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


data_rs-21

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H42 Cu6 N12 Se6, H2O'
_chemical_formula_sum            'C36 H44 Cu6 N12 O Se6'
_chemical_formula_weight         1515.87


# start Validation Reply Form

_vrf_PLAT026_rs-21               
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         38 %     
RESPONSE: Crystal quality was poor
;
_vrf_PLAT220_rs-21               
;
PROBLEM: Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        4.1 Ratio 
RESPONSE: atomic species identification has been checked
;
# end Validation Reply Form

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   12.0837(19)
_cell_length_b                   18.286(5)
_cell_length_c                   12.1000(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.492(11)
_cell_angle_gamma                90.00
_cell_volume                     2550.0(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      10.2
_cell_measurement_theta_max      14.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_exptl_absorpt_coefficient_mu    6.780
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_correction_T_min  0.3441
_exptl_absorpt_correction_T_max  0.3441


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       ω-2θ
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 150
_diffrn_standards_decay_%        0.84
_diffrn_reflns_number            7026
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.1795
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5851
_reflns_number_gt                2230
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       WinAFC
_computing_cell_refinement       WinAFC
_computing_data_reduction        CrystalStructure
_computing_structure_solution    SIR92
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for windows'
_computing_publication_material  'WinGX 1.70.01'

_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0479P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5851
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2159
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1592
_refine_ls_wR_factor_gt          0.1148
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_restrained_S_all      0.960
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.52886(11) 0.02500(8) 0.33294(11) 0.0610(4) Uani 1 1 d . . .
Cu2 Cu 0.44560(11) -0.10209(7) 0.39808(11) 0.0599(4) Uani 1 1 d . . .
Cu3 Cu 0.68462(12) -0.01214(7) 0.54645(10) 0.0625(4) Uani 1 1 d . . .
Se1 Se 0.32531(9) 0.03463(6) 0.26283(8) 0.0521(3) Uani 1 1 d . . .
Se2 Se 0.59832(9) 0.13532(6) 0.43020(8) 0.0542(3) Uani 1 1 d . . .
Se3 Se 0.64612(9) -0.11750(6) 0.42815(9) 0.0540(3) Uani 1 1 d . . .
C1 C 0.6709(5) -0.0890(3) 0.2926(4) 0.053(3) Uani 1 1 d G . .
N1 N 0.6252(5) -0.0228(3) 0.2428(5) 0.054(2) Uani 1 1 d G . .
C2 C 0.6477(6) 0.0016(3) 0.1429(5) 0.067(3) Uani 1 1 d G . .
C3 C 0.7160(7) -0.0402(4) 0.0928(5) 0.078(4) Uani 1 1 d G . .
H3 H 0.7311 -0.0238 0.0260 0.094 Uiso 1 1 calc R . .
C4 C 0.7618(6) -0.1063(4) 0.1426(6) 0.074(4) Uani 1 1 d G . .
N2 N 0.7392(6) -0.1308(3) 0.2425(6) 0.067(3) Uani 1 1 d G . .
C5 C 0.5969(11) 0.0715(7) 0.0959(9) 0.088(4) Uani 1 1 d . . .
H5A H 0.5206 0.0757 0.1041 0.132 Uiso 1 1 calc R . .
H5B H 0.5920 0.0743 0.0153 0.132 Uiso 1 1 calc R . .
H5C H 0.6447 0.1107 0.1372 0.132 Uiso 1 1 calc R . .
C6 C 0.8348(13) -0.1545(8) 0.0985(12) 0.129(6) Uani 1 1 d . . .
H6A H 0.9097 -0.1587 0.1551 0.193 Uiso 1 1 calc R . .
H6B H 0.8433 -0.1345 0.0282 0.193 Uiso 1 1 calc R . .
H6C H 0.7994 -0.2019 0.0833 0.193 Uiso 1 1 calc R . .
C7 C 0.2721(5) -0.0521(3) 0.1956(5) 0.054(3) Uani 1 1 d G . .
N3 N 0.3183(5) -0.1174(4) 0.2484(4) 0.057(2) Uani 1 1 d G . .
C8 C 0.2741(7) -0.1838(3) 0.1980(6) 0.072(3) Uani 1 1 d G . .
C9 C 0.1837(7) -0.1848(3) 0.0949(6) 0.088(4) Uani 1 1 d G . .
H9 H 0.1542 -0.2292 0.0612 0.106 Uiso 1 1 calc R . .
C10 C 0.1375(5) -0.1195(5) 0.0421(4) 0.073(3) Uani 1 1 d G . .
N4 N 0.1817(5) -0.0531(4) 0.0924(5) 0.056(2) Uani 1 1 d G . .
C11 C 0.3234(13) -0.2507(6) 0.2608(12) 0.122(6) Uani 1 1 d . . .
H11A H 0.3128 -0.2501 0.3363 0.184 Uiso 1 1 calc R . .
H11B H 0.4048 -0.2532 0.2686 0.184 Uiso 1 1 calc R . .
H11C H 0.2849 -0.2926 0.2186 0.184 Uiso 1 1 calc R . .
C12 C 0.0484(12) -0.1142(8) -0.0722(10) 0.118(5) Uani 1 1 d . . .
H12A H -0.0054 -0.1539 -0.0811 0.178 Uiso 1 1 calc R . .
H12B H 0.0851 -0.1165 -0.1323 0.178 Uiso 1 1 calc R . .
H12C H 0.0077 -0.0686 -0.0774 0.178 Uiso 1 1 calc R . .
C13 C 0.7546(5) 0.1256(4) 0.4798(5) 0.068(3) Uani 1 1 d G . .
N5 N 0.8045(6) 0.0642(4) 0.5428(6) 0.067(3) Uani 1 1 d G . .
C14 C 0.9244(7) 0.0595(4) 0.5894(7) 0.091(4) Uani 1 1 d G . .
C15 C 0.9943(5) 0.1163(6) 0.5729(8) 0.125(6) Uani 1 1 d G . .
H15 H 1.0745 0.1131 0.6040 0.150 Uiso 1 1 calc R . .
C16 C 0.9443(7) 0.1777(5) 0.5098(8) 0.118(5) Uani 1 1 d G . .
N6 N 0.8245(8) 0.1824(4) 0.4633(6) 0.091(3) Uani 1 1 d G . .
C17 C 0.9706(12) -0.0056(9) 0.6574(13) 0.139(7) Uani 1 1 d . . .
H17A H 0.9108 -0.0279 0.6833 0.209 Uiso 1 1 calc R . .
H17B H 1.0343 0.0080 0.7233 0.209 Uiso 1 1 calc R . .
H17C H 0.9969 -0.0396 0.6103 0.209 Uiso 1 1 calc R . .
C18 C 1.0115(15) 0.2406(11) 0.488(2) 0.220(12) Uani 1 1 d . . .
H18A H 0.9879 0.2516 0.4071 0.330 Uiso 1 1 calc R . .
H18B H 1.0927 0.2289 0.5137 0.330 Uiso 1 1 calc R . .
H18C H 0.9976 0.2824 0.5306 0.330 Uiso 1 1 calc R . .
O1S O 0.7141(15) -0.2916(8) 0.2873(13) 0.086(5) Uani 0.50 1 d P . .


