

data_global


data_Cs4L
#TrackingRef '16829_web_deposit_cif_file_0_YoichiHabata_1357997395.All_1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H30 Cs2 N2 O7 S'
_chemical_formula_weight         732.36

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'
Cs Cs -0.3680 2.1192 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9076(5)
_cell_length_b                   9.0591(5)
_cell_length_c                   17.7228(10)
_cell_angle_alpha                97.8800(10)
_cell_angle_beta                 103.7500(10)
_cell_angle_gamma                102.0670(10)
_cell_volume                     1331.93(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    5565
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             716
_exptl_absorpt_coefficient_mu    2.858
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5203
_exptl_absorpt_correction_T_max  0.9091
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8549
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.21
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6039
_reflns_number_gt                5376
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0399P)²+0.0946P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6039
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0723
_refine_ls_wR_factor_gt          0.0621
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_restrained_S_all      1.134
_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
C4 C 0.3292(3) -0.2827(3) 0.52176(17) 0.0168(5) Uani 1 1 d . . .
H4A H 0.2819 -0.3369 0.4659 0.020 Uiso 1 1 calc R . .
H4B H 0.2964 -0.3539 0.5559 0.020 Uiso 1 1 calc R . .
Cs1 Cs 1.23771(2) 0.473982(19) 0.046083(10) 0.01879(6) Uani 1 1 d . . .
Cs2 Cs 0.780284(19) 0.071564(19) 0.013973(10) 0.01666(6) Uani 1 1 d . . .
S1S S 0.74201(9) -0.13129(9) -0.18099(4) 0.02069(15) Uani 1 1 d . . .
N2 N 0.5701(3) -0.2001(2) 0.47303(13) 0.0135(4) Uani 1 1 d . . .
N1 N 0.7329(3) 0.1466(3) 0.46500(13) 0.0142(4) Uani 1 1 d . . .
C2 C 0.7347(3) -0.1046(3) 0.50373(17) 0.0158(5) Uani 1 1 d . . .
H2A H 0.7904 -0.1129 0.4618 0.019 Uiso 1 1 calc R . .
H2B H 0.7919 -0.1434 0.5488 0.019 Uiso 1 1 calc R . .
C8 C 1.0387(3) 0.4460(3) 0.32096(17) 0.0181(6) Uani 1 1 d . . .
H8 H 1.1236 0.5334 0.3263 0.022 Uiso 1 1 calc R . .
C6 C 0.8993(3) 0.2565(3) 0.38118(16) 0.0157(5) Uani 1 1 d . . .
C1 C 0.7395(3) 0.0634(3) 0.53088(16) 0.0155(5) Uani 1 1 d . . .
H1A H 0.6479 0.0696 0.5527 0.019 Uiso 1 1 calc R . .
H1B H 0.8389 0.1128 0.5736 0.019 Uiso 1 1 calc R . .
C10 C 0.8073(3) 0.2527(3) 0.24109(17) 0.0183(6) Uani 1 1 d . . .
H10 H 0.7317 0.2084 0.1912 0.022 Uiso 1 1 calc R . .
C7 C 1.0216(3) 0.3851(3) 0.38686(17) 0.0191(6) Uani 1 1 d . . .
H7 H 1.0949 0.4321 0.4370 0.023 Uiso 1 1 calc R . .
C5 C 0.8921(3) 0.1883(3) 0.45370(16) 0.0168(5) Uani 1 1 d . . .
H5A H 0.9337 0.0952 0.4500 0.020 Uiso 1 1 calc R . .
H5B H 0.9635 0.2635 0.5010 0.020 Uiso 1 1 calc R . .
C9 C 0.9320(3) 0.3798(3) 0.24688(17) 0.0162(5) Uani 1 1 d . . .
C11 C 0.7917(3) 0.1897(3) 0.30712(17) 0.0186(6) Uani 1 1 d . . .
H11 H 0.7079 0.1013 0.3017 0.022 Uiso 1 1 calc R . .
O1 O 1.0857(2) 0.5458(2) 0.18644(13) 0.0239(5) Uani 1 1 d . . .
O2 O 0.8511(2) 0.3959(2) 0.11071(12) 0.0222(4) Uani 1 1 d . . .
C14 C 0.5829(3) -0.3013(3) 0.33878(16) 0.0168(5) Uani 1 1 d . . .
C13 C 0.5615(4) -0.3377(3) 0.41686(17) 0.0185(6) Uani 1 1 d . . .
H13A H 0.4567 -0.4115 0.4073 0.022 Uiso 1 1 calc R . .
H13B H 0.6455 -0.3876 0.4402 0.022 Uiso 1 1 calc R . .
C19 C 0.4700(3) -0.2440(3) 0.29106(17) 0.0189(6) Uani 1 1 d . . .
H19 H 0.3815 -0.2259 0.3086 0.023 Uiso 1 1 calc R . .
C12 C 0.9580(3) 0.4461(3) 0.17543(17) 0.0178(6) Uani 1 1 d . . .
C18 C 0.4843(3) -0.2129(3) 0.21836(17) 0.0181(6) Uani 1 1 d . . .
H18 H 0.4051 -0.1752 0.1862 0.022 Uiso 1 1 calc R . .
C15 C 0.7130(3) -0.3257(3) 0.31227(17) 0.0201(6) Uani 1 1 d . . .
H15 H 0.7912 -0.3652 0.3439 0.024 Uiso 1 1 calc R . .
C16 C 0.7289(3) -0.2924(3) 0.23958(17) 0.0196(6) Uani 1 1 d . . .
H16 H 0.8187 -0.3079 0.2224 0.024 Uiso 1 1 calc R . .
C17 C 0.6146(3) -0.2368(3) 0.19226(16) 0.0161(5) Uani 1 1 d . . .
O3 O 0.7558(3) -0.2084(3) 0.09449(13) 0.0242(5) Uani 1 1 d . . .
O4 O 0.5082(3) -0.1804(3) 0.06670(12) 0.0258(5) Uani 1 1 d . . .
C20 C 0.6281(3) -0.2063(3) 0.11212(17) 0.0187(6) Uani 1 1 d . . .
O1S O 0.8606(2) -0.1644(2) -0.11337(12) 0.0226(4) Uani 1 1 d . . .
C2S C 0.6275(4) -0.3148(4) -0.24022(18) 0.0264(7) Uani 1 1 d . . .
H2S1 H 0.6997 -0.3781 -0.2508 0.040 Uiso 1 1 calc R . .
H2S2 H 0.5631 -0.3002 -0.2905 0.040 Uiso 1 1 calc R . .
H2S3 H 0.5570 -0.3665 -0.2118 0.040 Uiso 1 1 calc R . .
C1S C 0.8508(4) -0.0683(4) -0.24863(19) 0.0277(7) Uani 1 1 d . . .
H1S1 H 0.9341 0.0259 -0.2220 0.042 Uiso 1 1 calc R . .
H1S2 H 0.7777 -0.0475 -0.2944 0.042 Uiso 1 1 calc R . .
H1S3 H 0.9000 -0.1488 -0.2665 0.042 Uiso 1 1 calc R . .
O1W O 1.0573(3) 0.7596(3) 0.09550(14) 0.0232(5) Uani 1 1 d . . .
O2W O 1.5207(3) 0.3300(4) 0.08415(17) 0.0408(7) Uani 1 1 d . . .
C3 C 0.5102(3) -0.2416(3) 0.53958(16) 0.0155(5) Uani 1 1 d . . .
H3A H 0.5552 -0.1542 0.5852 0.019 Uiso 1 1 calc R . .
H3B H 0.5493 -0.3305 0.5554 0.019 Uiso 1 1 calc R . .
H2W H 1.503(5) 0.280(5) 0.040(3) 0.041(13) Uiso 1 1 d . . .
H1W H 1.628(6) 0.359(6) 0.096(3) 0.059(14) Uiso 1 1 d . . .
H3W H 0.966(5) 0.778(5) 0.097(2) 0.037(11) Uiso 1 1 d . . .
H4W H 1.063(5) 0.703(5) 0.119(3) 0.037(12) Uiso 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
