data_global


#==============================================================================
#                          1. SUBMISSION DETAILS
#==============================================================================


_publ_contact_author_name   'Dr. Alan Shaver'

_publ_contact_author_address
;
      University of McGill
      Department of Chemistry
      Otto Maass Chemistry Building
      801 Sherbrooke St. West     
      Montréal, Québec
      Canada H3A 2K6

;


_publ_contact_author_phone        '+1 514 343 6237''
_publ_contact_author_fax          '+1 514 343 2382''
_publ_contact_author_email        'alan.shaver@mcgill.ca'

_publ_requested_journal           'Acta Crystallographica C'
_publ_requested_category          'FO'



_publ_requested_coeditor_name
;
     Dr Anthony Linden
     Institute of Organic Chemistry
     University of Zurich
     Winterthurerstrasse 190
     CH-8057 Zurich, Switzerland
;


_publ_contact_letter
;

Please consider this CIF submission for publication in Acta Crystallographica
Section C.  All authors have seen and approved of this submission.

The CIF has passed the Chester CHECKCIF routines and gives a satisfactory
PRINTCIF file.

When I hear back from you by e-mail with your reference number I will fax and
air-mail a formal Letter of Submission and a signed Copyright Transfer Form.

I will then ftp the Artwork and Structure Factor Listing to you (as Postscript
and ASCII files respectively).

;

#==============================================================================
#                   2. PROCESSING SUMMARY (IUCr Office Use Only)
#==============================================================================


_journal_date_recd_electronic     ?

_journal_date_to_coeditor         ?
_journal_date_from_coeditor       ?
_journal_date_accepted            ?

_journal_date_printers_first      ?
_journal_date_printers_final      ?
_journal_date_proofs_out          ?
_journal_date_proofs_in           ?

_journal_coeditor_name            ?
_journal_coeditor_code            ?
_journal_coeditor_notes
; ?
;

_journal_techeditor_code          ?
_journal_techeditor_notes
; ?
;

_journal_coden_ASTM               ?
_journal_name_full                ?
_journal_year                     ?
_journal_volume                   ?
_journal_issue                    ?
_journal_page_first               ?
_journal_page_last                ?

_journal_suppl_publ_number        ?
_journal_suppl_publ_pages         ?

#==============================================================================
#                        3. TITLE AND AUTHOR LIST
#==============================================================================


_publ_section_title
;
Structure of SHAV58
;

# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.

loop_
    _publ_author_name
    _publ_author_address
     'Shaver,  Alan'
;
      University of McGill
      Department of Chemistry
      Otto Maass Chemistry Building
      801 Sherbrooke St. West     
      Montréal, Québec
      Canada H3A 2K6
;
      'Mortini, Florent'
;
      University of McGill
      Department of Chemistry
      Otto Maass Chemistry Building
      801 Sherbrooke St. West     
      Montréal, Québec
      Canada H3A 2K6
;
      "Bélanger-Gariépy, Francine"
;
       Département de Chimie
       Université de Montréal
       C.P. 6128, Succ. Centre-ville,
       Montréal, Québec
       Canada H3C 3J7

;
#==============================================================================
#                              4. TEXT
#==============================================================================


_publ_section_abstract
;
 The crystal stucture of the title compound, recrystallized from ...
;


_publ_section_comment
;
 comment
;

_publ_section_exptl_prep
;
 Small details about the preparation of the compound.
;

_publ_section_acknowledgements

;
 We are grateful to the Natural Sciences and Engineering Research
 Council of Canada and the Ministère de l'Education du Québec
 for financial support.
;
_publ_section_exptl_refinement

;
 Data reduction processing was carried out by the use of the program 
 SAINT (Bruker, 1999), which applied Lorentz and polarization 
 corrections to three-dimensionally integrated diffraction spots. 
 The program SADABS (Sheldrick, 1996) was utilized for the scaling 
 of diffraction data, the application of a decay correction, and an 
 empirical absorption correction based on redundant reflections. 
 The space group was confirmed by XPREP routine in SHELXTL program 
 (Sheldrick, 1997).  The structure was solved by direct method using 
 SHELXS97 (Sheldrick, 1997) and difmap synthesis using SHELXL96 
 (Sheldrick, 1996). All non-hydrogen atoms anisotropic, hydrogen 
 atoms isotropic.  Hydrogen atoms constrained to the parent 
 site using a riding model; SHELXL97 defaults,  C-H 0.93 to 0.98, 
 N-H 0.86 and O-H 0.82Å.   
 The isotropic factors, Uiso, were adjusted to 50% higher 
 value of the parent site (methyl) and 20% higher (others).  A final 
 verification of possible voids was performed using the VOID routine 
 of the PLATON program (Spek, 2000). 
; 

_publ_section_references
;

 Flack, H.D. (1983). Acta Cryst. A39, 876-881.

 Flack, H.D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506.

 International Tables for Crystallography (1992).  Vol. C.  Tables 4.2.6.8 and
 6.1.1.4, Dordrecht: Kluwer Academic Publishers.

 SAINT Release 6.06 (1999) Integration Software for Single Crystal Data.
 Bruker AXS Inc., Madison, WI 53719-1173.

 Sheldrick, G.M. (1996) SADABS, Bruker Area Detector Absorption Corrections.
 Bruker AXS Inc., Madison, WI 53719-1173.

 Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure
 solution. University of Göttingen, Germany.

 Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure
 refinement. University of Göttingen, Germany.

 SHELXTL (1997) Release 5.10; The Complete Software Package for Single
 Crystal Structure Determination.  Bruker AXS Inc.,
 Madison, WI 53719-1173.

