 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2002-02-23 at 16:04:36
#  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  : ljf074a sortav absorb dreduc struct
 
 
data_ljf074a
 
_audit_creation_date            2002-02-23T16:04:36-00:00
_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                'C16 H28 Br1.25 Cl0.75 Cu N4 O4'
_chemical_formula_sum                   'C16 H28 Br1.25 Cl0.75 Cu N4 O4'
_chemical_formula_weight                530.44
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 1 21/c 1'
_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                          7.5989(12)
_cell_length_b                          11.1613(18)
_cell_length_c                          25.212
_cell_angle_alpha                       90
_cell_angle_beta                        92.44(8)
_cell_angle_gamma                       90
_cell_volume                            2136.4(5)
_cell_formula_units_Z                   4
_cell_measurement_temperature           100(2)
_cell_measurement_reflns_used           14134
_cell_measurement_theta_min             2
_cell_measurement_theta_max             30.034
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   blue
_exptl_crystal_size_max                 0.43
_exptl_crystal_size_mid                 0.25
_exptl_crystal_size_min                 0.08
_exptl_crystal_density_diffrn           1.649
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    1078
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           3.482
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min         0.211
_exptl_absorpt_correction_T_max         0.438
 
#----------------------------------------------------------------------------#
#                   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             0.344373E-1
_diffrn_orient_matrix_ub_12             0.765417E-1
_diffrn_orient_matrix_ub_13             0.182596E-1
_diffrn_orient_matrix_ub_21             -0.100822
_diffrn_orient_matrix_ub_22             0.418443E-1
_diffrn_orient_matrix_ub_23             -0.188512E-1
_diffrn_orient_matrix_ub_31             -0.774491E-1
_diffrn_orient_matrix_ub_32             -0.204385E-1
_diffrn_orient_matrix_ub_33             0.297872E-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         0.0973
_diffrn_reflns_av_unetI/netI            0.0652
_diffrn_reflns_number                   23277
_diffrn_reflns_limit_h_min              -10
_diffrn_reflns_limit_h_max              10
_diffrn_reflns_limit_k_min              -15
_diffrn_reflns_limit_k_max              14
_diffrn_reflns_limit_l_min              -35
_diffrn_reflns_limit_l_max              25
_diffrn_reflns_theta_min                2
_diffrn_reflns_theta_max                30.62
_diffrn_reflns_theta_full               30.62
_diffrn_measured_fraction_theta_full
                                        0.966
_diffrn_measured_fraction_theta_max
                                        0.966
_reflns_number_total                    6357
_reflns_number_gt                       4895
_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)+(0.0855P)²+17.5516P] 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                6357
_refine_ls_number_parameters            244
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.1097
_refine_ls_R_factor_gt                  0.0856
_refine_ls_wR_factor_ref                0.2282
_refine_ls_wR_factor_gt                 0.2138
_refine_ls_goodness_of_fit_ref          1.065
_refine_ls_restrained_S_all             1.065
_refine_ls_shift/su_max                 0
_refine_ls_shift/su_mean                0
_refine_diff_density_max                2.192
_refine_diff_density_min                -1.296
_refine_diff_density_rms                0.168
 