C4 N1 1.466(3) 2_656 ?
C4 C3 1.520(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
Cs1 O2W 3.052(3) . ?
Cs1 O1 3.158(2) . ?
Cs1 O2 3.159(2) 2_765 ?
Cs1 O1S 3.232(2) 2_755 ?
Cs1 O3 3.237(2) 2_755 ?
Cs1 O1W 3.281(2) 2_765 ?
Cs1 O1W 3.439(2) . ?
Cs1 O4 3.443(2) 1_665 ?
Cs1 C18 3.745(3) 1_665 ?
Cs1 C20 3.844(3) 1_665 ?
Cs1 C17 3.896(3) 1_665 ?
Cs1 S1S 4.1775(8) 2_755 ?
Cs1 H2W 3.24(4) . ?
Cs1 H4W 3.16(4) . ?
Cs2 O2 3.050(2) . ?
Cs2 O4 3.053(2) 2_655 ?
Cs2 O1W 3.069(2) 2_765 ?
Cs2 O3 3.070(2) . ?
Cs2 O1S 3.136(2) 2_755 ?
Cs2 O1S 3.203(2) . ?
Cs2 O4 3.363(2) . ?
Cs2 Cs1 4.4163(3) 2_765 ?
Cs2 Cs2 4.4850(4) 2_755 ?
Cs2 Cs2 4.7750(4) 2_655 ?
Cs2 Cs1 4.8712(4) 2_755 ?
S1S O1S 1.507(2) . ?
S1S C2S 1.792(3) . ?
S1S C1S 1.792(3) . ?
S1S Cs1 4.1775(8) 2_755 ?
N2 C13 1.461(3) . ?
N2 C3 1.468(3) . ?
N2 C2 1.468(3) . ?
N1 C5 1.458(3) . ?
N1 C4 1.466(3) 2_656 ?
N1 C1 1.470(3) . ?
C2 C1 1.521(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C8 C7 1.385(4) . ?
C8 C9 1.393(4) . ?
C8 H8 0.9500 . ?
C6 C7 1.393(4) . ?
C6 C11 1.396(4) . ?
C6 C5 1.509(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C10 C11 1.394(4) . ?
C10 C9 1.396(4) . ?
C10 H10 0.9500 . ?
C7 H7 0.9500 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C9 C12 1.519(4) . ?
C11 H11 0.9500 . ?
O1 C12 1.250(3) . ?
O2 C12 1.259(4) . ?
O2 Cs1 3.159(2) 2_765 ?
C14 C19 1.389(4) . ?
C14 C15 1.396(4) . ?
C14 C13 1.512(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C19 C18 1.385(4) . ?
C19 H19 0.9500 . ?
C18 C17 1.393(4) . ?
C18 Cs1 3.745(3) 1_445 ?
C18 H18 0.9500 . ?
C15 C16 1.395(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.384(4) . ?
C16 H16 0.9500 . ?
C17 C20 1.511(4) . ?
C17 Cs1 3.896(3) 1_445 ?
O3 C20 1.252(3) . ?
O3 Cs1 3.237(2) 2_755 ?
O4 C20 1.262(3) . ?
O4 Cs2 3.053(2) 2_655 ?
O4 Cs1 3.443(2) 1_445 ?
C20 Cs1 3.844(3) 1_445 ?
O1S Cs2 3.136(2) 2_755 ?
O1S Cs1 3.232(2) 2_755 ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O1W Cs2 3.069(2) 2_765 ?
O1W Cs1 3.281(2) 2_765 ?
O1W H3W 0.87(4) . ?
O1W H4W 0.71(4) . ?
O2W H2W 0.81(4) . ?
O2W H1W 0.90(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C4 C3 112.3(2) 2_656 . ?
N1 C4 H4A 109.1 2_656 . ?
C3 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 2_656 . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
O2W Cs1 O1 115.73(6) . . ?
O2W Cs1 O2 121.63(7) . 2_765 ?
O1 Cs1 O2 121.51(5) . 2_765 ?
O2W Cs1 O1S 69.88(7) . 2_755 ?
O1 Cs1 O1S 70.51(5) . 2_755 ?
O2 Cs1 O1S 139.74(5) 2_765 2_755 ?
O2W Cs1 O3 65.19(7) . 2_755 ?
O1 Cs1 O3 144.51(5) . 2_755 ?
O2 Cs1 O3 74.78(5) 2_765 2_755 ?
O1S Cs1 O3 77.75(5) 2_755 2_755 ?
O2W Cs1 O1W 110.38(8) . 2_765 ?
O1 Cs1 O1W 104.59(6) . 2_765 ?
O2 Cs1 O1W 65.80(6) 2_765 2_765 ?
O1S Cs1 O1W 74.02(5) 2_755 2_765 ?
O3 Cs1 O1W 50.04(6) 2_755 2_765 ?
O2W Cs1 O1W 148.85(7) . . ?
O1 Cs1 O1W 48.05(5) . . ?
O2 Cs1 O1W 75.84(5) 2_765 . ?
O1S Cs1 O1W 115.15(5) 2_755 . ?
O3 Cs1 O1W 145.08(6) 2_755 . ?
O1W Cs1 O1W 100.24(5) 2_765 . ?
O2W Cs1 O4 87.74(7) . 1_665 ?
O1 Cs1 O4 101.49(5) . 1_665 ?
O2 Cs1 O4 71.31(5) 2_765 1_665 ?
O1S Cs1 O4 148.12(5) 2_755 1_665 ?
O3 Cs1 O4 113.91(5) 2_755 1_665 ?
O1W Cs1 O4 136.83(5) 2_765 1_665 ?
O1W Cs1 O4 73.16(5) . 1_665 ?
O2W Cs1 C18 84.45(7) . 1_665 ?
O1 Cs1 C18 62.75(6) . 1_665 ?
O2 Cs1 C18 111.52(6) 2_765 1_665 ?
O1S Cs1 C18 107.84(6) 2_755 1_665 ?
O3 Cs1 C18 145.55(6) 2_755 1_665 ?
O1W Cs1 C18 164.28(6) 2_765 1_665 ?
O1W Cs1 C18 64.56(6) . 1_665 ?
O4 Cs1 C18 45.54(6) 1_665 1_665 ?
O2W Cs1 C20 70.68(8) . 1_665 ?
O1 Cs1 C20 101.11(6) . 1_665 ?
O2 Cs1 C20 87.81(6) 2_765 1_665 ?
O1S Cs1 C20 129.91(6) 2_755 1_665 ?
O3 Cs1 C20 111.44(6) 2_755 1_665 ?
O1W Cs1 C20 150.10(6) 2_765 1_665 ?
O1W Cs1 C20 85.74(6) . 1_665 ?
O4 Cs1 C20 18.92(5) 1_665 1_665 ?
C18 Cs1 C20 38.71(6) 1_665 1_665 ?
O2W Cs1 C17 67.97(7) . 1_665 ?
O1 Cs1 C17 82.47(6) . 1_665 ?
O2 Cs1 C17 108.37(6) 2_765 1_665 ?
O1S Cs1 C17 111.41(5) 2_755 1_665 ?
O3 Cs1 C17 124.83(5) 2_755 1_665 ?
O1W Cs1 C17 172.44(6) 2_765 1_665 ?
O1W Cs1 C17 82.40(6) . 1_665 ?
O4 Cs1 C17 37.06(5) 1_665 1_665 ?
C18 Cs1 C17 20.89(6) 1_665 1_665 ?
C20 Cs1 C17 22.50(6) 1_665 1_665 ?
O2W Cs1 S1S 56.41(6) . 2_755 ?
O1 Cs1 S1S 71.03(4) . 2_755 ?
O2 Cs1 S1S 155.45(4) 2_765 2_755 ?
O1S Cs1 S1S 18.37(4) 2_755 2_755 ?
O3 Cs1 S1S 83.83(4) 2_755 2_755 ?
O1W Cs1 S1S 91.27(4) 2_765 2_755 ?
O1W Cs1 S1S 119.01(4) . 2_755 ?
O4 Cs1 S1S 129.87(4) 1_665 2_755 ?
C18 Cs1 S1S 92.93(5) 1_665 2_755 ?
C20 Cs1 S1S 111.54(4) 1_665 2_755 ?
C17 Cs1 S1S 93.62(4) 1_665 2_755 ?
O2W Cs1 H2W 14.4(8) . . ?
O1 Cs1 H2W 127.7(8) . . ?
O2 Cs1 H2W 110.8(8) 2_765 . ?
O1S Cs1 H2W 71.3(7) 2_755 . ?
O3 Cs1 H2W 50.9(8) 2_755 . ?
O1W Cs1 H2W 97.7(8) 2_765 . ?
O1W Cs1 H2W 162.0(8) . . ?
O4 Cs1 H2W 92.7(7) 1_665 . ?
C18 Cs1 H2W 97.6(8) 1_665 . ?
C20 Cs1 H2W 78.0(7) 1_665 . ?
C17 Cs1 H2W 79.6(8) 1_665 . ?
S1S Cs1 H2W 61.6(7) 2_755 . ?
O2W Cs1 H4W 143.6(8) . . ?
O1 Cs1 H4W 36.7(8) . . ?
O2 Cs1 H4W 86.6(8) 2_765 . ?
O1S Cs1 H4W 104.6(8) 2_755 . ?
O3 Cs1 H4W 150.7(8) 2_755 . ?
O1W Cs1 H4W 101.8(8) 2_765 . ?
O1W Cs1 H4W 11.3(8) . . ?
O4 Cs1 H4W 79.9(8) 1_665 . ?
C18 Cs1 H4W 62.5(8) 1_665 . ?
C20 Cs1 H4W 89.8(8) 1_665 . ?
C17 Cs1 H4W 82.2(8) 1_665 . ?
S1S Cs1 H4W 107.7(8) 2_755 . ?
H2W Cs1 H4W 158.0(11) . . ?
O2 Cs2 O4 78.36(6) . 2_655 ?
O2 Cs2 O1W 83.16(6) . 2_765 ?
O4 Cs2 O1W 84.13(6) 2_655 2_765 ?
O2 Cs2 O3 120.70(6) . . ?
