# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_2
_audit_block_doi                 10.5517/cc13kjz5
_database_code_depnum_ccdc_archive 'CCDC 1029757'
_audit_update_record             
;
2016-02-22 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
#=====================================================================
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            '[ZnCl(N3)(tzmb)]n'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '[ZnCl(N3)(tzmb)]n'
_chemical_formula_sum            'C12 H10 Cl N9 Zn'
_chemical_formula_weight         381.11

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.372(4)
_cell_length_b                   21.350(11)
_cell_length_c                   9.953(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.790(9)
_cell_angle_gamma                90
_cell_volume                     1507.4(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3824
_cell_measurement_theta_min      2.1265
_cell_measurement_theta_max      27.4701

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_F_000             768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.820
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            9020
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.331
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total             2725
_reflns_number_gt                2526
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0481P)²+2.5662P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2725
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.1021
_refine_ls_wR_factor_gt          0.1000
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.08908(5) 0.32355(2) 0.88482(4) 0.03271(15) Uani 1 1 d . . . . .
Cl1 Cl 0.18280(15) 0.42220(4) 0.89803(11) 0.0540(3) Uani 1 1 d . . . . .
N1 N 0.2037(4) 0.27819(11) 1.0679(3) 0.0319(6) Uani 1 1 d . . . . .
N2 N 0.0852(4) 0.24793(12) 1.1266(3) 0.0358(6) Uani 1 1 d . . . . .
N3 N 0.1876(4) 0.22719(12) 1.2479(3) 0.0357(6) Uani 1 1 d . . . . .
N4 N 0.3700(4) 0.24268(13) 1.2717(3) 0.0382(6) Uani 1 1 d . . . . .
N5 N 0.6186(4) 0.35474(12) 1.2311(3) 0.0337(6) Uani 1 1 d . . . . .
N6 N 0.8280(6) 0.61209(17) 1.6942(4) 0.0637(10) Uani 1 1 d . . . . .
N7 N -0.1920(5) 0.31614(16) 0.8255(4) 0.0537(9) Uani 1 1 d . . . . .
N8 N -0.2730(5) 0.35441(19) 0.8414(4) 0.0542(9) Uani 1 1 d . . . . .
N9 N -0.3731(7) 0.3972(2) 0.8599(7) 0.1009(17) Uani 1 1 d . . . . .
C1 C 0.3758(4) 0.27433(13) 1.1581(3) 0.0303(6) Uani 1 1 d . . . . .
C2 C 0.5530(5) 0.30076(16) 1.1361(4) 0.0383(7) Uani 1 1 d . . . . .
H2A H 0.6498 0.2687 1.1539 0.046 Uiso 1 1 calc R U . . .
H2B H 0.5305 0.3143 1.0399 0.046 Uiso 1 1 calc R U . . .
C3 C 0.5724(5) 0.41316(16) 1.1855(4) 0.0459(9) Uani 1 1 d . . . . .
H3A H 0.5088 0.4197 1.0922 0.055 Uiso 1 1 calc R U . . .
C4 C 0.7125(6) 0.34433(17) 1.3650(4) 0.0479(9) Uani 1 1 d . . . . .
H4A H 0.7439 0.3036 1.3961 0.057 Uiso 1 1 calc R U . . .
C5 C 0.7626(6) 0.39388(16) 1.4562(4) 0.0472(9) Uani 1 1 d . . . . .
H5A H 0.8309 0.3863 1.5481 0.057 Uiso 1 1 calc R U . . .
C6 C 0.6170(5) 0.46331(15) 1.2733(4) 0.0437(8) Uani 1 1 d . . . . .
H6A H 0.5829 0.5034 1.2390 0.052 Uiso 1 1 calc R U . . .
C7 C 0.7126(4) 0.45538(14) 1.4131(3) 0.0325(7) Uani 1 1 d . . . . .
C8 C 0.7556(5) 0.50943(15) 1.5101(4) 0.0351(7) Uani 1 1 d . . . . .
C9 C 0.7153(7) 0.57020(17) 1.4631(4) 0.0587(11) Uani 1 1 d . . . . .
H9A H 0.6646 0.5783 1.3685 0.070 Uiso 1 1 calc R U . . .
C10 C 0.8342(6) 0.50195(18) 1.6512(4) 0.0505(9) Uani 1 1 d . . . . .
H10A H 0.8640 0.4621 1.6883 0.061 Uiso 1 1 calc R U . . .
C11 C 0.8692(7) 0.5538(2) 1.7379(5) 0.0614(11) Uani 1 1 d . . . . .
H11A H 0.9249 0.5474 1.8326 0.074 Uiso 1 1 calc R U . . .
C12 C 0.7517(8) 0.61857(19) 1.5586(5) 0.0700(13) Uani 1 1 d . . . . .
H12A H 0.7200 0.6589 1.5248 0.084 Uiso 1 1 calc R U . . .


