 
data_2005slh0428
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C56 H60 Cl2 N8 Ni Pt2'
_chemical_formula_weight          1364.91
 
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'
 'Ni'  'Ni'   0.3393   1.1124
 '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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    C2/m
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x, -y, z'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z'
 
_cell_length_a                    10.2973(8)
_cell_length_b                    29.825(5)
_cell_length_c                    9.3067(11)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.417(10)
_cell_angle_gamma                 90.00
_cell_volume                      2858.2(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3111
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        slab
_exptl_crystal_colour             green
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.586
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1340
_exptl_absorpt_coefficient_mu     5.344
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4146
_exptl_absorpt_correction_T_max   0.8147
_exptl_absorpt_process_details    
'SADABS V2.10 (Sheldrick, G.M., 2003)' 
 
_exptl_special_details
;
 ?
;
 
_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   '10cm confocal mirrors'
_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             14390
_diffrn_reflns_av_R_equivalents   0.0377
_diffrn_reflns_av_sigmaI/netI     0.0332
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -38
_diffrn_reflns_limit_k_max        38
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          3.04
_diffrn_reflns_theta_max          27.47
_reflns_number_total              3326
_reflns_number_gt                 3101
_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     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_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)+(0.0352P)²+6.5305P] 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      SHELXL
_refine_ls_extinction_coef        0.00025(9)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          3326
_refine_ls_number_parameters      162
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0295
_refine_ls_R_factor_gt            0.0269
_refine_ls_wR_factor_ref          0.0675
_refine_ls_wR_factor_gt           0.0666
_refine_ls_goodness_of_fit_ref    1.076
_refine_ls_restrained_S_all       1.076
_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
C1 C 0.3213(3) 0.07989(12) 0.5381(4) 0.0235(7) Uani 1 1 d . . .
H1 H 0.3571 0.0780 0.6324 0.028 Uiso 1 1 calc R . .
C2 C 0.2244(3) 0.11161(11) 0.5124(4) 0.0228(7) Uani 1 1 d . . .
C3 C 0.1732(4) 0.11392(13) 0.3744(4) 0.0283(8) Uani 1 1 d . . .
H3 H 0.1052 0.1344 0.3526 0.034 Uiso 1 1 calc R . .
C4 C 0.2223(4) 0.08611(15) 0.2688(4) 0.0364(9) Uani 1 1 d . . .
H4 H 0.1904 0.0880 0.1729 0.044 Uiso 1 1 calc R . .
C5 C 0.3180(4) 0.05566(13) 0.3045(4) 0.0335(9) Uani 1 1 d . . .
H5 H 0.3506 0.0366 0.2315 0.040 Uiso 1 1 calc R . .
C6 C 0.1747(3) 0.13995(11) 0.6312(4) 0.0201(7) Uani 1 1 d . . .
C7 C 0.1350(3) 0.18447(12) 0.6068(4) 0.0207(7) Uani 1 1 d . . .
H7 H 0.1449 0.1973 0.5141 0.025 Uiso 1 1 calc R . .
C8 C 0.0818(3) 0.20993(12) 0.7164(4) 0.0195(7) Uani 1 1 d . . .
C9 C 0.0651(3) 0.19279(11) 0.8561(3) 0.0180(6) Uani 1 1 d . . .
C10 C 0.1105(3) 0.14889(12) 0.8801(4) 0.0210(7) Uani 1 1 d . . .
H10 H 0.1053 0.1367 0.9742 0.025 Uiso 1 1 calc R . .
C11 C 0.1629(3) 0.12275(12) 0.7709(4) 0.0227(7) Uani 1 1 d . . .
H11 H 0.1910 0.0931 0.7911 0.027 Uiso 1 1 calc R . .
C12 C 0.0353(4) 0.25716(12) 0.6931(4) 0.0222(7) Uani 1 1 d . . .
H12A H 0.0844 0.2711 0.6137 0.027 Uiso 1 1 calc R . .
H12B H -0.0579 0.2570 0.6661 0.027 Uiso 1 1 calc R . .
C13 C -0.0222(4) 0.32569(12) 0.8116(4) 0.0284(8) Uani 1 1 d . . .
H13A H -0.0119 0.3440 0.8982 0.043 Uiso 1 1 calc R . .
H13B H -0.1141 0.3182 0.7977 0.043 Uiso 1 1 calc R . .
H13C H 0.0090 0.3425 0.7281 0.043 Uiso 1 1 calc R . .
C14 C 0.1945(3) 0.29518(13) 0.8435(4) 0.0276(8) Uani 1 1 d . . .
H14A H 0.2454 0.2676 0.8537 0.041 Uiso 1 1 calc R . .
H14B H 0.2070 0.3139 0.9289 0.041 Uiso 1 1 calc R . .
H14C H 0.2233 0.3116 0.7582 0.041 Uiso 1 1 calc R . .
N1 N 0.3672(3) 0.05178(10) 0.4374(3) 0.0235(6) Uani 1 1 d . . .
N2 N 0.0545(3) 0.28369(9) 0.8277(3) 0.0194(6) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.0000 0.5000 0.02156(19) Uani 1 4 d S . .
Pt1 Pt 0.0000 0.237047(6) 1.0000 0.01767(8) Uani 1 2 d S . .
Cl1 Cl 0.59016(16) 0.0000 0.25306(19) 0.0463(4) Uani 1 2 d S . .
 
