 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C33 H29 I2 N O3 P2 Pt'
_chemical_formula_sum
 'C33 H29 I2 N O3 P2 Pt'
_chemical_formula_weight          998.40
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'I'  'I'  -0.4742   1.8119
 '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'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
_symmetry_space_group_name_hall   '-P 2ybc'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    16.4439(4)
_cell_length_b                    17.3353(3)
_cell_length_c                    15.1356(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  109.9110(10)
_cell_angle_gamma                 90.00
_cell_volume                      4056.64(13)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     47925
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             orange
_exptl_crystal_size_max           0.04
_exptl_crystal_size_mid           0.02
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.635
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1888
_exptl_absorpt_coefficient_mu     5.087
_exptl_absorpt_correction_type    Multi-scan
_exptl_absorpt_correction_T_min   0.8224
_exptl_absorpt_correction_T_max   0.9051
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)'
 
_exptl_special_details
;
?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker Nonius Kappa CCD Area detector'
_diffrn_measurement_method        'φ and ω scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean  '9.091 pixels mm^1^'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             48913
_diffrn_reflns_av_R_equivalents   0.0642
_diffrn_reflns_av_sigmaI/netI     0.0391
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.96
_diffrn_reflns_theta_max          25.03
_reflns_number_total              7149
_reflns_number_gt                 5580
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'COLLECT (Hooft, 1998)'
_computing_cell_refinement        'DENZO (Otwinowski and MInor, 1997)'
_computing_data_reduction         'DENZO, COLLECT, MAXUS (Mackay et al., 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'CAMERON (Watkin, et al., 1993)'
_computing_publication_material   'WINGX (Farrugia, 1998)'
 
_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 > 2σ(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)+(0.0753P)²+35.3648P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          7149
_refine_ls_number_parameters      344
_refine_ls_number_restraints      72
_refine_ls_R_factor_all           0.0713
_refine_ls_R_factor_gt            0.0522
_refine_ls_wR_factor_ref          0.1521
_refine_ls_wR_factor_gt           0.1377
_refine_ls_goodness_of_fit_ref    1.041
_refine_ls_restrained_S_all       1.035
_refine_ls_shift/su_max           0.048
_refine_ls_shift/su_mean          0.001
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pt1 Pt 0.08937(2) 0.305684(16) 0.324778(19) 0.04071(8) Uani 1 1 d . A .
I1 I -0.06700(4) 0.32728(3) 0.33665(4) 0.05694(14) Uani 1 1 d . . .
I2 I 0.11367(4) 0.18473(3) 0.43894(3) 0.05080(14) Uani 1 1 d . . .
P1 P 0.06611(13) 0.41350(11) 0.23799(13) 0.0410(4) Uani 1 1 d . . .
P2 P 0.21922(14) 0.27842(13) 0.31615(14) 0.0464(5) Uani 1 1 d . . .
N1 N 0.2339(5) 0.4183(4) 0.2395(4) 0.0518(17) Uani 1 1 d . . .
O1 O 0.2722(5) 0.5465(5) 0.3509(5) 0.103(2) Uani 1 1 d . A .
H1 H 0.2185 0.5502 0.3236 0.154 Uiso 1 1 calc R . .
O2 O 0.4239(4) 0.4521(4) 0.0345(4) 0.0684(17) Uani 1 1 d . A .
O3 O 0.4939(4) 0.5634(4) 0.0843(4) 0.0773(19) Uani 1 1 d . A .
H3 H 0.5147 0.5532 0.0421 0.116 Uiso 1 1 calc R . .
C1 C -0.0330(5) 0.4135(4) 0.1389(5) 0.0435(18) Uani 1 1 d . . .
C2 C -0.1030(6) 0.4664(5) 0.1258(6) 0.051(2) Uani 1 1 d . . .
H2 H -0.0988 0.5050 0.1717 0.061 Uiso 1 1 calc R . .
C3 C -0.1760(5) 0.4619(5) 0.0475(6) 0.050(2) Uani 1 1 d . . .
H3A H -0.2220 0.4971 0.0405 0.060 Uiso 1 1 calc R . .
C4 C -0.1842(6) 0.4067(5) -0.0219(6) 0.050(2) Uani 1 1 d . . .
H4 H -0.2351 0.4039 -0.0757 0.061 Uiso 1 1 calc R . .
C5 C -0.1156(6) 0.3558(5) -0.0102(6) 0.052(2) Uani 1 1 d . . .
H5 H -0.1197 0.3185 -0.0575 0.062 Uiso 1 1 calc R . .
