# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co358K
_database_code_depnum_ccdc_archive 'CCDC 1429214'
_audit_update_record             
;
2015-12-02 deposited with the CCDC.
2015-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H15 Cl5 Co N2'
_chemical_formula_weight         363.39

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   11.178(11)
_cell_length_b                   10.166(10)
_cell_length_c                   12.216(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1388(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    358(2)
_cell_measurement_reflns_used    4460
_cell_measurement_theta_min      2.4698
_cell_measurement_theta_max      25.9602

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    2.169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5528
_exptl_absorpt_correction_T_max  0.6024
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      358(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9732
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         25.01
_reflns_number_total             1299
_reflns_number_gt                1181
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
difx 0.93 0.01 h2a c2 h3a c3
isor 0.01 c14 h1wa h1 h1e
dfix 0.94 0.01 c1 h1wa
exyz h1 h1e
eadp h1 h1e
;

_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)+(0.0349P)²+1.6779P] 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     SHELXL
_refine_ls_extinction_coef       0.0096(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1299
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0789
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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
Co1 Co 0.28738(4) 0.2500 0.57524(4) 0.0474(2) Uani 1 2 d S . .
Cl1 Cl 0.26724(14) 0.2500 0.39421(10) 0.1044(6) Uani 1 2 d S . .
N1 N 0.8245(2) 0.2500 0.4603(2) 0.0361(6) Uani 1 2 d S . .
C1 C 0.9358(4) 0.2500 0.3914(4) 0.0589(12) Uani 1 2 d S . .
H1WA H 0.926(7) 0.182(7) 0.336(6) 0.071 Uiso 0.50 1 d P A 2
H1 H 1.002(5) 0.2500 0.444(4) 0.071 Uiso 1 2 d S B 1
Cl2 Cl 0.39520(7) 0.07754(7) 0.64058(7) 0.0599(3) Uani 1 1 d . . .
N2 N 0.6418(3) 0.2500 0.5803(2) 0.0426(7) Uani 1 2 d S . .
H2 H 0.582(4) 0.2500 0.621(4) 0.051 Uiso 1 2 d S . .
C2 C 0.7127(3) 0.2500 0.3908(3) 0.0435(9) Uani 1 2 d S . .
H2A H 0.716(2) 0.177(3) 0.350(2) 0.052 Uiso 1 1 d . . .
Cl3 Cl 0.10183(10) 0.2500 0.64735(10) 0.1039(7) Uani 1 2 d S . .
C3 C 0.6035(3) 0.2500 0.4631(3) 0.0450(9) Uani 1 2 d S C .
H3A H 0.561(3) 0.175(3) 0.453(2) 0.054 Uiso 1 1 d . . .
C4 C 0.7122(3) 0.1291(3) 0.6028(2) 0.0556(8) Uani 1 1 d . C .
H4A H 0.6641 0.0519 0.5869 0.067 Uiso 1 1 calc R . .
H4B H 0.7345 0.1264 0.6795 0.067 Uiso 1 1 calc R . .
Cl4 Cl 0.96228(15) 0.1195(2) 0.31503(15) 0.0719(5) Uani 0.50 1 d P C 1
C5 C 0.8236(2) 0.1289(3) 0.5320(2) 0.0473(6) Uani 1 1 d . . .
H5A H 0.8943 0.1280 0.5780 0.057 Uiso 1 1 calc R C .
H5B H 0.8248 0.0505 0.4867 0.057 Uiso 1 1 calc R . .

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
Co1 0.0368(3) 0.0692(4) 0.0361(3) 0.000 -0.0005(2) 0.000
Cl1 0.0808(9) 0.199(2) 0.0337(6) 0.000 -0.0027(6) 0.000
N1 0.0300(14) 0.0442(16) 0.0342(14) 0.000 0.0000(12) 0.000
C1 0.038(2) 0.088(4) 0.051(2) 0.000 0.012(2) 0.000
Cl2 0.0582(5) 0.0474(4) 0.0741(5) -0.0008(4) -0.0002(4) -0.0022(3)
N2 0.0384(17) 0.0542(19) 0.0353(16) 0.000 0.0062(13) 0.000
C2 0.0377(19) 0.061(2) 0.0319(19) 0.000 -0.0055(15) 0.000
Cl3 0.0337(6) 0.232(2) 0.0455(6) 0.000 -0.0021(5) 0.000
C3 0.034(2) 0.058(2) 0.042(2) 0.000 -0.0046(16) 0.000
C4 0.0573(17) 0.0620(19) 0.0476(16) 0.0179(14) 0.0038(13) 0.0066(15)
Cl4 0.0601(9) 0.0923(13) 0.0634(9) -0.0218(9) 0.0080(8) 0.0244(9)
C5 0.0454(14) 0.0445(15) 0.0521(15) 0.0102(12) -0.0018(12) 0.0069(12)

