Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               CrystEngComm

# SUBMISSION DETAILS

_journal_coden_Cambridge         1350
#==============================================================================
_audit_creation_method           'manual editing of form.cif'
_publ_contact_author_name        'Krzysztof Wozniak'
_publ_contact_author_address     
;
Chemistry Department, Warsaw University,
ul. Pasteura 1, 02-093 Warszawa,
Poland
;
_publ_contact_author_email       kwozniak@chem.uw.edu.pl
_publ_contact_author_fax         48(22)8222892
_publ_contact_author_phone       48(22)8220292
_publ_contact_letter             
;
Please consider this CIF submission as a supplementary information
for publication in CrystEngComm
;
# TITLE AND AUTHOR LIST
_publ_section_title              
;
On Polymorphism and Planarity of Benzidine Dihydrochloride
;
_publ_section_title_footnote     
; Contribution No. ...
;
loop_
_publ_author_name
_publ_author_address
'Lukasz Dobrzycki'
; Chemistry Department, Warsaw University,
ul. Pasteura 1, 02-093 Warszawa,
Poland
;
K.Wozniak
; Chemistry Department, Warsaw University,
ul. Pasteura 1, 02-093 Warszawa,
Poland.
;
_publ_section_abstract           
; ?
;
_publ_section_experimental       
; ?
;
_publ_section_comment            
; ?
;
_publ_section_references         
; ?
;
_publ_section_figure_captions    
; ?
;
#############################################################

data_1a_120
_database_code_depnum_ccdc_archive 'CCDC 618057'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H14 Cl2 N2'
_chemical_formula_weight         257.15

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.0000 '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                   6.5705(11)
_cell_length_b                   7.6756(14)
_cell_length_c                   12.6098(18)
_cell_angle_alpha                85.165(13)
_cell_angle_beta                 76.785(13)
_cell_angle_gamma                73.868(16)
_cell_volume                     594.58(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             268
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.6479
_diffrn_standards_number         '1 frame'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        2
_diffrn_reflns_number            14508
_diffrn_reflns_av_R_equivalents  0.0107
_diffrn_reflns_av_sigmaI/netI    0.0079
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         30.00
_reflns_number_total             3452
_reflns_number_gt                3131
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL-97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0468P)^2^+0.0795P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.074(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3452
_refine_ls_number_parameters     202
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0734
_refine_ls_wR_factor_gt          0.0708
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_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
Cl1 Cl 0.03971(3) 0.17640(2) 0.080928(13) 0.01292(7) Uani 1 1 d . . .
Cl2 Cl 0.46084(3) 0.32459(2) 0.911442(13) 0.01369(7) Uani 1 1 d . . .
N1 N 1.10319(11) 0.56602(9) 0.11552(5) 0.01224(13) Uani 1 1 d . . .
N2 N 0.41134(11) 0.92387(9) 0.88626(5) 0.01268(13) Uani 1 1 d . . .
C1 C 0.99392(12) 0.61926(10) 0.22723(6) 0.01067(14) Uani 1 1 d . . .
C2 C 0.93435(12) 0.49065(10) 0.30275(6) 0.01262(14) Uani 1 1 d . . .
C3 C 0.83649(12) 0.54304(10) 0.40961(6) 0.01247(14) Uani 1 1 d . . .
C4 C 0.79494(12) 0.72235(10) 0.44152(6) 0.01071(13) Uani 1 1 d . . .
C5 C 0.85604(12) 0.84863(10) 0.36231(6) 0.01291(14) Uani 1 1 d . . .
C6 C 0.95750(12) 0.79762(10) 0.25581(6) 0.01276(14) Uani 1 1 d . . .
C7 C 0.51270(12) 0.87111(10) 0.77336(6) 0.01119(14) Uani 1 1 d . . .
C8 C 0.63209(12) 0.97726(10) 0.70655(6) 0.01357(14) Uani 1 1 d . . .
C9 C 0.72207(12) 0.92866(10) 0.59858(6) 0.01352(14) Uani 1 1 d . . .
C10 C 0.69376(12) 0.77577(10) 0.55622(6) 0.01093(14) Uani 1 1 d . . .
C11 C 0.57249(12) 0.67204(10) 0.62650(6) 0.01326(14) Uani 1 1 d . . .
C12 C 0.48199(12) 0.71832(10) 0.73493(6) 0.01302(14) Uani 1 1 d . . .
H1A H 1.102(2) 0.459(2) 0.1028(11) 0.025(3) Uiso 1 1 d . . .
H1B H 1.238(2) 0.5746(18) 0.1001(11) 0.022(3) Uiso 1 1 d . . .
H1C H 1.041(2) 0.6414(19) 0.0648(11) 0.021(3) Uiso 1 1 d . . .
H2 H 0.967(2) 0.3652(16) 0.2839(9) 0.022(3) Uiso 1 1 d . . .
H2A H 0.414(2) 1.033(2) 0.8964(11) 0.026(3) Uiso 1 1 d . . .
H2B H 0.479(2) 0.8498(18) 0.9357(11) 0.020(3) Uiso 1 1 d . . .
H2C H 0.274(2) 0.9178(18) 0.9052(11) 0.021(3) Uiso 1 1 d . . .
H3 H 0.804(2) 0.4514(16) 0.4620(10) 0.023(3) Uiso 1 1 d . . .
H5 H 0.8224(19) 0.9748(15) 0.3787(9) 0.019(3) Uiso 1 1 d . . .
H6 H 0.999(2) 0.8835(17) 0.2030(10) 0.028(3) Uiso 1 1 d . . .
H8 H 0.654(2) 1.0793(17) 0.7335(10) 0.025(3) Uiso 1 1 d . . .
H9 H 0.805(2) 1.0028(17) 0.5546(10) 0.025(3) Uiso 1 1 d . . .
H11 H 0.545(2) 0.5682(16) 0.6011(9) 0.024(3) Uiso 1 1 d . . .
H12 H 0.398(2) 0.6481(17) 0.7797(10) 0.025(3) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.01479(11) 0.01178(11) 0.01207(10) -0.00023(6) -0.00047(7) -0.00531(7)
Cl2 0.01517(11) 0.01305(11) 0.01284(10) -0.00004(6) -0.00078(7) -0.00566(7)
N1 0.0151(3) 0.0130(3) 0.0084(3) -0.0014(2) -0.0003(2) -0.0050(2)
N2 0.0147(3) 0.0144(3) 0.0085(3) -0.0016(2) -0.0005(2) -0.0044(2)
C1 0.0109(3) 0.0132(3) 0.0077(3) -0.0008(2) -0.0010(2) -0.0035(2)
C2 0.0156(3) 0.0117(3) 0.0107(3) -0.0005(2) -0.0017(2) -0.0046(2)
C3 0.0152(3) 0.0122(3) 0.0100(3) 0.0007(2) -0.0012(2) -0.0052(2)
C4 0.0107(3) 0.0123(3) 0.0091(3) -0.0009(2) -0.0016(2) -0.0032(2)
C5 0.0162(3) 0.0113(3) 0.0110(3) -0.0003(2) -0.0020(2) -0.0039(2)
C6 0.0163(3) 0.0117(3) 0.0103(3) 0.0009(2) -0.0019(2) -0.0049(2)
C7 0.0111(3) 0.0134(3) 0.0083(3) -0.0012(2) -0.0011(2) -0.0026(2)
C8 0.0155(3) 0.0148(3) 0.0113(3) -0.0023(2) -0.0006(2) -0.0068(3)
C9 0.0154(3) 0.0147(3) 0.0109(3) -0.0013(2) 0.0003(2) -0.0070(3)
C10 0.0109(3) 0.0125(3) 0.0090(3) -0.0009(2) -0.0013(2) -0.0029(2)
C11 0.0147(3) 0.0136(3) 0.0116(3) -0.0016(2) -0.0003(2) -0.0057(2)
C12 0.0147(3) 0.0133(3) 0.0108(3) -0.0003(2) -0.0001(2) -0.0056(3)

