# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_CdCl4-1
_database_code_depnum_ccdc_archive 'CCDC 1406455'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H36 Cd Cl5 N3'
_chemical_formula_weight         728.28

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'
Cd Cd -0.8075 1.2024 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   P213

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

_cell_length_a                   14.759(2)
_cell_length_b                   14.759(2)
_cell_length_c                   14.759(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3214.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20151
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         27.43
_reflns_number_total             2466
_reflns_number_gt                2399
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0300P)²+0.4901P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.03(2)
_refine_ls_number_reflns         2466
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0513
_refine_ls_wR_factor_gt          0.0507
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
N5 N 0.23147(11) -0.71654(10) -0.03219(10) 0.0308(3) Uani 1 1 d . . .
H5A H 0.1765 -0.7408 -0.0199 0.037 Uiso 1 1 d R . .
H5B H 0.2642 -0.7607 -0.0526 0.037 Uiso 1 1 d R . .
C1 C 0.16743(12) -0.71011(12) 0.17918(12) 0.0277(3) Uani 1 1 d . . .
C2 C 0.24514(12) -0.74311(11) 0.13558(12) 0.0268(3) Uani 1 1 d . . .
C3 C 0.11822(14) -0.62708(13) 0.14356(14) 0.0369(4) Uani 1 1 d . . .
H3A H 0.0540 -0.6361 0.1487 0.055 Uiso 1 1 calc R . .
H3B H 0.1339 -0.6177 0.0811 0.055 Uiso 1 1 calc R . .
H3C H 0.1357 -0.5750 0.1783 0.055 Uiso 1 1 calc R . .
C4 C 0.28124(12) -0.69234(12) 0.05427(13) 0.0313(3) Uani 1 1 d . . .
H4A H 0.3451 -0.7061 0.0469 0.038 Uiso 1 1 calc R . .
H4B H 0.2756 -0.6277 0.0650 0.038 Uiso 1 1 calc R . .
C6 C 0.21734(14) -0.64107(14) -0.09607(13) 0.0354(4) Uani 1 1 d . . .
C7 C 0.27829(18) -0.57122(17) -0.10166(16) 0.0515(6) Uani 1 1 d . . .
H7A H 0.3296 -0.5708 -0.0651 0.062 Uiso 1 1 calc R . .
C8 C 0.2629(2) -0.50163(18) -0.16191(19) 0.0590(6) Uani 1 1 d . . .
H8A H 0.3036 -0.4537 -0.1658 0.071 Uiso 1 1 calc R . .
C9 C 0.1875(2) -0.5031(2) -0.2162(2) 0.0777(10) Uani 1 1 d . . .
H9A H 0.1764 -0.4554 -0.2559 0.093 Uiso 1 1 calc R . .
C10 C 0.1287(2) -0.5743(3) -0.2121(3) 0.1112(17) Uani 1 1 d . . .
H10A H 0.0784 -0.5756 -0.2500 0.133 Uiso 1 1 calc R . .
C11 C 0.1435(2) -0.6450(2) -0.1518(2) 0.0817(11) Uani 1 1 d . . .
H11A H 0.1040 -0.6940 -0.1494 0.098 Uiso 1 1 calc R . .
Cd1 Cd 0.047118(8) -0.952882(8) 0.047118(8) 0.03294(7) Uani 1 3 d S . .
Cl1 Cl -0.04777(3) -1.04777(3) -0.04777(3) 0.0635(3) Uani 1 3 d S . .
Cl2 Cl 0.02801(3) -0.79312(3) 0.00733(4) 0.04471(13) Uani 1 1 d . . .
Cl3 Cl -0.15556(4) -0.65556(4) -0.84444(4) 0.04101(19) Uani 1 3 d S . .


_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
N5 C6 1.474(2) . ?
N5 C4 1.515(2) . ?
N5 H5A 0.9054 . ?
N5 H5B 0.8657 . ?
C1 C2 1.402(2) . ?
C1 C2 1.405(2) 5_546 ?
C1 C3 1.518(2) . ?
C2 C1 1.405(2) 9_645 ?
C2 C4 1.512(2) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C11 1.366(3) . ?
C6 C7 1.371(3) . ?
C7 C8 1.377(3) . ?
C7 H7A 0.9300 . ?
C8 C9 1.372(5) . ?
C8 H8A 0.9300 . ?
C9 C10 1.364(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.388(4) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
Cd1 Cl1 2.4256(10) . ?
Cd1 Cl2 2.4462(6) 9_645 ?
Cd1 Cl2 2.4462(6) 5_546 ?
Cd1 Cl2 2.4462(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
C6 N5 C4 115.42(14) . . ?
C6 N5 H5A 107.5 . . ?
C4 N5 H5A 111.1 . . ?
C6 N5 H5B 115.2 . . ?
C4 N5 H5B 101.6 . . ?
H5A N5 H5B 105.7 . . ?
C2 C1 C2 119.02(18) . 5_546 ?
C2 C1 C3 120.84(17) . . ?
C2 C1 C3 120.14(16) 5_546 . ?
C1 C2 C1 120.97(18) . 9_645 ?
C1 C2 C4 118.71(16) . . ?
C1 C2 C4 120.31(16) 9_645 . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 N5 112.39(13) . . ?
C2 C4 H4A 109.1 . . ?
N5 C4 H4A 109.1 . . ?
C2 C4 H4B 109.1 . . ?
N5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
C11 C6 C7 121.2(2) . . ?
C11 C6 N5 117.8(2) . . ?
C7 C6 N5 120.93(18) . . ?
C6 C7 C8 119.4(2) . . ?
C6 C7 H7A 120.3 . . ?
C8 C7 H7A 120.3 . . ?
C9 C8 C7 120.0(3) . . ?
C9 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C10 C9 C8 120.1(3) . . ?
C10 C9 H9A 119.9 . . ?
C8 C9 H9A 119.9 . . ?
C9 C10 C11 120.5(3) . . ?
C9 C10 H10A 119.8 . . ?
C11 C10 H10A 119.8 . . ?
C6 C11 C10 118.7(3) . . ?
C6 C11 H11A 120.7 . . ?
C10 C11 H11A 120.7 . . ?
Cl1 Cd1 Cl2 110.571(13) . 9_645 ?
Cl1 Cd1 Cl2 110.571(13) . 5_546 ?
Cl2 Cd1 Cl2 108.350(14) 9_645 5_546 ?
Cl1 Cd1 Cl2 110.571(13) . . ?
Cl2 Cd1 Cl2 108.350(14) 9_645 . ?
Cl2 Cd1 Cl2 108.350(14) 5_546 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C1 1.3(3) 5_546 . . 9_645 ?
C3 C1 C2 C1 -178.87(13) . . . 9_645 ?
C2 C1 C2 C4 -177.51(11) 5_546 . . . ?
C3 C1 C2 C4 2.3(2) . . . . ?
C1 C2 C4 N5 -82.12(19) . . . . ?
C1 C2 C4 N5 99.01(19) 9_645 . . . ?
C6 N5 C4 C2 143.22(16) . . . . ?
C4 N5 C6 C11 -151.7(2) . . . . ?
C4 N5 C6 C7 30.8(3) . . . . ?
C11 C6 C7 C8 2.8(4) . . . . ?
N5 C6 C7 C8 -179.8(2) . . . . ?
C6 C7 C8 C9 -0.6(5) . . . . ?
C7 C8 C9 C10 -1.5(6) . . . . ?
C8 C9 C10 C11 1.4(7) . . . . ?
C7 C6 C11 C10 -2.9(5) . . . . ?
N5 C6 C11 C10 179.6(3) . . . . ?
C9 C10 C11 C6 0.8(7) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.047
####################################################################### 
# 
# 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 1406456'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H36 Cl5 N3 Zn'
_chemical_formula_weight         681.26

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   P213

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

_cell_length_a                   14.6693(4)
_cell_length_b                   14.6693(4)
_cell_length_c                   14.6693(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3156.66(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.18
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19823
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         27.53
_reflns_number_total             2430
_reflns_number_gt                2303
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0314P)²+0.8863P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.985(12)
_refine_ls_number_reflns         2430
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0255
_refine_ls_wR_factor_ref         0.0644
_refine_ls_wR_factor_gt          0.0631
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.002
_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
N5 N -0.28322(12) -0.96692(12) -0.22994(12) 0.0341(4) Uani 1 1 d . . .
H5A H -0.2541 -0.9790 -0.1720 0.041 Uiso 1 1 d R . .
H5B H -0.2381 -0.9370 -0.2570 0.041 Uiso 1 1 d R . .
C1 C -0.25799(13) -1.13556(13) -0.24523(13) 0.0287(4) Uani 1 1 d . . .
C2 C -0.17988(13) -1.16711(14) -0.29074(13) 0.0301(4) Uani 1 1 d . . .
C3 C -0.14320(16) -1.11627(16) -0.37293(15) 0.0394(5) Uani 1 1 d . . .
H3A H -0.0797 -1.1300 -0.3805 0.059 Uiso 1 1 calc R . .
H3B H -0.1507 -1.0519 -0.3639 0.059 Uiso 1 1 calc R . .
H3C H -0.1760 -1.1347 -0.4264 0.059 Uiso 1 1 calc R . .
C4 C -0.30873(14) -1.05358(14) -0.28065(13) 0.0342(4) Uani 1 1 d . . .
H4A H -0.3737 -1.0640 -0.2745 0.041 Uiso 1 1 calc R . .
H4B H -0.2953 -1.0459 -0.3449 0.041 Uiso 1 1 calc R . .
C6 C -0.35908(16) -0.90274(15) -0.21527(16) 0.0395(5) Uani 1 1 d . . .
C7 C -0.4272(2) -0.89366(18) -0.27802(19) 0.0560(7) Uani 1 1 d . . .
H7 H -0.4259 -0.9278 -0.3314 0.067 Uiso 1 1 calc R . .
C8 C -0.0027(2) -1.1658(2) 0.2378(2) 0.0663(8) Uani 1 1 d . . .
H8 H 0.0444 -1.1713 0.1958 0.080 Uiso 1 1 calc R . .
C9 C -0.0022(3) -1.2172(3) 0.3159(3) 0.0882(12) Uani 1 1 d . . .
H9A H 0.0465 -1.2561 0.3276 0.106 Uiso 1 1 calc R . .
C10 C -0.0728(4) -1.2116(3) 0.3768(3) 0.123(2) Uani 1 1 d . . .
H10 H -0.0735 -1.2487 0.4282 0.147 Uiso 1 1 calc R . .
C11 C -0.3567(3) -0.8497(3) -0.1385(2) 0.0894(13) Uani 1 1 d . . .
H11 H -0.3087 -0.8546 -0.0973 0.107 Uiso 1 1 calc R . .
Zn1 Zn -0.047384(15) -1.047384(15) -0.047384(15) 0.03160(10) Uani 1 3 d S . .
Cl1 Cl -0.02803(4) -1.19664(4) -0.01116(4) 0.04438(14) Uani 1 1 d . . .
Cl2 Cl 0.04113(4) -0.95887(4) 0.04113(4) 0.0602(3) Uani 1 3 d S . .
Cl3 Cl 0.15430(4) -1.34570(4) -0.15430(4) 0.0435(2) Uani 1 3 d S . .


_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
N5 C6 1.473(3) . ?
N5 C4 1.520(3) . ?
N5 H5A 0.9670 . ?
N5 H5B 0.8878 . ?
C1 C2 1.403(3) 5_546 ?
C1 C2 1.404(3) . ?
C1 C4 1.507(3) . ?
C2 C1 1.403(3) 9_645 ?
C2 C3 1.516(3) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.365(3) . ?
C6 C11 1.370(4) . ?
C7 C8 1.369(4) 2_434 ?
C7 H7 0.9300 . ?
C8 C9 1.371(5) . ?
C8 C7 1.369(4) 2_435 ?
C8 H8 0.9300 . ?
C9 C10 1.371(6) . ?
C9 H9A 0.9300 . ?
C10 C11 1.388(5) 2_435 ?
C10 H10 0.9300 . ?
C11 C10 1.388(5) 2_434 ?
C11 H11 0.9300 . ?
Zn1 Cl2 2.2489(10) . ?
Zn1 Cl1 2.2709(5) 9_645 ?
Zn1 Cl1 2.2709(5) . ?
Zn1 Cl1 2.2709(5) 5_546 ?

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
C6 N5 C4 114.84(17) . . ?
C6 N5 H5A 108.8 . . ?
C4 N5 H5A 112.6 . . ?
C6 N5 H5B 108.2 . . ?
C4 N5 H5B 112.2 . . ?
H5A N5 H5B 98.9 . . ?
C2 C1 C2 121.0(2) 5_546 . ?
C2 C1 C4 118.85(17) 5_546 . ?
C2 C1 C4 120.14(18) . . ?
C1 C2 C1 119.0(2) 9_645 . ?
C1 C2 C3 120.65(18) 9_645 . ?
C1 C2 C3 120.35(19) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 N5 112.16(15) . . ?
C1 C4 H4A 109.2 . . ?
N5 C4 H4A 109.2 . . ?
C1 C4 H4B 109.2 . . ?
N5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C7 C6 C11 121.2(2) . . ?
C7 C6 N5 121.1(2) . . ?
C11 C6 N5 117.6(2) . . ?
C8 C7 C6 119.8(3) 2_434 . ?
C8 C7 H7 120.1 2_434 . ?
C6 C7 H7 120.1 . . ?
C9 C8 C7 119.8(3) . 2_435 ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 2_435 . ?
C8 C9 C10 120.5(3) . . ?
C8 C9 H9A 119.7 . . ?
C10 C9 H9A 119.7 . . ?
C9 C10 C11 119.8(3) . 2_435 ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 2_435 . ?
C6 C11 C10 118.8(3) . 2_434 ?
C6 C11 H11 120.6 . . ?
C10 C11 H11 120.6 2_434 . ?
Cl2 Zn1 Cl1 110.448(17) . 9_645 ?
Cl2 Zn1 Cl1 110.448(17) . . ?
Cl1 Zn1 Cl1 108.477(18) 9_645 . ?
Cl2 Zn1 Cl1 110.448(17) . 5_546 ?
Cl1 Zn1 Cl1 108.477(18) 9_645 5_546 ?
Cl1 Zn1 Cl1 108.477(18) . 5_546 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C1 1.3(4) 5_546 . . 9_645 ?
C4 C1 C2 C1 -178.04(13) . . . 9_645 ?
C2 C1 C2 C3 -177.59(14) 5_546 . . . ?
C4 C1 C2 C3 3.1(3) . . . . ?
C2 C1 C4 N5 82.2(2) 5_546 . . . ?
C2 C1 C4 N5 -98.5(2) . . . . ?
C6 N5 C4 C1 -143.35(18) . . . . ?
C4 N5 C6 C7 -33.8(3) . . . . ?
C4 N5 C6 C11 149.0(3) . . . . ?
C11 C6 C7 C8 -3.6(5) . . . 2_434 ?
N5 C6 C7 C8 179.3(3) . . . 2_434 ?
C7 C8 C9 C10 2.1(6) 2_435 . . . ?
C8 C9 C10 C11 -3.1(8) . . . 2_435 ?
C7 C6 C11 C10 2.6(6) . . . 2_434 ?
N5 C6 C11 C10 179.8(4) . . . 2_434 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.038
####################################################################### 
# 
# 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_MnCl4-3
_database_code_depnum_ccdc_archive 'CCDC 1406457'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H36 Cl5 Mn N3 O0'
_chemical_formula_weight         670.81

