 
#==============================================================================
data_global
#==============================================================================
 
# 0. AUDIT DETAILS
 
_audit_creation_date                              'Friday, 9 February 2018 '
_audit_creation_method                            'PLATON <TABLE ACC> option'
_audit_update_record
;
;
 
#===============================================================================
 
# 1. SUBMISSION DETAILS
 
_publ_contact_author_name
;
'Thomas Strassner'
;
_publ_contact_author_address
;
Fakultät Chemie und Lebensmittelchemie
Professur fuer Physikalische Organische Chemie
TU Dresden
01062 Dresden	
Germany
;
 
_publ_contact_author_email          
'thomas.strassner@chemie.tu-dresden.de'      
_publ_contact_author_fax                          '+49 351 463 39679'
_publ_contact_author_phone                        '+49 351 463 38571'

_publ_requested_category                          ?
_publ_requested_coeditor_name                     ?
 
_publ_contact_letter                             # Include date of submission
;
;
 
#===============================================================================
 
# 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY)
 
 
#===============================================================================
 
# 3. TITLE AND AUTHOR LIST
 
_publ_section_title
;
Enhanced quantum yields by sterically demanding aryl 
substituted β-diketonate ancillary ligands
;
_publ_section_title_footnote
;
;
 
 
 
loop_
_publ_author_name
_publ_author_address
'Pittkowski, Rebecca'
;Fakultät Chemie und Lebensmittelchemie
Professur fuer Physikalische Organische Chemie
TU Dresden
01062 Dresden	
Germany
;
'Strassner, Thomas'
;Fakultätung Chemie und Lebensmittelchemie
Professur fuer Physikalische Organische Chemie
TU Dresden
01062 Dresden	
Germany
;
 
#===============================================================================
 
# 4. TEXT
 
_publ_section_synopsis
;
 ?
;
_publ_section_abstract
;
 Luminescent organometallic platinum(II) compounds are of interest 
as phosphors for organic light emitting devices. Their emissive 
properties can be tuned by variation of the ligands or by specific 
electron-withdrawing or -donating substituents. Different ancillary 
ligands can have a profound impact on the emission color and emission 
efficiency of these complexes. We studied the influence of sterically 
hindered, aryl substituted β-diketonates on the emission properties 
of CĈ* cyclometalated complexes employing the original ligand, 
the unsubstituted methyl-phenyl-imidazolium ligand. 
The quantum yield was significantly enhanced by changing the 
auxiliary ligand from acetylacetonate, where the corresponding 
platinum(II) complex shows only a very weak emission, to mesityl(mes) 
or duryl(dur) substituted acetylacetonates. The new complexes 
show very efficient emission with quantum yields > 70% in the 
sky-blue spectral region (480 nm) and short decay times (< 3μs). 
;
  
_publ_section_comment
;
;
_publ_section_exptl_prep
;
 The crystal was fixed on the top of a MiTeGen MicroMount with
 perfluorinated ether and transferred to the diffractometer.
;
_publ_section_exptl_refinement
;
 ?
;
 
_publ_section_references
;
 Allen, F.H. (2002).
   Acta Cryst. B58, 380-388.
 
 Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C.
   Guagliardi, A., Moliterni, A.G.G., Polidori, G. & Spagna, R.
   (1999) J. Appl. Cryst. 32, 115-119.
 
 Beurskens, P.T., Beurskens, G., de Gelder, R., García-Granda, S.,
 Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF99 Program System,
   Technical Report of the Crystallography Laboratory,
   University of Nijmegen, The Netherlands.
 
 Boer, J.L. de & Duisenberg, A.J.M. (1984). Acta Cryst. A40, C-410.
 
 Boeyens, J.C.A. (1978). J.Cryst.Mol.Struct. 8, 317-320.
 
 Cremer, D. & Pople, J.A. (1975). J. Am. Chem. Soc. 97, 1354-1358.
 
 Duisenberg, A.J.M. (1992). J. Appl. Cryst. 25, 92-96.
 
 Duisenberg, A.J.M., Kroon-Batenburg, L.M.J. & Schreurs, A.M.M. (2003).
   J. Appl. Cryst. 36, 220-229.
 
 Enraf-Nonius (1989). CAD-4 Software. Version 5. Enraf-Nonius, Delft,
   The Netherlands.
 
 Flack, H.D. (1983). Acta Cryst. A39, 876-881.
 
 Hooft, R.W.W. (1998). Collect Software, Nonius B.V., Delft, The Netherlands.
 
 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269.
 
 Mackay, A.L. (1984). Acta Cryst. A40, 165-166.
 
 Meulenaer, J. de & Tompa, H. (1965). Acta Cryst. 19, 1014-1018.
 
 North, A.C.T., Phillips, D.C. & Mathews, F.S. (1968).
  Acta Cryst. A24, 351-359.
 
 Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
   Macromolecular Crystallography, Part A, edited by C.W. Carter &
    R.M. Sweet, pp. 307-326. London: Academic Press.
 
 Sheldrick, G.M. (1986). SHELXS86. University of Göttingen, Germany.
 
 Sheldrick, G.M. (1993). SHELXL93. University of Göttingen, Germany.
 