_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
N1 C1 1.4623(9) . ?
N1 H1A 0.850(15) . ?
N1 H1B 0.882(15) . ?
N1 H1C 0.916(13) . ?
N2 C7 1.4656(9) . ?
N2 H2A 0.863(15) . ?
N2 H2B 0.913(13) . ?
N2 H2C 0.891(14) . ?
C1 C2 1.3858(10) . ?
C1 C6 1.3868(10) . ?
C2 C3 1.3937(10) . ?
C2 H2 0.964(12) . ?
C3 C4 1.4018(10) . ?
C3 H3 0.957(12) . ?
C4 C5 1.4029(10) . ?
C4 C10 1.4869(11) . ?
C5 C6 1.3912(10) . ?
C5 H5 0.961(11) . ?
C6 H6 0.947(13) . ?
C7 C12 1.3868(10) . ?
C7 C8 1.3879(11) . ?
C8 C9 1.3920(10) . ?
C8 H8 0.940(12) . ?
C9 C10 1.4033(10) . ?
C9 H9 0.955(13) . ?
C10 C11 1.4017(10) . ?
C11 C12 1.3936(10) . ?
C11 H11 0.958(12) . ?
C12 H12 0.942(13) . ?

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
C1 N1 H1A 112.3(9) . . ?
C1 N1 H1B 111.7(9) . . ?
H1A N1 H1B 109.7(12) . . ?
C1 N1 H1C 112.5(8) . . ?
H1A N1 H1C 106.6(13) . . ?
H1B N1 H1C 103.7(12) . . ?
C7 N2 H2A 110.7(9) . . ?
C7 N2 H2B 112.8(8) . . ?
H2A N2 H2B 107.3(13) . . ?
C7 N2 H2C 112.6(8) . . ?
H2A N2 H2C 108.5(13) . . ?
H2B N2 H2C 104.6(12) . . ?
C2 C1 C6 121.44(7) . . ?
C2 C1 N1 119.72(7) . . ?
C6 C1 N1 118.82(7) . . ?
C1 C2 C3 118.79(7) . . ?
C1 C2 H2 121.4(7) . . ?
C3 C2 H2 119.7(7) . . ?
C2 C3 C4 121.52(7) . . ?
C2 C3 H3 118.0(7) . . ?
C4 C3 H3 120.4(7) . . ?
C3 C4 C5 117.86(6) . . ?
C3 C4 C10 120.97(7) . . ?
C5 C4 C10 121.16(7) . . ?
C6 C5 C4 121.27(7) . . ?
C6 C5 H5 117.5(7) . . ?
C4 C5 H5 121.1(7) . . ?
C1 C6 C5 119.10(7) . . ?
C1 C6 H6 120.1(7) . . ?
C5 C6 H6 120.7(7) . . ?
C12 C7 C8 121.48(7) . . ?
C12 C7 N2 119.00(7) . . ?
C8 C7 N2 119.51(7) . . ?
C7 C8 C9 118.92(7) . . ?
C7 C8 H8 121.0(7) . . ?
C9 C8 H8 120.1(7) . . ?
C8 C9 C10 121.43(7) . . ?
C8 C9 H9 117.3(7) . . ?
C10 C9 H9 121.2(7) . . ?
C11 C10 C9 117.82(6) . . ?
C11 C10 C4 121.10(7) . . ?
C9 C10 C4 121.05(7) . . ?
C12 C11 C10 121.51(7) . . ?
C12 C11 H11 117.4(7) . . ?
C10 C11 H11 121.1(7) . . ?
C7 C12 C11 118.84(7) . . ?
C7 C12 H12 121.5(7) . . ?
C11 C12 H12 119.6(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.22(11) . . . . ?
N1 C1 C2 C3 178.02(7) . . . . ?
C1 C2 C3 C4 0.85(11) . . . . ?
C2 C3 C4 C5 -0.29(11) . . . . ?
C2 C3 C4 C10 -178.97(7) . . . . ?
C3 C4 C5 C6 -0.92(11) . . . . ?
C10 C4 C5 C6 177.76(7) . . . . ?
C2 C1 C6 C5 -0.95(11) . . . . ?
N1 C1 C6 C5 -179.21(7) . . . . ?
C4 C5 C6 C1 1.53(11) . . . . ?
C12 C7 C8 C9 0.16(11) . . . . ?
N2 C7 C8 C9 -178.10(7) . . . . ?
C7 C8 C9 C10 0.25(11) . . . . ?
C8 C9 C10 C11 -0.39(11) . . . . ?
C8 C9 C10 C4 -178.51(7) . . . . ?
C3 C4 C10 C11 -21.60(12) . . . . ?
C5 C4 C10 C11 159.76(7) . . . . ?
C3 C4 C10 C9 156.45(7) . . . . ?
C5 C4 C10 C9 -22.18(12) . . . . ?
C9 C10 C11 C12 0.12(11) . . . . ?
C4 C10 C11 C12 178.24(7) . . . . ?
C8 C7 C12 C11 -0.41(11) . . . . ?
N2 C7 C12 C11 177.85(6) . . . . ?
C10 C11 C12 C7 0.27(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl1 0.850(15) 2.368(15) 3.2099(9) 171.1(13) 1_655
N1 H1B Cl2 0.882(15) 2.289(15) 3.1415(9) 162.7(12) 2_766
N1 H1C Cl1 0.916(13) 2.283(13) 3.1833(9) 167.6(12) 2_665
N2 H2A Cl2 0.863(15) 2.371(15) 3.2303(9) 173.6(13) 1_565
N2 H2B Cl2 0.913(13) 2.299(13) 3.1810(8) 162.3(11) 2_667
N2 H2C Cl1 0.891(14) 2.334(14) 3.1937(9) 161.9(11) 2_566