_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 N1 2.018(5) . ?
Cu1 Se1 2.3550(17) . ?
Cu1 Se2 2.3590(17) . ?
Cu1 Cu2 2.7406(19) . ?
Cu1 Cu3 2.7848(18) . ?
Cu2 N3 2.012(5) . ?
Cu2 Se3 2.3565(17) . ?
Cu2 Se2 2.3730(16) 3_656 ?
Cu2 Cu3 2.8149(19) 3_656 ?
Cu3 N5 2.022(6) . ?
Cu3 Se3 2.3616(17) . ?
Cu3 Se1 2.3823(16) 3_656 ?
Cu3 Cu2 2.8149(19) 3_656 ?
Se1 C7 1.810(5) . ?
Se1 Cu3 2.3823(16) 3_656 ?
Se2 C13 1.810(6) . ?
Se2 Cu2 2.3730(16) 3_656 ?
Se3 C1 1.830(4) . ?
C1 N1 1.3900 . ?
C1 N2 1.3900 . ?
N1 C2 1.3900 . ?
C2 C3 1.3900 . ?
C2 C5 1.459(12) . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 N2 1.3900 . ?
C4 C6 1.455(13) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N3 1.3900 . ?
C7 N4 1.3900 . ?
N3 C8 1.3900 . ?
C8 C9 1.3900 . ?
C8 C11 1.469(12) . ?
C9 C10 1.3900 . ?
C9 H9 0.9300 . ?
C10 N4 1.3900 . ?
C10 C12 1.478(12) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N5 1.3900 . ?
C13 N6 1.3900 . ?
N5 C14 1.3900 . ?
C14 C15 1.3900 . ?
C14 C17 1.459(14) . ?
C15 C16 1.3900 . ?
C15 H15 0.9300 . ?
C16 N6 1.3900 . ?
C16 C18 1.475(17) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 Se1 123.18(18) . . ?
N1 Cu1 Se2 117.63(18) . . ?
Se1 Cu1 Se2 106.99(7) . . ?
N1 Cu1 Cu2 96.26(19) . . ?
Se1 Cu1 Cu2 74.52(5) . . ?
Se2 Cu1 Cu2 133.47(7) . . ?
N1 Cu1 Cu3 93.26(18) . . ?
Se1 Cu1 Cu3 133.94(7) . . ?
Se2 Cu1 Cu3 72.89(5) . . ?
Cu2 Cu1 Cu3 74.37(5) . . ?
N3 Cu2 Se3 126.47(18) . . ?
N3 Cu2 Se2 116.16(18) . 3_656 ?
Se3 Cu2 Se2 108.93(6) . 3_656 ?
N3 Cu2 Cu1 96.13(19) . . ?
Se3 Cu2 Cu1 72.33(5) . . ?
Se2 Cu2 Cu1 131.84(7) 3_656 . ?
N3 Cu2 Cu3 89.28(19) . 3_656 ?
Se3 Cu2 Cu3 132.41(7) . 3_656 ?
Se2 Cu2 Cu3 72.12(5) 3_656 3_656 ?
Cu1 Cu2 Cu3 73.69(5) . 3_656 ?
N5 Cu3 Se3 124.2(2) . . ?
N5 Cu3 Se1 112.66(19) . 3_656 ?
Se3 Cu3 Se1 112.84(7) . 3_656 ?
N5 Cu3 Cu1 95.8(2) . . ?
Se3 Cu3 Cu1 71.43(5) . . ?
Se1 Cu3 Cu1 136.38(7) 3_656 . ?
N5 Cu3 Cu2 87.1(2) . 3_656 ?
Se3 Cu3 Cu2 136.68(7) . 3_656 ?
Se1 Cu3 Cu2 72.70(5) 3_656 3_656 ?
Cu1 Cu3 Cu2 76.70(5) . 3_656 ?
C7 Se1 Cu1 106.7(2) . . ?
C7 Se1 Cu3 99.8(2) . 3_656 ?
Cu1 Se1 Cu3 89.39(6) . 3_656 ?
C13 Se2 Cu1 105.1(2) . . ?
C13 Se2 Cu2 99.8(2) . 3_656 ?
Cu1 Se2 Cu2 94.48(6) . 3_656 ?
C1 Se3 Cu2 105.4(2) . . ?
C1 Se3 Cu3 104.8(2) . . ?
Cu2 Se3 Cu3 90.12(6) . . ?
N1 C1 N2 120.0 . . ?
N1 C1 Se3 119.0(4) . . ?
N2 C1 Se3 120.9(4) . . ?
C2 N1 C1 120.0 . . ?
C2 N1 Cu1 128.8(4) . . ?
C1 N1 Cu1 111.2(4) . . ?
N1 C2 C3 120.0 . . ?
N1 C2 C5 116.9(6) . . ?
C3 C2 C5 123.1(6) . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
N2 C4 C3 120.0 . . ?
N2 C4 C6 115.0(7) . . ?
C3 C4 C6 125.0(7) . . ?
C4 N2 C1 120.0 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 N4 120.0 . . ?
N3 C7 Se1 120.5(4) . . ?
N4 C7 Se1 119.5(4) . . ?
C7 N3 C8 120.0 . . ?
C7 N3 Cu2 112.7(4) . . ?
C8 N3 Cu2 127.2(4) . . ?
C9 C8 N3 120.0 . . ?
C9 C8 C11 122.7(7) . . ?
N3 C8 C11 117.2(7) . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