 Sheldrick, G.M. (1997). SHELXS97. University of Göttingen, Germany.
 
 Sheldrick, G.M. (1997). SHELXL97. University of Göttingen, Germany.
 
 Sluis, P. van der & Spek, A.L. (1990). Acta Cryst. A46, 194-201.
 
 Spek, A.L. (1987). Acta Cryst. C43, 1233-1235.
 
 Spek, A.L. (1988). J. Appl. Cryst. 21, 578-579.
 
 Spek, A.L. (1994). Am. Crystallogr. Assoc.-Abstracts, 22, 66.
 
 Spek, A.L. (1997). HELENA, Program for Datareduction, Utrecht
   University, The Netherlands.
 
 Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
 
 Wilson, A.J.C. (1992). Ed. International Tables for Crystallography,
   Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands.
;
_publ_section_acknowledgements
;
;
_publ_section_figure_captions
; 
;
 
#===============================================================================
 
data_rp47_pl
 
#===============================================================================
 
# 5. CHEMICAL DATA
 
_chemical_name_systematic
;
;
_chemical_name_common                             ?
_chemical_melting_point                           ?
_chemical_formula_moiety
'C33 H36 N2 O2 Pt'
_chemical_formula_structural                      ?
_chemical_formula_sum
'C33 H36 N2 O2 Pt'
_chemical_formula_iupac                           ?
_chemical_formula_weight                             687.72
_chemical_compound_source                        '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    0.0033    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'
Pt  Pt   -1.7033    8.3905
' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
#===============================================================================
 
# 6. CRYSTAL DATA
 
_symmetry_cell_setting                              monoclinic
_symmetry_space_group_name_Hall                   '-P 2yn'
_symmetry_space_group_name_H-M                    'P 21/n'
_symmetry_Int_Tables_number                              14
 
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
   1 x,y,z
   2 1/2-x,1/2+y,1/2-z
   3 -x,-y,-z
   4 1/2+x,1/2-y,1/2+z
 
_cell_length_a                                       9.8385(19)
_cell_length_b                                        27.837(6)
_cell_length_c                                        11.285(2)
_cell_angle_alpha                                            90
_cell_angle_beta                                     110.846(7)
_cell_angle_gamma                                            90
_cell_volume                                         2888.4(10)
_cell_formula_units_Z                                 4
_cell_measurement_temperature                       100
_cell_measurement_reflns_used                     839
_cell_measurement_theta_min                       0.1
_cell_measurement_theta_max                       60.0
_cell_special_details
;
;
 
_exptl_crystal_description                       'fragment'
_exptl_crystal_colour                            'orange'
 
_exptl_crystal_size_max                           0.908
_exptl_crystal_size_mid                           0.874
_exptl_crystal_size_min                           0.518
_exptl_crystal_size_rad                           ?
_exptl_crystal_density_meas                       ?
_exptl_crystal_density_diffrn                         1.582
_exptl_crystal_density_method                    'Not Measured'
_exptl_crystal_F_000                                   1368
_exptl_absorpt_coefficient_mu                         4.889
_exptl_crystal_density_meas_temp                  ?
 
_exptl_absorpt_correction_type                   'multi-scan'
_exptl_absorpt_process_details                   'SADABS (Bruker)'
_exptl_absorpt_correction_T_min                   0.281
_exptl_absorpt_correction_T_max                   0.745
 
#===============================================================================
 
# 7. EXPERIMENTAL DATA
 
_exptl_special_details
;
Diffraction operator				T. Strassner
scanspeed					4 s per frame
dx						37 mm
4170 frames measured in 23 data sets
phi-scans with delta_phi         = 0.5 
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature                         100
_diffrn_detector                  'Bruker Photon II detector'
_diffrn_detector_type             'Charge-Integrating Pixel Array Detector'
_diffrn_radiation_wavelength                        0.71073
_diffrn_radiation_probe                           'x-ray'
_diffrn_radiation_type                            'MoK\a'
_diffrn_radiation_source                          'sealed X-ray tube'
_diffrn_radiation_monochromator                   'Multilayer'
 
_diffrn_measurement_device_type                   'Bruker Photon II detector'
_diffrn_measurement_method                        'φ and ω scans'

_diffrn_reflns_number                            209519
_diffrn_reflns_av_R_equivalents                    0.0800
_diffrn_reflns_av_unetI/netI                       0.0205
_diffrn_reflns_limit_h_min                          -12
_diffrn_reflns_limit_h_max                           12
_diffrn_reflns_limit_k_min                          -36
_diffrn_reflns_limit_k_max                           36
_diffrn_reflns_limit_l_min                          -14
_diffrn_reflns_limit_l_max                           14
_diffrn_reflns_theta_min                           2.33
_diffrn_reflns_theta_max                          27.53
_diffrn_reflns_theta_full                         25.24
_diffrn_measured_fraction_theta_max               0.996
_diffrn_measured_fraction_theta_full              0.998
_diffrn_reflns_reduction_process
;
;
 
# number of unique reflections
_reflns_number_total                                 6641
# number of observed reflections (> n sig(I))
_reflns_number_gt                                    6282
_reflns_threshold_expression                      I>2σ(I)
 