_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
Co1 Cl1 2.223(2) . ?
Co1 Cl3 2.253(2) . ?
Co1 Cl2 2.2724(17) 7_565 ?
Co1 Cl2 2.2724(17) . ?
N1 C1 1.502(5) . ?
N1 C2 1.511(5) . ?
N1 C5 1.511(3) 7_565 ?
N1 C5 1.511(3) . ?
C1 Cl4 1.648(3) 7_565 ?
C1 Cl4 1.648(3) . ?
C1 H1WA 0.97(8) . ?
C1 H1 0.98(5) . ?
N2 C4 1.485(4) 7_565 ?
N2 C4 1.485(4) . ?
N2 C3 1.494(5) . ?
N2 H2 0.83(4) . ?
C2 C3 1.507(5) . ?
C2 H2A 0.90(3) . ?
C3 H3A 0.91(3) . ?
C4 C5 1.517(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
Cl4 H1WA 0.79(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?

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
Cl1 Co1 Cl3 107.20(6) . . ?
Cl1 Co1 Cl2 113.78(4) . 7_565 ?
Cl3 Co1 Cl2 110.54(5) . 7_565 ?
Cl1 Co1 Cl2 113.78(4) . . ?
Cl3 Co1 Cl2 110.54(5) . . ?
Cl2 Co1 Cl2 100.99(8) 7_565 . ?
C1 N1 C2 111.7(3) . . ?
C1 N1 C5 109.31(19) . 7_565 ?
C2 N1 C5 108.65(18) . 7_565 ?
C1 N1 C5 109.31(19) . . ?
C2 N1 C5 108.65(19) . . ?
C5 N1 C5 109.1(3) 7_565 . ?
N1 C1 Cl4 117.76(19) . 7_565 ?
N1 C1 Cl4 117.76(19) . . ?
Cl4 C1 Cl4 107.2(3) 7_565 . ?
N1 C1 H1WA 107(4) . . ?
Cl4 C1 H1WA 102(4) 7_565 . ?
Cl4 C1 H1WA 19(4) . . ?
N1 C1 H1 105(3) . . ?
Cl4 C1 H1 103.6(17) 7_565 . ?
Cl4 C1 H1 103.6(17) . . ?
H1WA C1 H1 122(5) . . ?
C4 N2 C4 111.7(3) 7_565 . ?
C4 N2 C3 109.2(2) 7_565 . ?
C4 N2 C3 109.2(2) . . ?
C4 N2 H2 108.5(15) 7_565 . ?
C4 N2 H2 108.5(15) . . ?
C3 N2 H2 110(3) . . ?
C3 C2 N1 109.9(3) . . ?
C3 C2 H2A 110.8(19) . . ?
N1 C2 H2A 106.5(19) . . ?
N2 C3 C2 109.3(3) . . ?
N2 C3 H3A 106.6(19) . . ?
C2 C3 H3A 110.2(19) . . ?
N2 C4 C5 109.3(2) . . ?
N2 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
N2 C4 H4B 109.8 . . ?
C5 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
C1 Cl4 H1WA 24(5) . . ?
N1 C5 C4 109.6(2) . . ?
N1 C5 H5A 109.8 . . ?
C4 C5 H5A 109.8 . . ?
N1 C5 H5B 109.8 . . ?
C4 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.051
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co100K
_database_code_depnum_ccdc_archive 'CCDC 1429215'
_audit_update_record             
;
2015-12-02 deposited with the CCDC.
2015-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H15 Cl5 Co N2 '
_chemical_formula_weight         363.39

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   10.0525(19)
_cell_length_b                   12.081(2)
_cell_length_c                   11.042(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.329(3)
_cell_angle_gamma                90.00
_cell_volume                     1340.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5500
_cell_measurement_theta_min      2.4994
_cell_measurement_theta_max      27.4351