O4 Cs2 O3 123.63(6) 2_655 . ?
O1W Cs2 O3 144.72(6) 2_765 . ?
O2 Cs2 O1S 71.98(5) . 2_755 ?
O4 Cs2 O1S 146.99(6) 2_655 2_755 ?
O1W Cs2 O1S 78.36(6) 2_765 2_755 ?
O3 Cs2 O1S 84.80(6) . 2_755 ?
O2 Cs2 O1S 149.28(5) . . ?
O4 Cs2 O1S 109.50(5) 2_655 . ?
O1W Cs2 O1S 68.69(6) 2_765 . ?
O3 Cs2 O1S 80.64(5) . . ?
O1S Cs2 O1S 89.93(5) 2_755 . ?
O2 Cs2 O4 111.98(5) . . ?
O4 Cs2 O4 83.92(6) 2_655 . ?
O1W Cs2 O4 158.29(6) 2_765 . ?
O3 Cs2 O4 40.03(5) . . ?
O1S Cs2 O4 120.34(5) 2_755 . ?
O1S Cs2 O4 98.53(5) . . ?
O2 Cs2 Cs1 45.66(4) . 2_765 ?
O4 Cs2 Cs1 51.00(4) 2_655 2_765 ?
O1W Cs2 Cs1 50.91(5) 2_765 2_765 ?
O3 Cs2 Cs1 163.48(4) . 2_765 ?
O1S Cs2 Cs1 96.83(4) 2_755 2_765 ?
O1S Cs2 Cs1 115.74(4) . 2_765 ?
O4 Cs2 Cs1 129.43(4) . 2_765 ?
O2 Cs2 Cs2 113.43(4) . 2_755 ?
O4 Cs2 Cs2 145.56(4) 2_655 2_755 ?
O1W Cs2 Cs2 66.38(5) 2_765 2_755 ?
O3 Cs2 Cs2 79.66(4) . 2_755 ?
O1S Cs2 Cs2 45.57(4) 2_755 2_755 ?
O1S Cs2 Cs2 44.36(4) . 2_755 ?
O4 Cs2 Cs2 117.33(4) . 2_755 ?
Cs1 Cs2 Cs2 113.156(6) 2_765 2_755 ?
O2 Cs2 Cs1 54.14(4) . . ?
O4 Cs2 Cs1 106.93(4) 2_655 . ?
O1W Cs2 Cs1 43.65(5) 2_765 . ?
O3 Cs2 Cs1 127.66(4) . . ?
O1S Cs2 Cs1 42.86(4) 2_755 . ?
O1S Cs2 Cs1 95.70(4) . . ?
O4 Cs2 Cs1 158.06(4) . . ?
Cs1 Cs2 Cs1 56.141(5) 2_765 . ?
Cs2 Cs2 Cs1 63.793(6) 2_755 . ?
O2 Cs2 Cs2 97.73(4) . 2_655 ?
O4 Cs2 Cs2 44.45(4) 2_655 2_655 ?
O1W Cs2 Cs2 126.08(5) 2_765 2_655 ?
O3 Cs2 Cs2 79.33(4) . 2_655 ?
O1S Cs2 Cs2 153.10(4) 2_755 2_655 ?
O1S Cs2 Cs2 108.53(4) . 2_655 ?
O4 Cs2 Cs2 39.47(3) . 2_655 ?
Cs1 Cs2 Cs2 92.577(5) 2_765 2_655 ?
Cs2 Cs2 Cs2 148.265(8) 2_755 2_655 ?
Cs1 Cs2 Cs2 147.069(6) . 2_655 ?
O2 Cs2 Cs1 159.14(4) . 2_755 ?
O4 Cs2 Cs1 118.48(4) 2_655 2_755 ?
O1W Cs2 Cs1 109.46(5) 2_765 2_755 ?
O3 Cs2 Cs1 40.71(4) . 2_755 ?
O1S Cs2 Cs1 93.81(4) 2_755 2_755 ?
O1S Cs2 Cs1 41.02(4) . 2_755 ?
O4 Cs2 Cs1 61.49(4) . 2_755 ?
Cs1 Cs2 Cs1 154.499(6) 2_765 2_755 ?
Cs2 Cs2 Cs1 60.509(4) 2_755 2_755 ?
Cs1 Cs2 Cs1 124.302(5) . 2_755 ?
Cs2 Cs2 Cs1 88.211(5) 2_655 2_755 ?
O1S S1S C2S 106.13(14) . . ?
O1S S1S C1S 106.52(14) . . ?
C2S S1S C1S 98.24(15) . . ?
O1S S1S Cs1 42.52(8) . 2_755 ?
C2S S1S Cs1 69.74(11) . 2_755 ?
C1S S1S Cs1 132.46(11) . 2_755 ?
C13 N2 C3 110.9(2) . . ?
C13 N2 C2 111.0(2) . . ?
C3 N2 C2 109.2(2) . . ?
C5 N1 C4 111.2(2) . 2_656 ?
C5 N1 C1 108.7(2) . . ?
C4 N1 C1 112.1(2) 2_656 . ?
N2 C2 C1 111.7(2) . . ?
N2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
C7 C8 C9 120.3(3) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C7 C6 C11 118.6(3) . . ?
C7 C6 C5 119.4(2) . . ?
C11 C6 C5 122.0(2) . . ?
N1 C1 C2 111.2(2) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C11 C10 C9 121.2(3) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C8 C7 C6 121.4(3) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
N1 C5 C6 114.5(2) . . ?
N1 C5 H5A 108.6 . . ?
C6 C5 H5A 108.6 . . ?
N1 C5 H5B 108.6 . . ?
C6 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
C8 C9 C10 118.5(3) . . ?
C8 C9 C12 118.9(3) . . ?
C10 C9 C12 122.6(3) . . ?
C10 C11 C6 120.0(3) . . ?
C10 C11 H11 120.0 . . ?
C6 C11 H11 120.0 . . ?
C12 O1 Cs1 109.25(18) . . ?
C12 O2 Cs2 123.69(18) . . ?
C12 O2 Cs1 133.37(18) . 2_765 ?
Cs2 O2 Cs1 90.66(5) . 2_765 ?
C19 C14 C15 118.5(3) . . ?
C19 C14 C13 119.8(2) . . ?
C15 C14 C13 121.7(3) . . ?
N2 C13 C14 112.2(2) . . ?
N2 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
N2 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C18 C19 C14 121.1(3) . . ?
C18 C19 H19 119.4 . . ?
C14 C19 H19 119.4 . . ?
O1 C12 O2 125.8(3) . . ?
O1 C12 C9 116.4(3) . . ?
O2 C12 C9 117.8(3) . . ?
C19 C18 C17 120.2(3) . . ?
C19 C18 Cs1 113.83(18) . 1_445 ?
C17 C18 Cs1 85.65(17) . 1_445 ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
Cs1 C18 H18 70.8 1_445 . ?
C16 C15 C14 120.5(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 119.3(3) . . ?
C16 C17 C20 120.6(2) . . ?
C18 C17 C20 120.1(2) . . ?
C16 C17 Cs1 119.42(19) . 1_445 ?
C18 C17 Cs1 73.46(16) . 1_445 ?
C20 C17 Cs1 76.85(15) . 1_445 ?
C20 O3 Cs2 98.21(17) . . ?
C20 O3 Cs1 120.09(19) . 2_755 ?
Cs2 O3 Cs1 101.08(6) . 2_755 ?
C20 O4 Cs2 168.44(19) . 2_655 ?
C20 O4 Cs2 84.54(17) . . ?
Cs2 O4 Cs2 96.08(6) 2_655 . ?
C20 O4 Cs1 98.83(18) . 1_445 ?
Cs2 O4 Cs1 85.45(5) 2_655 1_445 ?
Cs2 O4 Cs1 155.32(7) . 1_445 ?
O3 C20 O4 123.9(3) . . ?
O3 C20 C17 118.8(3) . . ?
O4 C20 C17 117.3(2) . . ?
O3 C20 Cs1 127.45(19) . 1_445 ?
O4 C20 Cs1 62.25(16) . 1_445 ?
C17 C20 Cs1 80.65(15) . 1_445 ?
S1S O1S Cs2 144.22(12) . 2_755 ?
S1S O1S Cs2 92.03(9) . . ?
Cs2 O1S Cs2 90.07(5) 2_755 . ?
S1S O1S Cs1 119.11(11) . 2_755 ?
Cs2 O1S Cs1 95.82(5) 2_755 2_755 ?
Cs2 O1S Cs1 98.41(6) . 2_755 ?
S1S C2S H2S1 109.5 . . ?
S1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
S1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
S1S C1S H1S1 109.5 . . ?
S1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
S1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
Cs2 O1W Cs1 96.13(7) 2_765 2_765 ?
Cs2 O1W Cs1 85.26(6) 2_765 . ?
Cs1 O1W Cs1 79.76(5) 2_765 . ?
Cs2 O1W H3W 114(3) 2_765 . ?
Cs1 O1W H3W 68(3) 2_765 . ?
Cs1 O1W H3W 144(3) . . ?
Cs2 O1W H4W 143(4) 2_765 . ?
Cs1 O1W H4W 93(4) 2_765 . ?
Cs1 O1W H4W 61(4) . . ?
H3W O1W H4W 103(4) . . ?
Cs1 O2W H2W 96(3) . . ?
Cs1 O2W H1W 139(3) . . ?
H2W O2W H1W 98(4) . . ?
N2 C3 C4 114.2(2) . . ?
N2 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N2 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.214