N4 C10 C9 120.0 . . ?
N4 C10 C12 115.4(7) . . ?
C9 C10 C12 124.4(7) . . ?
C10 N4 C7 120.0 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 N6 120.0 . . ?
N5 C13 Se2 119.9(5) . . ?
N6 C13 Se2 119.9(5) . . ?
C13 N5 C14 120.0 . . ?
C13 N5 Cu3 112.0(4) . . ?
C14 N5 Cu3 128.0(4) . . ?
C15 C14 N5 120.0 . . ?
C15 C14 C17 123.0(8) . . ?
N5 C14 C17 117.0(8) . . ?
C14 C15 C16 120.0 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
N6 C16 C15 120.0 . . ?
N6 C16 C18 116.2(10) . . ?
C15 C16 C18 123.8(10) . . ?
C16 N6 C13 120.0 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Cu1 Cu2 N3 -81.3(3) . . . . ?
Se1 Cu1 Cu2 N3 41.46(18) . . . . ?
Se2 Cu1 Cu2 N3 140.39(19) . . . . ?
Cu3 Cu1 Cu2 N3 -172.94(19) . . . . ?
N1 Cu1 Cu2 Se3 45.10(18) . . . . ?
Se1 Cu1 Cu2 Se3 167.84(6) . . . . ?
Se2 Cu1 Cu2 Se3 -93.22(9) . . . . ?
Cu3 Cu1 Cu2 Se3 -46.55(5) . . . . ?
N1 Cu1 Cu2 Se2 144.99(18) . . . 3_656 ?
Se1 Cu1 Cu2 Se2 -92.26(9) . . . 3_656 ?
Se2 Cu1 Cu2 Se2 6.67(15) . . . 3_656 ?
Cu3 Cu1 Cu2 Se2 53.34(8) . . . 3_656 ?
N1 Cu1 Cu2 Cu3 -168.73(18) . . . 3_656 ?
Se1 Cu1 Cu2 Cu3 -45.99(5) . . . 3_656 ?
Se2 Cu1 Cu2 Cu3 52.95(9) . . . 3_656 ?
Cu3 Cu1 Cu2 Cu3 99.62(5) . . . 3_656 ?
N1 Cu1 Cu3 N5 75.3(3) . . . . ?
Se1 Cu1 Cu3 N5 -140.0(2) . . . . ?
Se2 Cu1 Cu3 N5 -42.6(2) . . . . ?
Cu2 Cu1 Cu3 N5 170.9(2) . . . . ?
N1 Cu1 Cu3 Se3 -48.86(18) . . . . ?
Se1 Cu1 Cu3 Se3 95.85(10) . . . . ?
Se2 Cu1 Cu3 Se3 -166.80(6) . . . . ?
Cu2 Cu1 Cu3 Se3 46.73(5) . . . . ?
N1 Cu1 Cu3 Se1 -152.81(19) . . . 3_656 ?
Se1 Cu1 Cu3 Se1 -8.10(17) . . . 3_656 ?
Se2 Cu1 Cu3 Se1 89.25(10) . . . 3_656 ?
Cu2 Cu1 Cu3 Se1 -57.22(10) . . . 3_656 ?
N1 Cu1 Cu3 Cu2 160.91(18) . . . 3_656 ?
Se1 Cu1 Cu3 Cu2 -54.38(10) . . . 3_656 ?
Se2 Cu1 Cu3 Cu2 42.97(5) . . . 3_656 ?
Cu2 Cu1 Cu3 Cu2 -103.50(5) . . . 3_656 ?
N1 Cu1 Se1 C7 42.0(3) . . . . ?
Se2 Cu1 Se1 C7 -176.8(2) . . . . ?
Cu2 Cu1 Se1 C7 -45.4(2) . . . . ?
Cu3 Cu1 Se1 C7 -94.4(2) . . . . ?
N1 Cu1 Se1 Cu3 142.0(2) . . . 3_656 ?
Se2 Cu1 Se1 Cu3 -76.79(7) . . . 3_656 ?
Cu2 Cu1 Se1 Cu3 54.65(5) . . . 3_656 ?
Cu3 Cu1 Se1 Cu3 5.58(11) . . . 3_656 ?
N1 Cu1 Se2 C13 -35.3(3) . . . . ?
Se1 Cu1 Se2 C13 -179.0(2) . . . . ?
Cu2 Cu1 Se2 C13 96.5(3) . . . . ?
Cu3 Cu1 Se2 C13 49.3(2) . . . . ?
N1 Cu1 Se2 Cu2 -136.7(2) . . . 3_656 ?
Se1 Cu1 Se2 Cu2 79.57(7) . . . 3_656 ?
Cu2 Cu1 Se2 Cu2 -4.98(11) . . . 3_656 ?
Cu3 Cu1 Se2 Cu2 -52.12(5) . . . 3_656 ?
N3 Cu2 Se3 C1 34.6(3) . . . . ?
Se2 Cu2 Se3 C1 -179.0(2) 3_656 . . . ?
Cu1 Cu2 Se3 C1 -49.9(2) . . . . ?
Cu3 Cu2 Se3 C1 -96.2(2) 3_656 . . . ?
N3 Cu2 Se3 Cu3 140.0(2) . . . . ?
Se2 Cu2 Se3 Cu3 -73.58(7) 3_656 . . . ?
Cu1 Cu2 Se3 Cu3 55.53(5) . . . . ?
Cu3 Cu2 Se3 Cu3 9.17(10) 3_656 . . . ?
N5 Cu3 Se3 C1 -32.9(3) . . . . ?
Se1 Cu3 Se3 C1 -175.3(2) 3_656 . . . ?
Cu1 Cu3 Se3 C1 51.3(2) . . . . ?
Cu2 Cu3 Se3 C1 96.1(2) 3_656 . . . ?
N5 Cu3 Se3 Cu2 -138.9(3) . . . . ?
Se1 Cu3 Se3 Cu2 78.77(7) 3_656 . . . ?
