 
data_2005slh0421
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C56 H48 N8 Ni O4 P2 S4'
_chemical_formula_weight          1145.91
 
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'
 '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'
 'S'  'S'   0.1246   0.1234
 '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'
 
_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.2767(11)
_cell_length_b                    10.467(2)
_cell_length_c                    15.0969(13)
_cell_angle_alpha                 79.283(13)
_cell_angle_beta                  84.701(8)
_cell_angle_gamma                 65.476(16)
_cell_volume                      1310.2(4)
_cell_formula_units_Z             1
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     5860
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        lath
_exptl_crystal_colour             red
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.452
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              594
_exptl_absorpt_coefficient_mu     0.647
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9264
_exptl_absorpt_correction_T_max   0.9872
_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             26207
_diffrn_reflns_av_R_equivalents   0.0588
_diffrn_reflns_av_sigmaI/netI     0.0535
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.04
_diffrn_reflns_theta_max          27.49
_reflns_number_total              5955
_reflns_number_gt                 4790
_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)'
_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)+(0.0340P)²+1.1455P] 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        0.0056(11)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          5955
_refine_ls_number_parameters      343
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0573
_refine_ls_R_factor_gt            0.0416
_refine_ls_wR_factor_ref          0.0991
_refine_ls_wR_factor_gt           0.0918
_refine_ls_goodness_of_fit_ref    1.038
_refine_ls_restrained_S_all       1.038
_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 0.6495(3) 0.9751(2) 0.57205(17) 0.0281(5) Uani 1 1 d . . .
H1A H 0.6405 0.9925 0.5063 0.042 Uiso 1 1 calc R . .
H1B H 0.7083 1.0258 0.5889 0.042 Uiso 1 1 calc R . .
H1C H 0.5433 1.0094 0.5998 0.042 Uiso 1 1 calc R . .
C2 C 0.7992(3) 0.5663(2) 0.68195(14) 0.0187(4) Uani 1 1 d . . .
C3 C 0.7848(3) 0.5198(2) 0.77386(15) 0.0227(5) Uani 1 1 d . . .
H3 H 0.6902 0.5686 0.8056 0.027 Uiso 1 1 calc R . .
C4 C 0.9058(3) 0.4041(3) 0.81914(16) 0.0271(5) Uani 1 1 d . . .
H4 H 0.8937 0.3733 0.8816 0.032 Uiso 1 1 calc R . .
C5 C 1.0458(3) 0.3323(2) 0.77359(17) 0.0259(5) Uani 1 1 d . . .
C6 C 1.0650(3) 0.3792(3) 0.68288(16) 0.0254(5) Uani 1 1 d . . .
H6 H 1.1617 0.3327 0.6521 0.030 Uiso 1 1 calc R . .
C7 C 0.9414(3) 0.4951(2) 0.63747(16) 0.0229(5) Uani 1 1 d . . .
H7 H 0.9539 0.5263 0.5751 0.028 Uiso 1 1 calc R . .
C8 C 1.3062(3) 0.1444(3) 0.7817(2) 0.0462(8) Uani 1 1 d . . .
H8A H 1.2898 0.1086 0.7297 0.069 Uiso 1 1 calc R . .
H8B H 1.3751 0.0646 0.8248 0.069 Uiso 1 1 calc R . .
H8C H 1.3561 0.2113 0.7616 0.069 Uiso 1 1 calc R . .
C9 C 0.7172(3) 0.4525(2) 0.23733(14) 0.0174(4) Uani 1 1 d . . .
C10 C 0.8526(3) 0.3215(2) 0.25821(15) 0.0203(5) Uani 1 1 d . . .
C11 C 0.7858(3) 0.3318(2) 0.40644(14) 0.0187(5) Uani 1 1 d . . .
C12 C 0.6723(3) 0.5360(2) 0.14560(15) 0.0216(5) Uani 1 1 d . . .
C13 C 0.7854(3) 0.5525(3) 0.08129(15) 0.0254(5) Uani 1 1 d . . .
H13 H 0.8947 0.5084 0.0957 0.030 Uiso 1 1 calc R . .
C14 C 0.7382(3) 0.6329(3) -0.00320(17) 0.0318(6) Uani 1 1 d . . .
H14 H 0.8152 0.6443 -0.0462 0.038 Uiso 1 1 calc R . .
C15 C 0.5786(3) 0.6969(3) -0.02531(17) 0.0344(6) Uani 1 1 d . . .
H15 H 0.5468 0.7504 -0.0836 0.041 Uiso 1 1 calc R . .
C16 C 0.4670(3) 0.6822(3) 0.03788(16) 0.0313(6) Uani 1 1 d . . .
H16 H 0.3579 0.7270 0.0232 0.038 Uiso 1 1 calc R . .