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.066

data_1a_293
_database_code_depnum_ccdc_archive 'CCDC 618058'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H14 Cl2 N2'
_chemical_formula_weight         257.15

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.0000 '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                   6.6652(10)
_cell_length_b                   7.7196(12)
_cell_length_c                   12.572(2)
_cell_angle_alpha                84.567(14)
_cell_angle_beta                 76.328(14)
_cell_angle_gamma                74.007(14)
_cell_volume                     603.93(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             268
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.6479
_diffrn_standards_number         '1 frame'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        2
_diffrn_reflns_number            16213
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         30.00
_reflns_number_total             3516
_reflns_number_gt                2543
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL-97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.035(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3516
_refine_ls_number_parameters     202
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0940
_refine_ls_wR_factor_gt          0.0857
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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
Cl1 Cl 0.03650(4) 0.17812(3) 0.08153(2) 0.03311(10) Uani 1 1 d . . .
Cl2 Cl 0.46506(4) 0.32262(3) 0.91201(2) 0.03481(10) Uani 1 1 d . . .
N1 N 1.10432(17) 0.56381(14) 0.11573(7) 0.0303(2) Uani 1 1 d . . .
N2 N 0.40815(17) 0.92773(14) 0.88527(7) 0.0314(2) Uani 1 1 d . . .
C1 C 0.99557(16) 0.61768(14) 0.22728(7) 0.0253(2) Uani 1 1 d . . .
C2 C 0.92858(19) 0.49285(15) 0.30362(8) 0.0313(2) Uani 1 1 d . . .
C3 C 0.83129(19) 0.54531(15) 0.40999(8) 0.0312(2) Uani 1 1 d . . .
C4 C 0.79626(15) 0.72210(13) 0.44155(7) 0.0252(2) Uani 1 1 d . . .
C5 C 0.86495(19) 0.84426(15) 0.36139(8) 0.0319(2) Uani 1 1 d . . .
C6 C 0.96583(19) 0.79275(15) 0.25530(8) 0.0319(2) Uani 1 1 d . . .
C7 C 0.51028(16) 0.87444(14) 0.77283(7) 0.0267(2) Uani 1 1 d . . .
C8 C 0.62570(19) 0.98042(16) 0.70388(9) 0.0345(2) Uani 1 1 d . . .
C9 C 0.7167(2) 0.93089(16) 0.59675(9) 0.0343(2) Uani 1 1 d . . .
C10 C 0.69476(15) 0.77622(13) 0.55595(7) 0.0259(2) Uani 1 1 d . . .
C11 C 0.57707(19) 0.67273(16) 0.62849(8) 0.0331(2) Uani 1 1 d . . .
C12 C 0.48547(19) 0.72032(15) 0.73619(8) 0.0326(2) Uani 1 1 d . . .
H1A H 1.102(3) 0.458(2) 0.1045(13) 0.043(4) Uiso 1 1 d . . .
H1B H 1.231(3) 0.576(2) 0.1005(13) 0.044(4) Uiso 1 1 d . . .
H1C H 1.039(2) 0.651(2) 0.0626(13) 0.047(4) Uiso 1 1 d . . .
H2 H 0.955(3) 0.372(2) 0.2869(13) 0.062(5) Uiso 1 1 d . . .
H2A H 0.410(3) 1.038(2) 0.8945(13) 0.047(4) Uiso 1 1 d . . .
H2B H 0.474(2) 0.846(2) 0.9351(13) 0.048(4) Uiso 1 1 d . . .
H2C H 0.278(3) 0.919(2) 0.9052(13) 0.048(4) Uiso 1 1 d . . .
H3 H 0.791(2) 0.461(2) 0.4595(11) 0.043(4) Uiso 1 1 d . . .
H5 H 0.836(2) 0.963(2) 0.3770(11) 0.047(4) Uiso 1 1 d . . .
H6 H 1.012(2) 0.876(2) 0.2046(12) 0.052(4) Uiso 1 1 d . . .
H8 H 0.646(3) 1.085(2) 0.7285(13) 0.062(5) Uiso 1 1 d . . .
H9 H 0.792(2) 1.001(2) 0.5518(11) 0.041(4) Uiso 1 1 d . . .
H11 H 0.555(2) 0.570(2) 0.6059(11) 0.050(4) Uiso 1 1 d . . .
H12 H 0.404(2) 0.650(2) 0.7806(12) 0.050(4) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.03903(16) 0.02865(15) 0.03073(15) -0.00146(10) 0.00018(10) -0.01387(11)
Cl2 0.03983(17) 0.03148(16) 0.03259(15) -0.00126(10) -0.00045(11) -0.01479(12)
N1 0.0380(5) 0.0321(5) 0.0207(4) -0.0033(3) -0.0007(3) -0.0132(4)
N2 0.0375(5) 0.0344(5) 0.0210(4) -0.0040(3) -0.0009(4) -0.0108(4)
C1 0.0274(5) 0.0289(5) 0.0198(4) -0.0015(3) -0.0035(3) -0.0091(4)
C2 0.0426(6) 0.0267(5) 0.0252(4) -0.0028(4) -0.0024(4) -0.0134(4)
C3 0.0411(6) 0.0293(5) 0.0234(4) 0.0000(4) -0.0011(4) -0.0147(4)
C4 0.0256(5) 0.0281(5) 0.0221(4) -0.0021(3) -0.0035(3) -0.0084(4)
C5 0.0439(6) 0.0255(5) 0.0252(4) -0.0021(4) -0.0019(4) -0.0114(4)
C6 0.0429(6) 0.0282(5) 0.0238(4) 0.0017(4) -0.0019(4) -0.0136(4)
C7 0.0277(5) 0.0304(5) 0.0207(4) -0.0021(3) -0.0023(3) -0.0074(4)
C8 0.0430(6) 0.0366(6) 0.0269(5) -0.0071(4) 0.0006(4) -0.0202(5)
C9 0.0418(6) 0.0375(6) 0.0260(5) -0.0047(4) 0.0025(4) -0.0213(5)
C10 0.0267(5) 0.0281(5) 0.0219(4) -0.0024(3) -0.0026(4) -0.0076(4)
C11 0.0408(6) 0.0317(6) 0.0272(5) -0.0051(4) 0.0017(4) -0.0167(5)
C12 0.0388(6) 0.0313(6) 0.0266(5) -0.0020(4) 0.0024(4) -0.0149(5)