 SMART (1999) Release 5.059; Bruker Molecular Analysis Research Tool.
 Bruker AXS Inc., Madison, WI 53719-1173.

 Spek, A.L. (2000). PLATON, Molecular Geometry Program, 2000 version.
 University of Utrecht, Utrecht, Holland.

 XPREP (1997) Release 5.10; X-ray data Preparation and Reciprocal space
 Exploration Program.  Bruker AXS Inc., Madison, WI 53719-1173.

;


_publ_section_figure_captions
;
Fig 1 ORTEP (SHELXTL, 1999) drawing of the molecule. 
 Ellipsoids correspond to 30% probability.

;

_publ_section_table_legends
;

;





# ========================================================
#                     STRUCTURAL DATA                     
# ========================================================


 
data_shav58 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C22 H35 Cl2 Ir N P S3' 
_chemical_formula_weight          703.76 
_chemical_compound_source         'Synthesized by the authors. See text'

loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 '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'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'P'  'P'   0.2955   0.4335 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.3331   0.5567 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ir'  'Ir'  -4.7710   6.5667 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.3639   0.7018 
 '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
_symmetry_space_group_name_hall   '-P 1'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    8.8659(8) 
_cell_length_b                    12.3044(10) 
_cell_length_c                    13.2239(11) 
_cell_angle_alpha                 79.312(5) 
_cell_angle_beta                  83.152(6) 
_cell_angle_gamma                 81.035(6) 
_cell_volume                      1394.2(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     220(2)
_cell_measurement_reflns_used     7569
_cell_measurement_theta_min        3.42
_cell_measurement_theta_max       72.62
 
_exptl_crystal_description        needle-like
_exptl_crystal_colour             orange
_exptl_crystal_size_max           0.31
_exptl_crystal_size_mid           0.11
_exptl_crystal_size_min           0.08
_exptl_crystal_density_meas       none
_exptl_crystal_density_diffrn     1.676 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              696 
_exptl_absorpt_coefficient_mu     13.749 
_exptl_absorpt_correction_Type    multi-scan
_exptl_absorpt_correction_T_min   0.2100
_exptl_absorpt_correction_T_max   0.5400
_exptl_absorpt_process_details    'Sadabs (Sheldrick,1996)'
 
_exptl_special_details
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker Platform diffractometer, equipped with a Bruker SMART 2K
Charged-Coupled Device (CCD) Area Detector using the program SMART and
normal focus sealed tube source graphite monochromated Cu-Kα radiation.
The crystal-to-detector distance was 4.908 cm, and the data collection
was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 9.0 degree
scan in 30 frames over four different parts of the reciprocal space
(120 frames total).  One complete sphere of data was collected, to
better than 0.8Å resolution.  Upon completion of the data collection,
the first 101 frames were recollected in order to improve the decay
correction analysis.
;
 
_diffrn_ambient_temperature       220(2)
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'Sealed Tube'
_diffrn_radiation_monochromator   'graphite'
_diffrn_measurement_device_type   'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method        'ω'
_diffrn_detector_area_resol_mean   5.5
_diffrn_standards_number          5
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%           0.00
_diffrn_reflns_number             16762
_diffrn_reflns_av_R_equivalents   0.031
_diffrn_reflns_av_sigmaI/netI     0.0268 
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          3.42 
_diffrn_reflns_theta_max          72.69 
_reflns_number_total              5311
_reflns_number_gt                 5000
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'SAINT (Bruker, 1999)'
_computing_cell_refinement        'SMART (Bruker, 1999)'
_computing_data_reduction         'SAINT (Bruker, 1999)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'XP (Bruker, 1999)'
_computing_publication_material   'UdMX (local program)'
 
