# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
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#  as required by the journal to which it was submitted.
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data_msb304

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
1,3-Di-tert-butyl-2,4-bis-tert-butylamino-
2-methyl-4-selenoxo-4λ⁵-[1,3,2,4]diazadiphosphetidin-
2-ium iodide toluene solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H49 N4 P2 Se, I'
_chemical_formula_sum            'C24 H49 I N4 P2 Se'
_chemical_formula_weight         661.47

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

_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'

_cell_length_a                   9.3436(6)
_cell_length_b                   10.3905(7)
_cell_length_c                   16.7060(13)
_cell_angle_alpha                93.176(1)
_cell_angle_beta                 104.556(1)
_cell_angle_gamma                91.995(1)
_cell_volume                     1565.43(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6895
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             676
_exptl_transmission_factor_min   0.649
_exptl_transmission_factor_max   0.750
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.142
_exptl_absorpt_coefficient_mu    2.305
_shelx_estimated_absorpt_T_min   0.658
_shelx_estimated_absorpt_T_max   0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'

_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°.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27720
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.255
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_point_group_measured_fraction_full 0.942
_reflns_number_total             14366
_reflns_number_gt                13574
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_max     0.858
_reflns_Friedel_fraction_full    0.889

_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       'Bruker SMART (Bruker, 2000)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2000a)'

_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 on carbon were
 placed in  calculated positions (C---H = 0.95 - 0.98 Å) while those
 attached to nitrogen were placed in positions obtained from a difference
 map and then adjusted to have 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.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0124P)²] 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 
;
 Flack x determined using 5960 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.019(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         14366
_refine_ls_number_parameters     605
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0560
_refine_ls_wR_factor_gt          0.0554
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      0.979
_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
I1 I 0.32668(2) 0.70794(2) 0.91567(2) 0.01757(7) Uani 1 1 d . . . . .
I2 I 0.91256(2) 0.25098(2) 0.14438(2) 0.01805(7) Uani 1 1 d . . . . .
Se1 Se 0.48710(5) 0.56145(4) 0.39217(3) 0.02157(10) Uani 1 1 d . . . . .
P1 P 0.32779(11) 0.43519(10) 0.31448(7) 0.0134(2) Uani 1 1 d . . . . .
P2 P 0.38752(11) 0.24254(10) 0.23427(7) 0.0144(2) Uani 1 1 d . . . . .
N1 N 0.3497(4) 0.3946(3) 0.2183(2) 0.0144(7) Uani 1 1 d . . . . .
N2 N 0.3497(4) 0.2735(3) 0.3251(2) 0.0148(7) Uani 1 1 d . . . . .
N3 N 0.1568(4) 0.4675(3) 0.3064(2) 0.0156(7) Uani 1 1 d . . . . .
H3N H 0.0813 0.4248 0.2677 0.019 Uiso 1 1 d R U . . .
N4 N 0.2769(4) 0.1405(3) 0.1720(2) 0.0180(8) Uani 1 1 d . . . . .
H4N H 0.1835 0.1649 0.1698 0.022 Uiso 1 1 d R U . . .
C1 C 0.3647(5) 0.4767(4) 0.1496(3) 0.0167(9) Uani 1 1 d . . . . .
C2 C 0.5230(6) 0.5322(5) 0.1656(3) 0.0306(12) Uani 1 1 d . . . . .
H2A H 0.5509 0.5806 0.2198 0.046 Uiso 1 1 calc R U . . .
H2B H 0.5300 0.5901 0.1223 0.046 Uiso 1 1 calc R U . . .
H2C H 0.5899 0.4618 0.1652 0.046 Uiso 1 1 calc R U . . .
C3 C 0.3224(6) 0.3945(5) 0.0681(3) 0.0265(10) Uani 1 1 d . . . . .
H3A H 0.3932 0.3268 0.0694 0.040 Uiso 1 1 calc R U . . .
H3B H 0.3240 0.4490 0.0223 0.040 Uiso 1 1 calc R U . . .
H3C H 0.2227 0.3549 0.0602 0.040 Uiso 1 1 calc R U . . .
C4 C 0.2571(6) 0.5851(5) 0.1457(3) 0.0321(12) Uani 1 1 d . . . . .
H4A H 0.1568 0.5478 0.1395 0.048 Uiso 1 1 calc R U . . .
H4B H 0.2588 0.6360 0.0983 0.048 Uiso 1 1 calc R U . . .
H4C H 0.2867 0.6410 0.1969 0.048 Uiso 1 1 calc R U . . .
C5 C 0.3720(5) 0.1967(4) 0.4000(3) 0.0223(10) Uani 1 1 d . . . . .
C6 C 0.3336(6) 0.0544(4) 0.3701(3) 0.0297(11) Uani 1 1 d . . . . .
H6A H 0.2329 0.0455 0.3340 0.044 Uiso 1 1 calc R U . . .
H6B H 0.3397 0.0026 0.4180 0.044 Uiso 1 1 calc R U . . .
H6C H 0.4037 0.0242 0.3392 0.044 Uiso 1 1 calc R U . . .
C7 C 0.2663(6) 0.2437(5) 0.4504(3) 0.0289(11) Uani 1 1 d . . . . .
H7A H 0.2935 0.3338 0.4708 0.043 Uiso 1 1 calc R U . . .
H7B H 0.2727 0.1902 0.4975 0.043 Uiso 1 1 calc R U . . .
H7C H 0.1647 0.2375 0.4153 0.043 Uiso 1 1 calc R U . . .
C8 C 0.5316(6) 0.2135(5) 0.4525(3) 0.0358(13) Uani 1 1 d . . . . .
H8A H 0.5981 0.1778 0.4209 0.054 Uiso 1 1 calc R U . . .
H8B H 0.5415 0.1681 0.5033 0.054 Uiso 1 1 calc R U . . .
H8C H 0.5578 0.3056 0.4669 0.054 Uiso 1 1 calc R U . . .
C9 C 0.0808(5) 0.5709(5) 0.3445(3) 0.0198(10) Uani 1 1 d . . . . .
C10 C 0.1163(5) 0.5640(5) 0.4381(3) 0.0296(11) Uani 1 1 d . . . . .
H10A H 0.0866 0.4780 0.4514 0.044 Uiso 1 1 calc R U . . .
H10B H 0.0623 0.6291 0.4616 0.044 Uiso 1 1 calc R U . . .
H10C H 0.2230 0.5804 0.4617 0.044 Uiso 1 1 calc R U . . .
C11 C -0.0846(5) 0.5425(5) 0.3080(3) 0.0316(12) Uani 1 1 d . . . . .
H11A H -0.1080 0.5474 0.2478 0.047 Uiso 1 1 calc R U . . .
H11B H -0.1400 0.6060 0.3318 0.047 Uiso 1 1 calc R U . . .
H11C H -0.1120 0.4557 0.3211 0.047 Uiso 1 1 calc R U . . .
C12 C 0.1244(6) 0.7050(5) 0.3225(3) 0.0336(12) Uani 1 1 d . . . . .
H12A H 0.2319 0.7206 0.3424 0.050 Uiso 1 1 calc R U . . .
H12B H 0.0748 0.7703 0.3489 0.050 Uiso 1 1 calc R U . . .
H12C H 0.0946 0.7101 0.2623 0.050 Uiso 1 1 calc R U . . .
C13 C 0.2801(5) 0.0209(4) 0.1168(3) 0.0254(10) Uani 1 1 d . . . . .
C14 C 0.1608(6) -0.0727(5) 0.1295(5) 0.0505(17) Uani 1 1 d . . . . .
H14A H 0.1562 -0.1514 0.0936 0.076 Uiso 1 1 calc R U . . .
H14B H 0.0650 -0.0327 0.1155 0.076 Uiso 1 1 calc R U . . .
H14C H 0.1842 -0.0944 0.1875 0.076 Uiso 1 1 calc R U . . .
C15 C 0.4259(6) -0.0381(6) 0.1342(4) 0.0508(17) Uani 1 1 d . . . . .
H15A H 0.5001 0.0229 0.1234 0.076 Uiso 1 1 calc R U . . .
H15B H 0.4192 -0.1171 0.0983 0.076 Uiso 1 1 calc R U . . .
H15C H 0.4549 -0.0590 0.1924 0.076 Uiso 1 1 calc R U . . .
C16 C 0.2310(8) 0.0572(6) 0.0262(4) 0.0492(16) Uani 1 1 d . . . . .
H16A H 0.3073 0.1149 0.0143 0.074 Uiso 1 1 calc R U . . .
H16B H 0.1377 0.1011 0.0175 0.074 Uiso 1 1 calc R U . . .
H16C H 0.2169 -0.0212 -0.0109 0.074 Uiso 1 1 calc R U . . .
C17 C 0.5765(5) 0.2127(4) 0.2449(3) 0.0223(10) Uani 1 1 d . . . . .
H17A H 0.5956 0.1255 0.2630 0.033 Uiso 1 1 calc R U . . .
H17B H 0.6383 0.2758 0.2861 0.033 Uiso 1 1 calc R U . . .
H17C H 0.6004 0.2205 0.1915 0.033 Uiso 1 1 calc R U . . .
Se2 Se 0.63828(5) 0.98406(5) 0.65482(3) 0.02824(12) Uani 1 1 d . . . . .
P3 P 0.56259(11) 0.86883(11) 0.73513(7) 0.0159(2) Uani 1 1 d . . . . .
P4 P 0.72775(12) 0.73379(11) 0.83506(7) 0.0158(2) Uani 1 1 d . . . . .
N5 N 0.6575(4) 0.8784(3) 0.8371(2) 0.0162(7) Uani 1 1 d . . . . .
N6 N 0.6199(4) 0.7142(3) 0.7395(2) 0.0176(8) Uani 1 1 d . . . . .
N7 N 0.3870(4) 0.8723(4) 0.7300(2) 0.0174(7) Uani 1 1 d . . . . .
H7N H 0.3602 0.8295 0.7705 0.021 Uiso 1 1 d R U . . .
N8 N 0.6905(4) 0.6404(3) 0.9007(2) 0.0177(8) Uani 1 1 d . . . . .
H8N H 0.5982 0.6629 0.9029 0.021 Uiso 1 1 d R U . . .
C18 C 0.6947(5) 0.9906(4) 0.9004(3) 0.0235(10) Uani 1 1 d . . . . .
C19 C 0.5568(6) 1.0667(5) 0.8936(3) 0.0330(12) Uani 1 1 d . . . . .
H19A H 0.5270 1.1001 0.8385 0.049 Uiso 1 1 calc R U . . .
H19B H 0.5778 1.1388 0.9359 0.049 Uiso 1 1 calc R U . . .
H19C H 0.4765 1.0102 0.9022 0.049 Uiso 1 1 calc R U . . .
C20 C 0.7402(6) 0.9368(5) 0.9863(3) 0.0341(13) Uani 1 1 d . . . . .
H20A H 0.6601 0.8791 0.9939 0.051 Uiso 1 1 calc R U . . .
H20B H 0.7596 1.0083 1.0290 0.051 Uiso 1 1 calc R U . . .
H20C H 0.8300 0.8888 0.9909 0.051 Uiso 1 1 calc R U . . .
C21 C 0.8210(6) 1.0755(5) 0.8857(3) 0.0383(13) Uani 1 1 d . . . . .
H21A H 0.9061 1.0230 0.8855 0.057 Uiso 1 1 calc R U . . .
H21B H 0.8496 1.1444 0.9300 0.057 Uiso 1 1 calc R U . . .
H21C H 0.7884 1.1136 0.8321 0.057 Uiso 1 1 calc R U . . .
C22 C 0.6093(5) 0.6097(5) 0.6733(3) 0.0276(11) Uani 1 1 d . . . . .
C23 C 0.4549(5) 0.6088(5) 0.6146(3) 0.0316(11) Uani 1 1 d . . . . .
H23A H 0.3803 0.6011 0.6463 0.047 Uiso 1 1 calc R U . . .
H23B H 0.4418 0.5354 0.5735 0.047 Uiso 1 1 calc R U . . .
H23C H 0.4437 0.6893 0.5862 0.047 Uiso 1 1 calc R U . . .
C24 C 0.7271(6) 0.6324(6) 0.6259(3) 0.0438(15) Uani 1 1 d . . . . .
H24A H 0.7175 0.7180 0.6038 0.066 Uiso 1 1 calc R U . . .
H24B H 0.7137 0.5663 0.5801 0.066 Uiso 1 1 calc R U . . .
H24C H 0.8257 0.6276 0.6634 0.066 Uiso 1 1 calc R U . . .
C25 C 0.6261(7) 0.4811(5) 0.7133(3) 0.0447(15) Uani 1 1 d . . . . .
H25A H 0.7249 0.4796 0.7511 0.067 Uiso 1 1 calc R U . . .
H25B H 0.6132 0.4107 0.6702 0.067 Uiso 1 1 calc R U . . .
H25C H 0.5509 0.4702 0.7444 0.067 Uiso 1 1 calc R U . . .
C26 C 0.2611(5) 0.9369(5) 0.6759(3) 0.0245(10) Uani 1 1 d . . . . .
C27 C 0.2855(6) 1.0829(5) 0.6850(3) 0.0334(12) Uani 1 1 d . . . . .
H27A H 0.2922 1.1134 0.7425 0.050 Uiso 1 1 calc R U . . .
H27B H 0.2024 1.1220 0.6480 0.050 Uiso 1 1 calc R U . . .
H27C H 0.3777 1.1073 0.6706 0.050 Uiso 1 1 calc R U . . .
C28 C 0.1260(5) 0.8975(6) 0.7073(3) 0.0366(13) Uani 1 1 d . . . . .
H28A H 0.1143 0.8032 0.7048 0.055 Uiso 1 1 calc R U . . .
H28B H 0.0370 0.9322 0.6724 0.055 Uiso 1 1 calc R U . . .
H28C H 0.1405 0.9321 0.7647 0.055 Uiso 1 1 calc R U . . .
C29 C 0.2346(5) 0.8878(5) 0.5855(3) 0.0314(12) Uani 1 1 d . . . . .
H29A H 0.3242 0.9049 0.5667 0.047 Uiso 1 1 calc R U . . .
H29B H 0.1523 0.9321 0.5516 0.047 Uiso 1 1 calc R U . . .
H29C H 0.2103 0.7947 0.5802 0.047 Uiso 1 1 calc R U . . .
C30 C 0.7670(4) 0.5448(4) 0.9601(3) 0.0174(9) Uani 1 1 d . . . . .
C31 C 0.6516(5) 0.4366(4) 0.9554(3) 0.0257(10) Uani 1 1 d . . . . .
H31A H 0.5629 0.4722 0.9674 0.039 Uiso 1 1 calc R U . . .
H31B H 0.6915 0.3742 0.9961 0.039 Uiso 1 1 calc R U . . .
H31C H 0.6257 0.3933 0.8997 0.039 Uiso 1 1 calc R U . . .
C32 C 0.9022(5) 0.4913(5) 0.9372(3) 0.0305(13) Uani 1 1 d . . . . .
H32A H 0.8749 0.4583 0.8790 0.046 Uiso 1 1 calc R U . . .
H32B H 0.9387 0.4212 0.9725 0.046 Uiso 1 1 calc R U . . .
H32C H 0.9799 0.5601 0.9453 0.046 Uiso 1 1 calc R U . . .
C33 C 0.8121(5) 0.6114(5) 1.0470(3) 0.0252(10) Uani 1 1 d . . . . .
H33A H 0.8896 0.6787 1.0496 0.038 Uiso 1 1 calc R U . . .
H33B H 0.8498 0.5479 1.0873 0.038 Uiso 1 1 calc R U . . .
H33C H 0.7259 0.6505 1.0598 0.038 Uiso 1 1 calc R U . . .
C34 C 0.9186(5) 0.7405(5) 0.8378(3) 0.0294(12) Uani 1 1 d . . . . .
H34A H 0.9767 0.7664 0.8942 0.044 Uiso 1 1 calc R U . . .
H34B H 0.9378 0.8036 0.7998 0.044 Uiso 1 1 calc R U . . .
H34C H 0.9469 0.6552 0.8209 0.044 Uiso 1 1 calc R U . . .
C35 C 0.0841(5) 0.3345(5) 0.7581(3) 0.0262(10) Uani 1 1 d . . . . .
C36 C 0.1358(6) 0.4319(5) 0.7187(3) 0.0323(13) Uani 1 1 d . . . . .
H36 H 0.2156 0.4885 0.7487 0.039 Uiso 1 1 calc R U . . .
C37 C 0.0725(6) 0.4483(5) 0.6351(3) 0.0381(13) Uani 1 1 d . . . . .
H37 H 0.1108 0.5145 0.6082 0.046 Uiso 1 1 calc R U . . .
C38 C -0.0457(5) 0.3688(5) 0.5917(3) 0.0304(11) Uani 1 1 d . . . . .
H38 H -0.0895 0.3807 0.5350 0.036 Uiso 1 1 calc R U . . .
C39 C -0.0997(5) 0.2731(5) 0.6301(3) 0.0279(11) Uani 1 1 d . . . . .
H39 H -0.1813 0.2182 0.6001 0.033 Uiso 1 1 calc R U . . .
C40 C -0.0358(5) 0.2557(5) 0.7128(3) 0.0275(11) Uani 1 1 d . . . . .
H40 H -0.0745 0.1888 0.7390 0.033 Uiso 1 1 calc R U . . .
C41 C 0.1568(6) 0.3137(6) 0.8469(3) 0.0375(13) Uani 1 1 d . . . . .
H41A H 0.2454 0.2645 0.8499 0.056 Uiso 1 1 calc R U . . .
H41B H 0.0875 0.2655 0.8709 0.056 Uiso 1 1 calc R U . . .
H41C H 0.1850 0.3974 0.8780 0.056 Uiso 1 1 calc R U . . .
C42 C 0.7976(5) 0.9203(4) 0.3034(3) 0.0201(9) Uani 1 1 d . . . . .
C43 C 0.7126(5) 0.8485(4) 0.3441(3) 0.0248(10) Uani 1 1 d . . . . .
H43 H 0.6468 0.7804 0.3144 0.030 Uiso 1 1 calc R U . . .
C44 C 0.7230(5) 0.8753(5) 0.4272(3) 0.0289(11) Uani 1 1 d . . . . .
H44 H 0.6646 0.8253 0.4543 0.035 Uiso 1 1 calc R U . . .
C45 C 0.8170(5) 0.9735(5) 0.4712(3) 0.0279(11) Uani 1 1 d . . . . .
H45 H 0.8249 0.9904 0.5286 0.033 Uiso 1 1 calc R U . . .
C46 C 0.9010(5) 1.0485(5) 0.4312(3) 0.0267(10) Uani 1 1 d . . . . .
H46 H 0.9654 1.1174 0.4610 0.032 Uiso 1 1 calc R U . . .
C47 C 0.8893(5) 1.0212(5) 0.3473(3) 0.0227(10) Uani 1 1 d . . . . .
H47 H 0.9454 1.0727 0.3197 0.027 Uiso 1 1 calc R U . . .
C48 C 0.7931(5) 0.8869(5) 0.2136(3) 0.0271(10) Uani 1 1 d . . . . .
H48A H 0.8836 0.8446 0.2102 0.041 Uiso 1 1 calc R U . . .
H48B H 0.7857 0.9660 0.1838 0.041 Uiso 1 1 calc R U . . .
H48C H 0.7069 0.8285 0.1887 0.041 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
Se1 P1 2.0797(11) . ?
P1 N3 1.618(3) . ?
P1 N1 1.703(3) . ?
P1 N2 1.713(3) . ?
P2 N4 1.592(4) . ?
P2 N1 1.652(4) . ?
P2 N2 1.660(3) . ?
P2 C17 1.770(4) . ?
N1 C1 1.498(6) . ?
N2 C5 1.496(5) . ?
N3 C9 1.506(5) . ?
N3 H3N 0.9100 . ?
N4 C13 1.511(6) . ?
N4 H4N 0.9100 . ?
C1 C2 1.522(6) . ?
C1 C3 1.522(6) . ?
C1 C4 1.529(6) . ?
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 1.526(7) . ?
C5 C8 1.527(6) . ?
C5 C6 1.535(6) . ?
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 1.521(6) . ?
C9 C11 1.523(6) . ?
C9 C12 1.528(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 C15 1.482(7) . ?
C13 C14 1.515(7) . ?
C13 C16 1.540(7) . ?
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 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
Se2 P3 2.0808(12) . ?
P3 N7 1.623(3) . ?
P3 N5 1.706(3) . ?
P3 N6 1.711(4) . ?
P4 N8 1.598(4) . ?
P4 N6 1.657(4) . ?
P4 N5 1.662(4) . ?
P4 C34 1.771(5) . ?
N5 C18 1.500(5) . ?
N6 C22 1.488(6) . ?
N7 C26 1.497(5) . ?
N7 H7N 0.9100 . ?
N8 C30 1.511(5) . ?
N8 H8N 0.9099 . ?
C18 C19 1.519(7) . ?
C18 C21 1.526(6) . ?
C18 C20 1.533(6) . ?
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 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C25 1.522(7) . ?
C22 C23 1.526(6) . ?
C22 C24 1.528(7) . ?
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 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.519(7) . ?
C26 C29 1.522(7) . ?
C26 C28 1.535(7) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
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 C31 1.516(6) . ?
C30 C32 1.522(6) . ?
C30 C33 1.525(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.375(7) . ?
C35 C40 1.393(7) . ?
C35 C41 1.500(7) . ?
C36 C37 1.395(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.377(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.361(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.385(7) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C47 1.381(6) . ?
C42 C43 1.392(6) . ?
C42 C48 1.511(6) . ?
C43 C44 1.379(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.372(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.395(7) . ?
C45 H45 0.9500 . ?
C46 C47 1.391(6) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 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
N3 P1 N1 108.81(17) . . ?
N3 P1 N2 110.04(17) . . ?
N1 P1 N2 81.95(16) . . ?
N3 P1 Se1 116.48(13) . . ?
N1 P1 Se1 117.60(12) . . ?
N2 P1 Se1 116.97(12) . . ?
N4 P2 N1 114.10(18) . . ?
N4 P2 N2 115.72(18) . . ?
N1 P2 N2 85.12(17) . . ?
N4 P2 C17 113.6(2) . . ?
N1 P2 C17 113.1(2) . . ?
N2 P2 C17 112.2(2) . . ?
C1 N1 P2 131.2(3) . . ?
C1 N1 P1 131.0(3) . . ?
P2 N1 P1 96.53(18) . . ?
C5 N2 P2 131.1(3) . . ?
C5 N2 P1 130.8(3) . . ?
P2 N2 P1 95.86(17) . . ?
C9 N3 P1 134.4(3) . . ?
C9 N3 H3N 103.5 . . ?
P1 N3 H3N 121.7 . . ?
C13 N4 P2 140.1(3) . . ?
C13 N4 H4N 112.9 . . ?
P2 N4 H4N 107.0 . . ?
N1 C1 C2 110.2(4) . . ?
N1 C1 C3 108.9(4) . . ?
C2 C1 C3 110.2(4) . . ?
N1 C1 C4 108.0(4) . . ?
C2 C1 C4 110.5(4) . . ?
C3 C1 C4 109.0(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 . . ?
N2 C5 C7 107.8(3) . . ?
N2 C5 C8 111.0(4) . . ?
C7 C5 C8 110.1(4) . . ?
N2 C5 C6 107.8(4) . . ?
C7 C5 C6 110.0(4) . . ?
C8 C5 C6 110.2(4) . . ?
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 110.6(4) . . ?
N3 C9 C11 105.9(4) . . ?
C10 C9 C11 109.3(4) . . ?
N3 C9 C12 111.2(4) . . ?
C10 C9 C12 110.3(4) . . ?
C11 C9 C12 109.5(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 . . ?
C15 C13 N4 113.6(4) . . ?
C15 C13 C14 111.1(5) . . ?
N4 C13 C14 106.2(4) . . ?
C15 C13 C16 111.3(5) . . ?
N4 C13 C16 107.8(4) . . ?
C14 C13 C16 106.5(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 . . ?
P2 C17 H17A 109.5 . . ?
P2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N7 P3 N5 108.41(18) . . ?
N7 P3 N6 111.15(19) . . ?
N5 P3 N6 82.26(17) . . ?
N7 P3 Se2 115.70(14) . . ?
N5 P3 Se2 118.37(13) . . ?
N6 P3 Se2 116.37(13) . . ?
N8 P4 N6 116.34(19) . . ?
N8 P4 N5 114.52(18) . . ?
N6 P4 N5 85.25(18) . . ?
N8 P4 C34 112.2(2) . . ?
N6 P4 C34 112.7(2) . . ?
N5 P4 C34 113.4(2) . . ?
C18 N5 P4 131.4(3) . . ?
C18 N5 P3 131.2(3) . . ?
P4 N5 P3 95.85(18) . . ?
C22 N6 P4 131.0(3) . . ?
C22 N6 P3 131.3(3) . . ?
P4 N6 P3 95.84(18) . . ?
C26 N7 P3 133.7(3) . . ?
C26 N7 H7N 113.0 . . ?
P3 N7 H7N 113.2 . . ?
C30 N8 P4 138.8(3) . . ?
C30 N8 H8N 118.3 . . ?
P4 N8 H8N 102.6 . . ?
N5 C18 C19 108.2(4) . . ?
N5 C18 C21 110.2(4) . . ?
C19 C18 C21 110.7(4) . . ?
N5 C18 C20 107.9(4) . . ?
C19 C18 C20 109.5(4) . . ?
C21 C18 C20 110.3(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 C25 108.4(4) . . ?
N6 C22 C23 107.9(4) . . ?
C25 C22 C23 108.2(5) . . ?
N6 C22 C24 110.7(4) . . ?
C25 C22 C24 111.3(4) . . ?
C23 C22 C24 110.2(4) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N7 C26 C27 111.6(4) . . ?
N7 C26 C29 111.3(4) . . ?
C27 C26 C29 110.7(4) . . ?
N7 C26 C28 104.5(4) . . ?
C27 C26 C28 109.6(4) . . ?
C29 C26 C28 109.0(4) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N8 C30 C31 105.2(3) . . ?
N8 C30 C32 113.0(4) . . ?
C31 C30 C32 109.9(4) . . ?
N8 C30 C33 108.3(3) . . ?
C31 C30 C33 110.5(4) . . ?
C32 C30 C33 109.9(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
P4 C34 H34A 109.5 . . ?
P4 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
P4 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C40 118.0(5) . . ?
C36 C35 C41 120.5(5) . . ?
C40 C35 C41 121.5(5) . . ?
C35 C36 C37 120.7(5) . . ?
C35 C36 H36 119.6 . . ?
C37 C36 H36 119.6 . . ?
C38 C37 C36 120.1(5) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C39 C38 C37 120.0(5) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C38 C39 C40 120.0(5) . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
C39 C40 C35 121.2(5) . . ?
C39 C40 H40 119.4 . . ?
C35 C40 H40 119.4 . . ?
C35 C41 H41A 109.5 . . ?
C35 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C35 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C47 C42 C43 118.7(4) . . ?
C47 C42 C48 120.4(4) . . ?
C43 C42 C48 120.9(4) . . ?
C44 C43 C42 120.6(4) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C45 C44 C43 120.6(5) . . ?
C45 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
C44 C45 C46 119.8(5) . . ?
C44 C45 H45 120.1 . . ?
C46 C45 H45 120.1 . . ?
C47 C46 C45 119.2(4) . . ?
C47 C46 H46 120.4 . . ?
C45 C46 H46 120.4 . . ?
C42 C47 C46 121.1(4) . . ?
C42 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
C42 C48 H48A 109.5 . . ?
C42 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C42 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 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
N3 H3N I2 0.91 2.78 3.668(3) 164 1_455
N4 H4N I2 0.91 2.65 3.559(3) 172 1_455
N7 H7N I1 0.91 2.88 3.775(4) 170 .
N8 H8N I1 0.91 2.65 3.561(3) 175 .

