data_C11H16ClN3O
#OL
#------------------------------------------------------------------------------
_audit_creation_date                  'Mon Dec 17 15:50:32 2002'
_audit_creation_method                'from TEXRAY.INF file'
_audit_update_record                   ?
#------------------------------------------------------------------------------
_computing_data_collection            'MSC/AFC Diffractometer Control'
_computing_cell_refinement            'MSC/AFC Diffractometer Control'
_computing_data_reduction             'teXsan'
_computing_structure_solution         'SIR92'
_computing_structure_refinement       'teXsan'
_computing_publication_material       'teXsan'
#------------------------------------------------------------------------------
_cell_length_a                         10.496(6)
_cell_length_b                         13.985(6)
_cell_length_c                         9.237(5)
_cell_angle_alpha                      106.79(4)
_cell_angle_beta                       94.99(5)
_cell_angle_gamma                      84.92(4)
_cell_volume                           1290(1)
_cell_formula_units_Z                  4
_cell_measurement_temperature          173.2
_cell_measurement_reflns_used          25
_cell_measurement_theta_min            25.0
_cell_measurement_theta_max            30.0
#------------------------------------------------------------------------------
_symmetry_cell_setting                 triclinic
_symmetry_space_group_name_H-M        'P -1       '
_symmetry_Int_Tables_number            2
_symmetry_space_group_name_Hall        ?
loop_
_symmetry_equiv_pos_as_xyz
  '   +x,   +y,   +z'
  '   -x,   -y,   -z'
#------------------------------------------------------------------------------
_exptl_crystal_description            'needle'
_exptl_crystal_colour                 'colorless'
_exptl_crystal_size_max                0.410
_exptl_crystal_size_mid                0.210
_exptl_crystal_size_min                0.200
_exptl_crystal_density_diffrn          1.244
_exptl_crystal_density_meas            'not measured'
_chemical_formula_weight               241.72
_chemical_formula_analytical           ?
_chemical_formula_sum                  'C11 H16 Cl N3 O '
_chemical_formula_moiety               'C22 H32 Cl2 N6 O2'
_chemical_formula_structural           ?
_chemical_compound_source              ?
_exptl_crystal_F_000                   512.00
_exptl_absorpt_coefficient_mu          0.281
_exptl_absorpt_correction_type         none
#------------------------------------------------------------------------------
_diffrn_special_details                none
_diffrn_ambient_temperature            173.2
_diffrn_radiation_wavelength           0.7107
_diffrn_radiation_type                 MoKalpha
_diffrn_radiation_source              'X-ray tube'
_diffrn_radiation_monochromator        graphite
_diffrn_radiation_detector             ?
_diffrn_measurement_device            'AFC6S'
_diffrn_measurement_method            'omega/2-theta scans'

_diffrn_standards_number               3
_diffrn_standards_interval_count       100
_diffrn_standards_decay_%              0.00
_diffrn_reflns_number                  3829
_reflns_number_total                   3597
_reflns_number_observed                2297
_reflns_observed_criterion             3.00
_diffrn_reflns_av_R_equivalents        2.89
_diffrn_reflns_limit_h_min             0
_diffrn_reflns_limit_h_max             11
_diffrn_reflns_limit_k_min             -15
_diffrn_reflns_limit_k_max             15
_diffrn_reflns_limit_l_min             -10
_diffrn_reflns_limit_l_max             10
_diffrn_reflns_theta_min               2.00
_diffrn_reflns_theta_max               23.00
_diffrn_reflns_reduction_process       'texsan PROCESS'

_diffrn_orient_matrix_UB_11           -0.02073
_diffrn_orient_matrix_UB_12           -0.06674
_diffrn_orient_matrix_UB_13           -0.07009
_diffrn_orient_matrix_UB_21           -0.00612
_diffrn_orient_matrix_UB_22            0.02868
_diffrn_orient_matrix_UB_23           -0.08797
_diffrn_orient_matrix_UB_31            0.09338
_diffrn_orient_matrix_UB_32           -0.01804
_diffrn_orient_matrix_UB_33           -0.01383
#------------------------------------------------------------------------------
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
  C  0    44 0.003 0.002     'International Tables'
  H  0    64 0.000 0.000     'International Tables'
  N  0    12 0.006 0.003     'International Tables'
  O  0     4 0.011 0.006     'International Tables'
  Cl 0     4 0.148 0.159     'International Tables'
#------------------------------------------------------------------------------
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
 Cl(1)  1.8352(1)   -0.13707(8) 1.0874(1)   0.0299(3)   Uij ? ?