_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)+(0.0562P)²+0.1317P] 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          5311 
_refine_ls_number_parameters      288 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0300 
_refine_ls_R_factor_gt            0.0282 
_refine_ls_wR_factor_ref          0.0784 
_refine_ls_wR_factor_gt           0.0753 
_refine_ls_goodness_of_fit_ref    1.069 
_refine_ls_restrained_S_all       1.069 
_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_symetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ir Ir 0.142937(16) 0.240827(11) 0.641764(11) 0.03015(7) Uani 1 1 d . . . 
S1 S 0.02243(11) 0.07731(8) 0.67460(8) 0.0383(2) Uani 1 1 d . . . 
S2 S -0.08079(12) 0.36733(8) 0.59429(8) 0.0407(2) Uani 1 1 d . . . 
H2 H -0.032(11) 0.436(8) 0.574(7) 0.16(4) Uiso 1 1 d . . . 
S10 S -0.19367(13) -0.04055(9) 0.82021(9) 0.0471(2) Uani 1 1 d . . . 
P P 0.17630(13) 0.21244(9) 0.47479(8) 0.0399(2) Uani 1 1 d . . . 
N10 N -0.1949(4) 0.1830(3) 0.7890(3) 0.0398(7) Uani 1 1 d . . . 
H10 H -0.160(5) 0.245(4) 0.741(4) 0.039(12) Uiso 1 1 d . . . 
C10 C -0.1343(4) 0.0825(3) 0.7677(3) 0.0346(8) Uani 1 1 d . . . 
C11 C -0.3197(4) 0.2191(3) 0.8587(3) 0.0379(8) Uani 1 1 d . . . 
C12 C -0.3785(6) 0.3315(4) 0.8394(4) 0.0501(11) Uani 1 1 d . . . 
H12 H -0.3375 0.3781 0.7814 0.060 Uiso 1 1 calc R . . 
C13 C -0.4970(6) 0.3761(4) 0.9043(4) 0.0540(11) Uani 1 1 d . . . 
H13 H -0.5341 0.4527 0.8907 0.065 Uiso 1 1 calc R . . 
C14 C -0.5619(5) 0.3081(4) 0.9899(4) 0.0480(10) Uani 1 1 d . . . 
C15 C -0.5036(5) 0.1972(4) 1.0077(4) 0.0501(11) Uani 1 1 d . . . 
H15 H -0.5459 0.1508 1.0653 0.060 Uiso 1 1 calc R . . 
C16 C -0.3832(5) 0.1499(4) 0.9434(3) 0.0465(10) Uani 1 1 d . . . 
H16 H -0.3463 0.0733 0.9572 0.056 Uiso 1 1 calc R . . 
C17 C -0.6906(6) 0.3571(5) 1.0617(4) 0.0653(14) Uani 1 1 d . . . 
H17A H -0.7728 0.3113 1.0739 0.098 Uiso 1 1 calc R . . 
H17B H -0.7292 0.4324 1.0302 0.098 Uiso 1 1 calc R . . 
H17C H -0.6519 0.3589 1.1269 0.098 Uiso 1 1 calc R . . 
C18 C 0.0071(6) 0.1990(5) 0.4152(4) 0.0638(14) Uani 1 1 d . . . 
H18A H 0.0382 0.1718 0.3506 0.096 Uiso 1 1 calc R . . 
H18B H -0.0555 0.2713 0.4020 0.096 Uiso 1 1 calc R . . 
H18C H -0.0518 0.1467 0.4614 0.096 Uiso 1 1 calc R . . 
C19 C 0.3015(7) 0.0854(4) 0.4548(4) 0.0623(14) Uani 1 1 d . . . 
H19A H 0.2623 0.0219 0.4991 0.093 Uiso 1 1 calc R . . 
H19B H 0.4038 0.0898 0.4714 0.093 Uiso 1 1 calc R . . 
H19C H 0.3055 0.0766 0.3831 0.093 Uiso 1 1 calc R . . 
C20 C 0.2589(7) 0.3206(5) 0.3830(4) 0.0654(14) Uani 1 1 d . . . 
H20A H 0.3606 0.3253 0.4005 0.098 Uiso 1 1 calc R . . 
H20B H 0.1945 0.3916 0.3853 0.098 Uiso 1 1 calc R . . 
H20C H 0.2659 0.3027 0.3140 0.098 Uiso 1 1 calc R . . 
C21 C 0.2890(6) 0.3555(4) 0.6760(4) 0.0481(11) Uani 1 1 d . . . 
C22 C 0.3846(5) 0.2537(4) 0.6629(4) 0.0469(10) Uani 1 1 d . . . 
C23 C 0.3288(5) 0.1668(4) 0.7397(4) 0.0440(10) Uani 1 1 d . . . 
C24 C 0.2069(6) 0.2181(4) 0.8047(3) 0.0460(10) Uani 1 1 d . . . 
C25 C 0.1831(6) 0.3330(4) 0.7657(4) 0.0483(10) Uani 1 1 d . . . 
C26 C 0.3178(9) 0.4698(5) 0.6191(5) 0.083(2) Uani 1 1 d . . . 
H26A H 0.2207 0.5153 0.6047 0.124 Uiso 1 1 calc R . . 
H26B H 0.3802 0.4624 0.5547 0.124 Uiso 1 1 calc R . . 
H26C H 0.3712 0.5049 0.6615 0.124 Uiso 1 1 calc R . . 
C27 C 0.5281(6) 0.2391(6) 0.5894(5) 0.0787(18) Uani 1 1 d . . . 
H27A H 0.5239 0.3003 0.5314 0.118 Uiso 1 1 calc R . . 
H27B H 0.5350 0.1690 0.5644 0.118 Uiso 1 1 calc R . . 
H27C H 0.6175 0.2386 0.6254 0.118 Uiso 1 1 calc R . . 
C28 C 0.3984(7) 0.0461(4) 0.7593(5) 0.0689(16) Uani 1 1 d . . . 
H28A H 0.4725 0.0355 0.8099 0.103 Uiso 1 1 calc R . . 
H28B H 0.4492 0.0250 0.6953 0.103 Uiso 1 1 calc R . . 
H28C H 0.3183 -0.0001 0.7855 0.103 Uiso 1 1 calc R . . 
C29 C 0.1315(7) 0.1557(6) 0.9010(4) 0.0725(17) Uani 1 1 d . . . 
H29A H 0.1999 0.1411 0.9555 0.109 Uiso 1 1 calc R . . 
H29B H 0.1089 0.0854 0.8873 0.109 Uiso 1 1 calc R . . 
H29C H 0.0370 0.2001 0.9226 0.109 Uiso 1 1 calc R . . 
C30 C 0.0691(8) 0.4176(6) 0.8118(5) 0.084(2) Uani 1 1 d . . . 
H30A H -0.0116 0.3808 0.8540 0.125 Uiso 1 1 calc R . . 
H30B H 0.0251 0.4727 0.7569 0.125 Uiso 1 1 calc R . . 
H30C H 0.1199 0.4543 0.8544 0.125 Uiso 1 1 calc R . . 
Cl1 Cl 0.6556(2) 0.24349(19) 0.26783(18) 0.1063(7) Uani 1 1 d . . . 
Cl2 Cl 0.8696(3) 0.32808(18) 0.1036(2) 0.1410(11) Uani 1 1 d . . . 
C31 C 0.7977(6) 0.2124(5) 0.1718(5) 0.0646(14) Uani 1 1 d . . . 
H31A H 0.8814 0.1602 0.2033 0.078 Uiso 1 1 calc R . . 
H31B H 0.7558 0.1751 0.1242 0.078 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_site_symmetry_1            
        _geom_bond_site_symmetry_2            
        _geom_bond_distance                   
        _geom_bond_publ_flag                  
Ir             C21            .              .                     2.195(4)   Y
Ir             C23            .              .                     2.197(4)   Y
Ir             C22            .              .                     2.226(4)   Y
Ir             C25            .              .                     2.248(4)   Y
Ir             C24            .              .                     2.250(4)   Y