data_global

#END


data_5
#TrackingRef '16829_web_deposit_cif_file_0_YoichiHabata_1357997395.All_1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H40 Br4 N4'
_chemical_formula_weight         848.36

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.399(3)
_cell_length_b                   9.641(5)
_cell_length_c                   12.392(6)
_cell_angle_alpha                95.954(8)
_cell_angle_beta                 96.675(8)
_cell_angle_gamma                96.258(8)
_cell_volume                     866.7(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100
_cell_measurement_reflns_used    1603
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    4.675
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3442
_exptl_absorpt_correction_T_max  0.4579
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5174
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0926
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3794
_reflns_number_gt                2582
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.2000P)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         3794
_refine_ls_number_parameters     199
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1281
_refine_ls_R_factor_gt           0.0966
_refine_ls_wR_factor_ref         0.2815
_refine_ls_wR_factor_gt          0.2542
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
Br1 Br 1.50350(12) 0.28463(9) 0.49397(7) 0.0300(3) Uani 1 1 d . . .
Br2 Br 1.16379(12) 0.62796(9) 0.25865(9) 0.0349(3) Uani 1 1 d . . .
N2 N 0.6862(9) -0.0176(7) 0.1802(5) 0.0209(14) Uani 1 1 d . . .
C9 C 0.9248(11) 0.5290(8) 0.2126(7) 0.0219(17) Uani 1 1 d U . .
N1 N 0.3861(9) 0.1648(7) 0.0716(6) 0.0208(14) Uani 1 1 d . . .
C16 C 1.2706(11) 0.1920(9) 0.4304(7) 0.0219(17) Uani 1 1 d . . .
C12 C 0.7352(11) -0.0140(9) 0.2984(7) 0.0230(17) Uani 1 1 d . . .
H12A H 0.7261 -0.1115 0.3174 0.028 Uiso 1 1 calc R . .
H12B H 0.6456 0.0351 0.3363 0.028 Uiso 1 1 calc R . .
C5 C 0.3892(12) 0.3172(9) 0.0987(8) 0.0262(18) Uani 1 1 d . . .
H5A H 0.3054 0.3346 0.1540 0.031 Uiso 1 1 calc R . .
H5B H 0.3430 0.3579 0.0323 0.031 Uiso 1 1 calc R . .
C10 C 0.7855(12) 0.5461(8) 0.2767(7) 0.0257(18) Uani 1 1 d . . .
H10 H 0.8080 0.6053 0.3443 0.031 Uiso 1 1 calc R . .
C6 C 0.5765(12) 0.3898(8) 0.1421(7) 0.0222(17) Uani 1 1 d . . .
C3 C 0.7787(11) -0.1242(8) 0.1218(7) 0.0243(18) Uani 1 1 d . . .
H3A H 0.7159 -0.2188 0.1272 0.029 Uiso 1 1 calc R . .
H3B H 0.9067 -0.1191 0.1571 0.029 Uiso 1 1 calc R . .
C18 C 1.0636(12) -0.0189(8) 0.3789(7) 0.0232(17) Uani 1 1 d . . .
H18 H 1.0385 -0.1182 0.3749 0.028 Uiso 1 1 calc R . .
C13 C 0.9257(12) 0.0584(9) 0.3397(7) 0.0233(17) Uani 1 1 d . . .
C2 C 0.4863(12) -0.0419(8) 0.1541(7) 0.0233(17) Uani 1 1 d . . .
H2A H 0.4359 -0.1099 0.2009 0.028 Uiso 1 1 calc R . .
H2B H 0.4535 -0.0833 0.0769 0.028 Uiso 1 1 calc R . .
C4 C 0.7793(11) -0.1033(8) 0.0006(7) 0.0210(16) Uani 1 1 d . . .
H4A H 0.7979 -0.0012 -0.0051 0.025 Uiso 1 1 calc R . .
H4B H 0.8853 -0.1444 -0.0258 0.025 Uiso 1 1 calc R . .
C17 C 1.2370(12) 0.0469(9) 0.4238(7) 0.0242(17) Uani 1 1 d . . .
H17 H 1.3303 -0.0066 0.4492 0.029 Uiso 1 1 calc R . .
C11 C 0.6139(12) 0.4754(9) 0.2405(7) 0.0253(18) Uani 1 1 d . . .
H11 H 0.5182 0.4859 0.2845 0.030 Uiso 1 1 calc R . .
C1 C 0.4013(12) 0.0938(9) 0.1719(7) 0.0234(17) Uani 1 1 d . . .
H1A H 0.2778 0.0728 0.1940 0.028 Uiso 1 1 calc R . .
H1B H 0.4775 0.1574 0.2319 0.028 Uiso 1 1 calc R . .
C14 C 0.9662(12) 0.2034(9) 0.3447(7) 0.0247(18) Uani 1 1 d . . .
H14 H 0.8749 0.2569 0.3164 0.030 Uiso 1 1 calc R . .
C8 C 0.8958(13) 0.4395(9) 0.1152(7) 0.0281(18) Uani 1 1 d U . .
H8 H 0.9934 0.4249 0.0734 0.034 Uiso 1 1 calc R . .
C7 C 0.7211(12) 0.3724(9) 0.0809(7) 0.0283(19) Uani 1 1 d . . .
H7 H 0.6985 0.3126 0.0136 0.034 Uiso 1 1 calc R . .
C15 C 1.1369(12) 0.2717(9) 0.3898(7) 0.0260(18) Uani 1 1 d . . .
H15 H 1.1625 0.3709 0.3932 0.031 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
Br1 C16 1.895(8) . ?
Br2 C9 1.910(8) . ?
N2 C12 1.464(11) . ?
N2 C2 1.464(11) . ?
N2 C3 1.470(10) . ?
C9 C10 1.386(12) . ?
C9 C8 1.390(12) . ?
N1 C4 1.458(10) 2_655 ?
N1 C5 1.470(10) . ?
N1 C1 1.478(11) . ?
C16 C17 1.386(11) . ?
C16 C15 1.397(12) . ?
C12 C13 1.510(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C5 C6 1.496(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C10 C11 1.376(12) . ?
C10 H10 0.9500 . ?
C6 C11 1.381(12) . ?
C6 C7 1.396(12) . ?
C3 C4 1.536(12) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C18 C17 1.393(12) . ?
C18 C13 1.400(12) . ?
C18 H18 0.9500 . ?
C13 C14 1.391(11) . ?
C2 C1 1.519(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 N1 1.458(10) 2_655 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C17 H17 0.9500 . ?
C11 H11 0.9500 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C14 C15 1.385(12) . ?
C14 H14 0.9500 . ?
C8 C7 1.379(12) . ?
C8 H8 0.9500 . ?
C7 H7 0.9500 . ?
C15 H15 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
C12 N2 C2 109.1(6) . . ?
C12 N2 C3 110.0(7) . . ?
C2 N2 C3 112.9(6) . . ?
C10 C9 C8 121.5(8) . . ?
C10 C9 Br2 119.9(6) . . ?
C8 C9 Br2 118.6(6) . . ?
C4 N1 C5 111.7(6) 2_655 . ?
C4 N1 C1 109.7(6) 2_655 . ?
C5 N1 C1 110.9(6) . . ?
C17 C16 C15 121.3(7) . . ?
C17 C16 Br1 119.5(6) . . ?
C15 C16 Br1 119.1(6) . . ?
N2 C12 C13 113.6(7) . . ?
N2 C12 H12A 108.9 . . ?
C13 C12 H12A 108.9 . . ?
N2 C12 H12B 108.9 . . ?
C13 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
N1 C5 C6 112.9(7) . . ?
N1 C5 H5A 109.0 . . ?
C6 C5 H5A 109.0 . . ?
N1 C5 H5B 109.0 . . ?
C6 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
C11 C10 C9 118.6(8) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C11 C6 C7 117.8(8) . . ?
C11 C6 C5 122.9(8) . . ?
C7 C6 C5 119.3(8) . . ?
N2 C3 C4 111.9(7) . . ?
N2 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C17 C18 C13 121.3(7) . . ?
C17 C18 H18 119.4 . . ?
C13 C18 H18 119.4 . . ?
C14 C13 C18 118.4(7) . . ?
C14 C13 C12 121.1(8) . . ?
C18 C13 C12 120.3(7) . . ?
N2 C2 C1 111.4(6) . . ?
N2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N1 C4 C3 115.4(6) 2_655 . ?
N1 C4 H4A 108.4 2_655 . ?
C3 C4 H4A 108.4 . . ?
N1 C4 H4B 108.4 2_655 . ?
C3 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
C16 C17 C18 118.6(7) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
C10 C11 C6 122.0(8) . . ?
C10 C11 H11 119.0 . . ?
C6 C11 H11 119.0 . . ?
N1 C1 C2 111.4(7) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C15 C14 C13 121.5(8) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C7 C8 C9 118.0(8) . . ?
C7 C8 H8 121.0 . . ?
C9 C8 H8 121.0 . . ?
C8 C7 C6 122.0(8) . . ?
C8 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C14 C15 C16 118.8(7) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?