C17 C 0.5128(3) 0.6023(3) 0.12297(16) 0.0273(5) Uani 1 1 d . . .
H17 H 0.4347 0.5929 0.1659 0.033 Uiso 1 1 calc R . .
C18 C 0.9569(3) 0.2359(2) 0.19122(15) 0.0214(5) Uani 1 1 d . . .
C19 C 1.1192(3) 0.1651(2) 0.20642(15) 0.0236(5) Uani 1 1 d . . .
H19 H 1.1623 0.1736 0.2586 0.028 Uiso 1 1 calc R . .
C20 C 1.2181(3) 0.0820(3) 0.14510(17) 0.0317(6) Uani 1 1 d . . .
H20 H 1.3286 0.0335 0.1558 0.038 Uiso 1 1 calc R . .
C21 C 1.1566(3) 0.0695(3) 0.06876(17) 0.0345(6) Uani 1 1 d . . .
H21 H 1.2247 0.0142 0.0264 0.041 Uiso 1 1 calc R . .
C22 C 0.9945(3) 0.1384(3) 0.05427(17) 0.0340(6) Uani 1 1 d . . .
H22 H 0.9519 0.1288 0.0022 0.041 Uiso 1 1 calc R . .
C23 C 0.8946(3) 0.2208(3) 0.11484(16) 0.0288(5) Uani 1 1 d . . .
H23 H 0.7838 0.2670 0.1046 0.035 Uiso 1 1 calc R . .
C24 C 0.2732(3) 0.7193(2) 0.35091(15) 0.0203(5) Uani 1 1 d . . .
H24 H 0.3551 0.6786 0.3089 0.024 Uiso 1 1 calc R . .
C25 C 0.1333(3) 0.8305(2) 0.31840(15) 0.0227(5) Uani 1 1 d . . .
H25 H 0.1209 0.8645 0.2555 0.027 Uiso 1 1 calc R . .
C26 C 0.0122(3) 0.8915(2) 0.37818(16) 0.0238(5) Uani 1 1 d . . .
H26 H -0.0845 0.9673 0.3573 0.029 Uiso 1 1 calc R . .
C27 C 0.0363(3) 0.8384(2) 0.46988(15) 0.0223(5) Uani 1 1 d . . .
H27 H -0.0441 0.8774 0.5130 0.027 Uiso 1 1 calc R . .
C28 C 0.1790(3) 0.7280(2) 0.49704(14) 0.0178(4) Uani 1 1 d . . .
N1 N 0.6481(2) 0.4449(2) 0.38838(12) 0.0194(4) Uani 1 1 d . . .
N2 N 0.6186(2) 0.5094(2) 0.30299(12) 0.0207(4) Uani 1 1 d . . .
N3 N 0.8893(2) 0.2664(2) 0.34455(12) 0.0203(4) Uani 1 1 d . . .
N4 N 0.2978(2) 0.66684(19) 0.43895(12) 0.0174(4) Uani 1 1 d . . .
O1 O 0.73241(18) 0.82447(16) 0.60318(11) 0.0222(3) Uani 1 1 d . . .
O2 O 1.1563(2) 0.21586(19) 0.82442(13) 0.0373(4) Uani 1 1 d . . .
P1 P 0.64142(7) 0.71938(6) 0.62168(4) 0.01816(14) Uani 1 1 d . . .
S1 S 0.61510(7) 0.67832(6) 0.50011(4) 0.02037(14) Uani 1 1 d . . .
S2 S 0.45050(7) 0.79482(6) 0.69798(4) 0.02331(14) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.5000 0.5000 0.01547(11) 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 O1 1.443(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.396(3) . ?
C2 C7 1.397(3) . ?
C2 P1 1.815(2) . ?
C3 C4 1.378(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(3) . ?
C4 H4 0.9500 . ?
C5 O2 1.373(3) . ?
C5 C6 1.388(3) . ?
C6 C7 1.392(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 O2 1.435(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.332(3) . ?
C9 C10 1.429(3) . ?
C9 C12 1.486(3) . ?
C10 N3 1.337(3) . ?
C10 C18 1.482(3) . ?
C11 N3 1.338(3) . ?
C11 N1 1.340(3) . ?
C11 C28 1.484(3) 2_666 ?
C12 C17 1.393(3) . ?
C12 C13 1.405(3) . ?
C13 C14 1.387(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.391(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.379(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.391(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.394(3) . ?
C18 C23 1.398(3) . ?
C19 C20 1.391(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.390(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.383(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 N4 1.342(3) . ?
C24 C25 1.390(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.394(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.382(3) . ?
C27 H27 0.9500 . ?
C28 N4 1.355(3) . ?
C28 C11 1.484(3) 2_666 ?
N1 N2 1.335(3) . ?
N1 Ni1 2.0823(18) . ?
N4 Ni1 2.1022(19) . ?