_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 N7 2.001(4) . ?
Zn1 N3 2.024(3) 4_565 ?
Zn1 N1 2.033(3) . ?
Zn1 Cl1 2.2094(14) . ?
N1 N2 1.342(4) . ?
N1 C1 1.342(4) . ?
N2 N3 1.314(4) . ?
N3 N4 1.342(4) . ?
N3 Zn1 2.024(3) 4_566 ?
N4 C1 1.328(4) . ?
N5 C3 1.339(4) . ?
N5 C4 1.342(5) . ?
N5 C2 1.486(4) . ?
N6 C12 1.321(6) . ?
N6 C11 1.326(6) . ?
N7 N8 1.049(5) . ?
N8 N9 1.219(6) . ?
C1 C2 1.493(4) . ?
C3 C6 1.364(5) . ?
C4 C5 1.378(5) . ?
C5 C7 1.399(5) . ?
C6 C7 1.388(5) . ?
C7 C8 1.483(5) . ?
C8 C10 1.375(5) . ?
C8 C9 1.384(5) . ?
C9 C12 1.379(6) . ?
C10 C11 1.384(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Zn1 N3 106.96(13) . 4_565 ?
N7 Zn1 N1 111.80(14) . . ?
N3 Zn1 N1 102.16(11) 4_565 . ?
N7 Zn1 Cl1 112.02(11) . . ?
N3 Zn1 Cl1 112.75(9) 4_565 . ?
N1 Zn1 Cl1 110.72(8) . . ?
N2 N1 C1 106.7(2) . . ?
N2 N1 Zn1 117.3(2) . . ?
C1 N1 Zn1 135.7(2) . . ?
N3 N2 N1 106.5(3) . . ?
N2 N3 N4 112.1(2) . . ?
N2 N3 Zn1 125.3(2) . 4_566 ?
N4 N3 Zn1 122.6(2) . 4_566 ?
C1 N4 N3 103.8(3) . . ?
C3 N5 C4 120.4(3) . . ?
C3 N5 C2 119.9(3) . . ?
C4 N5 C2 119.6(3) . . ?
C12 N6 C11 115.4(4) . . ?
N8 N7 Zn1 118.7(3) . . ?
N7 N8 N9 177.3(5) . . ?
N4 C1 N1 110.9(3) . . ?
N4 C1 C2 123.3(3) . . ?
N1 C1 C2 125.7(3) . . ?
N5 C2 C1 110.2(3) . . ?
N5 C3 C6 121.3(3) . . ?
N5 C4 C5 120.0(3) . . ?
C4 C5 C7 121.1(3) . . ?
C3 C6 C7 120.9(3) . . ?
C6 C7 C5 116.2(3) . . ?
C6 C7 C8 121.2(3) . . ?
C5 C7 C8 122.6(3) . . ?
C10 C8 C9 116.5(3) . . ?
C10 C8 C7 122.1(3) . . ?
C9 C8 C7 121.4(3) . . ?
C12 C9 C8 119.0(4) . . ?
C8 C10 C11 119.9(4) . . ?
N6 C11 C10 124.0(4) . . ?
N6 C12 C9 125.1(4) . . ?

_refine_diff_density_max         0.370
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.063

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_3
_audit_block_doi                 10.5517/cc13kk07
_database_code_depnum_ccdc_archive 'CCDC 1029758'
_audit_update_record             
;
2016-02-22 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
#===================================================================== 
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            '[Zn2Cl3(OH)(tzmb)]n'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '[Zn2Cl3(OH)(tzmb)]n'
_chemical_formula_sum            'C12 H11 Cl3 N6 O Zn2'
_chemical_formula_weight         492.36

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.026(2)
_cell_length_b                   16.449(4)
_cell_length_c                   12.895(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.776(8)
_cell_angle_gamma                90
_cell_volume                     1660.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7064
_cell_measurement_theta_min      2.0381
_cell_measurement_theta_max      32.5557