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   P213

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

_cell_length_a                   14.7135(6)
_cell_length_b                   14.7135(6)
_cell_length_c                   14.7135(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3185.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1388
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20015
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         27.52
_reflns_number_total             2466
_reflns_number_gt                2357
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0363P)²+0.8925P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.00(2)
_refine_ls_number_reflns         2466
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0683
_refine_ls_wR_factor_gt          0.0674
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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
N5 N -0.21652(10) -0.53256(10) -0.26921(10) 0.0307(3) Uani 1 1 d . . .
H5A H -0.2442 -0.5162 -0.3231 0.037 Uiso 1 1 d R . .
H5B H -0.2578 -0.5682 -0.2412 0.037 Uiso 1 1 d R . .
C1 C -0.24268(11) -0.36443(11) -0.25494(12) 0.0265(3) Uani 1 1 d . . .
C2 C -0.32066(12) -0.33276(12) -0.20972(11) 0.0280(3) Uani 1 1 d . . .
C3 C -0.35699(14) -0.38283(14) -0.12723(13) 0.0376(4) Uani 1 1 d . . .
H3A H -0.4200 -0.3680 -0.1188 0.056 Uiso 1 1 calc R . .
H3B H -0.3232 -0.3650 -0.0744 0.056 Uiso 1 1 calc R . .
H3C H -0.3508 -0.4471 -0.1364 0.056 Uiso 1 1 calc R . .
C4 C -0.19168(12) -0.44599(12) -0.21913(12) 0.0310(4) Uani 1 1 d . . .
H4A H -0.2051 -0.4535 -0.1550 0.037 Uiso 1 1 calc R . .
H4B H -0.1269 -0.4353 -0.2251 0.037 Uiso 1 1 calc R . .
C6 C -0.14086(14) -0.59697(13) -0.28394(13) 0.0359(4) Uani 1 1 d . . .
C7 C -0.1449(2) -0.6519(2) -0.3587(2) 0.0803(10) Uani 1 1 d . . .
H7A H -0.1934 -0.6479 -0.3990 0.096 Uiso 1 1 calc R . .
C8 C -0.0750(3) -0.7140(3) -0.3735(2) 0.1089(16) Uani 1 1 d . . .
H8A H -0.0772 -0.7531 -0.4231 0.131 Uiso 1 1 calc R . .
C9 C -0.0024(2) -0.7172(2) -0.3141(2) 0.0793(10) Uani 1 1 d . . .
H9A H 0.0463 -0.7558 -0.3259 0.095 Uiso 1 1 calc R . .
C10 C -0.00190(18) -0.66402(18) -0.2384(2) 0.0600(6) Uani 1 1 d . . .
H10A H 0.0459 -0.6684 -0.1973 0.072 Uiso 1 1 calc R . .
C21 C -0.07171(17) -0.60377(16) -0.22217(17) 0.0518(6) Uani 1 1 d . . .
H21A H -0.0718 -0.5682 -0.1699 0.062 Uiso 1 1 calc R . .
Mn1 Mn -0.047363(18) -0.547363(18) 0.047363(18) 0.03091(11) Uani 1 3 d S . .
Cl1 Cl 0.04436(3) -0.45564(3) -0.04436(3) 0.0595(3) Uani 1 3 d S . .
Cl2 Cl -0.02837(4) -0.70163(3) 0.00862(4) 0.04368(13) Uani 1 1 d . . .
Cl3 Cl -0.34479(4) -0.65521(4) -0.15521(4) 0.04078(19) Uani 1 3 d S . .


_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
N5 C6 1.478(2) . ?
N5 C4 1.516(2) . ?
N5 H5A 0.9234 . ?
N5 H5B 0.9018 . ?
C1 C2 1.400(2) 5 ?
C1 C2 1.406(2) . ?
C1 C4 1.510(2) . ?
C2 C1 1.400(2) 9 ?
C2 C3 1.517(3) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C21 1.368(3) . ?
C6 C7 1.366(3) . ?
C7 C8 1.392(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.381(5) . ?
C8 H8A 0.9300 . ?
C9 C10 1.362(5) . ?
C9 H9A 0.9300 . ?
C10 C21 1.378(3) . ?
C10 H10A 0.9300 . ?
C21 H21A 0.9300 . ?
Mn1 Cl1 2.3374(10) . ?
Mn1 Cl2 2.3568(5) 8_544 ?
Mn1 Cl2 2.3568(5) . ?
Mn1 Cl2 2.3568(5) 10_545 ?

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
C6 N5 C4 115.37(14) . . ?
C6 N5 H5A 111.9 . . ?
C4 N5 H5A 107.8 . . ?
C6 N5 H5B 101.6 . . ?
C4 N5 H5B 115.4 . . ?
H5A N5 H5B 104.3 . . ?
C2 C1 C2 121.14(17) 5 . ?
C2 C1 C4 118.60(15) 5 . ?
C2 C1 C4 120.25(15) . . ?
C1 C2 C1 118.85(17) 9 . ?
C1 C2 C3 120.80(16) 9 . ?
C1 C2 C3 120.35(16) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 N5 112.22(13) . . ?
C1 C4 H4A 109.2 . . ?
N5 C4 H4A 109.2 . . ?
C1 C4 H4B 109.2 . . ?
N5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C21 C6 C7 121.6(2) . . ?
C21 C6 N5 120.64(18) . . ?
C7 C6 N5 117.71(19) . . ?
C6 C7 C8 118.8(3) . . ?
C6 C7 H7A 120.6 . . ?
C8 C7 H7A 120.6 . . ?
C9 C8 C7 119.7(3) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
C10 C9 C8 120.1(3) . . ?
C10 C9 H9A 119.9 . . ?
C8 C9 H9A 119.9 . . ?
C9 C10 C21 120.5(3) . . ?
C9 C10 H10A 119.7 . . ?
C21 C10 H10A 119.7 . . ?
C6 C21 C10 119.1(2) . . ?
C6 C21 H21A 120.4 . . ?
C10 C21 H21A 120.4 . . ?
Cl1 Mn1 Cl2 110.360(16) . 8_544 ?
Cl1 Mn1 Cl2 110.360(16) . . ?
Cl2 Mn1 Cl2 108.568(17) 8_544 . ?
Cl1 Mn1 Cl2 110.360(16) . 10_545 ?
Cl2 Mn1 Cl2 108.568(17) 8_544 10_545 ?
Cl2 Mn1 Cl2 108.568(17) . 10_545 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C1 -1.3(3) 5 . . 9 ?
C4 C1 C2 C1 177.62(11) . . . 9 ?
C2 C1 C2 C3 178.10(12) 5 . . . ?
C4 C1 C2 C3 -3.0(2) . . . . ?
C2 C1 C4 N5 -82.32(19) 5 . . . ?
C2 C1 C4 N5 98.72(18) . . . . ?
C6 N5 C4 C1 143.28(15) . . . . ?
C4 N5 C6 C21 32.0(3) . . . . ?
C4 N5 C6 C7 -151.0(2) . . . . ?
C21 C6 C7 C8 -2.2(5) . . . . ?
N5 C6 C7 C8 -179.2(3) . . . . ?
C6 C7 C8 C9 -1.7(7) . . . . ?
C7 C8 C9 C10 4.2(7) . . . . ?
C8 C9 C10 C21 -2.8(5) . . . . ?
C7 C6 C21 C10 3.6(4) . . . . ?
N5 C6 C21 C10 -179.5(2) . . . . ?
C9 C10 C21 C6 -1.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.037
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1406458'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H36 Cl5 Co N3 O0'
_chemical_formula_weight         674.80

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'
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'
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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   P213

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

_cell_length_a                   14.6540(12)
_cell_length_b                   14.6540(12)
_cell_length_c                   14.6540(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3146.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.220
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19782
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         27.52
_reflns_number_total             2428
_reflns_number_gt                2283
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0305P)²+1.3467P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.987(17)
_refine_ls_number_reflns         2428
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0660
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.987
_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
N5 N -0.46704(11) -1.23025(11) -0.21655(11) 0.0310(4) Uani 1 1 d . . .
H5A H -0.4382 -1.2618 -0.2607 0.037 Uiso 1 1 d R . .
H5B H -0.4828 -1.1757 -0.2401 0.037 Uiso 1 1 d R . .
C1 C -0.63571(12) -1.24542(13) -0.24206(13) 0.0265(4) Uani 1 1 d . . .
C2 C -0.67984(13) -1.16729(14) -0.20914(13) 0.0284(4) Uani 1 1 d . . .
C3 C -0.64318(16) -1.11650(16) -0.12667(15) 0.0376(5) Uani 1 1 d . . .
H3A H -0.6478 -1.0520 -0.1369 0.056 Uiso 1 1 calc R . .
H3B H -0.5804 -1.1327 -0.1172 0.056 Uiso 1 1 calc R . .
H3C H -0.6782 -1.1327 -0.0737 0.056 Uiso 1 1 calc R . .
C4 C -0.55359(14) -1.28097(13) -0.19106(14) 0.0320(4) Uani 1 1 d . . .
H4A H -0.5458 -1.3453 -0.2044 0.038 Uiso 1 1 calc R . .
H4B H -0.5641 -1.2748 -0.1260 0.038 Uiso 1 1 calc R . .
C6 C -0.40263(15) -1.21532(15) -0.14072(16) 0.0363(5) Uani 1 1 d . . .
C7 C -0.39407(17) -1.27808(19) -0.07250(19) 0.0516(6) Uani 1 1 d . . .
H7A H -0.4284 -1.3314 -0.0736 0.062 Uiso 1 1 calc R . .
C8 C -0.3342(2) -1.2619(2) -0.0020(2) 0.0615(7) Uani 1 1 d . . .
H8 H -0.3292 -1.3035 0.0456 0.074 Uiso 1 1 calc R . .
C9 C -0.2821(3) -1.1843(2) -0.0020(2) 0.0817(11) Uani 1 1 d . . .
H9 H -0.2435 -1.1723 0.0469 0.098 Uiso 1 1 calc R . .
C10 C -0.2865(3) -1.1243(3) -0.0735(3) 0.1133(18) Uani 1 1 d . . .
H10 H -0.2478 -1.0739 -0.0752 0.136 Uiso 1 1 calc R . .
C11 C -0.3489(2) -1.1389(2) -0.1434(3) 0.0823(12) Uani 1 1 d . . .
H11 H -0.3541 -1.0976 -0.1913 0.099 Uiso 1 1 calc R . .
Co1 Co -0.047799(17) -0.452201(17) -0.547799(17) 0.02976(11) Uani 1 3 d S . .
Cl1 Cl -0.19708(4) -0.48912(4) -0.52845(4) 0.04317(14) Uani 1 1 d . . .
Cl2 Cl 0.04104(4) -0.54104(4) -0.45896(4) 0.0575(3) Uani 1 3 d S . .
Cl3 Cl 0.34578(4) -0.84578(4) -0.15422(4) 0.0417(2) Uani 1 3 d S . .


_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
N5 C6 1.474(3) . ?
N5 C4 1.517(3) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C1 C2 1.401(3) . ?
C1 C2 1.403(3) 10_534 ?
C1 C4 1.509(3) . ?
C2 C1 1.403(3) 8_443 ?
C2 C3 1.518(3) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.364(3) . ?
C6 C11 1.369(4) . ?
C7 C8 1.376(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.369(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.369(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.391(4) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
Co1 Cl2 2.2549(11) . ?
Co1 Cl1 2.2712(6) 12_444 ?
Co1 Cl1 2.2712(6) . ?
Co1 Cl1 2.2712(6) 7_544 ?

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
C6 N5 C4 114.99(16) . . ?
C6 N5 H5A 108.5 . . ?
C4 N5 H5A 108.5 . . ?
C6 N5 H5B 108.7 . . ?
C4 N5 H5B 108.4 . . ?
H5A N5 H5B 107.5 . . ?
C2 C1 C2 121.11(19) . 10_534 ?
C2 C1 C4 118.66(17) . . ?
C2 C1 C4 120.22(17) 10_534 . ?
C1 C2 C1 118.88(19) . 8_443 ?
C1 C2 C3 120.78(18) . . ?
C1 C2 C3 120.34(18) 8_443 . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 N5 112.06(15) . . ?
C1 C4 H4A 109.2 . . ?
N5 C4 H4A 109.2 . . ?
C1 C4 H4B 109.2 . . ?
N5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C7 C6 C11 121.3(2) . . ?
C7 C6 N5 120.7(2) . . ?
C11 C6 N5 117.9(2) . . ?
C6 C7 C8 119.5(3) . . ?
C6 C7 H7A 120.2 . . ?
C8 C7 H7A 120.2 . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.5(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 119.7(3) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C6 C11 C10 118.9(3) . . ?
C6 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
Cl2 Co1 Cl1 110.272(18) . 12_444 ?
Cl2 Co1 Cl1 110.272(18) . . ?
Cl1 Co1 Cl1 108.659(18) 12_444 . ?
Cl2 Co1 Cl1 110.272(18) . 7_544 ?
Cl1 Co1 Cl1 108.659(18) 12_444 7_544 ?
Cl1 Co1 Cl1 108.659(18) . 7_544 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C1 1.3(4) 10_534 . . 8_443 ?
C4 C1 C2 C1 -177.94(12) . . . 8_443 ?
C2 C1 C2 C3 -177.71(14) 10_534 . . . ?
C4 C1 C2 C3 3.0(3) . . . . ?
C2 C1 C4 N5 -82.2(2) . . . . ?
C2 C1 C4 N5 98.5(2) 10_534 . . . ?
C6 N5 C4 C1 143.33(17) . . . . ?
C4 N5 C6 C7 33.5(3) . . . . ?
C4 N5 C6 C11 -149.6(3) . . . . ?
C11 C6 C7 C8 4.0(5) . . . . ?
N5 C6 C7 C8 -179.2(2) . . . . ?
C6 C7 C8 C9 -1.7(5) . . . . ?
C7 C8 C9 C10 -2.5(6) . . . . ?
C8 C9 C10 C11 4.5(7) . . . . ?
C7 C6 C11 C10 -1.9(6) . . . . ?
N5 C6 C11 C10 -178.8(4) . . . . ?
C9 C10 C11 C6 -2.3(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.038
####################################################################### 
# 
# 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_ZnBr4-5
_database_code_depnum_ccdc_archive 'CCDC 1406459'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H36 Br5 N3 O0 Zn'
_chemical_formula_weight         903.51

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           Cubic
_symmetry_space_group_name_H-M   P213