 Cl(2)  2.3602(1)   -0.48812(8) 0.8038(1)   0.0314(3)   Uij ? ?
 O(1)   1.7632(3)   -0.1868(2)  0.6730(4)   0.043(1)    Uij ? ?
 O(2)   2.3303(3)   -0.2430(2)  0.6544(4)   0.039(1)    Uij ? ?
 N(1)   1.7306(4)   -0.3050(3)  0.4488(4)   0.031(1)    Uij ? ?
 N(2)   1.6276(3)   -0.3108(3)  0.6598(4)   0.025(1)    Uij ? ?
 N(3)   1.5463(3)   -0.3120(3)  0.8869(4)   0.026(1)    Uij ? ?
 N(4)   2.2802(3)   -0.0760(3)  0.7050(4)   0.033(1)    Uij ? ?
 N(5)   2.1474(3)   -0.1773(3)  0.7792(4)   0.028(1)    Uij ? ?
 N(6)   2.0544(3)   -0.2726(3)  0.9051(4)   0.027(1)    Uij ? ?
 C(1)   1.7135(4)   -0.2617(4)  0.5953(5)   0.030(1)    Uij ? ?
 C(2)   1.6203(4)   -0.2773(3)  0.8112(5)   0.026(1)    Uij ? ?
 C(3)   1.5508(4)   -0.2763(3)  1.0541(5)   0.027(1)    Uij ? ?
 C(4)   1.4303(4)   -0.2129(3)  1.1100(5)   0.026(1)    Uij ? ?
 C(5)   1.4005(5)   -0.1226(4)  1.0782(5)   0.040(2)    Uij ? ?
 C(6)   1.2904(6)   -0.0637(4)  1.1357(6)   0.050(2)    Uij ? ?
 C(7)   1.2132(5)   -0.0965(5)  1.2208(6)   0.055(2)    Uij ? ?
 C(8)   1.2420(5)   -0.1862(4)  1.2521(6)   0.049(2)    Uij ? ?
 C(9)   1.3505(4)   -0.2458(4)  1.1963(5)   0.036(1)    Uij ? ?
 C(10)  1.8096(5)   -0.2556(4)  0.3717(5)   0.049(2)    Uij ? ?
 C(11)  1.5532(4)   -0.3922(3)  0.5649(5)   0.030(1)    Uij ? ?
 C(12)  2.2609(4)   -0.1682(4)  0.7073(5)   0.028(1)    Uij ? ?
 C(13)  2.1441(4)   -0.2582(3)  0.8283(5)   0.026(1)    Uij ? ?
 C(14)  2.0554(4)   -0.3649(3)  0.9537(5)   0.029(1)    Uij ? ?
 C(15)  1.9629(4)   -0.4365(3)  0.8540(5)   0.026(1)    Uij ? ?
 C(16)  1.8414(4)   -0.4448(3)  0.8981(5)   0.030(1)    Uij ? ?
 C(17)  1.7578(4)   -0.5105(4)  0.8045(6)   0.036(1)    Uij ? ?
 C(18)  1.7942(5)   -0.5707(4)  0.6646(6)   0.038(2)    Uij ? ?
 C(19)  1.9154(5)   -0.5636(4)  0.6203(5)   0.044(2)    Uij ? ?
 C(20)  1.9992(5)   -0.4983(4)  0.7130(5)   0.038(2)    Uij ? ?
 C(21)  2.3930(5)   -0.0575(4)  0.6392(6)   0.047(2)    Uij ? ?
 C(22)  2.0420(4)   -0.0996(4)  0.8053(6)   0.038(1)    Uij ? ?
 H(1)   1.9773      -0.2223     0.9388      0.0450      Uij ? ?
 H(2)   2.2244      -0.0175     0.7600      0.0450      Uij ? ?
 H(3)   1.4947      -0.3725     0.8289      0.0450      Uij ? ?
