data_04src0339

#Prof. D. Bruce
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C24 H22 F7 N O4 Pt'
_chemical_formula_sum
 'C24 H22 F7 N O4 Pt'
_chemical_formula_weight          716.52
 
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'
 'F'  'F'   0.0171   0.0103
 '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                    14.879(2)
_cell_length_b                    12.024(1)
_cell_length_c                    14.605(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  111.4000(7)
_cell_angle_gamma                 90.00
_cell_volume                      2432.8(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     26481
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Slab
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.13
_exptl_crystal_size_mid           0.09
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.956
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1384
_exptl_absorpt_coefficient_mu     5.853
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.5166
_exptl_absorpt_correction_T_max   0.8440
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_exptl_special_details
;
SADABS was used to perform the Absorption correction
Parameter refinement on 25073 reflections reduced R(int) from 0.1093 to 0.0295
Ratio of minimum to maximum apparent transmission: 0.691275
The given Tmin and Tmax were generated using the SHELX SIZE command
;


_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             28836
_diffrn_reflns_av_R_equivalents   0.0306
_diffrn_reflns_av_sigmaI/netI     0.0259
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.98
_diffrn_reflns_theta_max          27.48
_reflns_number_total              5563
_reflns_number_gt                 5123
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX (Farrugia, 1999)'