_computing_data_collection                     'Bruker APEX3'
_computing_cell_refinement                     'SAINT (Bruker)'
_computing_data_reduction                      'SAINT (Bruker)'
_computing_structure_solution                  'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement                'SHELXT 2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics                  ?
_computing_publication_material                'PLATON (Spek, 2003)'
 
#===============================================================================
 
# 8. REFINEMENT DATA
 
_refine_special_details
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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
'W=1/[Σ²(FO²)+(0.0120P)²+7.0561P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary                     '?'
_atom_sites_solution_secondary                   '?'
_atom_sites_solution_hydrogens                   'geom'
 

_refine_ls_hydrogen_treatment                    'constr'
 
_refine_ls_extinction_method                      'none'
_refine_ls_abs_structure_details                  ?
_refine_ls_abs_structure_Flack                   .
_refine_ls_number_reflns                               6641
_refine_ls_number_parameters                            352
_refine_ls_number_restraints                              0
_refine_ls_number_constraints                     ?
_refine_ls_R_factor_all                              0.0271
_refine_ls_R_factor_gt                               0.0251
_refine_ls_wR_factor_ref                             0.0591
_refine_ls_wR_factor_gt                              0.0580
_refine_ls_goodness_of_fit_ref                        1.162
_refine_ls_restrained_S_all                           1.162
_refine_ls_shift/su_max                               0.004
_refine_ls_shift/su_mean                              0.000
_refine_diff_density_max                              1.780
_refine_diff_density_min                             -1.257
_refine_diff_density_rms                              0.093
 