_refine_diff_density_max         0.909
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.079

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 991947'
#######################################################################
#
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  from this site to visualise CIF-encoded structures and 
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data_msb310_sq_s

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
4-[1,3-di-tert-butyl-4-(4,4-dimethylpiperazin-4-ium-1-
yl)-2,4-diselanylidene-1,3,2λ⁵,4λ⁵-diazadiphosphedin-2-
yl]-1,1-dimethylpiperazin-1-ium iodide hydrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H94 N12 P4 Se4, O, 4I'
_chemical_formula_sum            'C40 H94 I4 N12 O P4 Se4'
_chemical_formula_weight         1706.59

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'
Se Se -0.0929 2.2259 '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           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

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

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

_cell_length_a                   32.556(3)
_cell_length_b                   9.5372(10)
_cell_length_c                   21.679(2)
_cell_angle_alpha                90
_cell_angle_beta                 107.558(2)
_cell_angle_gamma                90
_cell_volume                     6417.7(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9118
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      28.27

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_F_000             3336
_exptl_transmission_factor_min   0.551
_exptl_transmission_factor_max   0.727
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.134
_exptl_absorpt_coefficient_mu    4.350
_shelx_estimated_absorpt_T_min   0.548
_shelx_estimated_absorpt_T_max   0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5483
_exptl_absorpt_correction_T_max  0.5933
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'