_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
N1 C1 1.4592(13) . ?
N1 H1A 0.849(17) . ?
N1 H1B 0.850(17) . ?
N1 H1C 0.988(16) . ?
N2 C7 1.4601(13) . ?
N2 H2A 0.877(18) . ?
N2 H2B 0.943(16) . ?
N2 H2C 0.866(18) . ?
C1 C6 1.3781(15) . ?
C1 C2 1.3815(14) . ?
C2 C3 1.3859(14) . ?
C2 H2 0.938(18) . ?
C3 C4 1.3992(15) . ?
C3 H3 0.911(15) . ?
C4 C5 1.3980(14) . ?
C4 C10 1.4829(14) . ?
C5 C6 1.3850(15) . ?
C5 H5 0.916(15) . ?
C6 H6 0.922(16) . ?
C7 C12 1.3796(15) . ?
C7 C8 1.3820(15) . ?
C8 C9 1.3827(15) . ?
C8 H8 0.945(17) . ?
C9 C10 1.3993(14) . ?
C9 H9 0.909(14) . ?
C10 C11 1.3980(14) . ?
C11 C12 1.3861(14) . ?
C11 H11 0.927(15) . ?
C12 H12 0.927(16) . ?

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
C1 N1 H1A 111.8(11) . . ?
C1 N1 H1B 111.0(10) . . ?
H1A N1 H1B 112.0(15) . . ?
C1 N1 H1C 110.0(9) . . ?
H1A N1 H1C 110.5(14) . . ?
H1B N1 H1C 101.0(14) . . ?
C7 N2 H2A 110.7(11) . . ?
C7 N2 H2B 110.4(10) . . ?
H2A N2 H2B 111.5(14) . . ?
C7 N2 H2C 113.5(11) . . ?
H2A N2 H2C 109.0(15) . . ?
H2B N2 H2C 101.6(14) . . ?
C6 C1 C2 121.01(9) . . ?
C6 C1 N1 118.98(9) . . ?
C2 C1 N1 119.99(9) . . ?
C1 C2 C3 119.12(10) . . ?
C1 C2 H2 121.9(10) . . ?
C3 C2 H2 118.8(10) . . ?
C2 C3 C4 121.68(10) . . ?
C2 C3 H3 117.8(9) . . ?
C4 C3 H3 120.5(9) . . ?
C5 C4 C3 117.24(9) . . ?
C5 C4 C10 121.50(10) . . ?
C3 C4 C10 121.25(9) . . ?
C6 C5 C4 121.64(10) . . ?
C6 C5 H5 118.1(9) . . ?
C4 C5 H5 120.2(9) . . ?
C1 C6 C5 119.29(10) . . ?
C1 C6 H6 121.1(9) . . ?
C5 C6 H6 119.6(9) . . ?
C12 C7 C8 120.88(9) . . ?
C12 C7 N2 119.18(9) . . ?
C8 C7 N2 119.93(10) . . ?
C7 C8 C9 119.30(10) . . ?
C7 C8 H8 121.6(9) . . ?
C9 C8 H8 119.1(10) . . ?
C8 C9 C10 121.76(10) . . ?
C8 C9 H9 118.9(9) . . ?
C10 C9 H9 119.3(9) . . ?
C11 C10 C9 117.08(9) . . ?
C11 C10 C4 121.46(10) . . ?
C9 C10 C4 121.45(9) . . ?
C12 C11 C10 121.83(10) . . ?
C12 C11 H11 117.1(9) . . ?
C10 C11 H11 121.0(9) . . ?
C7 C12 C11 119.15(10) . . ?
C7 C12 H12 121.9(9) . . ?
C11 C12 H12 118.9(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.39(17) . . . . ?
N1 C1 C2 C3 178.09(10) . . . . ?
C1 C2 C3 C4 1.01(17) . . . . ?
C2 C3 C4 C5 -0.45(16) . . . . ?
C2 C3 C4 C10 -179.13(10) . . . . ?
C3 C4 C5 C6 -0.73(16) . . . . ?
C10 C4 C5 C6 177.95(11) . . . . ?
C2 C1 C6 C5 -0.75(17) . . . . ?
N1 C1 C6 C5 -179.25(10) . . . . ?
C4 C5 C6 C1 1.33(18) . . . . ?
C12 C7 C8 C9 0.17(18) . . . . ?
N2 C7 C8 C9 -178.27(11) . . . . ?
C7 C8 C9 C10 0.15(19) . . . . ?
C8 C9 C10 C11 -0.25(18) . . . . ?
C8 C9 C10 C4 -178.83(11) . . . . ?
C5 C4 C10 C11 163.09(10) . . . . ?
C3 C4 C10 C11 -18.28(16) . . . . ?
C5 C4 C10 C9 -18.39(16) . . . . ?
C3 C4 C10 C9 160.24(10) . . . . ?
C9 C10 C11 C12 0.04(17) . . . . ?
C4 C10 C11 C12 178.62(11) . . . . ?
C8 C7 C12 C11 -0.37(17) . . . . ?
N2 C7 C12 C11 178.08(10) . . . . ?
C10 C11 C12 C7 0.26(18) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl1 0.849(17) 2.372(18) 3.2140(12) 171.1(15) 1_655
N1 H1B Cl2 0.850(17) 2.332(17) 3.1597(12) 164.7(14) 2_766
N1 H1C Cl1 0.988(16) 2.213(16) 3.1836(11) 167.2(13) 2_665
N2 H2A Cl2 0.877(18) 2.360(18) 3.2312(12) 172.4(15) 1_565
N2 H2B Cl2 0.943(16) 2.270(16) 3.1828(12) 162.7(13) 2_667
N2 H2C Cl1 0.866(18) 2.377(18) 3.2110(12) 161.6(14) 2_566