#===============================================================================
 
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
 
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt Uani 0.04064(2) 0.33239(2) 0.88050(2) 1.000 0.0242(1) d . . .
O1 O Uani 0.1376(3) 0.34169(8) 0.7448(2) 1.000 0.0296(7) d . . .
O2 O Uani 0.1640(2) 0.38697(8) 0.9871(2) 1.000 0.0296(7) d . . .
N1 N Uani -0.1617(3) 0.25881(10) 0.8687(3) 1.000 0.0288(8) d . . .
N2 N Uani -0.1191(3) 0.25123(10) 0.6959(3) 1.000 0.0308(8) d . . .
C1 C Uani -0.0841(3) 0.27811(11) 0.8018(3) 1.000 0.0268(9) d . . .
C2 C Uani -0.2173(4) 0.21558(13) 0.6973(4) 1.000 0.0368(10) d . . .
C3 C Uani -0.2439(4) 0.22031(12) 0.8049(4) 1.000 0.0359(10) d . . .
C4 C Uani -0.0718(4) 0.25974(14) 0.5886(4) 1.000 0.0377(11) d . . .
C5 C Uani -0.1483(3) 0.28207(11) 0.9840(3) 1.000 0.0278(9) d . . .
C6 C Uani -0.0537(3) 0.32140(11) 1.0074(3) 1.000 0.0263(9) d . . .
C7 C Uani -0.0346(4) 0.34747(12) 1.1173(3) 1.000 0.0325(10) d . . .
C8 C Uani -0.1057(4) 0.33420(13) 1.1997(4) 1.000 0.0343(11) d . . .
C9 C Uani -0.1975(4) 0.29469(14) 1.1727(4) 1.000 0.0385(11) d . . .
C10 C Uani -0.2202(4) 0.26804(13) 1.0631(4) 1.000 0.0353(10) d . . .
C11 C Uani 0.2342(3) 0.37337(11) 0.7529(3) 1.000 0.0263(9) d . . .
C12 C Uani 0.2956(4) 0.40607(12) 0.8519(3) 1.000 0.0299(9) d . . .
C13 C Uani 0.2599(3) 0.41102(11) 0.9596(3) 1.000 0.0261(8) d . . .
C14 C Uani 0.2840(3) 0.37658(11) 0.6420(3) 1.000 0.0252(8) d . . .
C15 C Uani 0.4098(3) 0.35222(11) 0.6453(3) 1.000 0.0281(9) d . . .
C16 C Uani 0.4564(4) 0.35808(12) 0.5422(3) 1.000 0.0310(10) d . . .
C17 C Uani 0.3784(4) 0.38810(12) 0.4434(3) 1.000 0.0312(10) d . . .
C18 C Uani 0.2538(4) 0.41228(11) 0.4400(3) 1.000 0.0278(9) d . . .
C19 C Uani 0.2039(3) 0.40602(11) 0.5407(3) 1.000 0.0267(9) d . . .
C20 C Uani 0.4937(4) 0.32082(13) 0.7568(3) 1.000 0.0364(10) d . . .
C21 C Uani 0.5902(4) 0.33199(14) 0.5389(4) 1.000 0.0411(12) d . . .
C22 C Uani 0.1768(4) 0.44530(13) 0.3309(3) 1.000 0.0359(10) d . . .
C23 C Uani 0.0676(4) 0.43072(13) 0.5413(4) 1.000 0.0360(10) d . . .
C24 C Uani 0.3356(3) 0.44862(11) 1.0565(3) 1.000 0.0248(8) d . . .
C25 C Uani 0.4645(3) 0.43622(12) 1.1556(3) 1.000 0.0283(9) d . . .
C26 C Uani 0.5273(4) 0.46972(13) 1.2516(3) 1.000 0.0319(9) d . . .
C27 C Uani 0.4582(4) 0.51369(12) 1.2469(3) 1.000 0.0322(9) d . . .
C28 C Uani 0.3332(4) 0.52651(12) 1.1480(3) 1.000 0.0321(10) d . . .
C29 C Uani 0.2717(3) 0.49400(12) 1.0491(3) 1.000 0.0294(9) d . . .
C30 C Uani 0.5348(4) 0.38768(14) 1.1568(4) 1.000 0.0397(11) d . . .
C31 C Uani 0.6679(4) 0.45919(16) 1.3591(4) 1.000 0.0464(11) d . . .
C32 C Uani 0.2641(5) 0.57491(14) 1.1484(4) 1.000 0.0507(14) d . . .
C33 C Uani 0.1427(4) 0.50842(14) 0.9341(4) 1.000 0.0407(11) d . . .
H2 H Uiso -0.25808 0.19210 0.63333 1.000 0.0440 c RU . .
H3 H Uiso -0.30691 0.20100 0.83210 1.000 0.0430 c RU . .
H4A H Uiso -0.15658 0.26708 0.51285 1.000 0.0560 c RU . .
H4B H Uiso -0.02324 0.23094 0.57318 1.000 0.0560 c RU . .
H4C H Uiso -0.00400 0.28688 0.60783 1.000 0.0560 c RU . .
H7 H Uiso 0.02763 0.37471 1.13666 1.000 0.0390 c RU . .
H8 H Uiso -0.09115 0.35234 1.27458 1.000 0.0410 c RU . .
H9 H Uiso -0.24501 0.28576 1.22940 1.000 0.0460 c RU . .
H10 H Uiso -0.28337 0.24103 1.04337 1.000 0.0420 c RU . .
H12 H Uiso 0.36873 0.42688 0.84452 1.000 0.0360 c RU . .
H17 H Uiso 0.41187 0.39231 0.37479 1.000 0.0370 c RU . .
H20A H Uiso 0.50591 0.28872 0.72636 1.000 0.0550 c RU . .
H20B H Uiso 0.44017 0.31835 0.81504 1.000 0.0550 c RU . .
H20C H Uiso 0.58951 0.33506 0.80134 1.000 0.0550 c RU . .
H21A H Uiso 0.60268 0.33842 0.45798 1.000 0.0620 c RU . .
H21B H Uiso 0.57844 0.29737 0.54776 1.000 0.0620 c RU . .
H21C H Uiso 0.67605 0.34331 0.60877 1.000 0.0620 c RU . .
H22A H Uiso 0.22019 0.44213 0.26549 1.000 0.0540 c RU . .
H22B H Uiso 0.18648 0.47857 0.36122 1.000 0.0540 c RU . .
H22C H Uiso 0.07354 0.43667 0.29518 1.000 0.0540 c RU . .
H23A H Uiso 0.06627 0.46390 0.51184 1.000 0.0540 c RU . .
H23B H Uiso 0.06600 0.43073 0.62758 1.000 0.0540 c RU . .
H23C H Uiso -0.01784 0.41357 0.48473 1.000 0.0540 c RU . .
H27 H Uiso 0.49857 0.53578 1.31450 1.000 0.0390 c RU . .
H30A H Uiso 0.47252 0.36829 1.08572 1.000 0.0600 c RU . .
H30B H Uiso 0.54747 0.37121 1.23676 1.000 0.0600 c RU . .
H30C H Uiso 0.62990 0.39217 1.14864 1.000 0.0600 c RU . .
H31A H Uiso 0.74464 0.45269 1.32481 1.000 0.0700 c RU . .
H31B H Uiso 0.65504 0.43106 1.40626 1.000 0.0700 c RU . .
H31C H Uiso 0.69533 0.48698 1.41601 1.000 0.0700 c RU . .
H32A H Uiso 0.27154 0.59455 1.07889 1.000 0.0760 c RU . .
H32B H Uiso 0.31446 0.59106 1.22937 1.000 0.0760 c RU . .
H32C H Uiso 0.16142 0.57053 1.13720 1.000 0.0760 c RU . .
H33A H Uiso 0.17627 0.52749 0.87683 1.000 0.0610 c RU . .
H33B H Uiso 0.07527 0.52758 0.96099 1.000 0.0610 c RU . .
H33C H Uiso 0.09302 0.47954 0.88998 1.000 0.0610 c RU . .
 