 
_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
C1 N1 1.346(4) . ?
C1 C2 1.394(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.386(5) . ?
C2 C6 1.486(5) . ?
C3 C4 1.384(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(6) . ?
C4 H4 0.9500 . ?
C5 N1 1.338(5) . ?
C5 H5 0.9500 . ?
C6 C11 1.404(5) . ?
C6 C7 1.407(5) . ?
C7 C8 1.388(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.408(5) . ?
C8 C12 1.503(5) . ?
C9 C10 1.408(5) . ?
C9 Pt1 2.000(3) . ?
C10 C11 1.393(5) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 N2 1.493(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N2 1.488(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 N2 1.488(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N1 Ni1 2.141(3) . ?
N2 Pt1 2.199(3) . ?
Ni1 N1 2.141(3) 2_656 ?
Ni1 N1 2.141(3) 6 ?
Ni1 N1 2.141(3) 5_656 ?
Ni1 Cl1 2.4849(17) . ?
Ni1 Cl1 2.4849(17) 5_656 ?
Pt1 C9 2.000(3) 2_557 ?
Pt1 N2 2.199(3) 2_557 ?
 
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 C1 C2 123.9(3) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C3 C2 C1 117.4(3) . . ?
C3 C2 C6 122.0(3) . . ?
C1 C2 C6 120.5(3) . . ?
C4 C3 C2 119.3(4) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 119.1(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 123.0(4) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C11 C6 C7 117.9(3) . . ?
C11 C6 C2 120.9(3) . . ?
C7 C6 C2 121.2(3) . . ?
C8 C7 C6 120.9(3) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C7 C8 C9 122.1(3) . . ?
C7 C8 C12 122.3(3) . . ?
C9 C8 C12 115.6(3) . . ?
C10 C9 C8 116.2(3) . . ?
C10 C9 Pt1 128.3(2) . . ?
C8 C9 Pt1 115.0(2) . . ?
C11 C10 C9 122.3(3) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C10 C11 C6 120.5(3) . . ?
C10 C11 H11 119.7 . . ?
C6 C11 H11 119.7 . . ?
N2 C12 C8 109.6(3) . . ?
N2 C12 H12A 109.8 . . ?
C8 C12 H12A 109.8 . . ?
N2 C12 H12B 109.8 . . ?
C8 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 H14A 109.5 . . ?
N2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C5 N1 C1 117.2(3) . . ?
C5 N1 Ni1 123.4(2) . . ?
C1 N1 Ni1 119.1(2) . . ?
C13 N2 C14 109.2(3) . . ?
C13 N2 C12 107.2(3) . . ?
C14 N2 C12 109.1(3) . . ?
C13 N2 Pt1 117.9(2) . . ?
C14 N2 Pt1 109.0(2) . . ?
C12 N2 Pt1 104.1(2) . . ?
N1 Ni1 N1 180.00(11) 2_656 6 ?
N1 Ni1 N1 87.65(16) 2_656 . ?
N1 Ni1 N1 92.35(16) 6 . ?
N1 Ni1 N1 92.35(16) 2_656 5_656 ?
N1 Ni1 N1 87.65(16) 6 5_656 ?
N1 Ni1 N1 180.00(11) . 5_656 ?
N1 Ni1 Cl1 90.55(8) 2_656 . ?
N1 Ni1 Cl1 89.45(8) 6 . ?
N1 Ni1 Cl1 89.45(8) . . ?
N1 Ni1 Cl1 90.55(8) 5_656 . ?
N1 Ni1 Cl1 89.45(8) 2_656 5_656 ?
N1 Ni1 Cl1 90.55(8) 6 5_656 ?
N1 Ni1 Cl1 90.55(8) . 5_656 ?
N1 Ni1 Cl1 89.45(8) 5_656 5_656 ?
Cl1 Ni1 Cl1 180.0 . 5_656 ?
C9 Pt1 C9 97.38(19) . 2_557 ?
C9 Pt1 N2 174.09(11) . 2_557 ?
C9 Pt1 N2 80.83(13) 2_557 2_557 ?
C9 Pt1 N2 80.83(13) . . ?
C9 Pt1 N2 174.09(11) 2_557 . ?
N2 Pt1 N2 101.51(15) 2_557 . ?
 
_diffrn_measured_fraction_theta_max    0.994
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.994
_refine_diff_density_max    1.647
_refine_diff_density_min   -1.499
_refine_diff_density_rms    0.126
