Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002

data_global

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Schroder, Martin'
'Black, Daniel'
'Blake, A.'
'Finn, Rachel L.'
'Lindoy, Leonard F.'
'Nezhadali, Azizollah'
'Rougnaghi, Gholamhossein'
'Tasker, Peter A.'

_publ_contact_author_name     	'Prof Martin Schroder'  
_publ_contact_author_address 
;
School of Chemistry
The University of Nottingham
Nottingham
NG7 2RD
UNITED KINGDOM
;

_publ_contact_author_email       'M.SCHRODER@NOTTINGHAM.AC.UK'

_publ_section_title		
;
Compartmental Schiff-base Ligands as Selective Double-loaded
Extractants for Copper(II)
; 

data_POXICU

_database_code_CSD	173168


_refine_special_details 
; 
The quality of the refinemnt was limited by the weakness of the dataset.
Also, disorder was present in the tertiary butyl groups of the cation and
in the PF6- counteranions: in the latter this was modelled using distance 
and angle restraints.
; 

_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety         'C68 H88 Cu4 N12 O4 4+, 4(P F6 -)'
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum            'C68 H88 Cu4 F24 N12 O4 P4' 
_chemical_formula_weight          1971.54 
_chemical_melting_point           ? 
_chemical_compound_source         ? 

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' 
'Cu'  'Cu'   0.3201   1.2651 
'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' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'P'  'P'   0.1023   0.0942 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            Tetragonal 
_symmetry_space_group_name_H-M   'P 42/n m c'

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

_cell_length_a                    18.828(6) 
_cell_length_b                    18.828(6) 
_cell_length_c                    11.477(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      4069(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     20
_cell_measurement_theta_min       9 
_cell_measurement_theta_max       11 

_exptl_crystal_description        lath
_exptl_crystal_colour             green
_exptl_crystal_size_max           0.39 
_exptl_crystal_size_mid           0.16 
_exptl_crystal_size_min           0.16 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.609 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2008 
_exptl_absorpt_coefficient_mu     1.219 
_exptl_absorpt_correction_type    Psi-scan 
_exptl_absorpt_correction_T_min   0.609 
_exptl_absorpt_correction_T_max   0.670
_exptl_absorpt_process_details   'North et al., 1968)' 
_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Stoe Stadi-4 four-circle' 
_diffrn_measurement_method        \w/\q
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   60 
_diffrn_standards_decay_%        'random variation +/-1%' 
_diffrn_reflns_number             3510 
_diffrn_reflns_av_R_equivalents   0.173 
_diffrn_reflns_av_sigmaI/netI     0.186 
_diffrn_reflns_limit_h_min       -20 
_diffrn_reflns_limit_h_max        20 
_diffrn_reflns_limit_k_min       -20 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          2.80 
_diffrn_reflns_theta_max          22.52 
_reflns_number_total              1433 
_reflns_number_observed           651 
_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection        'Stoe DIF4' 
_computing_cell_refinement        'Stoe DIF4'
_computing_data_reduction         'Stoe REDU4' 
_computing_structure_solution     'SIR92 (Altomare et al., 1993)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'SHELXTL/PC version 5.10 (Bruker, 1997)' 
_computing_publication_material   'SHELXL-93; PLATON (Spek, 2001)'


_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.0998P)^2^+38.5323P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens   'geoemtrically or from delta-F' 
_refine_ls_hydrogen_treatment    'riding model or rigid rotating group' 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          1424 
_refine_ls_number_parameters      58 
_refine_ls_number_restraints      21 
_refine_ls_R_factor_all           0.219 
_refine_ls_R_factor_obs           0.102 
_refine_ls_wR_factor_all          0.281 
_refine_ls_wR_factor_obs          0.216 
_refine_ls_goodness_of_fit_all    1.03 
_refine_ls_goodness_of_fit_obs    1.21 
_refine_ls_restrained_S_all       1.05 
_refine_ls_restrained_S_obs       1.21 
_refine_ls_shift/esd_max          0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
Cu1 Cu 0.7500 0.16716(13) 0.8911(2) 0.0169(7) Uani 1 d S . 
O1 O 0.6846(6) 0.2500 0.8788(11) 0.019(3) Uiso 1 d S . 
C1 C 0.6164(9) 0.2500 0.9085(17) 0.013(4) Uiso 1 d S . 
C2 C 0.5796(7) 0.1874(7) 0.9234(11) 0.021(4) Uiso 1 d . . 
C3 C 0.5068(8) 0.1870(8) 0.9517(13) 0.032(4) Uiso 1 d . . 
H3 H 0.4836 0.1437 0.9600  0.038 Uiso 1 calc R . 
C4 C 0.4685(11) 0.2500 0.9677(19) 0.028(5) Uiso 1 d S . 
C20 C 0.6089(7) 0.1148(7) 0.9107(11) 0.022(3) Uiso 1 d . . 
H20 H 0.5768 0.0777 0.9211 0.026 Uiso 1 calc R . 
N21 N 0.6720(6) 0.0970(6) 0.8875(11) 0.025(3) Uiso 1 d . . 
C22 C 0.6829(7) 0.0200(7) 0.8794(14) 0.032(4) Uiso 1 d . . 
H22A H 0.6847 0.0064 0.7979 0.038 Uiso 1 calc R . 
H22B H 0.6428 -0.0041 0.9146 0.038 Uiso 1 calc R . 
C23 C 0.7500 -0.0038(11) 0.9385(19) 0.032(6) Uiso 1 d S . 
H23A H 0.7500 0.0141 1.0178 0.039 Uiso 1 calc SR . 
H23B H 0.7500 -0.0553 0.9425 0.039 Uiso 1 calc SR . 
C40 C 0.3877(8) 0.2500 0.9914(19) 0.046(7) Uiso 1 d S . 
C41 C 0.3616(8) 0.1739(12) 1.0024(19) 0.062(11) Uiso 0.50 d PR -1 
H41A H 0.3857 0.1510 1.0658 0.093 Uiso 0.50 calc PR -1 
H41B H 0.3712 0.1488 0.9313 0.093 Uiso 0.50 calc PR -1 
H41C H 0.3114 0.1739 1.0169 0.093 Uiso 0.50 calc PR -1 
C42 C 0.3496(8) 0.2863(12) 0.8910(19) 0.077(13) Uiso 0.50 d PR -1 
H42A H 0.3661 0.3343 0.8841  0.116 Uiso 0.50 calc PR -1 
H42B H 0.2994 0.2863 0.9056  0.116 Uiso 0.50 calc PR -1 
H42C H 0.3592 0.2611 0.8200  0.116 Uiso 0.50 calc PR -1 
C43 C 0.3725(8) 0.2898(13) 1.1039(19) 0.078(13) Uiso 0.50 d PR -1 
H43A H 0.3890 0.3379 1.0970 0.117 Uiso 0.50 calc PR -1 
H43B H 0.3966 0.2669 1.1673 0.117 Uiso 0.50 calc PR -1 
H43C H 0.3223 0.2898 1.1184 0.117 Uiso 0.50 calc PR -1 
N50 N 0.6658(10) 0.2500 1.4057(15) 0.034(4) Uiso 1 d S . 
C51 C 0.6312(12) 0.2500 1.3173(21) 0.037(6) Uiso 1 d S . 
C52 C 0.5911(6)  0.2500 1.2142(10) 0.037(6) Uiso 1 d S . 
H52A H 0.6094 0.2854 1.1621 0.055 Uiso 0.50 calc PR . 
H52B H 0.5424 0.2604 1.2322 0.055 Uiso 0.50 calc PR . 
H52C H 0.5942 0.2041 1.1780 0.055 Uiso 0.50 calc PR . 
P1 P 0.5374(5) 0.03113(13) 1.2262(8) 0.060(3) Uiso 0.50 d PRD -2 
F1 F 0.5788(5) 0.02265(14) 1.3397(8) 0.121(6) Uiso 0.342(12) d PRD -2 
F2 F 0.4720(5) -0.0054(3) 1.2821(8) 0.121(6) Uiso 0.50 d PRD -2 
F3 F 0.5095(5) 0.1053(3) 1.2681(8) 0.121(6) Uiso 0.342(12) d PRD -2 
F4 F 0.4946(5) 0.04204(14) 1.1098(8) 0.121(6) Uiso 0.342(12) d PRD -2 
F5 F 0.5638(5) -0.04067(3) 1.1814(8) 0.121(6) Uiso 0.342(12) d PRD -2 
F6 F 0.6028(5) 0.06773(8) 1.1702(8) 0.121(6) Uiso 0.50 d PRD -2 
F7 F 0.5874(5) -0.01748(7) 1.2979(8) 0.121(6) Uiso 0.158(12) d PRD -3 
F8 F 0.4874(5) 0.0798(2) 1.1544(8) 0.121(6) Uiso 0.158(12) d PRD -3 
F9 F 0.5381(5) 0.0866(3) 1.3260(8) 0.121(6) Uiso 0.158(12) d PRD -3 
F10 F 0.5367(5) -0.02431(4) 1.1264(8) 0.121(6) Uiso 0.158(12) d PRD -3 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Cu1 0.0138(14) 0.0153(14) 0.0215(12) -0.0001(14) 0.000 0.000 