Ir             P              .              .                   2.2767(10)   Y
Ir             S1             .              .                    2.3692(9)   Y
Ir             S2             .              .                   2.3924(10)   Y
S1             C10            .              .                     1.744(4)   Y
S2             H2             .              .                      0.99(9)   Y
S10            C10            .              .                     1.681(4)   Y
P              C20            .              .                     1.809(5)   Y
P              C19            .              .                     1.814(5)   Y
P              C18            .              .                     1.818(5)   Y
N10            C10            .              .                     1.335(5)   Y
N10            C11            .              .                     1.423(5)   Y
N10            H10            .              .                      0.96(5)   Y
C11            C12            .              .                     1.388(6)   Y
C11            C16            .              .                     1.393(6)   Y
C12            C13            .              .                     1.386(6)   Y
C12            H12            .              .                         0.94   ?
C13            C14            .              .                     1.398(6)   Y
C13            H13            .              .                         0.94   ?
C14            C15            .              .                     1.369(7)   Y
C14            C17            .              .                     1.519(6)   Y
C15            C16            .              .                     1.405(6)   Y
C15            H15            .              .                         0.94   ?
C16            H16            .              .                         0.94   ?
C17            H17a           .              .                         0.97   ?
C17            H17b           .              .                         0.97   ?
C17            H17c           .              .                         0.97   ?
C18            H18a           .              .                         0.97   ?
C18            H18b           .              .                         0.97   ?
C18            H18c           .              .                         0.97   ?
C19            H19a           .              .                         0.97   ?
C19            H19b           .              .                         0.97   ?
C19            H19c           .              .                         0.97   ?
C20            H20a           .              .                         0.97   ?
C20            H20b           .              .                         0.97   ?
C20            H20c           .              .                         0.97   ?
C21            C22            .              .                     1.426(7)   Y
C21            C25            .              .                     1.435(7)   Y
C21            C26            .              .                     1.510(6)   Y
C22            C23            .              .                     1.436(6)   Y
C22            C27            .              .                     1.515(7)   Y
C23            C24            .              .                     1.439(7)   Y
C23            C28            .              .                     1.505(6)   Y
C24            C25            .              .                     1.404(6)   Y
C24            C29            .              .                     1.501(7)   Y
C25            C30            .              .                     1.496(7)   Y
C26            H26a           .              .                         0.97   ?
C26            H26b           .              .                         0.97   ?
C26            H26c           .              .                         0.97   ?
C27            H27a           .              .                         0.97   ?
C27            H27b           .              .                         0.97   ?
C27            H27c           .              .                         0.97   ?
C28            H28a           .              .                         0.97   ?
C28            H28b           .              .                         0.97   ?
C28            H28c           .              .                         0.97   ?
C29            H29a           .              .                         0.97   ?
C29            H29b           .              .                         0.97   ?
C29            H29c           .              .                         0.97   ?
C30            H30a           .              .                         0.97   ?
C30            H30b           .              .                         0.97   ?
C30            H30c           .              .                         0.97   ?
Cl1            C31            .              .                     1.731(6)   Y
Cl2            C31            .              .                     1.708(6)   Y
C31            H31a           .              .                         0.98   ?
C31            H31b           .              .                         0.98   ?