 
#===============================================================================
 
# 10. MOLECULAR GEOMETRY
 
_geom_special_details
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;
 
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
 Pt1     O1         2.089(3)                     .       .                   yes
 Pt1     O2         2.047(2)                     .       .                   yes
 Pt1     C1         1.950(3)                     .       .                   yes
 Pt1     C6         1.988(3)                     .       .                   yes
 O1      C11        1.276(4)                     .       .                   yes
 O2      C13        1.282(4)                     .       .                   yes
 N1      C1         1.361(4)                     .       .                   yes
 N1      C3         1.381(5)                     .       .                   yes
 N1      C5         1.417(4)                     .       .                   yes
 N2      C1         1.347(4)                     .       .                   yes
 N2      C2         1.389(5)                     .       .                   yes
 N2      C4         1.463(5)                     .       .                   yes
 C2      C3         1.337(6)                     .       .                   no
 C5      C6         1.400(4)                     .       .                   no
 C5      C10        1.378(5)                     .       .                   no
 C6      C7         1.391(5)                     .       .                   no
 C7      C8         1.398(6)                     .       .                   no
 C8      C9         1.387(6)                     .       .                   no
 C9      C10        1.391(6)                     .       .                   no
 C11     C12        1.401(5)                     .       .                   no
 C11     C14        1.500(4)                     .       .                   no
 C12     C13        1.387(5)                     .       .                   no
 C13     C24        1.505(4)                     .       .                   no
 C14     C15        1.400(4)                     .       .                   no
 C14     C19        1.399(4)                     .       .                   no
 C15     C16        1.404(5)                     .       .                   no
 C15     C20        1.513(5)                     .       .                   no
 C16     C17        1.386(5)                     .       .                   no
 C16     C21        1.516(6)                     .       .                   no
 C17     C18        1.387(6)                     .       .                   no
 C18     C19        1.400(5)                     .       .                   no
 C18     C22        1.507(5)                     .       .                   no
 C19     C23        1.509(5)                     .       .                   no
 C24     C25        1.403(5)                     .       .                   no
 C24     C29        1.400(5)                     .       .                   no
 C25     C26        1.396(5)                     .       .                   no
 C25     C30        1.516(5)                     .       .                   no
 C26     C27        1.392(5)                     .       .                   no
 C26     C31        1.509(6)                     .       .                   no
 C27     C28        1.382(5)                     .       .                   no
 C28     C29        1.397(5)                     .       .                   no
 C28     C32        1.510(5)                     .       .                   no
 C29     C33        1.511(5)                     .       .                   no
 C2      H2           0.9500                     .       .                   no
 C3      H3           0.9500                     .       .                   no
 C4      H4A          0.9800                     .       .                   no
 C4      H4B          0.9800                     .       .                   no
 C4      H4C          0.9800                     .       .                   no
 C7      H7           0.9500                     .       .                   no
 C8      H8           0.9500                     .       .                   no
 C9      H9           0.9500                     .       .                   no
 C10     H10          0.9500                     .       .                   no
 C12     H12          0.9500                     .       .                   no
 C17     H17          0.9500                     .       .                   no
 C20     H20A         0.9800                     .       .                   no
 C20     H20B         0.9800                     .       .                   no
 C20     H20C         0.9800                     .       .                   no
 C21     H21A         0.9800                     .       .                   no
 C21     H21B         0.9800                     .       .                   no
 C21     H21C         0.9800                     .       .                   no
 C22     H22A         0.9800                     .       .                   no
 C22     H22B         0.9800                     .       .                   no
 C22     H22C         0.9800                     .       .                   no
 C23     H23A         0.9800                     .       .                   no
 C23     H23B         0.9800                     .       .                   no
 C23     H23C         0.9800                     .       .                   no
 C27     H27          0.9500                     .       .                   no
 C30     H30A         0.9800                     .       .                   no
 C30     H30B         0.9800                     .       .                   no
 C30     H30C         0.9800                     .       .                   no
 C31     H31A         0.9800                     .       .                   no
 C31     H31B         0.9800                     .       .                   no
 C31     H31C         0.9800                     .       .                   no
 C32     H32A         0.9800                     .       .                   no
 C32     H32B         0.9800                     .       .                   no
 C32     H32C         0.9800                     .       .                   no
 C33     H33A         0.9800                     .       .                   no
 C33     H33B         0.9800                     .       .                   no
 C33     H33C         0.9800                     .       .                   no
 