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

_cell_length_a                   14.9853(18)
_cell_length_b                   14.9853(18)
_cell_length_c                   14.9853(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3365.1(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1768
_exptl_absorpt_coefficient_mu    6.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8166
_exptl_absorpt_correction_T_max  0.8838
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21185
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         27.69
_reflns_number_total             2628
_reflns_number_gt                2206
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0303P)²+0.4642P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.037(12)
_refine_ls_number_reflns         2628
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0646
_refine_ls_wR_factor_gt          0.0606
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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
N5 N 0.2771(2) -0.5342(2) -0.0210(2) 0.0286(7) Uani 1 1 d . . .
H5A H 0.2662 -0.5053 -0.0799 0.034 Uiso 1 1 d R . .
H5B H 0.3130 -0.4884 0.0183 0.034 Uiso 1 1 d R . .
C1 C 0.0673(2) -0.5399(2) -0.0816(2) 0.0238(7) Uani 1 1 d . . .
C2 C 0.1119(2) -0.5085(2) -0.0054(2) 0.0235(8) Uani 1 1 d . . .
C3 C 0.1022(3) -0.6210(3) -0.1306(3) 0.0359(9) Uani 1 1 d . . .
H3A H 0.0890 -0.6155 -0.1931 0.054 Uiso 1 1 calc R . .
H3B H 0.0742 -0.6737 -0.1073 0.054 Uiso 1 1 calc R . .
H3C H 0.1656 -0.6251 -0.1225 0.054 Uiso 1 1 calc R . .
C4 C 0.1917(2) -0.5600(2) 0.0282(3) 0.0299(8) Uani 1 1 d . . .
H4A H 0.1810 -0.6234 0.0205 0.036 Uiso 1 1 calc R . .
H4B H 0.1993 -0.5487 0.0915 0.036 Uiso 1 1 calc R . .
C6 C 0.3411(3) -0.6079(3) -0.0351(3) 0.0342(9) Uani 1 1 d . . .
C7 C 0.3517(3) -0.6730(3) 0.0257(3) 0.0523(13) Uani 1 1 d . . .
H7A H 0.3193 -0.6715 0.0786 0.063 Uiso 1 1 calc R . .
C8 C 0.4105(3) -0.7419(4) 0.0102(4) 0.0607(13) Uani 1 1 d . . .
H8A H 0.4152 -0.7887 0.0507 0.073 Uiso 1 1 calc R . .
C9 C 0.4611(4) -0.7412(5) -0.0641(4) 0.086(2) Uani 1 1 d . . .
H9A H 0.5023 -0.7866 -0.0741 0.103 Uiso 1 1 calc R . .
C10 C 0.4519(6) -0.6743(6) -0.1239(5) 0.157(5) Uani 1 1 d . . .
H10A H 0.4866 -0.6745 -0.1754 0.188 Uiso 1 1 calc R . .
C11 C 0.3918(5) -0.6055(5) -0.1101(4) 0.105(3) Uani 1 1 d . . .
H11A H 0.3864 -0.5591 -0.1509 0.125 Uiso 1 1 calc R . .
Br1 Br -0.04987(2) -0.77067(3) -0.26463(3) 0.03932(12) Uani 1 1 d . . .
Br2 Br -0.29721(3) -0.70279(3) -0.20279(3) 0.0557(2) Uani 1 3 d S . .
Zn1 Zn -0.20541(3) -0.79459(3) -0.29459(3) 0.02878(17) Uani 1 3 d S . .
Br3 Br -0.40345(3) -0.90345(3) -0.59655(3) 0.03979(18) Uani 1 3 d S . .


_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
N5 C6 1.480(5) . ?
N5 C4 1.526(5) . ?
N5 H5A 0.9976 . ?
N5 H5B 1.0526 . ?
C1 C2 1.400(5) 10_545 ?
C1 C2 1.404(5) . ?
C1 C3 1.513(5) . ?
C2 C1 1.400(5) 8_544 ?
C2 C4 1.510(5) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.345(6) . ?
C6 C11 1.357(7) . ?
C7 C8 1.377(6) . ?
C7 H7A 0.9300 . ?
C8 C9 1.347(8) . ?
C8 H8A 0.9300 . ?
C9 C10 1.352(8) . ?
C9 H9A 0.9300 . ?
C10 C11 1.384(8) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9300 . ?
Br1 Zn1 2.4005(5) . ?
Br2 Zn1 2.3827(10) . ?
Zn1 Br1 2.4005(5) 11_444 ?
Zn1 Br1 2.4005(5) 6_445 ?

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
C6 N5 C4 115.0(3) . . ?
C6 N5 H5A 107.6 . . ?
C4 N5 H5A 113.7 . . ?
C6 N5 H5B 103.6 . . ?
C4 N5 H5B 108.9 . . ?
H5A N5 H5B 107.2 . . ?
C2 C1 C2 119.2(3) 10_545 . ?
C2 C1 C3 120.9(3) 10_545 . ?
C2 C1 C3 120.0(3) . . ?
C1 C2 C1 120.8(3) 8_544 . ?
C1 C2 C4 120.7(3) 8_544 . ?
C1 C2 C4 118.5(3) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 N5 111.9(3) . . ?
C2 C4 H4A 109.2 . . ?
N5 C4 H4A 109.2 . . ?
C2 C4 H4B 109.2 . . ?
N5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C7 C6 C11 121.0(4) . . ?
C7 C6 N5 121.4(4) . . ?
C11 C6 N5 117.5(4) . . ?
C6 C7 C8 120.3(4) . . ?
C6 C7 H7A 119.9 . . ?
C8 C7 H7A 119.9 . . ?
C9 C8 C7 119.6(5) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
C8 C9 C10 119.7(5) . . ?
C8 C9 H9A 120.1 . . ?
C10 C9 H9A 120.1 . . ?
C9 C10 C11 121.3(6) . . ?
C9 C10 H10A 119.3 . . ?
C11 C10 H10A 119.3 . . ?
C6 C11 C10 117.9(5) . . ?
C6 C11 H11A 121.0 . . ?
C10 C11 H11A 121.0 . . ?
Br2 Zn1 Br1 111.491(19) . . ?
Br2 Zn1 Br1 111.491(19) . 11_444 ?
Br1 Zn1 Br1 107.38(2) . 11_444 ?
Br2 Zn1 Br1 111.491(19) . 6_445 ?
Br1 Zn1 Br1 107.38(2) . 6_445 ?
Br1 Zn1 Br1 107.38(2) 11_444 6_445 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C1 -0.4(7) 10_545 . . 8_544 ?
C3 C1 C2 C1 178.8(2) . . . 8_544 ?
C2 C1 C2 C4 177.9(2) 10_545 . . . ?
C3 C1 C2 C4 -2.9(5) . . . . ?
C1 C2 C4 N5 -97.8(4) 8_544 . . . ?
C1 C2 C4 N5 83.8(4) . . . . ?
C6 N5 C4 C2 -145.2(3) . . . . ?
C4 N5 C6 C7 -35.0(6) . . . . ?
C4 N5 C6 C11 147.9(5) . . . . ?
C11 C6 C7 C8 -4.3(9) . . . . ?
N5 C6 C7 C8 178.7(4) . . . . ?
C6 C7 C8 C9 3.8(9) . . . . ?
C7 C8 C9 C10 -2.0(11) . . . . ?
C8 C9 C10 C11 0.7(15) . . . . ?
C7 C6 C11 C10 2.9(11) . . . . ?
N5 C6 C11 C10 -180.0(7) . . . . ?
C9 C10 C11 C6 -1.1(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.69
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.081
####################################################################### 
# 
# 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_CdCl4-6
_database_code_depnum_ccdc_archive 'CCDC 1406460'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H42 Cd Cl5 N3 O0'
_chemical_formula_weight         770.36

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'
Cd Cd -0.8075 1.2024 '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'
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'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   P213

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

_cell_length_a                   15.1987(19)
_cell_length_b                   15.1987(19)
_cell_length_c                   15.1987(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3510.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1576
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21889
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         27.58
_reflns_number_total             2707
_reflns_number_gt                2621
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0224P)²+0.9241P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.01(2)
_refine_ls_number_reflns         2707
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0546
_refine_ls_wR_factor_gt          0.0537
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.002
_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
N1 N -0.48136(11) -0.96446(11) -0.28800(12) 0.0360(4) Uani 1 1 d . . .
H1N H -0.5072 -0.9080 -0.2754 0.043 Uiso 1 1 d R . .
H2N H -0.5259 -0.9959 -0.3232 0.043 Uiso 1 1 d R . .
C1 C -0.40650(15) -0.95222(15) -0.34830(15) 0.0390(5) Uani 1 1 d . . .
C2 C -0.61270(16) -1.10509(15) -0.14476(17) 0.0454(5) Uani 1 1 d . . .
H2A H -0.6722 -1.1180 -0.1280 0.068 Uiso 1 1 calc R . .
H2B H -0.5757 -1.1542 -0.1303 0.068 Uiso 1 1 calc R . .
H2C H -0.6102 -1.0944 -0.2070 0.068 Uiso 1 1 calc R . .
C3 C -0.45625(14) -1.01255(14) -0.20391(14) 0.0384(4) Uani 1 1 d . . .
H3A H -0.4678 -1.0749 -0.2112 0.046 Uiso 1 1 calc R . .
H3B H -0.3937 -1.0053 -0.1936 0.046 Uiso 1 1 calc R . .
C4 C -0.58129(13) -1.02435(13) -0.09598(13) 0.0325(4) Uani 1 1 d . . .
C5 C -0.50625(13) -0.97924(13) -0.12522(13) 0.0315(4) Uani 1 1 d . . .
C6 C -0.3795(2) -0.86842(18) -0.3693(2) 0.0617(8) Uani 1 1 d . . .
H6A H -0.4080 -0.8195 -0.3460 0.074 Uiso 1 1 calc R . .
C7 C -0.26542(18) -0.92999(19) -0.46060(19) 0.0608(7) Uani 1 1 d . . .
C8 C -0.2922(2) -1.01217(18) -0.43503(19) 0.0610(7) Uani 1 1 d . . .
H8A H -0.2619 -1.0611 -0.4557 0.073 Uiso 1 1 calc R . .
C9 C -0.3086(2) -0.8586(2) -0.4262(2) 0.0788(11) Uani 1 1 d . . .
H9A H -0.2900 -0.8023 -0.4413 0.095 Uiso 1 1 calc R . .
C10 C -0.36321(17) -1.02465(18) -0.37930(18) 0.0529(6) Uani 1 1 d . . .
H10A H -0.3810 -1.0810 -0.3633 0.063 Uiso 1 1 calc R . .
C11 C -0.1895(2) -0.9193(3) -0.5239(3) 0.0978(13) Uani 1 1 d . . .
H11A H -0.2093 -0.8889 -0.5756 0.147 Uiso 1 1 calc R . .
H11B H -0.1674 -0.9762 -0.5401 0.147 Uiso 1 1 calc R . .
H11C H -0.1435 -0.8860 -0.4962 0.147 Uiso 1 1 calc R . .
Cd1 Cd -0.283743(10) -1.283743(10) -0.283743(10) 0.04067(8) Uani 1 3 d S . .
Cl1 Cl -0.19350(6) -1.19350(6) -0.19350(6) 0.1459(10) Uani 1 3 d S . .
Cl2 Cl -0.44235(4) -1.26310(4) -0.25451(4) 0.05198(15) Uani 1 1 d . . .
Cl3 Cl -0.40587(4) -0.59413(4) -0.09413(4) 0.0412(2) Uani 1 3 d S . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.473(3) . ?
N1 C3 1.521(3) . ?
N1 H1N 0.9629 . ?
N1 H2N 0.9866 . ?
C1 C10 1.366(3) . ?
C1 C6 1.376(4) . ?
C2 C4 1.511(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C5 1.505(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.403(3) . ?
C4 C5 1.403(3) 7_434 ?
C5 C4 1.403(3) 12_345 ?
C6 C9 1.389(4) . ?
C6 H6A 0.9300 . ?
C7 C8 1.370(4) . ?
C7 C9 1.372(4) . ?
C7 C11 1.511(4) . ?
C8 C10 1.384(4) . ?
C8 H8A 0.9300 . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
Cd1 Cl1 2.3756(17) . ?
Cd1 Cl2 2.4713(7) 5_546 ?
Cd1 Cl2 2.4713(7) . ?
Cd1 Cl2 2.4713(7) 9_645 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C3 112.93(16) . . ?
C1 N1 H1N 109.0 . . ?
C3 N1 H1N 111.3 . . ?
C1 N1 H2N 104.7 . . ?
C3 N1 H2N 113.2 . . ?
H1N N1 H2N 105.0 . . ?
C10 C1 C6 121.5(2) . . ?
C10 C1 N1 119.0(2) . . ?
C6 C1 N1 119.5(2) . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C5 C3 N1 112.30(16) . . ?
C5 C3 H3A 109.1 . . ?
N1 C3 H3A 109.1 . . ?
C5 C3 H3B 109.1 . . ?
N1 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C5 C4 C5 118.9(2) . 7_434 ?
C5 C4 C2 119.89(19) . . ?
C5 C4 C2 121.23(19) 7_434 . ?
C4 C5 C4 121.1(2) . 12_345 ?
C4 C5 C3 119.87(18) . . ?
C4 C5 C3 119.00(18) 12_345 . ?
C1 C6 C9 118.4(3) . . ?
C1 C6 H6A 120.8 . . ?
C9 C6 H6A 120.8 . . ?
C8 C7 C9 118.1(2) . . ?
C8 C7 C11 120.4(3) . . ?
C9 C7 C11 121.6(3) . . ?
C7 C8 C10 122.0(2) . . ?
C7 C8 H8A 119.0 . . ?
C10 C8 H8A 119.0 . . ?
C7 C9 C6 121.6(3) . . ?
C7 C9 H9A 119.2 . . ?
C6 C9 H9A 119.2 . . ?
C1 C10 C8 118.4(3) . . ?
C1 C10 H10A 120.8 . . ?
C8 C10 H10A 120.8 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Cl1 Cd1 Cl2 112.714(16) . 5_546 ?
Cl1 Cd1 Cl2 112.714(16) . . ?
Cl2 Cd1 Cl2 106.043(17) 5_546 . ?
Cl1 Cd1 Cl2 112.714(16) . 9_645 ?
Cl2 Cd1 Cl2 106.043(17) 5_546 9_645 ?
Cl2 Cd1 Cl2 106.043(17) . 9_645 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 C1 C10 59.6(3) . . . . ?
C3 N1 C1 C6 -117.7(3) . . . . ?
C1 N1 C3 C5 144.59(18) . . . . ?
C5 C4 C5 C4 -0.9(4) 7_434 . . 12_345 ?
C2 C4 C5 C4 179.91(15) . . . 12_345 ?
C5 C4 C5 C3 177.95(13) 7_434 . . . ?
C2 C4 C5 C3 -1.3(3) . . . . ?
N1 C3 C5 C4 97.7(2) . . . . ?
N1 C3 C5 C4 -83.4(2) . . . 12_345 ?
C10 C1 C6 C9 2.6(5) . . . . ?
N1 C1 C6 C9 179.9(3) . . . . ?
C9 C7 C8 C10 2.9(5) . . . . ?
C11 C7 C8 C10 -178.0(3) . . . . ?
C8 C7 C9 C6 -2.1(6) . . . . ?
C11 C7 C9 C6 178.8(4) . . . . ?
C1 C6 C9 C7 -0.5(6) . . . . ?
C6 C1 C10 C8 -1.9(4) . . . . ?
N1 C1 C10 C8 -179.2(2) . . . . ?
C7 C8 C10 C1 -1.0(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.040
####################################################################### 
# 
# 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_CoCl4-6
_database_code_depnum_ccdc_archive 'CCDC 1406461'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H36 Cl5 Co N3'
_chemical_formula_weight         710.83

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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   P213