C6 C -0.0417(5) 0.3585(4) 0.0687(5) 0.0420(18) Uani 1 1 d . . .
H6 H 0.0036 0.3226 0.0752 0.050 Uiso 1 1 calc R . .
C7 C 0.0690(5) 0.4993(4) 0.3076(5) 0.045(2) Uani 1 1 d . . .
C8 C 0.0574(6) 0.5726(5) 0.2653(6) 0.055(2) Uani 1 1 d . . .
H8 H 0.0456 0.5771 0.1995 0.066 Uiso 1 1 calc R . .
C9 C 0.0632(7) 0.6384(5) 0.3196(6) 0.067(3) Uani 1 1 d . . .
H9 H 0.0558 0.6880 0.2912 0.080 Uiso 1 1 calc R . .
C10 C 0.0798(8) 0.6313(5) 0.4145(6) 0.071(3) Uani 1 1 d . . .
H10 H 0.0821 0.6762 0.4512 0.086 Uiso 1 1 calc R . .
C11 C 0.0933(8) 0.5601(5) 0.4573(6) 0.072(3) Uani 1 1 d . . .
H11 H 0.1055 0.5562 0.5232 0.087 Uiso 1 1 calc R . .
C12 C 0.0889(6) 0.4938(5) 0.4039(6) 0.056(2) Uani 1 1 d . . .
H12 H 0.0997 0.4447 0.4336 0.068 Uiso 1 1 calc R . .
C13A C 0.3022(9) 0.2985(9) 0.4202(9) 0.0925(3) Uani 0.50 1 d PGU A 1
C14A C 0.2850(9) 0.3351(10) 0.4936(11) 0.0925(3) Uani 0.50 1 d PGU A 1
H14A H 0.2271 0.3468 0.4882 0.111 Uiso 0.50 1 calc PR A 1
C15A C 0.3526(11) 0.3545(10) 0.5750(10) 0.0925(3) Uani 0.50 1 d PGU A 1
H15A H 0.3409 0.3795 0.6252 0.111 Uiso 0.50 1 calc PR A 1
C16A C 0.4374(10) 0.3373(11) 0.5829(10) 0.0925(3) Uani 0.50 1 d PGU A 1
H16A H 0.4836 0.3506 0.6384 0.111 Uiso 0.50 1 calc PR A 1
C17A C 0.4545(8) 0.3007(11) 0.5094(12) 0.0925(3) Uani 0.50 1 d PGU A 1
H17A H 0.5125 0.2889 0.5148 0.111 Uiso 0.50 1 calc PR A 1
C18A C 0.3869(10) 0.2813(9) 0.4281(10) 0.0925(3) Uani 0.50 1 d PGU A 1
H18A H 0.3987 0.2562 0.3779 0.111 Uiso 0.50 1 calc PR A 1
C13B C 0.3119(9) 0.2803(9) 0.4337(9) 0.0925(3) Uani 0.50 1 d PGU A 2
C14B C 0.2992(9) 0.3106(10) 0.5129(11) 0.0925(3) Uani 0.50 1 d PGU A 2
H14B H 0.2444 0.3312 0.5085 0.111 Uiso 0.50 1 calc PR A 2
C15B C 0.3666(11) 0.3109(10) 0.5986(10) 0.0925(3) Uani 0.50 1 d PGU A 2
H15B H 0.3579 0.3317 0.6528 0.111 Uiso 0.50 1 calc PR A 2
C16B C 0.4468(10) 0.2809(11) 0.6050(10) 0.0925(3) Uani 0.50 1 d PGU A 2
H16B H 0.4929 0.2811 0.6636 0.111 Uiso 0.50 1 calc PR A 2
C17B C 0.4595(9) 0.2505(11) 0.5258(12) 0.0925(3) Uani 0.50 1 d PGU A 2
H17B H 0.5143 0.2299 0.5302 0.111 Uiso 0.50 1 calc PR A 2
C18B C 0.3921(10) 0.2502(9) 0.4401(10) 0.0925(3) Uani 0.50 1 d PGU A 2
H18B H 0.4008 0.2294 0.3859 0.111 Uiso 0.50 1 calc PR A 2
C19 C 0.2244(5) 0.1819(5) 0.2723(5) 0.0439(19) Uani 1 1 d . A .
C20 C 0.2772(8) 0.1248(8) 0.3213(9) 0.095(4) Uani 1 1 d . . .
H20 H 0.3157 0.1362 0.3827 0.115 Uiso 1 1 calc R A .