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
 O1      Pt1     O2         90.51(9)             .       .       .           yes
 O1      Pt1     C1        98.03(11)             .       .       .           yes
 O1      Pt1     C6       178.12(11)             .       .       .           yes
 O2      Pt1     C1       171.24(11)             .       .       .           yes
 O2      Pt1     C6        91.26(11)             .       .       .           yes
 C1      Pt1     C6        80.17(13)             .       .       .           yes
 Pt1     O1      C11        123.8(2)             .       .       .           yes
 Pt1     O2      C13        125.4(2)             .       .       .           yes
 C1      N1      C3         110.9(3)             .       .       .           yes
 C1      N1      C5         116.2(3)             .       .       .           yes
 C3      N1      C5         132.8(3)             .       .       .           yes
 C1      N2      C2         110.3(3)             .       .       .           yes
 C1      N2      C4         126.0(3)             .       .       .           yes
 C2      N2      C4         123.5(3)             .       .       .           yes
 Pt1     C1      N1         116.1(2)             .       .       .           yes
 Pt1     C1      N2         139.1(3)             .       .       .           yes
 N1      C1      N2         104.8(3)             .       .       .           yes
 N2      C2      C3         107.6(3)             .       .       .           yes
 N1      C3      C2         106.4(3)             .       .       .           yes
 N1      C5      C6         111.7(3)             .       .       .           yes
 N1      C5      C10        124.3(3)             .       .       .           yes
 C6      C5      C10        124.0(3)             .       .       .           no
 Pt1     C6      C5         115.7(2)             .       .       .           yes
 Pt1     C6      C7         127.8(3)             .       .       .           yes
 C5      C6      C7         116.5(3)             .       .       .           no
 C6      C7      C8         121.0(3)             .       .       .           no
 C7      C8      C9         120.3(4)             .       .       .           no
 C8      C9      C10        120.3(4)             .       .       .           no
 C5      C10     C9         117.9(3)             .       .       .           no
 O1      C11     C12        127.3(3)             .       .       .           yes
 O1      C11     C14        116.0(3)             .       .       .           yes
 C12     C11     C14        116.8(3)             .       .       .           no
 C11     C12     C13        126.3(3)             .       .       .           no
 O2      C13     C12        126.7(3)             .       .       .           yes
 O2      C13     C24        113.8(3)             .       .       .           yes
 C12     C13     C24        119.4(3)             .       .       .           no
 C11     C14     C15        119.8(3)             .       .       .           no
 C11     C14     C19        117.4(3)             .       .       .           no
 C15     C14     C19        122.7(3)             .       .       .           no
 C14     C15     C16        117.9(3)             .       .       .           no
 C14     C15     C20        121.2(3)             .       .       .           no
 C16     C15     C20        120.9(3)             .       .       .           no
 C15     C16     C17        119.1(3)             .       .       .           no
 C15     C16     C21        120.5(3)             .       .       .           no
 C17     C16     C21        120.4(3)             .       .       .           no
 C16     C17     C18        123.1(3)             .       .       .           no
 C17     C18     C19        118.6(3)             .       .       .           no
 C17     C18     C22        120.1(3)             .       .       .           no
 C19     C18     C22        121.3(3)             .       .       .           no
 C14     C19     C18        118.5(3)             .       .       .           no
 C14     C19     C23        120.4(3)             .       .       .           no
 C18     C19     C23        121.1(3)             .       .       .           no
 C13     C24     C25        118.8(3)             .       .       .           no
 C13     C24     C29        119.2(3)             .       .       .           no
 C25     C24     C29        121.9(3)             .       .       .           no
 C24     C25     C26        118.6(3)             .       .       .           no
 C24     C25     C30        120.4(3)             .       .       .           no
 C26     C25     C30        120.9(3)             .       .       .           no
 C25     C26     C27        118.9(3)             .       .       .           no
 C25     C26     C31        121.3(3)             .       .       .           no
 C27     C26     C31        119.8(3)             .       .       .           no
 C26     C27     C28        122.7(3)             .       .       .           no
 C27     C28     C29        119.1(3)             .       .       .           no
 C27     C28     C32        120.0(3)             .       .       .           no
 C29     C28     C32        120.9(3)             .       .       .           no
 C24     C29     C28        118.6(3)             .       .       .           no
 C24     C29     C33        120.9(3)             .       .       .           no
 C28     C29     C33        120.5(3)             .       .       .           no
 N2      C2      H2           126.00             .       .       .           no
 C3      C2      H2           126.00             .       .       .           no