_exptl_special_details           
; 
 The diffraction data were obtained from 3 sets of 400 frames,
 each of width 0.5° in ω, colllected 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°.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            110101
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.011
_diffrn_reflns_theta_max         28.333
_diffrn_reflns_theta_full        28.300
_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             15994
_reflns_number_gt                13166
_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       'Bruker SMART (Bruker, 2000)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2000a)'
_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. No H-atoms could be found in difference maps
 for the solvent water molecule. Residual density due possibly to partial 
occupancy or disordered additional water in the latticce was removed with 
PLATON SQUEEZE (Spek, 2013).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0421P)²+13.9217P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15994
_refine_ls_number_parameters     606
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1038
_refine_ls_wR_factor_gt          0.0987
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_restrained_S_all      1.151
_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
I1 I 0.48502(2) 0.35559(3) 0.37015(2) 0.02111(8) Uani 1 1 d . . . . .
I2 I 0.40198(2) 0.89222(4) 0.14135(2) 0.02047(8) Uani 1 1 d . . . . .
I3 I 0.99778(2) 0.27570(3) 0.10500(2) 0.01694(7) Uani 1 1 d . . . . .
I4 I 0.10050(2) 0.25292(3) 0.75221(2) 0.01661(7) Uani 1 1 d . . . . .
Se1 Se 0.25067(2) 0.33746(5) 0.26265(3) 0.01617(11) Uani 1 1 d . . . . .
Se2 Se 0.29778(2) -0.11329(6) 0.37659(3) 0.02315(12) Uani 1 1 d . . . . .
P1 P 0.30665(4) 0.22658(13) 0.26743(6) 0.0110(2) Uani 1 1 d . . . . .
P2 P 0.33262(4) 0.00491(13) 0.32921(6) 0.0115(2) Uani 1 1 d . . . . .
N1 N 0.30665(12) 0.0549(4) 0.25172(19) 0.0119(8) Uani 1 1 d . . . . .
N2 N 0.33975(12) 0.1788(4) 0.34173(19) 0.0108(8) Uani 1 1 d . . . . .
N3 N 0.33381(12) 0.3059(4) 0.22362(19) 0.0127(8) Uani 1 1 d . . . . .
N4 N 0.38049(13) 0.4375(4) 0.1440(2) 0.0151(8) Uani 1 1 d . . . . .
N5 N 0.38025(12) -0.0672(4) 0.3385(2) 0.0129(8) Uani 1 1 d . . . . .
N6 N 0.46539(13) -0.1941(4) 0.38172(19) 0.0130(8) Uani 1 1 d . . . . .
C1 C 0.27770(15) -0.0290(5) 0.1969(2) 0.0149(10) Uani 1 1 d . . . . .
C2 C 0.27934(16) 0.0373(5) 0.1340(2) 0.0166(10) Uani 1 1 d . . . . .
H2A H 0.3087 0.0308 0.1310 0.025 Uiso 1 1 calc R U . . .
H2B H 0.2709 0.1361 0.1331 0.025 Uiso 1 1 calc R U . . .
H2C H 0.2595 -0.0121 0.0974 0.025 Uiso 1 1 calc R U . . .
C3 C 0.23168(15) -0.0329(5) 0.2010(3) 0.0208(11) Uani 1 1 d . . . . .
H3A H 0.2135 -0.0878 0.1648 0.031 Uiso 1 1 calc R U . . .
H3B H 0.2204 0.0629 0.1989 0.031 Uiso 1 1 calc R U . . .
H3C H 0.2316 -0.0764 0.2420 0.031 Uiso 1 1 calc R U . . .
C4 C 0.29599(16) -0.1776(5) 0.2020(3) 0.0196(11) Uani 1 1 d . . . . .
H4A H 0.3259 -0.1740 0.2012 0.029 Uiso 1 1 calc R U . . .
H4B H 0.2788 -0.2338 0.1655 0.029 Uiso 1 1 calc R U . . .
H4C H 0.2950 -0.2204 0.2427 0.029 Uiso 1 1 calc R U . . .
C5 C 0.35133(15) 0.2600(5) 0.4044(2) 0.0149(10) Uani 1 1 d . . . . .
C6 C 0.31425(16) 0.2581(6) 0.4337(2) 0.0195(11) Uani 1 1 d . . . . .
H6A H 0.2884 0.2972 0.4026 0.029 Uiso 1 1 calc R U . . .
H6B H 0.3219 0.3145 0.4733 0.029 Uiso 1 1 calc R U . . .
H6C H 0.3086 0.1613 0.4440 0.029 Uiso 1 1 calc R U . . .
C7 C 0.36147(16) 0.4093(5) 0.3889(2) 0.0174(10) Uani 1 1 d . . . . .
H7A H 0.3843 0.4078 0.3681 0.026 Uiso 1 1 calc R U . . .
H7B H 0.3711 0.4638 0.4290 0.026 Uiso 1 1 calc R U . . .
H7C H 0.3355 0.4524 0.3597 0.026 Uiso 1 1 calc R U . . .
C8 C 0.39169(16) 0.1925(6) 0.4507(2) 0.0182(10) Uani 1 1 d . . . . .
H8A H 0.3868 0.0919 0.4541 0.027 Uiso 1 1 calc R U . . .
H8B H 0.3979 0.2359 0.4935 0.027 Uiso 1 1 calc R U . . .
H8C H 0.4162 0.2067 0.4340 0.027 Uiso 1 1 calc R U . . .
C9 C 0.37335(15) 0.2424(5) 0.2180(2) 0.0138(9) Uani 1 1 d . . . . .
H9A H 0.3717 0.1392 0.2216 0.017 Uiso 1 1 calc R U . . .
H9B H 0.3983 0.2760 0.2537 0.017 Uiso 1 1 calc R U . . .
C10 C 0.37975(17) 0.2806(5) 0.1533(2) 0.0164(10) Uani 1 1 d . . . . .
H10A H 0.4072 0.2400 0.1510 0.020 Uiso 1 1 calc R U . . .
H10B H 0.3561 0.2394 0.1179 0.020 Uiso 1 1 calc R U . . .
C11 C 0.33919(16) 0.4969(5) 0.1516(3) 0.0182(10) Uani 1 1 d . . . . .
H11A H 0.3398 0.6004 0.1481 0.022 Uiso 1 1 calc R U . . .
H11B H 0.3145 0.4620 0.1158 0.022 Uiso 1 1 calc R U . . .
C12 C 0.33253(16) 0.4581(5) 0.2149(2) 0.0166(10) Uani 1 1 d . . . . .
H12A H 0.3553 0.5021 0.2507 0.020 Uiso 1 1 calc R U . . .
H12B H 0.3043 0.4944 0.2163 0.020 Uiso 1 1 calc R U . . .
C13 C 0.41951(16) 0.5001(6) 0.1916(3) 0.0235(12) Uani 1 1 d . . . . .
H13A H 0.4197 0.6017 0.1849 0.035 Uiso 1 1 calc R U . . .
H13B H 0.4455 0.4587 0.1855 0.035 Uiso 1 1 calc R U . . .
H13C H 0.4188 0.4810 0.2357 0.035 Uiso 1 1 calc R U . . .
C14 C 0.38288(19) 0.4674(6) 0.0776(2) 0.0239(12) Uani 1 1 d . . . . .
H14A H 0.3815 0.5689 0.0703 0.036 Uiso 1 1 calc R U . . .
H14B H 0.3586 0.4220 0.0456 0.036 Uiso 1 1 calc R U . . .
H14C H 0.4100 0.4309 0.0734 0.036 Uiso 1 1 calc R U . . .
C15 C 0.41764(14) 0.0063(5) 0.3296(2) 0.0131(9) Uani 1 1 d . . . . .
H15A H 0.4136 0.1088 0.3320 0.016 Uiso 1 1 calc R U . . .
H15B H 0.4203 -0.0158 0.2863 0.016 Uiso 1 1 calc R U . . .
C16 C 0.45859(15) -0.0381(5) 0.3817(2) 0.0148(10) Uani 1 1 d . . . . .
H16A H 0.4836 0.0100 0.3742 0.018 Uiso 1 1 calc R U . . .
H16B H 0.4567 -0.0087 0.4245 0.018 Uiso 1 1 calc R U . . .
C17 C 0.42609(15) -0.2675(5) 0.3886(3) 0.0172(10) Uani 1 1 d . . . . .
H17A H 0.4231 -0.2471 0.4319 0.021 Uiso 1 1 calc R U . . .
H17B H 0.4296 -0.3701 0.3854 0.021 Uiso 1 1 calc R U . . .
C18 C 0.38555(16) -0.2207(5) 0.3368(3) 0.0170(10) Uani 1 1 d . . . . .
H18A H 0.3873 -0.2489 0.2937 0.020 Uiso 1 1 calc R U . . .
H18B H 0.3602 -0.2674 0.3438 0.020 Uiso 1 1 calc R U . . .
C19 C 0.47600(17) -0.2385(5) 0.3218(2) 0.0187(10) Uani 1 1 d . . . . .
H19A H 0.4818 -0.3395 0.3236 0.028 Uiso 1 1 calc R U . . .
H19B H 0.5016 -0.1877 0.3190 0.028 Uiso 1 1 calc R U . . .
H19C H 0.4516 -0.2174 0.2836 0.028 Uiso 1 1 calc R U . . .
C20 C 0.50321(16) -0.2314(6) 0.4389(3) 0.0200(11) Uani 1 1 d . . . . .
H20A H 0.4969 -0.2066 0.4789 0.030 Uiso 1 1 calc R U . . .
H20B H 0.5287 -0.1797 0.4365 0.030 Uiso 1 1 calc R U . . .
H20C H 0.5088 -0.3324 0.4385 0.030 Uiso 1 1 calc R U . . .
Se3 Se 0.18142(2) 0.24557(6) 1.08451(2) 0.01749(11) Uani 1 1 d . . . . .
Se4 Se 0.23364(2) 0.70624(5) 1.02272(2) 0.01535(11) Uani 1 1 d . . . . .
P3 P 0.15105(4) 0.36947(12) 1.00504(6) 0.0098(2) Uani 1 1 d . . . . .
P4 P 0.17902(4) 0.59385(13) 0.97218(6) 0.0102(2) Uani 1 1 d . . . . .
N7 N 0.18098(12) 0.4221(4) 0.95671(18) 0.0096(8) Uani 1 1 d . . . . .
N8 N 0.14346(12) 0.5423(4) 1.01183(18) 0.0101(8) Uani 1 1 d . . . . .
N9 N 0.10392(12) 0.3002(4) 0.9642(2) 0.0134(8) Uani 1 1 d . . . . .
N10 N 0.01923(12) 0.1746(4) 0.91081(19) 0.0119(8) Uani 1 1 d . . . . .
N11 N 0.15512(13) 0.6720(4) 0.90237(19) 0.0123(8) Uani 1 1 d . . . . .
N12 N 0.11982(12) 0.7995(4) 0.7754(2) 0.0132(8) Uani 1 1 d . . . . .
C21 C 0.21357(14) 0.3413(5) 0.9347(2) 0.0131(9) Uani 1 1 d . . . . .
C22 C 0.21849(15) 0.4126(5) 0.8744(2) 0.0145(10) Uani 1 1 d . . . . .
H22A H 0.2257 0.5117 0.8837 0.022 Uiso 1 1 calc R U . . .
H22B H 0.1914 0.4052 0.8391 0.022 Uiso 1 1 calc R U . . .
H22C H 0.2416 0.3667 0.8615 0.022 Uiso 1 1 calc R U . . .
C23 C 0.25715(15) 0.3382(6) 0.9884(2) 0.0172(10) Uani 1 1 d . . . . .
H23A H 0.2688 0.4335 0.9962 0.026 Uiso 1 1 calc R U . . .
H23B H 0.2773 0.2782 0.9749 0.026 Uiso 1 1 calc R U . . .
H23C H 0.2530 0.3009 1.0282 0.026 Uiso 1 1 calc R U . . .
C24 C 0.19628(15) 0.1933(5) 0.9184(2) 0.0140(10) Uani 1 1 d . . . . .
H24A H 0.2159 0.1398 0.9009 0.021 Uiso 1 1 calc R U . . .
H24B H 0.1678 0.1974 0.8862 0.021 Uiso 1 1 calc R U . . .
H24C H 0.1940 0.1474 0.9577 0.021 Uiso 1 1 calc R U . . .
C25 C 0.13068(15) 0.6174(5) 1.0643(2) 0.0130(9) Uani 1 1 d . . . . .
C26 C 0.16687(15) 0.6111(6) 1.1290(2) 0.0201(11) Uani 1 1 d . . . . .
H26A H 0.1726 0.5131 1.1424 0.030 Uiso 1 1 calc R U . . .
H26B H 0.1580 0.6626 1.1620 0.030 Uiso 1 1 calc R U . . .
H26C H 0.1930 0.6536 1.1238 0.030 Uiso 1 1 calc R U . . .
C27 C 0.09055(16) 0.5458(5) 1.0719(2) 0.0178(10) Uani 1 1 d . . . . .
H27A H 0.0665 0.5589 1.0323 0.027 Uiso 1 1 calc R U . . .
H27B H 0.0832 0.5871 1.1086 0.027 Uiso 1 1 calc R U . . .
H27C H 0.0962 0.4453 1.0796 0.027 Uiso 1 1 calc R U . . .
C28 C 0.12092(16) 0.7699(5) 1.0432(3) 0.0179(10) Uani 1 1 d . . . . .
H28A H 0.1470 0.8142 1.0384 0.027 Uiso 1 1 calc R U . . .
H28B H 0.1115 0.8205 1.0758 0.027 Uiso 1 1 calc R U . . .
H28C H 0.0981 0.7727 1.0016 0.027 Uiso 1 1 calc R U . . .
C29 C 0.09890(15) 0.1474(5) 0.9574(3) 0.0155(10) Uani 1 1 d . . . . .
H29A H 0.1218 0.1009 0.9921 0.019 Uiso 1 1 calc R U . . .
H29B H 0.1021 0.1181 0.9153 0.019 Uiso 1 1 calc R U . . .
C30 C 0.05544(14) 0.1021(5) 0.9614(2) 0.0147(10) Uani 1 1 d . . . . .
H30A H 0.0533 0.1241 1.0049 0.018 Uiso 1 1 calc R U . . .
H30B H 0.0525 -0.0006 0.9552 0.018 Uiso 1 1 calc R U . . .
C31 C 0.02570(14) 0.3303(5) 0.9195(2) 0.0118(9) Uani 1 1 d . . . . .
H31A H 0.0225 0.3580 0.9618 0.014 Uiso 1 1 calc R U . . .
H31B H 0.0031 0.3794 0.8852 0.014 Uiso 1 1 calc R U . . .
C32 C 0.06969(14) 0.3757(5) 0.9164(2) 0.0134(9) Uani 1 1 d . . . . .
H32A H 0.0718 0.3572 0.8725 0.016 Uiso 1 1 calc R U . . .
H32B H 0.0733 0.4778 0.9246 0.016 Uiso 1 1 calc R U . . .
C33 C 0.01679(16) 0.1297(5) 0.8434(2) 0.0171(10) Uani 1 1 d . . . . .
H33A H 0.0431 0.1590 0.8338 0.026 Uiso 1 1 calc R U . . .
H33B H -0.0083 0.1735 0.8125 0.026 Uiso 1 1 calc R U . . .
H33C H 0.0140 0.0275 0.8400 0.026 Uiso 1 1 calc R U . . .
C34 C -0.02259(14) 0.1354(5) 0.9221(2) 0.0150(10) Uani 1 1 d . . . . .
H34A H -0.0258 0.0332 0.9202 0.022 Uiso 1 1 calc R U . . .
H34B H -0.0465 0.1783 0.8886 0.022 Uiso 1 1 calc R U . . .
H34C H -0.0227 0.1691 0.9647 0.022 Uiso 1 1 calc R U . . .
C35 C 0.12012(15) 0.6034(5) 0.8520(2) 0.0130(9) Uani 1 1 d . . . . .
H35A H 0.0920 0.6318 0.8569 0.016 Uiso 1 1 calc R U . . .
H35B H 0.1228 0.5004 0.8574 0.016 Uiso 1 1 calc R U . . .
C36 C 0.12173(15) 0.6432(5) 0.7850(2) 0.0135(9) Uani 1 1 d . . . . .
H36A H 0.1487 0.6067 0.7788 0.016 Uiso 1 1 calc R U . . .
H36B H 0.0972 0.5991 0.7521 0.016 Uiso 1 1 calc R U . . .
C37 C 0.15607(16) 0.8650(5) 0.8288(2) 0.0162(10) Uani 1 1 d . . . . .
H37A H 0.1840 0.8348 0.8240 0.019 Uiso 1 1 calc R U . . .
H37B H 0.1543 0.9683 0.8245 0.019 Uiso 1 1 calc R U . . .
C38 C 0.15421(17) 0.8243(5) 0.8952(2) 0.0155(10) Uani 1 1 d . . . . .
H38A H 0.1790 0.8658 0.9285 0.019 Uiso 1 1 calc R U . . .
H38B H 0.1275 0.8618 0.9018 0.019 Uiso 1 1 calc R U . . .
C39 C 0.07654(16) 0.8557(5) 0.7739(3) 0.0180(10) Uani 1 1 d . . . . .
H39A H 0.0758 0.9572 0.7666 0.027 Uiso 1 1 calc R U . . .
H39B H 0.0713 0.8361 0.8152 0.027 Uiso 1 1 calc R U . . .
H39C H 0.0542 0.8104 0.7388 0.027 Uiso 1 1 calc R U . . .
C40 C 0.12676(17) 0.8324(5) 0.7115(2) 0.0194(11) Uani 1 1 d . . . . .
H40A H 0.1246 0.9339 0.7041 0.029 Uiso 1 1 calc R U . . .
H40B H 0.1048 0.7847 0.6768 0.029 Uiso 1 1 calc R U . . .
H40C H 0.1554 0.8001 0.7119 0.029 Uiso 1 1 calc R U . . .
O1 O 0.43905(15) 0.8817(5) 0.5320(2) 0.0428(12) Uani 1 1 d . . . . .
H1OA H 0.4568 0.8425 0.5644 0.051 Uiso 1 1 d R U . . .
H1OB H 0.4213 0.9197 0.5487 0.051 Uiso 1 1 d 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
Se1 P1 2.0823(12) . ?
Se2 P2 2.0773(13) . ?
P1 N3 1.662(4) . ?
P1 N1 1.673(4) . ?
P1 N2 1.708(4) . ?
P2 N5 1.652(4) . ?
P2 N2 1.685(4) . ?
P2 N1 1.705(4) . ?
N1 C1 1.505(6) . ?
N2 C5 1.509(6) . ?
N3 C9 1.461(6) . ?
N3 C12 1.463(6) . ?
N4 C14 1.491(6) . ?
N4 C13 1.499(7) . ?
N4 C10 1.511(6) . ?
N4 C11 1.513(6) . ?
N5 C15 1.467(6) . ?
N5 C18 1.476(6) . ?
N6 C20 1.502(6) . ?
N6 C19 1.503(6) . ?
N6 C16 1.505(6) . ?
N6 C17 1.505(6) . ?
C1 C2 1.520(7) . ?
C1 C3 1.528(7) . ?
C1 C4 1.528(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 C7 1.522(7) . ?
C5 C6 1.525(6) . ?
C5 C8 1.533(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 1.523(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.500(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
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 1.524(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.520(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Se3 P3 2.0771(13) . ?
Se4 P4 2.0822(13) . ?
P3 N9 1.660(4) . ?
P3 N8 1.680(4) . ?
P3 N7 1.707(4) . ?
P4 N11 1.656(4) . ?
P4 N7 1.677(4) . ?
P4 N8 1.709(4) . ?
N7 C21 1.501(5) . ?
N8 C25 1.506(6) . ?
N9 C32 1.462(6) . ?
N9 C29 1.468(6) . ?
N10 C33 1.501(6) . ?
N10 C34 1.501(6) . ?
N10 C31 1.504(6) . ?
N10 C30 1.513(6) . ?
N11 C38 1.460(6) . ?
N11 C35 1.472(6) . ?
N12 C39 1.498(6) . ?
N12 C40 1.503(6) . ?
N12 C36 1.504(6) . ?
N12 C37 1.516(6) . ?
C21 C24 1.521(6) . ?
C21 C22 1.524(6) . ?
C21 C23 1.540(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 C27 1.526(6) . ?
C25 C28 1.529(7) . ?
C25 C26 1.536(7) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.507(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.517(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.517(6) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.509(7) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
O1 H1OA 0.8502 . ?
O1 H1OB 0.8499 . ?

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
N3 P1 N1 107.3(2) . . ?
N3 P1 N2 111.6(2) . . ?
N1 P1 N2 83.79(19) . . ?
N3 P1 Se1 110.42(14) . . ?
N1 P1 Se1 122.73(14) . . ?
N2 P1 Se1 118.44(14) . . ?
N5 P2 N2 108.2(2) . . ?
N5 P2 N1 113.9(2) . . ?
N2 P2 N1 83.51(19) . . ?
N5 P2 Se2 110.26(15) . . ?
N2 P2 Se2 121.57(14) . . ?
N1 P2 Se2 117.14(14) . . ?
C1 N1 P1 130.0(3) . . ?
C1 N1 P2 129.5(3) . . ?
P1 N1 P2 95.9(2) . . ?
C5 N2 P2 129.4(3) . . ?
C5 N2 P1 128.8(3) . . ?
P2 N2 P1 95.4(2) . . ?
C9 N3 C12 113.1(4) . . ?
C9 N3 P1 119.6(3) . . ?
C12 N3 P1 121.7(3) . . ?
C14 N4 C13 108.0(4) . . ?
C14 N4 C10 109.0(4) . . ?
C13 N4 C10 110.3(4) . . ?
C14 N4 C11 109.8(4) . . ?
C13 N4 C11 111.9(4) . . ?
C10 N4 C11 107.8(4) . . ?
C15 N5 C18 111.3(4) . . ?
C15 N5 P2 124.8(3) . . ?
C18 N5 P2 121.5(3) . . ?
C20 N6 C19 107.5(4) . . ?
C20 N6 C16 108.6(4) . . ?
C19 N6 C16 110.5(4) . . ?
C20 N6 C17 108.5(4) . . ?
C19 N6 C17 112.3(4) . . ?
C16 N6 C17 109.3(4) . . ?
N1 C1 C2 107.7(4) . . ?
N1 C1 C3 111.0(4) . . ?
C2 C1 C3 111.3(4) . . ?
N1 C1 C4 107.4(4) . . ?
C2 C1 C4 109.4(4) . . ?
C3 C1 C4 109.9(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 . . ?
N2 C5 C7 107.1(4) . . ?
N2 C5 C6 110.8(4) . . ?
C7 C5 C6 110.8(4) . . ?
N2 C5 C8 107.8(4) . . ?
C7 C5 C8 109.7(4) . . ?
C6 C5 C8 110.7(4) . . ?
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 110.3(4) . . ?
N3 C9 H9A 109.6 . . ?
C10 C9 H9A 109.6 . . ?
N3 C9 H9B 109.6 . . ?
C10 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N4 C10 C9 111.9(4) . . ?
N4 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
N4 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C12 C11 N4 112.7(4) . . ?
C12 C11 H11A 109.1 . . ?
N4 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
N4 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
N3 C12 C11 110.9(4) . . ?
N3 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N4 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N5 C15 C16 110.1(4) . . ?
N5 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
N5 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
N6 C16 C15 111.8(4) . . ?
N6 C16 H16A 109.3 . . ?
C15 C16 H16A 109.3 . . ?
N6 C16 H16B 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?
N6 C17 C18 111.4(4) . . ?
N6 C17 H17A 109.4 . . ?
C18 C17 H17A 109.4 . . ?
N6 C17 H17B 109.4 . . ?
C18 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
N5 C18 C17 110.8(4) . . ?
N5 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
N5 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
N6 C19 H19A 109.5 . . ?
N6 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N6 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 H20A 109.5 . . ?
N6 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N6 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N9 P3 N8 107.5(2) . . ?
N9 P3 N7 113.3(2) . . ?
N8 P3 N7 83.79(18) . . ?
N9 P3 Se3 110.38(15) . . ?
N8 P3 Se3 122.10(15) . . ?
N7 P3 Se3 117.33(14) . . ?
N11 P4 N7 107.0(2) . . ?
N11 P4 N8 112.7(2) . . ?
N7 P4 N8 83.80(19) . . ?
N11 P4 Se4 109.91(15) . . ?
N7 P4 Se4 122.01(14) . . ?
N8 P4 Se4 118.93(14) . . ?
C21 N7 P4 129.6(3) . . ?
C21 N7 P3 129.3(3) . . ?
P4 N7 P3 95.80(19) . . ?
C25 N8 P3 127.9(3) . . ?
C25 N8 P4 128.8(3) . . ?
P3 N8 P4 95.64(19) . . ?
C32 N9 C29 112.3(4) . . ?
C32 N9 P3 124.5(3) . . ?
C29 N9 P3 120.4(3) . . ?
C33 N10 C34 107.6(4) . . ?
C33 N10 C31 111.5(4) . . ?
C34 N10 C31 109.0(3) . . ?
C33 N10 C30 112.1(4) . . ?
C34 N10 C30 108.3(4) . . ?
C31 N10 C30 108.2(4) . . ?
C38 N11 C35 112.1(4) . . ?
C38 N11 P4 122.3(3) . . ?
C35 N11 P4 121.5(3) . . ?
C39 N12 C40 107.8(4) . . ?
C39 N12 C36 110.9(4) . . ?
C40 N12 C36 108.9(4) . . ?
C39 N12 C37 112.3(4) . . ?
C40 N12 C37 108.6(4) . . ?
C36 N12 C37 108.2(4) . . ?
N7 C21 C24 107.6(4) . . ?
N7 C21 C22 108.2(4) . . ?
C24 C21 C22 110.0(4) . . ?
N7 C21 C23 110.3(4) . . ?
C24 C21 C23 110.4(4) . . ?
C22 C21 C23 110.2(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 . . ?
N8 C25 C27 108.0(4) . . ?
N8 C25 C28 107.7(4) . . ?
C27 C25 C28 110.5(4) . . ?
N8 C25 C26 111.1(4) . . ?
C27 C25 C26 109.3(4) . . ?
C28 C25 C26 110.1(4) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N9 C29 C30 110.9(4) . . ?
N9 C29 H29A 109.5 . . ?
C30 C29 H29A 109.5 . . ?
N9 C29 H29B 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 108.0 . . ?
C29 C30 N10 111.5(4) . . ?
C29 C30 H30A 109.3 . . ?
N10 C30 H30A 109.3 . . ?
C29 C30 H30B 109.3 . . ?
N10 C30 H30B 109.3 . . ?
H30A C30 H30B 108.0 . . ?
N10 C31 C32 112.0(4) . . ?
N10 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
N10 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
N9 C32 C31 110.9(4) . . ?
N9 C32 H32A 109.5 . . ?
C31 C32 H32A 109.5 . . ?
N9 C32 H32B 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
N10 C33 H33A 109.5 . . ?
N10 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N10 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N10 C34 H34A 109.5 . . ?
N10 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N10 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N11 C35 C36 110.9(4) . . ?
N11 C35 H35A 109.5 . . ?
C36 C35 H35A 109.5 . . ?
N11 C35 H35B 109.5 . . ?
C36 C35 H35B 109.5 . . ?
H35A C35 H35B 108.1 . . ?
N12 C36 C35 111.6(4) . . ?
N12 C36 H36A 109.3 . . ?
C35 C36 H36A 109.3 . . ?
N12 C36 H36B 109.3 . . ?
C35 C36 H36B 109.3 . . ?
H36A C36 H36B 108.0 . . ?
C38 C37 N12 112.1(4) . . ?
C38 C37 H37A 109.2 . . ?
N12 C37 H37A 109.2 . . ?
C38 C37 H37B 109.2 . . ?
N12 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
N11 C38 C37 110.6(4) . . ?
N11 C38 H38A 109.5 . . ?
C37 C38 H38A 109.5 . . ?
N11 C38 H38B 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
N12 C39 H39A 109.5 . . ?
N12 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N12 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N12 C40 H40A 109.5 . . ?
N12 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N12 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
H1OA O1 H1OB 102.3 . . ?

