# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012



data_global

#TrackingRef '- C2CE25366F_ccdc_871445_cif.txt'



_journal_name_full               CrystEngComm

_journal_coden_cambridge         1350

loop_

_publ_author_name

_publ_author_address

'Giovanna Bruni' 'Centro Grandi Strumenti, University of Pavia, Italy'

'Mariarosa Maietta' ?

'Lauretta Maggi' ?

'Marcella Bini' ''

'Doretta Capsoni' ''

'Stefania Ferrari' ''

;

M.Boiocchi

;

''

'Vittorio Berbenni' ''

'Chiara Milanese' ''

'Amedeo Marini' ''

#TrackingRef '- PFA21-mod.txt'



_publ_contact_author             

;

Giovanna Bruni

Dipartimento di Chimica Generale

University of Pavia

via Taramelli 12, I-27100 Pavia, ITALY

;



_publ_contact_author_email       giovanna.bruni@unipv.it



_publ_section_title              

;

?

;

_publ_contact_author_name        'Giovanna Bruni'





# Attachment '- PFA21-mod.txt'



data_per2fum1

_database_code_depnum_ccdc_archive 'CCDC 871445'

#TrackingRef '- PFA21-mod.txt'



_audit_creation_method           SHELXL-97

_chemical_name_systematic        

;

?

;

_chemical_name_common            'Perphenazine fumarate'

_chemical_melting_point          ?

_chemical_formula_moiety         'C21 H27 Cl N3 O S, 0.5(C4 H2 O4)'

_chemical_formula_sum            'C23 H28 Cl N3 O3 S'

_chemical_formula_weight         462.00



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source

C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

Cl Cl 0.1484 0.1585 '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'

S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           monoclinic

_symmetry_space_group_name_H-M   'P 21/a'

_symmetry_space_group_name_Hall  '-P 2yab'

_symmetry_Int_Tables_number      14



loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'

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

'-x, -y, -z'

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



_cell_length_a                   8.964(7)

_cell_length_b                   30.082(5)

_cell_length_c                   9.428(6)

_cell_angle_alpha                90.00

_cell_angle_beta                 115.94(5)

_cell_angle_gamma                90.00

_cell_volume                     2286(2)

_cell_formula_units_Z            4

_cell_measurement_temperature    293(2)

_cell_measurement_reflns_used    25

_cell_measurement_theta_min      7

_cell_measurement_theta_max      15



_exptl_crystal_description       PRISM

_exptl_crystal_colour            COLOURLESS

_exptl_crystal_size_max          0.65

_exptl_crystal_size_mid          0.45

_exptl_crystal_size_min          0.35

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.342

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             976

_exptl_absorpt_coefficient_mu    0.288

_exptl_absorpt_correction_type   psi-scan

_exptl_absorpt_correction_T_min  0.776

_exptl_absorpt_correction_T_max  0.995

_exptl_absorpt_process_details   

;

North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351

;



_exptl_special_details           

;

?

;



_diffrn_ambient_temperature      293(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Enraf-Nonius CAD4'

_diffrn_measurement_method       'omega scans'

_diffrn_standards_number         3

_diffrn_standards_interval_time  300

_diffrn_standards_decay_%        0

_diffrn_reflns_number            4239

_diffrn_reflns_av_R_equivalents  0.0000

_diffrn_reflns_av_sigmaI/netI    0.0357

_diffrn_reflns_limit_h_min       -10

_diffrn_reflns_limit_h_max       9

_diffrn_reflns_limit_k_min       0

_diffrn_reflns_limit_k_max       36

_diffrn_reflns_limit_l_min       0

_diffrn_reflns_limit_l_max       11

_diffrn_reflns_theta_min         1.35

_diffrn_reflns_theta_max         25.51

_reflns_number_total             4239

_reflns_number_gt                2843

_reflns_threshold_expression     >2\s(I)



_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'

_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'

_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'

_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'

_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'



_refine_special_details          

;

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and

goodness of fit S are based on F^2^, conventional R-factors R are based

on F, with F set to zero for negative F^2^. The threshold expression of

F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F^2^ are statistically about twice as large as those based on F, and R-

factors based on ALL data will be even larger.