C21 C 0.2781(9) 0.0520(8) 0.2873(10) 0.105(5) Uani 1 1 d . A .
H21 H 0.3168 0.0140 0.3235 0.126 Uiso 1 1 calc R . .
C22 C 0.2214(8) 0.0354(7) 0.1992(8) 0.084(4) Uani 1 1 d . . .
H22 H 0.2271 -0.0115 0.1694 0.100 Uiso 1 1 calc R A .
C23 C 0.1581(7) 0.0849(6) 0.1552(7) 0.075(3) Uani 1 1 d . A .
H23 H 0.1114 0.0698 0.1010 0.090 Uiso 1 1 calc R . .
C24 C 0.1631(7) 0.1594(7) 0.1915(8) 0.080(3) Uani 1 1 d . . .
H24 H 0.1212 0.1962 0.1577 0.096 Uiso 1 1 calc R A .
C25 C 0.2967(5) 0.4721(5) 0.2288(6) 0.054(2) Uani 1 1 d . A .
C26 C 0.3378(5) 0.4640(5) 0.1651(6) 0.050(2) Uani 1 1 d . . .
H26 H 0.3260 0.4201 0.1250 0.060 Uiso 1 1 calc R A .
C27 C 0.3968(5) 0.5188(6) 0.1578(6) 0.056(2) Uani 1 1 d . A .
C28 C 0.4122(7) 0.5849(7) 0.2142(8) 0.085(3) Uani 1 1 d . . .
H28 H 0.4511 0.6233 0.2079 0.102 Uiso 1 1 calc R A .
C29 C 0.3717(8) 0.5943(8) 0.2777(8) 0.102(4) Uani 1 1 d . A .
H29 H 0.3831 0.6386 0.3169 0.123 Uiso 1 1 calc R . .
C30 C 0.3122(7) 0.5376(7) 0.2853(7) 0.080(3) Uani 1 1 d . . .
C32 C 0.1450(5) 0.4352(5) 0.1799(5) 0.0424(18) Uani 1 1 d . A .
H32A H 0.1307 0.4045 0.1215 0.051 Uiso 1 1 calc R . .
H32B H 0.1405 0.4904 0.1623 0.051 Uiso 1 1 calc R . .
C33 C 0.2543(6) 0.3377(5) 0.2339(7) 0.061(2) Uani 1 1 d . A .
H33A H 0.3175 0.3319 0.2490 0.073 Uiso 1 1 calc R . .
H33B H 0.2253 0.3190 0.1690 0.073 Uiso 1 1 calc R . .
C31 C 0.4403(5) 0.5101(5) 0.0870(6) 0.053(2) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Pt1 P2 2.234(2) . ?
Pt1 P1 2.2411(19) . ?
Pt1 I2 2.6593(6) . ?
Pt1 I1 2.6645(6) . ?
P1 C1 1.801(8) . ?
P1 C7 1.815(8) . ?
P1 C32 1.837(8) . ?
P2 C13A 1.732(12) . ?
P2 C19 1.813(8) . ?
P2 C33 1.851(9) . ?
P2 C13B 1.908(12) . ?
N1 C25 1.441(11) . ?
N1 C33 1.447(11) . ?
N1 C32 1.462(10) . ?
O1 C30 1.374(12) . ?
O2 C31 1.253(11) . ?
O3 C31 1.288(10) . ?
C1 C6 1.397(10) . ?
C1 C2 1.432(11) . ?
C2 C3 1.373(11) . ?
C3 C4 1.392(11) . ?
C4 C5 1.395(12) . ?
C5 C6 1.384(11) . ?
C7 C12 1.385(11) . ?
C7 C8 1.406(11) . ?
C8 C9 1.390(12) . ?
C9 C10 1.374(13) . ?
C10 C11 1.376(13) . ?
C11 C12 1.394(12) . ?
C13A C14A 1.3900 . ?
C13A C18A 1.3900 . ?
C14A C15A 1.3900 . ?
C15A C16A 1.3900 . ?
C16A C17A 1.3900 . ?
C17A C18A 1.3900 . ?
C13B C14B 1.3900 . ?
C13B C18B 1.3900 . ?
C14B C15B 1.3900 . ?
C15B C16B 1.3900 . ?
C16B C17B 1.3900 . ?
C17B C18B 1.3900 . ?
C19 C24 1.350(13) . ?
C19 C20 1.358(14) . ?
C20 C21 1.365(18) . ?
C21 C22 1.372(16) . ?
C22 C23 1.337(15) . ?
C23 C24 1.396(14) . ?
C25 C26 1.360(12) . ?