#----------------------------------------------------------------------------#
#                   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
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
Cl Cl 0.1484 0.1585 '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
Cu1 Cu 0.05066(9) 0.12467(7) 0.20787(3) 0.02593(18) Uani 1 1 d . . .
Br1 Br -0.20233(12) 0.25814(10) 0.20882(4) 0.0407(3) Uani 0.5 1 d P . .
Br2 Br -0.11925(10) -0.03588(7) 0.16569(3) 0.0349(2) Uani 0.75 1 d P . .
Cl1 Cl -0.20233(12) 0.25814(10) 0.20882(4) 0.0407(3) Uani 0.5 1 d P . .
Cl2 Cl -0.11925(10) -0.03588(7) 0.16569(3) 0.0349(2) Uani 0.25 1 d P . .
N1 N 0.2110(6) 0.1956(5) 0.14139(19) 0.0293(10) Uani 1 1 d . . .
N4 N 0.2667(8) 0.0174(5) 0.2205(2) 0.0365(12) Uani 1 1 d . . .
H4 H 0.2286 -0.0574 0.2315 0.044 Uiso 1 1 calc R . .
N7 N 0.1942(7) 0.2430(5) 0.25220(19) 0.0285(10) Uani 1 1 d . . .
H7 H 0.1187 0.2902 0.2714 0.034 Uiso 1 1 calc R . .
N100 N 0.1775(9) 0.6421(8) 0.1218(3) 0.0548(18) Uani 1 1 d . . .
O3 O 0.2579(7) 0.5356(5) -0.0174(2) 0.0420(11) Uani 1 1 d . . .
O6 O 0.2439(7) 0.0458(5) 0.01656(19) 0.0418(11) Uani 1 1 d . . .
O101 O 0.0511(9) 0.5845(7) 0.1368(3) 0.071(2) Uani 1 1 d . . .
O102 O 0.3285(8) 0.6192(9) 0.1360(3) 0.085(3) Uani 1 1 d . . .
C3A C 0.3247(11) 0.5837(8) -0.0646(3) 0.0450(17) Uani 1 1 d . . .
H3A1 H 0.3158 0.6713 -0.0638 0.068 Uiso 1 1 calc R . .
H3A2 H 0.2559 0.5528 -0.0954 0.068 Uiso 1 1 calc R . .
H3A3 H 0.4483 0.5604 -0.0672 0.068 Uiso 1 1 calc R . .
C5 C 0.3883(10) 0.0667(7) 0.2622(3) 0.0469(17) Uani 1 1 d . . .
H5A H 0.4981 0.0937 0.2461 0.056 Uiso 1 1 calc R . .
H5B H 0.4193 0.0033 0.2884 0.056 Uiso 1 1 calc R . .
C6 C 0.3053(10) 0.1700(8) 0.2897(3) 0.0457(18) Uani 1 1 d . . .
H6A H 0.232 0.1392 0.3182 0.055 Uiso 1 1 calc R . .
H6B H 0.3988 0.2211 0.3063 0.055 Uiso 1 1 calc R . .
C6A C 0.2756(12) -0.0367(8) -0.0253(3) 0.0508(19) Uani 1 1 d . . .
H6A1 H 0.26 -0.1188 -0.0125 0.076 Uiso 1 1 calc R . .
H6A2 H 0.3962 -0.0265 -0.0368 0.076 Uiso 1 1 calc R . .
H6A3 H 0.1922 -0.0214 -0.0552 0.076 Uiso 1 1 calc R . .
C8 C 0.2999(12) 0.3208(8) 0.2188(3) 0.051(2) Uani 1 1 d . . .
H8A H 0.4249 0.2962 0.223 0.061 Uiso 1 1 calc R . .
H8B H 0.2912 0.4042 0.2318 0.061 Uiso 1 1 calc R . .
C9 C 0.2467(12) 0.3186(8) 0.1613(3) 0.0474(18) Uani 1 1 d . . .
H9A H 0.1395 0.368 0.1553 0.057 Uiso 1 1 calc R . .
H9B H 0.3416 0.3546 0.1408 0.057 Uiso 1 1 calc R . .
C10 C 0.0985(8) 0.1968(7) 0.0920(2) 0.0346(14) Uani 1 1 d . . .
H10A H -0.0075 0.2454 0.0985 0.042 Uiso 1 1 calc R . .
H10B H 0.0585 0.1138 0.0847 0.042 Uiso 1 1 calc R . .
C21 C 0.3454(11) 0.0031(8) 0.1668(3) 0.0504(19) Uani 1 1 d . . .
H21A H 0.462 -0.036 0.1713 0.06 Uiso 1 1 calc R . .
H21B H 0.2686 -0.0496 0.1443 0.06 Uiso 1 1 calc R . .
C31 C 0.3658(10) 0.1185(9) 0.1400(3) 0.052(2) Uani 1 1 d . . .
H31A H 0.4677 0.1612 0.1568 0.063 Uiso 1 1 calc R . .
H31B H 0.3924 0.1034 0.1024 0.063 Uiso 1 1 calc R . .
C101 C 0.1816(8) 0.2448(6) 0.0427(2) 0.0326(13) Uani 1 1 d . . .
C102 C 0.1841(8) 0.3666(7) 0.0325(2) 0.0337(13) Uani 1 1 d . . .
H102 H 0.1322 0.4199 0.0567 0.04 Uiso 1 1 calc R . .
C103 C 0.2614(8) 0.4135(6) -0.0127(2) 0.0328(13) Uani 1 1 d . . .
C104 C 0.3341(9) 0.3348(7) -0.0488(2) 0.0357(14) Uani 1 1 d . . .
H104 H 0.3879 0.3654 -0.0793 0.043 Uiso 1 1 calc R . .
C105 C 0.3281(9) 0.2114(7) -0.0402(2) 0.0356(14) Uani 1 1 d . . .
H105 H 0.3746 0.1578 -0.0653 0.043 Uiso 1 1 calc R . .
C106 C 0.2531(9) 0.1669(7) 0.0057(2) 0.0347(13) Uani 1 1 d . . .
C201 C 0.1370(12) 0.7332(8) 0.0804(4) 0.054(2) Uani 1 1 d . . .
H20A H 0.0094 0.7367 0.0732 0.08 Uiso 1 1 calc R . .
H20B H 0.1953 0.7114 0.0479 0.08 Uiso 1 1 calc R . .
H20C H 0.1795 0.8116 0.0928 0.08 Uiso 1 1 calc R . .
 
