 
data_2005slh0424
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C40 H28 I2 N8 Ni'
_chemical_formula_weight          933.21
 
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'
 'I'  'I'  -0.4742   1.8119
 '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/c
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    25.0178(10)
_cell_length_b                    8.8338(2)
_cell_length_c                    16.5583(6)
_cell_angle_alpha                 90.00
_cell_angle_beta                  97.264(2)
_cell_angle_gamma                 90.00
_cell_volume                      3630.1(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4266
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        lath
_exptl_crystal_colour             orange
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.708
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1832
_exptl_absorpt_coefficient_mu     2.277
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6588
_exptl_absorpt_correction_T_max   0.9559
_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             20594
_diffrn_reflns_av_R_equivalents   0.0459
_diffrn_reflns_av_sigmaI/netI     0.0381
_diffrn_reflns_limit_h_min        -32
_diffrn_reflns_limit_h_max        32
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          3.14
_diffrn_reflns_theta_max          27.50
_reflns_number_total              4173
_reflns_number_gt                 3603
_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, 1997)'
_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)+(0.0510P)²+28.7479P] 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        0.00026(12)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          4173
_refine_ls_number_parameters      233
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0508
_refine_ls_R_factor_gt            0.0416
_refine_ls_wR_factor_ref          0.1101
_refine_ls_wR_factor_gt           0.1040
_refine_ls_goodness_of_fit_ref    1.042
_refine_ls_restrained_S_all       1.042
_refine_ls_shift/su_max           0.002
_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 0.86110(16) 0.5286(4) 0.3626(2) 0.0192(8) Uani 1 1 d . . .
C2 C 0.87189(18) 0.3922(5) 0.4075(3) 0.0258(9) Uani 1 1 d . . .
C3 C 0.80953(17) 0.4708(5) 0.4884(3) 0.0243(9) Uani 1 1 d . . .
C4 C 0.88327(18) 0.5740(6) 0.2871(3) 0.0274(9) Uani 1 1 d . . .
C5 C 0.88612(18) 0.4724(5) 0.2212(3) 0.0290(10) Uani 1 1 d . . .
H5 H 0.8737 0.3712 0.2246 0.035 Uiso 1 1 calc R . .
C6 C 0.9065(2) 0.5197(7) 0.1538(3) 0.0383(12) Uani 1 1 d . . .
H6 H 0.9079 0.4514 0.1098 0.046 Uiso 1 1 calc R . .
C7 C 0.9256(2) 0.6688(7) 0.1475(3) 0.0417(12) Uani 1 1 d . . .
H7 H 0.9403 0.7010 0.1002 0.050 Uiso 1 1 calc R . .
C8 C 0.9227(2) 0.7654(6) 0.2105(3) 0.0375(12) Uani 1 1 d . . .
H8 H 0.9356 0.8660 0.2069 0.045 Uiso 1 1 calc R . .
C9 C 0.9013(2) 0.7207(6) 0.2800(3) 0.0343(11) Uani 1 1 d . . .
H9 H 0.8990 0.7911 0.3229 0.041 Uiso 1 1 calc R . .
C10 C 0.91302(19) 0.2780(5) 0.3965(3) 0.0306(10) Uani 1 1 d . . .
C11 C 0.90685(18) 0.1317(5) 0.4263(3) 0.0252(9) Uani 1 1 d . . .
H11 H 0.8750 0.1066 0.4492 0.030 Uiso 1 1 calc R . .
C12 C 0.9458(2) 0.0247(7) 0.4230(3) 0.0454(13) Uani 1 1 d . . .
H12 H 0.9407 -0.0743 0.4431 0.054 Uiso 1 1 calc R . .
C13 C 0.9926(3) 0.0589(8) 0.3907(4) 0.0538(16) Uani 1 1 d . . .
H13 H 1.0197 -0.0159 0.3886 0.065 Uiso 1 1 calc R . .
C14 C 0.9998(2) 0.2050(8) 0.3611(4) 0.0507(15) Uani 1 1 d . . .
H14 H 1.0318 0.2286 0.3383 0.061 Uiso 1 1 calc R . .
C15 C 0.9613(2) 0.3146(7) 0.3647(3) 0.0409(12) Uani 1 1 d . . .
H15 H 0.9670 0.4142 0.3459 0.049 Uiso 1 1 calc R . .
C16 C 0.77976(15) 0.4431(4) 0.5599(2) 0.0179(8) Uani 1 1 d . . .
C17 C 0.78276(18) 0.3090(5) 0.6020(3) 0.0252(9) Uani 1 1 d . . .
H17 H 0.8035 0.2270 0.5857 0.030 Uiso 1 1 calc R . .
C18 C 0.75514(19) 0.2958(5) 0.6682(3) 0.0297(10) Uani 1 1 d . . .
H18 H 0.7565 0.2044 0.6987 0.036 Uiso 1 1 calc R . .
C19 C 0.72523(19) 0.4178(6) 0.6898(3) 0.0309(10) Uani 1 1 d . . .
H19 H 0.7060 0.4116 0.7356 0.037 Uiso 1 1 calc R . .