_exptl_crystal_description       Prism
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.385
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            10428
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.602
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3077
_reflns_number_gt                2356
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0704P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3077
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.1250
_refine_ls_wR_factor_gt          0.1176
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.39259(7) 0.66969(4) 0.56477(5) 0.0301(2) Uani 1 1 d . . . . .
Zn2 Zn 0.03030(8) 0.59552(4) 0.38813(5) 0.0318(2) Uani 1 1 d . . . . .
Cl1 Cl 0.5348(2) 0.66501(10) 0.73407(11) 0.0480(4) Uani 1 1 d . . . . .
Cl2 Cl 0.02732(19) 0.47703(8) 0.30390(11) 0.0437(4) Uani 1 1 d . . . . .
Cl3 Cl 0.06767(17) 0.70862(8) 0.29763(10) 0.0385(3) Uani 1 1 d . . . . .
O1 O 0.1843(4) 0.6091(2) 0.5265(3) 0.0335(8) Uani 1 1 d . . . . .
H1A H 0.1520 0.5821 0.5824 0.040 Uiso 1 1 calc R U . . .
N1 N 0.5580(5) 0.6424(3) 0.4716(3) 0.0303(10) Uani 1 1 d . . . . .
N2 N 0.5103(6) 0.5945(3) 0.3839(3) 0.0380(11) Uani 1 1 d . . . . .
N3 N 0.6463(6) 0.5757(3) 0.3504(4) 0.0411(11) Uani 1 1 d . . . . .
N4 N 0.7852(5) 0.6104(2) 0.4132(3) 0.0296(10) Uani 1 1 d . . . . .
N5 N 0.8082(5) 0.7890(2) 0.5519(3) 0.0283(9) Uani 1 1 d . . . . .
N6 N 0.6565(5) 1.2078(2) 0.4594(3) 0.0286(9) Uani 1 1 d . . . . .
C1 C 0.7267(6) 0.6517(3) 0.4865(4) 0.0267(11) Uani 1 1 d . . . . .
C2 C 0.8363(7) 0.7010(3) 0.5722(4) 0.0317(11) Uani 1 1 d . . . . .
H2A H 0.8104 0.6873 0.6400 0.038 Uiso 1 1 calc R U . . .
H2B H 0.9555 0.6882 0.5760 0.038 Uiso 1 1 calc R U . . .
C3 C 0.7409(6) 0.8349(3) 0.6190(4) 0.0284(11) Uani 1 1 d . . . . .
H3A H 0.7108 0.8107 0.6774 0.034 Uiso 1 1 calc R U . . .
C4 C 0.8535(7) 0.8242(3) 0.4676(4) 0.0325(12) Uani 1 1 d . . . . .
H4A H 0.9012 0.7926 0.4218 0.039 Uiso 1 1 calc R U . . .
C5 C 0.8303(7) 0.9054(3) 0.4485(4) 0.0345(12) Uani 1 1 d . . . . .
H5A H 0.8628 0.9286 0.3902 0.041 Uiso 1 1 calc R U . . .
C6 C 0.7168(6) 0.9157(3) 0.6024(4) 0.0296(11) Uani 1 1 d . . . . .
H6A H 0.6713 0.9462 0.6502 0.036 Uiso 1 1 calc R U . . .
C7 C 0.7583(6) 0.9540(3) 0.5157(4) 0.0269(11) Uani 1 1 d . . . . .
C8 C 0.7270(6) 1.0419(3) 0.4961(4) 0.0273(11) Uani 1 1 d . . . . .
C9 C 0.6924(7) 1.0924(3) 0.5750(4) 0.0313(11) Uani 1 1 d . . . . .
H9A H 0.6915 1.0714 0.6418 0.038 Uiso 1 1 calc R U . . .
C10 C 0.7208(7) 1.0775(3) 0.3963(4) 0.0367(13) Uani 1 1 d . . . . .
H10A H 0.7399 1.0460 0.3401 0.044 Uiso 1 1 calc R U . . .
C11 C 0.6868(7) 1.1586(3) 0.3821(4) 0.0353(13) Uani 1 1 d . . . . .
H11A H 0.6844 1.1811 0.3156 0.042 Uiso 1 1 calc R U . . .
C12 C 0.6595(7) 1.1733(3) 0.5544(4) 0.0311(12) Uani 1 1 d . . . . .
H12A H 0.6382 1.2060 0.6088 0.037 Uiso 1 1 calc R U . . .


_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 O1 1.915(3) . ?
Zn1 N1 2.028(4) . ?
Zn1 N6 2.065(4) 3_676 ?
Zn1 Cl1 2.2298(16) . ?
Zn2 O1 1.946(3) . ?
Zn2 N4 2.077(4) 1_455 ?
Zn2 Cl2 2.2289(15) . ?
Zn2 Cl3 2.2512(15) . ?
N1 C1 1.333(6) . ?
N1 N2 1.362(6) . ?
N2 N3 1.297(6) . ?
N3 N4 1.351(6) . ?
N4 C1 1.331(6) . ?
N4 Zn2 2.077(4) 1_655 ?
N5 C3 1.348(6) . ?
N5 C4 1.351(6) . ?
N5 C2 1.479(6) . ?
N6 C12 1.345(6) . ?
N6 C11 1.346(6) . ?
N6 Zn1 2.065(4) 3_676 ?
C1 C2 1.492(7) . ?
C3 C6 1.354(7) . ?
C4 C5 1.363(7) . ?
C5 C7 1.395(7) . ?
C6 C7 1.387(7) . ?
C7 C8 1.480(7) . ?
C8 C9 1.388(7) . ?
C8 C10 1.405(7) . ?
C9 C12 1.371(7) . ?
C10 C11 1.366(7) . ?

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
O1 Zn1 N1 112.38(16) . . ?
O1 Zn1 N6 110.05(16) . 3_676 ?
N1 Zn1 N6 104.79(17) . 3_676 ?
O1 Zn1 Cl1 117.55(11) . . ?
N1 Zn1 Cl1 108.18(12) . . ?
N6 Zn1 Cl1 102.76(12) 3_676 . ?
O1 Zn2 N4 105.96(15) . 1_455 ?
O1 Zn2 Cl2 118.90(12) . . ?
N4 Zn2 Cl2 105.69(12) 1_455 . ?
O1 Zn2 Cl3 104.49(11) . . ?
N4 Zn2 Cl3 102.86(12) 1_455 . ?
Cl2 Zn2 Cl3 117.28(6) . . ?
Zn1 O1 Zn2 129.56(18) . . ?
C1 N1 N2 106.0(4) . . ?
C1 N1 Zn1 131.8(3) . . ?
N2 N1 Zn1 121.3(3) . . ?
N3 N2 N1 108.2(4) . . ?
N2 N3 N4 110.0(4) . . ?
C1 N4 N3 105.5(4) . . ?
C1 N4 Zn2 131.8(3) . 1_655 ?
N3 N4 Zn2 122.7(3) . 1_655 ?
C3 N5 C4 119.6(4) . . ?
C3 N5 C2 120.1(4) . . ?
C4 N5 C2 120.3(4) . . ?
C12 N6 C11 116.8(4) . . ?
C12 N6 Zn1 120.9(3) . 3_676 ?
C11 N6 Zn1 122.3(3) . 3_676 ?
N4 C1 N1 110.2(4) . . ?
N4 C1 C2 124.1(4) . . ?
N1 C1 C2 125.7(4) . . ?
N5 C2 C1 111.1(4) . . ?
N5 C3 C6 120.8(5) . . ?
N5 C4 C5 121.0(5) . . ?
C4 C5 C7 120.5(5) . . ?
C3 C6 C7 121.4(5) . . ?
C6 C7 C5 116.6(5) . . ?
C6 C7 C8 121.3(4) . . ?
C5 C7 C8 122.1(5) . . ?
C9 C8 C10 116.7(5) . . ?
C9 C8 C7 120.9(4) . . ?
C10 C8 C7 122.3(4) . . ?
C12 C9 C8 120.0(5) . . ?
C11 C10 C8 119.7(5) . . ?
N6 C11 C10 123.4(5) . . ?
N6 C12 C9 123.3(5) . . ?