 
 
#----------------------------------------------------------------------------#
#                   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
Cu1 N7 2.020(5) . ?
Cu1 N4 2.046(6) . ?
Cu1 N1 2.257(5) . ?
Cu1 Br2 2.4275(13) . ?
Cu1 Br1 2.4330(12) . ?
N1 C31 1.459(9) . ?
N1 C10 1.479(7) . ?
N1 C9 1.482(10) . ?
N4 C5 1.476(9) . ?
N4 C21 1.511(10) . ?
N4 H4 0.93 . ?
N7 C8 1.471(9) . ?
N7 C6 1.484(9) . ?
N7 H7 0.93 . ?
N100 O102 1.215(9) . ?
N100 O101 1.228(10) . ?
N100 C201 1.479(12) . ?
O3 C103 1.368(9) . ?
O3 C3A 1.419(9) . ?
O6 C106 1.381(9) . ?
O6 C6A 1.428(9) . ?
C3A H3A1 0.98 . ?
C3A H3A2 0.98 . ?
C3A H3A3 0.98 . ?
C5 C6 1.498(11) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C6A H6A1 0.98 . ?
C6A H6A2 0.98 . ?
C6A H6A3 0.98 . ?
C8 C9 1.489(10) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
C10 C101 1.516(9) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C21 C31 1.466(13) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C31 H31A 0.99 . ?
C31 H31B 0.99 . ?
C101 C102 1.384(10) . ?
C101 C106 1.402(9) . ?
C102 C103 1.405(9) . ?
C102 H102 0.95 . ?
C103 C104 1.396(10) . ?
C104 C105 1.395(11) . ?
C104 H104 0.95 . ?
C105 C106 1.401(9) . ?
C105 H105 0.95 . ?
C201 H20A 0.98 . ?
C201 H20B 0.98 . ?
C201 H20C 0.98 . ?
 