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

_cell_length_a                   15.1477(8)
_cell_length_b                   15.1477(8)
_cell_length_c                   15.1477(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3475.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1468
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21842
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         27.56
_reflns_number_total             2697
_reflns_number_gt                2440
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0504P)²+0.6145P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(18)
_refine_ls_number_reflns         2697
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0844
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
N1 N -0.03654(12) -0.71780(12) -0.23285(11) 0.0354(4) Uani 1 1 d . . .
C1 C 0.04717(15) -0.76644(15) -0.20548(14) 0.0378(4) Uani 1 1 d . . .
H1B H 0.0561 -0.7592 -0.1425 0.045 Uiso 1 1 calc R . .
H1C H 0.0401 -0.8290 -0.2174 0.045 Uiso 1 1 calc R . .
C2 C 0.12721(13) -0.73273(13) -0.25401(13) 0.0311(4) Uani 1 1 d . . .
C3 C -0.1851(2) -0.76190(18) -0.0425(2) 0.0590(7) Uani 1 1 d . . .
H3A H -0.2057 -0.8102 -0.0106 0.071 Uiso 1 1 calc R . .
C4 C 0.17032(13) -0.65722(13) -0.22259(13) 0.0313(4) Uani 1 1 d . . .
C5 C 0.13771(16) -0.60805(17) -0.14231(15) 0.0438(5) Uani 1 1 d . . .
H5A H 0.1408 -0.5457 -0.1531 0.066 Uiso 1 1 calc R . .
H5B H 0.1739 -0.6227 -0.0924 0.066 Uiso 1 1 calc R . .
H5C H 0.0777 -0.6245 -0.1304 0.066 Uiso 1 1 calc R . .
C6 C -0.09772(14) -0.70343(15) -0.15856(15) 0.0382(5) Uani 1 1 d . . .
C7 C -0.1185(2) -0.61963(18) -0.13301(19) 0.0607(8) Uani 1 1 d . . .
H7A H -0.0950 -0.5712 -0.1625 0.073 Uiso 1 1 calc R . .
C8 C -0.21132(19) -0.6785(2) -0.01797(19) 0.0592(7) Uani 1 1 d . . .
C9 C -0.12914(18) -0.77603(17) -0.11316(18) 0.0512(6) Uani 1 1 d . . .
H9A H -0.1131 -0.8329 -0.1297 0.061 Uiso 1 1 calc R . .
C10 C -0.1761(2) -0.6077(2) -0.0615(2) 0.0748(10) Uani 1 1 d . . .
H10A H -0.1905 -0.5508 -0.0434 0.090 Uiso 1 1 calc R . .
C11 C -0.2746(3) -0.6647(3) 0.0585(2) 0.0910(12) Uani 1 1 d . . .
H11A H -0.2893 -0.7208 0.0841 0.137 Uiso 1 1 calc R . .
H11B H -0.3273 -0.6366 0.0374 0.137 Uiso 1 1 calc R . .
H11C H -0.2471 -0.6281 0.1023 0.137 Uiso 1 1 calc R . .
Co1 Co -0.039777(18) -1.039777(18) -0.039777(18) 0.03667(13) Uani 1 3 d S . .
Cl1 Cl 0.04457(6) -0.95543(6) 0.04457(6) 0.1258(8) Uani 1 3 d S . .
Cl2 Cl -0.00888(5) -1.01801(4) -0.18626(4) 0.05059(16) Uani 1 1 d . . .
Cl3 Cl -0.15275(4) -0.84725(4) -0.34725(4) 0.0403(2) Uani 1 3 d S . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C6 1.474(3) . ?
N1 C1 1.524(3) . ?
C1 C2 1.507(3) . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 C4 1.400(3) . ?
C2 C4 1.407(3) 12_444 ?
C3 C8 1.376(4) . ?
C3 C9 1.383(3) . ?
C3 H3A 0.9300 . ?
C4 C2 1.407(3) 7_544 ?
C4 C5 1.509(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.364(4) . ?
C6 C9 1.382(3) . ?
C7 C10 1.402(4) . ?
C7 H7A 0.9300 . ?
C8 C10 1.367(4) . ?
C8 C11 1.517(4) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
Co1 Cl1 2.2130(16) . ?
Co1 Cl2 2.2915(6) 9_645 ?
Co1 Cl2 2.2915(6) . ?
Co1 Cl2 2.2915(6) 5_546 ?

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
C6 N1 C1 112.75(16) . . ?
C2 C1 N1 111.89(16) . . ?
C2 C1 H1B 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1C 109.2 . . ?
N1 C1 H1C 109.2 . . ?
H1B C1 H1C 107.9 . . ?
C4 C2 C4 121.3(2) . 12_444 ?
C4 C2 C1 119.09(18) . . ?
C4 C2 C1 119.63(19) 12_444 . ?
C8 C3 C9 121.9(2) . . ?
C8 C3 H3A 119.1 . . ?
C9 C3 H3A 119.1 . . ?
C2 C4 C2 118.7(2) . 7_544 ?
C2 C4 C5 121.62(19) . . ?
C2 C4 C5 119.67(19) 7_544 . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C9 121.3(2) . . ?
C7 C6 N1 120.0(2) . . ?
C9 C6 N1 118.6(2) . . ?
C6 C7 C10 118.9(2) . . ?
C6 C7 H7A 120.6 . . ?
C10 C7 H7A 120.6 . . ?
C10 C8 C3 118.5(2) . . ?
C10 C8 C11 120.5(3) . . ?
C3 C8 C11 120.9(3) . . ?
C6 C9 C3 118.3(2) . . ?
C6 C9 H9A 120.9 . . ?
C3 C9 H9A 120.9 . . ?
C8 C10 C7 121.0(3) . . ?
C8 C10 H10A 119.5 . . ?
C7 C10 H10A 119.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Cl1 Co1 Cl2 110.98(2) . 9_645 ?
Cl1 Co1 Cl2 110.98(2) . . ?
Cl2 Co1 Cl2 107.92(2) 9_645 . ?
Cl1 Co1 Cl2 110.98(2) . 5_546 ?
Cl2 Co1 Cl2 107.92(2) 9_645 5_546 ?
Cl2 Co1 Cl2 107.92(2) . 5_546 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N1 C1 C2 -143.07(18) . . . . ?
N1 C1 C2 C4 83.2(2) . . . . ?
N1 C1 C2 C4 -96.8(2) . . . 12_444 ?
C4 C2 C4 C2 -1.2(4) 12_444 . . 7_544 ?
C1 C2 C4 C2 178.77(13) . . . 7_544 ?
C4 C2 C4 C5 179.01(14) 12_444 . . . ?
C1 C2 C4 C5 -1.0(3) . . . . ?
C1 N1 C6 C7 117.8(3) . . . . ?
C1 N1 C6 C9 -58.8(3) . . . . ?
C9 C6 C7 C10 -2.8(5) . . . . ?
N1 C6 C7 C10 -179.3(3) . . . . ?
C9 C3 C8 C10 -4.4(5) . . . . ?
C9 C3 C8 C11 178.5(3) . . . . ?
C7 C6 C9 C3 2.2(4) . . . . ?
N1 C6 C9 C3 178.7(2) . . . . ?
C8 C3 C9 C6 1.4(5) . . . . ?
C3 C8 C10 C7 3.7(5) . . . . ?
C11 C8 C10 C7 -179.1(4) . . . . ?
C6 C7 C10 C8 -0.2(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.049
####################################################################### 
# 
# 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_HgCl4-8
_database_code_depnum_ccdc_archive 'CCDC 1406462'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H39 Cl5 Hg N3'
_chemical_formula_weight         855.51

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 '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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   P213

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

_cell_length_a                   15.208(3)
_cell_length_b                   15.208(3)
_cell_length_c                   15.208(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3517.4(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1692
_exptl_absorpt_coefficient_mu    4.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8166
_exptl_absorpt_correction_T_max  0.8838
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21666
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2696
_reflns_number_gt                2471
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0408P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.985(8)
_refine_ls_number_reflns         2696
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0773
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_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
N1 N -0.2131(2) -0.5180(2) -0.4644(2) 0.0307(7) Uani 1 1 d . . .
H1N H -0.1685 -0.4802 -0.4939 0.037 Uiso 1 1 d R . .
C1 C -0.3864(3) -0.6059(3) -0.3559(3) 0.0379(11) Uani 1 1 d . . .
H1A H -0.3834 -0.5940 -0.2940 0.057 Uiso 1 1 calc R . .
H1B H -0.3290 -0.6214 -0.3771 0.057 Uiso 1 1 calc R . .
H1C H -0.4262 -0.6538 -0.3662 0.057 Uiso 1 1 calc R . .
C2 C -0.1303(4) -0.6195(4) -0.3692(4) 0.0560(15) Uani 1 1 d . . .
H2A H -0.1528 -0.5904 -0.3204 0.067 Uiso 1 1 calc R . .
C3 C -0.1519(3) -0.5929(3) -0.4517(3) 0.0340(9) Uani 1 1 d . . .
C4 C -0.3749(2) -0.4944(3) -0.4799(3) 0.0257(8) Uani 1 1 d . . .
C5 C -0.2960(3) -0.5440(3) -0.5129(3) 0.0318(9) Uani 1 1 d . . .
H5A H -0.2885 -0.5325 -0.5751 0.038 Uiso 1 1 calc R . .
H5B H -0.3059 -0.6066 -0.5055 0.038 Uiso 1 1 calc R . .
C6 C -0.4189(3) -0.5246(3) -0.4041(3) 0.0270(8) Uani 1 1 d . . .
C7 C -0.1212(4) -0.6366(4) -0.5261(4) 0.0493(12) Uani 1 1 d . . .
H7A H -0.1377 -0.6192 -0.5823 0.059 Uiso 1 1 calc R . .
C8 C -0.0653(4) -0.7065(4) -0.5129(4) 0.0556(14) Uani 1 1 d . . .
H8A H -0.0438 -0.7362 -0.5617 0.067 Uiso 1 1 calc R . .
C9 C -0.0396(4) -0.7347(4) -0.4299(4) 0.0600(16) Uani 1 1 d . . .
C10 C -0.0735(5) -0.6912(4) -0.3587(4) 0.075(2) Uani 1 1 d . . .
H10A H -0.0586 -0.7097 -0.3023 0.091 Uiso 1 1 calc R . .
C11 C 0.0235(6) -0.8111(5) -0.4181(6) 0.099(3) Uani 1 1 d . . .
H11A H 0.0217 -0.8480 -0.4693 0.149 Uiso 1 1 calc R . .
H11B H 0.0067 -0.8446 -0.3674 0.149 Uiso 1 1 calc R . .
H11C H 0.0821 -0.7889 -0.4103 0.149 Uiso 1 1 calc R . .
Hg1 Hg -0.219419(11) -0.719419(11) -0.780581(11) 0.03916(10) Uani 1 3 d S . .
Cl1 Cl -0.24448(9) -0.55699(8) -0.76300(8) 0.0464(3) Uani 1 1 d . . .
Cl2 Cl -0.30920(15) -0.80920(15) -0.69080(15) 0.168(3) Uani 1 3 d S . .
Cl3 Cl -0.40551(8) -0.59449(8) -0.09449(8) 0.0357(4) Uani 1 3 d S . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C3 1.484(6) . ?
N1 C5 1.513(5) . ?
N1 H1N 0.9953 . ?
C1 C6 1.520(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.358(7) . ?
C2 C10 1.400(8) . ?
C2 H2A 0.9300 . ?
C3 C7 1.392(7) . ?
C4 C6 1.406(6) 5 ?
C4 C6 1.409(6) . ?
C4 C5 1.504(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C4 1.406(6) 9 ?
C7 C8 1.375(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.389(8) . ?
C8 H8A 0.9300 . ?
C9 C10 1.370(9) . ?
C9 C11 1.517(8) . ?
C10 H10A 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
Hg1 Cl2 2.365(4) . ?
Hg1 Cl1 2.5137(13) 8_443 ?
Hg1 Cl1 2.5137(13) 10_534 ?
Hg1 Cl1 2.5137(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 N1 C5 112.7(3) . . ?
C3 N1 H1N 94.3 . . ?
C5 N1 H1N 119.9 . . ?
C6 C1 H1A 109.5 . . ?
C6 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C6 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C10 119.1(5) . . ?
C3 C2 H2A 120.4 . . ?
C10 C2 H2A 120.4 . . ?
C2 C3 C7 121.8(5) . . ?
C2 C3 N1 120.0(4) . . ?
C7 C3 N1 118.1(4) . . ?
C6 C4 C6 120.8(4) 5 . ?
C6 C4 C5 120.0(4) 5 . ?
C6 C4 C5 119.2(4) . . ?
C4 C5 N1 111.8(3) . . ?
C4 C5 H5A 109.3 . . ?
N1 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
N1 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
C4 C6 C4 119.1(4) 9 . ?
C4 C6 C1 120.5(4) 9 . ?
C4 C6 C1 120.4(4) . . ?
C8 C7 C3 117.2(5) . . ?
C8 C7 H7A 121.4 . . ?
C3 C7 H7A 121.4 . . ?
C7 C8 C9 123.1(5) . . ?
C7 C8 H8A 118.5 . . ?
C9 C8 H8A 118.5 . . ?
C10 C9 C8 117.6(5) . . ?
C10 C9 C11 121.0(6) . . ?
C8 C9 C11 121.5(6) . . ?
C9 C10 C2 121.2(6) . . ?
C9 C10 H10A 119.4 . . ?
C2 C10 H10A 119.4 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Cl2 Hg1 Cl1 114.73(3) . 8_443 ?
Cl2 Hg1 Cl1 114.73(3) . 10_534 ?
Cl1 Hg1 Cl1 103.73(3) 8_443 10_534 ?
Cl2 Hg1 Cl1 114.73(3) . . ?
Cl1 Hg1 Cl1 103.73(3) 8_443 . ?
Cl1 Hg1 Cl1 103.73(3) 10_534 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 C2 C3 C7 1.8(9) . . . . ?
C10 C2 C3 N1 179.0(6) . . . . ?
C5 N1 C3 C2 -118.5(5) . . . . ?
C5 N1 C3 C7 58.8(5) . . . . ?
C6 C4 C5 N1 97.1(4) 5 . . . ?
C6 C4 C5 N1 -83.0(4) . . . . ?
C3 N1 C5 C4 144.7(4) . . . . ?
C6 C4 C6 C4 2.0(8) 5 . . 9 ?
C5 C4 C6 C4 -177.9(3) . . . 9 ?
C6 C4 C6 C1 -179.6(3) 5 . . . ?
C5 C4 C6 C1 0.5(5) . . . . ?
C2 C3 C7 C8 -2.1(9) . . . . ?
N1 C3 C7 C8 -179.3(5) . . . . ?
C3 C7 C8 C9 0.5(9) . . . . ?
C7 C8 C9 C10 1.3(11) . . . . ?
C7 C8 C9 C11 -178.8(7) . . . . ?
C8 C9 C10 C2 -1.6(11) . . . . ?
C11 C9 C10 C2 178.5(8) . . . . ?
C3 C2 C10 C9 0.1(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.403
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.165
####################################################################### 
# 
# 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_ZnCl4-9
_database_code_depnum_ccdc_archive 'CCDC 1406463'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H42 Cl5 N3 Zn'
_chemical_formula_weight         723.34