Chlorine atom is disordered over two alternative positions.

;



_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     

'calc w=1/[\s^2^(Fo^2^)+(0.1469P)^2^+2.1033P] 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    mixed

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         4239

_refine_ls_number_parameters     296

_refine_ls_number_restraints     10

_refine_ls_R_factor_all          0.1151

_refine_ls_R_factor_gt           0.0844

_refine_ls_wR_factor_ref         0.2664

_refine_ls_wR_factor_gt          0.2414

_refine_ls_goodness_of_fit_ref   1.084

_refine_ls_restrained_S_all      1.104

_refine_ls_shift/su_max          0.006

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group

C1 C 0.7371(7) 0.33843(19) 0.7408(7) 0.0651(14) Uani 1 1 d . A 1

H1 H 0.8232 0.3362 0.8419 0.078 Uiso 0.133(5) 1 d PR B 1

C2 C 0.6493(8) 0.37774(18) 0.6938(8) 0.0717(16) Uani 1 1 d . A 1

H2 H 0.6782 0.4020 0.7618 0.086 Uiso 1 1 calc R A 1

C3 C 0.5174(8) 0.38081(17) 0.5443(8) 0.0709(17) Uani 1 1 d . A 1

H3 H 0.4582 0.4073 0.5129 0.085 Uiso 1 1 calc R A 1

C4 C 0.4749(7) 0.34642(16) 0.4454(7) 0.0618(13) Uani 1 1 d U A 1

C5 C 0.5702(6) 0.30530(15) 0.4909(6) 0.0509(11) Uani 1 1 d U A 1

C6 C 0.6985(6) 0.30227(15) 0.6389(6) 0.0516(12) Uani 1 1 d . A 1

H6 H 0.7596 0.2761 0.6712 0.062 Uiso 1 1 calc R A 1

C7 C 0.4095(6) 0.32281(17) 0.1550(7) 0.0617(14) Uani 1 1 d . A 1

C8 C 0.3887(7) 0.3375(2) 0.0091(7) 0.0743(18) Uani 1 1 d . A 1

H8 H 0.3233 0.3623 -0.0359 0.089 Uiso 1 1 calc R A 1

C9 C 0.4643(8) 0.3155(3) -0.0710(8) 0.085(2) Uani 1 1 d . A 1

H9 H 0.4490 0.3250 -0.1703 0.102 Uiso 1 1 calc R A 1

C10 C 0.5591(7) 0.2806(2) -0.0026(7) 0.0746(16) Uani 1 1 d D A 1

H10 H 0.6094 0.2658 -0.0567 0.089 Uiso 0.867(5) 1 calc PR B 1

C11 C 0.5874(6) 0.26501(18) 0.1474(6) 0.0572(12) Uani 1 1 d . A 1

H11 H 0.6580 0.2411 0.1928 0.069 Uiso 1 1 calc R A 1

C12 C 0.5096(5) 0.28553(15) 0.2250(6) 0.0500(11) Uani 1 1 d . A 1

C13 C 0.5898(5) 0.22631(14) 0.4291(6) 0.0471(10) Uani 1 1 d . A 1

H13A H 0.7095 0.2267 0.4899 0.057 Uiso 1 1 calc R A 1

H13B H 0.5637 0.2078 0.3370 0.057 Uiso 1 1 calc R A 1

C14 C 0.5117(6) 0.20616(14) 0.5290(6) 0.0510(11) Uani 1 1 d . A 1

H14A H 0.5485 0.2226 0.6270 0.061 Uiso 1 1 calc R A 1

H14B H 0.3920 0.2089 0.4732 0.061 Uiso 1 1 calc R A 1