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    2.247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5427
_exptl_absorpt_correction_T_max  0.5927
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6654
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         25.10
_reflns_number_total             2362
_reflns_number_gt                2277
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
dfix 0.86 0.01 N2 H2
;

_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)+(0.0260P)²+0.7433P] 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_extinction_coef       ?
_refine_ls_number_reflns         2362
_refine_ls_number_parameters     140
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0495
_refine_ls_wR_factor_gt          0.0490
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
Co1 Co 0.72965(2) 0.075592(18) 0.210440(19) 0.01381(8) Uani 1 1 d . . .
N1 N 0.75017(13) -0.04320(11) 0.67381(12) 0.0125(3) Uani 1 1 d . . .
Cl1 Cl 0.91150(4) 0.13447(3) 0.11018(4) 0.01940(10) Uani 1 1 d . . .
C1 C 0.74016(17) -0.11457(15) 0.56203(15) 0.0190(4) Uani 1 1 d . . .
H1A H 0.7198 -0.0671 0.4909 0.023 Uiso 1 1 calc R . .
H1B H 0.6657 -0.1674 0.5706 0.023 Uiso 1 1 calc R . .
N2 N 0.75219(14) 0.08017(11) 0.85808(13) 0.0143(3) Uani 1 1 d D . .
H2 H 0.7555(18) 0.1230(14) 0.9227(15) 0.015(5) Uiso 1 1 d D . .
Cl2 Cl 0.72459(6) 0.14820(4) 0.39901(4) 0.03274(13) Uani 1 1 d . . .
C2 C 0.86842(16) 0.03394(14) 0.67147(16) 0.0181(4) Uani 1 1 d . . .
H2A H 0.8636 0.0800 0.5974 0.022 Uiso 1 1 calc R . .
H2B H 0.9517 -0.0097 0.6700 0.022 Uiso 1 1 calc R . .
C3 C 0.86929(18) 0.10797(15) 0.78295(17) 0.0222(4) Uani 1 1 d . . .
H3A H 0.9526 0.0966 0.8309 0.027 Uiso 1 1 calc R . .
H3B H 0.8649 0.1866 0.7580 0.027 Uiso 1 1 calc R . .
Cl3 Cl 0.72015(5) -0.10893(4) 0.23143(4) 0.02669(11) Uani 1 1 d . . .
Cl4 Cl 0.56106(4) 0.14773(3) 0.09523(4) 0.01943(10) Uani 1 1 d . . .
C4 C 0.62396(16) 0.02507(14) 0.67628(15) 0.0167(3) Uani 1 1 d . . .
H4A H 0.5456 -0.0246 0.6765 0.020 Uiso 1 1 calc R . .
H4B H 0.6175 0.0720 0.6029 0.020 Uiso 1 1 calc R . .
Cl5 Cl 0.88712(4) -0.18858(4) 0.53663(4) 0.02503(11) Uani 1 1 d . . .
C5 C 0.62463(18) 0.09768(15) 0.78874(16) 0.0209(4) Uani 1 1 d . . .
H5A H 0.6160 0.1764 0.7651 0.025 Uiso 1 1 calc R . .
H5B H 0.5485 0.0783 0.8399 0.025 Uiso 1 1 calc R . .
C6 C 0.75836(17) -0.11284(14) 0.78703(14) 0.0162(3) Uani 1 1 d . . .
H6A H 0.8398 -0.1589 0.7865 0.019 Uiso 1 1 calc R . .
H6B H 0.6804 -0.1628 0.7898 0.019 Uiso 1 1 calc R . .
C7 C 0.76136(17) -0.03765(13) 0.89840(14) 0.0156(3) Uani 1 1 d . . .
H7A H 0.6858 -0.0556 0.9509 0.019 Uiso 1 1 calc R . .
H7B H 0.8450 -0.0494 0.9457 0.019 Uiso 1 1 calc R . .