 
_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)+(0.0061P)²+3.4191P] 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          5563
_refine_ls_number_parameters      337
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0218
_refine_ls_R_factor_gt            0.0186
_refine_ls_wR_factor_ref          0.0391
_refine_ls_wR_factor_gt           0.0376
_refine_ls_goodness_of_fit_ref    1.043
_refine_ls_restrained_S_all       1.043
_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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pt1 Pt 0.067134(6) 0.174464(7) 0.396212(6) 0.01263(3) Uani 1 1 d . . .
C1 C -0.06775(17) 0.19909(19) 0.38144(17) 0.0145(5) Uani 1 1 d . . .
C2 C -0.09304(18) 0.31255(19) 0.38086(17) 0.0168(5) Uani 1 1 d . . .
C3 C -0.1862(2) 0.3444(2) 0.37112(19) 0.0224(6) Uani 1 1 d . . .
H3 H -0.2018 0.4209 0.3724 0.027 Uiso 1 1 calc R . .
C4 C -0.25556(19) 0.2643(2) 0.35963(19) 0.0234(6) Uani 1 1 d . . .
H4 H -0.3193 0.2852 0.3526 0.028 Uiso 1 1 calc R . .
C5 C -0.23179(18) 0.1518(2) 0.35830(18) 0.0186(5) Uani 1 1 d . . .
C6 C -0.13834(17) 0.1191(2) 0.37050(17) 0.0161(5) Uani 1 1 d . . .
H6 H -0.1229 0.0423 0.3713 0.019 Uiso 1 1 calc R . .
C7 C -0.01352(18) 0.3857(2) 0.39463(17) 0.0168(5) Uani 1 1 d . . .
H7 H -0.0209 0.4641 0.3951 0.020 Uiso 1 1 calc R . .
C8 C 0.15316(18) 0.40790(19) 0.42377(17) 0.0158(5) Uani 1 1 d . . .
C9 C 0.23907(18) 0.3795(2) 0.49978(18) 0.0194(5) Uani 1 1 d . . .
H9 H 0.2415 0.3154 0.5386 0.023 Uiso 1 1 calc R . .
C10 C 0.32014(19) 0.4440(2) 0.51862(19) 0.0230(6) Uani 1 1 d . . .
H10 H 0.3781 0.4249 0.5712 0.028 Uiso 1 1 calc R . .
C11 C 0.31779(18) 0.5372(2) 0.46114(19) 0.0212(5) Uani 1 1 d . . .
C12 C 0.23261(19) 0.5656(2) 0.38513(18) 0.0199(5) Uani 1 1 d . . .
H12 H 0.2304 0.6292 0.3458 0.024 Uiso 1 1 calc R . .
C13 C 0.15086(18) 0.50096(19) 0.36690(17) 0.0178(5) Uani 1 1 d . . .
H13 H 0.0926 0.5206 0.3149 0.021 Uiso 1 1 calc R . .
C14 C -0.2866(2) -0.0370(2) 0.3388(2) 0.0259(6) Uani 1 1 d . . .
H14A H -0.2658 -0.0504 0.2834 0.039 Uiso 1 1 calc R . .
H14B H -0.3453 -0.0797 0.3294 0.039 Uiso 1 1 calc R . .
H14C H -0.2355 -0.0601 0.4001 0.039 Uiso 1 1 calc R . .
C15 C 0.4080(2) 0.6778(2) 0.4188(2) 0.0359(7) Uani 1 1 d . . .
H15A H 0.3916 0.6455 0.3531 0.054 Uiso 1 1 calc R . .
H15B H 0.4738 0.7076 0.4412 0.054 Uiso 1 1 calc R . .
H15C H 0.3626 0.7379 0.4162 0.054 Uiso 1 1 calc R . .
N1 N 0.06952(14) 0.34054(16) 0.40657(14) 0.0150(4) Uani 1 1 d . . .
O1 O -0.30592(13) 0.07927(15) 0.34386(14) 0.0251(4) Uani 1 1 d . . .
O2 O 0.40212(13) 0.59438(16) 0.48520(14) 0.0296(4) Uani 1 1 d . . .
C21 C 0.4644(2) 0.1326(3) 0.3187(2) 0.0292(6) Uani 1 1 d . . .
C22 C 0.3648(2) 0.1408(2) 0.3271(2) 0.0263(6) Uani 1 1 d . . .
C23 C 0.34996(18) 0.0704(2) 0.40845(18) 0.0197(5) Uani 1 1 d . . .
C24 C 0.24449(17) 0.0611(2) 0.39913(17) 0.0162(5) Uani 1 1 d . . .
C25 C 0.20116(18) -0.0418(2) 0.38452(18) 0.0190(5) Uani 1 1 d . . .
H25 H 0.2385 -0.1035 0.3785 0.023 Uiso 1 1 calc R . .
C26 C 0.10636(18) -0.06294(19) 0.37784(17) 0.0146(5) Uani 1 1 d . . .
C27 C 0.07031(18) -0.18075(18) 0.36773(18) 0.0164(5) Uani 1 1 d . . .
H27A H 0.1104 -0.2230 0.4267 0.020 Uiso 1 1 calc R . .
H27B H 0.0795 -0.2148 0.3101 0.020 Uiso 1 1 calc R . .
C28 C -0.03491(18) -0.19327(19) 0.35573(18) 0.0172(5) Uani 1 1 d . . .
H28A H -0.0762 -0.1576 0.2935 0.021 Uiso 1 1 calc R . .
H28B H -0.0461 -0.1548 0.4105 0.021 Uiso 1 1 calc R . .
C29 C -0.0629(2) -0.3151(2) 0.35470(19) 0.0216(6) Uani 1 1 d . . .
H29A H -0.0576 -0.3517 0.2969 0.032 Uiso 1 1 calc R . .
H29B H -0.1296 -0.3205 0.3520 0.032 Uiso 1 1 calc R . .
H29C H -0.0196 -0.3516 0.4145 0.032 Uiso 1 1 calc R . .
O21 O 0.21048(12) 0.15582(13) 0.40815(12) 0.0170(4) Uani 1 1 d . . .
O22 O 0.04550(12) 0.01041(13) 0.38044(12) 0.0162(3) Uani 1 1 d . . .
F21 F 0.47827(13) 0.03462(16) 0.28684(14) 0.0463(5) Uani 1 1 d . . .
F22 F 0.46996(14) 0.20682(19) 0.25372(15) 0.0538(5) Uani 1 1 d . . .
F23 F 0.53358(12) 0.15289(17) 0.40389(13) 0.0418(5) Uani 1 1 d . . .
F24 F 0.34889(14) 0.24756(14) 0.34056(16) 0.0481(5) Uani 1 1 d . . .
F25 F 0.29904(12) 0.10718(19) 0.24044(12) 0.0487(5) Uani 1 1 d . . .
F26 F 0.38925(11) -0.03031(13) 0.40638(13) 0.0342(4) Uani 1 1 d . . .
F27 F 0.40217(11) 0.11708(14) 0.49606(11) 0.0316(4) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Pt1 C1 1.961(2) . ?
Pt1 O22 1.9984(16) . ?
Pt1 N1 2.0020(19) . ?
Pt1 O21 2.0876(17) . ?
C1 C6 1.390(3) . ?
C1 C2 1.414(3) . ?
C2 C3 1.395(4) . ?
C2 C7 1.428(3) . ?
C3 C4 1.376(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.400(3) . ?
C4 H4 0.9500 . ?
C5 O1 1.361(3) . ?
C5 C6 1.393(3) . ?
C6 H6 0.9500 . ?
C7 N1 1.302(3) . ?
C7 H7 0.9500 . ?
C8 C13 1.387(3) . ?
C8 C9 1.395(3) . ?
C8 N1 1.428(3) . ?
C9 C10 1.375(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.393(4) . ?
C10 H10 0.9500 . ?
C11 O2 1.360(3) . ?
C11 C12 1.389(4) . ?
C12 C13 1.385(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 O1 1.434(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O2 1.420(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C21 F21 1.311(3) . ?
C21 F23 1.316(3) . ?
C21 F22 1.328(3) . ?
C21 C22 1.534(4) . ?
C22 F24 1.333(3) . ?
C22 F25 1.348(3) . ?
C22 C23 1.539(4) . ?
C23 F26 1.350(3) . ?
C23 F27 1.353(3) . ?
C23 C24 1.529(3) . ?
C24 O21 1.272(3) . ?
C24 C25 1.375(3) . ?
C25 C26 1.401(3) . ?
C25 H25 0.9500 . ?
C26 O22 1.275(3) . ?
C26 C27 1.503(3) . ?
C27 C28 1.518(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.521(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
 