loop_                                         
        _geom_angle_atom_site_label_1         
        _geom_angle_atom_site_label_2         
        _geom_angle_atom_site_label_3         
        _geom_angle_site_symmetry_1           
        _geom_angle_site_symmetry_2           
        _geom_angle_site_symmetry_3           
        _geom_angle                           
        _geom_angle_publ_flag                 
C21       IR        C23       .         .         .          63.33(16)        Y
C21       IR        C22       .         .         .          37.62(18)        Y
C23       IR        C22       .         .         .          37.88(17)        Y
C21       IR        C25       .         .         .          37.66(18)        Y
C23       IR        C25       .         .         .          62.36(17)        Y
C22       IR        C25       .         .         .          62.33(18)        Y
C21       IR        C24       .         .         .          62.42(16)        Y
C23       IR        C24       .         .         .          37.75(17)        Y
C22       IR        C24       .         .         .          62.53(17)        Y
C25       IR        C24       .         .         .          36.38(17)        Y
C21       IR        P         .         .         .         114.18(13)        Y
C23       IR        P         .         .         .         117.20(13)        Y
C22       IR        P         .         .         .          98.90(13)        Y
C25       IR        P         .         .         .         151.17(14)        Y
C24       IR        P         .         .         .         154.81(13)        Y
C21       IR        S1        .         .         .         154.98(12)        Y
C23       IR        S1        .         .         .          94.05(12)        Y
C22       IR        S1        .         .         .         127.35(13)        Y
C25       IR        S1        .         .         .         123.78(13)        Y
C24       IR        S1        .         .         .          93.34(12)        Y
P         IR        S1        .         .         .           84.84(4)        Y
C21       IR        S2        .         .         .         101.15(13)        Y
C23       IR        S2        .         .         .         155.11(13)        Y
C22       IR        S2        .         .         .         136.63(13)        Y
C25       IR        S2        .         .         .          93.27(12)        Y
C24       IR        S2        .         .         .         118.72(13)        Y
P         IR        S2        .         .         .           86.43(4)        Y
S1        IR        S2        .         .         .           95.93(4)        Y
C10       S1        IR        .         .         .         113.26(13)        Y
IR        S2        H2        .         .         .              98(6)        Y
C20       P         C19       .         .         .           103.9(3)        Y
C20       P         C18       .         .         .           102.3(3)        Y
C19       P         C18       .         .         .           101.9(3)        Y
C20       P         IR        .         .         .         115.18(19)        Y
C19       P         IR        .         .         .         114.05(18)        Y
C18       P         IR        .         .         .         117.52(18)        Y
C10       N10       C11       .         .         .           132.8(3)        Y
C10       N10       H10       .         .         .             115(3)        Y
C11       N10       H10       .         .         .             112(3)        Y
N10       C10       S10       .         .         .           127.0(3)        Y
N10       C10       S1        .         .         .           117.1(3)        Y
S10       C10       S1        .         .         .           115.9(2)        Y
C12       C11       C16       .         .         .           119.3(4)        Y
C12       C11       N10       .         .         .           116.2(4)        Y
C16       C11       N10       .         .         .           124.5(4)        Y
C13       C12       C11       .         .         .           120.9(4)        Y
C13       C12       H12       .         .         .              119.5        ?
C11       C12       H12       .         .         .              119.5        ?
C12       C13       C14       .         .         .           120.6(4)        Y
C12       C13       H13       .         .         .              119.7        ?
C14       C13       H13       .         .         .              119.7        ?
C15       C14       C13       .         .         .           118.0(4)        Y
C15       C14       C17       .         .         .           121.4(4)        Y
C13       C14       C17       .         .         .           120.6(5)        Y
C14       C15       C16       .         .         .           122.6(4)        Y
C14       C15       H15       .         .         .              118.7        ?
C16       C15       H15       .         .         .              118.7        ?
C11       C16       C15       .         .         .           118.6(4)        Y
C11       C16       H16       .         .         .              120.7        ?
C15       C16       H16       .         .         .              120.7        ?
C14       C17       H17A      .         .         .              109.5        ?
C14       C17       H17B      .         .         .              109.5        ?
H17A      C17       H17B      .         .         .              109.5        ?
C14       C17       H17C      .         .         .              109.5        ?
H17A      C17       H17C      .         .         .              109.5        ?
H17B      C17       H17C      .         .         .              109.5        ?
P         C18       H18A      .         .         .              109.5        ?
P         C18       H18B      .         .         .              109.5        ?
H18A      C18       H18B      .         .         .              109.5        ?
P         C18       H18C      .         .         .              109.5        ?
H18A      C18       H18C      .         .         .              109.5        ?
H18B      C18       H18C      .         .         .              109.5        ?