_diffrn_measured_fraction_theta_max 0.954
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.954
_refine_diff_density_max         3.941
_refine_diff_density_min         -2.395
_refine_diff_density_rms         0.304


data_global

#END


data_3
#TrackingRef '16829_web_deposit_cif_file_0_YoichiHabata_1357997395.All_1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H52 N4 O8'
_chemical_formula_weight         764.90

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0192(9)
_cell_length_b                   10.1213(9)
_cell_length_c                   11.6590(11)
_cell_angle_alpha                110.849(2)
_cell_angle_beta                 103.926(2)
_cell_angle_gamma                103.909(2)
_cell_volume                     1000.74(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    173
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             408
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9594
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7524
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         28.27
_reflns_number_total             4903
_reflns_number_gt                3763
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0783P)²+0.1714P] 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         4903
_refine_ls_number_parameters     255
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.1477
_refine_ls_wR_factor_gt          0.1359
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
N1 N 0.45484(13) 0.80655(13) 0.09025(11) 0.0248(3) Uani 1 1 d . . .
N2 N 0.42225(13) 1.13116(13) 0.12511(11) 0.0244(3) Uani 1 1 d . . .
O2 O 0.94975(12) 0.68138(14) 0.55467(12) 0.0412(3) Uani 1 1 d . . .
O3 O -0.13022(14) 1.31806(15) -0.25608(13) 0.0485(3) Uani 1 1 d . . .
C9 C 0.71263(16) 0.65234(16) 0.42746(14) 0.0271(3) Uani 1 1 d . . .
C6 C 0.52076(16) 0.66533(16) 0.21750(14) 0.0262(3) Uani 1 1 d . . .
O1 O 0.75771(14) 0.56985(17) 0.59562(12) 0.0484(3) Uani 1 1 d . . .
O4 O -0.15829(14) 1.08017(15) -0.38156(12) 0.0510(4) Uani 1 1 d . . .
C16 C 0.14063(17) 1.29490(17) 0.06941(16) 0.0328(3) Uani 1 1 d . . .
H16 H 0.1710 1.3716 0.1565 0.039 Uiso 1 1 calc R . .
C15 C 0.19379(16) 1.17687(17) 0.04612(15) 0.0279(3) Uani 1 1 d . . .
C8 C 0.56747(16) 0.63313(17) 0.41662(15) 0.0291(3) Uani 1 1 d . . .
H8 H 0.5332 0.6147 0.4807 0.035 Uiso 1 1 calc R . .
C7 C 0.47253(16) 0.64060(17) 0.31325(15) 0.0282(3) Uani 1 1 d . . .
H7 H 0.3738 0.6288 0.3074 0.034 Uiso 1 1 calc R . .
C2 C 0.49632(16) 1.07923(16) 0.21642(14) 0.0268(3) Uani 1 1 d . . .
H2A H 0.5068 1.1457 0.3067 0.032 Uiso 1 1 calc R . .
H2B H 0.5966 1.0908 0.2146 0.032 Uiso 1 1 calc R . .
C10 C 0.76340(16) 0.68235(18) 0.33477(16) 0.0315(3) Uani 1 1 d . . .
H10 H 0.8634 0.6988 0.3430 0.038 Uiso 1 1 calc R . .
C14 C 0.29902(17) 1.16798(18) 0.15756(15) 0.0306(3) Uani 1 1 d . . .
H14A H 0.3382 1.2664 0.2366 0.037 Uiso 1 1 calc R . .
H14B H 0.2449 1.0896 0.1787 0.037 Uiso 1 1 calc R . .
C18 C -0.00302(15) 1.19002(17) -0.16091(15) 0.0295(3) Uani 1 1 d . . .
C12 C 0.80569(17) 0.62984(17) 0.53428(14) 0.0308(3) Uani 1 1 d . . .
C21 C -0.10256(16) 1.20580(19) -0.26831(17) 0.0341(4) Uani 1 1 d . . .
C11 C 0.66748(16) 0.68811(17) 0.23068(15) 0.0307(3) Uani 1 1 d . . .
H11 H 0.7022 0.7079 0.1673 0.037 Uiso 1 1 calc R . .
C1 C 0.41668(16) 0.91549(16) 0.18622(14) 0.0273(3) Uani 1 1 d . . .
H1A H 0.4413 0.9042 0.2689 0.033 Uiso 1 1 calc R . .
H1B H 0.3090 0.8918 0.1520 0.033 Uiso 1 1 calc R . .
C3 C 0.52838(16) 1.26387(16) 0.13044(14) 0.0268(3) Uani 1 1 d . . .
H3A H 0.5957 1.3300 0.2226 0.032 Uiso 1 1 calc R . .
H3B H 0.4746 1.3226 0.1001 0.032 Uiso 1 1 calc R . .
C17 C 0.04376(18) 1.30139(18) -0.03337(16) 0.0344(4) Uani 1 1 d . . .
H17 H 0.0088 1.3832 -0.0164 0.041 Uiso 1 1 calc R . .
C5 C 0.41574(16) 0.66143(17) 0.09816(15) 0.0289(3) Uani 1 1 d . . .
H5A H 0.4148 0.5817 0.0180 0.035 Uiso 1 1 calc R . .
H5B H 0.3150 0.6339 0.1005 0.035 Uiso 1 1 calc R . .
C4 C 0.38164(15) 0.78160(17) -0.04534(14) 0.0266(3) Uani 1 1 d . . .
H4A H 0.3677 0.8757 -0.0440 0.032 Uiso 1 1 calc R . .
H4B H 0.2832 0.7009 -0.0840 0.032 Uiso 1 1 calc R . .
C20 C 0.14535(17) 1.06471(18) -0.08160(16) 0.0351(4) Uani 1 1 d . . .
H20 H 0.1803 0.9829 -0.0986 0.042 Uiso 1 1 calc R . .
C19 C 0.04706(17) 1.06987(19) -0.18466(16) 0.0349(4) Uani 1 1 d . . .
H19 H 0.0140 0.9915 -0.2713 0.042 Uiso 1 1 calc R . .
C13 C 1.0431(2) 0.6573(2) 0.65558(19) 0.0490(5) Uani 1 1 d . . .
H13A H 1.0406 0.7181 0.7413 0.073 Uiso 1 1 calc R . .
H13B H 1.1445 0.6877 0.6576 0.073 Uiso 1 1 calc R . .
H13C H 1.0073 0.5498 0.6360 0.073 Uiso 1 1 calc R . .
C22 C -0.2537(3) 1.0867(3) -0.4924(2) 0.0646(6) Uani 1 1 d . . .
H22A H -0.3394 1.1054 -0.4736 0.097 Uiso 1 1 calc R . .
H22B H -0.2868 0.9902 -0.5707 0.097 Uiso 1 1 calc R . .
H22C H -0.1997 1.1689 -0.5083 0.097 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
N1 C1 1.4643(18) . ?
N1 C5 1.4685(18) . ?
N1 C4 1.4730(17) . ?
N2 C14 1.4670(18) . ?
N2 C3 1.4700(19) . ?
N2 C2 1.4717(17) . ?
O2 C12 1.3404(19) . ?
O2 C13 1.4502(19) . ?
O3 C21 1.201(2) . ?
C9 C8 1.388(2) . ?
C9 C10 1.394(2) . ?
C9 C12 1.489(2) . ?
C6 C11 1.393(2) . ?
C6 C7 1.394(2) . ?
C6 C5 1.5102(19) . ?
O1 C12 1.202(2) . ?
O4 C21 1.334(2) . ?
O4 C22 1.444(2) . ?
C16 C17 1.382(2) . ?
C16 C15 1.389(2) . ?
C15 C20 1.388(2) . ?
C15 C14 1.509(2) . ?
C8 C7 1.382(2) . ?
C2 C1 1.523(2) . ?
C10 C11 1.384(2) . ?
C18 C17 1.385(2) . ?
C18 C19 1.388(2) . ?
C18 C21 1.485(2) . ?
C3 C4 1.521(2) 2_675 ?
C4 C3 1.521(2) 2_675 ?
C20 C19 1.384(2) . ?

