 
data_92car011
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C22 H18 Cl2 N4 O8 Pt'
_chemical_formula_weight          732.39
 
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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pt'  'Pt'  -2.3520   8.3880
 '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                    8.397(3)
_cell_length_b                    27.420(8)
_cell_length_c                    10.898(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  96.920(10)
_cell_angle_gamma                 90.00
_cell_volume                      2490.9(15)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        needles
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.953
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1416
_exptl_absorpt_coefficient_mu     5.699
_exptl_absorpt_correction_type    Empirical
_exptl_absorpt_correction_T_min   0.1628
_exptl_absorpt_correction_T_max   0.7261
_exptl_absorpt_process_details    
;
DIFABS (N. Walker and D. Stuart, Acta Cryst., 1983, A39, 158-166) adapted for FAST geometry by A. Karaulov, Univ. of Cardiff, 1990)
; 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
 'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_standards_number         'None'
_diffrn_standards_interval_count 'N/A'
_diffrn_standards_interval_time  'N/A'
_diffrn_standards_decay_%        'N/A'
_diffrn_reflns_number             2918
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0012
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        35
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          2.44
_diffrn_reflns_theta_max          27.49
_reflns_number_total              2819
_reflns_number_gt                 2819
_reflns_threshold_expression      >2σ(I)
 

_computing_data_collection        'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        REFINE
_computing_data_reduction         'ABSURD (Karaulov, 1992)'
_computing_structure_solution     'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SNOOPI (K. Davies, Univ. of Oxford, 1983)'
_computing_publication_material   SHELXL97
 
_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)+(0.1000P)²+0.0000P] 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        0
_refine_ls_number_reflns          2819
_refine_ls_number_parameters      353
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0331
_refine_ls_R_factor_gt            0.0331
_refine_ls_wR_factor_ref          0.1051
_refine_ls_wR_factor_gt           0.1051
_refine_ls_goodness_of_fit_ref    1.129
_refine_ls_restrained_S_all       1.129
_refine_ls_shift/su_max           0.000
_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
Pt Pt 0.13193(4) 0.121518(11) 0.18640(3) 0.05551(15) Uani 1 1 d . . .
N1 N 0.2520(8) 0.0584(2) 0.1815(6) 0.0549(15) Uani 1 1 d . . .
N2 N 0.0460(8) 0.1009(3) 0.0125(6) 0.0591(17) Uani 1 1 d . . .
C1 C 0.3532(10) 0.0374(3) 0.2669(8) 0.061(2) Uani 1 1 d . . .
H1 H 0.3740 0.0526 0.3434 0.120(10) Uiso 1 1 calc R . .
C2 C 0.4313(11) -0.0068(4) 0.2486(11) 0.078(3) Uani 1 1 d . . .
H2 H 0.5017 -0.0206 0.3114 0.120(10) Uiso 1 1 calc R . .
C3 C 0.4013(12) -0.0287(4) 0.1364(11) 0.076(3) Uani 1 1 d . . .
H3 H 0.4507 -0.0583 0.1235 0.120(10) Uiso 1 1 calc R . .
C4 C 0.2981(11) -0.0081(3) 0.0398(9) 0.068(2) Uani 1 1 d . . .
C5 C 0.2248(10) 0.0362(3) 0.0664(7) 0.0558(18) Uani 1 1 d . . .
C6 C 0.1147(10) 0.0587(3) -0.0222(7) 0.0565(19) Uani 1 1 d . . .
C7 C 0.0810(12) 0.0389(4) -0.1403(8) 0.069(3) Uani 1 1 d . . .
C8 C -0.0308(15) 0.0642(5) -0.2211(10) 0.091(4) Uani 1 1 d . . .
H8 H -0.0565 0.0528 -0.3015 0.120(10) Uiso 1 1 calc R . .
C9 C -0.1030(15) 0.1052(5) -0.1846(10) 0.093(4) Uani 1 1 d . . .