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   P213

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

_cell_length_a                   15.155(4)
_cell_length_b                   15.155(4)
_cell_length_c                   15.155(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3480.7(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21634
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         27.55
_reflns_number_total             2687
_reflns_number_gt                2473
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0343P)²+0.3237P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.993(10)
_refine_ls_number_reflns         2687
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001

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
N1 N 0.21843(10) -0.73241(9) -0.03599(10) 0.0347(3) Uani 1 1 d . . .
H1N H 0.2463 -0.7717 -0.0664 0.042 Uiso 1 1 d R . .
H2 H 0.1644 -0.7572 -0.0217 0.042 Uiso 1 1 d R . .
C3 C 0.26734(12) -0.70560(12) 0.04723(12) 0.0368(4) Uani 1 1 d . . .
H3A H 0.3297 -0.7181 0.0400 0.044 Uiso 1 1 calc R . .
H3B H 0.2608 -0.6426 0.0562 0.044 Uiso 1 1 calc R . .
C4 C 0.26258(14) -0.54247(16) -0.18439(16) 0.0569(6) Uani 1 1 d . . .
H1 H 0.3108 -0.5106 -0.2049 0.068 Uiso 1 1 calc R . .
C5 C 0.23312(11) -0.75398(10) 0.12724(10) 0.0302(3) Uani 1 1 d . . .
C6 C 0.15756(11) -0.72231(10) 0.17050(11) 0.0305(3) Uani 1 1 d . . .
C7 C 0.10849(14) -0.64195(12) 0.13756(13) 0.0430(4) Uani 1 1 d . . .
H7A H 0.0461 -0.6519 0.1422 0.064 Uiso 1 1 calc R . .
H7B H 0.1237 -0.6313 0.0770 0.064 Uiso 1 1 calc R . .
H7C H 0.1245 -0.5916 0.1725 0.064 Uiso 1 1 calc R . .
C8 C 0.17831(16) -0.51821(15) -0.21097(15) 0.0574(6) Uani 1 1 d . . .
C9 C 0.20403(12) -0.65853(12) -0.09744(12) 0.0368(4) Uani 1 1 d . . .
C10 C 0.11976(15) -0.63348(16) -0.11837(17) 0.0599(6) Uani 1 1 d . . .
H10A H 0.0714 -0.6630 -0.0947 0.072 Uiso 1 1 calc R . .
C12 C 0.27639(14) -0.61273(15) -0.12829(15) 0.0500(5) Uani 1 1 d . . .
H12A H 0.3332 -0.6289 -0.1116 0.060 Uiso 1 1 calc R . .
C15 C 0.1652(2) -0.4426(2) -0.2749(2) 0.0894(10) Uani 1 1 d . . .
H15A H 0.2185 -0.4085 -0.2785 0.134 Uiso 1 1 calc R . .
H15B H 0.1179 -0.4057 -0.2546 0.134 Uiso 1 1 calc R . .
H15C H 0.1510 -0.4656 -0.3322 0.134 Uiso 1 1 calc R . .
C16 C 0.10821(16) -0.56235(18) -0.1763(2) 0.0733(8) Uani 1 1 d . . .
H16A H 0.0513 -0.5449 -0.1913 0.088 Uiso 1 1 calc R . .
Zn1 Zn 0.039251(13) -0.960749(13) 0.039251(13) 0.03636(10) Uani 1 3 d S . .
Cl1 Cl 0.01826(3) -0.81389(3) 0.00945(4) 0.04952(13) Uani 1 1 d . . .
Cl2 Cl -0.04466(4) -1.04466(4) -0.04466(4) 0.1178(6) Uani 1 3 d S . .
Cl3 Cl 0.34755(3) -0.84755(3) -0.15245(3) 0.03942(17) Uani 1 3 d S . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C9 1.473(2) . ?
N1 C3 1.518(2) . ?
N1 H1N 0.8636 . ?
N1 H2 0.9260 . ?
C3 C5 1.509(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C12 1.379(3) . ?
C4 C8 1.389(3) . ?
C4 H1 0.9300 . ?
C5 C6 1.404(2) . ?
C5 C6 1.406(2) 9_645 ?
C6 C5 1.406(2) 5_546 ?
C6 C7 1.512(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C16 1.361(3) . ?
C8 C15 1.514(3) . ?
C9 C10 1.370(3) . ?
C9 C12 1.379(3) . ?
C10 C16 1.401(3) . ?
C10 H10A 0.9300 . ?
C12 H12A 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9300 . ?
Zn1 Cl2 2.2025(13) . ?
Zn1 Cl1 2.2932(8) 9_645 ?
Zn1 Cl1 2.2932(8) . ?
Zn1 Cl1 2.2932(8) 5_546 ?

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
C9 N1 C3 113.22(13) . . ?
C9 N1 H1N 105.1 . . ?
C3 N1 H1N 112.9 . . ?
C9 N1 H2 109.0 . . ?
C3 N1 H2 110.3 . . ?
H1N N1 H2 106.0 . . ?
C5 C3 N1 111.70(13) . . ?
C5 C3 H3A 109.3 . . ?
N1 C3 H3A 109.3 . . ?
C5 C3 H3B 109.3 . . ?
N1 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C12 C4 C8 121.5(2) . . ?
C12 C4 H1 119.2 . . ?
C8 C4 H1 119.2 . . ?
C6 C5 C6 121.16(16) . 9_645 ?
C6 C5 C3 119.30(15) . . ?
C6 C5 C3 119.54(15) 9_645 . ?
C5 C6 C5 118.84(16) . 5_546 ?
C5 C6 C7 121.49(15) . . ?
C5 C6 C7 119.67(15) 5_546 . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C16 C8 C4 118.4(2) . . ?
C16 C8 C15 121.1(2) . . ?
C4 C8 C15 120.4(2) . . ?
C10 C9 C12 121.56(18) . . ?
C10 C9 N1 119.70(16) . . ?
C12 C9 N1 118.63(17) . . ?
C9 C10 C16 118.4(2) . . ?
C9 C10 H10A 120.8 . . ?
C16 C10 H10A 120.8 . . ?
C4 C12 C9 118.5(2) . . ?
C4 C12 H12A 120.8 . . ?
C9 C12 H12A 120.8 . . ?
C8 C15 H15A 109.5 . . ?
C8 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C8 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C8 C16 C10 121.5(2) . . ?
C8 C16 H16A 119.2 . . ?
C10 C16 H16A 119.2 . . ?
Cl2 Zn1 Cl1 111.503(16) . 9_645 ?
Cl2 Zn1 Cl1 111.503(16) . . ?
Cl1 Zn1 Cl1 107.365(17) 9_645 . ?
Cl2 Zn1 Cl1 111.503(16) . 5_546 ?
Cl1 Zn1 Cl1 107.365(17) 9_645 5_546 ?
Cl1 Zn1 Cl1 107.365(17) . 5_546 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C3 C5 142.89(15) . . . . ?
N1 C3 C5 C6 -82.92(19) . . . . ?
N1 C3 C5 C6 97.52(18) . . . 9_645 ?
C6 C5 C6 C5 0.8(3) 9_645 . . 5_546 ?
C3 C5 C6 C5 -178.76(11) . . . 5_546 ?
C6 C5 C6 C7 -179.10(12) 9_645 . . . ?
C3 C5 C6 C7 1.4(2) . . . . ?
C12 C4 C8 C16 3.8(4) . . . . ?
C12 C4 C8 C15 -178.0(3) . . . . ?
C3 N1 C9 C10 -118.3(2) . . . . ?
C3 N1 C9 C12 57.8(2) . . . . ?
C12 C9 C10 C16 3.4(4) . . . . ?
N1 C9 C10 C16 179.3(2) . . . . ?
C8 C4 C12 C9 -0.9(4) . . . . ?
C10 C9 C12 C4 -2.7(3) . . . . ?
N1 C9 C12 C4 -178.7(2) . . . . ?
C4 C8 C16 C10 -3.1(4) . . . . ?
C15 C8 C16 C10 178.8(3) . . . . ?
C9 C10 C16 C8 -0.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.043
####################################################################### 
# 
# 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_ZnCl4-10
_database_code_depnum_ccdc_archive 'CCDC 1406464'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H30 Cl5 N3 O0 Zn'
_chemical_formula_weight         639.18

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'
Cl Cl 0.1484 0.1585 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.428(8)
_cell_length_b                   11.382(8)
_cell_length_c                   14.421(11)
_cell_angle_alpha                86.257(8)
_cell_angle_beta                 74.387(7)
_cell_angle_gamma                62.935(7)
_cell_volume                     1464.7(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.150
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9145
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6446
_reflns_number_gt                5568
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0468P)²+0.7054P] 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         6446
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0933
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
N1 N 0.06172(19) 0.45790(17) 0.19796(13) 0.0330(4) Uani 1 1 d . . .
H1 H 0.1000 0.5160 0.1939 0.040 Uiso 1 1 d R . .
H3 H -0.0239 0.5081 0.1833 0.040 Uiso 1 1 d R . .
N2 N 0.59486(19) -0.16267(17) 0.20902(13) 0.0322(4) Uani 1 1 d . . .
H2 H 0.6632 -0.1441 0.2237 0.039 Uiso 1 1 d R . .
H4 H 0.6414 -0.2552 0.1985 0.039 Uiso 1 1 d R . .
N3 N 0.7368(2) 0.28068(18) 0.15277(15) 0.0389(4) Uani 1 1 d . . .
H5 H 0.7784 0.3419 0.1377 0.047 Uiso 1 1 d R . .
H6 H 0.8165 0.1973 0.1476 0.047 Uiso 1 1 d R . .
C1 C 0.3062(2) 0.2613(2) 0.11934(14) 0.0287(4) Uani 1 1 d . . .
C2 C 0.4081(2) 0.3127(2) 0.10193(15) 0.0311(4) Uani 1 1 d . . .
H2A H 0.3749 0.4030 0.0958 0.037 Uiso 1 1 calc R . .
C3 C 0.5590(2) 0.2307(2) 0.09349(15) 0.0311(4) Uani 1 1 d . . .
C4 C 0.6089(2) 0.0951(2) 0.09887(15) 0.0319(4) Uani 1 1 d . . .
H4A H 0.7102 0.0395 0.0909 0.038 Uiso 1 1 calc R . .
C5 C 0.5085(2) 0.0422(2) 0.11617(14) 0.0297(4) Uani 1 1 d . . .
C6 C 0.3572(2) 0.1260(2) 0.12783(14) 0.0301(4) Uani 1 1 d . . .
H6A H 0.2894 0.0912 0.1414 0.036 Uiso 1 1 calc R . .
C7 C 0.1466(2) 0.3496(2) 0.11798(16) 0.0358(5) Uani 1 1 d . . .
H7A H 0.1464 0.3896 0.0565 0.043 Uiso 1 1 calc R . .
H7B H 0.0950 0.2959 0.1231 0.043 Uiso 1 1 calc R . .
C8 C 0.5657(3) -0.1056(2) 0.11489(16) 0.0352(5) Uani 1 1 d . . .
H8A H 0.4930 -0.1272 0.1003 0.042 Uiso 1 1 calc R . .
H8B H 0.6577 -0.1469 0.0637 0.042 Uiso 1 1 calc R . .
C9 C 0.6654(3) 0.2902(3) 0.07228(18) 0.0424(5) Uani 1 1 d . . .
H9A H 0.6119 0.3825 0.0603 0.051 Uiso 1 1 calc R . .
H9B H 0.7436 0.2457 0.0139 0.051 Uiso 1 1 calc R . .
C10 C 0.0373(2) 0.4106(2) 0.29521(16) 0.0341(4) Uani 1 1 d . . .
C12 C 0.1299(3) 0.3986(3) 0.35095(19) 0.0475(6) Uani 1 1 d . . .
H12A H 0.2082 0.4203 0.3279 0.057 Uiso 1 1 calc R . .
C13 C 0.1041(4) 0.3534(3) 0.4426(2) 0.0596(7) Uani 1 1 d . . .
H13A H 0.1654 0.3455 0.4814 0.071 Uiso 1 1 calc R . .
C14 C -0.0103(4) 0.3202(3) 0.4766(2) 0.0585(7) Uani 1 1 d . . .
H14A H -0.0265 0.2904 0.5382 0.070 Uiso 1 1 calc R . .
C15 C -0.1003(4) 0.3310(4) 0.4198(2) 0.0641(8) Uani 1 1 d . . .
H15A H -0.1769 0.3071 0.4426 0.077 Uiso 1 1 calc R . .
C16 C -0.0784(3) 0.3774(3) 0.3286(2) 0.0555(7) Uani 1 1 d . . .
H16A H -0.1407 0.3860 0.2903 0.067 Uiso 1 1 calc R . .
C17 C 0.4616(2) -0.1172(2) 0.29108(16) 0.0344(5) Uani 1 1 d . . .
C18 C 0.4395(3) -0.0256(2) 0.35893(18) 0.0452(6) Uani 1 1 d . . .
H18A H 0.5088 0.0064 0.3535 0.054 Uiso 1 1 calc R . .
C19 C 0.3121(3) 0.0179(3) 0.4353(2) 0.0622(8) Uani 1 1 d . . .
H19A H 0.2960 0.0787 0.4826 0.075 Uiso 1 1 calc R . .
C20 C 0.2102(4) -0.0278(4) 0.4418(3) 0.0754(10) Uani 1 1 d . . .
H20A H 0.1246 0.0022 0.4934 0.091 Uiso 1 1 calc R . .
C21 C 0.2326(4) -0.1181(4) 0.3724(3) 0.0743(10) Uani 1 1 d . . .
H21A H 0.1619 -0.1481 0.3771 0.089 Uiso 1 1 calc R . .
C22 C 0.3599(3) -0.1640(3) 0.2960(2) 0.0540(7) Uani 1 1 d . . .
H22A H 0.3764 -0.2251 0.2489 0.065 Uiso 1 1 calc R . .
C23 C 0.6376(3) 0.3109(2) 0.25129(18) 0.0390(5) Uani 1 1 d . . .
C24 C 0.5306(3) 0.4394(3) 0.2788(2) 0.0480(6) Uani 1 1 d . . .
H24A H 0.5194 0.5050 0.2353 0.058 Uiso 1 1 calc R . .
C25 C 0.4402(3) 0.4688(3) 0.3722(2) 0.0621(8) Uani 1 1 d . . .
H25A H 0.3679 0.5554 0.3918 0.075 Uiso 1 1 calc R . .
C26 C 0.4553(4) 0.3725(4) 0.4365(2) 0.0680(9) Uani 1 1 d . . .
H26A H 0.3948 0.3938 0.4995 0.082 Uiso 1 1 calc R . .
C27 C 0.5607(5) 0.2438(4) 0.4070(3) 0.0790(10) Uani 1 1 d . . .
H27A H 0.5694 0.1778 0.4501 0.095 Uiso 1 1 calc R . .
C28 C 0.6538(4) 0.2119(3) 0.3138(2) 0.0612(8) Uani 1 1 d . . .
H28A H 0.7257 0.1252 0.2940 0.073 Uiso 1 1 calc R . .
Zn1 Zn 0.01498(3) 0.82222(2) 0.179698(19) 0.03482(9) Uani 1 1 d . . .
Cl1 Cl -0.16753(7) 0.83506(8) 0.31346(5) 0.05801(19) Uani 1 1 d . . .
Cl2 Cl 0.03731(8) 1.01036(7) 0.15780(8) 0.0696(2) Uani 1 1 d . . .
Cl3 Cl 0.22892(7) 0.64742(6) 0.19470(6) 0.05342(18) Uani 1 1 d . . .
Cl4 Cl -0.03751(7) 0.76220(8) 0.05472(5) 0.05698(18) Uani 1 1 d . . .
Cl5 Cl 0.76632(6) 0.54480(5) 0.13174(4) 0.03951(13) 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
N1 C10 1.468(3) . ?
N1 C7 1.509(3) . ?
N1 H1 0.9076 . ?
N1 H3 0.8883 . ?
N2 C17 1.463(3) . ?
N2 C8 1.511(3) . ?
N2 H2 0.9063 . ?
N2 H4 0.9403 . ?
N3 C23 1.468(3) . ?
N3 C9 1.513(3) . ?
N3 H5 0.9620 . ?
N3 H6 0.9247 . ?
C1 C2 1.391(3) . ?
C1 C6 1.391(3) . ?
C1 C7 1.508(3) . ?
C2 C3 1.392(3) . ?
C2 H2A 0.9300 . ?
C3 C4 1.390(3) . ?
C3 C9 1.502(3) . ?
C4 C5 1.391(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.392(3) . ?
C5 C8 1.507(3) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C12 1.372(3) . ?
C10 C16 1.382(3) . ?
C12 C13 1.389(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.370(4) . ?
C13 H13A 0.9300 . ?
C14 C15 1.364(4) . ?
C14 H14A 0.9300 . ?
C15 C16 1.386(4) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C17 C22 1.371(3) . ?
C17 C18 1.375(3) . ?
C18 C19 1.381(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.361(5) . ?
C19 H19A 0.9300 . ?
C20 C21 1.379(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.381(4) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 C24 1.376(3) . ?
C23 C28 1.374(4) . ?
C24 C25 1.380(4) . ?
C24 H24A 0.9300 . ?
C25 C26 1.369(5) . ?
C25 H25A 0.9300 . ?
C26 C27 1.378(5) . ?
C26 H26A 0.9300 . ?
C27 C28 1.386(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Zn1 Cl4 2.2465(14) . ?
Zn1 Cl2 2.2507(17) . ?
Zn1 Cl3 2.2687(14) . ?
Zn1 Cl1 2.2742(14) . ?