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
C1 N1 C5 109.99(11) . . ?
C1 N1 C4 112.42(11) . . ?
C5 N1 C4 109.48(11) . . ?
C14 N2 C3 110.44(11) . . ?
C14 N2 C2 110.42(11) . . ?
C3 N2 C2 109.92(11) . . ?
C12 O2 C13 114.62(14) . . ?
C8 C9 C10 119.61(13) . . ?
C8 C9 C12 117.83(13) . . ?
C10 C9 C12 122.44(13) . . ?
C11 C6 C7 118.82(13) . . ?
C11 C6 C5 119.94(13) . . ?
C7 C6 C5 121.19(13) . . ?
C21 O4 C22 115.90(15) . . ?
C17 C16 C15 120.37(15) . . ?
C20 C15 C16 118.66(14) . . ?
C20 C15 C14 120.42(13) . . ?
C16 C15 C14 120.91(14) . . ?
C7 C8 C9 120.45(14) . . ?
C8 C7 C6 120.41(13) . . ?
N2 C2 C1 114.46(12) . . ?
C11 C10 C9 119.70(14) . . ?
N2 C14 C15 112.16(12) . . ?
C17 C18 C19 119.26(14) . . ?
C17 C18 C21 118.48(14) . . ?
C19 C18 C21 122.24(15) . . ?
O1 C12 O2 122.75(14) . . ?
O1 C12 C9 124.01(15) . . ?
O2 C12 C9 113.23(13) . . ?
O3 C21 O4 123.34(15) . . ?
O3 C21 C18 124.52(16) . . ?
O4 C21 C18 112.14(14) . . ?
C10 C11 C6 120.96(14) . . ?
N1 C1 C2 113.14(12) . . ?
N2 C3 C4 111.79(11) . 2_675 ?
C16 C17 C18 120.75(14) . . ?
N1 C5 C6 113.02(12) . . ?
N1 C4 C3 111.38(11) . 2_675 ?
C19 C20 C15 121.17(14) . . ?
C20 C19 C18 119.78(15) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        28.27
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.052


data_global

#END


data_3a
#TrackingRef '16829_web_deposit_cif_file_0_YoichiHabata_1357997395.All_1.cif'/AgCF3SO3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C90 H106 Ag2 F6 N8 O23 S2'
_chemical_formula_weight         2061.69