H9 H -0.1813 0.1206 -0.2389 0.120(10) Uiso 1 1 calc R . .
C10 C -0.0614(14) 0.1245(4) -0.0674(10) 0.080(3) Uani 1 1 d . . .
H10 H -0.1075 0.1534 -0.0444 0.120(10) Uiso 1 1 calc R . .
C11 C 0.2583(12) -0.0289(4) -0.0822(10) 0.076(3) Uani 1 1 d . . .
H11 H 0.3035 -0.0585 -0.1018 0.120(10) Uiso 1 1 calc R . .
C12 C 0.1539(16) -0.0052(4) -0.1689(10) 0.091(4) Uani 1 1 d . . .
H12 H 0.1311 -0.0184 -0.2476 0.120(10) Uiso 1 1 calc R . .
N3 N 0.0055(9) 0.1844(3) 0.1815(6) 0.0608(17) Uani 1 1 d . . .
N4 N 0.2327(10) 0.1393(3) 0.3582(7) 0.0689(19) Uani 1 1 d . . .
C13 C 0.0460(15) 0.2224(4) 0.1210(14) 0.105(4) Uani 1 1 d . . .
H13 H 0.1381 0.2205 0.0817 0.120(10) Uiso 1 1 calc R . .
C14 C -0.0395(18) 0.2652(5) 0.1117(15) 0.119(5) Uani 1 1 d . . .
H14 H -0.0100 0.2909 0.0635 0.120(10) Uiso 1 1 calc R . .
C15 C -0.1724(16) 0.2689(4) 0.1771(14) 0.103(4) Uani 1 1 d . . .
H15 H -0.2277 0.2982 0.1803 0.120(10) Uiso 1 1 calc R . .
C16 C -0.2178(15) 0.2292(4) 0.2350(13) 0.100(4) Uani 1 1 d . . .
H16 H -0.3099 0.2300 0.2745 0.120(10) Uiso 1 1 calc R . .
C17 C -0.1291(13) 0.1872(4) 0.2362(10) 0.088(3) Uani 1 1 d . . .
H17 H -0.1631 0.1598 0.2763 0.120(10) Uiso 1 1 calc R . .
C18 C 0.3468(14) 0.1736(4) 0.3718(10) 0.085(3) Uani 1 1 d . . .
H18 H 0.3790 0.1877 0.3011 0.120(10) Uiso 1 1 calc R . .
C19 C 0.4198(15) 0.1893(5) 0.4868(11) 0.099(4) Uani 1 1 d . . .
H19 H 0.4985 0.2134 0.4943 0.120(10) Uiso 1 1 calc R . .
C20 C 0.3694(17) 0.1674(6) 0.5873(10) 0.106(4) Uani 1 1 d . . .
H20 H 0.4172 0.1763 0.6655 0.120(10) Uiso 1 1 calc R . .
C21 C 0.2532(17) 0.1336(7) 0.5777(12) 0.115(5) Uani 1 1 d . . .
H21 H 0.2181 0.1202 0.6481 0.120(10) Uiso 1 1 calc R . .
C22 C 0.1865(14) 0.1191(5) 0.4612(10) 0.090(4) Uani 1 1 d . . .
H22 H 0.1083 0.0949 0.4537 0.120(10) Uiso 1 1 calc R . .
Cl1 Cl 0.7284(3) 0.41585(10) -0.0421(2) 0.0747(6) Uani 1 1 d . . .
O1 O 0.8034(14) 0.3734(3) 0.0151(9) 0.118(3) Uani 1 1 d . . .
O2 O 0.6752(12) 0.4064(3) -0.1689(6) 0.104(3) Uani 1 1 d . . .
O3 O 0.8422(13) 0.4551(4) -0.0309(8) 0.139(4) Uani 1 1 d . . .
O4 O 0.5923(12) 0.4291(5) 0.0162(9) 0.139(4) Uani 1 1 d . . .