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
C1 Pt1 O22 91.21(8) . . ?
C1 Pt1 N1 81.20(9) . . ?
O22 Pt1 N1 172.29(7) . . ?
C1 Pt1 O21 177.09(8) . . ?
O22 Pt1 O21 91.16(6) . . ?
N1 Pt1 O21 96.39(7) . . ?
C6 C1 C2 118.6(2) . . ?
C6 C1 Pt1 127.45(18) . . ?
C2 C1 Pt1 113.93(18) . . ?
C3 C2 C1 121.2(2) . . ?
C3 C2 C7 125.9(2) . . ?
C1 C2 C7 112.8(2) . . ?
C4 C3 C2 119.5(2) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.8(2) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
O1 C5 C6 123.6(2) . . ?
O1 C5 C4 115.3(2) . . ?
C6 C5 C4 121.1(2) . . ?
C1 C6 C5 119.8(2) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
N1 C7 C2 117.4(2) . . ?
N1 C7 H7 121.3 . . ?
C2 C7 H7 121.3 . . ?
C13 C8 C9 119.3(2) . . ?
C13 C8 N1 121.5(2) . . ?
C9 C8 N1 119.2(2) . . ?
C10 C9 C8 120.2(2) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 120.4(2) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
O2 C11 C12 124.7(2) . . ?
O2 C11 C10 115.7(2) . . ?
C12 C11 C10 119.6(2) . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C8 120.7(2) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
O1 C14 H14A 109.5 . . ?
O1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C15 H15A 109.5 . . ?
O2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 N1 C8 120.7(2) . . ?
C7 N1 Pt1 114.57(16) . . ?
C8 N1 Pt1 124.70(15) . . ?
C5 O1 C14 117.8(2) . . ?
C11 O2 C15 117.5(2) . . ?
F21 C21 F23 109.4(2) . . ?
F21 C21 F22 106.9(2) . . ?
F23 C21 F22 108.6(2) . . ?
F21 C21 C22 111.6(2) . . ?
F23 C21 C22 111.0(2) . . ?
F22 C21 C22 109.2(2) . . ?
F24 C22 F25 108.7(2) . . ?
F24 C22 C21 107.6(2) . . ?
F25 C22 C21 107.3(2) . . ?
F24 C22 C23 109.5(2) . . ?
F25 C22 C23 107.5(2) . . ?
C21 C22 C23 116.2(2) . . ?
F26 C23 F27 106.8(2) . . ?
F26 C23 C24 111.8(2) . . ?
F27 C23 C24 109.3(2) . . ?
F26 C23 C22 106.9(2) . . ?
F27 C23 C22 107.9(2) . . ?
C24 C23 C22 113.7(2) . . ?
O21 C24 C25 129.7(2) . . ?
O21 C24 C23 111.1(2) . . ?
C25 C24 C23 119.2(2) . . ?
C24 C25 C26 125.3(2) . . ?
C24 C25 H25 117.4 . . ?
C26 C25 H25 117.4 . . ?
O22 C26 C25 125.5(2) . . ?
O22 C26 C27 115.0(2) . . ?
C25 C26 C27 119.5(2) . . ?
C26 C27 C28 114.9(2) . . ?
C26 C27 H27A 108.5 . . ?
C28 C27 H27A 108.5 . . ?
C26 C27 H27B 108.5 . . ?
C28 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?
C27 C28 C29 111.3(2) . . ?
C27 C28 H28A 109.4 . . ?
C29 C28 H28A 109.4 . . ?
C27 C28 H28B 109.4 . . ?
C29 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C24 O21 Pt1 121.36(15) . . ?
C26 O22 Pt1 126.89(15) . . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.581
_refine_diff_density_min   -0.719
_refine_diff_density_rms    0.091
