 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2001-12-12 at 17:13:12
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.2
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : ljf067 struct dreduc gaussian sortav
 
 
data_ljf067
 
_audit_creation_date            2001-12-12T17:13:12-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.2
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category        FM
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'Cl, C18 H20 N3 Ni O2'
_chemical_formula_sum                   'C18 H20 Cl N3 Ni O2'
_chemical_formula_weight                404.53
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 21/c'
_symmetry_space_group_name_Hall         '-P 2ybc'
_symmetry_Int_Tables_number             14
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                          10.8360(1)
_cell_length_b                          14.6318(2)
_cell_length_c                          12.1862(2)
_cell_angle_alpha                       90
_cell_angle_beta                        113.8377(7)
_cell_angle_gamma                       90
_cell_volume                            1767.30(10)
_cell_formula_units_Z                   4
_cell_measurement_temperature           100(2)
_cell_measurement_reflns_used           7333
_cell_measurement_theta_min             1
_cell_measurement_theta_max             34.97
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   orange
_exptl_crystal_size_max                 0.34
_exptl_crystal_size_mid                 0.29
_exptl_crystal_size_min                 0.27
_exptl_crystal_density_diffrn           1.52
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    840
loop_
    _exptl_crystal_face_index_h
    _exptl_crystal_face_index_k
    _exptl_crystal_face_index_l
    _exptl_crystal_face_perp_dist
1 1 0 0.15
-1 -1 0 0.19
-1 1 0 0.17
1 -1 0 0.12
1 0 -2 0.11
-1 0 2 0.16
 
