.093 Uiso 1 1 calc R U . . .
H4C H 0.8615 0.7101 0.9117 0.093 Uiso 1 1 calc R U . . .
C5 C 0.6319(4) 1.0038(5) 0.8703(4) 0.0419(18) Uani 1 1 d . . . . .
C6 C 0.6045(4) 1.0215(6) 0.7951(4) 0.051(2) Uani 1 1 d . . . . .
H6A H 0.6510 1.0190 0.7647 0.077 Uiso 1 1 calc R U . . .
H6B H 0.5799 1.0799 0.7919 0.077 Uiso 1 1 calc R U . . .
H6C H 0.5650 0.9769 0.7802 0.077 Uiso 1 1 calc R U . . .
C7 C 0.6932(4) 1.0741(5) 0.8942(4) 0.054(2) Uani 1 1 d . . . . .
H7A H 0.7374 1.0762 0.8613 0.081 Uiso 1 1 calc R U . . .
H7B H 0.7146 1.0593 0.9411 0.081 Uiso 1 1 calc R U . . .
H7C H 0.6667 1.1316 0.8956 0.081 Uiso 1 1 calc R U . . .
C8 C 0.5598(4) 1.0066(5) 0.9186(4) 0.057(2) Uani 1 1 d . . . . .
H8A H 0.5329 1.0638 0.9141 0.085 Uiso 1 1 calc R U . . .
H8B H 0.5785 0.9981 0.9672 0.085 Uiso 1 1 calc R U . . .
H8C H 0.5218 0.9598 0.9054 0.085 Uiso 1 1 calc R U . . .
N3 N 0.8375(5) 0.8980(7) 0.8680(6) 0.028(2) Uani 0.585(6) 1 d D U P A 1
H3N H 0.8403 0.8970 0.9140 0.033 Uiso 0.585(6) 1 calc R U P A 1
C9 C 0.9125(5) 0.9223(6) 0.8323(6) 0.033(2) Uani 0.585(6) 1 d D . P A 1
C10 C 0.9242(7) 1.0209(8) 0.8409(9) 0.047(3) Uani 0.585(6) 1 d D . P A 1
H10A H 0.8802 1.0521 0.8164 0.071 Uiso 0.585(6) 1 calc R U P A 1
H10B H 0.9756 1.0382 0.8211 0.071 Uiso 0.585(6) 1 calc R U P A 1
H10C H 0.9243 1.0361 0.8908 0.071 Uiso 0.585(6) 1 calc R U P A 1
C11 C 0.9798(10) 0.8714(9) 0.8682(10) 0.040(3) Uani 0.585(6) 1 d D . P A 1
H11A H 0.9835 0.8880 0.9178 0.060 Uiso 0.585(6) 1 calc R U P A 1
H11B H 1.0308 0.8849 0.8459 0.060 Uiso 0.585(6) 1 calc R U P A 1
H11C H 0.9688 0.8083 0.8643 0.060 Uiso 0.585(6) 1 calc R U P A 1
C12 C 0.9072(7) 0.8971(9) 0.7563(6) 0.050(3) Uani 0.585(6) 1 d D . P A 1
H12A H 0.8646 0.9313 0.7326 0.076 Uiso 0.585(6) 1 calc R U P A 1
H12B H 0.8948 0.8342 0.7522 0.076 Uiso 0.585(6) 1 calc R U P A 1
H12C H 0.9588 0.9092 0.7345 0.076 Uiso 0.585(6) 1 calc R U P A 1
N3A N 0.8248(7) 0.9232(10) 0.8894(8) 0.028(2) Uani 0.415(6) 1 d D U P A 2
H3NA H 0.8117 0.9234 0.9337 0.033 Uiso 0.415(6) 1 calc R U P A 2
C9A C 0.9054(7) 0.9657(9) 0.8759(8) 0.033(2) Uani 0.415(6) 1 d D . P A 2
C10A C 0.9185(9) 1.0378(11) 0.9299(10) 0.047(3) Uani 0.415(6) 1 d D . P A 2
H10D H 0.9236 1.0116 0.9767 0.071 Uiso 0.415(6) 1 calc R U P A 2
H10E H 0.8725 1.0782 0.9281 0.071 Uiso 0.415(6) 1 calc R U P A 2
H10F H 0.9678 1.0702 0.9196 0.071 Uiso 0.415(6) 1 calc R U P A 2
C11A C 0.9751(14) 0.9035(14) 0.8830(15) 0.040(3) Uani 0.415(6) 1 d D . P A 2
H11D H 0.9750 0.8758 0.9294 0.060 Uiso 0.415(6) 1 calc R U P A 2
H11E H 1.0255 0.9359 0.8776 0.060 Uiso 0.415(6) 1 calc R U P A 2
H11F H 0.9703 0.8580 0.8468 0.060 Uiso 0.415(6) 1 calc R U P A 2
C12A C 0.8984(11) 1.0128(14) 0.8069(10) 0.050(3) Uani 0.415(6) 1 d D . P A 2
H12D H 0.8889 0.9700 0.7693 0.076 Uiso 0.415(6) 1 calc R U P A 2
H12E H 0.9484 1.0449 0.7986 0.076 Uiso 0.415(6) 1 calc R U P A 2
H12F H 0.8534 1.0544 0.8079 0.076 Uiso 0.415(6) 1 calc R U P A 2
C13 C 0.5229(3) 0.7652(4) 0.9955(3) 0.0274(13) Uani 1 1 d . . . . .
C14 C 0.5886(4) 0.7974(5) 1.0341(4) 0.0371(16) Uani 1 1 d . . . . .
C15 C 0.5923(4) 0.7985(5) 1.1060(4) 0.050(2) Uani 1 1 d . . . . .
H15 H 0.6377 0.8223 1.1306 0.060 Uiso 1 1 calc R U . . .
C16 C 0.5279(4) 0.7641(5) 1.1418(4) 0.0464(19) Uani 1 1 d . . . . .
H16 H 0.5298 0.7636 1.1915 0.056 Uiso 1 1 calc R U . . .
C17 C 0.4615(3) 0.7308(4) 1.1066(4) 0.0354(15) Uani 1 1 d . . . . .
H17 H 0.4176 0.7074 1.1314 0.042 Uiso 1 1 calc R U . . .
C18 C 0.4602(3) 0.7322(4) 1.0346(3) 0.0277(13) Uani 1 1 d . . . . .
C19 C 0.4100(4) 0.5257(4) 0.8763(4) 0.0413(18) Uani 1 1 d . . . . .
C20 C 0.5016(3) 0.5362(4) 0.8836(4) 0.0478(19) Uani 1 1 d . . . . .
H20A H 0.5212 0.5701 0.8439 0.072 Uiso 1 1 calc R U . . .
H20B H 0.5270 0.4780 0.8843 0.072 Uiso 1 1 calc R U . . .
H20C H 0.5152 0.5671 0.9274 0.072 Uiso 1 1 calc R U . . .
C21 C 0.3877(4) 0.4808(5) 0.8075(4) 0.054(2) Uani 1 1 d . . . . .
H21A H 0.3291 0.4742 0.8034 0.080 Uiso 1 1 calc R U . . .
H21B H 0.4130 0.4226 0.8061 0.080 Uiso 1 1 calc R U . . .
H21C H 0.4065 0.5165 0.7684 0.080 Uiso 1 1 calc R U . . .
C22 C 0.3781(4) 0.4728(5) 0.9361(5) 0.055(2) Uani 1 1 d . . . . .
H22A H 0.3891 0.5040 0.9802 0.083 Uiso 1 1 calc R U . . .
H22B H 0.4045 0.4152 0.9376 0.083 Uiso 1 1 calc R U . . .
H22C H 0.3199 0.4648 0.9294 0.083 Uiso 1 1 calc R U . . .
C23 C 0.2769(3) 0.8333(4) 0.8798(3) 0.0278(13) Uani 1 1 d . . . . .
C24 C 0.3408(4) 0.9030(4) 0.8975(4) 0.0372(16) Uani 1 1 d . . . . .
H24A H 0.3674 0.8887 0.9425 0.056 Uiso 1 1 calc R U . . .
H24B H 0.3151 0.9608 0.9006 0.056 Uiso 1 1 calc R U . . .
H24C H 0.3808 0.9041 0.8608 0.056 Uiso 1 1 calc R U . . .
C25 C 0.2126(3) 0.8331(5) 0.9340(4) 0.0393(16) Uani 1 1 d . . . . .
H25A H 0.1704 0.7910 0.9202 0.059 Uiso 1 1 calc R U . . .
H25B H 0.1892 0.8921 0.9374 0.059 Uiso 1 1 calc R U . . .
H25C H 0.2363 0.8161 0.9795 0.059 Uiso 1 1 calc R U . . .
C26 C 0.2400(5) 0.8522(5) 0.8088(4) 0.059(2) Uani 1 1 d . . . . .
H26A H 0.2822 0.8537 0.7740 0.088 Uiso 1 1 calc R U . . .
H26B H 0.2126 0.9092 0.8096 0.088 Uiso 1 1 calc R U . . .
H26C H 0.2010 0.8061 0.7963 0.088 Uiso 1 1 calc R U . . .
C27 C 0.1346(3) 0.5683(4) 0.8551(4) 0.0415(18) Uani 1 1 d . . . . .
C28 C 0.1325(5) 0.4761(5) 0.8830(6) 0.084(4) Uani 1 1 d . . . . .
H28A H 0.1806 0.4443 0.8685 0.125 Uiso 1 1 calc R U . . .
H28B H 0.0843 0.4461 0.8645 0.125 Uiso 1 1 calc R U . . .
H28C H 0.1313 0.4776 0.9343 0.125 Uiso 1 1 calc R U . . .
C29 C 0.1328(4) 0.5660(6) 0.7756(4) 0.058(2) Uani 1 1 d . . . . .
H29A H 0.1295 0.6262 0.7573 0.086 Uiso 1 1 calc R U . . .
H29B H 0.0857 0.5325 0.7588 0.086 Uiso 1 1 calc R U . . .
H29C H 0.1819 0.5379 0.7593 0.086 Uiso 1 1 calc R U . . .
C30 C 0.0633(4) 0.6202(6) 0.8815(5) 0.061(2) Uani 1 1 d . . . . .
H30A H 0.0668 0.6238 0.9327 0.092 Uiso 1 1 calc R U . . .
H30B H 0.0132 0.5906 0.8671 0.092 Uiso 1 1 calc R U . . .
H30C H 0.0640 0.6797 0.8617 0.092 Uiso 1 1 calc R U . . .
C31 C 0.6727(9) 0.8701(10) 0.6388(13) 0.042(4) Uani 0.428(3) 1 d D . P B 1
H31 H 0.6622 0.8644 0.6900 0.050 Uiso 0.428(3) 1 calc R U P B 1
Cl1 Cl 0.6063(6) 0.9477(6) 0.6021(8) 0.0572(15) Uani 0.428(3) 1 d D . P B 1
Cl2 Cl 0.7718(3) 0.9063(4) 0.6286(3) 0.0601(9) Uani 0.428(3) 1 d D . P B 1
Cl3 Cl 0.6592(4) 0.7670(4) 0.5986(4) 0.0668(10) Uani 0.428(3) 1 d D . P B 1
C31A C 0.6551(7) 0.8405(7) 0.6287(9) 0.042(4) Uani 0.572(3) 1 d D . P B 2
H31A H 0.6598 0.8426 0.6809 0.050 Uiso 0.572(3) 1 calc R U P B 2
Cl1A Cl 0.5843(4) 0.9183(4) 0.6008(5) 0.0572(15) Uani 0.572(3) 1 d D . P B 2
Cl2A Cl 0.7492(2) 0.8642(3) 0.5945(2) 0.0601(9) Uani 0.572(3) 1 d D . P B 2
Cl3A Cl 0.6255(3) 0.7340(3) 0.6033(3) 0.0668(10) Uani 0.572(3) 1 d D . P B 2
C32 C 0.3590(7) 0.6988(9) 0.6270(7) 0.037(3) Uani 0.5 1 d . . P C 1
H32 H 0.3873 0.7008 0.6738 0.045 Uiso 0.5 1 calc R U P C 1
Cl4 Cl 0.4218(6) 0.7334(10) 0.5636(8) 0.053(2) Uani 0.5 1 d . . P C 1
Cl5 Cl 0.27356(19) 0.7664(2) 0.6272(2) 0.0456(8) Uani 0.5 1 d . . P C 1
Cl6 Cl 0.3294(2) 0.5888(2) 0.6067(2) 0.0575(11) Uani 0.5 1 d . . P C 1
C33 C 0.3361(7) 0.6577(9) 0.5783(7) 0.037(3) Uani 0.5 1 d . . P D 2
H33 H 0.2849 0.6708 0.5517 0.044 Uiso 0.5 1 calc R U P D 2
Cl7 Cl 0.3155(2) 0.6487(3) 0.66664(19) 0.0487(9) Uani 0.5 1 d . . P D 2
Cl8 Cl 0.3763(2) 0.5566(2) 0.5473(2) 0.0530(10) Uani 0.5 1 d . . P D 2
Cl9 Cl 0.4069(8) 0.7452(11) 0.5635(9) 0.088(4) Uani 0.5 1 d . . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C13 1.868(6) . ?
Ni1 P3 2.1621(15) . ?
Ni1 P1 2.1668(16) . ?
Ni1 I1 2.5027(9) . ?
P1 N2 1.648(6) . ?
P1 O1 1.650(5) . ?
P1 N1 1.664(5) . ?
P2 N3 1.603(9) . ?
P2 N1 1.737(6) . ?
P2 N2 1.744(6) . ?
P2 N3A 1.775(13) . ?
P3 N4 1.648(5) . ?
P3 O2 1.653(5) . ?
P3 N5 1.655(5) . ?
P4 N6 1.652(6) . ?
P4 N5 1.738(5) . ?
P4 N4 1.744(5) . ?
O1 C14 1.398(7) . ?
O2 C18 1.396(7) . ?
N1 C1 1.483(10) . ?
N2 C5 1.482(10) . ?
N4 C19 1.484(7) . ?
N5 C23 1.473(7) . ?
N6 C27 1.476(7) . ?
N6 H6N 0.8800 . ?
C1 C2 1.519(10) . ?
C1 C4 1.529(8) . ?
C1 C3 1.531(11) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.517(10) . ?
C5 C8 1.532(9) . ?
C5 C7 1.538(9) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N3 C9 1.484(11) . ?
N3 H3N 0.8800 . ?
C9 C12 1.502(13) . ?
C9 C11 1.510(14) . ?
C9 C10 1.520(13) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N3A C9A 1.516(15) . ?
N3A H3NA 0.8800 . ?
C9A C11A 1.499(16) . ?
C9A C12A 1.501(15) . ?
C9A C10A 1.517(16) . ?
C10A H10D 0.9800 . ?
C10A H10E 0.9800 . ?
C10A H10F 0.9800 . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C13 C14 1.391(8) . ?
C13 C18 1.392(8) . ?
C14 C15 1.371(9) . ?
C15 C16 1.387(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.376(9) . ?
C17 H17 0.9500 . ?
C19 C22 1.504(11) . ?
C19 C21 1.518(10) . ?
C19 C20 1.534(8) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C26 1.502(9) . ?
C23 C25 1.507(8) . ?
C23 C24 1.532(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.501(10) . ?
C27 C29 1.518(11) . ?
C27 C30 1.521(10) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 Cl1 1.749(15) . ?
C31 Cl2 1.753(15) . ?
C31 Cl3 1.757(14) . ?
C31 H31 1.0000 . ?
C31A Cl1A 1.741(12) . ?
C31A Cl2A 1.748(13) . ?
C31A Cl3A 1.757(11) . ?
C31A H31A 1.0000 . ?
C32 Cl4 1.703(19) . ?
C32 Cl5 1.753(13) . ?
C32 Cl6 1.784(14) . ?
C32 H32 1.0000 . ?
C33 Cl7 1.734(14) . ?
C33 Cl8 1.785(14) . ?
C33 Cl9 1.80(2) . ?
C33 H33 1.0000 . ?