Cu1 Cu3 Se3 Cu2 -54.64(5) . . . . ?
Cu2 Cu3 Se3 Cu2 -9.87(11) 3_656 . . . ?
Cu2 Se3 C1 N1 48.7(3) . . . . ?
Cu3 Se3 C1 N1 -45.6(3) . . . . ?
Cu2 Se3 C1 N2 -134.5(3) . . . . ?
Cu3 Se3 C1 N2 131.2(3) . . . . ?
N2 C1 N1 C2 0.0 . . . . ?
Se3 C1 N1 C2 176.8(5) . . . . ?
N2 C1 N1 Cu1 179.5(4) . . . . ?
Se3 C1 N1 Cu1 -3.7(4) . . . . ?
Se1 Cu1 N1 C2 70.0(4) . . . . ?
Se2 Cu1 N1 C2 -67.5(4) . . . . ?
Cu2 Cu1 N1 C2 145.5(4) . . . . ?
Cu3 Cu1 N1 C2 -139.8(4) . . . . ?
Se1 Cu1 N1 C1 -109.4(3) . . . . ?
Se2 Cu1 N1 C1 113.2(3) . . . . ?
Cu2 Cu1 N1 C1 -33.8(3) . . . . ?
Cu3 Cu1 N1 C1 40.8(3) . . . . ?
C1 N1 C2 C3 0.0 . . . . ?
Cu1 N1 C2 C3 -179.3(5) . . . . ?
C1 N1 C2 C5 -179.9(8) . . . . ?
Cu1 N1 C2 C5 0.7(8) . . . . ?
N1 C2 C3 C4 0.0 . . . . ?
C5 C2 C3 C4 179.9(8) . . . . ?
C2 C3 C4 N2 0.0 . . . . ?
C2 C3 C4 C6 -179.7(9) . . . . ?
C3 C4 N2 C1 0.0 . . . . ?
C6 C4 N2 C1 179.7(9) . . . . ?
N1 C1 N2 C4 0.0 . . . . ?
Se3 C1 N2 C4 -176.8(5) . . . . ?
Cu1 Se1 C7 N3 42.6(4) . . . . ?
Cu3 Se1 C7 N3 -49.7(4) 3_656 . . . ?
Cu1 Se1 C7 N4 -139.6(3) . . . . ?
Cu3 Se1 C7 N4 128.1(3) 3_656 . . . ?
N4 C7 N3 C8 0.0 . . . . ?
Se1 C7 N3 C8 177.8(5) . . . . ?
N4 C7 N3 Cu2 -178.7(4) . . . . ?
Se1 C7 N3 Cu2 -0.9(4) . . . . ?
Se3 Cu2 N3 C7 -105.4(3) . . . . ?
Se2 Cu2 N3 C7 110.3(3) 3_656 . . . ?
Cu1 Cu2 N3 C7 -32.8(3) . . . . ?
Cu3 Cu2 N3 C7 40.7(3) 3_656 . . . ?
Se3 Cu2 N3 C8 76.0(4) . . . . ?
Se2 Cu2 N3 C8 -68.3(4) 3_656 . . . ?
Cu1 Cu2 N3 C8 148.5(4) . . . . ?
Cu3 Cu2 N3 C8 -137.9(4) 3_656 . . . ?
C7 N3 C8 C9 0.0 . . . . ?
Cu2 N3 C8 C9 178.5(4) . . . . ?
C7 N3 C8 C11 -177.4(9) . . . . ?
Cu2 N3 C8 C11 1.1(9) . . . . ?
N3 C8 C9 C10 0.0 . . . . ?
C11 C8 C9 C10 177.3(10) . . . . ?
C8 C9 C10 N4 0.0 . . . . ?
C8 C9 C10 C12 174.6(9) . . . . ?
C9 C10 N4 C7 0.0 . . . . ?
C12 C10 N4 C7 -175.1(8) . . . . ?
N3 C7 N4 C10 0.0 . . . . ?
Se1 C7 N4 C10 -177.8(5) . . . . ?
Cu1 Se2 C13 N5 -51.8(4) . . . . ?
Cu2 Se2 C13 N5 45.6(4) 3_656 . . . ?
Cu1 Se2 C13 N6 133.6(3) . . . . ?
Cu2 Se2 C13 N6 -129.0(4) 3_656 . . . ?
N6 C13 N5 C14 0.0 . . . . ?
Se2 C13 N5 C14 -174.5(5) . . . . ?
N6 C13 N5 Cu3 -176.9(5) . . . . ?
Se2 C13 N5 Cu3 8.5(5) . . . . ?
Se3 Cu3 N5 C13 100.7(4) . . . . ?
Se1 Cu3 N5 C13 -116.9(3) 3_656 . . . ?
Cu1 Cu3 N5 C13 29.3(3) . . . . ?
Cu2 Cu3 N5 C13 -47.0(3) 3_656 . . . ?
Se3 Cu3 N5 C14 -75.9(5) . . . . ?
Se1 Cu3 N5 C14 66.5(4) 3_656 . . . ?
Cu1 Cu3 N5 C14 -147.4(4) . . . . ?
Cu2 Cu3 N5 C14 136.3(4) 3_656 . . . ?
C13 N5 C14 C15 0.0 . . . . ?
Cu3 N5 C14 C15 176.4(5) . . . . ?
C13 N5 C14 C17 178.3(10) . . . . ?
Cu3 N5 C14 C17 -5.4(10) . . . . ?
N5 C14 C15 C16 0.0 . . . . ?
C17 C14 C15 C16 -178.1(11) . . . . ?
C14 C15 C16 N6 0.0 . . . . ?
C14 C15 C16 C18 179.7(13) . . . . ?
C15 C16 N6 C13 0.0 . . . . ?
C18 C16 N6 C13 -179.7(13) . . . . ?
N5 C13 N6 C16 0.0 . . . . ?
Se2 C13 N6 C16 174.5(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.141
_database_code_depnum_ccdc_archive 'CCDC 963090'