C20 C 0.72375(17) 0.5500(5) 0.6434(3) 0.0230(9) Uani 1 1 d . . .
H20 H 0.7031 0.6334 0.6582 0.028 Uiso 1 1 calc R . .
N1 N 0.80156(15) 0.6047(4) 0.4503(2) 0.0257(8) Uani 1 1 d . . .
N2 N 0.82594(15) 0.6293(4) 0.3856(2) 0.0271(8) Uani 1 1 d . . .
N3 N 0.84369(15) 0.3647(4) 0.4696(2) 0.0251(8) Uani 1 1 d . . .
N4 N 0.75060(13) 0.5630(4) 0.57860(19) 0.0168(6) Uani 1 1 d . . .
I1 I 0.663050(11) 0.61821(3) 0.405454(16) 0.02477(13) Uani 1 1 d . . .
Ni1 Ni 0.7500 0.7500 0.5000 0.01586(17) 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 N2 1.340(5) . ?
C1 C2 1.423(6) . ?
C1 C4 1.486(6) . ?
C2 N3 1.340(6) . ?
C2 C10 1.469(6) . ?
C3 N3 1.332(5) . ?
C3 N1 1.344(6) . ?
C3 C16 1.496(6) . ?
C4 C9 1.382(7) . ?
C4 C5 1.421(7) . ?
C5 C6 1.350(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.410(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.357(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.387(7) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.399(6) . ?
C10 C15 1.415(7) . ?
C11 C12 1.364(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.400(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.372(8) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 N4 1.344(5) . ?
C16 C17 1.372(6) . ?
C17 C18 1.373(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.396(6) . ?
C19 H19 0.9500 . ?
C20 N4 1.341(5) . ?
C20 H20 0.9500 . ?
N1 N2 1.317(5) . ?
N1 Ni1 2.063(4) . ?
N4 Ni1 2.102(3) . ?
I1 Ni1 2.7707(3) . ?
Ni1 N1 2.063(4) 7_666 ?
Ni1 N4 2.102(3) 7_666 ?
Ni1 I1 2.7707(3) 7_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
N2 C1 C2 120.1(4) . . ?
N2 C1 C4 112.8(4) . . ?
C2 C1 C4 127.0(4) . . ?
N3 C2 C1 118.1(4) . . ?
N3 C2 C10 114.5(4) . . ?
C1 C2 C10 127.3(4) . . ?
N3 C3 N1 124.8(4) . . ?
N3 C3 C16 118.0(4) . . ?
N1 C3 C16 117.1(4) . . ?
C9 C4 C5 118.6(4) . . ?
C9 C4 C1 119.0(4) . . ?
C5 C4 C1 122.4(4) . . ?
C6 C5 C4 119.9(5) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 121.2(5) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C6 118.6(5) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
C7 C8 C9 121.6(5) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C4 C9 C8 120.1(5) . . ?
C4 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C15 118.7(5) . . ?
C11 C10 C2 118.7(4) . . ?
C15 C10 C2 122.2(5) . . ?
C12 C11 C10 121.0(5) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 120.6(6) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 119.3(5) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C15 C14 C13 120.9(5) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C10 119.4(6) . . ?
C14 C15 H15 120.3 . . ?
C10 C15 H15 120.3 . . ?
N4 C16 C17 124.0(4) . . ?
N4 C16 C3 113.1(3) . . ?
C17 C16 C3 122.8(4) . . ?
C16 C17 C18 118.6(4) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
C17 C18 C19 118.9(4) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C18 C19 C20 119.1(4) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
N4 C20 C19 122.1(4) . . ?
N4 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
N2 N1 C3 118.1(4) . . ?
N2 N1 Ni1 126.8(3) . . ?
C3 N1 Ni1 115.1(3) . . ?
N1 N2 C1 120.7(4) . . ?
C3 N3 C2 117.9(4) . . ?
C20 N4 C16 117.3(3) . . ?
C20 N4 Ni1 126.7(3) . . ?
C16 N4 Ni1 116.0(3) . . ?
N1 Ni1 N1 180.00(19) 7_666 . ?
N1 Ni1 N4 101.41(14) 7_666 . ?
N1 Ni1 N4 78.59(14) . . ?
N1 Ni1 N4 78.59(14) 7_666 7_666 ?
N1 Ni1 N4 101.41(14) . 7_666 ?
N4 Ni1 N4 180.000(1) . 7_666 ?
N1 Ni1 I1 89.95(10) 7_666 7_666 ?
N1 Ni1 I1 90.05(10) . 7_666 ?
N4 Ni1 I1 92.10(9) . 7_666 ?
N4 Ni1 I1 87.90(9) 7_666 7_666 ?
N1 Ni1 I1 90.05(10) 7_666 . ?
N1 Ni1 I1 89.95(10) . . ?
N4 Ni1 I1 87.90(9) . . ?
N4 Ni1 I1 92.10(9) 7_666 . ?
I1 Ni1 I1 180.000(8) 7_666 . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    1.507
_refine_diff_density_min   -0.912
_refine_diff_density_rms    0.136