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
Co1 0.01790(13) 0.01055(13) 0.01307(13) 0.00043(8) 0.00229(9) -0.00043(8)
N1 0.0144(7) 0.0119(6) 0.0111(7) 0.0000(5) 0.0017(5) 0.0012(5)
Cl1 0.0138(2) 0.0246(2) 0.0198(2) -0.00118(17) 0.00205(15) -0.00277(16)
C1 0.0234(9) 0.0196(9) 0.0141(8) -0.0061(7) 0.0022(7) 0.0035(7)
N2 0.0187(7) 0.0113(7) 0.0129(7) -0.0018(5) 0.0005(6) -0.0001(5)
Cl2 0.0726(4) 0.0141(2) 0.0117(2) 0.00053(16) 0.0035(2) 0.0026(2)
C2 0.0154(8) 0.0185(9) 0.0207(9) 0.0015(7) 0.0045(7) -0.0040(7)
C3 0.0251(9) 0.0176(9) 0.0243(10) 0.0001(7) 0.0054(7) -0.0086(7)
Cl3 0.0417(3) 0.0103(2) 0.0280(2) 0.00155(17) -0.0002(2) 0.00150(18)
Cl4 0.0153(2) 0.0226(2) 0.0203(2) 0.00283(16) 0.00103(15) 0.00014(15)
C4 0.0138(8) 0.0190(9) 0.0173(8) -0.0011(7) 0.0003(6) 0.0051(7)
Cl5 0.0308(2) 0.0225(2) 0.0221(2) -0.00308(17) 0.00931(18) 0.00851(18)
C5 0.0224(9) 0.0181(9) 0.0220(9) -0.0045(7) -0.0045(7) 0.0091(7)
C6 0.0250(9) 0.0110(8) 0.0127(8) 0.0024(6) 0.0020(7) 0.0009(7)
C7 0.0225(9) 0.0109(8) 0.0135(8) 0.0011(6) 0.0007(6) -0.0004(6)

_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
Co1 Cl3 2.2434(6) . ?
Co1 Cl2 2.2610(6) . ?
Co1 Cl4 2.2693(5) . ?
Co1 Cl1 2.2731(5) . ?
N1 C1 1.507(2) . ?
N1 C6 1.508(2) . ?
N1 C2 1.511(2) . ?
N1 C4 1.514(2) . ?
C1 Cl5 1.7550(17) . ?
N2 C5 1.493(2) . ?
N2 C7 1.494(2) . ?
N2 C3 1.494(2) . ?
C2 C3 1.521(2) . ?
C4 C5 1.520(2) . ?
C6 C7 1.529(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
Cl3 Co1 Cl2 106.76(2) . . ?
Cl3 Co1 Cl4 113.984(19) . . ?
Cl2 Co1 Cl4 109.56(2) . . ?
Cl3 Co1 Cl1 113.447(19) . . ?
Cl2 Co1 Cl1 111.26(2) . . ?
Cl4 Co1 Cl1 101.85(2) . . ?
C1 N1 C6 111.18(13) . . ?
C1 N1 C2 112.11(13) . . ?
C6 N1 C2 109.30(13) . . ?
C1 N1 C4 106.64(12) . . ?
C6 N1 C4 108.58(12) . . ?
C2 N1 C4 108.92(13) . . ?
N1 C1 Cl5 112.45(11) . . ?
C5 N2 C7 109.52(13) . . ?
C5 N2 C3 111.21(14) . . ?
C7 N2 C3 109.62(13) . . ?
N1 C2 C3 109.78(13) . . ?
N2 C3 C2 109.11(13) . . ?
N1 C4 C5 109.95(13) . . ?
N2 C5 C4 108.94(13) . . ?
N1 C6 C7 109.59(13) . . ?
N2 C7 C6 109.06(13) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.061
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Zn363K
_database_code_depnum_ccdc_archive 'CCDC 1429216'
_audit_update_record             
;
2015-12-02 deposited with the CCDC.
2015-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H15 Cl5 N2  Zn'
_chemical_formula_weight         369.85

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'
O O 0.0106 0.0060 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   11.190(6)
_cell_length_b                   10.204(6)
_cell_length_c                   12.278(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1402.0(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    363(2)
_cell_measurement_reflns_used    3971
_cell_measurement_theta_min      2.4626
_cell_measurement_theta_max      25.8192

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    2.676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4814
_exptl_absorpt_correction_T_max  0.5108
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      363(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9844
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         25.09
_reflns_number_total             1326
_reflns_number_gt                1193
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
difx 0.95 0.01 c1 h1 c1 h1ac c1 h1a
dfix 0.96 0.01 c3 h3a c2 h2a
exyz h1 h1ac
eadp h1 h1ac
dfix 0.96 0.01 c1 h1wa
isor 0.01 c14 h1wa h1 h1ac
;