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
N7 Cu1 N4 83.4(2) . . ?
N7 Cu1 N1 83.43(19) . . ?
N4 Cu1 N1 82.3(2) . . ?
N7 Cu1 Br2 171.81(15) . . ?
N4 Cu1 Br2 92.55(17) . . ?
N1 Cu1 Br2 103.15(14) . . ?
N7 Cu1 Br1 90.16(16) . . ?
N4 Cu1 Br1 170.40(17) . . ?
N1 Cu1 Br1 104.13(14) . . ?
Br2 Cu1 Br1 92.90(5) . . ?
C31 N1 C10 115.0(5) . . ?
C31 N1 C9 114.8(6) . . ?
C10 N1 C9 111.5(6) . . ?
C31 N1 Cu1 105.8(4) . . ?
C10 N1 Cu1 108.5(4) . . ?
C9 N1 Cu1 99.8(4) . . ?
C5 N4 C21 114.7(6) . . ?
C5 N4 Cu1 111.5(5) . . ?
C21 N4 Cu1 105.6(4) . . ?
C5 N4 H4 108.3 . . ?
C21 N4 H4 108.3 . . ?
Cu1 N4 H4 108.3 . . ?
C8 N7 C6 112.3(6) . . ?
C8 N7 Cu1 111.4(4) . . ?
C6 N7 Cu1 105.8(4) . . ?
C8 N7 H7 109.1 . . ?
C6 N7 H7 109.1 . . ?
Cu1 N7 H7 109.1 . . ?
O102 N100 O101 122.7(9) . . ?
O102 N100 C201 121.2(8) . . ?
O101 N100 C201 115.8(7) . . ?
C103 O3 C3A 116.4(6) . . ?
C106 O6 C6A 118.2(6) . . ?
O3 C3A H3A1 109.5 . . ?
O3 C3A H3A2 109.5 . . ?
H3A1 C3A H3A2 109.5 . . ?
O3 C3A H3A3 109.5 . . ?
H3A1 C3A H3A3 109.5 . . ?
H3A2 C3A H3A3 109.5 . . ?
N4 C5 C6 110.7(6) . . ?
N4 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N7 C6 C5 111.5(6) . . ?
N7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
N7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108 . . ?
O6 C6A H6A1 109.5 . . ?
O6 C6A H6A2 109.5 . . ?
H6A1 C6A H6A2 109.5 . . ?
O6 C6A H6A3 109.5 . . ?
H6A1 C6A H6A3 109.5 . . ?
H6A2 C6A H6A3 109.5 . . ?
N7 C8 C9 114.5(6) . . ?
N7 C8 H8A 108.6 . . ?
C9 C8 H8A 108.6 . . ?
N7 C8 H8B 108.6 . . ?
C9 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
N1 C9 C8 112.5(6) . . ?
N1 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
N1 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
N1 C10 C101 116.6(5) . . ?
N1 C10 H10A 108.2 . . ?
C101 C10 H10A 108.2 . . ?
N1 C10 H10B 108.2 . . ?
C101 C10 H10B 108.2 . . ?
H10A C10 H10B 107.3 . . ?
C31 C21 N4 111.9(6) . . ?
C31 C21 H21A 109.2 . . ?
N4 C21 H21A 109.2 . . ?
C31 C21 H21B 109.2 . . ?
N4 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
N1 C31 C21 114.0(7) . . ?
N1 C31 H31A 108.8 . . ?
C21 C31 H31A 108.8 . . ?
N1 C31 H31B 108.8 . . ?
C21 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C102 C101 C106 118.5(6) . . ?
C102 C101 C10 120.6(6) . . ?
C106 C101 C10 120.9(6) . . ?
C101 C102 C103 121.8(6) . . ?
C101 C102 H102 119.1 . . ?
C103 C102 H102 119.1 . . ?
O3 C103 C104 125.2(6) . . ?
O3 C103 C102 115.8(6) . . ?
C104 C103 C102 119.0(7) . . ?
C105 C104 C103 120.2(6) . . ?
C105 C104 H104 119.9 . . ?
C103 C104 H104 119.9 . . ?
C104 C105 C106 119.7(6) . . ?
C104 C105 H105 120.1 . . ?
C106 C105 H105 120.1 . . ?
O6 C106 C105 122.4(6) . . ?
O6 C106 C101 116.8(6) . . ?
C105 C106 C101 120.8(7) . . ?
N100 C201 H20A 109.5 . . ?
N100 C201 H20B 109.5 . . ?
H20A C201 H20B 109.5 . . ?
N100 C201 H20C 109.5 . . ?
H20A C201 H20C 109.5 . . ?
H20B C201 H20C 109.5 . . ?
 