P         C19       H19A      .         .         .              109.5        ?
P         C19       H19B      .         .         .              109.5        ?
H19A      C19       H19B      .         .         .              109.5        ?
P         C19       H19C      .         .         .              109.5        ?
H19A      C19       H19C      .         .         .              109.5        ?
H19B      C19       H19C      .         .         .              109.5        ?
P         C20       H20A      .         .         .              109.5        ?
P         C20       H20B      .         .         .              109.5        ?
H20A      C20       H20B      .         .         .              109.5        ?
P         C20       H20C      .         .         .              109.5        ?
H20A      C20       H20C      .         .         .              109.5        ?
H20B      C20       H20C      .         .         .              109.5        ?
C22       C21       C25       .         .         .           108.1(4)        Y
C22       C21       C26       .         .         .           124.8(5)        Y
C25       C21       C26       .         .         .           125.9(5)        Y
C22       C21       IR        .         .         .            72.4(2)        Y
C25       C21       IR        .         .         .            73.2(2)        Y
C26       C21       IR        .         .         .           130.1(3)        Y
C21       C22       C23       .         .         .           107.3(4)        Y
C21       C22       C27       .         .         .           127.2(5)        Y
C23       C22       C27       .         .         .           125.2(5)        Y
C21       C22       IR        .         .         .            70.0(2)        Y
C23       C22       IR        .         .         .            69.9(2)        Y
C27       C22       IR        .         .         .           129.7(3)        Y
C22       C23       C24       .         .         .           107.8(4)        Y
C22       C23       C28       .         .         .           126.5(5)        Y
C24       C23       C28       .         .         .           125.2(5)        Y
C22       C23       IR        .         .         .            72.2(2)        Y
C24       C23       IR        .         .         .            73.1(2)        Y
C28       C23       IR        .         .         .           126.8(3)        Y
C25       C24       C23       .         .         .           108.1(4)        Y
C25       C24       C29       .         .         .           128.3(5)        Y
C23       C24       C29       .         .         .           123.4(5)        Y
C25       C24       IR        .         .         .            71.8(2)        Y
C23       C24       IR        .         .         .            69.1(2)        Y
C29       C24       IR        .         .         .           128.1(3)        Y
C24       C25       C21       .         .         .           108.4(4)        Y
C24       C25       C30       .         .         .           125.6(5)        Y
C21       C25       C30       .         .         .           126.0(5)        Y
C24       C25       IR        .         .         .            71.9(2)        Y
C21       C25       IR        .         .         .            69.2(2)        Y
C30       C25       IR        .         .         .           125.9(4)        Y
C21       C26       H26A      .         .         .              109.5        ?
C21       C26       H26B      .         .         .              109.5        ?
H26A      C26       H26B      .         .         .              109.5        ?
C21       C26       H26C      .         .         .              109.5        ?
H26A      C26       H26C      .         .         .              109.5        ?
H26B      C26       H26C      .         .         .              109.5        ?
C22       C27       H27A      .         .         .              109.5        ?
C22       C27       H27B      .         .         .              109.5        ?
H27A      C27       H27B      .         .         .              109.5        ?
C22       C27       H27C      .         .         .              109.5        ?
H27A      C27       H27C      .         .         .              109.5        ?
H27B      C27       H27C      .         .         .              109.5        ?
C23       C28       H28A      .         .         .              109.5        ?
C23       C28       H28B      .         .         .              109.5        ?
H28A      C28       H28B      .         .         .              109.5        ?
C23       C28       H28C      .         .         .              109.5        ?
H28A      C28       H28C      .         .         .              109.5        ?
H28B      C28       H28C      .         .         .              109.5        ?
C24       C29       H29A      .         .         .              109.5        ?
C24       C29       H29B      .         .         .              109.5        ?
H29A      C29       H29B      .         .         .              109.5        ?
C24       C29       H29C      .         .         .              109.5        ?
H29A      C29       H29C      .         .         .              109.5        ?
H29B      C29       H29C      .         .         .              109.5        ?
C25       C30       H30A      .         .         .              109.5        ?
C25       C30       H30B      .         .         .              109.5        ?
H30A      C30       H30B      .         .         .              109.5        ?
C25       C30       H30C      .         .         .              109.5        ?
H30A      C30       H30C      .         .         .              109.5        ?
H30B      C30       H30C      .         .         .              109.5        ?
CL2       C31       CL1       .         .         .           112.7(3)        Y
CL2       C31       H31A      .         .         .                109        ?
CL1       C31       H31A      .         .         .                109        ?
CL2       C31       H31B      .         .         .                109        ?
CL1       C31       H31B      .         .         .                109        ?
H31A      C31       H31B      .         .         .              107.8        ?