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4/n

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

_cell_length_a                   13.997(4)
_cell_length_b                   13.997(4)
_cell_length_c                   23.804(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4664(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2132
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8913
_exptl_absorpt_correction_T_max  0.9462
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34383
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         0.86
_diffrn_reflns_theta_max         28.33
_reflns_number_total             5822
_reflns_number_gt                4762
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0830P)²+2.3621P] 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         5822
_refine_ls_number_parameters     332
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1540
_refine_ls_wR_factor_gt          0.1417
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.122
_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
Ag1 Ag 0.7500 0.7500 0.209745(18) 0.02492(14) Uani 1 4 d S . .
Ag2 Ag 0.7500 0.7500 0.672727(19) 0.02589(14) Uani 1 4 d S . .
C1 C 0.8210(2) 0.9279(2) 0.74597(14) 0.0327(7) Uani 1 1 d . . .
H1A H 0.8163 0.9778 0.7166 0.039 Uiso 1 1 calc R . .
H1B H 0.8592 0.9543 0.7773 0.039 Uiso 1 1 calc R . .
C2 C 0.9051(2) 0.7790(2) 0.76736(14) 0.0326(7) Uani 1 1 d . . .
H2A H 0.8551 0.7746 0.7966 0.039 Uiso 1 1 calc R . .
H2B H 0.9631 0.8064 0.7850 0.039 Uiso 1 1 calc R . .
C5 C 0.9551(2) 0.8773(2) 0.68860(14) 0.0323(7) Uani 1 1 d . . .
H5A H 1.0008 0.8238 0.6843 0.039 Uiso 1 1 calc R . .
H5B H 0.9880 0.9293 0.7091 0.039 Uiso 1 1 calc R . .
C6 C 0.9265(2) 0.9131(2) 0.63101(14) 0.0298(7) Uani 1 1 d . . .
C7 C 0.9115(2) 0.8472(2) 0.58766(14) 0.0340(7) Uani 1 1 d . . .
H7 H 0.9179 0.7809 0.5952 0.041 Uiso 1 1 calc R . .
C8 C 0.8874(2) 0.8770(2) 0.53422(15) 0.0360(7) Uani 1 1 d . . .
H8 H 0.8771 0.8311 0.5054 0.043 Uiso 1 1 calc R . .
C9 C 0.8783(2) 0.9741(2) 0.52245(14) 0.0322(7) Uani 1 1 d . . .
C10 C 0.8937(3) 1.0404(3) 0.56491(15) 0.0389(8) Uani 1 1 d . . .
H10 H 0.8883 1.1068 0.5572 0.047 Uiso 1 1 calc R . .
C11 C 0.9172(3) 1.0096(2) 0.61900(15) 0.0375(8) Uani 1 1 d . . .
H11 H 0.9269 1.0553 0.6479 0.045 Uiso 1 1 calc R . .
C12 C 0.8517(3) 1.0040(3) 0.46468(16) 0.0417(8) Uani 1 1 d . . .
C13 C 0.8273(3) 1.1325(3) 0.40332(18) 0.0555(11) Uani 1 1 d . . .
H13A H 0.7581 1.1271 0.3977 0.083 Uiso 1 1 calc R . .
H13B H 0.8606 1.0942 0.3750 0.083 Uiso 1 1 calc R . .
H13C H 0.8465 1.1996 0.3998 0.083 Uiso 1 1 calc R . .
C23 C 0.6610(2) 0.5809(2) 0.28292(14) 0.0299(7) Uani 1 1 d . . .
H23A H 0.6597 0.5299 0.2541 0.036 Uiso 1 1 calc R . .
H23B H 0.6205 0.5597 0.3146 0.036 Uiso 1 1 calc R . .
C24 C 0.5921(2) 0.7373(2) 0.30380(13) 0.0291(6) Uani 1 1 d . . .
H24A H 0.6419 0.7358 0.3333 0.035 Uiso 1 1 calc R . .
H24B H 0.5312 0.7164 0.3211 0.035 Uiso 1 1 calc R . .
C26 C 0.5333(2) 0.6447(2) 0.22495(14) 0.0314(7) Uani 1 1 d . . .
H26A H 0.4939 0.7028 0.2201 0.038 Uiso 1 1 calc R . .
H26B H 0.4946 0.5972 0.2458 0.038 Uiso 1 1 calc R . .
C27 C 0.5575(2) 0.6046(2) 0.16786(14) 0.0333(7) Uani 1 1 d . . .
C28 C 0.5787(3) 0.6665(3) 0.12344(16) 0.0476(9) Uani 1 1 d . . .
H28 H 0.5777 0.7336 0.1295 0.057 Uiso 1 1 calc R . .
C29 C 0.6009(3) 0.6316(4) 0.07131(17) 0.0574(12) Uani 1 1 d . . .
H29 H 0.6146 0.6748 0.0416 0.069 Uiso 1 1 calc R . .
C30 C 0.6036(3) 0.5339(4) 0.06144(17) 0.0555(11) Uani 1 1 d . . .
C31 C 0.5825(3) 0.4717(3) 0.1045(2) 0.0571(11) Uani 1 1 d . . .
H31 H 0.5837 0.4047 0.0981 0.069 Uiso 1 1 calc R . .
C32 C 0.5595(3) 0.5074(3) 0.15727(18) 0.0477(9) Uani 1 1 d . . .
H32 H 0.5447 0.4641 0.1867 0.057 Uiso 1 1 calc R . .
C33 C 0.6323(4) 0.4983(6) 0.0045(2) 0.086(2) Uani 1 1 d . . .
C34 C 0.6605(7) 0.3818(9) -0.0595(3) 0.165(4) Uani 1 1 d U . .
H34A H 0.6695 0.4404 -0.0814 0.248 Uiso 1 1 calc R . .
H34B H 0.6111 0.3424 -0.0772 0.248 Uiso 1 1 calc R . .
H34C H 0.7207 0.3461 -0.0582 0.248 Uiso 1 1 calc R . .
C2A C 0.2500 0.7500 0.1997(4) 0.115(4) Uani 1 2 d S . .
F1A F 0.1947(14) 0.7775(10) 0.1684(6) 0.131(6) Uani 0.50 1 d P . .
F2A F 0.2014(13) 0.8304(10) 0.1788(5) 0.117(5) Uani 0.50 1 d P . .
F3A F 0.3391(7) 0.8283(8) 0.2046(7) 0.183(6) Uani 0.50 1 d P . .
N1 N 0.87195(18) 0.84418(18) 0.72232(11) 0.0270(5) Uani 1 1 d . . .
N3 N 0.61859(17) 0.66888(17) 0.25841(11) 0.0257(5) Uani 1 1 d . . .
O1 O 0.8516(2) 1.0981(2) 0.45857(12) 0.0507(7) Uani 1 1 d . . .
O2 O 0.8310(3) 0.9479(2) 0.42751(13) 0.0702(10) Uani 1 1 d . . .
O5 O 0.6304(3) 0.4070(4) -0.00122(17) 0.0967(14) Uani 1 1 d U . .
O6 O 0.6532(4) 0.5523(4) -0.03294(19) 0.1119(17) Uani 1 1 d . . .
O1A O 0.1527(6) 0.6769(6) 0.2639(4) 0.089(3) Uani 0.50 1 d P . .
O2A O 0.1894(10) 0.8108(13) 0.2957(6) 0.076(5) Uani 0.50 1 d P . .
O3A O 0.2077(16) 0.8299(14) 0.2889(8) 0.121(8) Uani 0.50 1 d P . .
O1W O 0.7500 0.7500 0.8928(6) 0.213(7) Uani 1 4 d S . .
S1 S 0.23184(18) 0.7363(2) 0.27051(7) 0.0416(6) 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
Ag1 N3 2.452(2) 3_665 ?
Ag1 N3 2.452(2) 2_655 ?
Ag1 N3 2.452(2) . ?
Ag1 N3 2.452(2) 4_565 ?
Ag2 N1 2.459(3) . ?
Ag2 N1 2.459(3) 3_665 ?
Ag2 N1 2.459(3) 4_565 ?
Ag2 N1 2.459(3) 2_655 ?
C1 N1 1.482(4) . ?
C1 C2 1.523(5) 2_655 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N1 1.482(4) . ?
C2 C1 1.523(5) 4_565 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C5 N1 1.487(4) . ?
C5 C6 1.513(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C11 1.387(5) . ?
C6 C7 1.399(5) . ?
C7 C8 1.380(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.394(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(5) . ?
C9 C12 1.485(5) . ?
C10 C11 1.397(5) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 O2 1.218(5) . ?
C12 O1 1.325(5) . ?
C13 O1 1.441(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C23 N3 1.487(4) . ?
C23 C24 1.515(4) 2_655 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N3 1.491(4) . ?
C24 C23 1.515(4) 4_565 ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 N3 1.475(4) . ?
C26 C27 1.509(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C32 1.384(5) . ?
C27 C28 1.399(5) . ?
C28 C29 1.369(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.388(7) . ?
C29 H29 0.9500 . ?
C30 C31 1.376(7) . ?
C30 C33 1.499(6) . ?
C31 C32 1.391(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 O6 1.205(8) . ?
C33 O5 1.285(8) . ?
C34 O5 1.493(7) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C2A F1A 1.142(15) 3_565 ?
C2A F1A 1.142(15) . ?
C2A F2A 1.407(12) 3_565 ?
C2A F2A 1.407(12) . ?
C2A F3A 1.663(11) 3_565 ?
C2A F3A 1.663(11) . ?
C2A S1 1.715(10) . ?
C2A S1 1.715(10) 3_565 ?
F1A F2A 0.79(2) . ?
F1A F1A 1.73(3) 3_565 ?
F1A F3A 1.78(2) 3_565 ?
F3A O1A 1.419(16) 3_565 ?
F3A F1A 1.78(2) 3_565 ?
F3A S1 2.065(10) 3_565 ?
O1A S1 1.394(8) . ?
O1A F3A 1.419(16) 3_565 ?
O1A S1 2.028(8) 3_565 ?
O2A S1 1.342(16) . ?
O2A S1 1.418(12) 3_565 ?
O3A S1 1.329(17) 3_565 ?
O3A S1 1.421(18) . ?
S1 S1 0.637(4) 3_565 ?
S1 O3A 1.329(17) 3_565 ?
S1 O2A 1.418(12) 3_565 ?
S1 O1A 2.028(8) 3_565 ?
S1 F3A 2.065(10) 3_565 ?