_refine_diff_density_max         1.143
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.136

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_4
_audit_block_doi                 10.5517/cc13kk18
_database_code_depnum_ccdc_archive 'CCDC 1029759'
_audit_update_record             
;
2016-02-22 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
#===================================================================== 
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            '[Cd2(N3)2(C2O4)(tzmb)2]n'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '[Cd2(N3)2(C2O4)(tzmb)2]n'
_chemical_formula_sum            'C26 H20 Cd2 N18 O4'
_chemical_formula_weight         873.40

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.9251(7)
_cell_length_b                   9.9975(8)
_cell_length_c                   16.7168(13)
_cell_angle_alpha                90
_cell_angle_beta                 90.338(6)
_cell_angle_gamma                90
_cell_volume                     1491.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4085
_cell_measurement_theta_min      2.0371
_cell_measurement_theta_max      27.4971

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_F_000             860
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.496
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_T_max  0.688
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            10829
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.060
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.957
_reflns_number_total             3303
_reflns_number_gt                3047
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0308P)²+0.7561P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3303
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0682
_refine_ls_wR_factor_gt          0.0647
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.67395(2) 0.46772(2) 0.14918(2) 0.02106(8) Uani 1 1 d . . . . .
O1 O 0.65885(18) 0.58961(17) 0.03212(10) 0.0259(4) Uani 1 1 d . . . . .
O2 O 0.5078(2) 0.62837(16) -0.07086(11) 0.0297(4) Uani 1 1 d . . . . .
N1 N 0.6216(2) 0.29337(19) 0.24146(12) 0.0230(4) Uani 1 1 d . . . . .
N2 N 0.6548(2) 0.3071(2) 0.32069(13) 0.0280(5) Uani 1 1 d . . . . .
N3 N 0.5934(2) 0.2091(2) 0.36058(13) 0.0297(5) Uani 1 1 d . . . . .
N4 N 0.5177(2) 0.1285(2) 0.30906(13) 0.0262(4) Uani 1 1 d . . . . .
N5 N 0.5965(2) 0.04664(18) 0.11867(12) 0.0198(4) Uani 1 1 d . . . . .
N6 N 1.1369(2) -0.3387(2) -0.08322(13) 0.0275(5) Uani 1 1 d . . . . .
N7 N 0.8472(3) 0.5801(2) 0.22425(14) 0.0315(5) Uani 1 1 d . . . . .
N8 N 0.9677(4) 0.5504(3) 0.22233(19) 0.0510(8) Uani 1 1 d . . . . .
N9 N 1.0977(4) 0.5266(5) 0.2201(3) 0.0947(15) Uani 1 1 d . . . . .
C1 C 0.5378(3) 0.1820(2) 0.23719(15) 0.0211(5) Uani 1 1 d . . . . .
C2 C 0.4768(3) 0.1221(2) 0.16263(15) 0.0212(5) Uani 1 1 d . . . . .
H2A H 0.4371 0.1923 0.1285 0.025 Uiso 1 1 calc R U . . .
H2B H 0.3954 0.0618 0.1757 0.025 Uiso 1 1 calc R U . . .
C3 C 0.6336(3) 0.0807(2) 0.04352(15) 0.0234(5) Uani 1 1 d . . . . .
H3A H 0.5887 0.1545 0.0195 0.028 Uiso 1 1 calc R U . . .
C4 C 0.6631(3) -0.0583(3) 0.15490(15) 0.0256(5) Uani 1 1 d . . . . .
H4A H 0.6385 -0.0787 0.2075 0.031 Uiso 1 1 calc R U . . .
C5 C 0.7655(3) -0.1347(2) 0.11618(16) 0.0276(5) Uani 1 1 d . . . . .
H5A H 0.8091 -0.2073 0.1422 0.033 Uiso 1 1 calc R U . . .
C6 C 0.7376(3) 0.0071(2) 0.00189(15) 0.0239(5) Uani 1 1 d . . . . .
H6A H 0.7628 0.0316 -0.0500 0.029 Uiso 1 1 calc R U . . .
C7 C 0.8059(3) -0.1049(2) 0.03751(15) 0.0222(5) Uani 1 1 d . . . . .
C8 C 0.9188(3) -0.1860(2) -0.00487(16) 0.0243(5) Uani 1 1 d . . . . .
C9 C 0.9357(3) -0.1813(3) -0.08720(16) 0.0331(6) Uani 1 1 d . . . . .
H9A H 0.8736 -0.1270 -0.1180 0.040 Uiso 1 1 calc R U . . .
C10 C 1.0140(3) -0.2717(3) 0.03776(17) 0.0319(6) Uani 1 1 d . . . . .
H10A H 1.0064 -0.2791 0.0930 0.038 Uiso 1 1 calc R U . . .
C11 C 1.1200(3) -0.3455(3) -0.00365(17) 0.0341(6) Uani 1 1 d . . . . .
H11A H 1.1824 -0.4026 0.0252 0.041 Uiso 1 1 calc R U . . .
C12 C 1.0449(3) -0.2576(3) -0.12314(17) 0.0352(6) Uani 1 1 d . . . . .
H12A H 1.0548 -0.2521 -0.1784 0.042 Uiso 1 1 calc R U . . .
C13 C 0.5490(3) 0.5629(2) -0.01091(15) 0.0204(5) Uani 1 1 d . . . . .