 N1      C3      H3           127.00             .       .       .           no
 C2      C3      H3           127.00             .       .       .           no
 N2      C4      H4A          109.00             .       .       .           no
 N2      C4      H4B          109.00             .       .       .           no
 N2      C4      H4C          109.00             .       .       .           no
 H4A     C4      H4B          109.00             .       .       .           no
 H4A     C4      H4C          109.00             .       .       .           no
 H4B     C4      H4C          109.00             .       .       .           no
 C6      C7      H7           120.00             .       .       .           no
 C8      C7      H7           119.00             .       .       .           no
 C7      C8      H8           120.00             .       .       .           no
 C9      C8      H8           120.00             .       .       .           no
 C8      C9      H9           120.00             .       .       .           no
 C10     C9      H9           120.00             .       .       .           no
 C5      C10     H10          121.00             .       .       .           no
 C9      C10     H10          121.00             .       .       .           no
 C11     C12     H12          117.00             .       .       .           no
 C13     C12     H12          117.00             .       .       .           no
 C16     C17     H17          118.00             .       .       .           no
 C18     C17     H17          118.00             .       .       .           no
 C15     C20     H20A         110.00             .       .       .           no
 C15     C20     H20B         110.00             .       .       .           no
 C15     C20     H20C         109.00             .       .       .           no
 H20A    C20     H20B         109.00             .       .       .           no
 H20A    C20     H20C         109.00             .       .       .           no
 H20B    C20     H20C         109.00             .       .       .           no
 C16     C21     H21A         109.00             .       .       .           no
 C16     C21     H21B         109.00             .       .       .           no
 C16     C21     H21C         109.00             .       .       .           no
 H21A    C21     H21B         109.00             .       .       .           no
 H21A    C21     H21C         109.00             .       .       .           no
 H21B    C21     H21C         109.00             .       .       .           no
 C18     C22     H22A         109.00             .       .       .           no
 C18     C22     H22B         109.00             .       .       .           no
 C18     C22     H22C         109.00             .       .       .           no
 H22A    C22     H22B         110.00             .       .       .           no
 H22A    C22     H22C         110.00             .       .       .           no
 H22B    C22     H22C         109.00             .       .       .           no
 C19     C23     H23A         109.00             .       .       .           no
 C19     C23     H23B         109.00             .       .       .           no
 C19     C23     H23C         109.00             .       .       .           no
 H23A    C23     H23B         110.00             .       .       .           no
 H23A    C23     H23C         109.00             .       .       .           no
 H23B    C23     H23C         110.00             .       .       .           no
 C26     C27     H27          119.00             .       .       .           no
 C28     C27     H27          119.00             .       .       .           no
 C25     C30     H30A         109.00             .       .       .           no
 C25     C30     H30B         109.00             .       .       .           no
 C25     C30     H30C         109.00             .       .       .           no
 H30A    C30     H30B         109.00             .       .       .           no
 H30A    C30     H30C         109.00             .       .       .           no
 H30B    C30     H30C         109.00             .       .       .           no
 C26     C31     H31A         109.00             .       .       .           no
 C26     C31     H31B         109.00             .       .       .           no
 C26     C31     H31C         109.00             .       .       .           no
 H31A    C31     H31B         109.00             .       .       .           no
 H31A    C31     H31C         109.00             .       .       .           no
 H31B    C31     H31C         109.00             .       .       .           no
 C28     C32     H32A         109.00             .       .       .           no
 C28     C32     H32B         109.00             .       .       .           no
 C28     C32     H32C         109.00             .       .       .           no
 H32A    C32     H32B         109.00             .       .       .           no
 H32A    C32     H32C         109.00             .       .       .           no
 H32B    C32     H32C         109.00             .       .       .           no
 C29     C33     H33A         109.00             .       .       .           no
 C29     C33     H33B         109.00             .       .       .           no
 C29     C33     H33C         109.00             .       .       .           no
 H33A    C33     H33B         109.00             .       .       .           no
 H33A    C33     H33C         109.00             .       .       .           no
 H33B    C33     H33C         109.00             .       .       .           no
 