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
C13 Ni1 P3 83.21(17) . . ?
C13 Ni1 P1 83.19(16) . . ?
P3 Ni1 P1 166.27(8) . . ?
C13 Ni1 I1 176.91(17) . . ?
P3 Ni1 I1 95.36(5) . . ?
P1 Ni1 I1 98.31(5) . . ?
N2 P1 O1 106.6(3) . . ?
N2 P1 N1 84.4(3) . . ?
O1 P1 N1 106.0(3) . . ?
N2 P1 Ni1 126.7(2) . . ?
O1 P1 Ni1 104.53(15) . . ?
N1 P1 Ni1 126.0(2) . . ?
N3 P2 N1 103.7(4) . . ?
N3 P2 N2 113.4(4) . . ?
N1 P2 N2 79.4(3) . . ?
N1 P2 N3A 103.5(5) . . ?
N2 P2 N3A 93.8(5) . . ?
N4 P3 O2 107.2(3) . . ?
N4 P3 N5 84.4(2) . . ?
O2 P3 N5 107.6(2) . . ?
N4 P3 Ni1 124.8(2) . . ?
O2 P3 Ni1 104.73(14) . . ?
N5 P3 Ni1 125.99(19) . . ?
N6 P4 N5 105.0(3) . . ?
N6 P4 N4 106.2(3) . . ?
N5 P4 N4 79.1(2) . . ?
C14 O1 P1 113.2(4) . . ?
C18 O2 P3 112.9(4) . . ?
C1 N1 P1 130.4(4) . . ?
C1 N1 P2 128.7(4) . . ?
P1 N1 P2 97.4(3) . . ?
C5 N2 P1 131.1(4) . . ?
C5 N2 P2 129.3(4) . . ?
P1 N2 P2 97.7(3) . . ?
C19 N4 P3 132.3(4) . . ?
C19 N4 P4 129.6(4) . . ?
P3 N4 P4 98.1(3) . . ?
C23 N5 P3 132.3(4) . . ?
C23 N5 P4 129.3(4) . . ?
P3 N5 P4 98.0(2) . . ?
C27 N6 P4 128.6(5) . . ?
C27 N6 H6N 119.3 . . ?
P4 N6 H6N 111.9 . . ?
N1 C1 C2 111.6(6) . . ?
N1 C1 C4 108.4(6) . . ?
C2 C1 C4 109.8(6) . . ?
N1 C1 C3 108.3(6) . . ?
C2 C1 C3 109.5(7) . . ?
C4 C1 C3 109.2(6) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 111.2(6) . . ?
N2 C5 C8 108.4(6) . . ?
C6 C5 C8 110.2(6) . . ?
N2 C5 C7 108.3(6) . . ?
C6 C5 C7 109.7(6) . . ?
C8 C5 C7 108.9(6) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 N3 P2 127.8(8) . . ?
C9 N3 H3N 116.1 . . ?
P2 N3 H3N 116.1 . . ?
N3 C9 C12 110.6(8) . . ?
N3 C9 C11 106.5(11) . . ?
C12 C9 C11 109.4(10) . . ?
N3 C9 C10 107.6(9) . . ?
C12 C9 C10 111.1(11) . . ?
C11 C9 C10 111.5(10) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9A N3A P2 132.2(11) . . ?
C9A N3A H3NA 113.9 . . ?
P2 N3A H3NA 113.9 . . ?
C11A C9A C12A 115.1(17) . . ?
C11A C9A N3A 113.6(15) . . ?
C12A C9A N3A 107.7(12) . . ?
C11A C9A C10A 107.3(13) . . ?
C12A C9A C10A 104.9(15) . . ?
N3A C9A C10A 107.7(11) . . ?
C9A C10A H10D 109.5 . . ?
C9A C10A H10E 109.5 . . ?
H10D C10A H10E 109.5 . . ?
C9A C10A H10F 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?
C9A C11A H11D 109.5 . . ?
C9A C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
C9A C11A H11F 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C9A C12A H12D 109.5 . . ?
C9A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C9A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C14 C13 C18 115.5(6) . . ?
C14 C13 Ni1 122.2(4) . . ?
C18 C13 Ni1 122.2(4) . . ?
C15 C14 C13 123.2(5) . . ?
C15 C14 O1 120.0(5) . . ?
C13 C14 O1 116.8(6) . . ?
C14 C15 C16 118.3(6) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
C17 C16 C15 121.3(6) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 118.2(5) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
C17 C18 C13 123.4(5) . . ?
C17 C18 O2 119.7(5) . . ?
C13 C18 O2 116.9(5) . . ?
N4 C19 C22 109.1(6) . . ?
N4 C19 C21 108.5(6) . . ?
C22 C19 C21 109.5(6) . . ?
N4 C19 C20 108.7(5) . . ?
C22 C19 C20 110.8(6) . . ?
C21 C19 C20 110.2(6) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N5 C23 C26 109.3(5) . . ?
N5 C23 C25 108.2(5) . . ?
C26 C23 C25 109.8(6) . . ?
N5 C23 C24 109.6(5) . . ?
C26 C23 C24 109.3(6) . . ?
C25 C23 C24 110.5(5) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C27 C28 108.8(5) . . ?
N6 C27 C29 109.7(6) . . ?
C28 C27 C29 109.5(7) . . ?
N6 C27 C30 108.6(6) . . ?
C28 C27 C30 109.9(7) . . ?
C29 C27 C30 110.4(6) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Cl1 C31 Cl2 109.1(11) . . ?
Cl1 C31 Cl3 110.8(11) . . ?
Cl2 C31 Cl3 109.9(10) . . ?
Cl1 C31 H31 109.0 . . ?
Cl2 C31 H31 109.0 . . ?
Cl3 C31 H31 109.0 . . ?
Cl1A C31A Cl2A 110.5(9) . . ?
Cl1A C31A Cl3A 111.1(8) . . ?
Cl2A C31A Cl3A 109.5(7) . . ?
Cl1A C31A H31A 108.6 . . ?
Cl2A C31A H31A 108.6 . . ?
Cl3A C31A H31A 108.6 . . ?
Cl4 C32 Cl5 109.4(9) . . ?
Cl4 C32 Cl6 107.8(9) . . ?
Cl5 C32 Cl6 109.4(7) . . ?
Cl4 C32 H32 110.1 . . ?
Cl5 C32 H32 110.1 . . ?
Cl6 C32 H32 110.1 . . ?
Cl7 C33 Cl8 109.8(7) . . ?
Cl7 C33 Cl9 111.0(9) . . ?
Cl8 C33 Cl9 109.3(8) . . ?
Cl7 C33 H33 108.9 . . ?
Cl8 C33 H33 108.9 . . ?
Cl9 C33 H33 108.9 . . ?

_refine_diff_density_max         1.038
_refine_diff_density_min         -1.560
_refine_diff_density_rms         0.131

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_msb490_0m_sq
_database_code_depnum_ccdc_archive 'CCDC 1023324'
_audit_update_record             
;
2014-09-08 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H118 Cu4 I6 N12 O4 P8 Pd2'
_chemical_formula_sum            'C60 H118 Cu4 I6 N12 O4 P8 Pd2'
_chemical_formula_weight         2547.78

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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   15.390(4)
_cell_length_b                   19.203(5)
_cell_length_c                   18.045(5)
_cell_angle_alpha                90
_cell_angle_beta                 111.990(4)
_cell_angle_gamma                90
_cell_volume                     4945(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9110
_cell_measurement_theta_min      2.4382
_cell_measurement_theta_max      28.1988

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_F_000             2480
_exptl_transmission_factor_min   0.608
_exptl_transmission_factor_max   0.862
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.086
_exptl_absorpt_coefficient_mu    3.245
_shelx_estimated_absorpt_T_min   0.572
_shelx_estimated_absorpt_T_max   0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_T_max  0.77