_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
Cd1 N7 2.282(2) . ?
Cd1 O2 2.2896(18) 3_665 ?
Cd1 O1 2.3086(17) . ?
Cd1 N1 2.376(2) . ?
Cd1 N6 2.399(2) 3_755 ?
Cd1 N4 2.452(2) 2_655 ?
O1 C13 1.242(3) . ?
O2 C13 1.250(3) . ?
O2 Cd1 2.2896(18) 3_665 ?
N1 C1 1.343(3) . ?
N1 N2 1.363(3) . ?
N2 N3 1.307(3) . ?
N3 N4 1.357(3) . ?
N4 C1 1.328(3) . ?
N4 Cd1 2.452(2) 2_645 ?
N5 C3 1.345(3) . ?
N5 C4 1.348(3) . ?
N5 C2 1.504(3) . ?
N6 C12 1.331(3) . ?
N6 C11 1.341(4) . ?
N6 Cd1 2.399(2) 3_755 ?
N7 N8 1.116(4) . ?
N8 N9 1.185(5) . ?
C1 C2 1.483(3) . ?
C3 C6 1.376(3) . ?
C4 C5 1.359(3) . ?
C5 C7 1.398(4) . ?
C6 C7 1.406(3) . ?
C7 C8 1.477(3) . ?
C8 C9 1.386(4) . ?
C8 C10 1.399(4) . ?
C9 C12 1.378(4) . ?
C10 C11 1.388(4) . ?
C13 C13 1.576(4) 3_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Cd1 O2 175.31(7) . 3_665 ?
N7 Cd1 O1 104.02(7) . . ?
O2 Cd1 O1 72.49(6) 3_665 . ?
N7 Cd1 N1 98.02(8) . . ?
O2 Cd1 N1 85.53(6) 3_665 . ?
O1 Cd1 N1 157.95(6) . . ?
N7 Cd1 N6 92.35(8) . 3_755 ?
O2 Cd1 N6 90.54(7) 3_665 3_755 ?
O1 Cd1 N6 86.10(7) . 3_755 ?
N1 Cd1 N6 92.61(7) . 3_755 ?
N7 Cd1 N4 89.56(8) . 2_655 ?
O2 Cd1 N4 86.84(7) 3_665 2_655 ?
O1 Cd1 N4 81.83(7) . 2_655 ?
N1 Cd1 N4 98.97(7) . 2_655 ?
N6 Cd1 N4 167.88(7) 3_755 2_655 ?
C13 O1 Cd1 114.82(15) . . ?
C13 O2 Cd1 116.29(14) . 3_665 ?
C1 N1 N2 104.7(2) . . ?
C1 N1 Cd1 133.26(17) . . ?
N2 N1 Cd1 120.98(14) . . ?
N3 N2 N1 109.3(2) . . ?
N2 N3 N4 109.3(2) . . ?
C1 N4 N3 105.42(19) . . ?
C1 N4 Cd1 128.27(16) . 2_645 ?
N3 N4 Cd1 123.66(16) . 2_645 ?
C3 N5 C4 120.4(2) . . ?
C3 N5 C2 120.61(19) . . ?
C4 N5 C2 118.9(2) . . ?
C12 N6 C11 117.1(2) . . ?
C12 N6 Cd1 122.09(18) . 3_755 ?
C11 N6 Cd1 120.80(16) . 3_755 ?
N8 N7 Cd1 120.2(2) . . ?
N7 N8 N9 176.1(4) . . ?
N4 C1 N1 111.3(2) . . ?
N4 C1 C2 123.1(2) . . ?
N1 C1 C2 125.5(2) . . ?
C1 C2 N5 110.79(19) . . ?
N5 C3 C6 120.5(2) . . ?
N5 C4 C5 121.3(2) . . ?
C4 C5 C7 120.4(2) . . ?
C3 C6 C7 120.2(2) . . ?
C5 C7 C6 117.1(2) . . ?
C5 C7 C8 121.0(2) . . ?
C6 C7 C8 122.0(2) . . ?
C9 C8 C10 117.2(2) . . ?
C9 C8 C7 122.4(2) . . ?
C10 C8 C7 120.4(2) . . ?
C12 C9 C8 119.7(2) . . ?
C11 C10 C8 119.0(2) . . ?
N6 C11 C10 123.3(2) . . ?
N6 C12 C9 123.7(3) . . ?
O1 C13 O2 125.4(2) . . ?
O1 C13 C13 118.3(3) . 3_665 ?
O2 C13 C13 116.2(2) . 3_665 ?