data_shelxs

# start Validation Reply Form 
_vrf_PLAT306_shelxs              
; 
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W 
RESPONSE: hydrogen atoms for the water molecule could not be placed due to partial occupancey (0.1667)
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H42 Ag6 N12 Se6, 6(C H4 O),H2 O'
_chemical_formula_sum            'C42 H68 Ag6 N12 O7 Se6'
_chemical_formula_weight         1974.06

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 c:H'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_Int_Tables_number      167

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   22.157(6)
_cell_length_b                   22.157(6)
_cell_length_c                   22.197(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     9437(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      10.2
_cell_measurement_theta_max      14.3

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5664
_exptl_absorpt_coefficient_mu    5.354
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_correction_T_min  0.2233
_exptl_absorpt_correction_T_max  0.2233


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 150
_diffrn_standards_decay_%        -5.99
_diffrn_reflns_number            5608
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.81
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2418
_reflns_number_gt                985
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       WinAFC
_computing_cell_refinement       WinAFC
_computing_data_reduction        CrystalStructure
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  'WinGX 1.7.01'

_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0313P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2418
_refine_ls_number_parameters     115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1536
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_restrained_S_all      0.928
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2110(3) 0.0757(3) 0.1946(3) 0.0553(17) Uani 1 1 d . . .
C2 C 0.2709(4) 0.1011(3) 0.2847(3) 0.072(2) Uani 1 1 d . . .
C3 C 0.3239(4) 0.0967(3) 0.2543(4) 0.075(2) Uani 1 1 d . . .
H3 H 0.3635 0.1040 0.2750 0.090 Uiso 1 1 calc R . .
C4 C 0.3172(4) 0.0818(3) 0.1942(4) 0.063(2) Uani 1 1 d . . .
C5 C 0.2727(4) 0.1167(4) 0.3512(3) 0.091(3) Uani 1 1 d . . .
H5A H 0.2440 0.1369 0.3589 0.136 Uiso 1 1 calc R . .
H5B H 0.3198 0.1488 0.3631 0.136 Uiso 1 1 calc R . .
H5C H 0.2556 0.0743 0.3738 0.136 Uiso 1 1 calc R . .
C6 C 0.3703(4) 0.0746(4) 0.1612(3) 0.093(3) Uani 1 1 d . . .
H6A H 0.3779 0.0970 0.1227 0.140 Uiso 1 1 calc R . .
H6B H 0.3548 0.0261 0.1555 0.140 Uiso 1 1 calc R . .
H6C H 0.4130 0.0960 0.1837 0.140 Uiso 1 1 calc R . .
N2 N 0.2606(3) 0.0716(3) 0.1646(2) 0.0570(14) Uani 1 1 d . . .
N1 N 0.2131(3) 0.0894(3) 0.2543(2) 0.0577(14) Uani 1 1 d . . .
Se1 Se 0.13039(4) 0.05761(4) 0.15018(3) 0.0594(2) Uani 1 1 d . . .
Ag1 Ag 0.10782(3) 0.06238(3) 0.29975(2) 0.0774(2) Uani 1 1 d . . .