C15 C 0.5572(6) 0.15740(14) 0.5660(6) 0.0491(11) Uani 1 1 d . A 1

H15A H 0.6763 0.1551 0.6282 0.059 Uiso 1 1 calc R A 1

H15B H 0.5049 0.1463 0.6299 0.059 Uiso 1 1 calc R A 1

C16 C 0.3274(5) 0.12576(14) 0.3364(6) 0.0463(10) Uani 1 1 d . A 1

H16A H 0.2809 0.1553 0.3053 0.056 Uiso 1 1 calc R A 1

H16B H 0.2804 0.1129 0.4021 0.056 Uiso 1 1 calc R A 1

C17 C 0.2822(5) 0.09762(14) 0.1923(5) 0.0463(10) Uani 1 1 d . A 1

H17A H 0.1623 0.0954 0.1361 0.056 Uiso 1 1 calc R A 1

H17B H 0.3219 0.1118 0.1229 0.056 Uiso 1 1 calc R A 1

C18 C 0.5383(4) 0.05507(13) 0.3338(5) 0.0380(9) Uani 1 1 d . A 1

H18A H 0.5833 0.0256 0.3687 0.046 Uiso 1 1 calc R A 1

H18B H 0.5917 0.0674 0.2726 0.046 Uiso 1 1 calc R A 1

C19 C 0.5735(5) 0.08405(13) 0.4746(5) 0.0398(9) Uani 1 1 d . A 1

H19A H 0.5234 0.0710 0.5374 0.048 Uiso 1 1 calc R A 1

H19B H 0.6924 0.0855 0.5394 0.048 Uiso 1 1 calc R A 1

C20 C 0.3146(6) 0.02522(15) 0.0860(5) 0.0466(10) Uani 1 1 d . A 1

H20A H 0.1972 0.0282 0.0166 0.056 Uiso 1 1 calc R A 1

H20B H 0.3755 0.0374 0.0316 0.056 Uiso 1 1 calc R A 1

C21 C 0.3554(7) -0.02324(17) 0.1164(6) 0.0609(13) Uani 1 1 d . A 1

H21A H 0.4709 -0.0265 0.1913 0.073 Uiso 1 1 calc R A 1

H21B H 0.2878 -0.0363 0.1625 0.073 Uiso 1 1 calc R A 1

C22 C 0.0715(5) 0.01814(14) 0.3407(5) 0.0409(9) Uani 1 1 d . C 1

C23 C -0.0296(5) 0.00435(13) 0.4243(5) 0.0415(9) Uani 1 1 d . . 1

H23 H -0.1436 0.0017 0.3641 0.050 Uiso 1 1 calc R . 1

N1 N 0.5304(5) 0.27181(12) 0.3780(5) 0.0488(9) Uani 1 1 d . A 1

N2 N 0.5085(4) 0.12907(11) 0.4272(4) 0.0381(8) Uani 1 1 d . A 1

N3 N 0.3546(4) 0.05196(10) 0.2328(4) 0.0342(7) Uani 1 1 d D A 1

H3N H 0.306(5) 0.0383(13) 0.295(4) 0.041 Uiso 1 1 d D D 1

O1 O 0.3270(4) -0.04577(14) -0.0231(4) 0.0723(11) Uani 1 1 d D A 1

H1O H 0.211(2) -0.045(2) -0.094(5) 0.087 Uiso 1 1 d D E 1

O2 O -0.0024(4) 0.03181(15) 0.2033(4) 0.0678(11) Uani 1 1 d . C 1

O3 O 0.2283(4) 0.01632(11) 0.4161(4) 0.0544(9) Uani 1 1 d . C 1

S1 S 0.31084(17) 0.34949(5) 0.2564(2) 0.0699(5) Uani 1 1 d . A 1

Cl1A Cl 0.9060(2) 0.33507(7) 0.9216(2) 0.0809(7) Uani 0.867(5) 1 d P A 1

Cl1B Cl 0.617(2) 0.2501(5) -0.1078(18) 0.124(7) Uani 0.133(5) 1 d PDU B 2



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

C1 0.072(3) 0.070(3) 0.072(3) -0.017(3) 0.048(3) -0.018(3)