_refine_diff_density_max         0.465
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.074

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1451442'
_audit_update_record             
;
2016-02-22 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
#===================================================================== 
_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            '[ZnCl(N3)(tzmb)]2??H2O'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '[ZnCl(N3)(tzmb)]2??H2O'
_chemical_formula_sum            'C24 H22 Cl2 N18 O Zn2'
_chemical_formula_weight         780.23

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P n'
_space_group_name_Hall           'P -2yac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.467(3)
_cell_length_b                   13.587(4)
_cell_length_c                   11.900(4)
_cell_angle_alpha                90
_cell_angle_beta                 112.036(7)
_cell_angle_gamma                90
_cell_volume                     1568.8(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4359
_cell_measurement_theta_min      2.2128
_cell_measurement_theta_max      27.4778

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_F_000             788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.753
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5644
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            11438
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.579
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_point_group_measured_fraction_full 0.906
_reflns_number_total             5303
_reflns_number_gt                4351
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_max     0.814
_reflns_Friedel_fraction_full    0.814

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0660P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1494 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.121(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5303
_refine_ls_number_parameters     424
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1344
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.004

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.6192(3) 0.10379(7) 0.6724(3) 0.0465(3) Uani 1 1 d . . . . .
Cl1 Cl 0.7757(6) 0.1299(5) 0.8659(7) 0.160(2) Uani 1 1 d . . . . .
N26 N 0.7009(8) 0.0079(6) 0.5849(8) 0.0471(19) Uani 1 1 d . . . . .
N11 N 0.4547(7) 0.0337(5) 0.6846(8) 0.0411(17) Uani 1 1 d . . . . .
N18 N 0.5988(8) 0.2730(7) 0.5403(8) 0.0506(19) Uani 1 1 d . . . . .
C28 C 0.8204(9) -0.1251(7) 0.4766(9) 0.043(2) Uani 1 1 d . . . . .
C29 C 0.6756(10) -0.1238(7) 0.4414(10) 0.052(3) Uani 1 1 d . . . . .
H15A H 0.6188 -0.1668 0.3832 0.062 Uiso 1 1 calc R U . . .
C212 C 0.6232(9) -0.0554(8) 0.4978(10) 0.057(3) Uani 1 1 d . . . . .
H16A H 0.5280 -0.0522 0.4747 0.069 Uiso 1 1 calc R U . . .
C11 C 0.4402(9) -0.0301(7) 0.7640(9) 0.043(2) Uani 1 1 d . . . . .
C210 C 0.8984(10) -0.0585(8) 0.5625(11) 0.056(3) Uani 1 1 d . . . . .
H19A H 0.9937 -0.0571 0.5853 0.067 Uiso 1 1 calc R U . . .
N17 N 0.5511(9) 0.2256(6) 0.5838(9) 0.061(3) Uani 1 1 d . . . . .
C12 C 0.5525(9) -0.0809(7) 0.8613(9) 0.046(2) Uani 1 1 d . . . . .
H23A H 0.5169 -0.1102 0.9180 0.056 Uiso 1 1 calc R U . . .
H23B H 0.6234 -0.0339 0.9051 0.056 Uiso 1 1 calc R U . . .