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, collected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 30 sec/frame.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3660
_diffrn_reflns_number            84469
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.828
_diffrn_reflns_theta_max         28.211
_diffrn_reflns_theta_full        28.200
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             12130
_reflns_number_gt                10365
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2009)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. H-atoms attached to carbon
 were placed in calculated positions (C---H = 0.95 - 0.98 Å) while those
 attached to nitrogen were placed in locations derived from a difference
 map. All were included as riding contributions with isotropic displacement
 parameters 1.2 - 1.5 times those of the attached atoms. The Cu1 atom and
 all three iodine atoms are disordered over two distinct sites in an 84:16
 ratio. Additionally, one of the t-butyl groups is rotationally disordered
 over two sites in a similar ratio. Both disordered entities were refined
 subject to restraints that the geometries of the two components of each
 disorder were approximately the same. The density associated with an
 additional site which appeared to be partially occupied by disordered
 solvent dichloromethane was removed with the SQUEEZE option of the PLATON
 package (Spek, 2014) following unsuccessful attempts to model the contents.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0301P)²+27.7243P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_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         12130
_refine_ls_number_parameters     471
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1031
_refine_ls_wR_factor_gt          0.0969
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.002
_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
Pd1 Pd 0.76464(2) 0.87451(2) 0.48757(2) 0.01804(7) Uani 1 1 d . . . . .
I1 I 0.62275(2) 0.91469(2) 0.52896(2) 0.02704(9) Uani 0.8357(5) 1 d . . P A 1
I2 I 0.64921(3) 0.97092(2) 0.77007(3) 0.04176(12) Uani 0.8357(5) 1 d . . P A 1
I3 I 0.47286(3) 0.80251(2) 0.67185(3) 0.03926(12) Uani 0.8357(5) 1 d . . P A 1
Cu1 Cu 0.63651(5) 0.85757(4) 0.68354(5) 0.03742(19) Uani 0.8357(5) 1 d . . P A
1
I1A I 0.61435(12) 0.94631(11) 0.49790(12) 0.02704(9) Uani 0.1643(5) 1 d . . P A
2
I2A I 0.65358(13) 0.94834(12) 0.82101(17) 0.04176(12) Uani 0.1643(5) 1 d . . P
A 2
I3A I 0.47123(19) 0.78710(14) 0.70339(19) 0.03926(12) Uani 0.1643(5) 1 d . . P
A 2
Cu1A Cu 0.6368(2) 0.8365(2) 0.7366(3) 0.03742(19) Uani 0.1643(5) 1 d . . P A 2
Cu2 Cu 0.47990(4) 0.92734(3) 0.72263(4) 0.02809(12) Uani 1 1 d . . . . .
P1 P 0.75687(7) 0.78604(6) 0.70429(7) 0.0249(2) Uani 1 1 d . . . . .
P2 P 0.82118(8) 0.80472(6) 0.59579(7) 0.0240(2) Uani 1 1 d . . . . .
P3 P 0.74606(7) 0.92851(5) 0.36946(6) 0.01742(19) Uani 1 1 d . . . . .
P4 P 0.64137(7) 1.01669(5) 0.27068(6) 0.01799(19) Uani 1 1 d . . . . .
O1 O 0.9129(2) 0.76541(16) 0.58860(19) 0.0282(7) Uani 1 1 d . . . . .
O2 O 0.83359(19) 0.89767(15) 0.34679(18) 0.0224(6) Uani 1 1 d . . . . .
N1 N 0.8496(3) 0.82977(19) 0.6906(2) 0.0273(8) Uani 1 1 d . . . . .
N2 N 0.7525(3) 0.74709(19) 0.6163(2) 0.0267(8) Uani 1 1 d . . . . .
N3 N 0.8028(3) 0.7269(2) 0.7743(2) 0.0312(9) Uani 1 1 d . . . . .
H3N H 0.8524 0.7059 0.7716 0.037 Uiso 1 1 d R U . . .
N4 N 0.6526(2) 0.92762(17) 0.2842(2) 0.0191(6) Uani 1 1 d . . . . .
N5 N 0.7443(2) 1.01420(17) 0.3537(2) 0.0199(7) Uani 1 1 d . . . . .
N6 N 0.6706(3) 1.03318(18) 0.1937(2) 0.0249(7) Uani 1 1 d . . . . .
H6N H 0.7249 1.0071 0.1963 0.030 Uiso 1 1 d R U . . .
C1 C 0.9088(3) 0.8900(2) 0.7333(3) 0.0315(10) Uani 1 1 d . . . . .
C2 C 1.0066(4) 0.8797(3) 0.7317(4) 0.0426(12) Uani 1 1 d . . . . .
H2A H 1.0321 0.8351 0.7567 0.064 Uiso 1 1 calc R U . . .
H2B H 1.0476 0.9176 0.7613 0.064 Uiso 1 1 calc R U . . .
H2C H 1.0026 0.8799 0.6763 0.064 Uiso 1 1 calc R U . . .
C3 C 0.8684(4) 0.9588(3) 0.6934(4) 0.0497(15) Uani 1 1 d . . . . .
H3A H 0.8597 0.9569 0.6368 0.075 Uiso 1 1 calc R U . . .
H3B H 0.9116 0.9967 0.7196 0.075 Uiso 1 1 calc R U . . .
H3C H 0.8078 0.9670 0.6981 0.075 Uiso 1 1 calc R U . . .
C4 C 0.9150(4) 0.8883(3) 0.8200(3) 0.0398(12) Uani 1 1 d . . . . .
H4A H 0.8525 0.8958 0.8213 0.060 Uiso 1 1 calc R U . . .
H4B H 0.9574 0.9251 0.8506 0.060 Uiso 1 1 calc R U . . .
H4C H 0.9390 0.8429 0.8437 0.060 Uiso 1 1 calc R U . . .
C5 C 0.6888(3) 0.6931(2) 0.5644(3) 0.0335(10) Uani 1 1 d D . . . .
C6 C 0.5924(4) 0.6973(3) 0.5658(4) 0.0412(15) Uani 0.812(6) 1 d D . P B 1
H6A H 0.5961 0.6933 0.6211 0.062 Uiso 0.812(6) 1 calc R U P B 1
H6B H 0.5540 0.6593 0.5339 0.062 Uiso 0.812(6) 1 calc R U P B 1
H6C H 0.5640 0.7420 0.5435 0.062 Uiso 0.812(6) 1 calc R U P B 1
C7 C 0.7327(5) 0.6209(3) 0.5948(4) 0.0425(15) Uani 0.812(6) 1 d D . P B 1
H7A H 0.7959 0.6189 0.5937 0.064 Uiso 0.812(6) 1 calc R U P B 1
H7B H 0.6938 0.5844 0.5602 0.064 Uiso 0.812(6) 1 calc R U P B 1
H7C H 0.7363 0.6138 0.6496 0.064 Uiso 0.812(6) 1 calc R U P B 1
C8 C 0.6838(5) 0.7000(3) 0.4773(4) 0.0406(15) Uani 0.812(6) 1 d D . P B 1
H8A H 0.7473 0.6981 0.4769 0.061 Uiso 0.812(6) 1 calc R U P B 1
H8B H 0.6547 0.7445 0.4549 0.061 Uiso 0.812(6) 1 calc R U P B 1
H8C H 0.6464 0.6617 0.4451 0.061 Uiso 0.812(6) 1 calc R U P B 1
C6A C 0.6522(16) 0.6505(11) 0.6193(13) 0.0412(15) Uani 0.188(6) 1 d D . P B 2
H6A1 H 0.6288 0.6823 0.6501 0.062 Uiso 0.188(6) 1 calc R U P B 2
H6A2 H 0.7033 0.6223 0.6560 0.062 Uiso 0.188(6) 1 calc R U P B 2
H6A3 H 0.6013 0.6199 0.5867 0.062 Uiso 0.188(6) 1 calc R U P B 2
C7A C 0.6051(14) 0.7314(12) 0.5041(13) 0.0425(15) Uani 0.188(6) 1 d D . P B 2
H7A1 H 0.5800 0.7645 0.5323 0.064 Uiso 0.188(6) 1 calc R U P B 2
H7A2 H 0.5564 0.6977 0.4752 0.064 Uiso 0.188(6) 1 calc R U P B 2
H7A3 H 0.6252 0.7567 0.4660 0.064 Uiso 0.188(6) 1 calc R U P B 2
C8A C 0.7384(16) 0.6485(11) 0.5261(14) 0.0406(15) Uani 0.188(6) 1 d D . P B 2
H8A1 H 0.7610 0.6771 0.4921 0.061 Uiso 0.188(6) 1 calc R U P B 2
H8A2 H 0.6953 0.6129 0.4934 0.061 Uiso 0.188(6) 1 calc R U P B 2
H8A3 H 0.7917 0.6258 0.5674 0.061 Uiso 0.188(6) 1 calc R U P B 2
C9 C 0.7767(4) 0.7044(3) 0.8425(3) 0.0424(13) Uani 1 1 d . . . . .
C10 C 0.6890(5) 0.6587(4) 0.8117(4) 0.0570(17) Uani 1 1 d . . . . .
H10A H 0.6364 0.6858 0.7751 0.086 Uiso 1 1 calc R U . . .
H10B H 0.6736 0.6425 0.8569 0.086 Uiso 1 1 calc R U . . .
H10C H 0.7007 0.6184 0.7833 0.086 Uiso 1 1 calc R U . . .
C11 C 0.8591(5) 0.6627(6) 0.8976(5) 0.087(3) Uani 1 1 d . . . . .
H11A H 0.8699 0.6226 0.8685 0.131 Uiso 1 1 calc R U . . .
H11B H 0.8456 0.6463 0.9436 0.131 Uiso 1 1 calc R U . . .
H11C H 0.9151 0.6921 0.9162 0.131 Uiso 1 1 calc R U . . .
C12 C 0.7595(6) 0.7666(5) 0.8857(5) 0.077(3) Uani 1 1 d . . . . .
H12A H 0.8146 0.7971 0.9022 0.116 Uiso 1 1 calc R U . . .
H12B H 0.7481 0.7511 0.9330 0.116 Uiso 1 1 calc R U . . .
H12C H 0.7048 0.7922 0.8500 0.116 Uiso 1 1 calc R U . . .
C13 C 0.8731(3) 0.8329(2) 0.4687(2) 0.0201(8) Uani 1 1 d . . . . .
C14 C 0.9315(3) 0.7849(2) 0.5211(3) 0.0234(8) Uani 1 1 d . . . . .
C15 C 1.0082(3) 0.7558(2) 0.5090(3) 0.0281(9) Uani 1 1 d . . . . .
H15 H 1.0485 0.7240 0.5464 0.034 Uiso 1 1 calc R U . . .
C16 C 1.0241(3) 0.7747(2) 0.4409(3) 0.0276(9) Uani 1 1 d . . . . .
H16 H 1.0757 0.7548 0.4316 0.033 Uiso 1 1 calc R U . . .
C17 C 0.9666(3) 0.8218(2) 0.3858(3) 0.0260(9) Uani 1 1 d . . . . .
H17 H 0.9779 0.8342 0.3392 0.031 Uiso 1 1 calc R U . . .
C18 C 0.8912(3) 0.8506(2) 0.4010(2) 0.0207(8) Uani 1 1 d . . . . .
C19 C 0.5890(3) 0.8691(2) 0.2437(3) 0.0215(8) Uani 1 1 d . . . . .
C20 C 0.5255(3) 0.8505(3) 0.2893(3) 0.0347(11) Uani 1 1 d . . . . .
H20A H 0.5643 0.8380 0.3445 0.052 Uiso 1 1 calc R U . . .
H20B H 0.4854 0.8109 0.2631 0.052 Uiso 1 1 calc R U . . .
H20C H 0.4862 0.8906 0.2893 0.052 Uiso 1 1 calc R U . . .
C21 C 0.6488(3) 0.8061(2) 0.2421(3) 0.0318(10) Uani 1 1 d . . . . .
H21A H 0.6898 0.8182 0.2136 0.048 Uiso 1 1 calc R U . . .
H21B H 0.6079 0.7674 0.2148 0.048 Uiso 1 1 calc R U . . .
H21C H 0.6870 0.7924 0.2970 0.048 Uiso 1 1 calc R U . . .
C22 C 0.5291(3) 0.8918(2) 0.1592(3) 0.0271(9) Uani 1 1 d . . . . .
H22A H 0.4913 0.9323 0.1614 0.041 Uiso 1 1 calc R U . . .