_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 O1 1.992(7) . ? 
Cu1 N21 1.975(11) . ? 
Cu1 N50 2.33(2) 12_658 ? 
Cu1 N21 1.975(11) 14_755 ? 
Cu1 O1 1.992(7) 2_655 ?
O1 C1 1.33(2) . ? 
O1 Cu1 1.992(7) 2_655 ? 
C1 C2 1.38(2) . ? 
C1 C2 1.38(2) 13_565 ? 
C2 C3 1.41(2) . ? 
C2 C20 1.48(2) . ? 
C3 C4 1.40(2) . ? 
C4 C3 1.40(2) 13_565 ? 
C4 C40 1.54(2) . ? 
C20 N21 1.26(2) . ? 
N21 C22 1.47(2) . ? 
C22 C23 1.50(2) . ? 
C23 C22 1.50(2) 14_755 ? 
C40 C41 1.52 . ? 
C40 C41 1.52 13_565 ? 
C40 C42 1.52 13_565 ? 
C40 C42 1.52 . ? 
C40 C43 1.52 13_565 ? 
C40 C43 1.52 . ? 
N50 C51 1.21(3) . ?
N50 Cu1 2.33(2) 11_668 ? 
C51 C52 1.40(3) . ? 
P1 F1 1.53 . ? 
P1 F5 1.529(2) . ? 
P1 F2 1.550(2) . ? 
P1 F6 1.550(2) . ? 
P1 F3 1.568(2) . ? 
P1 F4 1.57 . ? 

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 
N21 Cu1 N21 96.0(7) 14_755 . ? 
N21 Cu1 O1 168.9(4) 14_755 . ? 
N21 Cu1 O1 93.6(4) . . ? 
N21 Cu1 O1 93.6(4) 14_755 2_655 ? 
N21 Cu1 O1 168.9(4) . 2_655 ? 
O1 Cu1 O1 76.3(5) . 2_655 ? 
N21 Cu1 N50 90.8(5) 14_755 12_658 ? 
N21 Cu1 N50 90.8(5) . 12_658 ?
O1 Cu1 N50 94.5(6) . 12_658 ? 
O1 Cu1 N50 94.5(6) 2_655 12_658 ? 
C1 O1 Cu1 125.4(4) . 2_655 ? 
C1 O1 Cu1 125.4(4) . . ? 
Cu1 O1 Cu1 103.1(5) 2_655 . ? 
O1 C1 C2 121.2(8) . . ? 
O1 C1 C2 121.2(8) . 13_565 ? 
C2 C1 C2 117.7(17) . 13_565 ? 
C1 C2 C3 121.4(14) . . ? 
C1 C2 C20 126.2(12) . . ? 
C3 C2 C20 112.4(13) . . ? 
C4 C3 C2 121.9(15) . . ? 
C3 C4 C3 115.7(20) . 13_565 ? 
C3 C4 C40 122.1(10) . . ? 
C3 C4 C40 122.1(10) 13_565 . ? 
N21 C20 C2 127.9(12) . . ? 
C20 N21 C22 114.0(11) . . ? 
C20 N21 Cu1 121.2(10) . . ? 
C22 N21 Cu1 123.9(9) . . ? 
N21 C22 C23 112.6(14) . . ? 
C22 C23 C22 114.4(18) 14_755 . ? 
C41 C40 C41 140.9 . 13_565 ? 
C41 C40 C42 59.1 . 13_565 ? 
C41 C40 C42 109.5 13_565 13_565 ? 
C41 C40 C42 109.5 . . ? 
C41 C40 C42 59.1 13_565 . ? 
C42 C40 C42 53.4 13_565 . ? 
C41 C40 C43 53.4 . 13_565 ? 
C41 C40 C43 109.5 13_565 13_565 ? 
C42 C40 C43 109.5 13_565 13_565 ? 
C42 C40 C43 140.9 . 13_565 ? 
C41 C40 C43 109.5 . . ? 
C41 C40 C43 53.4 13_565 . ? 
C42 C40 C43 140.9 13_565 . ? 
C42 C40 C43 109.5 . . ? 
C43 C40 C43 59.1 13_565 . ? 
C41 C40 C4 109.48(3) . . ? 
C41 C40 C4 109.48(3) 13_565 . ? 
C42 C40 C4 109.4(10) 13_565 . ? 
C42 C40 C4 109.4(10) . . ? 
C43 C40 C4 109.6(10) 13_565 . ? 
C43 C40 C4 109.6(10) . . ? 
C51 N50 Cu1 147.9(17) . 11_668 ? 
N50 C51 C52 179.9(17) . . ? 
F1 P1 F5 91.7 . . ? 
F1 P1 F2 90.3 . . ? 
F5 P1 F2 90.2 . . ? 
F1 P1 F6 89.7 . . ? 
F5 P1 F6 89.80(9) . . ? 
F2 P1 F6 180.0(13) . . ? 
F1 P1 F3 90.1 . . ? 
F5 P1 F3 178.16(7) . . ? 
F2 P1 F3 90.1 . . ? 
F6 P1 F3 89.9 . . ? 
F1 P1 F4 178.48(9) . . ? 
F5 P1 F4 89.8 . . ? 
F2 P1 F4 90.1 . . ? 
F6 P1 F4 89.9 . . ? 
F3 P1 F4 88.4 . . ? 