C14 C 0.5316(10) -0.2257(8) 0.7374(11) 0.061(3) Uani 1 1 d . . . . .
H25A H 0.4387 -0.2267 0.7257 0.074 Uiso 1 1 calc R U . . .
N12 N 0.3261(7) 0.0576(6) 0.6089(8) 0.051(2) Uani 1 1 d . . . . .
N15 N 0.6131(8) -0.1594(5) 0.8081(7) 0.0441(17) Uani 1 1 d . . . . .
C211 C 0.8349(10) 0.0057(8) 0.6140(11) 0.062(3) Uani 1 1 d . . . . .
H36A H 0.8893 0.0496 0.6723 0.075 Uiso 1 1 calc R U . . .
C16 C 0.8020(9) -0.2287(7) 0.7797(9) 0.055(2) Uani 1 1 d . . . . .
H37A H 0.8967 -0.2308 0.7989 0.066 Uiso 1 1 calc R U . . .
N13 N 0.2389(8) 0.0105(6) 0.6448(9) 0.061(2) Uani 1 1 d . . . . .
C13 C 0.7483(10) -0.1593(8) 0.8327(9) 0.056(2) Uani 1 1 d . . . . .
H40A H 0.8052 -0.1128 0.8851 0.067 Uiso 1 1 calc R U . . .
N19 N 0.6465(11) 0.3334(8) 0.4878(11) 0.091(3) Uani 1 1 d . . . . .
Zn2 Zn 0.9456(3) -0.59760(8) 0.4149(3) 0.0539(4) Uani 1 1 d . . . . .
N16 N 0.8747(8) -0.4963(6) 0.5043(8) 0.0450(19) Uani 1 1 d . . . . .
N21 N 1.1309(8) -0.5490(6) 0.4202(8) 0.053(2) Uani 1 1 d . . . . .
C18 C 0.7743(9) -0.3690(7) 0.6341(9) 0.046(2) Uani 1 1 d . . . . .
N27 N 0.9759(14) -0.7301(8) 0.5034(9) 0.076(3) Uani 1 1 d D . . . .
N22 N 1.2444(10) -0.5962(6) 0.4939(9) 0.065(3) Uani 1 1 d . . . . .
C25 C 0.8221(10) -0.2329(7) 0.3049(9) 0.052(2) Uani 1 1 d . . . . .
H26A H 0.7356 -0.2089 0.2567 0.063 Uiso 1 1 calc R U . . .
C19 C 0.6950(11) -0.3946(7) 0.5161(11) 0.059(3) Uani 1 1 d . . . . .
H28A H 0.6068 -0.3691 0.4780 0.071 Uiso 1 1 calc R U . . .
C26 C 1.0164(9) -0.2375(6) 0.4937(9) 0.047(2) Uani 1 1 d . . . . .
H31A H 1.0611 -0.2167 0.5733 0.056 Uiso 1 1 calc R U . . .
C22 C 1.0833(13) -0.4075(8) 0.2773(10) 0.066(3) Uani 1 1 d . . . . .
H32A H 1.0141 -0.4441 0.2130 0.079 Uiso 1 1 calc R U . . .
H32B H 1.1384 -0.3712 0.2415 0.079 Uiso 1 1 calc R U . . .
N25 N 1.0128(8) -0.3361(6) 0.3312(7) 0.0501(19) Uani 1 1 d . . . . .
C21 C 1.1722(10) -0.4769(7) 0.3669(9) 0.053(2) Uani 1 1 d . . . . .
C23 C 1.0760(9) -0.3038(7) 0.4456(9) 0.053(2) Uani 1 1 d . . . . .
H35A H 1.1629 -0.3280 0.4924 0.063 Uiso 1 1 calc R U . . .
N28 N 0.9677(11) -0.7420(9) 0.5960(7) 0.138(8) Uani 1 1 d D . . . .
C112 C 0.7484(11) -0.4580(8) 0.4565(10) 0.065(3) Uani 1 1 d . . . . .
H42A H 0.6933 -0.4756 0.3776 0.078 Uiso 1 1 calc R U . . .
C24 C 0.8874(11) -0.3005(7) 0.2615(9) 0.057(3) Uani 1 1 d . . . . .
H43A H 0.8451 -0.3227 0.1822 0.068 Uiso 1 1 calc R U . . .
C110 C 0.9052(11) -0.4072(7) 0.6866(11) 0.057(3) Uani 1 1 d . . . . .
H47A H 0.9616 -0.3907 0.7656 0.069 Uiso 1 1 calc R U . . .
N24 N 1.3098(9) -0.4774(8) 0.4049(10) 0.071(3) Uani 1 1 d . . . . .
C111 C 0.9504(10) -0.4708(7) 0.6186(10) 0.055(3) Uani 1 1 d . . . . .
H53A H 1.0383 -0.4974 0.6544 0.066 Uiso 1 1 calc R U . . .
C17 C 0.7177(9) -0.2958(6) 0.6980(9) 0.044(2) Uani 1 1 d . . . . .
C27 C 0.8890(10) -0.2004(7) 0.4247(9) 0.046(2) Uani 1 1 d . . . . .
C15 C 0.5837(9) -0.2943(7) 0.6800(10) 0.054(3) Uani 1 1 d . . . . .
H18A H 0.5246 -0.3401 0.6280 0.065 Uiso 1 1 calc R U . . .
O1W O 0.6265(8) 0.1738(7) 0.3024(9) 0.091(3) Uani 1 1 d . . . . .
N14 N 0.3087(8) -0.0451(6) 0.7417(9) 0.057(2) Uani 1 1 d . . . . .
N23 N 1.3504(10) -0.5507(10) 0.4834(10) 0.088(3) Uani 1 1 d . . . . .
Cl2 Cl 0.7972(4) -0.5932(3) 0.2225(4) 0.0791(10) Uani 1 1 d . . . . .
N29 N 0.970(3) -0.7566(19) 0.6920(12) 0.309(15) Uani 1 1 d D U . . .