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
C10 N1 C7 114.34(18) . . ?
C10 N1 H1 111.9 . . ?
C7 N1 H1 113.0 . . ?
C10 N1 H3 111.9 . . ?
C7 N1 H3 103.8 . . ?
H1 N1 H3 100.8 . . ?
C17 N2 C8 114.43(17) . . ?
C17 N2 H2 108.7 . . ?
C8 N2 H2 110.2 . . ?
C17 N2 H4 111.1 . . ?
C8 N2 H4 106.9 . . ?
H2 N2 H4 105.1 . . ?
C23 N3 C9 116.39(18) . . ?
C23 N3 H5 110.3 . . ?
C9 N3 H5 104.2 . . ?
C23 N3 H6 110.1 . . ?
C9 N3 H6 108.6 . . ?
H5 N3 H6 106.7 . . ?
C2 C1 C6 119.07(18) . . ?
C2 C1 C7 119.8(2) . . ?
C6 C1 C7 120.78(19) . . ?
C1 C2 C3 120.9(2) . . ?
C1 C2 H2A 119.6 . . ?
C3 C2 H2A 119.6 . . ?
C4 C3 C2 119.33(19) . . ?
C4 C3 C9 121.59(19) . . ?
C2 C3 C9 119.0(2) . . ?
C5 C4 C3 120.46(19) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C4 C5 C6 119.5(2) . . ?
C4 C5 C8 119.80(19) . . ?
C6 C5 C8 120.56(19) . . ?
C5 C6 C1 120.68(18) . . ?
C5 C6 H6A 119.7 . . ?
C1 C6 H6A 119.7 . . ?
N1 C7 C1 113.69(17) . . ?
N1 C7 H7A 108.8 . . ?
C1 C7 H7A 108.8 . . ?
N1 C7 H7B 108.8 . . ?
C1 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N2 C8 C5 113.48(17) . . ?
N2 C8 H8A 108.9 . . ?
C5 C8 H8A 108.9 . . ?
N2 C8 H8B 108.9 . . ?
C5 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C3 C9 N3 113.65(19) . . ?
C3 C9 H9A 108.8 . . ?
N3 C9 H9A 108.8 . . ?
C3 C9 H9B 108.8 . . ?
N3 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C12 C10 C16 121.1(2) . . ?
C12 C10 N1 119.9(2) . . ?
C16 C10 N1 119.0(2) . . ?
C10 C12 C13 118.5(2) . . ?
C10 C12 H12A 120.8 . . ?
C13 C12 H12A 120.8 . . ?
C14 C13 C12 121.0(3) . . ?
C14 C13 H13A 119.5 . . ?
C12 C13 H13A 119.5 . . ?
C15 C14 C13 119.8(3) . . ?
C15 C14 H14A 120.1 . . ?
C13 C14 H14A 120.1 . . ?
C14 C15 C16 120.5(3) . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 H15A 119.8 . . ?
C10 C16 C15 119.1(2) . . ?
C10 C16 H16A 120.4 . . ?
C15 C16 H16A 120.4 . . ?
C22 C17 C18 122.1(2) . . ?
C22 C17 N2 118.8(2) . . ?
C18 C17 N2 119.1(2) . . ?
C17 C18 C19 118.5(3) . . ?
C17 C18 H18A 120.8 . . ?
C19 C18 H18A 120.8 . . ?
C20 C19 C18 120.4(3) . . ?
C20 C19 H19A 119.8 . . ?
C18 C19 H19A 119.8 . . ?
C19 C20 C21 120.5(3) . . ?
C19 C20 H20A 119.7 . . ?
C21 C20 H20A 119.7 . . ?
C20 C21 C22 120.1(3) . . ?
C20 C21 H21A 120.0 . . ?
C22 C21 H21A 120.0 . . ?
C17 C22 C21 118.4(3) . . ?
C17 C22 H22A 120.8 . . ?
C21 C22 H22A 120.8 . . ?
C24 C23 C28 121.6(3) . . ?
C24 C23 N3 118.6(2) . . ?
C28 C23 N3 119.9(2) . . ?
C23 C24 C25 118.7(3) . . ?
C23 C24 H24A 120.7 . . ?
C25 C24 H24A 120.7 . . ?
C26 C25 C24 121.0(3) . . ?
C26 C25 H25A 119.5 . . ?
C24 C25 H25A 119.5 . . ?
C27 C26 C25 119.6(3) . . ?
C27 C26 H26A 120.2 . . ?
C25 C26 H26A 120.2 . . ?
C26 C27 C28 120.6(3) . . ?
C26 C27 H27A 119.7 . . ?
C28 C27 H27A 119.7 . . ?
C23 C28 C27 118.6(3) . . ?
C23 C28 H28A 120.7 . . ?
C27 C28 H28A 120.7 . . ?
Cl4 Zn1 Cl2 112.45(4) . . ?
Cl4 Zn1 Cl3 105.24(5) . . ?
Cl2 Zn1 Cl3 112.47(6) . . ?
Cl4 Zn1 Cl1 106.41(6) . . ?
Cl2 Zn1 Cl1 113.35(4) . . ?
Cl3 Zn1 Cl1 106.31(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.3(3) . . . . ?
C7 C1 C2 C3 -173.71(19) . . . . ?
C1 C2 C3 C4 2.5(3) . . . . ?
C1 C2 C3 C9 178.5(2) . . . . ?
C2 C3 C4 C5 -2.4(3) . . . . ?
C9 C3 C4 C5 -178.3(2) . . . . ?
C3 C4 C5 C6 0.2(3) . . . . ?
C3 C4 C5 C8 175.74(19) . . . . ?
C4 C5 C6 C1 2.0(3) . . . . ?
C8 C5 C6 C1 -173.48(19) . . . . ?
C2 C1 C6 C5 -2.0(3) . . . . ?
C7 C1 C6 C5 171.35(19) . . . . ?
C10 N1 C7 C1 -65.9(2) . . . . ?
C2 C1 C7 N1 -65.8(3) . . . . ?
C6 C1 C7 N1 120.9(2) . . . . ?
C17 N2 C8 C5 63.8(2) . . . . ?
C4 C5 C8 N2 82.9(2) . . . . ?
C6 C5 C8 N2 -101.5(2) . . . . ?
C4 C3 C9 N3 -68.6(3) . . . . ?
C2 C3 C9 N3 115.5(2) . . . . ?
C23 N3 C9 C3 -43.1(3) . . . . ?
C7 N1 C10 C12 98.4(2) . . . . ?
C7 N1 C10 C16 -80.9(3) . . . . ?
C16 C10 C12 C13 -0.6(4) . . . . ?
N1 C10 C12 C13 -179.9(2) . . . . ?
C10 C12 C13 C14 0.6(5) . . . . ?
C12 C13 C14 C15 0.3(5) . . . . ?
C13 C14 C15 C16 -1.0(5) . . . . ?
C12 C10 C16 C15 -0.1(4) . . . . ?
N1 C10 C16 C15 179.1(3) . . . . ?
C14 C15 C16 C10 1.0(5) . . . . ?
C8 N2 C17 C22 72.9(3) . . . . ?
C8 N2 C17 C18 -104.8(2) . . . . ?
C22 C17 C18 C19 1.5(4) . . . . ?
N2 C17 C18 C19 179.1(2) . . . . ?
C17 C18 C19 C20 -1.1(4) . . . . ?
C18 C19 C20 C21 0.1(5) . . . . ?
C19 C20 C21 C22 0.6(6) . . . . ?
C18 C17 C22 C21 -0.8(4) . . . . ?
N2 C17 C22 C21 -178.4(3) . . . . ?
C20 C21 C22 C17 -0.3(5) . . . . ?
C9 N3 C23 C24 -69.2(3) . . . . ?
C9 N3 C23 C28 111.2(3) . . . . ?
C28 C23 C24 C25 1.5(4) . . . . ?
N3 C23 C24 C25 -178.1(2) . . . . ?
C23 C24 C25 C26 -0.5(4) . . . . ?
C24 C25 C26 C27 -1.0(5) . . . . ?
C25 C26 C27 C28 1.6(5) . . . . ?
C24 C23 C28 C27 -0.9(4) . . . . ?
N3 C23 C28 C27 178.6(3) . . . . ?
C26 C27 C28 C23 -0.7(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.103
####################################################################### 
# 
# 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_CdCl4-H2O-11
_database_code_depnum_ccdc_archive 'CCDC 1406465'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H37 Cd Cl5 N3 O'
_chemical_formula_weight         745.29