C2 0.089(4) 0.050(3) 0.104(5) -0.021(3) 0.069(4) -0.010(3)

C3 0.083(4) 0.041(3) 0.119(5) 0.000(3) 0.071(4) 0.002(3)

C4 0.073(3) 0.043(2) 0.090(4) -0.006(2) 0.055(3) -0.018(2)

C5 0.053(3) 0.043(2) 0.072(3) -0.009(2) 0.041(2) -0.0111(18)

C6 0.058(3) 0.045(2) 0.073(3) -0.013(2) 0.048(3) -0.009(2)

C7 0.040(2) 0.056(3) 0.089(4) 0.014(3) 0.029(2) -0.005(2)

C8 0.048(3) 0.074(4) 0.083(4) 0.034(3) 0.013(3) -0.008(3)

C9 0.074(4) 0.108(5) 0.069(4) 0.024(4) 0.026(3) -0.015(4)

C10 0.072(4) 0.080(4) 0.068(4) 0.006(3) 0.028(3) -0.017(3)

C11 0.052(3) 0.057(3) 0.058(3) -0.001(2) 0.021(2) -0.010(2)

C12 0.038(2) 0.047(2) 0.063(3) 0.007(2) 0.019(2) -0.0107(19)

C13 0.046(2) 0.036(2) 0.066(3) 0.001(2) 0.031(2) 0.0020(18)

C14 0.061(3) 0.037(2) 0.069(3) -0.004(2) 0.041(2) -0.001(2)

C15 0.054(3) 0.041(2) 0.056(3) 0.000(2) 0.027(2) -0.002(2)

C16 0.041(2) 0.037(2) 0.064(3) 0.007(2) 0.027(2) 0.0098(18)

C17 0.039(2) 0.043(2) 0.052(2) 0.013(2) 0.0148(19) 0.0094(18)

C18 0.0283(18) 0.039(2) 0.049(2) 0.0054(18) 0.0189(17) 0.0048(16)

C19 0.0317(19) 0.037(2) 0.046(2) 0.0042(17) 0.0125(17) 0.0020(16)

C20 0.049(2) 0.055(3) 0.039(2) -0.0002(19) 0.0222(19) -0.001(2)

C21 0.064(3) 0.055(3) 0.056(3) -0.010(2) 0.020(2) 0.003(2)

C22 0.035(2) 0.039(2) 0.055(3) 0.0018(19) 0.0254(19) 0.0036(17)

C23 0.032(2) 0.040(2) 0.057(2) 0.0025(19) 0.0241(19) -0.0003(16)

N1 0.048(2) 0.0359(19) 0.069(2) -0.0004(17) 0.0324(19) 0.0015(16)

N2 0.0348(16) 0.0334(17) 0.0476(19) 0.0043(15) 0.0194(15) 0.0002(13)

N3 0.0306(15) 0.0365(17) 0.0388(17) 0.0059(14) 0.0182(14) 0.0020(13)

O1 0.056(2) 0.086(3) 0.071(2) -0.033(2) 0.0238(18) 0.000(2)

O2 0.0429(17) 0.109(3) 0.054(2) 0.013(2) 0.0227(16) -0.0081(18)

O3 0.0377(15) 0.070(2) 0.065(2) 0.0272(17) 0.0311(15) 0.0094(15)

S1 0.0544(7) 0.0572(8) 0.1071(12) 0.0199(8) 0.0435(8) 0.0106(6)

Cl1A 0.0754(11) 0.0957(14) 0.0663(11) -0.0257(9) 0.0262(9) -0.0096(9)

Cl1B 0.133(10) 0.150(11) 0.097(9) 0.026(7) 0.057(7) -0.013(8)



_geom_special_details            

;

All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)

are estimated using the full covariance matrix. The cell s.u.'s are taken

into account individually in the estimation of s.u.'s in distances, angles

and torsion angles; correlations between s.u.'s in cell parameters are only

used when they are defined by crystal symmetry. An approximate (isotropic)

treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag

C1 C2 1.382(8) . ?