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.048

data_1b_120
_database_code_depnum_ccdc_archive 'CCDC 618059'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H14 Cl2 N2'
_chemical_formula_weight         257.15

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'
Cl Cl 0.1484 0.1585 '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                   4.3029(9)
_cell_length_b                   5.7033(9)
_cell_length_c                   12.6098(18)
_cell_angle_alpha                100.859(13)
_cell_angle_beta                 95.703(13)
_cell_angle_gamma                99.229(11)
_cell_volume                     297.29(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             134
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.6479
_diffrn_standards_number         '1 frame'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        2
_diffrn_reflns_number            7056
_diffrn_reflns_av_R_equivalents  0.0097
_diffrn_reflns_av_sigmaI/netI    0.0071
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         30.00
_reflns_number_total             1721
_reflns_number_gt                1683
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL-97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0428P)^2^+0.3514P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.27(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         1721
_refine_ls_number_parameters     86
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0912
_refine_ls_wR_factor_gt          0.0906
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.13651(8) 0.78469(6) 0.08470(3) 0.01395(13) Uani 1 1 d . . .
N1 N 0.4752(3) 0.3331(2) 0.11466(9) 0.0133(2) Uani 1 1 d . . .
C1 C 0.6333(3) 0.3853(2) 0.22697(10) 0.0112(2) Uani 1 1 d . . .
C2 C 0.6048(6) 0.5921(3) 0.29829(14) 0.0379(5) Uani 1 1 d . . .
H2 H 0.4877 0.7048 0.2746 0.045 Uiso 1 1 calc R . .
C3 C 0.7491(5) 0.6353(3) 0.40564(13) 0.0310(4) Uani 1 1 d . . .
H3 H 0.7275 0.7781 0.4548 0.037 Uiso 1 1 calc R . .
C4 C 0.9229(3) 0.4762(2) 0.44259(10) 0.0114(3) Uani 1 1 d . . .
C5 C 0.9465(6) 0.2699(4) 0.36776(15) 0.0422(6) Uani 1 1 d . . .
H5 H 1.0653 0.1572 0.3906 0.051 Uiso 1 1 calc R . .
C6 C 0.8019(5) 0.2229(4) 0.26040(13) 0.0318(5) Uani 1 1 d . . .
H6 H 0.8203 0.0794 0.2109 0.038 Uiso 1 1 calc R . .
H1A H 0.620(6) 0.325(4) 0.064(2) 0.026(6) Uiso 1 1 d . . .
H1B H 0.350(6) 0.192(5) 0.099(2) 0.027(6) Uiso 1 1 d . . .
H1C H 0.363(6) 0.449(4) 0.1038(19) 0.021(5) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.01527(18) 0.01136(18) 0.01460(18) 0.00087(11) 0.00027(11) 0.00385(11)
N1 0.0175(6) 0.0130(5) 0.0086(5) 0.0012(4) -0.0010(4) 0.0035(4)
C1 0.0123(6) 0.0122(6) 0.0082(5) 0.0019(4) 0.0002(4) 0.0004(4)
C2 0.0747(15) 0.0232(8) 0.0146(7) -0.0055(6) -0.0175(8) 0.0314(9)
C3 0.0592(12) 0.0195(8) 0.0127(7) -0.0054(5) -0.0120(7) 0.0230(8)
C4 0.0115(6) 0.0128(6) 0.0092(5) 0.0015(4) 0.0004(4) 0.0017(4)
C5 0.0688(15) 0.0401(11) 0.0168(8) -0.0124(7) -0.0202(8) 0.0445(11)
C6 0.0484(11) 0.0317(9) 0.0138(7) -0.0097(6) -0.0119(7) 0.0303(9)

_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
N1 C1 1.4635(17) . ?
N1 H1A 0.93(2) . ?
N1 H1B 0.87(3) . ?
N1 H1C 0.90(2) . ?
C1 C6 1.366(2) . ?
C1 C2 1.372(2) . ?
C2 C3 1.392(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(2) . ?
C4 C4 1.488(3) 2_766 ?
C5 C6 1.391(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?

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
C1 N1 H1A 112.1(15) . . ?
C1 N1 H1B 110.8(16) . . ?
H1A N1 H1B 106(2) . . ?
C1 N1 H1C 110.7(15) . . ?
H1A N1 H1C 108(2) . . ?
H1B N1 H1C 110(2) . . ?
C6 C1 C2 120.62(13) . . ?
C6 C1 N1 119.16(12) . . ?
C2 C1 N1 120.20(13) . . ?
C1 C2 C3 119.40(15) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 121.80(15) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 116.92(13) . . ?
C3 C4 C4 121.54(16) . 2_766 ?
C5 C4 C4 121.55(16) . 2_766 ?
C4 C5 C6 122.08(15) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C5 119.18(15) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.1(3) . . . . ?
N1 C1 C2 C3 178.13(19) . . . . ?
C1 C2 C3 C4 0.4(4) . . . . ?
C2 C3 C4 C5 -0.2(3) . . . . ?
C2 C3 C4 C4 179.9(2) . . . 2_766 ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C4 C4 C5 C6 179.6(2) 2_766 . . . ?
C2 C1 C6 C5 -0.3(3) . . . . ?
N1 C1 C6 C5 -178.6(2) . . . . ?
C4 C5 C6 C1 0.6(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl1 0.93(2) 2.28(2) 3.1813(14) 164(2) 2_665
N1 H1B Cl1 0.87(3) 2.32(3) 3.1672(14) 164(2) 1_545
N1 H1C Cl1 0.90(2) 2.32(2) 3.2192(14) 172(2) .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.081

data_1b_293
_database_code_depnum_ccdc_archive 'CCDC 618060'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H14 Cl2 N2'
_chemical_formula_weight         257.15