_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)+(0.0246P)²+1.6816P] 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_extinction_coef       0.0061(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1326
_refine_ls_number_parameters     105
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0669
_refine_ls_wR_factor_gt          0.0646
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.014
_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
Zn1 Zn 0.78674(4) 0.7500 0.42521(3) 0.04892(18) Uani 1 2 d S . .
Cl1 Cl 0.89426(7) 0.92261(7) 0.35950(7) 0.0607(2) Uani 1 1 d . . .
N1 N 0.3245(2) 0.7500 0.5399(2) 0.0371(7) Uani 1 2 d S . .
C1 C 0.4359(4) 0.7500 0.6084(4) 0.0603(12) Uani 1 2 d SD . .
H1A H 0.506(13) 0.7500 0.562(17) 0.072 Uiso 0.50 2 d SPD A 1
H1WA H 0.426(5) 0.817(4) 0.663(3) 0.045(17) Uiso 0.50 1 d PD B 2
H1AC H 0.501(13) 0.7500 0.556(14) 0.053 Uiso 0.50 2 d SPD C 2
Cl2 Cl 0.76883(14) 0.7500 0.60574(10) 0.1044(6) Uani 1 2 d S . .
N2 N 0.1411(3) 0.7500 0.4198(2) 0.0427(7) Uani 1 2 d SD . .
C2 C 0.2125(3) 0.7500 0.6091(3) 0.0430(9) Uani 1 2 d SD . .
Cl3 Cl 0.60149(10) 0.7500 0.35212(10) 0.1018(6) Uani 1 2 d S . .
C3 C 0.1030(3) 0.7500 0.5368(3) 0.0449(9) Uani 1 2 d SD D .
C4 C 0.2120(3) 0.8706(3) 0.3972(2) 0.0570(8) Uani 1 1 d . D .
H4A H 0.1647 0.9468 0.4127 0.068 Uiso 1 1 d R . .
H4B H 0.2343 0.8730 0.3218 0.068 Uiso 1 1 d R . .
Cl4 Cl 0.46249(15) 0.8805(2) 0.68478(14) 0.0724(5) Uani 0.50 1 d PU D 1
C5 C 0.3232(2) 0.8708(3) 0.4680(2) 0.0482(7) Uani 1 1 d . . .
H5A H 0.3931 0.8716 0.4227 0.058 Uiso 1 1 d R D .
H5B H 0.3242 0.9481 0.5125 0.058 Uiso 1 1 d R . .
H2A H 0.216(2) 0.8275(18) 0.654(2) 0.059(9) Uiso 1 1 d D . .
H3A H 0.057(2) 0.8292(18) 0.546(2) 0.066(9) Uiso 1 1 d D . .
H2 H 0.074(2) 0.7500 0.379(3) 0.065(13) Uiso 1 2 d SD . .

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
Zn1 0.0378(3) 0.0715(3) 0.0375(3) 0.000 0.00053(18) 0.000
Cl1 0.0593(5) 0.0475(4) 0.0753(5) -0.0015(4) 0.0005(4) 0.0026(3)
N1 0.0303(14) 0.0452(17) 0.0358(15) 0.000 -0.0002(12) 0.000
C1 0.038(2) 0.090(4) 0.054(3) 0.000 -0.012(2) 0.000
Cl2 0.0794(9) 0.1994(19) 0.0344(6) 0.000 0.0026(6) 0.000
N2 0.0383(17) 0.0536(19) 0.0362(16) 0.000 -0.0053(13) 0.000
C2 0.0356(19) 0.062(3) 0.0315(18) 0.000 0.0055(15) 0.000
Cl3 0.0328(6) 0.226(2) 0.0467(6) 0.000 0.0020(5) 0.000
C3 0.035(2) 0.059(3) 0.041(2) 0.000 0.0040(16) 0.000
C4 0.0601(18) 0.0605(19) 0.0504(16) 0.0186(14) -0.0050(14) -0.0054(15)
Cl4 0.0608(10) 0.0911(13) 0.0654(9) -0.0217(9) -0.0083(8) -0.0244(9)
C5 0.0461(15) 0.0450(15) 0.0537(15) 0.0088(13) 0.0033(13) -0.0071(12)