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 Ag1 N3 77.11(5) 3_665 2_655 ?
N3 Ag1 N3 123.63(12) 3_665 . ?
N3 Ag1 N3 77.11(5) 2_655 . ?
N3 Ag1 N3 77.11(5) 3_665 4_565 ?
N3 Ag1 N3 123.63(12) 2_655 4_565 ?
N3 Ag1 N3 77.11(5) . 4_565 ?
N1 Ag2 N1 122.61(12) . 3_665 ?
N1 Ag2 N1 76.67(5) . 4_565 ?
N1 Ag2 N1 76.67(5) 3_665 4_565 ?
N1 Ag2 N1 76.67(5) . 2_655 ?
N1 Ag2 N1 76.67(5) 3_665 2_655 ?
N1 Ag2 N1 122.61(12) 4_565 2_655 ?
N1 C1 C2 113.8(2) . 2_655 ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 2_655 . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 2_655 . ?
H1A C1 H1B 107.7 . . ?
N1 C2 C1 112.9(3) . 4_565 ?
N1 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 4_565 . ?
N1 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 4_565 . ?
H2A C2 H2B 107.8 . . ?
N1 C5 C6 112.7(2) . . ?
N1 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
N1 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
C11 C6 C7 118.4(3) . . ?
C11 C6 C5 122.3(3) . . ?
C7 C6 C5 119.3(3) . . ?
C8 C7 C6 121.2(3) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C9 120.1(3) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 C12 121.6(3) . . ?
C8 C9 C12 118.9(3) . . ?
C9 C10 C11 120.0(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C6 C11 C10 120.9(3) . . ?
C6 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
O2 C12 O1 124.1(4) . . ?
O2 C12 C9 123.4(4) . . ?
O1 C12 C9 112.5(3) . . ?
O1 C13 H13A 109.5 . . ?
O1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C23 C24 114.7(2) . 2_655 ?
N3 C23 H23A 108.6 . . ?
C24 C23 H23A 108.6 2_655 . ?
N3 C23 H23B 108.6 . . ?
C24 C23 H23B 108.6 2_655 . ?
H23A C23 H23B 107.6 . . ?
N3 C24 C23 113.0(3) . 4_565 ?
N3 C24 H24A 109.0 . . ?
C23 C24 H24A 109.0 4_565 . ?
N3 C24 H24B 109.0 . . ?
C23 C24 H24B 109.0 4_565 . ?
H24A C24 H24B 107.8 . . ?
N3 C26 C27 112.9(3) . . ?
N3 C26 H26A 109.0 . . ?
C27 C26 H26A 109.0 . . ?
N3 C26 H26B 109.0 . . ?
C27 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
C32 C27 C28 117.9(3) . . ?
C32 C27 C26 122.3(3) . . ?
C28 C27 C26 119.8(3) . . ?
C29 C28 C27 120.8(4) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 120.7(4) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C31 C30 C29 119.4(4) . . ?
C31 C30 C33 121.3(5) . . ?
C29 C30 C33 119.2(5) . . ?
C30 C31 C32 119.7(4) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C27 C32 C31 121.5(4) . . ?
C27 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
O6 C33 O5 123.4(5) . . ?
O6 C33 C30 121.7(7) . . ?
O5 C33 C30 114.9(6) . . ?
O5 C34 H34A 109.5 . . ?
O5 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O5 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
F1A C2A F1A 98.4(17) 3_565 . ?
F1A C2A F2A 34.0(11) 3_565 3_565 ?
F1A C2A F2A 111.4(10) . 3_565 ?
F1A C2A F2A 111.4(10) 3_565 . ?
F1A C2A F2A 34.0(11) . . ?
F2A C2A F2A 138.5(12) 3_565 . ?
F1A C2A F3A 109.4(11) 3_565 3_565 ?
F1A C2A F3A 76.1(11) . 3_565 ?
F2A C2A F3A 81.9(9) 3_565 3_565 ?
F2A C2A F3A 100.9(9) . 3_565 ?
F1A C2A F3A 76.1(11) 3_565 . ?
F1A C2A F3A 109.4(11) . . ?
F2A C2A F3A 100.9(9) 3_565 . ?
F2A C2A F3A 81.9(9) . . ?
F3A C2A F3A 172.0(14) 3_565 . ?
F1A C2A S1 134.8(8) 3_565 . ?
F1A C2A S1 125.4(9) . . ?
F2A C2A S1 109.3(6) 3_565 . ?
F2A C2A S1 111.5(6) . . ?
F3A C2A S1 75.3(6) 3_565 . ?
F3A C2A S1 96.7(7) . . ?
F1A C2A S1 125.4(9) 3_565 3_565 ?
F1A C2A S1 134.8(8) . 3_565 ?
F2A C2A S1 111.5(6) 3_565 3_565 ?
F2A C2A S1 109.3(6) . 3_565 ?
F3A C2A S1 96.7(7) 3_565 3_565 ?
F3A C2A S1 75.3(6) . 3_565 ?
S1 C2A S1 21.38(17) . 3_565 ?
F2A F1A C2A 92(2) . . ?
F2A F1A F1A 108(3) . 3_565 ?
C2A F1A F1A 40.8(9) . 3_565 ?
F2A F1A F3A 132(2) . 3_565 ?
C2A F1A F3A 65.3(8) . 3_565 ?
F1A F1A F3A 82.4(9) 3_565 3_565 ?
F1A F2A C2A 54.2(16) . . ?
O1A F3A C2A 95.6(7) 3_565 . ?
O1A F3A F1A 117.5(8) 3_565 3_565 ?
C2A F3A F1A 38.6(7) . 3_565 ?
O1A F3A S1 42.3(4) 3_565 3_565 ?
C2A F3A S1 53.5(4) . 3_565 ?
F1A F3A S1 82.9(6) 3_565 3_565 ?
C2 N1 C1 111.2(2) . . ?
C2 N1 C5 109.7(2) . . ?
C1 N1 C5 109.6(2) . . ?
C2 N1 Ag2 103.59(18) . . ?
C1 N1 Ag2 105.78(18) . . ?
C5 N1 Ag2 116.80(19) . . ?
C26 N3 C23 110.2(2) . . ?
C26 N3 C24 109.7(2) . . ?
C23 N3 C24 110.3(2) . . ?
C26 N3 Ag1 117.30(19) . . ?
C23 N3 Ag1 105.63(17) . . ?
C24 N3 Ag1 103.39(17) . . ?
C12 O1 C13 115.6(3) . . ?
C33 O5 C34 109.1(7) . . ?
S1 O1A F3A 94.5(6) . 3_565 ?
S1 O1A S1 2.03(13) . 3_565 ?
F3A O1A S1 92.4(5) 3_565 3_565 ?
S1 O2A S1 26.5(3) . 3_565 ?
S1 O3A S1 26.5(4) 3_565 . ?
S1 S1 O3A 84.9(12) 3_565 3_565 ?
S1 S1 O2A 83.4(10) 3_565 . ?
O3A S1 O2A 132.6(6) 3_565 . ?
S1 S1 O1A 173.5(4) 3_565 . ?
O3A S1 O1A 97.3(11) 3_565 . ?
O2A S1 O1A 99.4(9) . . ?
S1 S1 O2A 70.1(10) 3_565 3_565 ?
O3A S1 O2A 16.5(15) 3_565 3_565 ?
O2A S1 O2A 121.1(12) . 3_565 ?
O1A S1 O2A 112.8(9) . 3_565 ?
S1 S1 O3A 68.6(11) 3_565 . ?
O3A S1 O3A 133.9(15) 3_565 . ?
O2A S1 O3A 16.5(14) . . ?
O1A S1 O3A 113.3(10) . . ?
O2A S1 O3A 118.9(11) 3_565 . ?
S1 S1 C2A 79.31(9) 3_565 . ?
O3A S1 C2A 107.8(9) 3_565 . ?
O2A S1 C2A 114.7(7) . . ?
O1A S1 C2A 94.2(4) . . ?
O2A S1 C2A 110.6(7) 3_565 . ?
O3A S1 C2A 103.5(8) . . ?
S1 S1 O1A 4.4(3) 3_565 3_565 ?
O3A S1 O1A 86.3(10) 3_565 3_565 ?
O2A S1 O1A 85.5(8) . 3_565 ?
O1A S1 O1A 169.1(7) . 3_565 ?
O2A S1 O1A 72.1(9) 3_565 3_565 ?
O3A S1 O1A 70.2(9) . 3_565 ?
C2A S1 O1A 74.9(3) . 3_565 ?
S1 S1 F3A 130.3(4) 3_565 3_565 ?
O3A S1 F3A 104.5(10) 3_565 3_565 ?
O2A S1 F3A 117.9(8) . 3_565 ?
O1A S1 F3A 43.2(5) . 3_565 ?
O2A S1 F3A 119.4(8) 3_565 3_565 ?
O3A S1 F3A 121.5(10) . 3_565 ?
C2A S1 F3A 51.2(4) . 3_565 ?
O1A S1 F3A 125.9(6) 3_565 3_565 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.784
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.107

#END