O1 P1 1.6166(16) . ?
P1 S2 1.9717(9) . ?
P1 S1 2.0189(8) . ?
S1 Ni1 2.5061(7) . ?
Ni1 N1 2.0823(18) 2_666 ?
Ni1 N4 2.1022(19) 2_666 ?
Ni1 S1 2.5061(7) 2_666 ?
 
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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C7 118.3(2) . . ?
C3 C2 P1 121.40(17) . . ?
C7 C2 P1 120.25(17) . . ?
C4 C3 C2 120.9(2) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.2(2) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
O2 C5 C6 124.7(2) . . ?
O2 C5 C4 115.3(2) . . ?
C6 C5 C4 120.0(2) . . ?
C5 C6 C7 119.4(2) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C6 C7 C2 121.2(2) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 120.0(2) . . ?
N2 C9 C12 114.4(2) . . ?
C10 C9 C12 125.54(19) . . ?
N3 C10 C9 119.1(2) . . ?
N3 C10 C18 115.5(2) . . ?
C9 C10 C18 125.3(2) . . ?
N3 C11 N1 125.2(2) . . ?
N3 C11 C28 118.2(2) . 2_666 ?
N1 C11 C28 116.61(19) . 2_666 ?
C17 C12 C13 118.8(2) . . ?
C17 C12 C9 119.1(2) . . ?
C13 C12 C9 122.1(2) . . ?
C14 C13 C12 120.2(2) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.4(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C16 C15 C14 119.6(2) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C17 120.6(2) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C16 C17 C12 120.4(2) . . ?
C16 C17 H17 119.8 . . ?
C12 C17 H17 119.8 . . ?
C19 C18 C23 119.5(2) . . ?
C19 C18 C10 119.3(2) . . ?
C23 C18 C10 121.2(2) . . ?
C20 C19 C18 120.0(2) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 120.4(2) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C22 119.6(2) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C23 C22 C21 120.6(2) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C18 119.9(2) . . ?
C22 C23 H23 120.1 . . ?
C18 C23 H23 120.1 . . ?
N4 C24 C25 122.9(2) . . ?
N4 C24 H24 118.5 . . ?
C25 C24 H24 118.5 . . ?
C26 C25 C24 119.6(2) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C27 118.1(2) . . ?
C25 C26 H26 121.0 . . ?
C27 C26 H26 121.0 . . ?
C28 C27 C26 118.9(2) . . ?
C28 C27 H27 120.6 . . ?
C26 C27 H27 120.6 . . ?
N4 C28 C27 123.5(2) . . ?
N4 C28 C11 114.68(19) . 2_666 ?
C27 C28 C11 121.9(2) . 2_666 ?
N2 N1 C11 118.35(18) . . ?
N2 N1 Ni1 126.75(15) . . ?
C11 N1 Ni1 114.90(14) . . ?
C9 N2 N1 119.81(19) . . ?
C10 N3 C11 116.6(2) . . ?
C24 N4 C28 117.03(19) . . ?
C24 N4 Ni1 128.15(15) . . ?
C28 N4 Ni1 114.83(14) . . ?
C1 O1 P1 121.60(14) . . ?
C5 O2 C8 117.1(2) . . ?
O1 P1 C2 97.28(9) . . ?
O1 P1 S2 111.15(7) . . ?
C2 P1 S2 112.24(8) . . ?
O1 P1 S1 106.34(6) . . ?
C2 P1 S1 109.64(8) . . ?
S2 P1 S1 118.06(4) . . ?
P1 S1 Ni1 116.58(3) . . ?
N1 Ni1 N1 180.0 . 2_666 ?
N1 Ni1 N4 101.33(7) . . ?
N1 Ni1 N4 78.67(7) 2_666 . ?
N1 Ni1 N4 78.67(7) . 2_666 ?
N1 Ni1 N4 101.33(7) 2_666 2_666 ?
N4 Ni1 N4 180.00(9) . 2_666 ?
N1 Ni1 S1 85.10(5) . . ?
N1 Ni1 S1 94.90(5) 2_666 . ?
N4 Ni1 S1 88.20(5) . . ?
N4 Ni1 S1 91.80(5) 2_666 . ?
N1 Ni1 S1 94.90(5) . 2_666 ?
N1 Ni1 S1 85.10(5) 2_666 2_666 ?
N4 Ni1 S1 91.80(5) . 2_666 ?
N4 Ni1 S1 88.20(5) 2_666 2_666 ?
S1 Ni1 S1 180.0 . 2_666 ?
 
_diffrn_measured_fraction_theta_max    0.992
_diffrn_reflns_theta_full              27.49
_diffrn_measured_fraction_theta_full   0.992
_refine_diff_density_max    0.508
_refine_diff_density_min   -0.375
_refine_diff_density_rms    0.071