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
C17 H17A O1 0.99 2.41 3.327(7) 154 1_545
C20 H20A O1 0.98 2.62 3.485(7) 147 1_545
O1 H1OA I1 0.85 2.75 3.545(4) 157 3_666
O1 H1OB I2 0.85 2.90 3.668(5) 151 4_576

_refine_diff_density_max         2.042
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.178

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 991948'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_msb319

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 1,3-Di-tert-butyl-2,4-diselenoxy-2λ⁵,4λ⁵-
[1,3,2,4]diazadiphosphetidin-2,4-di(yloxyethyl
trimethylammonium) Iodode Hydrate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H44 N4 O2 P2 Se2, 2(I), H2 O'
_chemical_formula_sum            'C18 H46 I2 N4 O3 P2 Se2'
_chemical_formula_weight         840.25

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'
Se Se -0.0929 2.2259 '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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   12.1752(9)
_cell_length_b                   14.2395(11)
_cell_length_c                   36.578(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.6320(10)
_cell_angle_gamma                90
_cell_volume                     6320.8(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8491
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      28.28

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_F_000             3280
_exptl_transmission_factor_min   0.44
_exptl_transmission_factor_max   0.69
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.089
_exptl_absorpt_coefficient_mu    4.419
_shelx_estimated_absorpt_T_min   0.442
_shelx_estimated_absorpt_T_max   0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'

_exptl_special_details           
; 
 The diffraction data were obtained from 3 sets of 400 frames,
 each of width 0.5° in ω, colllected 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°.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            55219
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         2.205
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_full        28.310
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7868
_reflns_number_gt                7232
_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       'Bruker SMART (Bruker, 2000)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2000a)'

_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
 in the lattice water molecule were placed in locations provided by a
 difference map. All were included as riding contributions with isotropic
 displacement parameters 1.2 - 1.5 times those of the attached carbon atoms.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0234P)²+15.7114P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7868
_refine_ls_number_parameters     292
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0579
_refine_ls_wR_factor_gt          0.0568
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_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
I1 I 0.72996(2) 0.37267(2) 0.05235(2) 0.01585(4) Uani 1 1 d . . . . .
I2 I 0.68966(2) 0.89927(2) 0.06576(2) 0.01548(4) Uani 1 1 d . . . . .
Se1 Se 0.63959(2) 0.61834(2) 0.23068(2) 0.02312(7) Uani 1 1 d . . . . .
Se2 Se 1.06155(2) 0.65391(2) 0.19970(2) 0.01653(6) Uani 1 1 d . . . . .
P1 P 0.71693(5) 0.63779(4) 0.18310(2) 0.01353(12) Uani 1 1 d . . . . .
P2 P 0.91238(5) 0.65448(4) 0.16840(2) 0.01153(11) Uani 1 1 d . . . . .
O1 O 0.62318(14) 0.64272(13) 0.14982(5) 0.0166(4) Uani 1 1 d . . . . .
O2 O 0.92543(14) 0.66606(12) 0.12542(5) 0.0150(3) Uani 1 1 d . . . . .
N1 N 0.80771(16) 0.72496(14) 0.17828(6) 0.0128(4) Uani 1 1 d . . . . .
N2 N 0.81928(16) 0.56792(14) 0.17017(6) 0.0128(4) Uani 1 1 d . . . . .
N3 N 0.45436(17) 0.61226(15) 0.08584(6) 0.0158(4) Uani 1 1 d . . . . .
N4 N 0.99193(17) 0.65221(14) 0.04542(6) 0.0127(4) Uani 1 1 d . . . . .
C1 C 0.8056(2) 0.82553(17) 0.19010(7) 0.0152(5) Uani 1 1 d . . . . .
C2 C 0.6887(2) 0.86305(19) 0.18141(8) 0.0213(5) Uani 1 1 d . . . . .
H2A H 0.6685 0.8577 0.1550 0.032 Uiso 1 1 calc R U . . .
H2B H 0.6856 0.9291 0.1888 0.032 Uiso 1 1 calc R U . . .
H2C H 0.6371 0.8263 0.1949 0.032 Uiso 1 1 calc R U . . .
C3 C 0.8403(2) 0.83316(19) 0.23093(7) 0.0209(5) Uani 1 1 d . . . . .
H3A H 0.7878 0.7987 0.2448 0.031 Uiso 1 1 calc R U . . .
H3B H 0.8412 0.8994 0.2383 0.031 Uiso 1 1 calc R U . . .
H3C H 0.9141 0.8063 0.2360 0.031 Uiso 1 1 calc R U . . .
C4 C 0.8849(2) 0.87999(18) 0.16776(8) 0.0211(5) Uani 1 1 d . . . . .
H4A H 0.9600 0.8564 0.1734 0.032 Uiso 1 1 calc R U . . .
H4B H 0.8821 0.9468 0.1740 0.032 Uiso 1 1 calc R U . . .
H4C H 0.8636 0.8717 0.1415 0.032 Uiso 1 1 calc R U . . .
C5 C 0.8367(2) 0.46407(17) 0.17457(7) 0.0157(5) Uani 1 1 d . . . . .
C6 C 0.8824(2) 0.44193(19) 0.21391(8) 0.0227(6) Uani 1 1 d . . . . .
H6A H 0.9539 0.4729 0.2189 0.034 Uiso 1 1 calc R U . . .
H6B H 0.8916 0.3739 0.2168 0.034 Uiso 1 1 calc R U . . .
H6C H 0.8310 0.4648 0.2312 0.034 Uiso 1 1 calc R U . . .
C7 C 0.9176(2) 0.43374(18) 0.14710(7) 0.0192(5) Uani 1 1 d . . . . .
H7A H 0.8867 0.4482 0.1222 0.029 Uiso 1 1 calc R U . . .
H7B H 0.9308 0.3660 0.1493 0.029 Uiso 1 1 calc R U . . .
H7C H 0.9874 0.4675 0.1521 0.029 Uiso 1 1 calc R U . . .
C8 C 0.7252(2) 0.41559(18) 0.16591(8) 0.0204(5) Uani 1 1 d . . . . .
H8A H 0.6715 0.4408 0.1819 0.031 Uiso 1 1 calc R U . . .
H8B H 0.7334 0.3479 0.1700 0.031 Uiso 1 1 calc R U . . .
H8C H 0.6993 0.4272 0.1402 0.031 Uiso 1 1 calc R U . . .
C9 C 0.6519(2) 0.64937(19) 0.11226(7) 0.0167(5) Uani 1 1 d . . . . .
H9A H 0.6798 0.5879 0.1044 0.020 Uiso 1 1 calc R U . . .
H9B H 0.7112 0.6963 0.1107 0.020 Uiso 1 1 calc R U . . .
C10 C 0.5529(2) 0.67764(18) 0.08707(7) 0.0172(5) Uani 1 1 d . . . . .
H10A H 0.5765 0.6835 0.0619 0.021 Uiso 1 1 calc R U . . .
H10B H 0.5288 0.7406 0.0946 0.021 Uiso 1 1 calc R U . . .
C11 C 0.3813(2) 0.6360(2) 0.11577(8) 0.0227(6) Uani 1 1 d . . . . .
H11A H 0.3201 0.5912 0.1153 0.034 Uiso 1 1 calc R U . . .
H11B H 0.3522 0.6997 0.1120 0.034 Uiso 1 1 calc R U . . .
H11C H 0.4241 0.6325 0.1396 0.034 Uiso 1 1 calc R U . . .
C12 C 0.3898(2) 0.62586(19) 0.04948(7) 0.0199(5) Uani 1 1 d . . . . .
H12A H 0.4357 0.6089 0.0297 0.030 Uiso 1 1 calc R U . . .
H12B H 0.3674 0.6918 0.0468 0.030 Uiso 1 1 calc R U . . .
H12C H 0.3241 0.5858 0.0482 0.030 Uiso 1 1 calc R U . . .
C13 C 0.4877(2) 0.51142(18) 0.08935(8) 0.0206(5) Uani 1 1 d . . . . .
H13A H 0.5252 0.5005 0.1137 0.031 Uiso 1 1 calc R U . . .
H13B H 0.5377 0.4961 0.0705 0.031 Uiso 1 1 calc R U . . .
H13C H 0.4220 0.4715 0.0861 0.031 Uiso 1 1 calc R U . . .
C14 C 1.0165(2) 0.71601(18) 0.11131(7) 0.0183(5) Uani 1 1 d . . . . .
H14A H 1.0746 0.7263 0.1314 0.022 Uiso 1 1 calc R U . . .
H14B H 0.9907 0.7783 0.1022 0.022 Uiso 1 1 calc R U . . .
C15 C 1.0642(2) 0.66335(17) 0.08091(7) 0.0142(5) Uani 1 1 d . . . . .
H15A H 1.0851 0.5999 0.0901 0.017 Uiso 1 1 calc R U . . .
H15B H 1.1329 0.6955 0.0752 0.017 Uiso 1 1 calc R U . . .
C16 C 0.9293(2) 0.73967(18) 0.03506(8) 0.0200(5) Uani 1 1 d . . . . .
H16A H 0.8942 0.7332 0.0101 0.030 Uiso 1 1 calc R U . . .
H16B H 0.9800 0.7932 0.0360 0.030 Uiso 1 1 calc R U . . .
H16C H 0.8727 0.7500 0.0522 0.030 Uiso 1 1 calc R U . . .
C17 C 0.9126(2) 0.57246(18) 0.04841(7) 0.0178(5) Uani 1 1 d . . . . .
H17A H 0.8641 0.5860 0.0679 0.027 Uiso 1 1 calc R U . . .
H17B H 0.9537 0.5145 0.0543 0.027 Uiso 1 1 calc R U . . .
H17C H 0.8682 0.5648 0.0250 0.027 Uiso 1 1 calc R U . . .
C18 C 1.0662(2) 0.63057(18) 0.01578(7) 0.0164(5) Uani 1 1 d . . . . .
H18A H 1.0218 0.6213 -0.0075 0.025 Uiso 1 1 calc R U . . .
H18B H 1.1082 0.5733 0.0221 0.025 Uiso 1 1 calc R U . . .
H18C H 1.1173 0.6830 0.0133 0.025 Uiso 1 1 calc R U . . .
O3 O 0.86532(19) 0.91734(16) 0.99041(6) 0.0346(5) Uani 1 1 d . . . . .
H1O H 0.8472 0.9753 0.9818 0.042 Uiso 1 1 d R U . . .
H2O H 0.8170 0.9049 1.0087 0.042 Uiso 1 1 d 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
Se1 P1 2.0635(7) . ?
Se2 P2 2.0672(7) . ?
P1 O1 1.6014(19) . ?
P1 N1 1.681(2) . ?
P1 N2 1.692(2) . ?
P2 O2 1.6015(18) . ?
P2 N2 1.679(2) . ?
P2 N1 1.684(2) . ?
O1 C9 1.448(3) . ?
O2 C14 1.447(3) . ?
N1 C1 1.497(3) . ?
N2 C5 1.501(3) . ?
N3 C13 1.495(3) . ?
N3 C12 1.502(3) . ?
N3 C11 1.504(3) . ?
N3 C10 1.517(3) . ?
N4 C16 1.493(3) . ?
N4 C18 1.499(3) . ?
N4 C17 1.500(3) . ?
N4 C15 1.517(3) . ?
C1 C3 1.523(4) . ?
C1 C4 1.526(4) . ?
C1 C2 1.530(3) . ?
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 1.526(4) . ?
C5 C8 1.533(3) . ?
C5 C6 1.533(4) . ?
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 1.511(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
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 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.497(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
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 . ?
O3 H1O 0.9047 . ?
O3 H2O 0.9427 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 N1 108.80(10) . . ?
O1 P1 N2 108.01(10) . . ?
N1 P1 N2 84.24(10) . . ?
O1 P1 Se1 107.53(7) . . ?
N1 P1 Se1 122.44(8) . . ?
N2 P1 Se1 123.61(8) . . ?
O2 P2 N2 103.54(10) . . ?
O2 P2 N1 106.62(10) . . ?
N2 P2 N1 84.51(10) . . ?
O2 P2 Se2 113.06(7) . . ?
N2 P2 Se2 122.78(8) . . ?
N1 P2 Se2 121.99(8) . . ?
C9 O1 P1 120.81(15) . . ?
C14 O2 P2 122.71(16) . . ?
C1 N1 P1 130.52(17) . . ?
C1 N1 P2 131.52(16) . . ?
P1 N1 P2 95.61(11) . . ?
C5 N2 P2 129.61(16) . . ?
C5 N2 P1 130.56(17) . . ?
P2 N2 P1 95.38(11) . . ?
C13 N3 C12 108.6(2) . . ?
C13 N3 C11 109.0(2) . . ?
C12 N3 C11 108.5(2) . . ?
C13 N3 C10 112.23(19) . . ?
C12 N3 C10 107.67(19) . . ?
C11 N3 C10 110.7(2) . . ?
C16 N4 C18 108.26(19) . . ?
C16 N4 C17 109.4(2) . . ?
C18 N4 C17 109.07(19) . . ?
C16 N4 C15 112.27(19) . . ?
C18 N4 C15 107.33(18) . . ?
C17 N4 C15 110.45(19) . . ?
N1 C1 C3 110.0(2) . . ?
N1 C1 C4 107.8(2) . . ?
C3 C1 C4 110.6(2) . . ?
N1 C1 C2 108.1(2) . . ?
C3 C1 C2 111.0(2) . . ?
C4 C1 C2 109.2(2) . . ?
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 107.5(2) . . ?
N2 C5 C8 107.9(2) . . ?
C7 C5 C8 110.2(2) . . ?
N2 C5 C6 109.9(2) . . ?
C7 C5 C6 110.8(2) . . ?
C8 C5 C6 110.5(2) . . ?
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 . . ?
O1 C9 C10 110.7(2) . . ?
O1 C9 H9A 109.5 . . ?
C10 C9 H9A 109.5 . . ?
O1 C9 H9B 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C9 C10 N3 116.4(2) . . ?
C9 C10 H10A 108.2 . . ?
N3 C10 H10A 108.2 . . ?
C9 C10 H10B 108.2 . . ?
N3 C10 H10B 108.2 . . ?
H10A C10 H10B 107.3 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O2 C14 C15 111.9(2) . . ?
O2 C14 H14A 109.2 . . ?
C15 C14 H14A 109.2 . . ?
O2 C14 H14B 109.2 . . ?
C15 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C14 C15 N4 117.0(2) . . ?
C14 C15 H15A 108.0 . . ?
N4 C15 H15A 108.0 . . ?
C14 C15 H15B 108.0 . . ?
N4 C15 H15B 108.0 . . ?
H15A C15 H15B 107.3 . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 H17A 109.5 . . ?
N4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
H1O O3 H2O 105.6 . . ?

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
O3 H1O I1 0.90 2.63 3.527(2) 169 7_666
O3 H2O I2 0.94 2.70 3.632(2) 170 1_556

_refine_diff_density_max         1.877
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.107

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 991949'
#######################################################################
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_msb328

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
μ-Triiodobis(1,3-di(tert-butyl)-2,4-bis(tert-
butylamino)-2-methyl-[1,3,2,4]diazadiphosphetidin-
2-ium)-κ-P dicopper(I) iodide acetonitrile solvate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H82 Cu2 I3 N8 P4, C2 H3 N, I'
_chemical_formula_sum            'C36 H85 Cu2 I4 N9 P4'
_chemical_formula_weight         1402.68

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'
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'
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/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                   10.3950(7)
_cell_length_b                   29.9149(18)
_cell_length_c                   17.8929(11)
_cell_angle_alpha                90
_cell_angle_beta                 95.847(1)
_cell_angle_gamma                90
_cell_volume                     5535.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4622
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      26.74

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_F_000             2776
_exptl_transmission_factor_min   0.684
_exptl_transmission_factor_max   0.838
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.058
_exptl_absorpt_coefficient_mu    3.148
_shelx_estimated_absorpt_T_min   0.570
_shelx_estimated_absorpt_T_max   0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2005a)'

_exptl_special_details           
;
 The diffraction data were obtained from 3 sets of 400 frames,
 each of width 0.5° in ω, colllected 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°.