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           1.265
_exptl_absorpt_correction_type          gaussian
_exptl_absorpt_process_details
;
   P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
   (1965), 18, 1035-1038
;
_exptl_absorpt_correction_T_min         0.623
_exptl_absorpt_correction_T_max         0.769
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             100(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_detector                        'CCD plate'
_diffrn_orient_matrix_type              'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11             -0.656527E-1
_diffrn_orient_matrix_ub_12             -0.322901E-1
_diffrn_orient_matrix_ub_13             0.251848E-1
_diffrn_orient_matrix_ub_21             0.215366E-1
_diffrn_orient_matrix_ub_22             -0.591244E-1
_diffrn_orient_matrix_ub_23             -0.29509E-1
_diffrn_orient_matrix_ub_31             0.735189E-1
_diffrn_orient_matrix_ub_32             -0.115153E-1
_diffrn_orient_matrix_ub_33             0.808912E-1
_diffrn_measurement_device              '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type         KappaCCD
_diffrn_measurement_method              'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents         0.0376
_diffrn_reflns_av_unetI/netI            0.026
_diffrn_reflns_number                   31674
_diffrn_reflns_limit_h_min              -17
_diffrn_reflns_limit_h_max              17
_diffrn_reflns_limit_k_min              -23
_diffrn_reflns_limit_k_max              21
_diffrn_reflns_limit_l_min              -19
_diffrn_reflns_limit_l_max              19
_diffrn_reflns_theta_min                2.05
_diffrn_reflns_theta_max                35.01
_diffrn_reflns_theta_full               35.01
_diffrn_measured_fraction_theta_full
                                        0.996
_diffrn_measured_fraction_theta_max
                                        0.996
_reflns_number_total                    7765
_reflns_number_gt                       6402
_reflns_threshold_expression            >2sigma(I)
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement
                                       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
                             'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution           'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1999)'
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_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)+(0.0351P)²+0.7763P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            none
_refine_ls_number_reflns                7765
_refine_ls_number_parameters            227
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0432
_refine_ls_R_factor_gt                  0.0315
_refine_ls_wR_factor_ref                0.0785
_refine_ls_wR_factor_gt                 0.0743
_refine_ls_goodness_of_fit_ref          1.018
_refine_ls_restrained_S_all             1.018
_refine_ls_shift/su_max                 0.001
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.528
_refine_diff_density_min                -0.682
_refine_diff_density_rms                0.069
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
Ni Ni 0.3393 1.1124 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
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
Ni Ni 0.223635(13) 0.248570(9) 0.596503(12) 0.01464(4) Uani 1 1 d . . .
Cl1 Cl 0.92789(3) 0.39373(2) 1.07571(3) 0.02274(6) Uani 1 1 d . . .
N1 N 0.33800(9) 0.20145(6) 0.74983(8) 0.01618(15) Uani 1 1 d . . .
N2 N 0.20290(9) 0.12496(7) 0.54407(8) 0.01823(16) Uani 1 1 d . . .
H2 H 0.1264 0.1021 0.5513 0.022 Uiso 1 1 calc R . .
N3 N 0.12142(9) 0.27875(7) 0.43849(8) 0.01840(16) Uani 1 1 d . . .
O1 O 0.63595(9) 0.34860(6) 0.96845(7) 0.02397(17) Uani 1 1 d . . .
H10 H 0.7174 0.3637 1.0035 0.036 Uiso 1 1 calc R . .
O2 O 0.24275(8) 0.36576(5) 0.65432(7) 0.01786(14) Uani 1 1 d . . .
C1 C 0.41234(10) 0.25032(7) 0.84015(9) 0.01536(16) Uani 1 1 d . . .
H1 H 0.4119 0.314 0.8249 0.018 Uiso 1 1 calc R . .
C2 C 0.34219(12) 0.10035(8) 0.75191(10) 0.0209(2) Uani 1 1 d . . .
H2A H 0.2705 0.0754 0.7741 0.025 Uiso 1 1 calc R . .
H2B H 0.4307 0.0783 0.8105 0.025 Uiso 1 1 calc R . .
C3 C 0.31970(12) 0.07138(8) 0.62548(11) 0.0226(2) Uani 1 1 d . . .
H3A H 0.4006 0.0847 0.6097 0.027 Uiso 1 1 calc R . .
H3B H 0.3003 0.0051 0.6143 0.027 Uiso 1 1 calc R . .
C4 C 0.17693(13) 0.12329(8) 0.41505(10) 0.0232(2) Uani 1 1 d . . .
H4A H 0.1404 0.0632 0.3792 0.028 Uiso 1 1 calc R . .
H4B H 0.261 0.1353 0.4038 0.028 Uiso 1 1 calc R . .
C5 C 0.07449(13) 0.19831(9) 0.35817(10) 0.0241(2) Uani 1 1 d . . .
H5A H 0.0695 0.2131 0.2772 0.029 Uiso 1 1 calc R . .
H5B H -0.016 0.1789 0.3509 0.029 Uiso 1 1 calc R . .
C6 C 0.09007(11) 0.35990(8) 0.39445(9) 0.01933(19) Uani 1 1 d . . .
H6 H 0.0351 0.3654 0.3112 0.023 Uiso 1 1 calc R . .
C101 C 0.49741(10) 0.22231(7) 0.96281(9) 0.01531(16) Uani 1 1 d . . .
C102 C 0.46632(11) 0.14972(7) 1.02291(10) 0.01830(18) Uani 1 1 d . . .
H102 H 0.39 0.1124 0.981 0.022 Uiso 1 1 calc R . .
C103 C 0.54565(11) 0.13202(8) 1.14251(10) 0.01954(19) Uani 1 1 d . . .
H103 H 0.5233 0.0831 1.1824 0.023 Uiso 1 1 calc R . .
C104 C 0.65841(11) 0.18611(8) 1.20431(10) 0.01951(19) Uani 1 1 d . . .
H104 H 0.7137 0.1732 1.2859 0.023 Uiso 1 1 calc R . .
C105 C 0.69032(11) 0.25857(8) 1.14739(9) 0.01876(19) Uani 1 1 d . . .
H105 H 0.7671 0.2953 1.1902 0.023 Uiso 1 1 calc R . .
C106 C 0.60984(10) 0.27776(7) 1.02725(9) 0.01608(17) Uani 1 1 d . . .
C111 C 0.13316(10) 0.44239(8) 0.46349(9) 0.01733(18) Uani 1 1 d . . .
C112 C 0.09894(11) 0.52675(8) 0.40188(10) 0.0209(2) Uani 1 1 d . . .
H112 H 0.046 0.527 0.3179 0.025 Uiso 1 1 calc R . .
C113 C 0.14054(12) 0.60832(8) 0.46094(11) 0.0224(2) Uani 1 1 d . . .
H113 H 0.1165 0.6646 0.4187 0.027 Uiso 1 1 calc R . .
C114 C 0.21942(12) 0.60709(8) 0.58510(10) 0.0216(2) Uani 1 1 d . . .
H114 H 0.2508 0.6631 0.6263 0.026 Uiso 1 1 calc R . .
C115 C 0.25214(11) 0.52594(8) 0.64830(10) 0.01970(19) Uani 1 1 d . . .
H115 H 0.3042 0.5272 0.7324 0.024 Uiso 1 1 calc R . .
C116 C 0.20936(10) 0.44082(7) 0.58969(9) 0.01638(17) Uani 1 1 d . . .
 