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 
O1 C1 C2 C3 -178.2(15) . . . . ? 
C2 C1 C2 C3 0.6(28) 13_565 . . . ? 
O1 C1 C2 C20 0.7(26) . . . . ? 
C2 C1 C2 C20 179.5(11) 13_565 . . . ? 
C1 C2 C3 C4 -0.9(26) . . . . ? 
C20 C2 C3 C4 -180.0(16) . . . . ? 
C2 C3 C4 C3 1.1(32) . . . 13_565 ? 
C2 C3 C4 C40 176.2(16) . . . . ? 
C1 C2 C20 N21 2.1(24) . . . . ? 
C3 C2 C20 N21 -178.9(14) . . . . ? 
C2 C20 N21 C22 -179.1(13) . . . . ? 
C20 N21 C22 C23 -137.2(14) . . . . ? 
N21 C22 C23 C22 -68.5(23) . . . 14_755 ? 
C3 C4 C40 C41 4.1(22) . . . . ? 
C3 C4 C40 C41 178.9(16) 13_565 . . . ? 
C3 C4 C40 C41 -178.9(16) . . . 13_565 ? 
C3 C4 C40 C41 -4.1(22) 13_565 . . 13_565 ? 
C3 C4 C40 C42 -59.0(21) . . . 13_565 ? 
C3 C4 C40 C42 115.8(17) 13_565 . . 13_565 ? 
C3 C4 C40 C42 -115.8(17) . . . . ? 
C3 C4 C40 C42 59.0(21) 13_565 . . . ? 
C3 C4 C40 C43 61.0(21) . . . 13_565 ? 
C3 C4 C40 C43 -124.2(17) 13_565 . . 13_565 ? 
C3 C4 C40 C43 124.2(17) . . . . ? 
C3 C4 C40 C43 -61.0(21) 13_565 . . . ? 

_refine_diff_density_max    0.99
_refine_diff_density_min   -0.96 
_refine_diff_density_rms    0.14 

data_BUPHNO

_database_code_CSD	173169


_refine_special_details 
; 
One PF6- anion is rotationally disordered about a general direction,
leading to two sets of six fluorine sites. The group occupancies of
these sets refined to 0.702(5) for the major component and 0.298(5)
for the minor component. Restraints were applied to P---F distances
(1.55 Angstroms) and to F---P---F angles (90 or 180 degrees).
; 


_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety         'C30 H42 N4 O2 2+, 2(P F6 -), C2 H3 N' 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum            'C32 H45 F12 N5 O2 P2' 
_chemical_formula_weight          821.67 
_chemical_melting_point           ? 
_chemical_compound_source         ? 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'P'  'P'   0.1023   0.0942 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'F'  'F'   0.0171   0.0103 
'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                    9.576(3) 
_cell_length_b                    10.916(3) 
_cell_length_c                    18.415(4) 
_cell_angle_alpha                 89.67(3) 
_cell_angle_beta                  86.13(3) 
_cell_angle_gamma                 78.81(2) 
_cell_volume                      1884.0(9) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     40 
_cell_measurement_theta_min       11
_cell_measurement_theta_max       15

_exptl_crystal_description        block 
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.49 
_exptl_crystal_size_mid           0.27 
_exptl_crystal_size_min           0.27 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.448 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              852 
_exptl_absorpt_coefficient_mu     0.212 
_exptl_absorpt_correction_type   'Psi-scan' 
_exptl_absorpt_correction_T_min   0.848 
_exptl_absorpt_correction_T_max   0.888 
_exptl_absorpt_PROCESS_details   '(North et al., 1968)' 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device       'Stoe Stadi-4 four-circle' 
_diffrn_measurement_method       '\w/\q' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   60 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             4940 
_diffrn_reflns_av_R_equivalents   ? 
_diffrn_reflns_av_sigmaI/netI     0.043 
_diffrn_reflns_limit_h_min       -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min       -11 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min         0 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          2.51 
_diffrn_reflns_theta_max          22.55 
_reflns_number_total              4940 
_reflns_number_observed           3482 
_reflns_observed_criterion        I>2\s(I) 

_computing_data_collection       'DIF4 (Stoe & Cie, 1992)' 
_computing_cell_refinement        DIF4 
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992)' 
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)' 
_computing_publication_material  'SHELXL-93; PLATON (Spek, 2001)' 