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'
Cl Cl 0.1484 0.1585 '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                   4.3493(8)
_cell_length_b                   5.7526(8)
_cell_length_c                   12.572(2)
_cell_angle_alpha                101.564(14)
_cell_angle_beta                 95.572(14)
_cell_angle_gamma                98.717(10)
_cell_volume                     301.97(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             134
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.6479
_diffrn_standards_number         '1 frame'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        2
_diffrn_reflns_number            8048
_diffrn_reflns_av_R_equivalents  0.0140
_diffrn_reflns_av_sigmaI/netI    0.0098
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         30.00
_reflns_number_total             1749
_reflns_number_gt                1561
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL_97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0746P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.149(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         1749
_refine_ls_number_parameters     86
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0875
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.14201(8) 0.78650(5) 0.08471(3) 0.03439(13) Uani 1 1 d . . .
N1 N 0.4698(3) 0.3339(2) 0.11521(8) 0.0313(2) Uani 1 1 d . . .
C1 C 0.6289(3) 0.3859(2) 0.22736(9) 0.0260(2) Uani 1 1 d . . .
C2 C 0.6036(5) 0.5924(3) 0.30001(12) 0.0481(4) Uani 1 1 d . . .
H2 H 0.4899 0.7027 0.2778 0.058 Uiso 1 1 calc R . .
C3 C 0.7491(4) 0.6353(3) 0.40689(11) 0.0440(4) Uani 1 1 d . . .
H3 H 0.7296 0.7750 0.4560 0.053 Uiso 1 1 calc R . .
C4 C 0.9222(3) 0.4765(2) 0.44266(9) 0.0257(2) Uani 1 1 d . . .
C5 C 0.9417(5) 0.2700(3) 0.36638(12) 0.0500(4) Uani 1 1 d . . .
H5 H 1.0564 0.1593 0.3877 0.060 Uiso 1 1 calc R . .
C6 C 0.7957(4) 0.2235(3) 0.25938(11) 0.0437(4) Uani 1 1 d . . .
H6 H 0.8113 0.0832 0.2100 0.052 Uiso 1 1 calc R . .
H1A H 0.616(5) 0.320(4) 0.0631(19) 0.055(6) Uiso 1 1 d . . .
H1B H 0.348(5) 0.191(4) 0.1003(18) 0.055(6) Uiso 1 1 d . . .
H1C H 0.362(5) 0.452(4) 0.1050(16) 0.044(5) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0394(2) 0.02872(18) 0.03326(18) 0.00143(11) -0.00062(12) 0.01101(12)
N1 0.0397(6) 0.0325(5) 0.0205(5) 0.0032(4) -0.0017(4) 0.0094(5)
C1 0.0297(5) 0.0272(5) 0.0199(5) 0.0040(4) 0.0008(4) 0.0038(4)
C2 0.0803(12) 0.0353(7) 0.0278(6) -0.0002(5) -0.0130(7) 0.0294(7)
C3 0.0721(10) 0.0318(6) 0.0256(6) -0.0027(5) -0.0093(6) 0.0235(7)
C4 0.0278(5) 0.0261(5) 0.0220(5) 0.0038(4) 0.0004(4) 0.0043(4)
C5 0.0719(11) 0.0456(8) 0.0302(7) -0.0066(6) -0.0152(7) 0.0371(8)
C6 0.0595(9) 0.0410(7) 0.0273(6) -0.0072(5) -0.0088(6) 0.0276(7)

_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
N1 C1 1.4612(15) . ?
N1 H1A 0.96(2) . ?
N1 H1B 0.88(2) . ?
N1 H1C 0.91(2) . ?
C1 C6 1.3638(18) . ?
C1 C2 1.3721(18) . ?
C2 C3 1.3861(19) . ?
C2 H2 0.9300 . ?
C3 C4 1.3827(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.3884(18) . ?
C4 C4 1.486(2) 2_766 ?
C5 C6 1.3868(19) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

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
C1 N1 H1A 111.4(14) . . ?
C1 N1 H1B 109.9(15) . . ?
H1A N1 H1B 104.3(19) . . ?
C1 N1 H1C 110.5(13) . . ?
H1A N1 H1C 108.3(19) . . ?
H1B N1 H1C 112.2(19) . . ?
C6 C1 C2 120.62(12) . . ?
C6 C1 N1 119.09(11) . . ?
C2 C1 N1 120.26(11) . . ?
C1 C2 C3 119.42(13) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 121.90(12) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 116.73(11) . . ?
C3 C4 C4 121.65(13) . 2_766 ?
C5 C4 C4 121.63(14) . 2_766 ?
C6 C5 C4 122.10(13) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
C1 C6 C5 119.24(12) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.1(3) . . . . ?
N1 C1 C2 C3 178.20(16) . . . . ?
C1 C2 C3 C4 0.5(3) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
C2 C3 C4 C4 179.94(17) . . . 2_766 ?
C3 C4 C5 C6 0.0(3) . . . . ?
C4 C4 C5 C6 179.57(18) 2_766 . . . ?
C2 C1 C6 C5 -0.4(3) . . . . ?
N1 C1 C6 C5 -178.70(16) . . . . ?
C4 C5 C6 C1 0.4(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl1 0.96(2) 2.25(2) 3.1826(14) 165.2(19) 2_665
N1 H1B Cl1 0.88(2) 2.33(2) 3.1851(14) 165(2) 1_545
N1 H1C Cl1 0.91(2) 2.32(2) 3.2214(13) 173.4(18) .