O1S O 0.2467(5) 0.0272(6) 0.0358(3) 0.163(3) Uani 1 1 d . . .
H1S H 0.2410 0.0365 0.0703 0.244 Uiso 1 1 calc R . .
C1S C 0.2066(6) 0.0396(6) -0.0022(4) 0.153(4) Uani 1 1 d . . .
H1SA H 0.1583 0.0077 0.0062 0.229 Uiso 1 1 calc R . .
H1SB H 0.2168 0.0333 -0.0430 0.229 Uiso 1 1 calc R . .
H1SC H 0.2160 0.0865 0.0031 0.229 Uiso 1 1 calc R . .
O1W O 0.0000 0.0000 0.0000 0.297(15) Uani 1 6 d S . .


_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
C1 N2 1.326(8) . ?
C1 N1 1.354(7) . ?
C1 Se1 1.899(7) . ?
C2 N1 1.353(8) . ?
C2 C3 1.398(9) . ?
C2 C5 1.514(9) . ?
C3 C4 1.365(9) . ?
C3 H3 0.9300 . ?
C4 N2 1.331(8) . ?
C4 C6 1.460(9) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N1 Ag1 2.329(5) . ?
Se1 Ag1 2.5337(10) 6 ?
Se1 Ag1 2.6158(11) 4 ?
Ag1 Se1 2.5337(10) 6 ?
Ag1 Se1 2.6158(11) 4 ?
Ag1 Ag1 2.8141(12) 6 ?
Ag1 Ag1 3.2573(13) 4 ?
O1S C1S 1.350(10) . ?
O1S H1S 0.8200 . ?
C1S H1SA 0.9600 . ?
C1S H1SB 0.9600 . ?
C1S H1SC 0.9600 . ?

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
N2 C1 N1 124.7(6) . . ?
N2 C1 Se1 116.6(5) . . ?
N1 C1 Se1 118.6(5) . . ?
N1 C2 C3 119.6(7) . . ?
N1 C2 C5 116.4(7) . . ?
C3 C2 C5 124.0(7) . . ?
C4 C3 C2 119.7(7) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
N2 C4 C3 120.1(7) . . ?
N2 C4 C6 118.4(7) . . ?
C3 C4 C6 121.4(7) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 N2 C4 118.9(6) . . ?
C2 N1 C1 117.0(6) . . ?
C2 N1 Ag1 124.3(5) . . ?
C1 N1 Ag1 116.6(4) . . ?
C1 Se1 Ag1 112.5(2) . 6 ?
C1 Se1 Ag1 96.71(18) . 4 ?
Ag1 Se1 Ag1 88.64(3) 6 4 ?
N1 Ag1 Se1 135.93(13) . 6 ?
N1 Ag1 Se1 101.28(13) . 4 ?
Se1 Ag1 Se1 115.00(4) 6 4 ?
N1 Ag1 Ag1 93.41(13) . 6 ?
Se1 Ag1 Ag1 77.84(3) 6 6 ?
Se1 Ag1 Ag1 136.02(2) 4 6 ?
N1 Ag1 Ag1 82.52(13) . 4 ?
Se1 Ag1 Ag1 132.53(2) 6 4 ?
Se1 Ag1 Ag1 68.97(3) 4 4 ?
Ag1 Ag1 Ag1 72.27(3) 6 4 ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1SA 109.5 . . ?
O1S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
O1S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 C4 1.0(10) . . . . ?
C5 C2 C3 C4 179.5(6) . . . . ?
C2 C3 C4 N2 0.1(10) . . . . ?
C2 C3 C4 C6 -178.0(7) . . . . ?
N1 C1 N2 C4 -0.5(9) . . . . ?
Se1 C1 N2 C4 -178.1(4) . . . . ?
C3 C4 N2 C1 -0.4(9) . . . . ?
C6 C4 N2 C1 177.8(6) . . . . ?
C3 C2 N1 C1 -1.7(9) . . . . ?
C5 C2 N1 C1 179.7(6) . . . . ?
C3 C2 N1 Ag1 161.4(5) . . . . ?
C5 C2 N1 Ag1 -17.3(8) . . . . ?
N2 C1 N1 C2 1.5(9) . . . . ?
Se1 C1 N1 C2 179.1(5) . . . . ?
N2 C1 N1 Ag1 -162.9(5) . . . . ?
Se1 C1 N1 Ag1 14.7(6) . . . . ?
N2 C1 Se1 Ag1 -159.6(4) . . . 6 ?
N1 C1 Se1 Ag1 22.6(5) . . . 6 ?
N2 C1 Se1 Ag1 109.1(5) . . . 4 ?
N1 C1 Se1 Ag1 -68.7(5) . . . 4 ?
C2 N1 Ag1 Se1 81.8(5) . . . 6 ?
C1 N1 Ag1 Se1 -115.1(4) . . . 6 ?
C2 N1 Ag1 Se1 -63.9(5) . . . 4 ?
C1 N1 Ag1 Se1 99.2(4) . . . 4 ?
C2 N1 Ag1 Ag1 157.8(5) . . . 6 ?
C1 N1 Ag1 Ag1 -39.1(4) . . . 6 ?
C2 N1 Ag1 Ag1 -130.6(5) . . . 4 ?
C1 N1 Ag1 Ag1 32.5(4) . . . 4 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.102
_database_code_depnum_ccdc_archive 'CCDC 963091'