_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 N17 1.948(9) . ?
Zn1 N11 2.020(7) . ?
Zn1 N26 2.045(9) . ?
Zn1 Cl1 2.297(7) . ?
N26 C211 1.313(12) . ?
N26 C212 1.357(13) . ?
N11 C11 1.331(12) . ?
N11 N12 1.349(9) . ?
N18 N17 1.062(11) . ?
N18 N19 1.244(13) . ?
C28 C210 1.380(13) . ?
C28 C29 1.413(13) . ?
C28 C27 1.508(13) . ?
C29 C212 1.376(15) . ?
C11 N14 1.316(11) . ?
C11 C12 1.476(12) . ?
C210 C211 1.373(14) . ?
C12 N15 1.497(11) . ?
C14 N15 1.307(12) . ?
C14 C15 1.382(14) . ?
N12 N13 1.310(12) . ?
N15 C13 1.333(11) . ?
C16 C13 1.366(13) . ?
C16 C17 1.383(13) . ?
N13 N14 1.342(11) . ?
Zn2 N27 2.049(12) . ?
Zn2 N21 2.027(8) . ?
Zn2 N16 2.042(8) . ?
Zn2 Cl2 2.234(3) . ?
N16 C111 1.337(13) . ?
N16 C112 1.334(12) . ?
N21 C21 1.325(13) . ?
N21 N22 1.345(10) . ?
C18 C19 1.381(14) . ?
C18 C110 1.377(14) . ?
C18 C17 1.503(13) . ?
N27 N28 1.1491(15) . ?
N22 N23 1.317(15) . ?
C25 C24 1.357(14) . ?
C25 C27 1.404(13) . ?
C19 C112 1.361(14) . ?
C26 C23 1.340(13) . ?
C26 C27 1.373(12) . ?
C22 C21 1.465(13) . ?
C22 N25 1.500(12) . ?
N25 C23 1.345(11) . ?
N25 C24 1.352(12) . ?
C21 N24 1.338(12) . ?
N28 N29 1.1503(15) . ?
C110 C111 1.383(15) . ?
N24 N23 1.322(15) . ?
C17 C15 1.337(12) . ?

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
N17 Zn1 N11 106.9(3) . . ?
N17 Zn1 N26 113.8(4) . . ?
N11 Zn1 N26 105.5(3) . . ?
N17 Zn1 Cl1 113.0(3) . . ?
N11 Zn1 Cl1 107.9(3) . . ?
N26 Zn1 Cl1 109.4(3) . . ?
C211 N26 C212 117.5(9) . . ?
C211 N26 Zn1 119.3(7) . . ?
C212 N26 Zn1 123.2(7) . . ?
C11 N11 N12 106.2(7) . . ?
C11 N11 Zn1 133.2(6) . . ?
N12 N11 Zn1 120.2(6) . . ?
N17 N18 N19 175.2(11) . . ?
C210 C28 C29 118.8(9) . . ?
C210 C28 C27 120.5(8) . . ?
C29 C28 C27 120.7(8) . . ?
C212 C29 C28 116.4(9) . . ?
N26 C212 C29 124.5(9) . . ?
N14 C11 N11 110.3(8) . . ?
N14 C11 C12 123.4(9) . . ?
N11 C11 C12 126.3(8) . . ?
C211 C210 C28 119.7(8) . . ?
N18 N17 Zn1 129.5(8) . . ?
C11 C12 N15 109.9(7) . . ?
N15 C14 C15 120.0(9) . . ?
N13 N12 N11 107.9(8) . . ?
C14 N15 C13 121.6(9) . . ?
C14 N15 C12 119.1(8) . . ?
C13 N15 C12 119.4(8) . . ?
N26 C211 C210 123.1(10) . . ?
C13 C16 C17 120.9(8) . . ?
N12 N13 N14 109.5(7) . . ?
N15 C13 C16 119.0(9) . . ?
N27 Zn2 N21 108.0(4) . . ?
N27 Zn2 N16 109.9(4) . . ?
N21 Zn2 N16 107.2(3) . . ?
N27 Zn2 Cl2 117.6(4) . . ?
N21 Zn2 Cl2 108.2(3) . . ?
N16 Zn2 Cl2 105.5(2) . . ?
C111 N16 C112 116.6(8) . . ?
C111 N16 Zn2 120.8(6) . . ?
C112 N16 Zn2 122.4(7) . . ?
C21 N21 N22 107.3(8) . . ?
C21 N21 Zn2 134.9(6) . . ?
N22 N21 Zn2 117.7(7) . . ?
C19 C18 C110 118.8(10) . . ?
C19 C18 C17 118.8(9) . . ?
C110 C18 C17 122.3(9) . . ?
N28 N27 Zn2 124.3(10) . . ?
N23 N22 N21 106.5(9) . . ?
C24 C25 C27 118.0(9) . . ?
C112 C19 C18 118.8(9) . . ?
C23 C26 C27 119.7(9) . . ?
C21 C22 N25 112.6(9) . . ?
C23 N25 C24 119.9(8) . . ?
C23 N25 C22 120.7(8) . . ?
C24 N25 C22 119.3(8) . . ?
N21 C21 N24 109.7(9) . . ?
N21 C21 C22 126.3(9) . . ?
N24 C21 C22 124.0(11) . . ?
C26 C23 N25 121.4(8) . . ?
N27 N28 N29 175(2) . . ?
N16 C112 C19 124.0(10) . . ?
N25 C24 C25 121.4(9) . . ?
C18 C110 C111 118.1(10) . . ?
N23 N24 C21 105.3(10) . . ?
N16 C111 C110 123.7(9) . . ?
C15 C17 C16 117.2(9) . . ?
C15 C17 C18 121.2(9) . . ?
C16 C17 C18 121.6(8) . . ?
C26 C27 C25 119.6(9) . . ?
C26 C27 C28 120.6(9) . . ?
C25 C27 C28 119.8(9) . . ?
C17 C15 C14 121.0(9) . . ?
C11 N14 N13 106.1(8) . . ?
N22 N23 N24 111.2(9) . . ?

_refine_diff_density_max         0.808
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.079

_shelxl_version_number           2014/6