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.050

data_2_120
_database_code_depnum_ccdc_archive 'CCDC 618061'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H14 Cl2 N2'
_chemical_formula_weight         257.15

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   27.4793(11)
_cell_length_b                   6.0280(3)
_cell_length_c                   7.3190(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1212.36(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       planar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
(compiled Nov 11 2005,15:50:43)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.6479
_diffrn_standards_number         '1 frame'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        2
_diffrn_reflns_number            37294
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0068
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         30.00
_reflns_number_total             1776
_reflns_number_gt                1515
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
(compiled Nov 11 2005,15:50:43)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
(compiled Nov 11 2005,15:50:43)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
(compiled Nov 11 2005,15:50:43)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL-97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0476P)^2^+0.3709P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0061(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         1776
_refine_ls_number_parameters     102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0807
_refine_ls_wR_factor_gt          0.0785
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.206334(8) 0.25787(3) 0.10819(4) 0.01901(11) Uani 1 1 d . . .
N1 N 0.18119(3) 0.75332(14) 0.19972(14) 0.01725(19) Uani 1 1 d . . .
C1 C 0.12794(4) 0.74954(14) 0.20897(14) 0.0145(2) Uani 1 1 d . . .
C2 C 0.10139(3) 0.93249(16) 0.15241(14) 0.0162(2) Uani 1 1 d . . .
C3 C 0.05094(3) 0.92850(16) 0.16907(14) 0.01555(19) Uani 1 1 d . . .
C4 C 0.02693(3) 0.74350(13) 0.24072(13) 0.01327(19) Uani 1 1 d . . .
C5 C 0.05467(3) 0.56051(16) 0.29485(14) 0.0158(2) Uani 1 1 d . . .
C6 C 0.10518(3) 0.56298(16) 0.28004(14) 0.0164(2) Uani 1 1 d . . .
H1A H 0.1940(5) 0.635(3) 0.144(2) 0.033(4) Uiso 1 1 d . . .
H1B H 0.1962(7) 0.748(2) 0.317(3) 0.036(5) Uiso 1 1 d . . .
H1C H 0.1927(5) 0.865(3) 0.147(2) 0.028(4) Uiso 1 1 d . . .
H2 H 0.1166(5) 1.060(2) 0.1049(18) 0.022(3) Uiso 1 1 d . . .
H3 H 0.0338(4) 1.054(2) 0.1281(18) 0.021(3) Uiso 1 1 d . . .
H5 H 0.0400(4) 0.432(2) 0.3457(19) 0.021(3) Uiso 1 1 d . . .
H6 H 0.1232(4) 0.436(2) 0.3175(19) 0.021(3) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.01185(15) 0.01366(14) 0.03151(17) -0.00030(8) -0.00275(8) -0.00027(7)
N1 0.0090(4) 0.0156(4) 0.0271(5) 0.0004(3) 0.0011(3) 0.0003(3)
C1 0.0090(4) 0.0161(4) 0.0184(4) -0.0016(3) 0.0005(3) 0.0001(3)
C2 0.0119(4) 0.0148(4) 0.0219(5) 0.0016(4) 0.0006(3) -0.0008(3)
C3 0.0115(4) 0.0146(4) 0.0205(4) 0.0018(3) -0.0008(3) 0.0007(3)
C4 0.0097(4) 0.0152(4) 0.0149(4) -0.0012(3) 0.0002(3) 0.0000(3)
C5 0.0124(4) 0.0149(4) 0.0202(4) 0.0017(3) 0.0015(3) -0.0003(3)
C6 0.0126(4) 0.0146(4) 0.0219(5) 0.0017(3) 0.0000(3) 0.0018(3)

_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
N1 C1 1.4650(13) . ?
N1 H1A 0.894(17) . ?
N1 H1B 0.96(2) . ?
N1 H1C 0.839(16) . ?
C1 C2 1.3856(13) . ?
C1 C6 1.3879(13) . ?
C2 C3 1.3919(12) . ?
C2 H2 0.943(14) . ?
C3 C4 1.3979(12) . ?
C3 H3 0.940(13) . ?
C4 C5 1.3982(12) . ?
C4 C4 1.4860(18) 3 ?
C5 C6 1.3924(13) . ?
C5 H5 0.951(13) . ?
C6 H6 0.952(13) . ?

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
C1 N1 H1A 113.6(10) . . ?
C1 N1 H1B 112.9(11) . . ?
H1A N1 H1B 102.2(13) . . ?
C1 N1 H1C 114.2(10) . . ?
H1A N1 H1C 106.6(16) . . ?
H1B N1 H1C 106.3(13) . . ?
C2 C1 C6 121.31(9) . . ?
C2 C1 N1 119.98(8) . . ?
C6 C1 N1 118.68(8) . . ?
C1 C2 C3 118.98(9) . . ?
C1 C2 H2 121.8(8) . . ?
C3 C2 H2 119.2(8) . . ?
C2 C3 C4 121.12(9) . . ?
C2 C3 H3 117.3(8) . . ?
C4 C3 H3 121.6(8) . . ?
C3 C4 C5 118.57(9) . . ?
C3 C4 C4 120.29(6) . 3 ?
C5 C4 C4 121.14(6) . 3 ?
C6 C5 C4 120.87(9) . . ?
C6 C5 H5 117.5(7) . . ?
C4 C5 H5 121.6(7) . . ?
C1 C6 C5 119.14(9) . . ?
C1 C6 H6 121.6(7) . . ?
C5 C6 H6 119.3(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.54(15) . . . . ?
N1 C1 C2 C3 -177.52(9) . . . . ?
C1 C2 C3 C4 -0.30(15) . . . . ?
C2 C3 C4 C5 -0.36(14) . . . . ?
C2 C3 C4 C4 179.32(10) . . . 3 ?
C3 C4 C5 C6 0.79(14) . . . . ?
C4 C4 C5 C6 -178.89(11) 3 . . . ?
C2 C1 C6 C5 -0.12(15) . . . . ?
N1 C1 C6 C5 177.97(9) . . . . ?
C4 C5 C6 C1 -0.56(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1B Cl1 0.96(2) 2.15(2) 3.0691(10) 161.8(16) 7_566
N1 H1C Cl1 0.839(16) 2.414(16) 3.1901(9) 154.2(14) 1_565
N1 H1C Cl1 0.839(16) 2.863(14) 3.1626(9) 103.3(11) 8_665
N1 H1A Cl1 0.894(17) 2.312(17) 3.1378(9) 153.6(14) .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.049

data_2_293
_database_code_depnum_ccdc_archive 'CCDC 618062'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H14 Cl2 N2'
_chemical_formula_weight         257.15