C25 C30 1.392(14) . ?
C26 C27 1.390(12) . ?
C27 C28 1.399(14) . ?
C27 C31 1.485(12) . ?
C28 C29 1.351(15) . ?
C29 C30 1.420(15) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
P2 Pt1 P1 96.77(8) . . ?
P2 Pt1 I2 86.33(6) . . ?
P1 Pt1 I2 175.06(5) . . ?
P2 Pt1 I1 175.84(6) . . ?
P1 Pt1 I1 86.93(5) . . ?
I2 Pt1 I1 90.106(19) . . ?
C1 P1 C7 108.7(4) . . ?
C1 P1 C32 100.8(3) . . ?
C7 P1 C32 103.1(4) . . ?
C1 P1 Pt1 114.4(2) . . ?
C7 P1 Pt1 112.2(2) . . ?
C32 P1 Pt1 116.3(3) . . ?
C13A P2 C19 113.4(6) . . ?
C13A P2 C33 99.8(6) . . ?
C19 P2 C33 101.6(4) . . ?
C19 P2 C13B 103.6(5) . . ?
C33 P2 C13B 106.5(6) . . ?
C13A P2 Pt1 112.2(5) . . ?
C19 P2 Pt1 112.5(3) . . ?
C33 P2 Pt1 116.4(3) . . ?
C13B P2 Pt1 114.7(5) . . ?
C25 N1 C33 115.4(7) . . ?
C25 N1 C32 113.9(7) . . ?
C33 N1 C32 111.1(7) . . ?
C6 C1 C2 117.6(7) . . ?
C6 C1 P1 117.6(6) . . ?
C2 C1 P1 124.9(6) . . ?
C3 C2 C1 120.5(7) . . ?
C2 C3 C4 121.5(8) . . ?
C3 C4 C5 118.2(8) . . ?
C6 C5 C4 121.4(7) . . ?
C5 C6 C1 120.8(7) . . ?
C12 C7 C8 119.3(7) . . ?
C12 C7 P1 120.3(6) . . ?
C8 C7 P1 120.2(6) . . ?
C9 C8 C7 120.0(7) . . ?
C10 C9 C8 119.6(8) . . ?
C9 C10 C11 121.1(8) . . ?
C10 C11 C12 119.9(8) . . ?
C7 C12 C11 120.0(8) . . ?
C14A C13A C18A 120.0 . . ?
C14A C13A P2 120.5(8) . . ?
C18A C13A P2 119.4(8) . . ?
C15A C14A C13A 120.0 . . ?
C14A C15A C16A 120.0 . . ?
C17A C16A C15A 120.0 . . ?
C16A C17A C18A 120.0 . . ?
C17A C18A C13A 120.0 . . ?
C14B C13B C18B 120.0 . . ?
C14B C13B P2 120.2(8) . . ?
C18B C13B P2 119.8(8) . . ?
C13B C14B C15B 120.0 . . ?
C16B C15B C14B 120.0 . . ?
C15B C16B C17B 120.0 . . ?
C16B C17B C18B 120.0 . . ?
C17B C18B C13B 120.0 . . ?
C24 C19 C20 115.2(9) . . ?
C24 C19 P2 119.0(7) . . ?
C20 C19 P2 125.0(7) . . ?
C19 C20 C21 123.6(11) . . ?
C20 C21 C22 118.0(12) . . ?
C23 C22 C21 120.4(11) . . ?
C22 C23 C24 117.8(10) . . ?
C19 C24 C23 123.3(10) . . ?
C26 C25 C30 119.3(8) . . ?
C26 C25 N1 124.1(8) . . ?
C30 C25 N1 116.5(8) . . ?
C25 C26 C27 120.9(8) . . ?
C26 C27 C28 119.9(8) . . ?
C26 C27 C31 120.5(8) . . ?
C28 C27 C31 119.5(8) . . ?
C29 C28 C27 120.1(10) . . ?
C28 C29 C30 119.6(10) . . ?
O1 C30 C25 120.3(9) . . ?
O1 C30 C29 119.6(9) . . ?
C25 C30 C29 120.1(9) . . ?
N1 C32 P1 112.6(5) . . ?
N1 C33 P2 111.5(6) . . ?
O2 C31 O3 123.9(8) . . ?
O2 C31 C27 119.2(8) . . ?
O3 C31 C27 116.9(8) . . ?
 
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
O3 H3 O2  0.84 1.78 2.606(9) 167.0 3_665
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              25.03
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    2.120
_refine_diff_density_min   -2.256
_refine_diff_density_rms    0.185