H22B H 0.4877 0.8535 0.1313 0.041 Uiso 1 1 calc R U . . .
H22C H 0.5697 0.9044 0.1304 0.041 Uiso 1 1 calc R U . . .
C23 C 0.8007(3) 1.0700(2) 0.4074(3) 0.0234(8) Uani 1 1 d . . . . .
C24 C 0.9004(3) 1.0443(3) 0.4458(3) 0.0351(11) Uani 1 1 d . . . . .
H24A H 0.9024 1.0041 0.4799 0.053 Uiso 1 1 calc R U . . .
H24B H 0.9400 1.0815 0.4783 0.053 Uiso 1 1 calc R U . . .
H24C H 0.9235 1.0305 0.4042 0.053 Uiso 1 1 calc R U . . .
C25 C 0.7596(4) 1.0873(3) 0.4703(3) 0.0387(11) Uani 1 1 d . . . . .
H25A H 0.6946 1.1027 0.4438 0.058 Uiso 1 1 calc R U . . .
H25B H 0.7965 1.1246 0.5051 0.058 Uiso 1 1 calc R U . . .
H25C H 0.7615 1.0458 0.5024 0.058 Uiso 1 1 calc R U . . .
C26 C 0.7968(3) 1.1343(2) 0.3566(3) 0.0325(10) Uani 1 1 d . . . . .
H26A H 0.8215 1.1228 0.3153 0.049 Uiso 1 1 calc R U . . .
H26B H 0.8347 1.1715 0.3907 0.049 Uiso 1 1 calc R U . . .
H26C H 0.7317 1.1500 0.3312 0.049 Uiso 1 1 calc R U . . .
C27 C 0.6294(4) 1.0821(3) 0.1252(3) 0.0347(11) Uani 1 1 d . . . . .
C28 C 0.5235(4) 1.0877(3) 0.1005(4) 0.0540(18) Uani 1 1 d . . . . .
H28A H 0.4957 1.0411 0.0894 0.081 Uiso 1 1 calc R U . . .
H28B H 0.4976 1.1165 0.0524 0.081 Uiso 1 1 calc R U . . .
H28C H 0.5091 1.1090 0.1440 0.081 Uiso 1 1 calc R U . . .
C29 C 0.6736(4) 1.1544(3) 0.1481(3) 0.0370(11) Uani 1 1 d . . . . .
H29A H 0.6592 1.1727 0.1929 0.056 Uiso 1 1 calc R U . . .
H29B H 0.6481 1.1858 0.1022 0.056 Uiso 1 1 calc R U . . .
H29C H 0.7417 1.1508 0.1639 0.056 Uiso 1 1 calc R U . . .
C30 C 0.6533(6) 1.0525(3) 0.0564(3) 0.065(2) Uani 1 1 d . . . . .
H30A H 0.7215 1.0497 0.0727 0.097 Uiso 1 1 calc R U . . .
H30B H 0.6275 1.0829 0.0097 0.097 Uiso 1 1 calc R U . . .
H30C H 0.6261 1.0058 0.0429 0.097 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
Pd1 C13 1.991(4) . ?
Pd1 P2 2.2570(12) . ?
Pd1 P3 2.2898(12) . ?
Pd1 I1 2.6726(7) . ?
Pd1 I1A 2.7583(18) . ?
I1 Cu1 2.9302(13) . ?
I2 Cu2 2.5596(9) . ?
I2 Cu1 2.6429(10) . ?
I3 Cu2 2.5540(9) . ?
I3 Cu1 2.6658(11) . ?
Cu1 P1 2.2223(13) . ?
I2A Cu1A 2.590(4) . ?
I2A Cu2 2.628(2) . ?
I3A Cu1A 2.571(5) . ?
I3A Cu2 2.712(3) . ?
Cu1A P1 2.344(4) . ?
Cu1A Cu2 2.913(4) . ?
Cu2 P4 2.1959(12) 3_676 ?
P1 N3 1.648(4) . ?
P1 N2 1.732(4) . ?
P1 N1 1.751(4) . ?
P2 O1 1.648(3) . ?
P2 N2 1.666(4) . ?
P2 N1 1.671(4) . ?
P3 O2 1.657(3) . ?
P3 N4 1.667(3) . ?
P3 N5 1.668(3) . ?
P4 N6 1.644(4) . ?
P4 N5 1.726(3) . ?
P4 N4 1.727(3) . ?
P4 Cu2 2.1959(12) 3_676 ?
O1 C14 1.403(5) . ?
O2 C18 1.382(5) . ?
N1 C1 1.495(6) . ?
N2 C5 1.491(6) . ?
N3 C9 1.495(6) . ?
N3 H3N 0.8809 . ?
N4 C19 1.490(5) . ?
N5 C23 1.486(5) . ?
N6 C27 1.492(6) . ?
N6 H6N 0.9589 . ?
C1 C3 1.520(7) . ?
C1 C2 1.529(7) . ?
C1 C4 1.532(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C8A 1.480(12) . ?
C5 C6 1.495(7) . ?
C5 C7A 1.528(13) . ?
C5 C6A 1.545(13) . ?
C5 C8 1.550(7) . ?
C5 C7 1.550(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C6A H6A3 0.9800 . ?
C7A H7A1 0.9800 . ?
C7A H7A2 0.9800 . ?
C7A H7A3 0.9800 . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9 C12 1.503(10) . ?
C9 C11 1.514(8) . ?
C9 C10 1.529(8) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.384(6) . ?
C13 C18 1.393(6) . ?
C14 C15 1.395(6) . ?
C15 C16 1.388(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.390(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.402(6) . ?
C17 H17 0.9500 . ?
C19 C22 1.521(6) . ?
C19 C21 1.526(6) . ?
C19 C20 1.539(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.510(6) . ?
C23 C26 1.525(6) . ?
C23 C25 1.530(7) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.525(8) . ?
C27 C30 1.529(8) . ?
C27 C29 1.532(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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
C13 Pd1 P2 80.41(12) . . ?
C13 Pd1 P3 80.97(12) . . ?
P2 Pd1 P3 161.36(4) . . ?
C13 Pd1 I1 171.28(12) . . ?
P2 Pd1 I1 91.16(4) . . ?
P3 Pd1 I1 107.40(3) . . ?
C13 Pd1 I1A 171.80(13) . . ?
P2 Pd1 I1A 107.44(6) . . ?
P3 Pd1 I1A 91.20(5) . . ?
Pd1 I1 Cu1 112.49(2) . . ?
Cu2 I2 Cu1 72.08(2) . . ?
Cu2 I3 Cu1 71.79(2) . . ?
P1 Cu1 I2 122.47(4) . . ?
P1 Cu1 I3 118.12(5) . . ?
I2 Cu1 I3 103.42(3) . . ?
P1 Cu1 I1 98.65(4) . . ?
I2 Cu1 I1 102.54(4) . . ?
I3 Cu1 I1 110.10(3) . . ?
Cu1A I2A Cu2 67.87(10) . . ?
Cu1A I3A Cu2 66.87(11) . . ?
P1 Cu1A I3A 126.48(17) . . ?
P1 Cu1A I2A 125.07(16) . . ?
I3A Cu1A I2A 108.33(15) . . ?
P1 Cu1A Cu2 158.6(2) . . ?
I3A Cu1A Cu2 58.89(9) . . ?
I2A Cu1A Cu2 56.68(9) . . ?
P4 Cu2 I3 123.80(4) 3_676 . ?
P4 Cu2 I2 126.97(4) 3_676 . ?
I3 Cu2 I2 109.14(2) . . ?
P4 Cu2 I2A 123.93(6) 3_676 . ?
P4 Cu2 I3A 119.40(7) 3_676 . ?
I2A Cu2 I3A 103.16(8) . . ?
P4 Cu2 Cu1A 169.31(11) 3_676 . ?
I2A Cu2 Cu1A 55.45(9) . . ?
I3A Cu2 Cu1A 54.25(10) . . ?
N3 P1 N2 105.2(2) . . ?
N3 P1 N1 107.48(19) . . ?
N2 P1 N1 80.36(18) . . ?
N3 P1 Cu1 130.26(15) . . ?
N2 P1 Cu1 111.61(14) . . ?
N1 P1 Cu1 110.59(14) . . ?
N3 P1 Cu1A 104.22(19) . . ?
N2 P1 Cu1A 129.93(17) . . ?
N1 P1 Cu1A 126.62(17) . . ?
O1 P2 N2 110.32(18) . . ?
O1 P2 N1 108.01(18) . . ?
N2 P2 N1 84.69(19) . . ?
O1 P2 Pd1 105.54(12) . . ?
N2 P2 Pd1 121.06(14) . . ?
N1 P2 Pd1 125.70(14) . . ?
O2 P3 N4 105.62(17) . . ?
O2 P3 N5 105.84(17) . . ?
N4 P3 N5 84.24(16) . . ?
O2 P3 Pd1 103.78(11) . . ?
N4 P3 Pd1 128.15(13) . . ?
N5 P3 Pd1 126.43(13) . . ?
N6 P4 N5 106.61(18) . . ?
N6 P4 N4 105.44(18) . . ?
N5 P4 N4 80.74(16) . . ?
N6 P4 Cu2 117.37(14) . 3_676 ?
N5 P4 Cu2 119.26(13) . 3_676 ?
N4 P4 Cu2 121.24(12) . 3_676 ?
C14 O1 P2 113.9(3) . . ?
C18 O2 P3 115.1(3) . . ?
C1 N1 P2 128.7(3) . . ?
C1 N1 P1 132.1(3) . . ?
P2 N1 P1 95.26(19) . . ?
C5 N2 P2 130.1(3) . . ?
C5 N2 P1 131.8(3) . . ?
P2 N2 P1 96.14(19) . . ?
C9 N3 P1 131.3(3) . . ?
C9 N3 H3N 114.7 . . ?
P1 N3 H3N 113.9 . . ?
C19 N4 P3 130.0(3) . . ?
C19 N4 P4 131.7(3) . . ?
P3 N4 P4 97.27(17) . . ?
C23 N5 P3 129.2(3) . . ?
C23 N5 P4 131.9(3) . . ?
P3 N5 P4 97.25(17) . . ?
C27 N6 P4 131.0(3) . . ?
C27 N6 H6N 117.5 . . ?
P4 N6 H6N 111.5 . . ?
N1 C1 C3 111.5(4) . . ?
N1 C1 C2 107.7(4) . . ?
C3 C1 C2 109.5(5) . . ?
N1 C1 C4 107.6(4) . . ?
C3 C1 C4 111.1(5) . . ?
C2 C1 C4 109.3(4) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C8A C5 N2 111.3(11) . . ?
N2 C5 C6 112.0(4) . . ?
C8A C5 C7A 113.0(10) . . ?
N2 C5 C7A 107.1(11) . . ?
C8A C5 C6A 111.6(10) . . ?
N2 C5 C6A 106.0(10) . . ?
C7A C5 C6A 107.4(10) . . ?
N2 C5 C8 110.5(4) . . ?
C6 C5 C8 109.9(5) . . ?
N2 C5 C7 107.6(4) . . ?
C6 C5 C7 110.2(5) . . ?
C8 C5 C7 106.5(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C6A H6A1 109.5 . . ?
C5 C6A H6A2 109.5 . . ?
H6A1 C6A H6A2 109.5 . . ?
C5 C6A H6A3 109.5 . . ?
H6A1 C6A H6A3 109.5 . . ?
H6A2 C6A H6A3 109.5 . . ?
C5 C7A H7A1 109.5 . . ?
C5 C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
C5 C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
C5 C8A H8A1 109.5 . . ?
C5 C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C5 C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
N3 C9 C12 110.5(5) . . ?
N3 C9 C11 106.0(4) . . ?
C12 C9 C11 110.3(7) . . ?
N3 C9 C10 109.8(5) . . ?
C12 C9 C10 110.1(5) . . ?
C11 C9 C10 110.1(6) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 118.0(4) . . ?
C14 C13 Pd1 121.5(3) . . ?
C18 C13 Pd1 120.5(3) . . ?
C13 C14 C15 122.1(4) . . ?
C13 C14 O1 118.6(4) . . ?
C15 C14 O1 119.3(4) . . ?
C16 C15 C14 118.3(4) . . ?
C16 C15 H15 120.8 . . ?
C14 C15 H15 120.8 . . ?
C15 C16 C17 121.8(4) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C16 C17 C18 118.0(4) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 H17 121.0 . . ?
O2 C18 C13 119.6(3) . . ?
O2 C18 C17 118.5(4) . . ?
C13 C18 C17 121.8(4) . . ?
N4 C19 C22 108.5(3) . . ?
N4 C19 C21 108.5(3) . . ?
C22 C19 C21 110.7(4) . . ?
N4 C19 C20 110.1(3) . . ?
C22 C19 C20 109.6(4) . . ?
C21 C19 C20 109.5(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N5 C23 C24 108.0(3) . . ?
N5 C23 C26 108.1(3) . . ?
C24 C23 C26 110.3(4) . . ?
N5 C23 C25 109.7(4) . . ?
C24 C23 C25 111.2(4) . . ?
C26 C23 C25 109.6(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C27 C28 111.2(4) . . ?
N6 C27 C30 106.3(4) . . ?
C28 C27 C30 110.2(5) . . ?
N6 C27 C29 109.8(4) . . ?
C28 C27 C29 109.5(5) . . ?
C30 C27 C29 109.9(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_refine_diff_density_max         4.230
_refine_diff_density_min         -2.297
_refine_diff_density_rms         0.136