data_AuSepymMe2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H22 Au N2 P Se'
_chemical_formula_weight         501.21

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'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_Int_Tables_number      92


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'-y, -x, -z+1/2'
'y, x, -z'
'y+1/2, -x+1/2, z+3/4'
'-y+1/2, x+1/2, z+1/4'

_cell_length_a                   8.900(5)
_cell_length_b                   8.900(5)
_cell_length_c                   42.382(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3357(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    18
_cell_measurement_theta_min      10.1
_cell_measurement_theta_max      15.6

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_exptl_absorpt_coefficient_mu    11.012
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_correction_T_min  0.2889
_exptl_absorpt_correction_T_max  0.4056


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 150
_diffrn_standards_decay_%        -0.81
_diffrn_reflns_number            3629
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_uavnetI/netI   0.1530
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2549
_reflns_number_gt                1123
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       WinAFC
_computing_cell_refinement       WinAFC
_computing_data_reduction        CrystalStructure
_computing_structure_solution    SIR92
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for windows'
_computing_publication_material  'WinGX 1.70.01'

_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0217P)²+28.3393P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         2549
_refine_ls_number_parameters     142
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1921
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1190
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.004
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.40476(11) 0.16875(10) 0.484430(19) 0.0597(3) Uani 1 1 d . . .
Se1 Se 0.4316(3) 0.3996(3) 0.45491(5) 0.0608(7) Uani 1 1 d . . .
P1 P 0.3954(8) -0.0561(7) 0.50994(13) 0.082(2) Uani 1 1 d . . .
N1 N 0.586(2) 0.195(2) 0.4164(4) 0.062(5) Uani 1 1 d . . .
N2 N 0.596(2) 0.454(2) 0.4021(4) 0.069(6) Uani 1 1 d . . .
C1 C 0.549(3) 0.340(3) 0.4201(5) 0.063(7) Uani 1 1 d . . .
C2 C 0.666(3) 0.161(3) 0.3901(6) 0.070(7) Uani 1 1 d . . .
C4 C 0.675(3) 0.419(4) 0.3762(6) 0.089(8) Uani 1 1 d . . .
C3 C 0.706(3) 0.271(4) 0.3690(6) 0.085(9) Uani 1 1 d . . .
H3 H 0.7527 0.2458 0.3501 0.102 Uiso 1 1 calc R . .
C5 C 0.703(3) -0.003(3) 0.3852(6) 0.114(11) Uani 1 1 d . . .
H5A H 0.7845 -0.0315 0.3989 0.172 Uiso 1 1 calc R . .
H5B H 0.7326 -0.0195 0.3637 0.172 Uiso 1 1 calc R . .
H5C H 0.6166 -0.0635 0.3899 0.172 Uiso 1 1 calc R . .
C8 C 0.545(5) -0.180(4) 0.4563(6) 0.255 Uani 1 1 d D . .
H8A H 0.5011 -0.0988 0.4446 0.383 Uiso 1 1 calc R . .
H8B H 0.5396 -0.2706 0.4441 0.383 Uiso 1 1 calc R . .
H8C H 0.6488 -0.1571 0.4606 0.383 Uiso 1 1 calc R . .
C9 C 0.207(4) -0.126(3) 0.5217(8) 0.148(14) Uani 1 1 d . . .
H9A H 0.1504 -0.1459 0.5025 0.178 Uiso 1 1 calc R . .
H9B H 0.2202 -0.2209 0.5324 0.178 Uiso 1 1 calc R . .
C10 C 0.116(4) -0.033(4) 0.5412(8) 0.19(2) Uani 1 1 d . . .
H10A H 0.1724 -0.0045 0.5596 0.291 Uiso 1 1 calc R . .
H10B H 0.0282 -0.0878 0.5475 0.291 Uiso 1 1 calc R . .
H10C H 0.0870 0.0550 0.5297 0.291 Uiso 1 1 calc R . .
C6 C 0.722(3) 0.548(3) 0.3549(6) 0.135(12) Uani 1 1 d . . .
H6A H 0.7909 0.5121 0.3392 0.203 Uiso 1 1 calc R . .
H6B H 0.7703 0.6248 0.3672 0.203 Uiso 1 1 calc R . .
H6C H 0.6350 0.5896 0.3447 0.203 Uiso 1 1 calc R . .
C11 C 0.489(4) -0.065(4) 0.5486(7) 0.151 Uani 1 1 d . . .
H11A H 0.4254 -0.0130 0.5637 0.181 Uiso 1 1 calc R . .
H11B H 0.4923 -0.1697 0.5550 0.181 Uiso 1 1 calc R . .
C12 C 0.635(3) -0.006(4) 0.5517(8) 0.177(15) Uani 1 1 d . . .
H12A H 0.7010 -0.0567 0.5371 0.265 Uiso 1 1 calc R . .
H12B H 0.6703 -0.0219 0.5728 0.265 Uiso 1 1 calc R . .
H12C H 0.6339 0.0992 0.5471 0.265 Uiso 1 1 calc R . .
C7 C 0.468(3) -0.199(3) 0.4846(6) 0.158 Uani 1 1 d D . .
H7A H 0.5337 -0.2596 0.4978 0.189 Uiso 1 1 calc R . .
H7B H 0.3829 -0.2629 0.4795 0.189 Uiso 1 1 calc R . .