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_site_symmetry_1         
        _geom_torsion_site_symmetry_2         
        _geom_torsion_site_symmetry_3         
        _geom_torsion_site_symmetry_4         
        _geom_torsion                         
        _geom_torsion_publ_flag               
C21     IR      S1      C10     .       .       .       .           75.6(4)   Y
C23     IR      S1      C10     .       .       .       .         99.80(19)   Y
C22     IR      S1      C10     .       .       .       .          119.5(2)   Y
C25     IR      S1      C10     .       .       .       .           40.6(2)   Y
C24     IR      S1      C10     .       .       .       .         61.98(19)   Y
P       IR      S1      C10     .       .       .       .       -143.22(14)   Y
S2      IR      S1      C10     .       .       .       .        -57.35(14)   Y
C21     IR      P       C20     .       .       .       .          -21.8(3)   Y
C23     IR      P       C20     .       .       .       .          -93.0(3)   Y
C22     IR      P       C20     .       .       .       .          -57.9(3)   Y
C25     IR      P       C20     .       .       .       .          -11.5(3)   Y
C24     IR      P       C20     .       .       .       .          -98.0(4)   Y
S1      IR      P       C20     .       .       .       .          175.1(2)   Y
S2      IR      P       C20     .       .       .       .           78.8(2)   Y
C21     IR      P       C19     .       .       .       .           98.3(3)   Y
C23     IR      P       C19     .       .       .       .           27.1(3)   Y
C22     IR      P       C19     .       .       .       .           62.2(3)   Y
C25     IR      P       C19     .       .       .       .          108.6(3)   Y
C24     IR      P       C19     .       .       .       .           22.0(4)   Y
S1      IR      P       C19     .       .       .       .          -64.8(2)   Y
S2      IR      P       C19     .       .       .       .         -161.1(2)   Y
C21     IR      P       C18     .       .       .       .         -142.5(3)   Y
C23     IR      P       C18     .       .       .       .          146.3(3)   Y
C22     IR      P       C18     .       .       .       .         -178.6(3)   Y
C25     IR      P       C18     .       .       .       .         -132.2(3)   Y
C24     IR      P       C18     .       .       .       .          141.2(4)   Y
S1      IR      P       C18     .       .       .       .           54.4(2)   Y
S2      IR      P       C18     .       .       .       .          -41.9(2)   Y
C11     N10     C10     S10     .       .       .       .            0.9(7)   Y
C11     N10     C10     S1      .       .       .       .         -179.8(3)   Y
IR      S1      C10     N10     .       .       .       .           17.7(3)   Y
IR      S1      C10     S10     .       .       .       .       -162.87(16)   Y
C10     N10     C11     C12     .       .       .       .         -161.7(4)   Y
C10     N10     C11     C16     .       .       .       .           18.9(7)   Y
C16     C11     C12     C13     .       .       .       .            1.4(7)   Y
N10     C11     C12     C13     .       .       .       .         -178.0(4)   Y
C11     C12     C13     C14     .       .       .       .           -1.2(8)   Y
C12     C13     C14     C15     .       .       .       .            0.7(8)   Y
C12     C13     C14     C17     .       .       .       .          179.3(5)   Y
C13     C14     C15     C16     .       .       .       .           -0.5(7)   Y
C17     C14     C15     C16     .       .       .       .         -179.1(5)   Y
C12     C11     C16     C15     .       .       .       .           -1.1(7)   Y
N10     C11     C16     C15     .       .       .       .          178.3(4)   Y
C14     C15     C16     C11     .       .       .       .            0.7(7)   Y
C23     IR      C21     C22     .       .       .       .           37.3(3)   Y
C25     IR      C21     C22     .       .       .       .          115.9(4)   Y
C24     IR      C21     C22     .       .       .       .           79.9(3)   Y
P       IR      C21     C22     .       .       .       .          -72.3(3)   Y
S1      IR      C21     C22     .       .       .       .           64.5(5)   Y
S2      IR      C21     C22     .       .       .       .         -163.3(2)   Y
C23     IR      C21     C25     .       .       .       .          -78.5(3)   Y
C22     IR      C21     C25     .       .       .       .         -115.9(4)   Y
C24     IR      C21     C25     .       .       .       .          -35.9(3)   Y
P       IR      C21     C25     .       .       .       .          171.9(2)   Y
S1      IR      C21     C25     .       .       .       .          -51.4(5)   Y
S2      IR      C21     C25     .       .       .       .           80.8(3)   Y
C23     IR      C21     C26     .       .       .       .          158.4(6)   Y
C22     IR      C21     C26     .       .       .       .          121.0(7)   Y
C25     IR      C21     C26     .       .       .       .         -123.1(7)   Y
C24     IR      C21     C26     .       .       .       .         -159.0(6)   Y
P       IR      C21     C26     .       .       .       .           48.8(6)   Y
S1      IR      C21     C26     .       .       .       .         -174.4(4)   Y
S2      IR      C21     C26     .       .       .       .          -42.3(6)   Y
C25     C21     C22     C23     .       .       .       .            4.7(5)   Y
C26     C21     C22     C23     .       .       .       .          172.8(4)   Y
IR      C21     C22     C23     .       .       .       .          -60.3(3)   Y
C25     C21     C22     C27     .       .       .       .         -169.8(4)   Y
C26     C21     C22     C27     .       .       .       .           -1.7(7)   Y
IR      C21     C22     C27     .       .       .       .          125.3(5)   Y
C25     C21     C22     IR      .       .       .       .           65.0(3)   Y
C26     C21     C22     IR      .       .       .       .         -127.0(5)   Y
C23     IR      C22     C21     .       .       .       .         -118.1(4)   Y
C25     IR      C22     C21     .       .       .       .          -38.4(3)   Y
C24     IR      C22     C21     .       .       .       .          -79.6(3)   Y
P       IR      C22     C21     .       .       .       .          118.4(3)   Y
S1      IR      C22     C21     .       .       .       .         -151.3(2)   Y
S2      IR      C22     C21     .       .       .       .           24.2(3)   Y
C21     IR      C22     C23     .       .       .       .          118.1(4)   Y
C25     IR      C22     C23     .       .       .       .           79.7(3)   Y
C24     IR      C22     C23     .       .       .       .           38.5(3)   Y
P       IR      C22     C23     .       .       .       .         -123.5(3)   Y
S1      IR      C22     C23     .       .       .       .          -33.2(3)   Y
S2      IR      C22     C23     .       .       .       .          142.2(2)   Y
C21     IR      C22     C27     .       .       .       .         -122.3(6)   Y
C23     IR      C22     C27     .       .       .       .          119.6(6)   Y
C25     IR      C22     C27     .       .       .       .         -160.7(6)   Y
C24     IR      C22     C27     .       .       .       .          158.0(6)   Y
P       IR      C22     C27     .       .       .       .           -3.9(5)   Y
S1      IR      C22     C27     .       .       .       .           86.4(5)   Y
S2      IR      C22     C27     .       .       .       .          -98.2(5)   Y
C21     C22     C23     C24     .       .       .       .           -4.6(5)   Y