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   27.459(3)
_cell_length_b                   6.0877(8)
_cell_length_c                   7.3074(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1221.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.6479
_diffrn_standards_number         '1 frame'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        2
_diffrn_reflns_number            39654
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0118
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         29.97
_reflns_number_total             1783
_reflns_number_gt                1231
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle2 beta (release 25-10-2005 CrysAlis171 .NET)
(compiled Oct 25 2005,08:50:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL-97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0727P)^2^+0.4919P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1783
_refine_ls_number_parameters     101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1465
_refine_ls_wR_factor_gt          0.1313
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.205962(17) 0.25667(7) 0.13427(9) 0.0471(2) Uani 1 1 d . . .
N1 N 0.18138(6) 0.7513(3) 0.2234(3) 0.0415(4) Uani 1 1 d . . .
C1 C 0.12792(6) 0.7486(3) 0.2258(3) 0.0333(4) Uani 1 1 d . . .
C2 C 0.10198(6) 0.9283(3) 0.1667(3) 0.0389(5) Uani 1 1 d . . .
C3 C 0.05157(6) 0.9252(3) 0.1766(3) 0.0368(4) Uani 1 1 d . . .
C4 C 0.02694(6) 0.7434(3) 0.2448(2) 0.0290(4) Uani 1 1 d . . .
C5 C 0.05399(6) 0.5630(3) 0.3023(3) 0.0357(4) Uani 1 1 d . . .
C6 C 0.10440(6) 0.5656(3) 0.2943(3) 0.0381(5) Uani 1 1 d . . .
H1A H 0.1994(10) 0.636(6) 0.170(5) 0.080(10) Uiso 1 1 d . . .
H1B H 0.1994(10) 0.750(3) 0.340(4) 0.051(8) Uiso 1 1 d . . .
H1C H 0.1982(10) 0.852(6) 0.171(5) 0.080(11) Uiso 1 1 d . . .
H2 H 0.1178(8) 1.054(4) 0.119(3) 0.056(7) Uiso 1 1 d . . .
H3 H 0.0317(8) 1.053(4) 0.137(3) 0.048(6) Uiso 1 1 d . . .
H5 H 0.0357(8) 0.432(4) 0.355(3) 0.054(7) Uiso 1 1 d . . .
H6 H 0.1222(8) 0.441(4) 0.329(3) 0.054(7) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0267(3) 0.0333(3) 0.0813(4) -0.0011(2) -0.0082(2) -0.00082(17)
N1 0.0194(7) 0.0395(9) 0.0657(12) -0.0002(9) 0.0007(7) 0.0007(7)
C1 0.0188(7) 0.0365(9) 0.0445(10) -0.0027(8) 0.0009(7) -0.0003(6)
C2 0.0259(9) 0.0341(9) 0.0567(12) 0.0064(9) 0.0000(8) -0.0029(7)
C3 0.0240(8) 0.0350(9) 0.0514(11) 0.0059(8) -0.0025(7) 0.0003(7)
C4 0.0204(7) 0.0344(9) 0.0321(8) -0.0015(8) -0.0008(6) 0.0001(7)
C5 0.0252(8) 0.0347(9) 0.0473(11) 0.0054(8) 0.0033(7) 0.0001(7)
C6 0.0269(9) 0.0352(9) 0.0523(12) 0.0046(9) 0.0004(8) 0.0047(7)

_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
N1 C1 1.468(2) . ?
N1 H1A 0.94(3) . ?
N1 H1B 0.99(3) . ?
N1 H1C 0.86(3) . ?
C1 C2 1.375(3) . ?
C1 C6 1.382(3) . ?
C2 C3 1.386(2) . ?
C2 H2 0.94(3) . ?
C3 C4 1.390(2) . ?
C3 H3 0.99(2) . ?
C4 C5 1.391(2) . ?
C4 C4 1.481(3) 3 ?
C5 C6 1.386(2) . ?
C5 H5 1.02(2) . ?
C6 H6 0.94(2) . ?

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
C1 N1 H1A 121.3(18) . . ?
C1 N1 H1B 119.4(16) . . ?
H1A N1 H1B 95(2) . . ?
C1 N1 H1C 123(2) . . ?
H1A N1 H1C 94(3) . . ?
H1B N1 H1C 97(2) . . ?
C2 C1 C6 120.88(17) . . ?
C2 C1 N1 120.33(17) . . ?
C6 C1 N1 118.74(16) . . ?
C1 C2 C3 119.36(18) . . ?
C1 C2 H2 121.3(14) . . ?
C3 C2 H2 119.3(14) . . ?
C2 C3 C4 121.01(17) . . ?
C2 C3 H3 121.5(13) . . ?
C4 C3 H3 117.5(13) . . ?
C3 C4 C5 118.51(16) . . ?
C3 C4 C4 120.30(12) . 3 ?
C5 C4 C4 121.19(12) . 3 ?
C6 C5 C4 120.81(17) . . ?
C6 C5 H5 121.1(13) . . ?
C4 C5 H5 118.0(13) . . ?
C1 C6 C5 119.42(17) . . ?
C1 C6 H6 120.4(14) . . ?
C5 C6 H6 120.1(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.1(3) . . . . ?
N1 C1 C2 C3 -177.6(2) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C2 C3 C4 C5 -0.4(3) . . . . ?
C2 C3 C4 C4 179.7(2) . . . 3 ?
C3 C4 C5 C6 0.9(3) . . . . ?
C4 C4 C5 C6 -179.1(2) 3 . . . ?
C2 C1 C6 C5 0.5(3) . . . . ?
N1 C1 C6 C5 178.19(19) . . . . ?
C4 C5 C6 C1 -1.0(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1B Cl1 0.99(3) 2.16(3) 3.078(2) 155(2) 7_566
N1 H1C Cl1 0.86(3) 2.48(4) 3.2161(19) 143(3) 1_565
N1 H1C Cl1 0.86(3) 2.71(3) 3.1614(18) 114(3) 8_665
N1 H1A Cl1 0.94(3) 2.33(4) 3.1540(18) 145(3) .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        29.97
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.054

#=END