_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+( 0.096P)^2^+12.030P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4913 
_refine_ls_number_parameters      516 
_refine_ls_number_restraints      246 
_refine_ls_R_factor_all           0.122 
_refine_ls_R_factor_obs           0.0861 
_refine_ls_wR_factor_all          0.249 
_refine_ls_wR_factor_obs          0.206 
_refine_ls_goodness_of_fit_all    1.023 
_refine_ls_goodness_of_fit_obs    1.053 
_refine_ls_restrained_S_all       1.084 
_refine_ls_restrained_S_obs       1.108 
_refine_ls_shift/esd_max         -0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
N1 N 0.7929(6) 0.4065(5) -0.3812(3) 0.0309(13) Uani 1 d D . 
H1 H 0.8337(71) 0.4015(66) -0.3443(28) 0.037 Uiso 1 d D . 
N2 N 0.8114(7) 0.1273(5) -0.3841(3) 0.0381(15) Uani 1 d D . 
H2N H 0.8440(79) 0.1442(71) -0.3474(29) 0.046 Uiso 1 d D . 
N3 N 0.7490(7) 0.1204(5) -0.1023(3) 0.0369(15) Uani 1 d D . 
H3 H 0.7982(72) 0.1207(73) -0.1393(29) 0.044 Uiso 1 d D . 
N4 N 0.7675(6) 0.3911(5) -0.0994(3) 0.0290(13) Uani 1 d D . 
H4 H 0.8194(66) 0.3973(65) -0.1347(29) 0.035 Uiso 1 d D . 
O1 O 0.7883(5) 0.1303(4) -0.2423(2) 0.0391(12) Uani 1 d . . 
O2 O 0.7904(4) 0.4241(4) -0.2398(2) 0.0292(11) Uani 1 d . . 
C1 C 0.4062(7) 0.0026(6) -0.2546(4) 0.032(2) Uani 1 d . . 
C2 C 0.4556(7) 0.0286(6) -0.1885(4) 0.033(2) Uani 1 d . . 
H2 H 0.4005(7) 0.0172(6) -0.1450(4) 0.040 Uiso 1 calc R . 
C3 C 0.5842(7) 0.0713(5) -0.1833(4) 0.029(2) Uani 1 d . . 
C4 C 0.6690(8) 0.0926(6) -0.2461(4) 0.033(2) Uani 1 d . . 
C5 C 0.6173(7) 0.0669(6) -0.3140(4) 0.031(2) Uani 1 d . . 
C6 C 0.4903(7) 0.0219(6) -0.3164(4) 0.035(2) Uani 1 d . . 
H6 H 0.4602(7) 0.0036(6) -0.3626(4) 0.041 Uiso 1 calc R . 
C7 C 0.3484(7) 0.4585(6) -0.2358(3) 0.0267(15) Uani 1 d . . 
C8 C 0.4305(7) 0.4582(6) -0.3004(3) 0.0256(14) Uani 1 d . . 
H8 H 0.3840(7) 0.4674(6) -0.3446(3) 0.031 Uiso 1 calc R . 
C9 C 0.5789(7) 0.4450(6) -0.3037(3) 0.0248(14) Uani 1 d . . 
C10 C 0.6543(7) 0.4341(6) -0.2388(3) 0.0255(15) Uani 1 d . . 
C11 C 0.5690(6) 0.4341(5) -0.1719(3) 0.0243(14) Uani 1 d . . 
C12 C 0.4208(7) 0.4454(6) -0.1725(3) 0.0272(15) Uani 1 d . . 
H12 H 0.3671(7) 0.4440(6) -0.1272(3) 0.033 Uiso 1 calc R . 
C13 C 0.6284(8) 0.0883(6) -0.1124(4) 0.034(2) Uani 1 d . . 
H13 H 0.5676(8) 0.0757(6) -0.0712(4) 0.041 Uiso 1 calc R . 
C14 C 0.8064(9) 0.1278(7) -0.0308(4) 0.043(2) Uani 1 d . . 
H14A H 0.8579(9) 0.0439(7) -0.0176(4) 0.052 Uiso 1 calc R . 
H14B H 0.7262(9) 0.1536(7) 0.0062(4) 0.052 Uiso 1 calc R . 
C15 C 0.9066(8) 0.2191(6) -0.0296(4) 0.037(2) Uani 1 d . . 
H15A H 0.9770(8) 0.2007(6) -0.0720(4) 0.044 Uiso 1 calc R . 
H15B H 0.9599(8) 0.2039(6) 0.0148(4) 0.044 Uiso 1 calc R . 
C16 C 0.8382(7) 0.3568(6) -0.0314(4) 0.032(2) Uani 1 d . . 
H16A H 0.7670(7) 0.3765(6) 0.0105(4) 0.038 Uiso 1 calc R . 
H16B H 0.9123(7) 0.4074(6) -0.0263(4) 0.038 Uiso 1 calc R . 
C17 C 0.6324(7) 0.4118(6) -0.1051(3) 0.0265(15) Uani 1 d . . 
H17 H 0.5718(7) 0.4120(6) -0.0621(3) 0.032 Uiso 1 calc R . 
C18 C 0.6554(7) 0.4305(6) -0.3734(3) 0.030(2) Uani 1 d . . 
H18 H 0.6029(7) 0.4389(6) -0.4158(3) 0.036 Uiso 1 calc R . 
C19 C 0.8772(8) 0.3781(7) -0.4498(4) 0.042(2) Uani 1 d . . 
H19A H 0.9377(8) 0.4412(7) -0.4593(4) 0.051 Uiso 1 calc R . 
H19B H 0.8129(8) 0.3816(7) -0.4900(4) 0.051 Uiso 1 calc R . 
C20 C 0.9717(10) 0.2480(10) -0.4475(5) 0.072(3) Uani 1 d . . 
H20A H 1.0449(10) 0.2406(10) -0.4886(5) 0.086 Uiso 1 calc R . 
H20B H 1.0222(10) 0.2419(10) -0.4020(5) 0.086 Uiso 1 calc R . 
C21 C 0.9000(9) 0.1403(8) -0.4508(4) 0.050(2) Uani 1 d . . 
H21A H 0.8394(9) 0.1503(8) -0.4927(4) 0.061 Uiso 1 calc R . 
H21B H 0.9730(9) 0.0631(8) -0.4588(4) 0.061 Uiso 1 calc R . 
C22 C 0.6956(8) 0.0839(6) -0.3811(4) 0.039(2) Uani 1 d . . 
H22 H 0.6604(8) 0.0622(6) -0.4253(4) 0.047 Uiso 1 calc R . 
C23 C 0.2731(8) -0.0531(6) -0.2617(4) 0.040(2) Uani 1 d . . 
C24 C 0.1797(9) -0.0411(9) -0.1907(5) 0.064(2) Uani 1 d . . 
H24A H 0.0934(28) -0.0741(47) -0.1976(9) 0.077 Uiso 1 calc R . 
H24B H 0.1531(47) 0.0470(10) -0.1762(16) 0.077 Uiso 1 calc R . 
H24C H 0.2327(22) -0.0885(41) -0.1526(9) 0.077 Uiso 1 calc R . 
C25 C 0.1817(10) 0.0169(9) -0.3204(5) 0.066(3) Uani 1 d . . 
H25A H 0.0926(27) -0.0144(36) -0.3215(21) 0.079 Uiso 1 calc R . 
H25B H 0.2345(25) 0.0032(41) -0.3681(7) 0.079 Uiso 1 calc R . 
H25C H 0.1598(49) 0.1065(11) -0.3091(16) 0.079 Uiso 1 calc R . 
C26 C 0.3175(9) -0.1901(7) -0.2834(5) 0.060(2) Uani 1 d . . 
H26A H 0.2323(9) -0.2260(14) -0.2877(27) 0.072 Uiso 1 calc R . 
H26B H 0.3754(46) -0.2352(12) -0.2462(14) 0.072 Uiso 1 calc R . 
H26C H 0.3736(46) -0.1973(8) -0.3302(14) 0.072 Uiso 1 calc R . 
C27 C 0.1871(7) 0.4611(6) -0.2332(4) 0.030(2) Uani 1 d . . 
C28 C 0.1265(7) 0.4954(7) -0.3068(4) 0.039(2) Uani 1 d . . 
H28A H 0.0221(7) 0.5092(38) -0.3014(6) 0.047 Uiso 1 calc R . 
H28B H 0.1623(35) 0.4272(18) -0.3416(7) 0.047 Uiso 1 calc R . 
H28C H 0.1561(37) 0.5718(22) -0.3246(11) 0.047 Uiso 1 calc R . 
C29 C 0.1081(8) 0.5568(7) -0.1772(4) 0.046(2) Uani 1 d . . 
H29A H 0.0057(9) 0.5564(30) -0.1758(18) 0.056 Uiso 1 calc R . 
H29B H 0.1245(39) 0.6400(10) -0.1908(14) 0.056 Uiso 1 calc R . 
H29C H 0.1433(34) 0.5353(24) -0.1291(6) 0.056 Uiso 1 calc R . 
C30 C 0.1641(8) 0.3301(7) -0.2124(5) 0.053(2) Uani 1 d . . 
H30A H 0.0622(10) 0.3280(14) -0.2117(26) 0.063 Uiso 1 calc R . 
H30B H 0.1984(47) 0.3092(19) -0.1641(12) 0.063 Uiso 1 calc R . 
H30C H 0.2170(41) 0.2694(9) -0.2482(15) 0.063 Uiso 1 calc R . 