Cl2 Cl 0.4594(4) 0.16978(11) -0.0364(3) 0.0885(8) Uani 1 1 d . . .
O5 O 0.4248(14) 0.1938(4) 0.0664(10) 0.140(4) Uani 1 1 d . . .
O6 O 0.5735(14) 0.1901(5) -0.0964(10) 0.161(5) Uani 1 1 d . . .
O7A O 0.333(4) 0.1499(18) -0.110(2) 0.23(2) Uani 0.65 1 d P . .
O7B O 0.328(6) 0.2026(16) -0.114(3) 0.19(2) Uani 0.35 1 d P . .
O8A O 0.552(4) 0.1296(7) 0.044(3) 0.213(14) Uani 0.65 1 d P . .
O8B O 0.405(7) 0.1284(13) -0.075(7) 0.19(3) Uani 0.35 1 d P . .
 
 
_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
Pt N1 2.008(6) . ?
Pt N4 2.020(8) . ?
Pt N2 2.025(7) . ?
Pt N3 2.021(7) . ?
N1 C1 1.315(11) . ?
N1 C5 1.388(10) . ?
N2 C10 1.342(13) . ?
N2 C6 1.366(12) . ?
C1 C2 1.403(14) . ?
C1 H1 0.9300 . ?
C2 C3 1.359(15) . ?
C2 H2 0.9300 . ?
C3 C4 1.400(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.406(12) . ?
C4 C11 1.448(14) . ?
C5 C6 1.398(12) . ?
C6 C7 1.394(12) . ?
C7 C12 1.407(16) . ?
C7 C8 1.392(16) . ?
C8 C9 1.362(18) . ?
C8 H8 0.9300 . ?
C9 C10 1.388(16) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.373(17) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
N3 C13 1.300(12) . ?
N3 C17 1.342(11) . ?
N4 C22 1.350(13) . ?
N4 C18 1.339(13) . ?
C13 C14 1.374(17) . ?
C13 H13 0.9300 . ?
C14 C15 1.399(17) . ?
C14 H14 0.9300 . ?
C15 C16 1.337(17) . ?
C15 H15 0.9300 . ?
C16 C17 1.371(15) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.395(14) . ?
C18 H18 0.9300 . ?
C19 C20 1.360(18) . ?
C19 H19 0.9300 . ?
C20 C21 1.34(2) . ?
C20 H20 0.9300 . ?
C21 C22 1.383(18) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
Cl1 O4 1.420(9) . ?
Cl1 O3 1.434(9) . ?
Cl1 O1 1.430(8) . ?
Cl1 O2 1.424(7) . ?
Cl2 O8B 1.27(4) . ?
Cl2 O6 1.345(9) . ?
Cl2 O7A 1.37(2) . ?
Cl2 O5 1.360(10) . ?
Cl2 O8A 1.56(2) . ?
Cl2 O7B 1.59(3) . ?
O7A O8B 0.90(7) . ?
O7A O7B 1.45(5) . ?
O8A O8B 1.67(7) . ?
 
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
N1 Pt N4 94.4(3) . . ?
N1 Pt N2 81.8(3) . . ?
N4 Pt N2 175.7(3) . . ?
N1 Pt N3 176.8(3) . . ?
N4 Pt N3 88.8(3) . . ?
N2 Pt N3 94.9(3) . . ?
C1 N1 C5 118.0(7) . . ?
C1 N1 Pt 129.9(6) . . ?
C5 N1 Pt 112.0(5) . . ?
C10 N2 C6 120.1(8) . . ?
C10 N2 Pt 127.5(7) . . ?
C6 N2 Pt 112.4(6) . . ?
N1 C1 C2 123.4(9) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 118.1(10) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 121.9(10) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C5 116.1(9) . . ?
C3 C4 C11 125.7(10) . . ?
C5 C4 C11 118.1(10) . . ?