 H(4)   1.6912      -0.3724     0.3773      0.0450      Uij ? ?
 H(5)   2.2184      -0.3079     0.8034      0.0450      Uij ? ?
 H(6)   2.1528      -0.4013     0.9416      0.0450      Uij ? ?
 H(7)   2.0282      -0.3405     1.0673      0.0450      Uij ? ?
 H(8)   1.8148      -0.3952     1.0068      0.0450      Uij ? ?
 H(9)   1.6605      -0.5161     0.8353      0.0450      Uij ? ?
 H(10)  1.7271      -0.6163     0.5919      0.0450      Uij ? ?
 H(11)  1.9467      -0.6177     0.5063      0.0450      Uij ? ?
 H(12)  2.1006      -0.4890     0.6978      0.0450      Uij ? ?
 H(13)  1.6871      -0.2207     0.8680      0.0450      Uij ? ?
 H(14)  1.3775      -0.3182     1.2327      0.0450      Uij ? ?
 H(15)  1.1634      -0.2207     1.2979      0.0450      Uij ? ?
 H(16)  1.5682      -0.3347     1.1004      0.0450      Uij ? ?
 H(17)  1.6440      -0.2364     1.0967      0.0450      Uij ? ?
 H(18)  1.5014      -0.4133     0.6214      0.0450      Uij ? ?
 H(19)  1.5079      -0.3720     0.4780      0.0450      Uij ? ?
 H(20)  1.6055      -0.4553     0.5129      0.0450      Uij ? ?
 H(21)  2.0393      -0.0636     0.7246      0.0450      Uij ? ?
 H(22)  1.9642      -0.1300     0.7958      0.0450      Uij ? ?
 H(23)  2.0515      -0.0483     0.9097      0.0450      Uij ? ?
 H(24)  2.3984      -0.1098     0.5402      0.0450      Uij ? ?
 H(25)  2.4764      -0.0635     0.6898      0.0450      Uij ? ?
 H(26)  2.3799      -0.0140     0.5980      0.0450      Uij ? ?
 H(27)  1.8818      -0.2998     0.3317      0.0570      Uij ? ?
 H(28)  1.7613      -0.2381     0.2901      0.0570      Uij ? ?
 H(29)  1.8418      -0.1964     0.4409      0.0570      Uij ? ?
 H(30)  1.4566      -0.0999     1.0168      0.0481      Uij ? ?
 H(31)  1.2708      0.0007      1.1134      0.0623      Uij ? ?
 H(32)  1.1371      -0.0555     1.2606      0.0651      Uij ? ?

#------------------------------------------------------------------------------
_refine_special_details                none
_refine_ls_structure_factor_coef       F
_refine_ls_matrix_type                 full
_refine_ls_weighting_scheme            sigma
_refine_ls_hydrogen_treatment          noref
_refine_ls_extinction_method           none
_refine_ls_extinction_coef             none
_refine_ls_abs_structure_details       none
_refine_ls_abs_structure_Flack         none
_refine_ls_number_reflns               2297
_refine_ls_number_parameters           289
_refine_ls_number_restraints           0
_refine_ls_number_constraints          0
_refine_ls_R_factor_obs                0.0467
_refine_ls_wR_factor_obs               0.0620
_refine_ls_goodness_of_fit_obs         1.608
_refine_ls_shift/esd_max               0.0010
_refine_diff_density_min               -0.38
_refine_diff_density_max               0.37
#------------------------------------------------------------------------------
_geom_special_details                  ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
    O(1)      C(1)      1.217(5)   ? ? yes
    O(2)      C(12)     1.222(5)   ? ? yes
    N(1)      C(1)      1.334(6)   ? ? yes
    N(1)      C(10)     1.470(6)   ? ? yes
    N(2)      C(1)      1.441(5)   ? ? yes
    N(2)      C(2)      1.348(5)   ? ? yes