P1 P 0.3995(2) 0.2644(2) 0.49169(10) 0.0543(6) Uani 1 d DU . 
F1A F 0.2668(6) 0.3637(6) 0.5094(3) 0.0717(13) Uani 0.702(5) d PDU 1 
F1B F 0.4888(7) 0.3697(6) 0.4828(3) 0.0731(12) Uani 0.702(5) d PDU 1 
F1C F 0.5409(7) 0.1582(6) 0.4723(3) 0.0717(13) Uani 0.702(5) d PDU 1 
F1D F 0.3653(8) 0.2745(6) 0.4099(3) 0.0687(13) Uani 0.702(5) d PDU 1 
F1E F 0.4355(8) 0.2537(6) 0.5741(3) 0.0687(13) Uani 0.702(5) d PDU 1 
F1F F 0.3124(7) 0.1574(6) 0.4999(3) 0.0731(12) Uani 0.702(5) d PDU 1 
F1G F 0.3870(18) 0.4084(8) 0.5137(7) 0.069(2) Uani 0.298(5) d PDU 2 
F1H F 0.3728(18) 0.2294(15) 0.5729(5) 0.069(2) Uani 0.298(5) d PDU 2 
F1I F 0.4105(17) 0.1288(8) 0.4712(7) 0.069(2) Uani 0.298(5) d PDU 2 
F1J F 0.2321(9) 0.2924(15) 0.4873(8) 0.075(2) Uani 0.298(5) d PDU 2 
F1K F 0.4254(18) 0.2998(15) 0.4110(5) 0.069(2) Uani 0.298(5) d PDU 2 
F1L F 0.5613(9) 0.2380(14) 0.4960(7) 0.075(2) Uani 0.298(5) d PDU 2 
P2 P 0.3007(2) 0.2557(2) 0.03747(10) 0.0369(5) Uani 1 d D . 
F2A F 0.3889(5) 0.3510(5) 0.0020(3) 0.076(2) Uani 1 d D . 
F2B F 0.1583(5) 0.3522(4) 0.0246(3) 0.0643(14) Uani 1 d D . 
F2C F 0.4441(5) 0.1598(4) 0.0501(3) 0.0638(13) Uani 1 d D . 
F2D F 0.3095(6) 0.3175(5) 0.1134(2) 0.0664(14) Uani 1 d D . 
F2E F 0.2096(5) 0.1639(4) 0.0762(3) 0.0687(15) Uani 1 d D . 
F2F F 0.2901(7) 0.1934(6) -0.0374(3) 0.100(2) Uani 1 d D . 
N1S N 0.0558(8) 0.1768(7) 0.3688(4) 0.065(2) Uani 1 d . . 
C1S C 0.1299(9) 0.2090(7) 0.3255(4) 0.042(2) Uani 1 d . . 
C2S C 0.2258(9) 0.2472(7) 0.2703(4) 0.053(2) Uani 1 d . . 
H2S1 H 0.2017(33) 0.3380(9) 0.2645(19) 0.064 Uiso 1 calc R . 
H2S2 H 0.2170(37) 0.2063(35) 0.2240(7) 0.064 Uiso 1 calc R . 
H2S3 H 0.3241(10) 0.2233(40) 0.2846(13) 0.064 Uiso 1 calc R . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
N1 0.031(4) 0.034(3) 0.028(3) 0.007(3) -0.004(3) -0.007(3) 
N2 0.045(4) 0.030(3) 0.040(4) -0.005(3) -0.003(3) -0.007(3) 
N3 0.049(4) 0.032(3) 0.032(3) 0.001(3) -0.014(3) -0.011(3) 
N4 0.035(4) 0.028(3) 0.026(3) 0.003(2) -0.008(2) -0.009(3) 
O1 0.046(3) 0.039(3) 0.038(3) -0.002(2) -0.008(2) -0.020(2) 
O2 0.022(3) 0.037(3) 0.030(3) 0.002(2) -0.005(2) -0.009(2) 
C1 0.035(4) 0.029(4) 0.034(4) -0.001(3) -0.012(3) -0.006(3) 
C2 0.038(4) 0.024(3) 0.038(4) -0.001(3) -0.003(3) -0.007(3) 
C3 0.037(4) 0.017(3) 0.035(4) -0.001(3) -0.012(3) -0.004(3) 
C4 0.040(4) 0.018(3) 0.042(4) 0.003(3) -0.012(3) -0.002(3) 
C5 0.038(4) 0.020(3) 0.034(4) 0.003(3) -0.014(3) -0.002(3) 
C6 0.042(4) 0.026(4) 0.037(4) -0.002(3) -0.015(3) -0.007(3) 
C7 0.026(4) 0.025(3) 0.031(4) 0.002(3) -0.003(3) -0.008(3) 
C8 0.026(4) 0.029(3) 0.022(3) 0.002(3) -0.007(3) -0.003(3) 
C9 0.026(4) 0.024(3) 0.025(4) 0.005(3) -0.004(3) -0.006(3) 
C10 0.027(4) 0.023(3) 0.028(4) -0.001(3) -0.004(3) -0.009(3) 
C11 0.025(4) 0.023(3) 0.027(4) 0.003(3) -0.004(3) -0.008(3) 
C12 0.034(4) 0.026(3) 0.023(3) 0.002(3) 0.001(3) -0.011(3) 
C13 0.038(4) 0.026(4) 0.040(4) 0.002(3) -0.008(3) -0.010(3) 
C14 0.062(5) 0.039(4) 0.036(4) 0.010(3) -0.028(4) -0.020(4) 
C15 0.041(4) 0.037(4) 0.035(4) 0.003(3) -0.016(3) -0.008(3) 
C16 0.034(4) 0.034(4) 0.030(4) 0.001(3) -0.016(3) -0.010(3) 
C17 0.026(4) 0.028(4) 0.028(4) -0.001(3) -0.006(3) -0.008(3) 
C18 0.033(4) 0.030(4) 0.027(4) 0.004(3) -0.003(3) -0.005(3) 
C19 0.031(4) 0.060(5) 0.031(4) 0.016(3) 0.010(3) -0.004(4) 
C20 0.065(6) 0.102(8) 0.043(5) 0.003(5) 0.008(4) -0.004(6) 
C21 0.048(5) 0.052(5) 0.050(5) -0.015(4) 0.016(4) -0.013(4) 
C22 0.052(5) 0.026(4) 0.037(4) -0.002(3) -0.012(4) 0.000(4) 
C23 0.039(4) 0.032(4) 0.054(5) -0.004(3) -0.013(4) -0.014(3) 
C24 0.050(5) 0.075(6) 0.074(6) -0.008(5) -0.003(5) -0.026(5) 
C25 0.055(6) 0.075(6) 0.079(7) 0.009(5) -0.035(5) -0.030(5) 
C26 0.057(6) 0.045(5) 0.084(7) -0.012(4) -0.003(5) -0.024(4) 
C27 0.020(3) 0.034(4) 0.035(4) -0.001(3) -0.001(3) -0.005(3) 
C28 0.026(4) 0.048(4) 0.043(4) -0.007(3) -0.008(3) -0.003(3) 
C29 0.029(4) 0.060(5) 0.048(5) -0.007(4) -0.001(3) -0.003(4) 
C30 0.028(4) 0.045(5) 0.090(6) 0.019(4) -0.014(4) -0.014(4) 
P1 0.0722(14) 0.0517(12) 0.0455(12) 0.0076(10) -0.0221(10) -0.0221(11) 
F1A 0.079(3) 0.063(2) 0.065(3) -0.005(2) -0.009(2) 0.008(3) 
F1B 0.079(3) 0.065(2) 0.083(3) 0.010(2) -0.016(2) -0.027(2) 
F1C 0.079(3) 0.063(2) 0.065(3) -0.005(2) -0.009(2) 0.008(3) 
F1D 0.084(3) 0.074(3) 0.053(2) 0.003(2) -0.031(2) -0.019(3) 
F1E 0.084(3) 0.074(3) 0.053(2) 0.003(2) -0.031(2) -0.019(3) 
F1F 0.079(3) 0.065(2) 0.083(3) 0.010(2) -0.016(2) -0.027(2) 
F1G 0.089(4) 0.057(3) 0.064(3) -0.003(3) -0.015(4) -0.016(4) 
F1H 0.089(4) 0.065(3) 0.055(3) 0.014(4) -0.009(4) -0.017(4) 
F1I 0.089(4) 0.057(3) 0.064(3) -0.003(3) -0.015(4) -0.016(4) 
F1J 0.074(3) 0.077(3) 0.075(3) -0.003(4) -0.021(3) -0.014(3) 
F1K 0.089(4) 0.065(3) 0.055(3) 0.014(4) -0.009(4) -0.017(4) 
F1L 0.074(3) 0.077(3) 0.075(3) -0.003(4) -0.021(3) -0.014(3) 
P2 0.0406(11) 0.0339(10) 0.0361(11) 0.0025(8) -0.0065(8) -0.0061(9) 
F2A 0.057(3) 0.094(4) 0.078(4) 0.042(3) 0.008(3) -0.024(3) 
F2B 0.048(3) 0.036(2) 0.109(4) 0.010(2) -0.021(3) -0.002(2) 
F2C 0.049(3) 0.060(3) 0.078(3) 0.005(2) -0.018(2) 0.006(2) 
F2D 0.090(4) 0.074(3) 0.040(3) -0.007(2) -0.004(2) -0.028(3) 
F2E 0.067(3) 0.044(3) 0.102(4) 0.017(3) -0.012(3) -0.025(2) 
F2F 0.115(5) 0.106(5) 0.066(4) -0.050(3) -0.035(3) 0.025(4) 
N1S 0.062(5) 0.073(5) 0.068(5) 0.011(4) -0.007(4) -0.031(4) 
C1S 0.050(5) 0.036(4) 0.041(5) 0.000(4) -0.019(4) -0.004(4) 
C2S 0.066(6) 0.041(5) 0.043(5) 0.009(4) 0.001(4) 0.008(4) 