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'
Cd Cd -0.8075 1.2024 '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'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5477(7)
_cell_length_b                   11.5561(9)
_cell_length_c                   16.7666(13)
_cell_angle_alpha                94.5640(10)
_cell_angle_beta                 90.6690(10)
_cell_angle_gamma                92.3010(10)
_cell_volume                     1649.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             758
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10426
_diffrn_reflns_av_R_equivalents  0.0114
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         27.57
_reflns_number_total             7329
_reflns_number_gt                6416
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0341P)²+2.8280P] 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         7329
_refine_ls_number_parameters     364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0962
_refine_ls_wR_factor_gt          0.0923
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N11 N 1.0333(3) 0.2918(2) 0.08168(14) 0.0357(5) Uani 1 1 d . . .
H11A H 1.0375 0.3614 0.0919 0.043 Uiso 1 1 d R . .
H11B H 1.0363 0.2671 0.1307 0.043 Uiso 1 1 d R . .
N19 N 0.8515(3) -0.0057(2) 0.29819(16) 0.0450(6) Uani 1 1 d . . .
H19A H 0.9151 0.0499 0.2800 0.054 Uiso 1 1 d R . .
H19B H 0.9080 -0.0615 0.2889 0.054 Uiso 1 1 d R . .
N27 N 0.5021(3) 0.4355(2) 0.30473(16) 0.0392(6) Uani 1 1 d . . .
H27A H 0.4820 0.5120 0.2967 0.047 Uiso 1 1 d R . .
H27B H 0.6037 0.4340 0.3050 0.047 Uiso 1 1 d R . .
C1 C 0.5688(3) 0.1635(2) 0.23321(16) 0.0313(6) Uani 1 1 d . . .
C2 C 0.5587(3) 0.2720(2) 0.20213(16) 0.0308(5) Uani 1 1 d . . .
C3 C 0.6589(3) 0.3046(2) 0.14130(17) 0.0344(6) Uani 1 1 d . . .
C4 C 0.7625(3) 0.2242(3) 0.10779(16) 0.0328(6) Uani 1 1 d . . .
C5 C 0.7714(3) 0.1143(2) 0.13696(17) 0.0337(6) Uani 1 1 d . . .
C6 C 0.6799(3) 0.0868(2) 0.20194(17) 0.0327(6) Uani 1 1 d . . .
C7 C 0.4602(4) 0.1271(3) 0.29810(19) 0.0435(7) Uani 1 1 d . . .
H7A H 0.3828 0.1842 0.3077 0.065 Uiso 1 1 calc R . .
H7B H 0.5195 0.1205 0.3464 0.065 Uiso 1 1 calc R . .
H7C H 0.4094 0.0534 0.2814 0.065 Uiso 1 1 calc R . .
C8 C 0.8839(4) 0.0287(3) 0.0998(2) 0.0495(8) Uani 1 1 d . . .
H8A H 0.8502 -0.0487 0.1105 0.074 Uiso 1 1 calc R . .
H8B H 0.9869 0.0460 0.1222 0.074 Uiso 1 1 calc R . .
H8C H 0.8861 0.0345 0.0430 0.074 Uiso 1 1 calc R . .
C9 C 0.6549(5) 0.4248(3) 0.1123(2) 0.0575(10) Uani 1 1 d . . .
H9A H 0.7592 0.4511 0.1000 0.086 Uiso 1 1 calc R . .
H9B H 0.6133 0.4771 0.1533 0.086 Uiso 1 1 calc R . .
H9C H 0.5898 0.4227 0.0651 0.086 Uiso 1 1 calc R . .
C10 C 0.8741(3) 0.2560(3) 0.04364(18) 0.0418(7) Uani 1 1 d . . .
H10A H 0.8341 0.3197 0.0161 0.050 Uiso 1 1 calc R . .
H10B H 0.8844 0.1901 0.0048 0.050 Uiso 1 1 calc R . .
C12 C 1.1696(3) 0.2575(2) 0.03443(18) 0.0363(6) Uani 1 1 d . . .
C13 C 1.2695(4) 0.1809(3) 0.0649(2) 0.0458(7) Uani 1 1 d . . .
H13A H 1.2505 0.1512 0.1140 0.055 Uiso 1 1 calc R . .
C14 C 1.3990(4) 0.1491(4) 0.0205(3) 0.0594(10) Uani 1 1 d . . .
H14A H 1.4680 0.0973 0.0397 0.071 Uiso 1 1 calc R . .
C15 C 1.4256(4) 0.1938(4) -0.0518(3) 0.0646(12) Uani 1 1 d . . .
H15A H 1.5133 0.1729 -0.0810 0.078 Uiso 1 1 calc R . .
C16 C 1.3233(5) 0.2696(3) -0.0815(2) 0.0621(11) Uani 1 1 d . . .
H16A H 1.3419 0.2990 -0.1307 0.074 Uiso 1 1 calc R . .
C17 C 1.1928(4) 0.3020(3) -0.0382(2) 0.0494(8) Uani 1 1 d . . .
H17A H 1.1227 0.3527 -0.0579 0.059 Uiso 1 1 calc R . .
C18 C 0.7103(4) -0.0233(3) 0.2410(2) 0.0445(7) Uani 1 1 d . . .
H18A H 0.7297 -0.0851 0.2001 0.053 Uiso 1 1 calc R . .
H18B H 0.6185 -0.0463 0.2703 0.053 Uiso 1 1 calc R . .
C20 C 0.8174(4) 0.0209(3) 0.3831(2) 0.0449(7) Uani 1 1 d . . .
C21 C 0.7367(7) -0.0611(4) 0.4225(3) 0.0779(14) Uani 1 1 d . . .
H21A H 0.7021 -0.1313 0.3959 0.093 Uiso 1 1 calc R . .
C22 C 0.7078(8) -0.0370(4) 0.5027(3) 0.0948(18) Uani 1 1 d . . .
H22A H 0.6529 -0.0919 0.5302 0.114 Uiso 1 1 calc R . .
C23 C 0.7579(6) 0.0653(5) 0.5424(3) 0.0808(14) Uani 1 1 d . . .
H23A H 0.7403 0.0792 0.5969 0.097 Uiso 1 1 calc R . .
C24 C 0.8336(7) 0.1463(5) 0.5017(3) 0.0892(16) Uani 1 1 d . . .
H24A H 0.8644 0.2176 0.5280 0.107 Uiso 1 1 calc R . .
C25 C 0.8660(6) 0.1243(4) 0.4211(2) 0.0740(13) Uani 1 1 d . . .
H25A H 0.9203 0.1796 0.3936 0.089 Uiso 1 1 calc R . .
C26 C 0.4391(3) 0.3566(3) 0.23334(18) 0.0372(6) Uani 1 1 d . . .
H26A H 0.3463 0.3135 0.2491 0.045 Uiso 1 1 calc R . .
H26B H 0.4091 0.4039 0.1909 0.045 Uiso 1 1 calc R . .
C28 C 0.4325(4) 0.4109(3) 0.3810(2) 0.0464(8) Uani 1 1 d . . .
C29 C 0.2769(5) 0.4346(4) 0.3923(3) 0.0684(12) Uani 1 1 d . . .
H29A H 0.2181 0.4670 0.3535 0.082 Uiso 1 1 calc R . .
C30 C 0.2122(8) 0.4075(5) 0.4651(4) 0.105(2) Uani 1 1 d . . .
H30A H 0.1076 0.4212 0.4752 0.126 Uiso 1 1 calc R . .
C31 C 0.3034(12) 0.3602(5) 0.5220(4) 0.117(3) Uani 1 1 d . . .
H31A H 0.2595 0.3434 0.5705 0.141 Uiso 1 1 calc R . .
C32 C 0.4530(10) 0.3385(4) 0.5083(3) 0.101(2) Uani 1 1 d . . .
H32A H 0.5118 0.3058 0.5472 0.121 Uiso 1 1 calc R . .
C33 C 0.5221(6) 0.3636(3) 0.4375(2) 0.0669(11) Uani 1 1 d . . .
H33A H 0.6268 0.3489 0.4283 0.080 Uiso 1 1 calc R . .
Cd1 Cd 0.19797(3) 0.71829(2) 0.214974(14) 0.04201(8) Uani 1 1 d . . .
Cl1 Cl 0.45280(11) 0.69866(8) 0.28264(6) 0.0559(2) Uani 1 1 d . . .
Cl2 Cl 0.16701(13) 0.54794(7) 0.11700(6) 0.0621(3) Uani 1 1 d . . .
Cl3 Cl -0.03616(14) 0.72186(10) 0.29862(8) 0.0777(3) Uani 1 1 d . . .
Cl4 Cl 0.22130(14) 0.90499(8) 0.15894(8) 0.0755(3) Uani 1 1 d . . .
O1W O 0.8308(3) 0.4420(3) 0.3105(2) 0.0825(10) Uani 1 1 d . . .
H2 H 0.8612 0.5009 0.3230 0.124 Uiso 1 1 d R . .
Cl5 Cl 0.05212(9) 0.23004(8) 0.25810(5) 0.04788(19) 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
N11 C12 1.466(3) . ?
N11 C10 1.524(4) . ?
N11 H11A 0.8076 . ?
N11 H11B 0.8923 . ?
N19 C20 1.468(4) . ?
N19 C18 1.530(4) . ?
N19 H19A 0.8993 . ?
N19 H19B 0.8265 . ?
N27 C28 1.461(4) . ?
N27 C26 1.525(4) . ?
N27 H27A 0.9280 . ?
N27 H27B 0.8695 . ?
C1 C2 1.401(4) . ?
C1 C6 1.403(4) . ?
C1 C7 1.512(4) . ?
C2 C3 1.404(4) . ?
C2 C26 1.512(4) . ?
C3 C4 1.400(4) . ?
C3 C9 1.509(4) . ?
C4 C5 1.402(4) . ?
C4 C10 1.503(4) . ?
C5 C6 1.398(4) . ?
C5 C8 1.511(4) . ?
C6 C18 1.507(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C13 1.377(5) . ?
C12 C17 1.373(5) . ?
C13 C14 1.387(5) . ?
C13 H13A 0.9300 . ?
C14 C15 1.374(6) . ?
C14 H14A 0.9300 . ?
C15 C16 1.378(6) . ?
C15 H15A 0.9300 . ?
C16 C17 1.386(5) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C20 C25 1.356(5) . ?
C20 C21 1.366(5) . ?
C21 C22 1.378(6) . ?
C21 H21A 0.9300 . ?
C22 C23 1.361(7) . ?
C22 H22A 0.9300 . ?
C23 C24 1.351(7) . ?
C23 H23A 0.9300 . ?
C24 C25 1.388(6) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C28 C33 1.371(6) . ?
C28 C29 1.381(5) . ?
C29 C30 1.398(7) . ?
C29 H29A 0.9300 . ?
C30 C31 1.384(10) . ?
C30 H30A 0.9300 . ?
C31 C32 1.333(10) . ?
C31 H31A 0.9300 . ?
C32 C33 1.378(7) . ?
C32 H32A 0.9300 . ?
C33 H33A 0.9300 . ?
Cd1 Cl4 2.4228(10) . ?
Cd1 Cl3 2.4570(10) . ?
Cd1 Cl2 2.4653(9) . ?
Cd1 Cl1 2.4711(9) . ?
O1W H2 0.7328 . ?

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
C12 N11 C10 115.7(2) . . ?
C12 N11 H11A 109.6 . . ?
C10 N11 H11A 108.8 . . ?
C12 N11 H11B 112.4 . . ?
C10 N11 H11B 108.4 . . ?
H11A N11 H11B 100.9 . . ?
C20 N19 C18 116.5(3) . . ?
C20 N19 H19A 110.8 . . ?
C18 N19 H19A 107.5 . . ?
C20 N19 H19B 114.7 . . ?
C18 N19 H19B 107.4 . . ?
H19A N19 H19B 98.3 . . ?
C28 N27 C26 114.2(2) . . ?
C28 N27 H27A 106.9 . . ?
C26 N27 H27A 109.3 . . ?
C28 N27 H27B 113.5 . . ?
C26 N27 H27B 108.3 . . ?
H27A N27 H27B 104.0 . . ?
C2 C1 C6 118.9(2) . . ?
C2 C1 C7 121.3(3) . . ?
C6 C1 C7 119.8(3) . . ?
C1 C2 C3 120.9(3) . . ?
C1 C2 C26 120.6(2) . . ?
C3 C2 C26 118.5(3) . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 C9 120.3(3) . . ?
C2 C3 C9 120.5(3) . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 C10 121.0(3) . . ?
C5 C4 C10 118.4(3) . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 C8 120.9(3) . . ?
C4 C5 C8 119.6(3) . . ?
C5 C6 C1 120.7(3) . . ?
C5 C6 C18 118.6(3) . . ?
C1 C6 C18 120.6(3) . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C9 H9A 109.5 . . ?
C3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 N11 109.2(2) . . ?
C4 C10 H10A 109.8 . . ?
N11 C10 H10A 109.8 . . ?
C4 C10 H10B 109.8 . . ?
N11 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
C13 C12 C17 122.5(3) . . ?
C13 C12 N11 118.3(3) . . ?
C17 C12 N11 119.2(3) . . ?
C12 C13 C14 118.3(3) . . ?
C12 C13 H13A 120.9 . . ?
C14 C13 H13A 120.9 . . ?
C15 C14 C13 120.2(4) . . ?
C15 C14 H14A 119.9 . . ?
C13 C14 H14A 119.9 . . ?
C14 C15 C16 120.5(3) . . ?
C14 C15 H15A 119.7 . . ?
C16 C15 H15A 119.7 . . ?
C15 C16 C17 120.2(4) . . ?
C15 C16 H16A 119.9 . . ?
C17 C16 H16A 119.9 . . ?
C12 C17 C16 118.3(4) . . ?
C12 C17 H17A 120.8 . . ?
C16 C17 H17A 120.8 . . ?
C6 C18 N19 110.7(2) . . ?
C6 C18 H18A 109.5 . . ?
N19 C18 H18A 109.5 . . ?
C6 C18 H18B 109.5 . . ?
N19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C25 C20 C21 121.3(4) . . ?
C25 C20 N19 120.4(3) . . ?
C21 C20 N19 118.3(3) . . ?
C20 C21 C22 118.3(4) . . ?
C20 C21 H21A 120.9 . . ?
C22 C21 H21A 120.9 . . ?
C23 C22 C21 121.5(4) . . ?
C23 C22 H22A 119.3 . . ?
C21 C22 H22A 119.3 . . ?
C24 C23 C22 119.2(4) . . ?
C24 C23 H23A 120.4 . . ?
C22 C23 H23A 120.4 . . ?
C23 C24 C25 120.7(4) . . ?
C23 C24 H24A 119.6 . . ?
C25 C24 H24A 119.6 . . ?
C20 C25 C24 119.0(4) . . ?
C20 C25 H25A 120.5 . . ?
C24 C25 H25A 120.5 . . ?
C2 C26 N27 112.0(2) . . ?
C2 C26 H26A 109.2 . . ?
N27 C26 H26A 109.2 . . ?
C2 C26 H26B 109.2 . . ?
N27 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?
C33 C28 C29 122.8(4) . . ?
C33 C28 N27 119.3(3) . . ?
C29 C28 N27 117.9(3) . . ?
C28 C29 C30 116.7(5) . . ?
C28 C29 H29A 121.6 . . ?
C30 C29 H29A 121.6 . . ?
C31 C30 C29 120.2(6) . . ?
C31 C30 H30A 119.9 . . ?
C29 C30 H30A 119.9 . . ?
C32 C31 C30 120.9(5) . . ?
C32 C31 H31A 119.5 . . ?
C30 C31 H31A 119.5 . . ?
C31 C32 C33 121.0(6) . . ?
C31 C32 H32A 119.5 . . ?
C33 C32 H32A 119.5 . . ?
C28 C33 C32 118.3(5) . . ?
C28 C33 H33A 120.8 . . ?
C32 C33 H33A 120.8 . . ?
Cl4 Cd1 Cl3 106.77(4) . . ?
Cl4 Cd1 Cl2 115.62(4) . . ?
Cl3 Cd1 Cl2 107.51(4) . . ?
Cl4 Cd1 Cl1 104.50(4) . . ?
Cl3 Cd1 Cl1 117.32(4) . . ?
Cl2 Cd1 Cl1 105.53(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.7(4) . . . . ?
C7 C1 C2 C3 -179.3(3) . . . . ?
C6 C1 C2 C26 179.2(2) . . . . ?
C7 C1 C2 C26 0.6(4) . . . . ?
C1 C2 C3 C4 4.4(4) . . . . ?
C26 C2 C3 C4 -175.5(3) . . . . ?
C1 C2 C3 C9 -175.6(3) . . . . ?
C26 C2 C3 C9 4.5(4) . . . . ?
C2 C3 C4 C5 -2.9(4) . . . . ?
C9 C3 C4 C5 177.2(3) . . . . ?
C2 C3 C4 C10 -178.8(3) . . . . ?
C9 C3 C4 C10 1.2(4) . . . . ?
C3 C4 C5 C6 -2.4(4) . . . . ?
C10 C4 C5 C6 173.7(3) . . . . ?
C3 C4 C5 C8 179.9(3) . . . . ?
C10 C4 C5 C8 -4.1(4) . . . . ?
C4 C5 C6 C1 6.2(4) . . . . ?
C8 C5 C6 C1 -176.1(3) . . . . ?
C4 C5 C6 C18 -170.0(3) . . . . ?
C8 C5 C6 C18 7.7(4) . . . . ?
C2 C1 C6 C5 -4.6(4) . . . . ?
C7 C1 C6 C5 174.0(3) . . . . ?
C2 C1 C6 C18 171.5(3) . . . . ?
C7 C1 C6 C18 -9.9(4) . . . . ?
C3 C4 C10 N11 96.8(3) . . . . ?
C5 C4 C10 N11 -79.2(3) . . . . ?
C12 N11 C10 C4 143.7(3) . . . . ?
C10 N11 C12 C13 -116.3(3) . . . . ?
C10 N11 C12 C17 63.4(4) . . . . ?
C17 C12 C13 C14 0.8(5) . . . . ?
N11 C12 C13 C14 -179.5(3) . . . . ?
C12 C13 C14 C15 0.1(5) . . . . ?
C13 C14 C15 C16 -0.7(6) . . . . ?
C14 C15 C16 C17 0.4(6) . . . . ?
C13 C12 C17 C16 -1.1(5) . . . . ?
N11 C12 C17 C16 179.2(3) . . . . ?
C15 C16 C17 C12 0.4(5) . . . . ?
C5 C6 C18 N19 80.0(3) . . . . ?
C1 C6 C18 N19 -96.1(3) . . . . ?
C20 N19 C18 C6 97.0(3) . . . . ?
C18 N19 C20 C25 -116.4(4) . . . . ?
C18 N19 C20 C21 64.0(4) . . . . ?
C25 C20 C21 C22 -1.1(8) . . . . ?
N19 C20 C21 C22 178.6(5) . . . . ?
C20 C21 C22 C23 -0.1(9) . . . . ?
C21 C22 C23 C24 2.0(10) . . . . ?
C22 C23 C24 C25 -2.7(9) . . . . ?
C21 C20 C25 C24 0.4(7) . . . . ?
N19 C20 C25 C24 -179.2(4) . . . . ?
C23 C24 C25 C20 1.5(9) . . . . ?
C1 C2 C26 N27 88.8(3) . . . . ?
C3 C2 C26 N27 -91.3(3) . . . . ?
C28 N27 C26 C2 -108.8(3) . . . . ?
C26 N27 C28 C33 110.4(3) . . . . ?
C26 N27 C28 C29 -68.4(4) . . . . ?
C33 C28 C29 C30 -0.3(6) . . . . ?
N27 C28 C29 C30 178.4(3) . . . . ?
C28 C29 C30 C31 0.6(7) . . . . ?
C29 C30 C31 C32 -0.8(8) . . . . ?
C30 C31 C32 C33 0.8(8) . . . . ?
C29 C28 C33 C32 0.3(5) . . . . ?
N27 C28 C33 C32 -178.5(3) . . . . ?
C31 C32 C33 C28 -0.5(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         1.430
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.072
####################################################################### 
# 
# 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_CuCl4-H2O-12
_database_code_depnum_ccdc_archive 'CCDC 1406466'
_audit_update_record             
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H37 Cl5 Cu N3 O'
_chemical_formula_weight         696.43