C1 C6 1.391(7) . ?

C1 Cl1A 1.717(6) . ?

C2 C3 1.391(9) . ?

C2 H2 0.9300 . ?

C3 C4 1.332(7) . ?

C3 H3 0.9300 . ?

C4 C5 1.457(7) . ?

C4 S1 1.747(6) . ?

C5 C6 1.369(7) . ?

C5 N1 1.394(6) . ?

C6 H6 0.9300 . ?

C7 C8 1.377(8) . ?

C7 C12 1.407(7) . ?

C7 S1 1.755(6) . ?

C8 C9 1.383(10) . ?

C8 H8 0.9300 . ?

C9 C10 1.327(9) . ?

C9 H9 0.9300 . ?

C10 C11 1.404(8) . ?

C10 H10 0.9300 . ?

C11 C12 1.360(7) . ?

C11 H11 0.9300 . ?

C12 N1 1.432(6) . ?

C13 N1 1.472(5) . ?

C13 C14 1.523(6) . ?

C13 H13A 0.9700 . ?

C13 H13B 0.9700 . ?

C14 C15 1.521(6) . ?

C14 H14A 0.9700 . ?

C14 H14B 0.9700 . ?

C15 N2 1.459(6) . ?

C15 H15A 0.9700 . ?

C15 H15B 0.9700 . ?

C16 N2 1.470(5) . ?

C16 C17 1.498(6) . ?

C16 H16A 0.9700 . ?

C16 H16B 0.9700 . ?

C17 N3 1.495(5) . ?

C17 H17A 0.9700 . ?

C17 H17B 0.9700 . ?

C18 C19 1.501(6) . ?

C18 N3 1.502(5) . ?

C18 H18A 0.9700 . ?

C18 H18B 0.9700 . ?

C19 N2 1.465(5) . ?

C19 H19A 0.9700 . ?

C19 H19B 0.9700 . ?

C20 C21 1.500(7) . ?

C20 N3 1.502(5) . ?

C20 H20A 0.9700 . ?

C20 H20B 0.9700 . ?

C21 O1 1.400(6) . ?

C21 H21A 0.9700 . ?

C21 H21B 0.9700 . ?

C22 O2 1.240(5) . ?

C22 O3 1.269(5) . ?

C22 C23 1.496(6) . ?

C23 C23 1.313(8) 3_556 ?

C23 H23 0.9300 . ?

N3 H3N 0.958(10) . ?

O1 H1O 0.958(10) . ?



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

C2 C1 C6 120.9(6) . . ?

C2 C1 Cl1A 120.0(5) . . ?

C6 C1 Cl1A 119.0(5) . . ?

C1 C2 C3 119.6(5) . . ?

C1 C2 H2 120.2 . . ?

C3 C2 H2 120.2 . . ?

C4 C3 C2 120.9(5) . . ?

C4 C3 H3 119.5 . . ?

C2 C3 H3 119.5 . . ?

C3 C4 C5 120.1(6) . . ?

C3 C4 S1 121.9(5) . . ?

C5 C4 S1 118.0(4) . . ?

C6 C5 N1 123.4(4) . . ?

C6 C5 C4 118.7(4) . . ?

N1 C5 C4 117.8(5) . . ?

C5 C6 C1 119.7(5) . . ?

C5 C6 H6 120.1 . . ?

C1 C6 H6 120.1 . . ?

C8 C7 C12 120.2(5) . . ?

C8 C7 S1 121.1(4) . . ?

C12 C7 S1 118.6(4) . . ?

C7 C8 C9 120.5(6) . . ?

C7 C8 H8 119.8 . . ?

C9 C8 H8 119.8 . . ?

C10 C9 C8 118.4(6) . . ?

C10 C9 H9 120.8 . . ?

C8 C9 H9 120.8 . . ?