_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 C18 1.290(9) . ? 
N1 C19 1.455(9) . ? 
N2 C22 1.286(9) . ? 
N2 C21 1.466(9) . ? 
N3 C13 1.296(9) . ? 
N3 C14 1.468(9) . ? 
N4 C17 1.281(8) . ? 
N4 C16 1.475(8) . ? 
O1 C4 1.293(8) . ? 
O2 C10 1.286(7) . ? 
C1 C2 1.386(9) . ? 
C1 C6 1.388(10) . ? 
C1 C23 1.529(9) . ? 
C2 C3 1.408(9) . ? 
C3 C4 1.412(10) . ? 
C3 C13 1.424(9) . ? 
C4 C5 1.425(9) . ? 
C5 C6 1.400(9) . ? 
C5 C22 1.432(10) . ? 
C7 C8 1.381(9) . ? 
C7 C12 1.389(9) . ? 
C7 C27 1.537(9) . ? 
C8 C9 1.397(9) . ? 
C9 C18 1.429(9) . ? 
C9 C10 1.430(9) . ? 
C10 C11 1.430(9) . ? 
C11 C12 1.402(9) . ? 
C11 C17 1.408(9) . ? 
C14 C15 1.513(10) . ? 
C15 C16 1.520(9) . ? 
C19 C20 1.531(12) . ? 
C20 C21 1.475(12) . ? 
C23 C26 1.521(10) . ? 
C23 C24 1.525(11) . ? 
C23 C25 1.543(11) . ? 
C27 C29 1.525(10) . ? 
C27 C28 1.527(9) . ? 
C27 C30 1.531(10) . ? 
P1 F1A 1.520(6) . ? 
P1 F1B 1.562(5) . ? 
P1 F1C 1.623(6) . ? 
P1 F1D 1.561(5) . ? 
P1 F1E 1.578(5) . ? 
P1 F1F 1.562(6) . ? 
P1 F1G 1.606(8) . ? 
P1 F1H 1.558(8) . ? 
P1 F1I 1.511(8) . ? 
P1 F1J 1.580(8) . ? 
P1 F1L 1.528(8) . ? 
P1 F1K 1.550(8) . ? 
P2 F2A 1.576(5) . ? 
P2 F2B 1.584(4) . ? 
P2 F2C 1.586(4) . ? 
P2 F2D 1.570(4) . ? 
P2 F2E 1.588(4) . ? 
P2 F2F 1.558(5) . ? 
N1S C1S 1.131(10) . ? 
C1S C2S 1.439(12) . ? 