_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
Zn1 Cl2 2.2256(17) . ?
Zn1 Cl3 2.2589(16) . ?
Zn1 Cl1 2.2806(12) . ?
Zn1 Cl1 2.2806(12) 7_575 ?
N1 C1 1.504(5) . ?
N1 C2 1.514(4) . ?
N1 C5 1.516(3) 7_575 ?
N1 C5 1.516(3) . ?
C1 Cl4 1.656(3) . ?
C1 Cl4 1.656(3) 7_575 ?
C1 H1A 0.969(10) . ?
C1 H1WA 0.960(10) . ?
C1 H1AC 0.969(10) . ?
N2 C4 1.490(3) . ?
N2 C4 1.490(3) 7_575 ?
N2 C3 1.498(5) . ?
N2 H2 0.909(10) . ?
C2 C3 1.513(5) . ?
C2 H2A 0.965(10) . ?
C3 H3A 0.964(10) . ?
C4 C5 1.517(4) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
Cl4 H1WA 0.81(4) . ?
C5 H5A 0.9599 . ?
C5 H5B 0.9599 . ?

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
Cl2 Zn1 Cl3 108.24(6) . . ?
Cl2 Zn1 Cl1 113.57(3) . . ?
Cl3 Zn1 Cl1 110.10(4) . . ?
Cl2 Zn1 Cl1 113.57(3) . 7_575 ?
Cl3 Zn1 Cl1 110.10(4) . 7_575 ?
Cl1 Zn1 Cl1 101.13(6) . 7_575 ?
C1 N1 C2 111.8(3) . . ?
C1 N1 C5 109.50(19) . 7_575 ?
C2 N1 C5 108.58(18) . 7_575 ?
C1 N1 C5 109.50(19) . . ?
C2 N1 C5 108.58(18) . . ?
C5 N1 C5 108.8(3) 7_575 . ?
N1 C1 Cl4 117.76(18) . . ?
N1 C1 Cl4 117.76(18) . 7_575 ?
Cl4 C1 Cl4 107.1(3) . 7_575 ?
N1 C1 H1A 110(10) . . ?
Cl4 C1 H1A 101(9) . . ?
Cl4 C1 H1A 101(9) 7_575 . ?
N1 C1 H1WA 107(4) . . ?
Cl4 C1 H1WA 19(4) . . ?
Cl4 C1 H1WA 101(3) 7_575 . ?
H1A C1 H1WA 120(10) . . ?
N1 C1 H1AC 104(10) . . ?
Cl4 C1 H1AC 104(8) . . ?
Cl4 C1 H1AC 104(7) 7_575 . ?
H1A C1 H1AC 6(10) . . ?
H1WA C1 H1AC 123(8) . . ?
C4 N2 C4 111.3(3) . 7_575 ?
C4 N2 C3 109.25(19) . . ?
C4 N2 C3 109.25(19) 7_575 . ?
C4 N2 H2 109.8(14) . . ?
C4 N2 H2 109.8(14) 7_575 . ?
C3 N2 H2 107(3) . . ?
C3 C2 N1 109.9(3) . . ?
C3 C2 H2A 111.4(17) . . ?
N1 C2 H2A 107.0(18) . . ?
N2 C3 C2 109.4(3) . . ?
N2 C3 H3A 105.6(19) . . ?
C2 C3 H3A 111.0(19) . . ?
N2 C4 C5 109.3(2) . . ?
N2 C4 H4A 109.7 . . ?
C5 C4 H4A 109.8 . . ?
N2 C4 H4B 109.8 . . ?
C5 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
C1 Cl4 H1WA 23(3) . . ?
N1 C5 C4 109.9(2) . . ?
N1 C5 H5A 109.7 . . ?
C4 C5 H5A 109.6 . . ?
N1 C5 H5B 109.7 . . ?
C4 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.048
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Zn100K
_database_code_depnum_ccdc_archive 'CCDC 1429217'
_audit_update_record             
;
2015-12-02 deposited with the CCDC.
2015-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H15 Cl5 N2 Zn'
_chemical_formula_weight         369.83

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'
Zn Zn 0.2839 1.4301 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.0664(17)
_cell_length_b                   12.075(2)
_cell_length_c                   11.0158(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.262(2)
_cell_angle_gamma                90.00
_cell_volume                     1338.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8310
_cell_measurement_theta_min      2.5030
_cell_measurement_theta_max      27.6312