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_msb501_0m
_database_code_depnum_ccdc_archive 'CCDC 1023325'
_audit_update_record             
;
2014-09-08 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H120 Br4 Cu4 I2 N12 O5 P8 Pd2, C H2 Cl2'
_chemical_formula_sum            'C61 H122 Br4 Cl2 Cu4 I2 N12 O5 P8 Pd2'
_chemical_formula_weight         2462.76

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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   15.4735(8)
_cell_length_b                   19.4221(10)
_cell_length_c                   17.5182(9)
_cell_angle_alpha                90
_cell_angle_beta                 113.4600(10)
_cell_angle_gamma                90
_cell_volume                     4829.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9492
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.81

_exptl_crystal_description       Column
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_F_000             2440
_exptl_transmission_factor_min   0.469
_exptl_transmission_factor_max   0.734
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.093
_exptl_absorpt_coefficient_mu    3.757
_shelx_estimated_absorpt_T_min   0.588
_shelx_estimated_absorpt_T_max   0.721
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_T_max  0.72

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, collected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 20 sec/frame.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3660
_diffrn_reflns_number            82607
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.821
_diffrn_reflns_theta_max         27.874
_diffrn_reflns_theta_full        27.870
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11495
_reflns_number_gt                9073
_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       'APEX2 (Bruker, 2009)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2009)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. H-atoms attached to carbon
 were placed in calculated positions (C---H = 0.95 - 0.98 Å) while those
 attached to nitrogen and oxygen were placed in locations derived from a
 difference map and adjusted to have N---H or O---H distances appropriate
 for the temperature of data collection. All were included as riding
 contributions with isotropic displacement  parameters 1.2 - 1.5 times
 those of the attached atoms. The iodine and bromine atoms as well as Cu2
 and the t-butyl group based on C19 are each disordered over two resolved
 sites. Refinement was completed with restraints that the two components of
 each disordered moiety have the same geometry and that the total occupancy
 of the two sites equal to 1.0.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1032P)²+38.5776P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_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         11495
_refine_ls_number_parameters     503
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1950
_refine_ls_wR_factor_gt          0.1779
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.74177(3) -0.12665(2) 0.50132(3) 0.01473(12) Uani 1 1 d D . . . .
I1 I 0.87953(5) -0.08486(4) 0.46241(5) 0.0403(2) Uani 0.6996(13) 1 d D . P A 1
I1A I 0.87350(12) -0.04807(11) 0.48683(13) 0.0403(2) Uani 0.3004(13) 1 d D . P
A 2
Cu1 Cu 0.97242(5) 0.07764(4) 0.72567(5) 0.02148(18) Uani 1 1 d . . . . .
Cu2 Cu 1.13716(10) 0.16446(7) 0.74548(11) 0.0255(3) Uani 0.6239(18) 1 d D U P B
1
Br1 Br 0.97713(11) 0.20617(8) 0.71207(12) 0.0320(4) Uani 0.6239(18) 1 d . U P B
1
Br2 Br 1.1457(5) 0.0512(4) 0.8111(3) 0.0425(10) Uani 0.6239(18) 1 d . U P B 1
Cu2A Cu 1.13404(18) 0.15285(13) 0.70678(19) 0.0255(3) Uani 0.3761(18) 1 d D U P
B 2
Br1A Br 0.9729(2) 0.19362(14) 0.6789(2) 0.0320(4) Uani 0.3761(18) 1 d . U P B 2
Br2A Br 1.1365(8) 0.0475(7) 0.7897(6) 0.0425(10) Uani 0.3761(18) 1 d . U P B 2
P1 P 0.68894(11) -0.19637(8) 0.38869(9) 0.0199(3) Uani 1 1 d . . . . .
P2 P 0.75759(10) -0.07269(7) 0.62192(9) 0.0138(3) Uani 1 1 d . . . . .
P3 P 0.85316(10) 0.01856(7) 0.72577(9) 0.0134(3) Uani 1 1 d . . . . .
P4 P 1.25173(11) 0.21904(8) 0.72457(10) 0.0193(3) Uani 1 1 d D . . . .
O1 O 0.5989(3) -0.2373(2) 0.3945(3) 0.0241(9) Uani 1 1 d . . . . .
O2 O 0.6721(3) -0.1061(2) 0.6441(2) 0.0175(8) Uani 1 1 d . . . . .
O3 O 0.9612(8) 0.0582(6) 0.5977(7) 0.036(2) Uani 0.5 1 d . . P B .
H3OA H 1.0017 0.0690 0.5782 0.044 Uiso 0.5 1 d R U P . .
H3OB H 0.9980 0.0264 0.6255 0.044 Uiso 0.5 1 d R U P . .
N1 N 0.7545(3) 0.0119(2) 0.6339(3) 0.0152(9) Uani 1 1 d . . . . .
N2 N 0.8518(3) -0.0698(2) 0.7122(3) 0.0148(9) Uani 1 1 d . . . . .
N3 N 0.8170(4) 0.0311(2) 0.8012(3) 0.0190(10) Uani 1 1 d . . . . .
H3N H 0.7646 0.0043 0.8013 0.023 Uiso 1 1 d R U . . .
N4 N 1.2415(4) 0.2532(3) 0.6299(3) 0.0253(11) Uani 1 1 d . . . . .
N5 N 1.3402(4) 0.1736(3) 0.7107(3) 0.0226(11) Uani 1 1 d . . . . .
N6 N 1.3023(4) 0.2782(3) 0.7950(3) 0.0255(12) Uani 1 1 d . . . . .
H6N H 1.3402 0.3087 0.7784 0.031 Uiso 1 1 d R U . . .
C1 C 0.5785(4) -0.2189(3) 0.4634(4) 0.0190(11) Uani 1 1 d . . . . .
C2 C 0.5027(4) -0.2491(3) 0.4735(4) 0.0218(12) Uani 1 1 d . . . . .
H2 H 0.4632 -0.2809 0.4336 0.026 Uiso 1 1 calc R U . . .
C3 C 0.4857(4) -0.2319(3) 0.5431(4) 0.0223(12) Uani 1 1 d . . . . .
H3 H 0.4347 -0.2531 0.5512 0.027 Uiso 1 1 calc R U . . .
C4 C 0.5414(4) -0.1845(3) 0.6013(4) 0.0197(11) Uani 1 1 d . . . . .
H4 H 0.5292 -0.1729 0.6487 0.024 Uiso 1 1 calc R U . . .
C5 C 0.6163(4) -0.1545(3) 0.5875(3) 0.0148(10) Uani 1 1 d . . . . .
C6 C 0.6353(4) -0.1713(3) 0.5186(4) 0.0152(10) Uani 1 1 d . . . . .
C7 C 0.6829(4) 0.0632(3) 0.5842(4) 0.0167(11) Uani 1 1 d . . . . .
C8 C 0.6388(5) 0.0386(4) 0.4938(4) 0.0285(14) Uani 1 1 d . . . . .
H8A H 0.6070 -0.0056 0.4910 0.043 Uiso 1 1 calc R U . . .
H8B H 0.6882 0.0328 0.4726 0.043 Uiso 1 1 calc R U . . .
H8C H 0.5929 0.0727 0.4599 0.043 Uiso 1 1 calc R U . . .
C9 C 0.6080(4) 0.0699(4) 0.6210(5) 0.0281(14) Uani 1 1 d . . . . .
H9A H 0.5766 0.0254 0.6172 0.042 Uiso 1 1 calc R U . . .
H9B H 0.5613 0.1045 0.5897 0.042 Uiso 1 1 calc R U . . .
H9C H 0.6383 0.0838 0.6795 0.042 Uiso 1 1 calc R U . . .
C10 C 0.7316(4) 0.1319(3) 0.5894(4) 0.0231(12) Uani 1 1 d . . . . .
H10A H 0.7598 0.1472 0.6475 0.035 Uiso 1 1 calc R U . . .
H10B H 0.6854 0.1661 0.5560 0.035 Uiso 1 1 calc R U . . .
H10C H 0.7810 0.1269 0.5681 0.035 Uiso 1 1 calc R U . . .
C11 C 0.9240(4) -0.1231(3) 0.7527(4) 0.0181(11) Uani 1 1 d . . . . .
C12 C 0.9910(5) -0.1297(4) 0.7086(5) 0.0346(17) Uani 1 1 d . . . . .
H12A H 0.9556 -0.1441 0.6509 0.052 Uiso 1 1 calc R U . . .
H12B H 1.0395 -0.1640 0.7373 0.052 Uiso 1 1 calc R U . . .
H12C H 1.0210 -0.0851 0.7093 0.052 Uiso 1 1 calc R U . . .
C13 C 0.8730(5) -0.1908(3) 0.7494(4) 0.0282(14) Uani 1 1 d . . . . .
H13A H 0.8379 -0.2043 0.6913 0.042 Uiso 1 1 calc R U . . .
H13B H 0.8292 -0.1851 0.7768 0.042 Uiso 1 1 calc R U . . .
H13C H 0.9191 -0.2266 0.7781 0.042 Uiso 1 1 calc R U . . .
C14 C 0.9789(4) -0.1004(3) 0.8423(4) 0.0206(12) Uani 1 1 d . . . . .
H14A H 1.0106 -0.0566 0.8429 0.031 Uiso 1 1 calc R U . . .
H14B H 1.0259 -0.1355 0.8717 0.031 Uiso 1 1 calc R U . . .
H14C H 0.9354 -0.0946 0.8700 0.031 Uiso 1 1 calc R U . . .
C15 C 0.8505(5) 0.0816(3) 0.8715(4) 0.0218(12) Uani 1 1 d . . . . .
C16 C 0.8133(7) 0.0559(4) 0.9345(5) 0.0414(19) Uani 1 1 d . . . . .
H16A H 0.7443 0.0545 0.9088 0.062 Uiso 1 1 calc R U . . .
H16B H 0.8338 0.0870 0.9825 0.062 Uiso 1 1 calc R U . . .
H16C H 0.8378 0.0096 0.9529 0.062 Uiso 1 1 calc R U . . .
C17 C 0.8106(5) 0.1536(3) 0.8396(5) 0.0310(15) Uani 1 1 d . . . . .
H17A H 0.8357 0.1697 0.7995 0.046 Uiso 1 1 calc R U . . .
H17B H 0.8289 0.1858 0.8866 0.046 Uiso 1 1 calc R U . . .
H17C H 0.7417 0.1512 0.8125 0.046 Uiso 1 1 calc R U . . .
C18 C 0.9575(5) 0.0837(4) 0.9116(5) 0.0334(16) Uani 1 1 d . . . . .
H18A H 0.9817 0.1004 0.8711 0.050 Uiso 1 1 calc R U . . .
H18B H 0.9819 0.0373 0.9299 0.050 Uiso 1 1 calc R U . . .
H18C H 0.9780 0.1147 0.9597 0.050 Uiso 1 1 calc R U . . .
C19 C 1.1744(6) 0.3041(4) 0.5752(4) 0.042(2) Uani 1 1 d D . . . .
C20 C 1.0854(7) 0.3051(6) 0.5800(7) 0.045(3) Uani 0.787(9) 1 d D . P C 1
H20A H 1.0940 0.3088 0.6383 0.068 Uiso 0.787(9) 1 calc R U P C 1
H20B H 1.0515 0.2625 0.5561 0.068 Uiso 0.787(9) 1 calc R U P C 1
H20C H 1.0492 0.3447 0.5488 0.068 Uiso 0.787(9) 1 calc R U P C 1
C21 C 1.1719(7) 0.2991(5) 0.4879(5) 0.033(2) Uani 0.787(9) 1 d D . P C 1
H21A H 1.2364 0.2988 0.4906 0.050 Uiso 0.787(9) 1 calc R U P C 1
H21B H 1.1377 0.3387 0.4550 0.050 Uiso 0.787(9) 1 calc R U P C 1
H21C H 1.1398 0.2565 0.4616 0.050 Uiso 0.787(9) 1 calc R U P C 1
C22 C 1.2261(7) 0.3793(5) 0.6082(6) 0.037(2) Uani 0.787(9) 1 d D . P C 1
H22A H 1.2880 0.3797 0.6051 0.055 Uiso 0.787(9) 1 calc R U P C 1
H22B H 1.2339 0.3867 0.6659 0.055 Uiso 0.787(9) 1 calc R U P C 1
H22C H 1.1870 0.4161 0.5731 0.055 Uiso 0.787(9) 1 calc R U P C 1
C20A C 1.198(2) 0.3305(17) 0.5150(19) 0.045(3) Uani 0.213(9) 1 d D . P C 2
H20D H 1.2224 0.2937 0.4908 0.068 Uiso 0.213(9) 1 calc R U P C 2
H20E H 1.2465 0.3659 0.5389 0.068 Uiso 0.213(9) 1 calc R U P C 2
H20F H 1.1422 0.3510 0.4716 0.068 Uiso 0.213(9) 1 calc R U P C 2
C21A C 1.135(2) 0.3481(13) 0.6245(17) 0.033(2) Uani 0.213(9) 1 d D . P C 2
H21D H 1.1194 0.3190 0.6632 0.050 Uiso 0.213(9) 1 calc R U P C 2
H21E H 1.0772 0.3711 0.5863 0.050 Uiso 0.213(9) 1 calc R U P C 2
H21F H 1.1811 0.3828 0.6559 0.050 Uiso 0.213(9) 1 calc R U P C 2
C22A C 1.081(2) 0.2489(14) 0.5284(19) 0.037(2) Uani 0.213(9) 1 d D . P C 2
H22D H 1.0653 0.2265 0.5711 0.055 Uiso 0.213(9) 1 calc R U P C 2
H22E H 1.0992 0.2138 0.4970 0.055 Uiso 0.213(9) 1 calc R U P C 2
H22F H 1.0270 0.2748 0.4905 0.055 Uiso 0.213(9) 1 calc R U P C 2
C23 C 1.3990(5) 0.1139(4) 0.7572(4) 0.0269(14) Uani 1 1 d . . . . .