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 
C18 N1 C19 125.4(6) . . ? 
C22 N2 C21 125.2(6) . . ? 
C13 N3 C14 124.4(6) . . ? 
C17 N4 C16 124.9(6) . . ? 
C2 C1 C6 116.3(6) . . ? 
C2 C1 C23 123.6(6) . . ? 
C6 C1 C23 119.9(6) . . ? 
C1 C2 C3 122.5(6) . . ? 
C2 C3 C4 121.3(6) . . ? 
C2 C3 C13 117.6(6) . . ? 
C4 C3 C13 121.0(6) . . ? 
O1 C4 C3 122.1(6) . . ? 
O1 C4 C5 121.8(6) . . ? 
C3 C4 C5 116.0(6) . . ? 
C6 C5 C4 120.6(6) . . ? 
C6 C5 C22 118.7(6) . . ? 
C4 C5 C22 120.7(6) . . ? 
C1 C6 C5 123.2(6) . . ? 
C8 C7 C12 116.5(6) . . ? 
C8 C7 C27 122.5(6) . . ? 
C12 C7 C27 120.7(6) . . ? 
C7 C8 C9 123.0(6) . . ? 
C8 C9 C18 118.5(6) . . ? 
C8 C9 C10 121.0(6) . . ? 
C18 C9 C10 120.3(6) . . ? 
O2 C10 C9 122.5(6) . . ? 
O2 C10 C11 121.6(5) . . ? 
C9 C10 C11 115.9(6) . . ? 
C12 C11 C17 118.4(6) . . ? 
C12 C11 C10 120.3(5) . . ? 
C17 C11 C10 121.0(6) . . ? 
C7 C12 C11 123.3(6) . . ? 
N3 C13 C3 122.0(7) . . ? 
N3 C14 C15 112.5(6) . . ? 
C14 C15 C16 116.3(6) . . ? 
N4 C16 C15 112.2(5) . . ? 
N4 C17 C11 123.4(6) . . ? 
N1 C18 C9 122.6(6) . . ? 
N1 C19 C20 110.3(6) . . ? 
C21 C20 C19 117.0(8) . . ? 
N2 C21 C20 112.4(6) . . ? 
N2 C22 C5 122.9(6) . . ? 
C26 C23 C24 109.6(7) . . ? 
C26 C23 C1 109.4(6) . . ? 
C24 C23 C1 111.5(6) . . ? 
C26 C23 C25 109.1(7) . . ? 
C24 C23 C25 107.2(7) . . ? 
C1 C23 C25 110.1(6) . . ? 
C29 C27 C28 107.9(6) . . ? 
C29 C27 C30 110.3(6) . . ? 
C28 C27 C30 109.0(6) . . ? 
C29 C27 C7 110.5(5) . . ? 
C28 C27 C7 111.7(5) . . ? 
C30 C27 C7 107.4(5) . . ? 
F1I P1 F1L 88.3(8) . . ? 
F1I P1 F1K 91.3(8) . . ? 
F1L P1 F1K 87.5(8) . . ? 
F1I P1 F1H 88.9(8) . . ? 
F1L P1 F1H 92.8(8) . . ? 
F1K P1 F1H 179.7(2) . . ? 
F1A P1 F1D 88.5(3) . . ? 
F1A P1 F1F 91.9(3) . . ? 
F1D P1 F1F 88.5(3) . . ? 
F1A P1 F1B 89.1(3) . . ? 
F1D P1 F1B 91.3(3) . . ? 
F1F P1 F1B 179.0(2) . . ? 
F1A P1 F1E 91.9(3) . . ? 
F1D P1 F1E 179.5(2) . . ? 
F1F P1 F1E 91.7(3) . . ? 
F1B P1 F1E 88.5(3) . . ? 
F1I P1 F1J 92.0(8) . . ? 
F1L P1 F1J 179.7(2) . . ? 
F1K P1 F1J 92.5(8) . . ? 
F1H P1 F1J 87.2(8) . . ? 
F1I P1 F1G 179.6(2) . . ? 
F1L P1 F1G 92.0(8) . . ? 
F1K P1 F1G 88.9(8) . . ? 
F1H P1 F1G 90.9(8) . . ? 
F1J P1 F1G 87.7(8) . . ? 
F1A P1 F1C 179.68(15) . . ? 
F1D P1 F1C 91.2(3) . . ? 
F1F P1 F1C 88.0(3) . . ? 
F1B P1 F1C 91.0(3) . . ? 
F1E P1 F1C 88.4(3) . . ? 
F2F P2 F2D 179.2(4) . . ? 
F2F P2 F2A 92.4(4) . . ? 
F2D P2 F2A 88.4(3) . . ? 
F2F P2 F2B 89.3(3) . . ? 
F2D P2 F2B 90.4(3) . . ? 
F2A P2 F2B 89.1(3) . . ? 
F2F P2 F2C 90.7(3) . . ? 
F2D P2 F2C 89.6(3) . . ? 
F2A P2 F2C 90.4(3) . . ? 
F2B P2 F2C 179.5(3) . . ? 
F2F P2 F2E 89.9(4) . . ? 
F2D P2 F2E 89.3(3) . . ? 
F2A P2 F2E 177.4(3) . . ? 
F2B P2 F2E 89.9(3) . . ? 
F2C P2 F2E 90.6(3) . . ? 
N1S C1S C2S 178.8(8) . . ? 