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    2.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4770
_exptl_absorpt_correction_T_max  0.5075
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9301
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         25.10
_reflns_number_total             2353
_reflns_number_gt                2290
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
dfix 0.86 0.01 N2 H2
;

_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)+(0.0766P)²+15.2955P] 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     SHELXL
_refine_ls_extinction_coef       0.0061(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2353
_refine_ls_number_parameters     140
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1494
_refine_ls_wR_factor_gt          0.1490
_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
Zn1 Zn 0.72975(6) 0.92502(5) 0.21122(6) 0.0115(3) Uani 1 1 d . . .
Cl1 Cl 0.72599(19) 0.85094(12) 0.39977(13) 0.0247(4) Uani 1 1 d . . .
N1 N 0.7502(5) 0.0434(4) 0.6740(4) 0.0111(10) Uani 1 1 d . . .
C1 C 0.7401(6) 0.1158(5) 0.5616(5) 0.0140(12) Uani 1 1 d . . .
H1A H 0.6663 0.1691 0.5709 0.017 Uiso 1 1 calc R . .
H1B H 0.7190 0.0688 0.4901 0.017 Uiso 1 1 calc R . .
Cl2 Cl 0.91223(13) 0.86596(12) 0.11099(12) 0.0153(4) Uani 1 1 d . . .
N2 N 0.7529(5) -0.0802(4) 0.8592(4) 0.0129(10) Uani 1 1 d D . .
H2 H 0.759(7) -0.119(5) 0.929(4) 0.015 Uiso 1 1 d D . .
C2 C 0.8682(6) -0.0328(5) 0.6714(5) 0.0141(12) Uani 1 1 d . . .
H2A H 0.9511 0.0112 0.6708 0.017 Uiso 1 1 calc R . .
H2B H 0.8641 -0.0785 0.5968 0.017 Uiso 1 1 calc R . .
Cl3 Cl 0.71950(15) 1.10932(12) 0.23033(13) 0.0195(4) Uani 1 1 d . . .
C3 C 0.8682(6) -0.1076(5) 0.7829(5) 0.0174(12) Uani 1 1 d . . .
H3A H 0.8630 -0.1860 0.7573 0.021 Uiso 1 1 calc R . .
H3B H 0.9517 -0.0971 0.8306 0.021 Uiso 1 1 calc R . .
Cl4 Cl 0.56053(14) 0.85251(12) 0.09610(12) 0.0156(4) Uani 1 1 d . . .
C4 C 0.7603(6) 0.0380(5) 0.8993(5) 0.0118(11) Uani 1 1 d . . .
H4A H 0.8427 0.0503 0.9481 0.014 Uiso 1 1 calc R . .
H4B H 0.6835 0.0556 0.9505 0.014 Uiso 1 1 calc R . .
Cl5 Cl 0.88745(15) 0.18900(12) 0.53600(13) 0.0193(4) Uani 1 1 d . . .
C5 C 0.7591(6) 0.1131(5) 0.7881(5) 0.0149(12) Uani 1 1 d . . .
H5A H 0.6822 0.1640 0.7907 0.018 Uiso 1 1 calc R . .
H5B H 0.8413 0.1581 0.7878 0.018 Uiso 1 1 calc R . .
C6 C 0.6243(6) -0.0245(5) 0.6764(5) 0.0144(12) Uani 1 1 d . . .
H6A H 0.6179 -0.0716 0.6029 0.017 Uiso 1 1 calc R . .
H6B H 0.5462 0.0253 0.6764 0.017 Uiso 1 1 calc R . .
C7 C 0.6243(6) -0.0972(5) 0.7893(5) 0.0163(12) Uani 1 1 d . . .
H7C H 0.5484 -0.0773 0.8406 0.020 Uiso 1 1 calc R . .
H7A H 0.6151 -0.1759 0.7656 0.020 Uiso 1 1 calc R . .