C24 C 1.3521(8) 0.0449(4) 0.7204(5) 0.057(3) Uani 1 1 d . . . . .
H24A H 1.2909 0.0417 0.7245 0.085 Uiso 1 1 calc R U . . .
H24B H 1.3926 0.0069 0.7514 0.085 Uiso 1 1 calc R U . . .
H24C H 1.3431 0.0422 0.6618 0.085 Uiso 1 1 calc R U . . .
C25 C 1.4093(6) 0.1190(5) 0.8472(5) 0.0391(18) Uani 1 1 d . . . . .
H25A H 1.3473 0.1140 0.8494 0.059 Uiso 1 1 calc R U . . .
H25B H 1.4361 0.1639 0.8700 0.059 Uiso 1 1 calc R U . . .
H25C H 1.4512 0.0824 0.8801 0.059 Uiso 1 1 calc R U . . .
C26 C 1.4952(6) 0.1205(6) 0.7538(7) 0.056(3) Uani 1 1 d . . . . .
H26A H 1.4885 0.1166 0.6960 0.083 Uiso 1 1 calc R U . . .
H26B H 1.5365 0.0838 0.7871 0.083 Uiso 1 1 calc R U . . .
H26C H 1.5225 0.1654 0.7762 0.083 Uiso 1 1 calc R U . . .
C27 C 1.2777(6) 0.3032(4) 0.8645(5) 0.0343(16) Uani 1 1 d . . . . .
C28 C 1.2776(8) 0.2456(5) 0.9212(6) 0.053(2) Uani 1 1 d . . . . .
H28A H 1.2306 0.2111 0.8897 0.080 Uiso 1 1 calc R U . . .
H28B H 1.2619 0.2637 0.9663 0.080 Uiso 1 1 calc R U . . .
H28C H 1.3401 0.2242 0.9446 0.080 Uiso 1 1 calc R U . . .
C29 C 1.3496(9) 0.3586(6) 0.9085(7) 0.076(4) Uani 1 1 d . U . . .
H29A H 1.3475 0.3946 0.8686 0.113 Uiso 1 1 calc R U . . .
H29B H 1.4127 0.3381 0.9321 0.113 Uiso 1 1 calc R U . . .
H29C H 1.3350 0.3787 0.9533 0.113 Uiso 1 1 calc R U . . .
C30 C 1.1770(8) 0.3355(6) 0.8280(7) 0.064(3) Uani 1 1 d . . . . .
H30A H 1.1753 0.3735 0.7906 0.096 Uiso 1 1 calc R U . . .
H30B H 1.1615 0.3530 0.8735 0.096 Uiso 1 1 calc R U . . .
H30C H 1.1310 0.3004 0.7969 0.096 Uiso 1 1 calc R U . . .
C31 C 0.3476(13) 0.1224(14) 0.0958(16) 0.073(7) Uani 0.427(3) 1 d D U P D 1
H31A H 0.3819 0.1663 0.1005 0.087 Uiso 0.427(3) 1 calc R U P D 1
H31B H 0.3505 0.0962 0.0484 0.087 Uiso 0.427(3) 1 calc R U P D 1
Cl1 Cl 0.2289(3) 0.1400(2) 0.0768(3) 0.0304(8) Uani 0.427(3) 1 d D . P D 1
Cl2 Cl 0.4025(3) 0.0743(2) 0.1886(3) 0.0381(10) Uani 0.427(3) 1 d D . P D 1
C31A C 0.439(4) 0.070(8) 0.170(4) 0.073(7) Uani 0.073(3) 1 d D U P D 2
H31C H 0.4633 0.0304 0.2089 0.087 Uiso 0.073(3) 1 calc R U P D 2
H31D H 0.4888 0.1055 0.1871 0.087 Uiso 0.073(3) 1 calc R U P D 2
Cl1A Cl 0.3399(16) 0.1027(12) 0.1802(15) 0.0304(8) Uani 0.073(3) 1 d D . P D 2
Cl2A Cl 0.4195(19) 0.0419(13) 0.0694(16) 0.0381(10) Uani 0.073(3) 1 d D . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C6 1.989(6) . ?
Pd1 P1 2.2605(15) . ?
Pd1 P2 2.2826(14) . ?
Pd1 I1 2.6123(8) . ?
Pd1 I1A 2.6382(17) . ?
Cu1 P3 2.1738(16) . ?
Cu1 O3 2.212(10) . ?
Cu1 Br1A 2.398(3) . ?
Cu1 Br2A 2.404(12) . ?
Cu1 Br1 2.5114(17) . ?
Cu1 Br2 2.549(6) . ?
Cu1 Cu2 2.9592(16) . ?
Cu1 Cu2A 3.026(3) . ?
Cu2 P4 2.218(2) . ?
Cu2 Br1 2.445(2) . ?
Cu2 Br2 2.462(7) . ?
Cu2A P4 2.148(3) . ?
Cu2A Br1A 2.472(4) . ?
Cu2A Br2A 2.501(13) . ?
P1 O1 1.642(5) . ?
P1 N4 1.662(5) 3_756 ?
P1 N5 1.676(5) 3_756 ?
P1 P4 2.535(2) 3_756 ?
P2 O2 1.652(4) . ?
P2 N1 1.659(5) . ?
P2 N2 1.671(5) . ?
P3 N3 1.645(5) . ?
P3 N1 1.727(5) . ?
P3 N2 1.732(5) . ?
P4 N6 1.640(5) . ?
P4 N5 1.726(5) . ?
P4 N4 1.734(6) . ?
O1 C1 1.410(7) . ?
O2 C5 1.388(7) . ?
O3 H3OA 0.8500 . ?
O3 H3OB 0.8500 . ?
N1 C7 1.487(7) . ?
N2 C11 1.480(7) . ?
N3 C15 1.497(7) . ?
N3 H3N 0.9633 . ?
N4 C19 1.476(9) . ?
N4 P1 1.662(5) 3_756 ?
N5 C23 1.498(8) . ?
N5 P1 1.676(5) 3_756 ?
N6 C27 1.493(8) . ?
N6 H6N 0.9570 . ?
C1 C6 1.373(8) . ?
C1 C2 1.383(8) . ?
C2 C3 1.386(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.401(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(8) . ?
C7 C10 1.516(8) . ?
C7 C8 1.531(8) . ?
C7 C9 1.540(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C14 1.523(8) . ?
C11 C12 1.524(9) . ?
C11 C13 1.524(9) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.518(10) . ?
C15 C18 1.521(10) . ?
C15 C17 1.541(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20A 1.347(18) . ?
C19 C20 1.413(11) . ?
C19 C21A 1.511(17) . ?
C19 C21 1.518(11) . ?
C19 C22 1.655(12) . ?
C19 C22A 1.718(18) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C23 C26 1.518(11) . ?
C23 C25 1.523(10) . ?
C23 C24 1.538(11) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.496(12) . ?
C27 C29 1.519(11) . ?
C27 C30 1.561(13) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 Cl1 1.765(19) . ?
C31 Cl2 1.770(19) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31A Cl1A 1.74(2) . ?
C31A Cl2A 1.75(2) . ?
C31A H31C 0.9900 . ?
C31A H31D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 Pd1 P1 80.66(17) . . ?
C6 Pd1 P2 81.35(17) . . ?
P1 Pd1 P2 162.01(6) . . ?
C6 Pd1 I1 170.63(16) . . ?
P1 Pd1 I1 90.43(5) . . ?
P2 Pd1 I1 107.51(4) . . ?
C6 Pd1 I1A 170.23(17) . . ?
P1 Pd1 I1A 106.70(7) . . ?
P2 Pd1 I1A 91.21(6) . . ?
P3 Cu1 O3 100.8(3) . . ?
P3 Cu1 Br1A 127.90(8) . . ?
O3 Cu1 Br1A 79.9(3) . . ?
P3 Cu1 Br2A 127.6(3) . . ?
O3 Cu1 Br2A 94.2(4) . . ?
Br1A Cu1 Br2A 104.0(3) . . ?
P3 Cu1 Br1 125.56(6) . . ?
O3 Cu1 Br1 93.9(3) . . ?
P3 Cu1 Br2 126.00(17) . . ?
O3 Cu1 Br2 101.5(3) . . ?
Br1 Cu1 Br2 101.12(18) . . ?
P3 Cu1 Cu2 173.05(6) . . ?
O3 Cu1 Cu2 86.1(3) . . ?
Br1 Cu1 Cu2 52.31(5) . . ?
Br2 Cu1 Cu2 52.45(17) . . ?
P3 Cu1 Cu2A 173.62(8) . . ?
O3 Cu1 Cu2A 72.9(3) . . ?
Br1A Cu1 Cu2A 52.70(8) . . ?
Br2A Cu1 Cu2A 53.4(3) . . ?
P4 Cu2 Br1 127.03(8) . . ?
P4 Cu2 Br2 127.36(19) . . ?
Br1 Cu2 Br2 105.59(19) . . ?
P4 Cu2 Cu1 163.94(9) . . ?
Br1 Cu2 Cu1 54.38(5) . . ?
Br2 Cu2 Cu1 55.17(15) . . ?
Cu2 Br1 Cu1 73.31(6) . . ?
Cu2 Br2 Cu1 72.38(18) . . ?
P4 Cu2A Br1A 124.54(14) . . ?
P4 Cu2A Br2A 126.1(3) . . ?
Br1A Cu2A Br2A 99.1(3) . . ?
P4 Cu2A Cu1 164.34(14) . . ?
Br1A Cu2A Cu1 50.49(8) . . ?
Br2A Cu2A Cu1 50.5(3) . . ?
Cu1 Br1A Cu2A 76.81(11) . . ?
Cu1 Br2A Cu2A 76.1(4) . . ?
O1 P1 N4 108.8(3) . 3_756 ?
O1 P1 N5 107.9(3) . 3_756 ?
N4 P1 N5 84.2(3) 3_756 3_756 ?
O1 P1 Pd1 104.88(16) . . ?
N4 P1 Pd1 122.1(2) 3_756 . ?
N5 P1 Pd1 127.1(2) 3_756 . ?
O1 P1 P4 123.04(17) . 3_756 ?
N4 P1 P4 42.8(2) 3_756 3_756 ?
N5 P1 P4 42.59(18) 3_756 3_756 ?
Pd1 P1 P4 132.03(8) . 3_756 ?
O2 P2 N1 107.1(2) . . ?
O2 P2 N2 105.7(2) . . ?
N1 P2 N2 84.6(2) . . ?
O2 P2 Pd1 103.66(15) . . ?
N1 P2 Pd1 124.99(18) . . ?
N2 P2 Pd1 128.50(18) . . ?
N3 P3 N1 107.7(3) . . ?
N3 P3 N2 105.5(2) . . ?
N1 P3 N2 80.8(2) . . ?
N3 P3 Cu1 118.86(19) . . ?
N1 P3 Cu1 118.32(18) . . ?
N2 P3 Cu1 119.12(18) . . ?
N6 P4 N5 107.2(3) . . ?
N6 P4 N4 106.6(3) . . ?
N5 P4 N4 80.6(3) . . ?
N6 P4 Cu2A 130.7(2) . . ?
N5 P4 Cu2A 110.4(2) . . ?
N4 P4 Cu2A 109.9(2) . . ?
N6 P4 Cu2 112.6(2) . . ?
N5 P4 Cu2 120.7(2) . . ?
N4 P4 Cu2 124.5(2) . . ?
N6 P4 P1 119.9(2) . 3_756 ?
N5 P4 P1 41.07(18) . 3_756 ?
N4 P4 P1 40.66(18) . 3_756 ?
Cu2A P4 P1 109.44(11) . 3_756 ?
Cu2 P4 P1 127.50(9) . 3_756 ?
C1 O1 P1 114.5(4) . . ?
C5 O2 P2 115.3(3) . . ?
Cu1 O3 H3OA 126.3 . . ?
Cu1 O3 H3OB 77.2 . . ?
H3OA O3 H3OB 88.7 . . ?
C7 N1 P2 130.0(4) . . ?
C7 N1 P3 132.1(4) . . ?
P2 N1 P3 97.6(2) . . ?
C11 N2 P2 129.6(4) . . ?
C11 N2 P3 131.4(4) . . ?
P2 N2 P3 97.0(2) . . ?
C15 N3 P3 129.9(4) . . ?
C15 N3 H3N 111.6 . . ?
P3 N3 H3N 118.5 . . ?
C19 N4 P1 131.3(5) . 3_756 ?
C19 N4 P4 130.5(5) . . ?
P1 N4 P4 96.5(3) 3_756 . ?
C23 N5 P1 128.6(4) . 3_756 ?
C23 N5 P4 131.6(4) . . ?
P1 N5 P4 96.3(3) 3_756 . ?
C27 N6 P4 129.8(5) . . ?
C27 N6 H6N 115.7 . . ?
P4 N6 H6N 111.8 . . ?
C6 C1 C2 122.2(6) . . ?
C6 C1 O1 118.3(5) . . ?
C2 C1 O1 119.5(5) . . ?
C1 C2 C3 118.5(5) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C2 C3 C4 121.7(6) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 117.6(6) . . ?
C3 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
O2 C5 C6 119.5(5) . . ?
O2 C5 C4 118.7(5) . . ?
C6 C5 C4 121.7(5) . . ?
C1 C6 C5 118.2(5) . . ?
C1 C6 Pd1 121.6(4) . . ?
C5 C6 Pd1 120.2(4) . . ?
N1 C7 C10 108.6(5) . . ?
N1 C7 C8 108.5(5) . . ?
C10 C7 C8 110.1(5) . . ?
N1 C7 C9 108.7(5) . . ?
C10 C7 C9 109.9(5) . . ?
C8 C7 C9 111.0(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C14 107.3(5) . . ?
N2 C11 C12 110.6(5) . . ?
C14 C11 C12 109.5(5) . . ?
N2 C11 C13 107.7(5) . . ?
C14 C11 C13 110.8(5) . . ?
C12 C11 C13 110.8(6) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 C16 106.0(5) . . ?
N3 C15 C18 110.7(5) . . ?
C16 C15 C18 109.3(6) . . ?
N3 C15 C17 109.9(5) . . ?
C16 C15 C17 110.4(6) . . ?
C18 C15 C17 110.4(6) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20A C19 N4 115.1(16) . . ?
C20 C19 N4 114.9(7) . . ?
C20A C19 C21A 122.1(15) . . ?
N4 C19 C21A 110.5(13) . . ?
C20 C19 C21 115.2(7) . . ?
N4 C19 C21 109.9(6) . . ?
C20 C19 C22 108.3(7) . . ?
N4 C19 C22 104.4(6) . . ?
C21 C19 C22 102.9(7) . . ?
C20A C19 C22A 107.5(13) . . ?
N4 C19 C22A 97.5(13) . . ?
C21A C19 C22A 99.8(11) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C20A H20D 109.5 . . ?
C19 C20A H20E 109.5 . . ?
H20D C20A H20E 109.5 . . ?
C19 C20A H20F 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C19 C21A H21D 109.5 . . ?
C19 C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
C19 C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C19 C22A H22D 109.5 . . ?
C19 C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C19 C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
N5 C23 C26 107.8(6) . . ?
N5 C23 C25 107.6(5) . . ?
C26 C23 C25 109.5(7) . . ?
N5 C23 C24 111.3(6) . . ?
C26 C23 C24 111.3(8) . . ?
C25 C23 C24 109.2(7) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C27 C28 111.5(6) . . ?
N6 C27 C29 105.7(6) . . ?
C28 C27 C29 112.7(9) . . ?
N6 C27 C30 109.5(7) . . ?
C28 C27 C30 107.9(8) . . ?
C29 C27 C30 109.4(8) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Cl1 C31 Cl2 111.0(15) . . ?
Cl1 C31 H31A 109.4 . . ?
Cl2 C31 H31A 109.4 . . ?
Cl1 C31 H31B 109.4 . . ?
Cl2 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
Cl1A C31A Cl2A 114(3) . . ?
Cl1A C31A H31C 108.7 . . ?
Cl2A C31A H31C 108.7 . . ?
Cl1A C31A H31D 108.7 . . ?
Cl2A C31A H31D 108.7 . . ?
H31C C31A H31D 107.6 . . ?