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 
C6 C1 C2 C3 -0.5(9) . . . . ? 
C23 C1 C2 C3 175.2(6) . . . . ? 
C1 C2 C3 C4 1.3(10) . . . . ? 
C1 C2 C3 C13 -176.5(6) . . . . ? 
C2 C3 C4 O1 -179.1(6) . . . . ? 
C13 C3 C4 O1 -1.3(9) . . . . ? 
C2 C3 C4 C5 -0.7(9) . . . . ? 
C13 C3 C4 C5 177.1(6) . . . . ? 
O1 C4 C5 C6 177.7(6) . . . . ? 
C3 C4 C5 C6 -0.7(9) . . . . ? 
O1 C4 C5 C22 -0.9(9) . . . . ? 
C3 C4 C5 C22 -179.4(6) . . . . ? 
C2 C1 C6 C5 -1.0(10) . . . . ? 
C23 C1 C6 C5 -176.9(6) . . . . ? 
C4 C5 C6 C1 1.6(10) . . . . ? 
C22 C5 C6 C1 -179.7(6) . . . . ? 
C12 C7 C8 C9 0.3(9) . . . . ? 
C27 C7 C8 C9 -174.3(6) . . . . ? 
C7 C8 C9 C18 172.4(6) . . . . ? 
C7 C8 C9 C10 -1.7(9) . . . . ? 
C8 C9 C10 O2 -178.7(6) . . . . ? 
C18 C9 C10 O2 7.3(9) . . . . ? 
C8 C9 C10 C11 1.8(8) . . . . ? 
C18 C9 C10 C11 -172.3(5) . . . . ? 
O2 C10 C11 C12 179.9(5) . . . . ? 
C9 C10 C11 C12 -0.6(8) . . . . ? 
O2 C10 C11 C17 -5.8(9) . . . . ? 
C9 C10 C11 C17 173.8(5) . . . . ? 
C8 C7 C12 C11 1.0(9) . . . . ? 
C27 C7 C12 C11 175.6(6) . . . . ? 
C17 C11 C12 C7 -175.3(6) . . . . ? 
C10 C11 C12 C7 -0.8(9) . . . . ? 
C14 N3 C13 C3 -174.0(6) . . . . ? 
C2 C3 C13 N3 176.0(6) . . . . ? 
C4 C3 C13 N3 -1.9(10) . . . . ? 
C13 N3 C14 C15 -153.9(7) . . . . ? 
N3 C14 C15 C16 72.4(8) . . . . ? 
C17 N4 C16 C15 104.5(7) . . . . ? 
C14 C15 C16 N4 -63.5(8) . . . . ? 
C16 N4 C17 C11 -174.5(6) . . . . ? 
C12 C11 C17 N4 174.9(6) . . . . ? 
C10 C11 C17 N4 0.4(9) . . . . ? 
C19 N1 C18 C9 173.3(6) . . . . ? 
C8 C9 C18 N1 -173.6(6) . . . . ? 
C10 C9 C18 N1 0.6(9) . . . . ? 
C18 N1 C19 C20 -119.6(8) . . . . ? 
N1 C19 C20 C21 72.8(9) . . . . ? 
C22 N2 C21 C20 148.0(8) . . . . ? 
C19 C20 C21 N2 -70.1(10) . . . . ? 
C21 N2 C22 C5 176.5(6) . . . . ? 
C6 C5 C22 N2 178.4(6) . . . . ? 
C4 C5 C22 N2 -2.9(10) . . . . ? 
C2 C1 C23 C26 -104.9(8) . . . . ? 
C6 C1 C23 C26 70.7(8) . . . . ? 
C2 C1 C23 C24 16.5(10) . . . . ? 
C6 C1 C23 C24 -167.9(7) . . . . ? 
C2 C1 C23 C25 135.3(7) . . . . ? 
C6 C1 C23 C25 -49.2(9) . . . . ? 
C8 C7 C27 C29 -134.2(7) . . . . ? 
C12 C7 C27 C29 51.5(8) . . . . ? 
C8 C7 C27 C28 -14.1(9) . . . . ? 
C12 C7 C27 C28 171.6(6) . . . . ? 
C8 C7 C27 C30 105.4(7) . . . . ? 
C12 C7 C27 C30 -68.9(8) . . . . ? 

_refine_diff_density_max    1.17 
_refine_diff_density_min   -1.06 
_refine_diff_density_rms    0.09