 Using 2273 reflections with I/σ(I) > 15 selected from the
 full data set, it was determined that the crystal consisted
 of two components rotated by 1.9° about b* (CELL_NOW
 (Sheldrick, 2005)). The data were processed using the
 two-component version of SAINT and the two-component
 control file generated by CELL_NOW.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30384
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.084
_diffrn_reflns_theta_max         26.752
_diffrn_reflns_theta_full        26.750
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             26164
_reflns_number_gt                19149
_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       'Bruker SMART (Bruker, 2000)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2000a)'
_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 = 0.98 Å) and included as
 riding contributions with isotropic displacement parameters 1.5 times those
 of the attached carbon atoms. H-atoms attached to nitrogen were placed in
 positions indicated by a difference map, adjusted to give N---H distances
 of 0.91 Å and included as riding contributions with isotropic
 displacement parameters 1.2 times those of the attached nitrogen atoms.
 The tert-butyl groups built on C26 and C30 are rotationally disordered in
 82/18 and 77/23 ratios, respectively. the two orientations of each
 tert-butyl group were restrained to have approximately idealized geometry. 
 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)+(0.0311P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         26164
_refine_ls_number_parameters     538
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_restrained_S_all      0.956
_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
I1 I -0.12311(3) 0.03797(2) 0.31418(2) 0.01822(8) Uani 1 1 d . . . . .
I2 I -0.04522(3) 0.03982(2) 0.09410(2) 0.02161(8) Uani 1 1 d . . . . .
I3 I 0.24272(3) 0.08193(2) 0.25427(2) 0.02331(9) Uani 1 1 d . . . . .
I4 I 0.71177(3) 0.30270(2) 0.15849(2) 0.02459(9) Uani 1 1 d . . . . .
Cu1 Cu 0.06939(6) 0.01346(2) 0.22943(3) 0.01899(14) Uani 1 1 d . . . . .
Cu2 Cu -0.01887(6) 0.09294(2) 0.21246(3) 0.01929(14) Uani 1 1 d . . . . .
P1 P 0.17899(12) -0.04856(4) 0.25921(7) 0.0139(3) Uani 1 1 d . . . . .
P2 P 0.40601(12) -0.05241(4) 0.32737(7) 0.0151(3) Uani 1 1 d . . . . .
P3 P -0.11196(11) 0.15871(4) 0.22043(7) 0.0131(3) Uani 1 1 d . . . . .
P4 P -0.30427(12) 0.17462(4) 0.29327(7) 0.0159(3) Uani 1 1 d . . . . .
N1 N 0.2560(3) -0.05271(11) 0.3501(2) 0.0125(8) Uani 1 1 d . . . . .
N2 N 0.3409(3) -0.04959(11) 0.2402(2) 0.0142(8) Uani 1 1 d . . . . .
N3 N 0.4875(3) -0.09701(12) 0.3511(2) 0.0163(9) Uani 1 1 d . . . . .
H3N H 0.4375 -0.1220 0.3464 0.020 Uiso 1 1 d R U . . .
N4 N 0.1197(4) -0.09858(11) 0.2413(2) 0.0163(9) Uani 1 1 d . . . . .
H4N H 0.1747 -0.1199 0.2622 0.020 Uiso 1 1 d R U . . .
N5 N -0.1459(4) 0.17447(12) 0.3102(2) 0.0155(9) Uani 1 1 d . . . . .
N6 N -0.2802(3) 0.16207(11) 0.2063(2) 0.0139(8) Uani 1 1 d . . . . .
N7 N -0.0609(3) 0.20314(12) 0.1787(2) 0.0155(9) Uani 1 1 d . . . . .
H7N H -0.1095 0.2283 0.1811 0.019 Uiso 1 1 d R U . . .
N8 N -0.3785(4) 0.22130(12) 0.3028(2) 0.0180(9) Uani 1 1 d . . . . .
H8N H -0.3547 0.2400 0.2665 0.022 Uiso 1 1 d R U . . .
C1 C 0.2034(4) -0.04717(15) 0.4240(3) 0.0175(11) Uani 1 1 d . . . . .
C2 C 0.2918(5) -0.07096(16) 0.4843(3) 0.0221(11) Uani 1 1 d . . . . .
H2A H 0.2973 -0.1027 0.4715 0.033 Uiso 1 1 calc R U . . .
H2B H 0.2568 -0.0679 0.5329 0.033 Uiso 1 1 calc R U . . .
H2C H 0.3782 -0.0576 0.4874 0.033 Uiso 1 1 calc R U . . .
C3 C 0.0697(4) -0.06808(15) 0.4185(3) 0.0198(11) Uani 1 1 d . . . . .
H3A H 0.0132 -0.0529 0.3793 0.030 Uiso 1 1 calc R U . . .
H3B H 0.0338 -0.0650 0.4668 0.030 Uiso 1 1 calc R U . . .
H3C H 0.0759 -0.0998 0.4059 0.030 Uiso 1 1 calc R U . . .
C4 C 0.1948(5) 0.00253(15) 0.4444(3) 0.0222(11) Uani 1 1 d . . . . .
H4A H 0.2814 0.0158 0.4480 0.033 Uiso 1 1 calc R U . . .
H4B H 0.1591 0.0055 0.4928 0.033 Uiso 1 1 calc R U . . .
H4C H 0.1385 0.0180 0.4055 0.033 Uiso 1 1 calc R U . . .
C5 C 0.3972(5) -0.05319(15) 0.1669(3) 0.0206(11) Uani 1 1 d . . . . .
C6 C 0.5253(5) -0.02805(18) 0.1731(3) 0.0349(14) Uani 1 1 d . . . . .
H6A H 0.5108 0.0032 0.1864 0.052 Uiso 1 1 calc R U . . .
H6B H 0.5619 -0.0292 0.1248 0.052 Uiso 1 1 calc R U . . .
H6C H 0.5856 -0.0419 0.2120 0.052 Uiso 1 1 calc R U . . .
C7 C 0.4173(5) -0.10233(16) 0.1485(3) 0.0300(13) Uani 1 1 d . . . . .
H7A H 0.4781 -0.1158 0.1876 0.045 Uiso 1 1 calc R U . . .
H7B H 0.4524 -0.1047 0.0998 0.045 Uiso 1 1 calc R U . . .
H7C H 0.3344 -0.1181 0.1462 0.045 Uiso 1 1 calc R U . . .
C8 C 0.3026(5) -0.03191(18) 0.1068(3) 0.0331(14) Uani 1 1 d . . . . .
H8A H 0.2205 -0.0482 0.1033 0.050 Uiso 1 1 calc R U . . .
H8B H 0.3387 -0.0331 0.0583 0.050 Uiso 1 1 calc R U . . .
H8C H 0.2878 -0.0007 0.1201 0.050 Uiso 1 1 calc R U . . .
C9 C 0.6178(4) -0.10986(15) 0.3892(3) 0.0213(11) Uani 1 1 d . . . . .
C10 C 0.6067(6) -0.1171(2) 0.4721(3) 0.0518(19) Uani 1 1 d . . . . .
H10A H 0.5812 -0.0890 0.4948 0.078 Uiso 1 1 calc R U . . .
H10B H 0.6903 -0.1269 0.4970 0.078 Uiso 1 1 calc R U . . .
H10C H 0.5413 -0.1400 0.4783 0.078 Uiso 1 1 calc R U . . .
C11 C 0.6552(5) -0.15329(18) 0.3526(4) 0.052(2) Uani 1 1 d . . . . .
H11A H 0.5904 -0.1763 0.3598 0.077 Uiso 1 1 calc R U . . .
H11B H 0.7399 -0.1632 0.3757 0.077 Uiso 1 1 calc R U . . .
H11C H 0.6592 -0.1484 0.2987 0.077 Uiso 1 1 calc R U . . .
C12 C 0.7205(5) -0.07496(16) 0.3790(3) 0.0303(13) Uani 1 1 d . . . . .
H12A H 0.7213 -0.0683 0.3254 0.045 Uiso 1 1 calc R U . . .
H12B H 0.8054 -0.0864 0.3991 0.045 Uiso 1 1 calc R U . . .
H12C H 0.7012 -0.0476 0.4059 0.045 Uiso 1 1 calc R U . . .
C13 C -0.0006(5) -0.11448(15) 0.1973(3) 0.0196(11) Uani 1 1 d . . . . .
C14 C 0.0317(5) -0.13155(19) 0.1211(3) 0.0386(15) Uani 1 1 d . . . . .
H14A H 0.0590 -0.1065 0.0912 0.058 Uiso 1 1 calc R U . . .
H14B H -0.0450 -0.1456 0.0946 0.058 Uiso 1 1 calc R U . . .
H14C H 0.1018 -0.1535 0.1284 0.058 Uiso 1 1 calc R U . . .
C15 C -0.0520(5) -0.15334(16) 0.2411(3) 0.0323(14) Uani 1 1 d . . . . .
H15A H 0.0133 -0.1770 0.2471 0.048 Uiso 1 1 calc R U . . .
H15B H -0.1311 -0.1651 0.2135 0.048 Uiso 1 1 calc R U . . .
H15C H -0.0710 -0.1428 0.2907 0.048 Uiso 1 1 calc R U . . .
C16 C -0.1031(5) -0.07836(15) 0.1882(3) 0.0288(13) Uani 1 1 d . . . . .
H16A H -0.1192 -0.0670 0.2378 0.043 Uiso 1 1 calc R U . . .
H16B H -0.1833 -0.0909 0.1630 0.043 Uiso 1 1 calc R U . . .
H16C H -0.0732 -0.0539 0.1579 0.043 Uiso 1 1 calc R U . . .
C17 C 0.4951(4) -0.00374(14) 0.3576(3) 0.0197(11) Uani 1 1 d . . . . .
H17A H 0.5145 -0.0045 0.4124 0.029 Uiso 1 1 calc R U . . .
H17B H 0.4438 0.0229 0.3432 0.029 Uiso 1 1 calc R U . . .
H17C H 0.5761 -0.0029 0.3340 0.029 Uiso 1 1 calc R U . . .
C18 C -0.0575(5) 0.18825(14) 0.3772(3) 0.0187(11) Uani 1 1 d . . . . .
C19 C -0.1176(6) 0.17406(18) 0.4473(3) 0.0347(14) Uani 1 1 d . . . . .
H19A H -0.2000 0.1897 0.4494 0.052 Uiso 1 1 calc R U . . .
H19B H -0.0589 0.1816 0.4918 0.052 Uiso 1 1 calc R U . . .
H19C H -0.1327 0.1417 0.4459 0.052 Uiso 1 1 calc R U . . .
C20 C -0.0386(5) 0.23879(15) 0.3750(3) 0.0330(14) Uani 1 1 d . . . . .
H20A H -0.0040 0.2471 0.3279 0.050 Uiso 1 1 calc R U . . .
H20B H 0.0224 0.2480 0.4176 0.050 Uiso 1 1 calc R U . . .
H20C H -0.1218 0.2537 0.3779 0.050 Uiso 1 1 calc R U . . .
C21 C 0.0698(5) 0.16384(18) 0.3753(3) 0.0347(14) Uani 1 1 d . . . . .
H21A H 0.0544 0.1315 0.3745 0.052 Uiso 1 1 calc R U . . .
H21B H 0.1279 0.1717 0.4200 0.052 Uiso 1 1 calc R U . . .
H21C H 0.1096 0.1725 0.3301 0.052 Uiso 1 1 calc R U . . .
C22 C -0.3708(5) 0.14693(16) 0.1410(3) 0.0223(12) Uani 1 1 d . . . . .
C23 C -0.3985(5) 0.09651(15) 0.1478(3) 0.0284(13) Uani 1 1 d . . . . .
H23A H -0.3167 0.0800 0.1534 0.043 Uiso 1 1 calc R U . . .
H23B H -0.4512 0.0863 0.1024 0.043 Uiso 1 1 calc R U . . .
H23C H -0.4453 0.0912 0.1918 0.043 Uiso 1 1 calc R U . . .
C24 C -0.3078(5) 0.15592(18) 0.0697(3) 0.0318(13) Uani 1 1 d . . . . .
H24A H -0.2832 0.1875 0.0680 0.048 Uiso 1 1 calc R U . . .
H24B H -0.3689 0.1489 0.0259 0.048 Uiso 1 1 calc R U . . .
H24C H -0.2305 0.1372 0.0690 0.048 Uiso 1 1 calc R U . . .
C25 C -0.4955(5) 0.17381(16) 0.1407(3) 0.0290(13) Uani 1 1 d . . . . .
H25A H -0.5375 0.1667 0.1858 0.044 Uiso 1 1 calc R U . . .
H25B H -0.5536 0.1662 0.0959 0.044 Uiso 1 1 calc R U . . .
H25C H -0.4754 0.2058 0.1401 0.044 Uiso 1 1 calc R U . . .
C26 C 0.0506(5) 0.20960(15) 0.1338(3) 0.0223(12) Uani 1 1 d D . . . .
C27 C 0.0697(7) 0.17082(19) 0.0830(4) 0.0315(17) Uani 0.818(5) 1 d D . P A 1
H27A H 0.0855 0.1436 0.1131 0.047 Uiso 0.818(5) 1 calc R U P A 1
H27B H 0.1441 0.1767 0.0549 0.047 Uiso 0.818(5) 1 calc R U P A 1
H27C H -0.0080 0.1668 0.0477 0.047 Uiso 0.818(5) 1 calc R U P A 1
C28 C 0.1751(6) 0.2161(2) 0.1897(3) 0.0281(15) Uani 0.818(5) 1 d D . P A 1
H28A H 0.1627 0.2414 0.2230 0.042 Uiso 0.818(5) 1 calc R U P A 1
H28B H 0.2491 0.2221 0.1614 0.042 Uiso 0.818(5) 1 calc R U P A 1
H28C H 0.1915 0.1889 0.2198 0.042 Uiso 0.818(5) 1 calc R U P A 1
C29 C 0.0277(6) 0.25287(19) 0.0910(4) 0.0280(16) Uani 0.818(5) 1 d D . P A 1
H29A H 0.0165 0.2773 0.1263 0.042 Uiso 0.818(5) 1 calc R U P A 1
H29B H -0.0503 0.2502 0.0556 0.042 Uiso 0.818(5) 1 calc R U P A 1
H29C H 0.1021 0.2593 0.0632 0.042 Uiso 0.818(5) 1 calc R U P A 1
C27A C 0.099(3) 0.2569(5) 0.1349(16) 0.0315(17) Uani 0.182(5) 1 d D . P A 2
H27D H 0.0250 0.2774 0.1294 0.047 Uiso 0.182(5) 1 calc R U P A 2
H27E H 0.1519 0.2614 0.0933 0.047 Uiso 0.182(5) 1 calc R U P A 2
H27F H 0.1509 0.2627 0.1826 0.047 Uiso 0.182(5) 1 calc R U P A 2
C28A C -0.020(2) 0.2036(8) 0.0478(11) 0.0281(15) Uani 0.182(5) 1 d D . P A 2
H28D H -0.0899 0.2257 0.0388 0.042 Uiso 0.182(5) 1 calc R U P A 2
H28E H -0.0566 0.1734 0.0417 0.042 Uiso 0.182(5) 1 calc R U P A 2
H28F H 0.0432 0.2082 0.0117 0.042 Uiso 0.182(5) 1 calc R U P A 2
C29A C 0.152(2) 0.1743(7) 0.1405(15) 0.0280(16) Uani 0.182(5) 1 d D . P A 2
H29D H 0.1106 0.1448 0.1378 0.042 Uiso 0.182(5) 1 calc R U P A 2
H29E H 0.2049 0.1774 0.1887 0.042 Uiso 0.182(5) 1 calc R U P A 2
H29F H 0.2067 0.1774 0.0994 0.042 Uiso 0.182(5) 1 calc R U P A 2
C30 C -0.4758(5) 0.24095(16) 0.3503(3) 0.0283(13) Uani 1 1 d D . . . .
C31 C -0.5769(9) 0.2070(2) 0.3698(6) 0.054(3) Uani 0.766(9) 1 d D . P B 1
H31A H -0.6189 0.1937 0.3236 0.082 Uiso 0.766(9) 1 calc R U P B 1
H31B H -0.6419 0.2220 0.3969 0.082 Uiso 0.766(9) 1 calc R U P B 1
H31C H -0.5347 0.1834 0.4016 0.082 Uiso 0.766(9) 1 calc R U P B 1
C32 C -0.5471(7) 0.2769(2) 0.3028(4) 0.0316(18) Uani 0.766(9) 1 d D . P B 1
H32A H -0.5890 0.2635 0.2566 0.047 Uiso 0.766(9) 1 calc R U P B 1
H32B H -0.4856 0.2998 0.2900 0.047 Uiso 0.766(9) 1 calc R U P B 1
H32C H -0.6128 0.2906 0.3310 0.047 Uiso 0.766(9) 1 calc R U P B 1
C33 C -0.4091(9) 0.2618(4) 0.4203(5) 0.079(4) Uani 0.766(9) 1 d D . P B 1
H33A H -0.3629 0.2387 0.4512 0.118 Uiso 0.766(9) 1 calc R U P B 1
H33B H -0.4735 0.2760 0.4489 0.118 Uiso 0.766(9) 1 calc R U P B 1
H33C H -0.3474 0.2844 0.4065 0.118 Uiso 0.766(9) 1 calc R U P B 1
C31A C -0.412(2) 0.2827(6) 0.3788(17) 0.054(3) Uani 0.234(9) 1 d D . P B 2
H31D H -0.3362 0.2753 0.4138 0.082 Uiso 0.234(9) 1 calc R U P B 2
H31E H -0.4727 0.3005 0.4047 0.082 Uiso 0.234(9) 1 calc R U P B 2
H31F H -0.3843 0.2998 0.3366 0.082 Uiso 0.234(9) 1 calc R U P B 2
C32A C -0.509(3) 0.2113(7) 0.4135(12) 0.0316(18) Uani 0.234(9) 1 d D . P B 2
H32D H -0.4305 0.2041 0.4461 0.047 Uiso 0.234(9) 1 calc R U P B 2
H32E H -0.5491 0.1837 0.3928 0.047 Uiso 0.234(9) 1 calc R U P B 2
H32F H -0.5702 0.2269 0.4429 0.047 Uiso 0.234(9) 1 calc R U P B 2
C33A C -0.594(2) 0.2499(12) 0.2953(13) 0.079(4) Uani 0.234(9) 1 d D . P B 2
H33D H -0.5714 0.2703 0.2560 0.118 Uiso 0.234(9) 1 calc R U P B 2
H33E H -0.6623 0.2634 0.3221 0.118 Uiso 0.234(9) 1 calc R U P B 2
H33F H -0.6260 0.2217 0.2725 0.118 Uiso 0.234(9) 1 calc R U P B 2
C34 C -0.3813(5) 0.13092(15) 0.3400(3) 0.0232(12) Uani 1 1 d . . . . .
H34A H -0.3786 0.1379 0.3937 0.035 Uiso 1 1 calc R U . . .
H34B H -0.3361 0.1027 0.3336 0.035 Uiso 1 1 calc R U . . .
H34C H -0.4715 0.1282 0.3185 0.035 Uiso 1 1 calc R U . . .
N9 N 0.3241(5) 0.15274(17) 0.9486(3) 0.0425(13) Uani 1 1 d . . . . .
C35 C 0.3021(5) 0.1196(2) 0.9761(3) 0.0304(13) Uani 1 1 d . . . . .
C36 C 0.2725(6) 0.07779(19) 1.0124(3) 0.0416(16) Uani 1 1 d . . . . .
H36A H 0.2830 0.0818 1.0671 0.062 Uiso 1 1 calc R U . . .
H36B H 0.3315 0.0544 0.9984 0.062 Uiso 1 1 calc R U . . .
H36C H 0.1831 0.0691 0.9962 0.062 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 Cu1 2.7313(7) . ?
I1 Cu2 2.7555(7) . ?
I2 Cu2 2.6395(7) . ?
I2 Cu1 2.7050(7) . ?
I3 Cu1 2.7342(7) . ?
I3 Cu2 2.7655(7) . ?
Cu1 P1 2.2137(13) . ?
Cu1 Cu2 2.5553(8) . ?
Cu2 P3 2.2037(12) . ?
P1 N4 1.637(4) . ?
P1 N1 1.743(4) . ?
P1 N2 1.752(4) . ?
P2 N3 1.613(4) . ?
P2 N2 1.638(4) . ?
P2 N1 1.651(4) . ?
P2 C17 1.780(4) . ?
P3 N7 1.639(4) . ?
P3 N5 1.743(4) . ?
P3 N6 1.744(4) . ?
P4 N8 1.613(4) . ?
P4 N5 1.643(4) . ?
P4 N6 1.644(4) . ?
P4 C34 1.785(5) . ?
N1 C1 1.490(6) . ?
N2 C5 1.492(6) . ?
N3 C9 1.504(6) . ?
N3 H3N 0.9100 . ?
N4 C13 1.487(6) . ?
N4 H4N 0.9100 . ?
N5 C18 1.493(6) . ?
N6 C22 1.495(6) . ?
N7 C26 1.488(6) . ?
N7 H7N 0.9101 . ?
N8 C30 1.506(6) . ?
N8 H8N 0.9100 . ?
C1 C3 1.518(6) . ?
C1 C2 1.520(6) . ?
C1 C4 1.536(6) . ?
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 C8 1.521(7) . ?
C5 C6 1.524(7) . ?
C5 C7 1.526(6) . ?
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 1.516(7) . ?
C9 C12 1.517(6) . ?
C9 C11 1.523(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 C16 1.515(6) . ?
C13 C14 1.526(7) . ?
C13 C15 1.528(7) . ?
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 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C21 1.515(7) . ?
C18 C19 1.517(7) . ?
C18 C20 1.526(6) . ?
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 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.517(7) . ?
C22 C25 1.525(6) . ?
C22 C23 1.543(6) . ?
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 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C29A 1.488(15) . ?
C26 C27A 1.499(16) . ?
C26 C27 1.500(7) . ?
C26 C29 1.511(6) . ?
C26 C28 1.565(7) . ?
C26 C28A 1.648(16) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C27A H27D 0.9800 . ?
C27A H27E 0.9800 . ?
C27A H27F 0.9800 . ?
C28A H28D 0.9800 . ?
C28A H28E 0.9800 . ?
C28A H28F 0.9800 . ?
C29A H29D 0.9800 . ?
C29A H29E 0.9800 . ?
C29A H29F 0.9800 . ?
C30 C31A 1.480(16) . ?
C30 C33 1.505(8) . ?
C30 C32A 1.506(15) . ?
C30 C32 1.516(7) . ?
C30 C33A 1.520(16) . ?
C30 C31 1.527(8) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C31A H31D 0.9800 . ?
C31A H31E 0.9800 . ?
C31A H31F 0.9800 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?
C33A H33D 0.9800 . ?
C33A H33E 0.9800 . ?
C33A H33F 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
N9 C35 1.140(7) . ?
C35 C36 1.457(7) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 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
Cu1 I1 Cu2 55.512(17) . . ?
Cu2 I2 Cu1 57.110(18) . . ?
Cu1 I3 Cu2 55.370(18) . . ?
P1 Cu1 Cu2 168.00(4) . . ?
P1 Cu1 I2 128.96(4) . . ?
Cu2 Cu1 I2 60.155(19) . . ?
P1 Cu1 I1 118.65(4) . . ?
Cu2 Cu1 I1 62.724(19) . . ?
I2 Cu1 I1 97.93(2) . . ?
P1 Cu1 I3 105.91(4) . . ?
Cu2 Cu1 I3 62.94(2) . . ?
I2 Cu1 I3 98.63(2) . . ?
I1 Cu1 I3 102.51(2) . . ?
P3 Cu2 Cu1 167.90(4) . . ?
P3 Cu2 I2 125.38(4) . . ?
Cu1 Cu2 I2 62.74(2) . . ?
P3 Cu2 I1 106.58(4) . . ?
Cu1 Cu2 I1 61.764(19) . . ?
I2 Cu2 I1 98.92(2) . . ?
P3 Cu2 I3 121.00(4) . . ?
Cu1 Cu2 I3 61.693(19) . . ?
I2 Cu2 I3 99.45(2) . . ?
I1 Cu2 I3 101.08(2) . . ?
N4 P1 N1 104.20(18) . . ?
N4 P1 N2 107.21(18) . . ?
N1 P1 N2 79.70(18) . . ?
N4 P1 Cu1 123.00(14) . . ?
N1 P1 Cu1 117.42(12) . . ?
N2 P1 Cu1 116.69(13) . . ?
N3 P2 N2 116.60(19) . . ?
N3 P2 N1 114.47(19) . . ?
N2 P2 N1 85.78(19) . . ?
N3 P2 C17 110.7(2) . . ?
N2 P2 C17 113.5(2) . . ?
N1 P2 C17 113.9(2) . . ?
N7 P3 N5 107.81(18) . . ?
N7 P3 N6 104.70(18) . . ?
N5 P3 N6 79.83(18) . . ?
N7 P3 Cu2 121.98(14) . . ?
N5 P3 Cu2 115.62(13) . . ?
N6 P3 Cu2 118.85(13) . . ?
N8 P4 N5 117.6(2) . . ?
N8 P4 N6 114.72(19) . . ?
N5 P4 N6 85.80(19) . . ?
N8 P4 C34 110.0(2) . . ?
N5 P4 C34 113.6(2) . . ?
N6 P4 C34 113.3(2) . . ?
C1 N1 P2 131.2(3) . . ?
C1 N1 P1 130.2(3) . . ?
P2 N1 P1 97.18(19) . . ?
C5 N2 P2 132.2(3) . . ?
C5 N2 P1 130.0(3) . . ?
P2 N2 P1 97.3(2) . . ?
C9 N3 P2 139.0(3) . . ?
C9 N3 H3N 108.1 . . ?
P2 N3 H3N 112.1 . . ?
C13 N4 P1 132.5(3) . . ?
C13 N4 H4N 116.9 . . ?
P1 N4 H4N 110.6 . . ?
C18 N5 P4 132.1(3) . . ?
C18 N5 P3 130.5(3) . . ?
P4 N5 P3 97.15(19) . . ?
C22 N6 P4 131.6(3) . . ?
C22 N6 P3 129.7(3) . . ?
P4 N6 P3 97.10(19) . . ?
C26 N7 P3 131.1(3) . . ?
C26 N7 H7N 112.7 . . ?
P3 N7 H7N 116.2 . . ?
C30 N8 P4 138.9(3) . . ?
C30 N8 H8N 114.2 . . ?
P4 N8 H8N 106.8 . . ?
N1 C1 C3 108.3(4) . . ?
N1 C1 C2 109.2(4) . . ?
C3 C1 C2 109.6(4) . . ?
N1 C1 C4 110.8(4) . . ?
C3 C1 C4 109.8(4) . . ?
C2 C1 C4 109.2(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 . . ?
N2 C5 C8 107.9(4) . . ?
N2 C5 C6 108.6(4) . . ?
C8 C5 C6 110.0(4) . . ?
N2 C5 C7 109.5(4) . . ?
C8 C5 C7 110.1(4) . . ?
C6 C5 C7 110.7(4) . . ?
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 109.0(4) . . ?
N3 C9 C12 112.5(4) . . ?
C10 C9 C12 109.9(5) . . ?
N3 C9 C11 106.3(4) . . ?
C10 C9 C11 110.3(5) . . ?
C12 C9 C11 108.8(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 C16 111.9(4) . . ?
N4 C13 C14 109.3(4) . . ?
C16 C13 C14 111.0(4) . . ?
N4 C13 C15 106.9(4) . . ?
C16 C13 C15 108.6(4) . . ?
C14 C13 C15 108.9(4) . . ?
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 . . ?
P2 C17 H17A 109.5 . . ?
P2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N5 C18 C21 108.5(4) . . ?
N5 C18 C19 108.4(4) . . ?
C21 C18 C19 108.5(4) . . ?
N5 C18 C20 108.9(4) . . ?
C21 C18 C20 111.2(4) . . ?
C19 C18 C20 111.3(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 C24 108.2(4) . . ?
N6 C22 C25 108.1(4) . . ?
C24 C22 C25 110.1(4) . . ?
N6 C22 C23 110.1(4) . . ?
C24 C22 C23 109.8(4) . . ?
C25 C22 C23 110.5(4) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N7 C26 C29A 116.6(11) . . ?
N7 C26 C27A 113.2(11) . . ?
C29A C26 C27A 115.9(13) . . ?
N7 C26 C27 112.7(4) . . ?
N7 C26 C29 107.1(4) . . ?
C27 C26 C29 112.2(5) . . ?
N7 C26 C28 108.1(4) . . ?
C27 C26 C28 109.4(4) . . ?
C29 C26 C28 107.2(4) . . ?
N7 C26 C28A 101.0(10) . . ?
C29A C26 C28A 104.1(11) . . ?
C27A C26 C28A 103.4(11) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C27A H27D 109.5 . . ?
C26 C27A H27E 109.5 . . ?
H27D C27A H27E 109.5 . . ?
C26 C27A H27F 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
C26 C28A H28D 109.5 . . ?
C26 C28A H28E 109.5 . . ?
H28D C28A H28E 109.5 . . ?
C26 C28A H28F 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
C26 C29A H29D 109.5 . . ?
C26 C29A H29E 109.5 . . ?
H29D C29A H29E 109.5 . . ?
C26 C29A H29F 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
C31A C30 C32A 111.6(12) . . ?
C31A C30 N8 102.6(11) . . ?
C33 C30 N8 110.6(5) . . ?
C32A C30 N8 114.5(10) . . ?
C33 C30 C32 109.3(6) . . ?
N8 C30 C32 106.1(4) . . ?
C31A C30 C33A 112.4(12) . . ?
C32A C30 C33A 110.8(13) . . ?
N8 C30 C33A 104.5(11) . . ?
C33 C30 C31 110.8(6) . . ?
N8 C30 C31 112.8(4) . . ?
C32 C30 C31 107.0(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C31A H31D 109.5 . . ?
C30 C31A H31E 109.5 . . ?
H31D C31A H31E 109.5 . . ?
C30 C31A H31F 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
C30 C32A H32D 109.5 . . ?
C30 C32A H32E 109.5 . . ?
H32D C32A H32E 109.5 . . ?
C30 C32A H32F 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
C30 C33A H33D 109.5 . . ?
C30 C33A H33E 109.5 . . ?
H33D C33A H33E 109.5 . . ?
C30 C33A H33F 109.5 . . ?
H33D C33A H33F 109.5 . . ?
H33E C33A H33F 109.5 . . ?
P4 C34 H34A 109.5 . . ?
P4 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
P4 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N9 C35 C36 178.7(6) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 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
N3 H3N I4 0.91 2.73 3.640(4) 176 2_645
N4 H4N I4 0.91 2.90 3.790(4) 165 2_645
N7 H7N I4 0.91 2.90 3.796(4) 168 1_455
N8 H8N I4 0.91 2.83 3.737(4) 176 1_455