C9 C10 C11 123.3(7) . . ?

C9 C10 H10 118.3 . . ?

C11 C10 H10 118.3 . . ?

C12 C11 C10 118.7(5) . . ?

C12 C11 H11 120.6 . . ?

C10 C11 H11 120.6 . . ?

C11 C12 C7 118.8(5) . . ?

C11 C12 N1 122.7(4) . . ?

C7 C12 N1 118.5(5) . . ?

N1 C13 C14 112.0(4) . . ?

N1 C13 H13A 109.2 . . ?

C14 C13 H13A 109.2 . . ?

N1 C13 H13B 109.2 . . ?

C14 C13 H13B 109.2 . . ?

H13A C13 H13B 107.9 . . ?

C15 C14 C13 112.1(4) . . ?

C15 C14 H14A 109.2 . . ?

C13 C14 H14A 109.2 . . ?

C15 C14 H14B 109.2 . . ?

C13 C14 H14B 109.2 . . ?

H14A C14 H14B 107.9 . . ?

N2 C15 C14 114.4(4) . . ?

N2 C15 H15A 108.7 . . ?

C14 C15 H15A 108.7 . . ?

N2 C15 H15B 108.7 . . ?

C14 C15 H15B 108.7 . . ?

H15A C15 H15B 107.6 . . ?

N2 C16 C17 111.0(3) . . ?

N2 C16 H16A 109.4 . . ?

C17 C16 H16A 109.4 . . ?

N2 C16 H16B 109.4 . . ?

C17 C16 H16B 109.4 . . ?

H16A C16 H16B 108.0 . . ?

N3 C17 C16 111.9(3) . . ?

N3 C17 H17A 109.2 . . ?

C16 C17 H17A 109.2 . . ?

N3 C17 H17B 109.2 . . ?

C16 C17 H17B 109.2 . . ?

H17A C17 H17B 107.9 . . ?

C19 C18 N3 110.2(3) . . ?

C19 C18 H18A 109.6 . . ?

N3 C18 H18A 109.6 . . ?

C19 C18 H18B 109.6 . . ?

N3 C18 H18B 109.6 . . ?

H18A C18 H18B 108.1 . . ?

N2 C19 C18 111.5(3) . . ?

N2 C19 H19A 109.3 . . ?

C18 C19 H19A 109.3 . . ?

N2 C19 H19B 109.3 . . ?

C18 C19 H19B 109.3 . . ?

H19A C19 H19B 108.0 . . ?

C21 C20 N3 113.9(4) . . ?

C21 C20 H20A 108.8 . . ?

N3 C20 H20A 108.8 . . ?

C21 C20 H20B 108.8 . . ?

N3 C20 H20B 108.8 . . ?

H20A C20 H20B 107.7 . . ?

O1 C21 C20 111.2(4) . . ?

O1 C21 H21A 109.4 . . ?

C20 C21 H21A 109.4 . . ?

O1 C21 H21B 109.4 . . ?

C20 C21 H21B 109.4 . . ?

H21A C21 H21B 108.0 . . ?

O2 C22 O3 123.6(4) . . ?

O2 C22 C23 118.2(4) . . ?

O3 C22 C23 118.1(4) . . ?

C23 C23 C22 125.3(5) 3_556 . ?

C23 C23 H23 117.4 3_556 . ?

C22 C23 H23 117.4 . . ?

C5 N1 C12 116.0(4) . . ?

C5 N1 C13 119.1(4) . . ?

C12 N1 C13 117.9(4) . . ?

C15 N2 C19 110.1(3) . . ?

C15 N2 C16 112.5(3) . . ?

C19 N2 C16 107.8(3) . . ?

C17 N3 C20 110.8(3) . . ?

C17 N3 C18 109.7(3) . . ?

C20 N3 C18 111.8(3) . . ?

C17 N3 H3N 107(3) . . ?

C20 N3 H3N 110(3) . . ?

C18 N3 H3N 108(3) . . ?