_refine_diff_density_max         3.226
_refine_diff_density_min         -3.546
_refine_diff_density_rms         0.217

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_MSB426_0mm
_database_code_depnum_ccdc_archive 'CCDC 1023326'
_audit_update_record             
;
2014-09-08 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H59 I N6 O2 P4'
_chemical_formula_sum            'C30 H59 I N6 O2 P4'
_chemical_formula_weight         786.61

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'
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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   28.754(3)
_cell_length_b                   8.4632(8)
_cell_length_c                   16.4274(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3997.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9385
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      29.02

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             1640
_exptl_transmission_factor_min   0.776
_exptl_transmission_factor_max   0.982
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.147
_exptl_absorpt_coefficient_mu    0.994
_shelx_estimated_absorpt_T_min   0.768
_shelx_estimated_absorpt_T_max   0.868
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.87

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, collected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 20 sec/frame.
;


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3660
_diffrn_reflns_number            67723
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.407
_diffrn_reflns_theta_max         29.051
_diffrn_reflns_theta_full        29.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             10480
_reflns_number_gt                9838
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_max     0.991
_reflns_Friedel_fraction_full    0.994

_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       'APEX2 (Bruker, 2009)'
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2009)'

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based 
on F, with F set to zero for negative F². The threshold expression of 
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F² are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. H-atoms were placed in
calculated positions (C---H = 0.95 - 0.98 Å) and included as riding
contributions with isotropic displacement parameters 1.2 - 1.5 times those
of the attached carbon atoms. Refined as a 2-component inversion 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)+(0.0412P)²+4.1580P] 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_abs_structure_details 
;
 Refined as an inversion twin (Parsons et al., 2013).
;
_refine_ls_abs_structure_Flack   0.154(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10480
_refine_ls_number_parameters     407
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0929
_refine_ls_wR_factor_gt          0.0915
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.131
_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
I1 I 0.22109(2) 0.33196(3) 0.37049(2) 0.02651(8) Uani 1 1 d . . . . .
P1 P 0.11416(4) 0.07248(14) 0.51942(7) 0.0204(2) Uani 1 1 d . . . . .
P2 P 0.05934(4) 0.07781(14) 0.39394(7) 0.0204(2) Uani 1 1 d . . . . .
P3 P 0.36221(4) 0.39698(13) 0.49708(7) 0.0182(2) Uani 1 1 d . . . . .
P4 P 0.38014(3) 0.58695(12) 0.37663(8) 0.0184(2) Uani 1 1 d . . . . .
O1 O 0.15345(11) 0.2200(4) 0.5081(2) 0.0224(7) Uani 1 1 d . . . . .
O2 O 0.31491(11) 0.2917(4) 0.4653(2) 0.0203(6) Uani 1 1 d . . . . .
N1 N 0.11171(14) -0.0063(5) 0.4253(3) 0.0239(8) Uani 1 1 d . . . . .
N2 N 0.06678(13) 0.1719(5) 0.4872(2) 0.0218(8) Uani 1 1 d . . . . .
N3 N 0.07416(14) 0.2177(5) 0.3275(2) 0.0225(8) Uani 1 1 d . . . . .
H3N H 0.1027 0.2638 0.3321 0.027 Uiso 1 1 d R U . . .
N4 N 0.34855(15) 0.5830(4) 0.4672(3) 0.0222(8) Uani 1 1 d . . . . .
N5 N 0.39198(13) 0.3951(4) 0.4093(2) 0.0172(7) Uani 1 1 d . . . . .
N6 N 0.34072(14) 0.5642(5) 0.3038(3) 0.0229(8) Uani 1 1 d . . . . .
H6N H 0.3180 0.5189 0.3232 0.028 Uiso 1 1 d R U . . .
C1 C 0.23446(15) 0.2542(5) 0.4890(3) 0.0184(8) Uani 1 1 d . . . . .
C2 C 0.19736(15) 0.2066(5) 0.5388(3) 0.0182(8) Uani 1 1 d . . . . .
C3 C 0.20651(18) 0.1521(5) 0.6175(3) 0.0211(9) Uani 1 1 d . . . . .
H3 H 0.1817 0.1194 0.6518 0.025 Uiso 1 1 calc R U . . .
C4 C 0.25197(18) 0.1459(5) 0.6452(3) 0.0224(9) Uani 1 1 d . . . . .
H4 H 0.2582 0.1071 0.6983 0.027 Uiso 1 1 calc R U . . .
C5 C 0.28864(18) 0.1957(5) 0.5963(3) 0.0212(9) Uani 1 1 d . . . . .
H5 H 0.3195 0.1935 0.6167 0.025 Uiso 1 1 calc R U . . .
C6 C 0.28004(14) 0.2490(5) 0.5174(3) 0.0182(8) Uani 1 1 d . . . . .
C7 C 0.1317(2) -0.1611(6) 0.4007(4) 0.0280(11) Uani 1 1 d . . . . .
C8 C 0.1819(2) -0.1673(7) 0.4311(5) 0.0400(14) Uani 1 1 d . . . . .
H8A H 0.1999 -0.0829 0.4052 0.060 Uiso 1 1 calc R U . . .
H8B H 0.1955 -0.2699 0.4173 0.060 Uiso 1 1 calc R U . . .
H8C H 0.1823 -0.1530 0.4903 0.060 Uiso 1 1 calc R U . . .
C9 C 0.1309(3) -0.1741(7) 0.3088(4) 0.0425(16) Uani 1 1 d . . . . .
H9A H 0.0986 -0.1798 0.2900 0.064 Uiso 1 1 calc R U . . .
H9B H 0.1475 -0.2698 0.2920 0.064 Uiso 1 1 calc R U . . .
H9C H 0.1460 -0.0812 0.2849 0.064 Uiso 1 1 calc R U . . .
C10 C 0.1037(2) -0.2968(7) 0.4376(4) 0.0408(14) Uani 1 1 d . . . . .
H10A H 0.1018 -0.2829 0.4968 0.061 Uiso 1 1 calc R U . . .
H10B H 0.1190 -0.3974 0.4253 0.061 Uiso 1 1 calc R U . . .
H10C H 0.0723 -0.2970 0.4145 0.061 Uiso 1 1 calc R U . . .
C11 C 0.03259(15) 0.2568(6) 0.5369(3) 0.0213(9) Uani 1 1 d . . . . .
C12 C 0.05879(19) 0.3729(6) 0.5914(3) 0.0295(11) Uani 1 1 d . . . . .
H12A H 0.0794 0.3143 0.6282 0.044 Uiso 1 1 calc R U . . .
H12B H 0.0365 0.4344 0.6235 0.044 Uiso 1 1 calc R U . . .
H12C H 0.0773 0.4445 0.5576 0.044 Uiso 1 1 calc R U . . .
C13 C 0.00465(18) 0.1404(6) 0.5896(3) 0.0296(11) Uani 1 1 d . . . . .
H13A H -0.0141 0.0719 0.5544 0.044 Uiso 1 1 calc R U . . .
H13B H -0.0159 0.1995 0.6263 0.044 Uiso 1 1 calc R U . . .
H13C H 0.0261 0.0756 0.6218 0.044 Uiso 1 1 calc R U . . .
C14 C -0.00005(19) 0.3482(7) 0.4808(3) 0.0322(12) Uani 1 1 d . . . . .
H14A H 0.0182 0.4176 0.4453 0.048 Uiso 1 1 calc R U . . .
H14B H -0.0215 0.4119 0.5135 0.048 Uiso 1 1 calc R U . . .
H14C H -0.0178 0.2736 0.4474 0.048 Uiso 1 1 calc R U . . .
C15 C 0.05469(18) 0.2493(6) 0.2465(3) 0.0243(9) Uani 1 1 d . . . . .
C16 C 0.0782(2) 0.1442(7) 0.1833(3) 0.0341(12) Uani 1 1 d . . . . .
H16A H 0.1120 0.1526 0.1889 0.051 Uiso 1 1 calc R U . . .
H16B H 0.0690 0.1782 0.1286 0.051 Uiso 1 1 calc R U . . .
H16C H 0.0686 0.0342 0.1917 0.051 Uiso 1 1 calc R U . . .
C17 C 0.0652(2) 0.4232(7) 0.2267(4) 0.0408(14) Uani 1 1 d . . . . .