C27     C22     C23     C24     .       .       .       .          170.0(4)   Y
IR      C22     C23     C24     .       .       .       .          -64.9(3)   Y
C21     C22     C23     C28     .       .       .       .         -176.6(4)   Y
C27     C22     C23     C28     .       .       .       .           -2.0(7)   Y
IR      C22     C23     C28     .       .       .       .          123.1(5)   Y
C21     C22     C23     IR      .       .       .       .           60.3(3)   Y
C27     C22     C23     IR      .       .       .       .         -125.1(5)   Y
C21     IR      C23     C22     .       .       .       .          -37.1(3)   Y
C25     IR      C23     C22     .       .       .       .          -79.6(3)   Y
C24     IR      C23     C22     .       .       .       .         -115.7(4)   Y
P       IR      C23     C22     .       .       .       .           67.8(3)   Y
S1      IR      C23     C22     .       .       .       .          154.1(3)   Y
S2      IR      C23     C22     .       .       .       .          -92.4(4)   Y
C21     IR      C23     C24     .       .       .       .           78.6(3)   Y
C22     IR      C23     C24     .       .       .       .          115.7(4)   Y
C25     IR      C23     C24     .       .       .       .           36.1(3)   Y
P       IR      C23     C24     .       .       .       .         -176.5(2)   Y
S1      IR      C23     C24     .       .       .       .          -90.2(2)   Y
S2      IR      C23     C24     .       .       .       .           23.3(4)   Y
C21     IR      C23     C28     .       .       .       .         -159.8(5)   Y
C22     IR      C23     C28     .       .       .       .         -122.7(6)   Y
C25     IR      C23     C28     .       .       .       .          157.7(5)   Y
C24     IR      C23     C28     .       .       .       .          121.6(6)   Y
P       IR      C23     C28     .       .       .       .          -54.9(5)   Y
S1      IR      C23     C28     .       .       .       .           31.4(5)   Y
S2      IR      C23     C28     .       .       .       .          144.9(4)   Y
C22     C23     C24     C25     .       .       .       .            2.8(5)   Y
C28     C23     C24     C25     .       .       .       .          174.9(4)   Y
IR      C23     C24     C25     .       .       .       .          -61.5(3)   Y
C22     C23     C24     C29     .       .       .       .         -173.0(4)   Y
C28     C23     C24     C29     .       .       .       .           -0.9(7)   Y
IR      C23     C24     C29     .       .       .       .          122.6(4)   Y
C22     C23     C24     IR      .       .       .       .           64.3(3)   Y
C28     C23     C24     IR      .       .       .       .         -123.5(4)   Y
C21     IR      C24     C25     .       .       .       .           37.2(3)   Y
C23     IR      C24     C25     .       .       .       .          118.4(4)   Y
C22     IR      C24     C25     .       .       .       .           79.8(3)   Y
P       IR      C24     C25     .       .       .       .          125.8(3)   Y
S1      IR      C24     C25     .       .       .       .         -149.3(3)   Y
S2      IR      C24     C25     .       .       .       .          -50.7(3)   Y
C21     IR      C24     C23     .       .       .       .          -81.2(3)   Y
C22     IR      C24     C23     .       .       .       .          -38.6(3)   Y
C25     IR      C24     C23     .       .       .       .         -118.4(4)   Y
P       IR      C24     C23     .       .       .       .            7.3(4)   Y
S1      IR      C24     C23     .       .       .       .           92.3(2)   Y
S2      IR      C24     C23     .       .       .       .         -169.1(2)   Y
C21     IR      C24     C29     .       .       .       .          162.0(6)   Y
C23     IR      C24     C29     .       .       .       .         -116.8(6)   Y
C22     IR      C24     C29     .       .       .       .         -155.3(6)   Y
C25     IR      C24     C29     .       .       .       .          124.8(6)   Y
P       IR      C24     C29     .       .       .       .         -109.4(5)   Y
S1      IR      C24     C29     .       .       .       .          -24.4(5)   Y
S2      IR      C24     C29     .       .       .       .           74.2(5)   Y
C23     C24     C25     C21     .       .       .       .            0.1(5)   Y
C29     C24     C25     C21     .       .       .       .          175.7(4)   Y
IR      C24     C25     C21     .       .       .       .          -59.7(3)   Y
C23     C24     C25     C30     .       .       .       .         -178.5(5)   Y
C29     C24     C25     C30     .       .       .       .           -2.9(8)   Y
IR      C24     C25     C30     .       .       .       .          121.6(5)   Y
C23     C24     C25     IR      .       .       .       .           59.8(3)   Y
C29     C24     C25     IR      .       .       .       .         -124.6(5)   Y
C22     C21     C25     C24     .       .       .       .           -3.0(5)   Y
C26     C21     C25     C24     .       .       .       .         -170.9(4)   Y
IR      C21     C25     C24     .       .       .       .           61.4(3)   Y
C22     C21     C25     C30     .       .       .       .          175.6(5)   Y
C26     C21     C25     C30     .       .       .       .            7.7(8)   Y
IR      C21     C25     C30     .       .       .       .         -119.9(5)   Y
C22     C21     C25     IR      .       .       .       .          -64.4(3)   Y
C26     C21     C25     IR      .       .       .       .          127.7(5)   Y
C21     IR      C25     C24     .       .       .       .         -118.7(4)   Y
C23     IR      C25     C24     .       .       .       .          -37.4(3)   Y
C22     IR      C25     C24     .       .       .       .          -80.4(3)   Y
P       IR      C25     C24     .       .       .       .         -134.2(3)   Y
S1      IR      C25     C24     .       .       .       .           37.8(3)   Y
S2      IR      C25     C24     .       .       .       .          137.2(3)   Y
C23     IR      C25     C21     .       .       .       .           81.3(3)   Y
C22     IR      C25     C21     .       .       .       .           38.3(3)   Y
C24     IR      C25     C21     .       .       .       .          118.7(4)   Y
P       IR      C25     C21     .       .       .       .          -15.5(4)   Y
S1      IR      C25     C21     .       .       .       .          156.6(2)   Y
S2      IR      C25     C21     .       .       .       .         -104.1(3)   Y
C21     IR      C25     C30     .       .       .       .          120.0(6)   Y
C23     IR      C25     C30     .       .       .       .         -158.7(6)   Y
C22     IR      C25     C30     .       .       .       .          158.4(6)   Y
C24     IR      C25     C30     .       .       .       .         -121.2(7)   Y
P       IR      C25     C30     .       .       .       .          104.5(5)   Y
S1      IR      C25     C30     .       .       .       .          -83.4(5)   Y
S2      IR      C25     C30     .       .       .       .           16.0(5)   Y

loop_                                         
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10   H10   S2       0.96(5)     2.34(5)    3.275(3)      165(4) .       
S2    H2    S2       0.99(9)     3.16(9)    4.064(2)      152(7) 2_566   



_diffrn_measured_fraction_theta_max    0.958 
_diffrn_reflns_theta_full              72.69 
_diffrn_measured_fraction_theta_full   0.958 
_refine_diff_density_max    1.028 
_refine_diff_density_min   -0.640 
_refine_diff_density_rms    0.115 