N1 C5 C6 116.9(7) . . ?
N1 C5 C4 122.5(8) . . ?
C6 C5 C4 120.6(8) . . ?
N2 C6 C7 122.6(9) . . ?
N2 C6 C5 116.8(7) . . ?
C7 C6 C5 120.6(9) . . ?
C12 C7 C6 119.6(10) . . ?
C12 C7 C8 124.4(10) . . ?
C6 C7 C8 115.9(10) . . ?
C9 C8 C7 121.1(10) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 120.8(11) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
N2 C10 C9 119.3(12) . . ?
N2 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C12 C11 C4 120.1(10) . . ?
C12 C11 H11 119.9 . . ?
C4 C11 H11 119.9 . . ?
C11 C12 C7 120.9(10) . . ?
C11 C12 H12 119.5 . . ?
C7 C12 H12 119.5 . . ?
C13 N3 C17 117.7(9) . . ?
C13 N3 Pt 121.9(7) . . ?
C17 N3 Pt 120.3(7) . . ?
C22 N4 C18 118.1(9) . . ?
C22 N4 Pt 122.8(8) . . ?
C18 N4 Pt 119.1(7) . . ?
N3 C13 C14 123.8(11) . . ?
N3 C13 H13 118.1 . . ?
C14 C13 H13 118.1 . . ?
C15 C14 C13 117.9(12) . . ?
C15 C14 H14 121.1 . . ?
C13 C14 H14 121.1 . . ?
C16 C15 C14 118.1(11) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C15 C16 C17 120.3(11) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
N3 C17 C16 122.0(10) . . ?
N3 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
N4 C18 C19 123.2(11) . . ?
N4 C18 H18 118.4 . . ?
C19 C18 H18 118.4 . . ?
C18 C19 C20 116.2(12) . . ?
C18 C19 H19 121.9 . . ?
C20 C19 H19 121.9 . . ?
C21 C20 C19 122.4(11) . . ?
C21 C20 H20 118.8 . . ?
C19 C20 H20 118.8 . . ?
C20 C21 C22 118.8(13) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
N4 C22 C21 121.3(12) . . ?
N4 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
O4 Cl1 O3 109.5(7) . . ?
O4 Cl1 O1 110.4(7) . . ?
O3 Cl1 O1 108.7(7) . . ?
O4 Cl1 O2 107.8(6) . . ?
O3 Cl1 O2 110.3(6) . . ?
O1 Cl1 O2 110.2(6) . . ?
O8B Cl2 O6 117(2) . . ?
O8B Cl2 O7A 40(3) . . ?
O6 Cl2 O7A 115.3(11) . . ?
O8B Cl2 O5 127(3) . . ?
O6 Cl2 O5 115.8(7) . . ?
O7A Cl2 O5 116.7(16) . . ?
O8B Cl2 O8A 72(3) . . ?
O6 Cl2 O8A 103.3(14) . . ?
O7A Cl2 O8A 110(2) . . ?
O5 Cl2 O8A 91.3(13) . . ?
O8B Cl2 O7B 98(3) . . ?
O6 Cl2 O7B 90(2) . . ?
O7A Cl2 O7B 58(2) . . ?
O5 Cl2 O7B 87.7(13) . . ?
O8A Cl2 O7B 166(2) . . ?
O8B O7A Cl2 64(3) . . ?
O8B O7A O7B 133(4) . . ?
Cl2 O7A O7B 68.7(17) . . ?
O7A O7B Cl2 53.4(16) . . ?
Cl2 O8A O8B 46.3(14) . . ?
O7A O8B Cl2 76(3) . . ?
O7A O8B O8A 136(5) . . ?
Cl2 O8B O8A 62(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.494
_diffrn_reflns_theta_full              27.49
_diffrn_measured_fraction_theta_full   0.494
_refine_diff_density_max    1.150
_refine_diff_density_min   -0.855
_refine_diff_density_rms    0.103