H17A H 0.0509 0.4913 0.2680 0.061 Uiso 1 1 calc R U . . .
H17B H 0.0525 0.4494 0.1730 0.061 Uiso 1 1 calc R U . . .
H17C H 0.0989 0.4399 0.2264 0.061 Uiso 1 1 calc R U . . .
C18 C 0.00236(18) 0.2214(7) 0.2464(3) 0.0325(11) Uani 1 1 d . . . . .
H18A H -0.0040 0.1107 0.2598 0.049 Uiso 1 1 calc R U . . .
H18B H -0.0102 0.2455 0.1924 0.049 Uiso 1 1 calc R U . . .
H18C H -0.0123 0.2901 0.2870 0.049 Uiso 1 1 calc R U . . .
C19 C 0.33379(17) 0.7160(6) 0.5182(3) 0.0226(9) Uani 1 1 d . . . . .
C20 C 0.3749(2) 0.7819(7) 0.5664(4) 0.0346(12) Uani 1 1 d . . . . .
H20A H 0.3875 0.6993 0.6019 0.052 Uiso 1 1 calc R U . . .
H20B H 0.3645 0.8714 0.5995 0.052 Uiso 1 1 calc R U . . .
H20C H 0.3991 0.8174 0.5286 0.052 Uiso 1 1 calc R U . . .
C21 C 0.3143(2) 0.8451(6) 0.4620(4) 0.0379(13) Uani 1 1 d . . . . .
H21A H 0.3396 0.8888 0.4288 0.057 Uiso 1 1 calc R U . . .
H21B H 0.3005 0.9293 0.4950 0.057 Uiso 1 1 calc R U . . .
H21C H 0.2905 0.7995 0.4263 0.057 Uiso 1 1 calc R U . . .
C22 C 0.2957(2) 0.6593(7) 0.5754(4) 0.0444(15) Uani 1 1 d . . . . .
H22A H 0.2708 0.6096 0.5438 0.067 Uiso 1 1 calc R U . . .
H22B H 0.2831 0.7495 0.6057 0.067 Uiso 1 1 calc R U . . .
H22C H 0.3086 0.5823 0.6138 0.067 Uiso 1 1 calc R U . . .
C23 C 0.41615(14) 0.2656(5) 0.3668(4) 0.0204(7) Uani 1 1 d . . . . .
C24 C 0.45810(17) 0.3316(6) 0.3223(3) 0.0262(10) Uani 1 1 d . . . . .
H24A H 0.4478 0.4087 0.2816 0.039 Uiso 1 1 calc R U . . .
H24B H 0.4747 0.2454 0.2951 0.039 Uiso 1 1 calc R U . . .
H24C H 0.4789 0.3834 0.3613 0.039 Uiso 1 1 calc R U . . .
C25 C 0.38326(19) 0.1852(6) 0.3080(3) 0.0295(11) Uani 1 1 d . . . . .
H25A H 0.3560 0.1465 0.3377 0.044 Uiso 1 1 calc R U . . .
H25B H 0.3992 0.0961 0.2819 0.044 Uiso 1 1 calc R U . . .
H25C H 0.3734 0.2609 0.2664 0.044 Uiso 1 1 calc R U . . .
C26 C 0.4325(2) 0.1467(6) 0.4318(3) 0.0340(12) Uani 1 1 d . . . . .
H26A H 0.4526 0.2005 0.4712 0.051 Uiso 1 1 calc R U . . .
H26B H 0.4499 0.0611 0.4055 0.051 Uiso 1 1 calc R U . . .
H26C H 0.4054 0.1026 0.4600 0.051 Uiso 1 1 calc R U . . .
C27 C 0.33369(19) 0.6579(5) 0.2294(3) 0.0246(10) Uani 1 1 d . . . . .
C28 C 0.31922(19) 0.5445(6) 0.1617(3) 0.0296(11) Uani 1 1 d . . . . .
H28A H 0.3426 0.4609 0.1563 0.044 Uiso 1 1 calc R U . . .
H28B H 0.3167 0.6025 0.1102 0.044 Uiso 1 1 calc R U . . .
H28C H 0.2891 0.4973 0.1751 0.044 Uiso 1 1 calc R U . . .
C29 C 0.3789(2) 0.7400(7) 0.2049(3) 0.0304(12) Uani 1 1 d . . . . .
H29A H 0.3890 0.8102 0.2489 0.046 Uiso 1 1 calc R U . . .
H29B H 0.3738 0.8019 0.1553 0.046 Uiso 1 1 calc R U . . .
H29C H 0.4030 0.6603 0.1948 0.046 Uiso 1 1 calc R U . . .
C30 C 0.2951(2) 0.7804(7) 0.2419(4) 0.0338(12) Uani 1 1 d . . . . .
H30A H 0.2679 0.7290 0.2660 0.051 Uiso 1 1 calc R U . . .
H30B H 0.2866 0.8268 0.1893 0.051 Uiso 1 1 calc R U . . .
H30C H 0.3062 0.8637 0.2785 0.051 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
I1 C1 2.091(5) . ?
P1 N1 1.686(4) . ?
P1 N2 1.686(4) . ?
P1 O1 1.694(3) . ?
P2 N3 1.666(4) . ?
P2 N2 1.740(4) . ?
P2 N1 1.743(4) . ?
P3 N5 1.677(4) . ?
P3 N4 1.695(4) . ?
P3 O2 1.708(3) . ?
P4 N6 1.659(4) . ?
P4 N4 1.744(4) . ?
P4 N5 1.744(4) . ?
O1 C2 1.364(5) . ?
O2 C6 1.367(5) . ?
N1 C7 1.487(6) . ?
N2 C11 1.466(6) . ?
N3 C15 1.468(6) . ?
N3 H3N 0.9125 . ?
N4 C19 1.466(6) . ?
N5 C23 1.474(5) . ?
N6 C27 1.471(6) . ?
N6 H6N 0.8212 . ?
C1 C6 1.392(6) . ?
C1 C2 1.403(6) . ?
C2 C3 1.399(7) . ?
C3 C4 1.385(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(7) . ?
C5 H5 0.9500 . ?
C7 C9 1.514(10) . ?
C7 C8 1.527(8) . ?
C7 C10 1.528(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C14 1.527(7) . ?
C11 C12 1.528(7) . ?
C11 C13 1.538(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C18 1.523(7) . ?
C15 C16 1.525(7) . ?
C15 C17 1.538(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C22 1.522(8) . ?
C19 C20 1.529(7) . ?
C19 C21 1.536(8) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.513(7) . ?
C23 C24 1.518(6) . ?
C23 C26 1.540(7) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.527(7) . ?
C27 C29 1.528(7) . ?
C27 C30 1.531(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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
N1 P1 N2 82.9(2) . . ?
N1 P1 O1 102.6(2) . . ?
N2 P1 O1 97.86(18) . . ?
N3 P2 N2 102.7(2) . . ?
N3 P2 N1 105.2(2) . . ?
N2 P2 N1 79.67(19) . . ?
N5 P3 N4 83.01(19) . . ?
N5 P3 O2 97.96(17) . . ?
N4 P3 O2 102.20(19) . . ?
N6 P4 N4 104.9(2) . . ?
N6 P4 N5 104.30(19) . . ?
N4 P4 N5 79.69(18) . . ?
C2 O1 P1 121.0(3) . . ?
C6 O2 P3 122.0(3) . . ?
C7 N1 P1 125.6(4) . . ?
C7 N1 P2 127.9(4) . . ?
P1 N1 P2 98.4(2) . . ?
C11 N2 P1 127.7(3) . . ?
C11 N2 P2 129.2(3) . . ?
P1 N2 P2 98.5(2) . . ?
C15 N3 P2 128.7(3) . . ?
C15 N3 H3N 110.0 . . ?
P2 N3 H3N 118.6 . . ?
C19 N4 P3 127.9(3) . . ?
C19 N4 P4 128.6(3) . . ?
P3 N4 P4 98.3(2) . . ?
C23 N5 P3 130.9(3) . . ?
C23 N5 P4 129.7(3) . . ?
P3 N5 P4 98.97(19) . . ?
C27 N6 P4 129.1(3) . . ?
C27 N6 H6N 117.7 . . ?
P4 N6 H6N 108.5 . . ?
C6 C1 C2 120.8(4) . . ?
C6 C1 I1 119.7(3) . . ?
C2 C1 I1 119.5(3) . . ?
O1 C2 C3 122.9(4) . . ?
O1 C2 C1 117.7(4) . . ?
C3 C2 C1 119.4(4) . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 121.0(4) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 120.0(4) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
O2 C6 C1 118.2(4) . . ?
O2 C6 C5 122.5(4) . . ?
C1 C6 C5 119.3(4) . . ?
N1 C7 C9 109.2(5) . . ?
N1 C7 C8 107.8(4) . . ?
C9 C7 C8 109.8(6) . . ?
N1 C7 C10 110.5(5) . . ?
C9 C7 C10 109.5(5) . . ?
C8 C7 C10 110.0(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C14 108.9(4) . . ?
N2 C11 C12 108.1(4) . . ?
C14 C11 C12 109.4(4) . . ?
N2 C11 C13 110.5(4) . . ?
C14 C11 C13 110.1(4) . . ?
C12 C11 C13 109.9(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 C18 110.5(4) . . ?
N3 C15 C16 110.0(4) . . ?
C18 C15 C16 110.3(4) . . ?
N3 C15 C17 106.9(4) . . ?
C18 C15 C17 110.0(5) . . ?
C16 C15 C17 109.1(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 C22 108.6(4) . . ?
N4 C19 C20 110.6(4) . . ?
C22 C19 C20 110.6(5) . . ?
N4 C19 C21 108.0(4) . . ?
C22 C19 C21 109.5(5) . . ?
C20 C19 C21 109.5(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N5 C23 C25 110.0(4) . . ?
N5 C23 C24 109.2(3) . . ?
C25 C23 C24 110.8(5) . . ?
N5 C23 C26 107.6(4) . . ?
C25 C23 C26 109.8(4) . . ?
C24 C23 C26 109.4(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C27 C28 107.7(4) . . ?
N6 C27 C29 110.3(4) . . ?
C28 C27 C29 109.0(5) . . ?
N6 C27 C30 110.7(5) . . ?
C28 C27 C30 109.0(4) . . ?
C29 C27 C30 110.1(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
N6 H6N I1 0.82 3.30 4.110(4) 171 .

_refine_diff_density_max         1.420
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.098

_shelxl_version_number           2013-4