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_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
Ni O2 1.8335(8) . ?
Ni N3 1.8455(9) . ?
Ni N2 1.9011(10) . ?
Ni N1 1.9055(9) . ?
N1 C1 1.2864(13) . ?
N1 C2 1.4798(14) . ?
N2 C3 1.4784(15) . ?
N2 C4 1.4813(15) . ?
N2 H2 0.93 . ?
N3 C6 1.2907(15) . ?
N3 C5 1.4831(15) . ?
O1 C106 1.3533(13) . ?
O1 H10 0.84 . ?
O2 C116 1.3141(13) . ?
C1 C101 1.4623(14) . ?
C1 H1 0.95 . ?
C2 C3 1.5197(16) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 C5 1.5152(18) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 C111 1.4370(16) . ?
C6 H6 0.95 . ?
C101 C102 1.4062(15) . ?
C101 C106 1.4093(15) . ?
C102 C103 1.3847(15) . ?
C102 H102 0.95 . ?
C103 C104 1.3938(16) . ?
C103 H103 0.95 . ?
C104 C105 1.3851(15) . ?
C104 H104 0.95 . ?
C105 C106 1.3967(15) . ?
C105 H105 0.95 . ?
C111 C112 1.4141(15) . ?
C111 C116 1.4216(14) . ?
C112 C113 1.3724(17) . ?
C112 H112 0.95 . ?
C113 C114 1.4052(17) . ?
C113 H113 0.95 . ?
C114 C115 1.3813(16) . ?
C114 H114 0.95 . ?
C115 C116 1.4173(15) . ?
C115 H115 0.95 . ?
 
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
O2 Ni N3 95.98(4) . . ?
O2 Ni N2 176.96(4) . . ?
N3 Ni N2 86.41(4) . . ?
O2 Ni N1 91.94(4) . . ?
N3 Ni N1 171.11(4) . . ?
N2 Ni N1 85.81(4) . . ?
C1 N1 C2 122.46(9) . . ?
C1 N1 Ni 124.89(8) . . ?
C2 N1 Ni 112.45(7) . . ?
C3 N2 C4 116.57(9) . . ?
C3 N2 Ni 109.03(7) . . ?
C4 N2 Ni 108.57(7) . . ?
C3 N2 H2 107.4 . . ?
C4 N2 H2 107.4 . . ?
Ni N2 H2 107.4 . . ?
C6 N3 C5 119.56(9) . . ?
C6 N3 Ni 126.87(8) . . ?
C5 N3 Ni 113.57(8) . . ?
C106 O1 H10 109.5 . . ?
C116 O2 Ni 126.17(7) . . ?
N1 C1 C101 129.56(10) . . ?
N1 C1 H1 115.2 . . ?
C101 C1 H1 115.2 . . ?
N1 C2 C3 105.68(9) . . ?
N1 C2 H2A 110.6 . . ?
C3 C2 H2A 110.6 . . ?
N1 C2 H2B 110.6 . . ?
C3 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N2 C3 C2 105.99(9) . . ?
N2 C3 H3A 110.5 . . ?
C2 C3 H3A 110.5 . . ?
N2 C3 H3B 110.5 . . ?
C2 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
N2 C4 C5 105.27(10) . . ?
N2 C4 H4A 110.7 . . ?
C5 C4 H4A 110.7 . . ?
N2 C4 H4B 110.7 . . ?
C5 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
N3 C5 C4 106.30(9) . . ?
N3 C5 H5A 110.5 . . ?
C4 C5 H5A 110.5 . . ?
N3 C5 H5B 110.5 . . ?
C4 C5 H5B 110.5 . . ?
H5A C5 H5B 108.7 . . ?
N3 C6 C111 124.10(10) . . ?
N3 C6 H6 117.9 . . ?
C111 C6 H6 117.9 . . ?
C102 C101 C106 118.67(9) . . ?
C102 C101 C1 124.01(9) . . ?
C106 C101 C1 117.01(9) . . ?
C103 C102 C101 120.79(10) . . ?
C103 C102 H102 119.6 . . ?
C101 C102 H102 119.6 . . ?
C102 C103 C104 119.89(10) . . ?
C102 C103 H103 120.1 . . ?
C104 C103 H103 120.1 . . ?
C105 C104 C103 120.38(10) . . ?
C105 C104 H104 119.8 . . ?
C103 C104 H104 119.8 . . ?
C104 C105 C106 120.16(10) . . ?
C104 C105 H105 119.9 . . ?
C106 C105 H105 119.9 . . ?
O1 C106 C105 122.24(10) . . ?
O1 C106 C101 117.68(9) . . ?
C105 C106 C101 120.08(10) . . ?
C112 C111 C116 120.10(10) . . ?
C112 C111 C6 117.96(10) . . ?
C116 C111 C6 121.93(10) . . ?
C113 C112 C111 121.37(10) . . ?
C113 C112 H112 119.3 . . ?
C111 C112 H112 119.3 . . ?
C112 C113 C114 118.78(11) . . ?
C112 C113 H113 120.6 . . ?
C114 C113 H113 120.6 . . ?
C115 C114 C113 121.24(11) . . ?
C115 C114 H114 119.4 . . ?
C113 C114 H114 119.4 . . ?
C114 C115 C116 121.10(10) . . ?
C114 C115 H115 119.5 . . ?
C116 C115 H115 119.5 . . ?
O2 C116 C115 118.53(9) . . ?
O2 C116 C111 124.11(10) . . ?
C115 C116 C111 117.36(10) . . ?
 