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
 O2      Pt1     O1      C11         -0.5(3)     .       .       .       .   no
 C1      Pt1     O1      C11       -178.6(3)     .       .       .       .   no
 O1      Pt1     O2      C13         -1.5(2)     .       .       .       .   no
 C6      Pt1     O2      C13        177.9(3)     .       .       .       .   no
 O1      Pt1     C1      N1         176.0(2)     .       .       .       .   no
 O1      Pt1     C1      N2          -2.7(4)     .       .       .       .   no
 C6      Pt1     C1      N1          -3.5(2)     .       .       .       .   no
 C6      Pt1     C1      N2         177.9(4)     .       .       .       .   no
 O2      Pt1     C6      C5        -175.0(2)     .       .       .       .   no
 O2      Pt1     C6      C7           3.7(3)     .       .       .       .   no
 C1      Pt1     C6      C5           3.2(2)     .       .       .       .   no
 C1      Pt1     C6      C7        -178.2(3)     .       .       .       .   no
 Pt1     O1      C11     C12          2.0(5)     .       .       .       .   no
 Pt1     O1      C11     C14       -176.2(2)     .       .       .       .   no
 Pt1     O2      C13     C12          2.2(5)     .       .       .       .   no
 Pt1     O2      C13     C24     -179.13(19)     .       .       .       .   no
 C3      N1      C1      Pt1       -179.0(2)     .       .       .       .   no
 C3      N1      C1      N2           0.1(4)     .       .       .       .   no
 C5      N1      C1      Pt1          3.2(4)     .       .       .       .   no
 C5      N1      C1      N2        -177.7(3)     .       .       .       .   no
 C1      N1      C3      C2           0.0(4)     .       .       .       .   no
 C5      N1      C3      C2         177.2(4)     .       .       .       .   no
 C1      N1      C5      C6          -0.5(4)     .       .       .       .   no
 C1      N1      C5      C10        179.0(3)     .       .       .       .   no
 C3      N1      C5      C6        -177.6(4)     .       .       .       .   no
 C3      N1      C5      C10          1.9(6)     .       .       .       .   no
 C2      N2      C1      Pt1        178.7(3)     .       .       .       .   no
 C2      N2      C1      N1          -0.1(4)     .       .       .       .   no
 C4      N2      C1      Pt1         -6.0(6)     .       .       .       .   no
 C4      N2      C1      N1         175.3(3)     .       .       .       .   no
 C1      N2      C2      C3           0.1(4)     .       .       .       .   no
 C4      N2      C2      C3        -175.4(3)     .       .       .       .   no
 N2      C2      C3      N1          -0.1(4)     .       .       .       .   no
 N1      C5      C6      Pt1         -2.4(4)     .       .       .       .   no
 N1      C5      C6      C7         178.8(3)     .       .       .       .   no
 C10     C5      C6      Pt1        178.1(3)     .       .       .       .   no
 C10     C5      C6      C7          -0.7(5)     .       .       .       .   no
 N1      C5      C10     C9        -179.3(3)     .       .       .       .   no
 C6      C5      C10     C9           0.1(6)     .       .       .       .   no
 Pt1     C6      C7      C8        -177.9(3)     .       .       .       .   no
 C5      C6      C7      C8           0.8(5)     .       .       .       .   no
 C6      C7      C8      C9          -0.3(6)     .       .       .       .   no
 C7      C8      C9      C10         -0.3(6)     .       .       .       .   no
 C8      C9      C10     C5           0.4(6)     .       .       .       .   no
 O1      C11     C12     C13         -1.7(6)     .       .       .       .   no
 C14     C11     C12     C13        176.5(3)     .       .       .       .   no
 O1      C11     C14     C15        -95.8(4)     .       .       .       .   no
 O1      C11     C14     C19         86.9(4)     .       .       .       .   no
 C12     C11     C14     C15         85.8(4)     .       .       .       .   no
 C12     C11     C14     C19        -91.5(4)     .       .       .       .   no
 C11     C12     C13     O2          -0.6(6)     .       .       .       .   no
 C11     C12     C13     C24       -179.2(3)     .       .       .       .   no
 O2      C13     C24     C25         91.3(4)     .       .       .       .   no
 O2      C13     C24     C29        -85.3(4)     .       .       .       .   no
 C12     C13     C24     C25        -89.9(4)     .       .       .       .   no
 C12     C13     C24     C29         93.5(4)     .       .       .       .   no
 C11     C14     C15     C16       -177.0(3)     .       .       .       .   no
 C11     C14     C15     C20          2.6(5)     .       .       .       .   no
 C19     C14     C15     C16          0.2(5)     .       .       .       .   no
 C19     C14     C15     C20        179.8(3)     .       .       .       .   no
 C11     C14     C19     C18        175.6(3)     .       .       .       .   no
 C11     C14     C19     C23         -3.8(4)     .       .       .       .   no
 C15     C14     C19     C18         -1.6(5)     .       .       .       .   no
 C15     C14     C19     C23        178.9(3)     .       .       .       .   no
 C14     C15     C16     C17          1.2(5)     .       .       .       .   no
 C14     C15     C16     C21       -178.9(3)     .       .       .       .   no
 C20     C15     C16     C17       -178.4(3)     .       .       .       .   no
 C20     C15     C16     C21          1.5(5)     .       .       .       .   no
 C15     C16     C17     C18         -1.2(5)     .       .       .       .   no
 C21     C16     C17     C18        178.9(3)     .       .       .       .   no
 C16     C17     C18     C19         -0.2(5)     .       .       .       .   no
 C16     C17     C18     C22        178.5(3)     .       .       .       .   no
 C17     C18     C19     C14          1.6(5)     .       .       .       .   no
 C17     C18     C19     C23       -179.0(3)     .       .       .       .   no
 C22     C18     C19     C14       -177.1(3)     .       .       .       .   no
 C22     C18     C19     C23          2.3(5)     .       .       .       .   no
 C13     C24     C25     C26       -174.2(3)     .       .       .       .   no
 C13     C24     C25     C30          6.7(5)     .       .       .       .   no
 C29     C24     C25     C26          2.3(5)     .       .       .       .   no
 C29     C24     C25     C30       -176.8(3)     .       .       .       .   no
 C13     C24     C29     C28        172.1(3)     .       .       .       .   no
 C13     C24     C29     C33        -10.4(5)     .       .       .       .   no
 C25     C24     C29     C28         -4.4(5)     .       .       .       .   no
 C25     C24     C29     C33        173.0(3)     .       .       .       .   no
 C24     C25     C26     C27          1.4(5)     .       .       .       .   no
 C24     C25     C26     C31       -178.4(3)     .       .       .       .   no
 C30     C25     C26     C27       -179.6(3)     .       .       .       .   no
 C30     C25     C26     C31          0.7(5)     .       .       .       .   no
 C25     C26     C27     C28         -3.0(6)     .       .       .       .   no
 C31     C26     C27     C28        176.8(4)     .       .       .       .   no
 C26     C27     C28     C29          0.9(6)     .       .       .       .   no
 C26     C27     C28     C32       -179.7(4)     .       .       .       .   no
 C27     C28     C29     C24          2.8(5)     .       .       .       .   no
 C27     C28     C29     C33       -174.7(3)     .       .       .       .   no
 C32     C28     C29     C24       -176.7(3)     .       .       .       .   no
 C32     C28     C29     C33          5.9(5)     .       .       .       .   no
 
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
_geom_hbond_publ_flag
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
C4      H4C     O1          0.9800     2.2600   3.158(5)     151.00     .   yes
C7      H7      O2          0.9500     2.5300   3.038(4)     114.00     .   yes
 
# start Validation Reply Form
_vrf_CRYSS02_rp47_pl
;
PROBLEM: The value of _exptl_crystal_size_mid is > 0.8
RESPONSE: We are aware of the crystal size. Nevertheless, we still obtained a 
good data set from the measurement, suitable for publication and 
validating the proposed structure.
;
# end Validation Reply Form 
 
 
#===END