_refine_diff_density_max         1.969
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.129

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 991950'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_msb371_0m

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
Iodo(2,2'-bipyridine-\kN:\kN')(1,3-di-<i>tert</i>-
butyl-2,4-bis(tert-butylamino)-2-methyl-[1,3,2,4]
diazadiphosphetidin-2-ium-\kP)copper(I) Iodide 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H49 Cu I N6 P2, I'
_chemical_formula_sum            'C27 H49 Cu I2 N6 P2'
_chemical_formula_weight         837.00

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'
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'
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           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   14.1715(6)
_cell_length_b                   14.6142(6)
_cell_length_c                   16.8817(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3496.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9771
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      28.27

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_F_000             1672
_exptl_transmission_factor_min   0.697
_exptl_transmission_factor_max   0.743
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.126
_exptl_absorpt_coefficient_mu    2.508
_shelx_estimated_absorpt_T_min   0.709
_shelx_estimated_absorpt_T_max   0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'

_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°.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61743
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.337
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_full        28.300
_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 1.000
_reflns_number_total             8681
_reflns_number_gt                7987
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_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       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2006a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2000a)'
_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) and included
 as riding contributions with isotropic displacement parameters 1.2 - 1.5
 times those of the attached atoms. Those attached to nitrogen (H1n and H4n)
 were placed in positions derived from a difference map, adjusted to an
 N---H distance of 0.91 Å and included as riding contributions with
 isotropic displacement parameters 1.2 times those of the attached atoms.
 From the refinement of the Flack parameter, it was determined that the
 crystal is a racemic twin and was refined as such.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0297P)²+11.6297P] 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.
;
_refine_ls_abs_structure_Flack   0.48(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8681
_refine_ls_number_parameters     357
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0869
_refine_ls_wR_factor_gt          0.0840
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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
Cu1 Cu 0.74350(6) 0.10765(5) 0.57827(4) 0.01742(15) Uani 1 1 d . . . . .
I1 I 0.75808(3) 0.18997(3) 0.44122(2) 0.02106(10) Uani 1 1 d . . . . .
I2 I 0.76458(3) 0.35219(3) 0.92377(2) 0.02473(11) Uani 1 1 d . . . . .
P1 P 0.75465(13) 0.20779(10) 0.67482(8) 0.0150(3) Uani 1 1 d . . . . .
P2 P 0.75371(13) 0.38024(10) 0.65629(9) 0.0178(3) Uani 1 1 d . . . . .
N1 N 0.7667(4) 0.1766(4) 0.7679(3) 0.0197(11) Uani 1 1 d . . . . .
H1N H 0.7648 0.2321 0.7924 0.024 Uiso 1 1 d R U . . .
N2 N 0.8328(4) 0.2988(4) 0.6623(4) 0.0163(12) Uani 1 1 d . . . . .
N3 N 0.6752(4) 0.3002(4) 0.6741(4) 0.0171(12) Uani 1 1 d . . . . .
N4 N 0.7598(5) 0.4601(3) 0.7228(3) 0.0240(12) Uani 1 1 d . . . . .
H4N H 0.7610 0.4375 0.7731 0.029 Uiso 1 1 d R U . . .
N5 N 0.8259(4) -0.0095(4) 0.5641(4) 0.0225(12) Uani 1 1 d . . . . .
N6 N 0.6394(4) 0.0072(4) 0.5747(4) 0.0244(13) Uani 1 1 d . . . . .
C1 C 0.7675(6) 0.0874(4) 0.8101(4) 0.0252(16) Uani 1 1 d . . . . .
C2 C 0.8532(6) 0.0881(7) 0.8651(5) 0.035(2) Uani 1 1 d . . . . .
H2A H 0.9111 0.0853 0.8334 0.053 Uiso 1 1 calc R U . . .
H2B H 0.8504 0.0350 0.9005 0.053 Uiso 1 1 calc R U . . .
H2C H 0.8530 0.1444 0.8966 0.053 Uiso 1 1 calc R U . . .
C3 C 0.7728(8) 0.0075(5) 0.7538(4) 0.042(2) Uani 1 1 d . . . . .
H3A H 0.7188 0.0094 0.7175 0.063 Uiso 1 1 calc R U . . .
H3B H 0.7715 -0.0498 0.7839 0.063 Uiso 1 1 calc R U . . .
H3C H 0.8315 0.0110 0.7233 0.063 Uiso 1 1 calc R U . . .
C4 C 0.6768(6) 0.0811(6) 0.8584(5) 0.0294(18) Uani 1 1 d . . . . .
H4A H 0.6706 0.1356 0.8918 0.044 Uiso 1 1 calc R U . . .
H4B H 0.6789 0.0264 0.8920 0.044 Uiso 1 1 calc R U . . .
H4C H 0.6226 0.0772 0.8225 0.044 Uiso 1 1 calc R U . . .
C5 C 0.9377(5) 0.3011(6) 0.6602(5) 0.0238(16) Uani 1 1 d . . . . .
C6 C 0.9766(5) 0.3253(6) 0.7422(4) 0.0284(17) Uani 1 1 d . . . . .
H6A H 0.9527 0.3854 0.7582 0.043 Uiso 1 1 calc R U . . .
H6B H 1.0457 0.3269 0.7401 0.043 Uiso 1 1 calc R U . . .
H6C H 0.9562 0.2791 0.7806 0.043 Uiso 1 1 calc R U . . .
C7 C 0.9696(5) 0.3703(5) 0.5988(5) 0.0306(18) Uani 1 1 d . . . . .
H7A H 0.9431 0.3540 0.5470 0.046 Uiso 1 1 calc R U . . .
H7B H 1.0387 0.3701 0.5955 0.046 Uiso 1 1 calc R U . . .
H7C H 0.9478 0.4314 0.6140 0.046 Uiso 1 1 calc R U . . .
C8 C 0.9719(5) 0.2064(5) 0.6356(5) 0.0259(15) Uani 1 1 d . . . . .
H8A H 0.9501 0.1610 0.6743 0.039 Uiso 1 1 calc R U . . .
H8B H 1.0410 0.2060 0.6336 0.039 Uiso 1 1 calc R U . . .
H8C H 0.9465 0.1914 0.5833 0.039 Uiso 1 1 calc R U . . .
C9 C 0.5707(5) 0.2987(5) 0.6644(4) 0.0194(15) Uani 1 1 d . . . . .
C10 C 0.5319(5) 0.2215(6) 0.7161(5) 0.0286(17) Uani 1 1 d . . . . .
H10A H 0.5586 0.1630 0.6987 0.043 Uiso 1 1 calc R U . . .
H10B H 0.4630 0.2195 0.7113 0.043 Uiso 1 1 calc R U . . .
H10C H 0.5492 0.2326 0.7715 0.043 Uiso 1 1 calc R U . . .
C11 C 0.5450(5) 0.2844(5) 0.5777(5) 0.0269(16) Uani 1 1 d . . . . .
H11A H 0.5611 0.3395 0.5474 0.040 Uiso 1 1 calc R U . . .
H11B H 0.4772 0.2725 0.5732 0.040 Uiso 1 1 calc R U . . .
H11C H 0.5803 0.2321 0.5567 0.040 Uiso 1 1 calc R U . . .
C12 C 0.5296(6) 0.3901(5) 0.6933(5) 0.0309(17) Uani 1 1 d . . . . .
H12A H 0.5490 0.4008 0.7483 0.046 Uiso 1 1 calc R U . . .
H12B H 0.4606 0.3880 0.6903 0.046 Uiso 1 1 calc R U . . .
H12C H 0.5531 0.4399 0.6598 0.046 Uiso 1 1 calc R U . . .
C13 C 0.7658(6) 0.5633(4) 0.7226(4) 0.0279(15) Uani 1 1 d . . . . .
C14 C 0.8592(7) 0.5940(6) 0.6871(7) 0.041(2) Uani 1 1 d . . . . .
H14A H 0.8617 0.5762 0.6311 0.062 Uiso 1 1 calc R U . . .
H14B H 0.9113 0.5648 0.7157 0.062 Uiso 1 1 calc R U . . .
H14C H 0.8648 0.6606 0.6915 0.062 Uiso 1 1 calc R U . . .
C15 C 0.7638(11) 0.5898(5) 0.8096(5) 0.054(3) Uani 1 1 d . . . . .
H15A H 0.7619 0.6567 0.8143 0.081 Uiso 1 1 calc R U . . .
H15B H 0.8205 0.5664 0.8359 0.081 Uiso 1 1 calc R U . . .
H15C H 0.7076 0.5636 0.8347 0.081 Uiso 1 1 calc R U . . .
C16 C 0.6847(7) 0.6070(6) 0.6794(6) 0.041(2) Uani 1 1 d . . . . .
H16A H 0.6916 0.5965 0.6223 0.061 Uiso 1 1 calc R U . . .
H16B H 0.6843 0.6730 0.6899 0.061 Uiso 1 1 calc R U . . .
H16C H 0.6252 0.5801 0.6977 0.061 Uiso 1 1 calc R U . . .
C17 C 0.7445(6) 0.4323(4) 0.5572(4) 0.0265(14) Uani 1 1 d . . . . .
H17A H 0.6891 0.4723 0.5553 0.040 Uiso 1 1 calc R U . . .
H17B H 0.7381 0.3840 0.5173 0.040 Uiso 1 1 calc R U . . .
H17C H 0.8014 0.4682 0.5463 0.040 Uiso 1 1 calc R U . . .
C18 C 0.9195(6) -0.0136(6) 0.5559(5) 0.0285(16) Uani 1 1 d . . . . .
H18 H 0.9537 0.0419 0.5498 0.034 Uiso 1 1 calc R U . . .
C19 C 0.9697(6) -0.0970(6) 0.5560(5) 0.0353(19) Uani 1 1 d . . . . .
H19 H 1.0363 -0.0982 0.5499 0.042 Uiso 1 1 calc R U . . .
C20 C 0.9184(7) -0.1772(6) 0.5652(5) 0.037(2) Uani 1 1 d . . . . .
H20 H 0.9498 -0.2345 0.5673 0.045 Uiso 1 1 calc R U . . .
C21 C 0.8237(6) -0.1731(5) 0.5711(4) 0.0331(18) Uani 1 1 d . . . . .
H21 H 0.7888 -0.2281 0.5770 0.040 Uiso 1 1 calc R U . . .
C22 C 0.7758(5) -0.0897(4) 0.5688(4) 0.0235(15) Uani 1 1 d . . . . .
C23 C 0.6725(5) -0.0792(5) 0.5733(4) 0.0231(15) Uani 1 1 d . . . . .
C24 C 0.6103(6) -0.1546(5) 0.5735(5) 0.0278(16) Uani 1 1 d . . . . .
H24 H 0.6347 -0.2151 0.5732 0.033 Uiso 1 1 calc R U . . .
C25 C 0.5163(6) -0.1406(6) 0.5741(5) 0.0324(17) Uani 1 1 d . . . . .
H25 H 0.4741 -0.1911 0.5745 0.039 Uiso 1 1 calc R U . . .
C26 C 0.4821(6) -0.0520(6) 0.5742(5) 0.0327(17) Uani 1 1 d . . . . .
H26 H 0.4160 -0.0408 0.5740 0.039 Uiso 1 1 calc R U . . .
C27 C 0.5450(5) 0.0195(5) 0.5745(5) 0.0264(15) Uani 1 1 d . . . . .
H27 H 0.5210 0.0803 0.5746 0.032 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
Cu1 N6 2.082(6) . ?
Cu1 N5 2.086(6) . ?
Cu1 P1 2.1963(16) . ?
Cu1 I1 2.6159(8) . ?
P1 N1 1.645(5) . ?
P1 N2 1.744(6) . ?
P1 N3 1.758(6) . ?
P2 N4 1.622(5) . ?
P2 N2 1.637(6) . ?
P2 N3 1.642(6) . ?
P2 C17 1.843(7) . ?
N1 C1 1.486(8) . ?
N1 H1N 0.9100 . ?
N2 C5 1.488(9) . ?
N3 C9 1.490(8) . ?
N4 C13 1.510(8) . ?
N4 H4N 0.9101 . ?
N5 C18 1.336(10) . ?
N5 C22 1.373(9) . ?
N6 C23 1.347(9) . ?
N6 C27 1.351(9) . ?
C1 C3 1.509(9) . ?
C1 C4 1.525(12) . ?
C1 C2 1.528(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 C7 1.518(11) . ?
C5 C8 1.523(11) . ?
C5 C6 1.530(10) . ?
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 C11 1.522(10) . ?
C9 C10 1.529(11) . ?
C9 C12 1.537(10) . ?
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 C16 1.504(12) . ?
C13 C15 1.519(10) . ?
C13 C14 1.521(12) . ?
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 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.411(11) . ?
C18 H18 0.9500 . ?
C19 C20 1.388(13) . ?
C19 H19 0.9500 . ?
C20 C21 1.347(12) . ?
C20 H20 0.9500 . ?
C21 C22 1.395(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.473(11) . ?
C23 C24 1.410(10) . ?
C24 C25 1.348(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.383(12) . ?
C25 H25 0.9500 . ?
C26 C27 1.374(10) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Cu1 N5 79.3(2) . . ?
N6 Cu1 P1 122.84(19) . . ?
N5 Cu1 P1 126.28(18) . . ?
N6 Cu1 I1 110.79(19) . . ?
N5 Cu1 I1 103.41(18) . . ?
P1 Cu1 I1 110.14(5) . . ?
N1 P1 N2 105.2(3) . . ?
N1 P1 N3 106.6(3) . . ?
N2 P1 N3 79.6(2) . . ?
N1 P1 Cu1 122.1(2) . . ?
N2 P1 Cu1 117.6(2) . . ?
N3 P1 Cu1 117.4(2) . . ?
N4 P2 N2 116.3(3) . . ?
N4 P2 N3 115.0(3) . . ?
N2 P2 N3 86.3(3) . . ?
N4 P2 C17 109.6(3) . . ?
N2 P2 C17 113.9(3) . . ?
N3 P2 C17 114.3(3) . . ?
C1 N1 P1 134.6(4) . . ?
C1 N1 H1N 124.3 . . ?
P1 N1 H1N 100.6 . . ?
C5 N2 P2 131.8(5) . . ?
C5 N2 P1 130.8(5) . . ?
P2 N2 P1 97.3(3) . . ?
C9 N3 P2 131.6(5) . . ?
C9 N3 P1 128.8(5) . . ?
P2 N3 P1 96.6(3) . . ?
C13 N4 P2 136.0(4) . . ?
C13 N4 H4N 111.4 . . ?
P2 N4 H4N 112.6 . . ?
C18 N5 C22 118.8(6) . . ?
C18 N5 Cu1 127.2(5) . . ?
C22 N5 Cu1 113.9(5) . . ?
C23 N6 C27 118.1(6) . . ?
C23 N6 Cu1 114.5(5) . . ?
C27 N6 Cu1 127.4(5) . . ?
N1 C1 C3 112.2(5) . . ?
N1 C1 C4 107.6(6) . . ?
C3 C1 C4 109.4(7) . . ?
N1 C1 C2 107.0(6) . . ?
C3 C1 C2 110.4(7) . . ?
C4 C1 C2 110.2(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 C7 109.1(6) . . ?
N2 C5 C8 107.7(6) . . ?
C7 C5 C8 108.9(6) . . ?
N2 C5 C6 110.1(6) . . ?
C7 C5 C6 110.9(7) . . ?
C8 C5 C6 110.0(7) . . ?
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 C11 110.2(6) . . ?
N3 C9 C10 107.8(6) . . ?
C11 C9 C10 111.2(6) . . ?
N3 C9 C12 109.2(6) . . ?
C11 C9 C12 109.5(6) . . ?
C10 C9 C12 108.9(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 . . ?
C16 C13 N4 112.5(7) . . ?
C16 C13 C15 110.3(8) . . ?
N4 C13 C15 104.6(6) . . ?
C16 C13 C14 110.4(7) . . ?
N4 C13 C14 110.1(6) . . ?
C15 C13 C14 108.8(9) . . ?
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 . . ?
P2 C17 H17A 109.5 . . ?
P2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N5 C18 C19 122.6(8) . . ?
N5 C18 H18 118.7 . . ?
C19 C18 H18 118.7 . . ?
C20 C19 C18 117.7(8) . . ?
C20 C19 H19 121.1 . . ?
C18 C19 H19 121.1 . . ?
C21 C20 C19 119.5(8) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 121.5(8) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
N5 C22 C21 119.7(7) . . ?
N5 C22 C23 115.3(6) . . ?
C21 C22 C23 125.0(7) . . ?
N6 C23 C24 120.9(7) . . ?
N6 C23 C22 116.4(7) . . ?
C24 C23 C22 122.6(7) . . ?
C25 C24 C23 120.0(7) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 119.3(7) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C27 C26 C25 119.0(8) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
N6 C27 C26 122.8(7) . . ?
N6 C27 H27 118.6 . . ?
C26 C27 H27 118.6 . . ?