    N(2)      C(11)     1.461(5)   ? ? yes
    N(3)      C(2)      1.297(5)   ? ? yes
    N(3)      C(3)      1.477(5)   ? ? yes
    N(4)      C(12)     1.330(6)   ? ? yes
    N(4)      C(21)     1.452(6)   ? ? yes
    N(5)      C(12)     1.446(5)   ? ? yes
    N(5)      C(13)     1.340(6)   ? ? yes
    N(5)      C(22)     1.465(6)   ? ? yes
    N(6)      C(13)     1.289(5)   ? ? yes
    N(6)      C(14)     1.482(6)   ? ? yes
    C(3)      C(4)      1.517(6)   ? ? yes
    C(4)      C(5)      1.382(6)   ? ? yes
    C(4)      C(9)      1.395(6)   ? ? yes
    C(5)      C(6)      1.407(7)   ? ? yes
    C(6)      C(7)      1.368(8)   ? ? yes
    C(7)      C(8)      1.369(8)   ? ? yes
    C(8)      C(9)      1.394(7)   ? ? yes
    C(14)     C(15)     1.509(6)   ? ? yes
    C(15)     C(16)     1.396(6)   ? ? yes
    C(15)     C(20)     1.402(6)   ? ? yes
    C(16)     C(17)     1.384(6)   ? ? yes
    C(17)     C(18)     1.387(7)   ? ? yes
    C(18)     C(19)     1.390(7)   ? ? yes
    C(19)     C(20)     1.378(7)   ? ? yes
#------------------------------------------------------------------------------
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
   C(1)      N(1)      C(10)     117.8(4)   ? ? ? yes
   C(1)      N(2)      C(2)      116.2(4)   ? ? ? yes
   C(1)      N(2)      C(11)     121.3(3)   ? ? ? yes
   C(2)      N(2)      C(11)     122.4(4)   ? ? ? yes
   C(2)      N(3)      C(3)      120.8(4)   ? ? ? yes
   C(12)     N(4)      C(21)     120.0(4)   ? ? ? yes
   C(12)     N(5)      C(13)     117.3(4)   ? ? ? yes
   C(12)     N(5)      C(22)     122.2(4)   ? ? ? yes
   C(13)     N(5)      C(22)     120.4(4)   ? ? ? yes
   C(13)     N(6)      C(14)     121.6(4)   ? ? ? yes
   O(1)      C(1)      N(1)      125.3(4)   ? ? ? yes
   O(1)      C(1)      N(2)      120.3(4)   ? ? ? yes
   N(1)      C(1)      N(2)      114.4(4)   ? ? ? yes
   N(2)      C(2)      N(3)      124.2(4)   ? ? ? yes
   N(3)      C(3)      C(4)      111.6(3)   ? ? ? yes
   C(3)      C(4)      C(5)      120.6(4)   ? ? ? yes
   C(3)      C(4)      C(9)      119.4(4)   ? ? ? yes
   C(5)      C(4)      C(9)      120.0(4)   ? ? ? yes
   C(4)      C(5)      C(6)      119.4(5)   ? ? ? yes
   C(5)      C(6)      C(7)      120.1(5)   ? ? ? yes
   C(6)      C(7)      C(8)      120.8(5)   ? ? ? yes
   C(7)      C(8)      C(9)      120.2(5)   ? ? ? yes
   C(4)      C(9)      C(8)      119.5(5)   ? ? ? yes
   O(2)      C(12)     N(4)      125.4(4)   ? ? ? yes
   O(2)      C(12)     N(5)      119.4(4)   ? ? ? yes
   N(4)      C(12)     N(5)      115.2(4)   ? ? ? yes
   N(5)      C(13)     N(6)      124.4(4)   ? ? ? yes
   N(6)      C(14)     C(15)     111.1(3)   ? ? ? yes
   C(14)     C(15)     C(16)     122.1(4)   ? ? ? yes
   C(14)     C(15)     C(20)     119.7(4)   ? ? ? yes
   C(16)     C(15)     C(20)     118.1(4)   ? ? ? yes
   C(15)     C(16)     C(17)     121.2(4)   ? ? ? yes
   C(16)     C(17)     C(18)     120.2(4)   ? ? ? yes
   C(17)     C(18)     C(19)     119.0(4)   ? ? ? yes
   C(18)     C(19)     C(20)     121.0(5)   ? ? ? yes
   C(15)     C(20)     C(19)     120.4(4)   ? ? ? yes
#------------------------------------------------------------------------------
#---END