C21 O1 H1O 110(4) . . ?

C4 S1 C7 97.5(3) . . ?



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 1.9(8) . . . . ?

Cl1A C1 C2 C3 177.0(4) . . . . ?

C1 C2 C3 C4 -0.3(8) . . . . ?

C2 C3 C4 C5 -2.1(8) . . . . ?

C2 C3 C4 S1 -179.5(4) . . . . ?

C3 C4 C5 C6 2.8(7) . . . . ?

S1 C4 C5 C6 -179.6(3) . . . . ?

C3 C4 C5 N1 -174.1(4) . . . . ?

S1 C4 C5 N1 3.4(6) . . . . ?

N1 C5 C6 C1 175.6(4) . . . . ?

C4 C5 C6 C1 -1.2(6) . . . . ?

C2 C1 C6 C5 -1.1(7) . . . . ?

Cl1A C1 C6 C5 -176.2(3) . . . . ?

C12 C7 C8 C9 0.7(8) . . . . ?

S1 C7 C8 C9 -178.6(4) . . . . ?

C7 C8 C9 C10 -1.1(9) . . . . ?

C8 C9 C10 C11 -0.4(9) . . . . ?

C9 C10 C11 C12 2.3(8) . . . . ?

C10 C11 C12 C7 -2.7(7) . . . . ?

C10 C11 C12 N1 179.7(4) . . . . ?

C8 C7 C12 C11 1.3(7) . . . . ?

S1 C7 C12 C11 -179.4(4) . . . . ?

C8 C7 C12 N1 179.0(4) . . . . ?

S1 C7 C12 N1 -1.8(6) . . . . ?

N1 C13 C14 C15 173.3(4) . . . . ?

C13 C14 C15 N2 -58.7(5) . . . . ?

N2 C16 C17 N3 57.5(5) . . . . ?

N3 C18 C19 N2 -59.6(4) . . . . ?

N3 C20 C21 O1 -175.6(4) . . . . ?

O2 C22 C23 C23 -169.1(6) . . . 3_556 ?

O3 C22 C23 C23 9.0(8) . . . 3_556 ?

C6 C5 N1 C12 -130.3(4) . . . . ?

C4 C5 N1 C12 46.5(5) . . . . ?

C6 C5 N1 C13 19.7(6) . . . . ?

C4 C5 N1 C13 -163.5(4) . . . . ?

C11 C12 N1 C5 129.6(5) . . . . ?

C7 C12 N1 C5 -48.0(5) . . . . ?

C11 C12 N1 C13 -20.8(6) . . . . ?

C7 C12 N1 C13 161.6(4) . . . . ?

C14 C13 N1 C5 65.7(5) . . . . ?

C14 C13 N1 C12 -144.8(4) . . . . ?

C14 C15 N2 C19 173.8(3) . . . . ?

C14 C15 N2 C16 -66.0(5) . . . . ?

C18 C19 N2 C15 -175.0(3) . . . . ?

C18 C19 N2 C16 61.9(4) . . . . ?

C17 C16 N2 C15 178.2(3) . . . . ?

C17 C16 N2 C19 -60.2(4) . . . . ?

C16 C17 N3 C20 -177.1(3) . . . . ?

C16 C17 N3 C18 -53.2(4) . . . . ?

C21 C20 N3 C17 -169.3(4) . . . . ?

C21 C20 N3 C18 67.9(5) . . . . ?

C19 C18 N3 C17 53.6(4) . . . . ?

C19 C18 N3 C20 176.9(3) . . . . ?

C3 C4 S1 C7 136.3(4) . . . . ?

C5 C4 S1 C7 -41.1(4) . . . . ?

C8 C7 S1 C4 -140.4(4) . . . . ?

C12 C7 S1 C4 40.4(4) . . . . ?



_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        25.51

_diffrn_measured_fraction_theta_full 0.993

_refine_diff_density_max         1.069

_refine_diff_density_min         -0.728

_refine_diff_density_rms         0.077





# END of CIF