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 I2 0.91 2.83 3.741(5) 175 .
N1 H1N I2 0.91 2.83 3.675(5) 155 .

_refine_diff_density_max         2.502
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.119

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 991951'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_msb372_a

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
Iodo(1,10-phenanthroline-\kN:\kN')(1,3-di-<i>tert</i>-
butyl-2,4-bis(tert-butylamino)-2-methyl-[1,3,2,4]
diazadiphosphetidin-2-ium-\kP)copper(I) Iodide 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H49 Cu I N6 P2, I'
_chemical_formula_sum            'C29 H49 Cu I2 N6 P2'
_chemical_formula_weight         861.02

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'
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'
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                   24.7202(11)
_cell_length_b                   10.1169(4)
_cell_length_c                   14.2381(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3560.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9717
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      29.19

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_F_000             1720
_exptl_transmission_factor_min   0.802
_exptl_transmission_factor_max   0.914
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    2.465
_shelx_estimated_absorpt_T_min   0.567
_shelx_estimated_absorpt_T_max   0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2013b)'
_exptl_absorpt_correction_T_min  0.68
_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°.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62138
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.013
_diffrn_reflns_theta_max         29.191
_diffrn_reflns_theta_full        29.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             9502
_reflns_number_gt                8952
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_max     0.979
_reflns_Friedel_fraction_full    0.989

_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 AXS, 2006)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2013a)'
_computing_data_reduction        'SAINT  (Bruker AXS, 2013a)'
_computing_structure_solution    'SHELXT (Bruker AXS 2013c)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker AXS, 2008)'

_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 bound to carbon
 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 atoms. Those attached to nitrogen (H1n and H4n)
 were placed in locations obtained from a difference map, their parameters 
 adjusted to give N---H = 0.91 Å and included as riding contributions with
 isotropic displacement parameters 1.2 times those of the attached atoms.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0188P)²+1.4760P] 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 
;
 Flack x determined using 4035 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons & Flack, 2004).
;
_refine_ls_abs_structure_Flack   -0.005(5)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         9502
_refine_ls_number_parameters     374
_refine_ls_number_restraints     122
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_ref         0.0487
_refine_ls_wR_factor_gt          0.0470
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.055
_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
I1 I 0.28821(2) 0.17081(2) 0.90628(2) 0.01937(6) Uani 1 1 d . U . . .
Cu1 Cu 0.30555(2) 0.34158(4) 0.77254(3) 0.01324(9) Uani 1 1 d . U . . .
P1 P 0.37396(4) 0.27217(9) 0.68765(6) 0.01047(18) Uani 1 1 d . U . . .
P2 P 0.43989(4) 0.09316(10) 0.74012(6) 0.01127(18) Uani 1 1 d . U . . .
N1 N 0.39019(13) 0.3319(3) 0.5843(2) 0.0140(6) Uani 1 1 d . U . . .
H1N H 0.4245 0.3097 0.5677 0.017 Uiso 1 1 d R U . . .
N2 N 0.38382(12) 0.1014(3) 0.6776(2) 0.0113(6) Uani 1 1 d . U . . .
N3 N 0.43562(12) 0.2547(3) 0.7476(2) 0.0101(6) Uani 1 1 d . U . . .
N4 N 0.49398(13) 0.0415(3) 0.6876(2) 0.0131(6) Uani 1 1 d . U . . .
H4N H 0.5025 0.0999 0.6412 0.016 Uiso 1 1 d R U . . .
N5 N 0.23028(13) 0.3955(3) 0.7188(2) 0.0143(6) Uani 1 1 d . U . . .
N6 N 0.29749(12) 0.5302(3) 0.8339(2) 0.0140(6) Uani 1 1 d . U . . .
C1 C 0.36825(15) 0.4383(4) 0.5234(2) 0.0145(7) Uani 1 1 d . U . . .
C2 C 0.37090(18) 0.3867(5) 0.4224(3) 0.0230(9) Uani 1 1 d . U . . .
H2A H 0.4078 0.3575 0.4084 0.035 Uiso 1 1 calc R U . . .
H2B H 0.3606 0.4575 0.3789 0.035 Uiso 1 1 calc R U . . .
H2C H 0.3459 0.3122 0.4152 0.035 Uiso 1 1 calc R U . . .
C3 C 0.30999(17) 0.4732(5) 0.5476(3) 0.0246(9) Uani 1 1 d . U . . .
H3A H 0.2872 0.3943 0.5412 0.037 Uiso 1 1 calc R U . . .
H3B H 0.2970 0.5421 0.5048 0.037 Uiso 1 1 calc R U . . .
H3C H 0.3082 0.5055 0.6124 0.037 Uiso 1 1 calc R U . . .
C4 C 0.40395(17) 0.5615(4) 0.5333(3) 0.0215(9) Uani 1 1 d . U . . .
H4A H 0.4021 0.5942 0.5980 0.032 Uiso 1 1 calc R U . . .
H4B H 0.3911 0.6302 0.4902 0.032 Uiso 1 1 calc R U . . .
H4C H 0.4415 0.5387 0.5180 0.032 Uiso 1 1 calc R U . . .
C5 C 0.35218(16) 0.0003(4) 0.6259(3) 0.0153(7) Uani 1 1 d . U . . .
C6 C 0.37575(19) -0.0162(5) 0.5271(3) 0.0255(10) Uani 1 1 d . U . . .
H6A H 0.3744 0.0688 0.4941 0.038 Uiso 1 1 calc R U . . .
H6B H 0.3545 -0.0817 0.4924 0.038 Uiso 1 1 calc R U . . .
H6C H 0.4134 -0.0460 0.5317 0.038 Uiso 1 1 calc R U . . .
C7 C 0.35408(18) -0.1296(4) 0.6794(3) 0.0221(9) Uani 1 1 d . U . . .
H7A H 0.3914 -0.1620 0.6814 0.033 Uiso 1 1 calc R U . . .
H7B H 0.3311 -0.1948 0.6477 0.033 Uiso 1 1 calc R U . . .
H7C H 0.3409 -0.1158 0.7436 0.033 Uiso 1 1 calc R U . . .
C8 C 0.29365(16) 0.0479(4) 0.6202(3) 0.0220(9) Uani 1 1 d . U . . .
H8A H 0.2793 0.0601 0.6838 0.033 Uiso 1 1 calc R U . . .
H8B H 0.2718 -0.0180 0.5870 0.033 Uiso 1 1 calc R U . . .
H8C H 0.2923 0.1320 0.5863 0.033 Uiso 1 1 calc R U . . .
C9 C 0.46379(16) 0.3520(4) 0.8091(3) 0.0141(7) Uani 1 1 d . U . . .
C10 C 0.45347(17) 0.4902(4) 0.7694(3) 0.0189(8) Uani 1 1 d . U . . .
H10A H 0.4689 0.5565 0.8119 0.028 Uiso 1 1 calc R U . . .
H10B H 0.4144 0.5047 0.7636 0.028 Uiso 1 1 calc R U . . .
H10C H 0.4705 0.4979 0.7075 0.028 Uiso 1 1 calc R U . . .
C11 C 0.44207(16) 0.3427(4) 0.9096(3) 0.0173(7) Uani 1 1 d . U . . .
H11A H 0.4537 0.2590 0.9378 0.026 Uiso 1 1 calc R U . . .
H11B H 0.4025 0.3465 0.9085 0.026 Uiso 1 1 calc R U . . .
H11C H 0.4562 0.4165 0.9468 0.026 Uiso 1 1 calc R U . . .
C12 C 0.52438(16) 0.3242(4) 0.8066(3) 0.0211(9) Uani 1 1 d . U . . .
H12A H 0.5316 0.2377 0.8350 0.032 Uiso 1 1 calc R U . . .
H12B H 0.5436 0.3929 0.8418 0.032 Uiso 1 1 calc R U . . .
H12C H 0.5369 0.3240 0.7413 0.032 Uiso 1 1 calc R U . . .
C13 C 0.53502(16) -0.0666(4) 0.7036(3) 0.0161(8) Uani 1 1 d . U . . .
C14 C 0.50884(19) -0.2026(4) 0.6965(4) 0.0301(11) Uani 1 1 d . U . . .
H14A H 0.4815 -0.2121 0.7459 0.045 Uiso 1 1 calc R U . . .
H14B H 0.5366 -0.2710 0.7041 0.045 Uiso 1 1 calc R U . . .
H14C H 0.4916 -0.2122 0.6349 0.045 Uiso 1 1 calc R U . . .
C15 C 0.57672(17) -0.0507(4) 0.6255(3) 0.0214(9) Uani 1 1 d . U . . .
H15A H 0.5591 -0.0630 0.5645 0.032 Uiso 1 1 calc R U . . .
H15B H 0.6053 -0.1169 0.6333 0.032 Uiso 1 1 calc R U . . .
H15C H 0.5925 0.0380 0.6286 0.032 Uiso 1 1 calc R U . . .
C16 C 0.56375(18) -0.0514(5) 0.7984(3) 0.0261(10) Uani 1 1 d . U . . .
H16A H 0.5784 0.0383 0.8038 0.039 Uiso 1 1 calc R U . . .
H16B H 0.5933 -0.1156 0.8027 0.039 Uiso 1 1 calc R U . . .
H16C H 0.5379 -0.0671 0.8494 0.039 Uiso 1 1 calc R U . . .
C17 C 0.43178(16) 0.0091(4) 0.8489(3) 0.0170(8) Uani 1 1 d . U . . .
H17A H 0.4320 -0.0866 0.8380 0.025 Uiso 1 1 calc R U . . .
H17B H 0.3973 0.0347 0.8776 0.025 Uiso 1 1 calc R U . . .
H17C H 0.4615 0.0327 0.8912 0.025 Uiso 1 1 calc R U . . .
C18 C 0.19770(16) 0.3284(4) 0.6619(3) 0.0177(8) Uani 1 1 d . U . . .
H18 H 0.2058 0.2384 0.6492 0.021 Uiso 1 1 calc R U . . .
C19 C 0.15181(17) 0.3850(4) 0.6199(3) 0.0205(8) Uani 1 1 d . U . . .
H19 H 0.1302 0.3346 0.5779 0.025 Uiso 1 1 calc R U . . .
C20 C 0.13847(16) 0.5132(4) 0.6397(3) 0.0217(9) Uani 1 1 d . U . . .
H20 H 0.1074 0.5525 0.6121 0.026 Uiso 1 1 calc R U . . .
C21 C 0.17130(16) 0.5860(4) 0.7013(3) 0.0172(8) Uani 1 1 d . U . . .
C22 C 0.16033(17) 0.7210(4) 0.7275(3) 0.0233(9) Uani 1 1 d . U . . .
H22 H 0.1301 0.7651 0.7008 0.028 Uiso 1 1 calc R U . . .
C23 C 0.19203(18) 0.7862(4) 0.7890(3) 0.0238(9) Uani 1 1 d . U . . .
H23 H 0.1835 0.8746 0.8058 0.029 Uiso 1 1 calc R U . . .
C24 C 0.23877(16) 0.7232(4) 0.8298(3) 0.0178(8) Uani 1 1 d . U . . .
C25 C 0.27201(17) 0.7855(4) 0.8965(3) 0.0232(9) Uani 1 1 d . U . . .
H25 H 0.2636 0.8717 0.9184 0.028 Uiso 1 1 calc R U . . .
C26 C 0.31663(18) 0.7205(4) 0.9295(3) 0.0218(9) Uani 1 1 d . U . . .
H26 H 0.3395 0.7609 0.9748 0.026 Uiso 1 1 calc R U . . .
C27 C 0.32800(16) 0.5934(4) 0.8955(3) 0.0193(8) Uani 1 1 d . U . . .
H27 H 0.3595 0.5501 0.9182 0.023 Uiso 1 1 calc R U . . .
C28 C 0.25220(16) 0.5934(4) 0.8022(3) 0.0142(7) Uani 1 1 d . U . . .
C29 C 0.21727(15) 0.5234(4) 0.7390(3) 0.0138(7) Uani 1 1 d . U . . .
I2 I 0.52795(2) 0.27563(2) 0.50442(2) 0.01598(5) 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 Cu1 2.6067(5) . ?
Cu1 N5 2.085(3) . ?
Cu1 N6 2.108(3) . ?
Cu1 P1 2.1939(10) . ?
P1 N1 1.640(3) . ?
P1 N2 1.751(3) . ?
P1 N3 1.756(3) . ?
P2 N4 1.619(3) . ?
P2 N3 1.641(3) . ?
P2 N2 1.649(3) . ?
P2 C17 1.779(4) . ?
N1 C1 1.485(4) . ?
N1 H1N 0.9100 . ?
N2 C5 1.483(5) . ?
N3 C9 1.490(5) . ?
N4 C13 1.509(5) . ?
N4 H4N 0.9098 . ?
N5 C18 1.328(5) . ?
N5 C29 1.364(5) . ?
N6 C27 1.322(5) . ?
N6 C28 1.366(5) . ?
C1 C3 1.522(5) . ?
C1 C2 1.531(5) . ?
C1 C4 1.533(6) . ?
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 1.519(5) . ?
C5 C8 1.527(5) . ?
C5 C6 1.532(5) . ?
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 C12 1.525(5) . ?
C9 C10 1.529(5) . ?
C9 C11 1.532(5) . ?
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 1.524(6) . ?
C13 C15 1.524(5) . ?
C13 C16 1.533(6) . ?
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 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.405(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.367(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.404(6) . ?
C20 H20 0.9500 . ?
C21 C29 1.407(5) . ?
C21 C22 1.442(6) . ?
C22 C23 1.348(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.441(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.405(6) . ?
C24 C28 1.410(5) . ?
C25 C26 1.367(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.403(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.435(5) . ?

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
N5 Cu1 N6 80.27(12) . . ?
N5 Cu1 P1 124.70(9) . . ?
N6 Cu1 P1 126.22(9) . . ?
N5 Cu1 I1 107.16(9) . . ?
N6 Cu1 I1 106.35(9) . . ?
P1 Cu1 I1 108.49(3) . . ?
N1 P1 N2 104.87(16) . . ?
N1 P1 N3 105.10(16) . . ?
N2 P1 N3 79.59(14) . . ?
N1 P1 Cu1 124.38(12) . . ?
N2 P1 Cu1 117.91(11) . . ?
N3 P1 Cu1 115.71(11) . . ?
N4 P2 N3 113.85(17) . . ?
N4 P2 N2 117.48(16) . . ?
N3 P2 N2 86.02(15) . . ?
N4 P2 C17 109.94(18) . . ?
N3 P2 C17 114.38(18) . . ?
N2 P2 C17 113.54(18) . . ?
C1 N1 P1 134.6(3) . . ?
C1 N1 H1N 111.6 . . ?
P1 N1 H1N 111.7 . . ?
C5 N2 P2 132.5(3) . . ?
C5 N2 P1 130.4(2) . . ?
P2 N2 P1 97.07(16) . . ?
C9 N3 P2 131.8(3) . . ?
C9 N3 P1 128.6(2) . . ?
P2 N3 P1 97.16(16) . . ?
C13 N4 P2 136.0(3) . . ?
C13 N4 H4N 115.1 . . ?
P2 N4 H4N 108.5 . . ?
C18 N5 C29 118.0(3) . . ?
C18 N5 Cu1 129.1(3) . . ?
C29 N5 Cu1 112.4(2) . . ?
C27 N6 C28 117.4(3) . . ?
C27 N6 Cu1 131.2(3) . . ?
C28 N6 Cu1 111.4(2) . . ?
N1 C1 C3 112.4(3) . . ?
N1 C1 C2 106.6(3) . . ?
C3 C1 C2 109.4(3) . . ?
N1 C1 C4 109.0(3) . . ?
C3 C1 C4 109.6(3) . . ?
C2 C1 C4 109.8(3) . . ?
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 109.4(3) . . ?
N2 C5 C8 108.0(3) . . ?
C7 C5 C8 109.2(3) . . ?
N2 C5 C6 109.3(3) . . ?
C7 C5 C6 110.8(3) . . ?
C8 C5 C6 110.2(3) . . ?
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 C12 108.9(3) . . ?
N3 C9 C10 108.0(3) . . ?
C12 C9 C10 108.9(3) . . ?
N3 C9 C11 110.1(3) . . ?
C12 C9 C11 110.8(3) . . ?
C10 C9 C11 110.1(3) . . ?
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 111.0(3) . . ?
N4 C13 C15 105.5(3) . . ?
C14 C13 C15 109.5(4) . . ?
N4 C13 C16 111.8(3) . . ?
C14 C13 C16 110.3(4) . . ?
C15 C13 C16 108.5(3) . . ?
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 . . ?
P2 C17 H17A 109.5 . . ?
P2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N5 C18 C19 122.8(4) . . ?
N5 C18 H18 118.6 . . ?
C19 C18 H18 118.6 . . ?
C20 C19 C18 119.6(4) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 119.1(4) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C20 C21 C29 118.0(4) . . ?
C20 C21 C22 123.4(4) . . ?
C29 C21 C22 118.7(4) . . ?
C23 C22 C21 121.5(4) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C22 C23 C24 120.8(4) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C25 C24 C28 117.9(4) . . ?
C25 C24 C23 122.9(4) . . ?
C28 C24 C23 119.2(4) . . ?
C26 C25 C24 119.3(4) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C25 C26 C27 118.9(4) . . ?
C25 C26 H26 120.5 . . ?
C27 C26 H26 120.5 . . ?
N6 C27 C26 123.9(4) . . ?
N6 C27 H27 118.0 . . ?
C26 C27 H27 118.0 . . ?
N6 C28 C24 122.5(3) . . ?
N6 C28 C29 118.0(3) . . ?
C24 C28 C29 119.5(4) . . ?
N5 C29 C21 122.5(4) . . ?
N5 C29 C28 117.3(3) . . ?
C21 C29 C28 120.2(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
N1 H1N I2 0.91 2.73 3.635(3) 172 .
N4 H4N I2 0.91 2.71 3.622(3) 179 .