_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 2.276(6) . ?
Au1 Se1 2.418(3) . ?
Au1 Au1 3.251(2) 6_556 ?
Se1 C1 1.88(2) . ?
P1 C7 1.79(3) . ?
P1 C11 1.84(3) . ?
P1 C9 1.86(3) . ?
N1 C1 1.34(3) . ?
N1 C2 1.36(3) . ?
N2 C4 1.34(3) . ?
N2 C1 1.34(3) . ?
C2 C3 1.37(3) . ?
C2 C5 1.51(3) . ?
C4 C3 1.38(3) . ?
C4 C6 1.52(3) . ?
C3 H3 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C8 C7 1.396(18) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.42(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C11 C12 1.41(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Au1 Se1 175.37(18) . . ?
P1 Au1 Au1 110.58(17) . 6_556 ?
Se1 Au1 Au1 74.02(6) . 6_556 ?
C1 Se1 Au1 102.8(8) . . ?
C7 P1 C11 109.9(13) . . ?
C7 P1 C9 104.5(15) . . ?
C11 P1 C9 99.0(14) . . ?
C7 P1 Au1 109.2(9) . . ?
C11 P1 Au1 116.4(11) . . ?
C9 P1 Au1 116.9(10) . . ?
C1 N1 C2 116(2) . . ?
C4 N2 C1 117(2) . . ?
N1 C1 N2 126(2) . . ?
N1 C1 Se1 120.0(17) . . ?
N2 C1 Se1 114.2(19) . . ?
C3 C2 N1 121(2) . . ?
C3 C2 C5 123(3) . . ?
N1 C2 C5 116(2) . . ?
N2 C4 C3 120(2) . . ?
N2 C4 C6 117(3) . . ?
C3 C4 C6 122(3) . . ?
C2 C3 C4 119(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P1 118(3) . . ?
C10 C9 H9A 107.7 . . ?
P1 C9 H9A 107.7 . . ?
C10 C9 H9B 107.7 . . ?
P1 C9 H9B 107.7 . . ?
H9A C9 H9B 107.1 . . ?
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 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C11 P1 119(2) . . ?
C12 C11 H11A 107.6 . . ?
P1 C11 H11A 107.6 . . ?
C12 C11 H11B 107.6 . . ?
P1 C11 H11B 107.6 . . ?
H11A C11 H11B 107.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C8 C7 P1 127(3) . . ?
C8 C7 H7A 105.5 . . ?
P1 C7 H7A 105.5 . . ?
C8 C7 H7B 105.5 . . ?
P1 C7 H7B 105.5 . . ?
H7A C7 H7B 106.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 Au1 Se1 C1 17(2) . . . . ?
Au1 Au1 Se1 C1 -168.7(7) 6_556 . . . ?
Se1 Au1 P1 C7 -27(3) . . . . ?
Au1 Au1 P1 C7 158.5(11) 6_556 . . . ?
Se1 Au1 P1 C11 98(2) . . . . ?
Au1 Au1 P1 C11 -76.4(11) 6_556 . . . ?
Se1 Au1 P1 C9 -146(2) . . . . ?
Au1 Au1 P1 C9 40.2(13) 6_556 . . . ?
C2 N1 C1 N2 -7(3) . . . . ?
C2 N1 C1 Se1 177.4(15) . . . . ?
C4 N2 C1 N1 7(3) . . . . ?
C4 N2 C1 Se1 -177.3(18) . . . . ?
Au1 Se1 C1 N1 4(2) . . . . ?
Au1 Se1 C1 N2 -171.9(15) . . . . ?
C1 N1 C2 C3 0(3) . . . . ?
C1 N1 C2 C5 -178(2) . . . . ?
C1 N2 C4 C3 0(4) . . . . ?
C1 N2 C4 C6 177(2) . . . . ?
N1 C2 C3 C4 6(4) . . . . ?
C5 C2 C3 C4 -176(3) . . . . ?
N2 C4 C3 C2 -6(4) . . . . ?
C6 C4 C3 C2 177(2) . . . . ?
C7 P1 C9 C10 -178(3) . . . . ?
C11 P1 C9 C10 69(3) . . . . ?
Au1 P1 C9 C10 -57(3) . . . . ?
C7 P1 C11 C12 77(3) . . . . ?
C9 P1 C11 C12 -174(3) . . . . ?
Au1 P1 C11 C12 -47(3) . . . . ?
C11 P1 C7 C8 -117(3) . . . . ?
C9 P1 C7 C8 137(3) . . . . ?
Au1 P1 C7 C8 12(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.911
_refine_diff_density_rms         0.229
_database_code_depnum_ccdc_archive 'CCDC 963092'