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
Zn1 0.0126(4) 0.0089(4) 0.0130(4) -0.0003(2) 0.0015(3) 0.0001(2)
Cl1 0.0501(11) 0.0122(7) 0.0118(7) -0.0002(5) 0.0022(6) -0.0019(7)
N1 0.014(2) 0.008(2) 0.011(2) 0.0012(18) 0.0009(18) 0.0001(19)
C1 0.013(3) 0.016(3) 0.014(3) 0.006(2) 0.002(2) 0.000(2)
Cl2 0.0092(7) 0.0188(7) 0.0180(7) 0.0011(5) 0.0013(5) 0.0021(5)
N2 0.015(2) 0.011(2) 0.013(2) 0.0016(18) -0.0009(19) -0.0015(19)
C2 0.007(3) 0.016(3) 0.019(3) 0.001(2) 0.003(2) 0.003(2)
Cl3 0.0270(8) 0.0089(7) 0.0225(7) -0.0011(5) -0.0002(6) -0.0011(6)
C3 0.016(3) 0.015(3) 0.022(3) 0.002(2) 0.004(2) 0.009(2)
Cl4 0.0106(7) 0.0182(7) 0.0181(7) -0.0017(5) 0.0002(5) -0.0003(5)
C4 0.012(3) 0.009(3) 0.014(3) -0.002(2) 0.001(2) 0.000(2)
Cl5 0.0210(8) 0.0180(7) 0.0190(7) 0.0019(5) 0.0062(6) -0.0068(6)
C5 0.019(3) 0.014(3) 0.012(3) -0.004(2) 0.000(2) -0.002(2)
C6 0.010(3) 0.017(3) 0.016(3) 0.002(2) 0.001(2) -0.003(2)
C7 0.014(3) 0.013(3) 0.021(3) 0.004(2) -0.006(2) -0.009(2)

_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
Zn1 Cl3 2.2380(16) . ?
Zn1 Cl1 2.2626(16) . ?
Zn1 Cl4 2.2762(15) . ?
Zn1 Cl2 2.2784(15) . ?
N1 C2 1.503(7) . ?
N1 C6 1.511(7) . ?
N1 C5 1.513(7) . ?
N1 C1 1.517(7) . ?
C1 Cl5 1.755(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
N2 C3 1.484(8) . ?
N2 C4 1.496(7) . ?
N2 C7 1.505(7) . ?
N2 H2 0.91(2) . ?
C2 C3 1.524(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.523(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.522(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7C 0.9900 . ?
C7 H7A 0.9900 . ?

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
Cl3 Zn1 Cl1 107.76(6) . . ?
Cl3 Zn1 Cl4 113.54(6) . . ?
Cl1 Zn1 Cl4 109.38(6) . . ?
Cl3 Zn1 Cl2 113.34(6) . . ?
Cl1 Zn1 Cl2 110.55(6) . . ?
Cl4 Zn1 Cl2 102.18(6) . . ?
C2 N1 C6 109.4(4) . . ?
C2 N1 C5 108.9(4) . . ?
C6 N1 C5 108.8(4) . . ?
C2 N1 C1 112.1(4) . . ?
C6 N1 C1 106.6(4) . . ?
C5 N1 C1 111.0(4) . . ?
N1 C1 Cl5 112.3(4) . . ?
N1 C1 H1A 109.1 . . ?
Cl5 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
Cl5 C1 H1B 109.1 . . ?
H1A C1 H1B 107.9 . . ?
C3 N2 C4 110.2(5) . . ?
C3 N2 C7 110.8(5) . . ?
C4 N2 C7 108.5(4) . . ?
C3 N2 H2 109(5) . . ?
C4 N2 H2 104(4) . . ?
C7 N2 H2 114(4) . . ?
N1 C2 C3 109.5(4) . . ?
N1 C2 H2A 109.8 . . ?
C3 C2 H2A 109.8 . . ?
N1 C2 H2B 109.8 . . ?
C3 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 C2 109.8(5) . . ?
N2 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 . . ?
N2 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N2 C4 C5 109.3(4) . . ?
N2 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
N2 C4 H4B 109.8 . . ?
C5 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
N1 C5 C4 109.6(5) . . ?
N1 C5 H5A 109.7 . . ?
C4 C5 H5A 109.7 . . ?
N1 C5 H5B 109.7 . . ?
C4 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
N1 C6 C7 110.0(4) . . ?
N1 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
N1 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 C6 108.9(5) . . ?
N2 C7 H7C 109.9 . . ?
C6 C7 H7C 109.9 . . ?
N2 C7 H7A 109.9 . . ?
C6 C7 H7A 109.9 . . ?
H7C C7 H7A 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.142