_refine_diff_density_max         0.898
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.082

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 991952'
#######################################################################
#
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  to carry out CIF format checking respectively.
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data_msb657_0m_a_sq_s

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
Chlorido{1,3-di-tert-butylbis(tert-butylamino)-2-methyl-1,3,2,4-
diazadiphosphetidin-2-ium}gold(I) trifluoromethanesulfonate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H41 Au Cl N4 P2, C F3 O3 S'
_chemical_formula_sum            'C18 H41 Au Cl F3 N4 O3 P2 S'
_chemical_formula_weight         744.96

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'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.714(3)
_cell_length_b                   10.396(3)
_cell_length_c                   17.440(6)
_cell_angle_alpha                81.865(4)
_cell_angle_beta                 85.488(4)
_cell_angle_gamma                62.617(4)
_cell_volume                     1547.9(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9890
_cell_measurement_theta_min      2.388
_cell_measurement_theta_max      29.492

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_F_000             740
_exptl_transmission_factor_min   0.254
_exptl_transmission_factor_max   0.496
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    5.051
_shelx_estimated_absorpt_T_min   0.390
_shelx_estimated_absorpt_T_max   0.606
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2013b)'
_exptl_absorpt_correction_T_min  0.31
_exptl_absorpt_correction_T_max  0.61

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, colllected 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 10 sec/frame.
;

_diffrn_ambient_temperature      150(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            27070
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.222
_diffrn_reflns_theta_max         29.492
_diffrn_reflns_theta_full        28.000
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             8002
_reflns_number_gt                7522
_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 AXS, 2013)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2013a)'
_computing_data_reduction        'SAINT (Bruker AXS, 2013a)'
_computing_structure_solution    'SHELXT (Bruker AXS 2013c)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker AXS, 2008)'

_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 = 0.98 Å) while those 
attached to nitrogen were placed in locations derived from a difference 
map and their coordiantes 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 tert-butyl 
group C13--C16 is rotationally disordered over two sites. It was refined 
with restraints that the two components of the disorder have comparable 
geometries. A region of density well removed from the main portions of 
the molecule defied reasonable attempts to model it as disordered 
solvent dichloromethane and so was removed with the SQUEEZE 
option of PLATON (Spek, 2013).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0484P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8002
_refine_ls_number_parameters     318
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0873
_refine_ls_wR_factor_gt          0.0857
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.043
_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
Au1 Au 0.72467(2) 0.84840(2) 0.54898(2) 0.01929(5) Uani 1 1 d . . . . .
Cl1 Cl 0.66186(12) 0.89316(10) 0.42045(5) 0.0332(2) Uani 1 1 d . . . . .
P1 P 0.79646(9) 0.81073(8) 0.67091(5) 0.01602(15) Uani 1 1 d . . . . .
P2 P 0.70962(9) 1.00107(8) 0.76296(5) 0.01823(16) Uani 1 1 d . . . . .
N1 N 0.9212(3) 0.6466(3) 0.70300(16) 0.0205(5) Uani 1 1 d . . . . .
H1 H 0.9669 0.6363 0.7486 0.025 Uiso 1 1 d R U . . .
N2 N 0.8500(3) 0.9354(3) 0.69696(15) 0.0169(5) Uani 1 1 d . . . . .
N3 N 0.6577(3) 0.8798(3) 0.74107(15) 0.0186(5) Uani 1 1 d . . . . .
N4 N 0.7680(3) 0.9787(3) 0.84971(16) 0.0237(6) Uani 1 1 d D . . . .
H4 H 0.8493 0.8888 0.8608 0.028 Uiso 1 1 d R U . . .
C1 C 0.9993(4) 0.5082(3) 0.6652(2) 0.0268(7) Uani 1 1 d . . . . .
C2 C 0.8780(5) 0.4669(4) 0.6394(3) 0.0400(10) Uani 1 1 d . . . . .
H2A H 0.8198 0.4499 0.6848 0.060 Uiso 1 1 calc R U . . .
H2B H 0.9307 0.3780 0.6138 0.060 Uiso 1 1 calc R U . . .
H2C H 0.8065 0.5466 0.6031 0.060 Uiso 1 1 calc R U . . .
C3 C 1.1003(5) 0.3909(4) 0.7277(3) 0.0426(10) Uani 1 1 d . . . . .
H3A H 1.1760 0.4180 0.7450 0.064 Uiso 1 1 calc R U . . .
H3B H 1.1550 0.2973 0.7065 0.064 Uiso 1 1 calc R U . . .
H3C H 1.0348 0.3819 0.7717 0.064 Uiso 1 1 calc R U . . .
C4 C 1.0990(6) 0.5241(4) 0.5955(3) 0.0483(12) Uani 1 1 d . . . . .
H4A H 1.0342 0.6063 0.5583 0.072 Uiso 1 1 calc R U . . .
H4B H 1.1451 0.4343 0.5706 0.072 Uiso 1 1 calc R U . . .
H4C H 1.1816 0.5417 0.6131 0.072 Uiso 1 1 calc R U . . .
C5 C 0.9612(4) 0.9879(3) 0.65847(19) 0.0207(6) Uani 1 1 d . . . . .
C6 C 0.8848(4) 1.1027(4) 0.5893(2) 0.0280(7) Uani 1 1 d . . . . .
H6A H 0.8501 1.0608 0.5526 0.042 Uiso 1 1 calc R U . . .
H6B H 0.9599 1.1336 0.5635 0.042 Uiso 1 1 calc R U . . .
H6C H 0.7954 1.1873 0.6075 0.042 Uiso 1 1 calc R U . . .
C7 C 1.1023(4) 0.8572(4) 0.6309(2) 0.0259(7) Uani 1 1 d . . . . .
H7A H 1.1490 0.7831 0.6751 0.039 Uiso 1 1 calc R U . . .
H7B H 1.1784 0.8886 0.6071 0.039 Uiso 1 1 calc R U . . .
H7C H 1.0703 0.8160 0.5927 0.039 Uiso 1 1 calc R U . . .
C8 C 1.0106(4) 1.0530(4) 0.7182(2) 0.0289(7) Uani 1 1 d . . . . .
H8A H 0.9200 1.1384 0.7349 0.043 Uiso 1 1 calc R U . . .
H8B H 1.0884 1.0825 0.6948 0.043 Uiso 1 1 calc R U . . .
H8C H 1.0549 0.9798 0.7631 0.043 Uiso 1 1 calc R U . . .
C9 C 0.5451(4) 0.8270(4) 0.77946(19) 0.0240(6) Uani 1 1 d . . . . .
C10 C 0.5002(4) 0.7584(4) 0.7205(2) 0.0308(8) Uani 1 1 d . . . . .
H10A H 0.4511 0.8315 0.6762 0.046 Uiso 1 1 calc R U . . .
H10B H 0.4274 0.7231 0.7446 0.046 Uiso 1 1 calc R U . . .
H10C H 0.5933 0.6765 0.7028 0.046 Uiso 1 1 calc R U . . .
C11 C 0.6213(5) 0.7143(5) 0.8498(2) 0.0384(9) Uani 1 1 d . . . . .
H11A H 0.7138 0.6311 0.8326 0.058 Uiso 1 1 calc R U . . .
H11B H 0.5477 0.6807 0.8746 0.058 Uiso 1 1 calc R U . . .
H11C H 0.6510 0.7593 0.8868 0.058 Uiso 1 1 calc R U . . .
C12 C 0.4019(4) 0.9575(5) 0.8047(2) 0.0365(9) Uani 1 1 d . . . . .
H12A H 0.4311 1.0022 0.8422 0.055 Uiso 1 1 calc R U . . .
H12B H 0.3264 0.9256 0.8286 0.055 Uiso 1 1 calc R U . . .
H12C H 0.3558 1.0292 0.7594 0.055 Uiso 1 1 calc R U . . .
C13 C 0.7344(4) 1.0714(4) 0.9148(2) 0.0353(8) Uani 1 1 d D . . . .
C14 C 0.8066(16) 0.9621(13) 0.9869(6) 0.040(2) Uani 0.553(19) 1 d D U P A 1
H14A H 0.9171 0.9008 0.9769 0.059 Uiso 0.553(19) 1 calc R U P A 1
H14B H 0.7541 0.9004 0.9987 0.059 Uiso 0.553(19) 1 calc R U P A 1
H14C H 0.7947 1.0153 1.0311 0.059 Uiso 0.553(19) 1 calc R U P A 1
C15 C 0.5656(9) 1.1699(13) 0.9274(6) 0.048(2) Uani 0.553(19) 1 d D U P A 1
H15A H 0.5242 1.2395 0.8809 0.071 Uiso 0.553(19) 1 calc R U P A 1
H15B H 0.5530 1.2232 0.9717 0.071 Uiso 0.553(19) 1 calc R U P A 1
H15C H 0.5093 1.1114 0.9380 0.071 Uiso 0.553(19) 1 calc R U P A 1
C16 C 0.8249(16) 1.1634(13) 0.8972(7) 0.045(2) Uani 0.553(19) 1 d D U P A 1
H16A H 0.9356 1.0981 0.8906 0.068 Uiso 0.553(19) 1 calc R U P A 1
H16B H 0.8102 1.2199 0.9403 0.068 Uiso 0.553(19) 1 calc R U P A 1
H16C H 0.7860 1.2301 0.8495 0.068 Uiso 0.553(19) 1 calc R U P A 1
C14A C 0.834(2) 0.9668(17) 0.9831(7) 0.040(2) Uani 0.447(19) 1 d D U P A 2
H14D H 0.8071 0.8861 0.9961 0.059 Uiso 0.447(19) 1 calc R U P A 2
H14E H 0.8138 1.0198 1.0282 0.059 Uiso 0.447(19) 1 calc R U P A 2
H14F H 0.9439 0.9280 0.9684 0.059 Uiso 0.447(19) 1 calc R U P A 2
C15A C 0.5600(10) 1.1207(17) 0.9402(8) 0.048(2) Uani 0.447(19) 1 d D U P A 2
H15D H 0.5435 1.0344 0.9556 0.071 Uiso 0.447(19) 1 calc R U P A 2
H15E H 0.4926 1.1809 0.8968 0.071 Uiso 0.447(19) 1 calc R U P A 2
H15F H 0.5353 1.1776 0.9841 0.071 Uiso 0.447(19) 1 calc R U P A 2
C16A C 0.768(2) 1.1984(13) 0.8949(9) 0.045(2) Uani 0.447(19) 1 d D U P A 2
H16D H 0.7044 1.2621 0.8510 0.068 Uiso 0.447(19) 1 calc R U P A 2
H16E H 0.8778 1.1637 0.8811 0.068 Uiso 0.447(19) 1 calc R U P A 2
H16F H 0.7432 1.2531 0.9397 0.068 Uiso 0.447(19) 1 calc R U P A 2
C17 C 0.5680(4) 1.1846(4) 0.7364(2) 0.0309(8) Uani 1 1 d . . . . .
H17A H 0.4767 1.2076 0.7706 0.046 Uiso 1 1 calc R U . . .
H17B H 0.5377 1.1960 0.6827 0.046 Uiso 1 1 calc R U . . .
H17C H 0.6118 1.2511 0.7415 0.046 Uiso 1 1 calc R U . . .
S1 S 0.17675(10) 0.64655(9) 0.86695(5) 0.02615(18) Uani 1 1 d . . . . .
O1 O 0.1938(4) 0.7679(3) 0.88694(18) 0.0401(7) Uani 1 1 d . . . . .
O2 O 0.0175(3) 0.6809(3) 0.85115(16) 0.0333(6) Uani 1 1 d . . . . .
O3 O 0.2906(4) 0.5576(4) 0.81413(18) 0.0438(7) Uani 1 1 d . . . . .
C18 C 0.2145(4) 0.5257(4) 0.9581(2) 0.0305(8) Uani 1 1 d . . . . .
F1 F 0.3547(3) 0.4898(3) 0.98345(17) 0.0519(7) Uani 1 1 d . . . . .
F2 F 0.1110(3) 0.5893(3) 1.01302(14) 0.0483(6) Uani 1 1 d . . . . .
F3 F 0.2089(3) 0.4027(2) 0.94837(17) 0.0479(6) 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
Au1 P1 2.2155(11) . ?
Au1 Cl1 2.2960(11) . ?
P1 N1 1.621(3) . ?
P1 N3 1.711(3) . ?
P1 N2 1.726(3) . ?
P2 N4 1.606(3) . ?
P2 N3 1.656(3) . ?
P2 N2 1.664(3) . ?
P2 C17 1.784(3) . ?
N1 C1 1.505(4) . ?
N1 H1 0.9099 . ?
N2 C5 1.497(4) . ?
N3 C9 1.510(4) . ?
N4 C13 1.513(4) . ?
N4 H4 0.9100 . ?
C1 C3 1.527(5) . ?
C1 C4 1.532(6) . ?
C1 C2 1.542(5) . ?
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 1.525(4) . ?
C5 C8 1.533(5) . ?
C5 C6 1.533(4) . ?
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 C12 1.519(5) . ?
C9 C10 1.523(5) . ?
C9 C11 1.537(5) . ?
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 C16A 1.489(9) . ?
C13 C15 1.499(8) . ?
C13 C14 1.538(8) . ?
C13 C14A 1.544(9) . ?
C13 C16 1.559(8) . ?
C13 C15A 1.574(9) . ?
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 . ?
C14A H14D 0.9800 . ?
C14A H14E 0.9800 . ?
C14A H14F 0.9800 . ?
C15A H15D 0.9800 . ?
C15A H15E 0.9800 . ?
C15A H15F 0.9800 . ?
C16A H16D 0.9800 . ?
C16A H16E 0.9800 . ?
C16A H16F 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
S1 O1 1.437(3) . ?
S1 O3 1.438(3) . ?
S1 O2 1.459(3) . ?
S1 C18 1.828(4) . ?
C18 F1 1.330(4) . ?
C18 F2 1.335(5) . ?
C18 F3 1.339(4) . ?

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
P1 Au1 Cl1 176.26(3) . . ?
N1 P1 N3 108.87(14) . . ?
N1 P1 N2 109.92(14) . . ?
N3 P1 N2 81.70(12) . . ?
N1 P1 Au1 116.94(10) . . ?
N3 P1 Au1 119.10(10) . . ?
N2 P1 Au1 115.06(9) . . ?
N4 P2 N3 116.33(14) . . ?
N4 P2 N2 115.04(14) . . ?
N3 P2 N2 85.26(13) . . ?
N4 P2 C17 111.29(17) . . ?
N3 P2 C17 112.73(17) . . ?
N2 P2 C17 114.01(16) . . ?
C1 N1 P1 131.7(2) . . ?
C1 N1 H1 111.1 . . ?
P1 N1 H1 116.3 . . ?
C5 N2 P2 132.5(2) . . ?
C5 N2 P1 130.0(2) . . ?
P2 N2 P1 96.05(13) . . ?
C9 N3 P2 131.8(2) . . ?
C9 N3 P1 130.4(2) . . ?
P2 N3 P1 96.96(13) . . ?
C13 N4 P2 137.0(2) . . ?
C13 N4 H4 111.6 . . ?
P2 N4 H4 111.1 . . ?
N1 C1 C3 105.4(3) . . ?
N1 C1 C4 111.0(3) . . ?
C3 C1 C4 110.5(3) . . ?
N1 C1 C2 110.6(3) . . ?
C3 C1 C2 109.3(3) . . ?
C4 C1 C2 109.9(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 . . ?
N2 C5 C7 108.1(2) . . ?
N2 C5 C8 108.4(3) . . ?
C7 C5 C8 109.7(3) . . ?
N2 C5 C6 110.3(3) . . ?
C7 C5 C6 109.8(3) . . ?
C8 C5 C6 110.4(3) . . ?
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 C12 108.4(3) . . ?
N3 C9 C10 108.4(3) . . ?
C12 C9 C10 109.5(3) . . ?
N3 C9 C11 109.8(3) . . ?
C12 C9 C11 110.4(3) . . ?
C10 C9 C11 110.3(3) . . ?
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 . . ?
C16A C13 N4 114.2(6) . . ?
C15 C13 N4 114.3(5) . . ?
C15 C13 C14 111.7(6) . . ?
N4 C13 C14 105.0(6) . . ?
C16A C13 C14A 111.2(7) . . ?
N4 C13 C14A 105.5(7) . . ?
C15 C13 C16 109.9(5) . . ?
N4 C13 C16 108.0(5) . . ?
C14 C13 C16 107.5(6) . . ?
C16A C13 C15A 111.6(6) . . ?
N4 C13 C15A 107.2(5) . . ?
C14A C13 C15A 106.7(7) . . ?
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 . . ?
C13 C14A H14D 109.5 . . ?
C13 C14A H14E 109.5 . . ?
H14D C14A H14E 109.5 . . ?
C13 C14A H14F 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C13 C15A H15D 109.5 . . ?
C13 C15A H15E 109.5 . . ?
H15D C15A H15E 109.5 . . ?
C13 C15A H15F 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
C13 C16A H16D 109.5 . . ?
C13 C16A H16E 109.5 . . ?
H16D C16A H16E 109.5 . . ?
C13 C16A H16F 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
P2 C17 H17A 109.5 . . ?
P2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O1 S1 O3 116.6(2) . . ?
O1 S1 O2 113.92(17) . . ?
O3 S1 O2 114.53(18) . . ?
O1 S1 C18 103.19(17) . . ?
O3 S1 C18 103.75(18) . . ?
O2 S1 C18 102.39(17) . . ?
F1 C18 F2 108.0(3) . . ?
F1 C18 F3 108.2(3) . . ?
F2 C18 F3 108.2(3) . . ?
F1 C18 S1 110.2(3) . . ?
F2 C18 S1 111.5(2) . . ?
F3 C18 S1 110.6(3) . . ?

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
N1 H1 O2 0.91 2.06 2.937(4) 162 1_655
N4 H4 O2 0.91 2.04 2.923(4) 162 1_655
C3 H3A O3 0.98 2.64 3.581(5) 160 1_655
C10 H10A Cl1 0.98 2.88 3.806(4) 159 2_676
C12 H12B O1 0.98 2.58 3.527(5) 163 .

_refine_diff_density_max         2.199
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.162

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 991953'