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5878(19)
_cell_length_b                   11.611(3)
_cell_length_c                   16.134(4)
_cell_angle_alpha                93.826(3)
_cell_angle_beta                 92.064(3)
_cell_angle_gamma                90.772(3)
_cell_volume                     1603.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.23
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_max          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9924
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         27.42
_reflns_number_total             6974
_reflns_number_gt                5460
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_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)+(0.0613P)²+2.0609P] 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         6974
_refine_ls_number_parameters     364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1336
_refine_ls_wR_factor_gt          0.1238
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      0.979
_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
N11 N 0.4638(3) 0.2091(2) 0.41895(16) 0.0366(5) Uani 1 1 d . . .
H1 H 0.4552 0.1411 0.4059 0.044 Uiso 1 1 d R . .
H2 H 0.4595 0.2350 0.3670 0.044 Uiso 1 1 d R . .
N19 N 0.6360(3) 0.5055(2) 0.19770(17) 0.0434(6) Uani 1 1 d . . .
H19A H 0.5740 0.4556 0.2117 0.052 Uiso 1 1 d R . .
H19B H 0.5820 0.5709 0.2040 0.052 Uiso 1 1 d R . .
N26 N 1.0006(3) 0.0654(2) 0.19767(17) 0.0415(6) Uani 1 1 d . . .
H26A H 1.0259 -0.0048 0.2104 0.050 Uiso 1 1 d R . .
H26B H 0.9083 0.0639 0.1951 0.050 Uiso 1 1 d R . .
C1 C 0.9219(3) 0.3364(2) 0.26857(17) 0.0310(6) Uani 1 1 d . . .
C2 C 0.9362(3) 0.2280(2) 0.30146(17) 0.0312(6) Uani 1 1 d . . .
C3 C 0.8385(3) 0.1944(2) 0.36330(18) 0.0340(6) Uani 1 1 d . . .
C4 C 0.7328(3) 0.2740(2) 0.39693(17) 0.0330(6) Uani 1 1 d . . .
C5 C 0.7202(3) 0.3833(2) 0.36669(17) 0.0321(6) Uani 1 1 d . . .
C6 C 0.8091(3) 0.4122(2) 0.30021(17) 0.0320(6) Uani 1 1 d . . .
C7 C 1.0266(4) 0.3733(3) 0.2017(2) 0.0418(7) Uani 1 1 d . . .
H7A H 1.1083 0.3184 0.1940 0.063 Uiso 1 1 calc R . .
H7B H 1.0714 0.4480 0.2179 0.063 Uiso 1 1 calc R . .
H7C H 0.9668 0.3770 0.1505 0.063 Uiso 1 1 calc R . .
C8 C 0.6075(4) 0.4683(3) 0.4049(2) 0.0464(8) Uani 1 1 d . . .
H8A H 0.6401 0.5454 0.3948 0.070 Uiso 1 1 calc R . .
H8B H 0.6056 0.4604 0.4637 0.070 Uiso 1 1 calc R . .
H8C H 0.5051 0.4532 0.3804 0.070 Uiso 1 1 calc R . .
C9 C 0.8483(5) 0.0749(3) 0.3945(3) 0.0590(10) Uani 1 1 d . . .
H9A H 0.7479 0.0374 0.3880 0.089 Uiso 1 1 calc R . .
H9B H 0.8808 0.0805 0.4522 0.089 Uiso 1 1 calc R . .
H9C H 0.9225 0.0308 0.3632 0.089 Uiso 1 1 calc R . .
C10 C 0.6218(4) 0.2401(3) 0.4615(2) 0.0432(7) Uani 1 1 d . . .
H10A H 0.6109 0.3036 0.5029 0.052 Uiso 1 1 calc R . .
H10B H 0.6618 0.1744 0.4891 0.052 Uiso 1 1 calc R . .
C12 C 0.3274(3) 0.2446(2) 0.46604(19) 0.0362(6) Uani 1 1 d . . .
C13 C 0.3046(4) 0.1995(3) 0.5415(2) 0.0474(8) Uani 1 1 d . . .
H13A H 0.3747 0.1478 0.5630 0.057 Uiso 1 1 calc R . .
C14 C 0.1738(4) 0.2334(3) 0.5847(2) 0.0551(9) Uani 1 1 d . . .
H14A H 0.1548 0.2032 0.6353 0.066 Uiso 1 1 calc R . .
C15 C 0.0719(4) 0.3117(3) 0.5528(3) 0.0585(10) Uani 1 1 d . . .
H15A H -0.0151 0.3343 0.5821 0.070 Uiso 1 1 calc R . .
C16 C 0.0993(4) 0.3566(3) 0.4774(2) 0.0551(9) Uani 1 1 d . . .
H16A H 0.0309 0.4096 0.4563 0.066 Uiso 1 1 calc R . .
C17 C 0.2278(4) 0.3230(3) 0.4334(2) 0.0451(7) Uani 1 1 d . . .
H17A H 0.2466 0.3529 0.3826 0.054 Uiso 1 1 calc R . .
C18 C 0.7751(4) 0.5229(3) 0.2594(2) 0.0430(7) Uani 1 1 d . . .
H18A H 0.8660 0.5469 0.2306 0.052 Uiso 1 1 calc R . .
H18B H 0.7525 0.5832 0.3016 0.052 Uiso 1 1 calc R . .
C19 C 0.6746(4) 0.4809(3) 0.1104(2) 0.0445(7) Uani 1 1 d . . .
C20 C 0.6378(6) 0.3771(4) 0.0711(3) 0.0716(12) Uani 1 1 d . . .
H20A H 0.5879 0.3203 0.0990 0.086 Uiso 1 1 calc R . .
C21 C 0.6755(7) 0.3564(5) -0.0116(3) 0.0865(15) Uani 1 1 d . . .
H21A H 0.6523 0.2847 -0.0387 0.104 Uiso 1 1 calc R . .
C22 C 0.7450(6) 0.4385(5) -0.0530(3) 0.0775(13) Uani 1 1 d . . .
H22A H 0.7678 0.4250 -0.1087 0.093 Uiso 1 1 calc R . .
C23 C 0.7809(8) 0.5409(5) -0.0119(3) 0.103(2) Uani 1 1 d . . .
H23A H 0.8305 0.5976 -0.0399 0.124 Uiso 1 1 calc R . .
C24 C 0.7465(7) 0.5643(4) 0.0700(3) 0.0841(15) Uani 1 1 d . . .
H24A H 0.7720 0.6356 0.0971 0.101 Uiso 1 1 calc R . .
C25 C 1.0589(3) 0.1458(3) 0.2709(2) 0.0388(7) Uani 1 1 d . . .
H25A H 1.0931 0.0999 0.3161 0.047 Uiso 1 1 calc R . .
H25B H 1.1482 0.1897 0.2545 0.047 Uiso 1 1 calc R . .
C28 C 1.0689(4) 0.0882(3) 0.1189(2) 0.0501(8) Uani 1 1 d . . .
C29 C 1.2248(5) 0.0619(4) 0.1099(3) 0.0719(12) Uani 1 1 d . . .
H29A H 1.2826 0.0283 0.1515 0.086 Uiso 1 1 calc R . .
C30 C 1.2899(8) 0.0881(5) 0.0361(4) 0.110(2) Uani 1 1 d . . .
H30A H 1.3948 0.0736 0.0283 0.132 Uiso 1 1 calc R . .
C31 C 1.2037(12) 0.1348(5) -0.0256(4) 0.125(3) Uani 1 1 d . . .
H31A H 1.2491 0.1497 -0.0753 0.150 Uiso 1 1 calc R . .
C32 C 1.0488(11) 0.1599(4) -0.0141(3) 0.105(2) Uani 1 1 d . . .
H32A H 0.9909 0.1932 -0.0557 0.126 Uiso 1 1 calc R . .
C33 C 0.9797(6) 0.1360(3) 0.0585(3) 0.0709(12) Uani 1 1 d . . .
H33A H 0.8753 0.1519 0.0663 0.085 Uiso 1 1 calc R . .
Cu1 Cu 0.31768(5) 0.78973(3) 0.28037(3) 0.04362(13) Uani 1 1 d . . .
Cl1 Cl 0.06872(10) 0.80987(8) 0.23526(6) 0.0543(2) Uani 1 1 d . . .
Cl2 Cl 0.34818(13) 0.95574(7) 0.36265(7) 0.0655(3) Uani 1 1 d . . .
Cl3 Cl 0.54912(13) 0.78611(10) 0.21914(8) 0.0766(3) Uani 1 1 d . . .
Cl4 Cl 0.30016(15) 0.60623(8) 0.30694(9) 0.0839(4) Uani 1 1 d . . .
O1W O 0.6695(3) 0.0603(3) 0.1903(2) 0.0773(9) Uani 1 1 d . . .
H4 H 0.6291 -0.0206 0.2058 0.116 Uiso 1 1 d R . .
Cl5 Cl 0.44079(9) 0.27540(7) 0.23706(5) 0.0467(2) 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
N11 C12 1.468(4) . ?
N11 C10 1.525(4) . ?
N11 H1 0.8054 . ?
N11 H2 0.9090 . ?
N19 C19 1.469(4) . ?
N19 C18 1.530(4) . ?
N19 H19A 0.8302 . ?
N19 H19B 0.8966 . ?
N26 C28 1.458(4) . ?
N26 C25 1.521(4) . ?
N26 H26A 0.8820 . ?
N26 H26B 0.7916 . ?
C1 C6 1.405(4) . ?
C1 C2 1.403(4) . ?
C1 C7 1.510(4) . ?
C2 C3 1.398(4) . ?
C2 C25 1.505(4) . ?
C3 C4 1.401(4) . ?
C3 C9 1.510(4) . ?
C4 C5 1.394(4) . ?
C4 C10 1.505(4) . ?
C5 C6 1.395(4) . ?
C5 C8 1.509(4) . ?
C6 C18 1.509(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C17 1.375(4) . ?
C12 C13 1.377(5) . ?
C13 C14 1.390(5) . ?
C13 H13A 0.9300 . ?
C14 C15 1.382(6) . ?
C14 H14A 0.9300 . ?
C15 C16 1.380(6) . ?
C15 H15A 0.9300 . ?
C16 C17 1.380(5) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C24 1.357(5) . ?
C19 C20 1.352(5) . ?
C20 C21 1.390(6) . ?
C20 H20A 0.9300 . ?
C21 C22 1.345(7) . ?
C21 H21A 0.9300 . ?
C22 C23 1.348(7) . ?
C22 H22A 0.9300 . ?
C23 C24 1.375(6) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C28 C33 1.369(6) . ?
C28 C29 1.388(6) . ?
C29 C30 1.384(7) . ?
C29 H29A 0.9300 . ?
C30 C31 1.364(11) . ?
C30 H30A 0.9300 . ?
C31 C32 1.382(10) . ?
C31 H31A 0.9300 . ?
C32 C33 1.374(7) . ?
C32 H32A 0.9300 . ?
C33 H33A 0.9300 . ?
Cu1 Cl4 2.2054(12) . ?
Cu1 Cl3 2.2508(12) . ?
Cu1 Cl1 2.2537(11) . ?
Cu1 Cl2 2.2730(10) . ?
O1W H4 1.0457 . ?

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
C12 N11 C10 115.6(2) . . ?
C12 N11 H1 108.4 . . ?
C10 N11 H1 112.0 . . ?
C12 N11 H2 111.6 . . ?
C10 N11 H2 110.0 . . ?
H1 N11 H2 97.9 . . ?
C19 N19 C18 115.7(3) . . ?
C19 N19 H19A 109.5 . . ?
C18 N19 H19A 111.9 . . ?
C19 N19 H19B 110.9 . . ?
C18 N19 H19B 104.8 . . ?
H19A N19 H19B 103.2 . . ?
C28 N26 C25 114.4(2) . . ?
C28 N26 H26A 108.6 . . ?
C25 N26 H26A 105.9 . . ?
C28 N26 H26B 112.9 . . ?
C25 N26 H26B 110.1 . . ?
H26A N26 H26B 104.2 . . ?
C6 C1 C2 118.7(2) . . ?
C6 C1 C7 119.8(3) . . ?
C2 C1 C7 121.4(3) . . ?
C3 C2 C1 121.0(2) . . ?
C3 C2 C25 118.7(3) . . ?
C1 C2 C25 120.3(3) . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 C9 120.6(3) . . ?
C4 C3 C9 120.4(3) . . ?
C5 C4 C3 120.5(3) . . ?
C5 C4 C10 118.5(3) . . ?
C3 C4 C10 120.7(3) . . ?
C4 C5 C6 119.8(2) . . ?
C4 C5 C8 119.6(3) . . ?
C6 C5 C8 120.6(3) . . ?
C5 C6 C1 120.5(2) . . ?
C5 C6 C18 118.8(3) . . ?
C1 C6 C18 120.5(3) . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C9 H9A 109.5 . . ?
C3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 N11 108.9(2) . . ?
C4 C10 H10A 109.9 . . ?
N11 C10 H10A 109.9 . . ?
C4 C10 H10B 109.9 . . ?
N11 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C17 C12 C13 122.3(3) . . ?
C17 C12 N11 118.6(3) . . ?
C13 C12 N11 119.0(3) . . ?
C12 C13 C14 118.1(3) . . ?
C12 C13 H13A 121.0 . . ?
C14 C13 H13A 121.0 . . ?
C15 C14 C13 120.5(3) . . ?
C15 C14 H14A 119.8 . . ?
C13 C14 H14A 119.8 . . ?
C16 C15 C14 120.0(3) . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C15 C16 C17 120.3(4) . . ?
C15 C16 H16A 119.9 . . ?
C17 C16 H16A 119.9 . . ?
C12 C17 C16 118.8(3) . . ?
C12 C17 H17A 120.6 . . ?
C16 C17 H17A 120.6 . . ?
C6 C18 N19 110.3(2) . . ?
C6 C18 H18A 109.6 . . ?
N19 C18 H18A 109.6 . . ?
C6 C18 H18B 109.6 . . ?
N19 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C24 C19 C20 120.8(4) . . ?
C24 C19 N19 118.8(3) . . ?
C20 C19 N19 120.4(3) . . ?
C19 C20 C21 119.0(4) . . ?
C19 C20 H20A 120.5 . . ?
C21 C20 H20A 120.5 . . ?
C22 C21 C20 121.0(5) . . ?
C22 C21 H21A 119.5 . . ?
C20 C21 H21A 119.5 . . ?
C23 C22 C21 118.5(4) . . ?
C23 C22 H22A 120.7 . . ?
C21 C22 H22A 120.7 . . ?
C22 C23 C24 122.1(4) . . ?
C22 C23 H23A 118.9 . . ?
C24 C23 H23A 118.9 . . ?
C19 C24 C23 118.5(4) . . ?
C19 C24 H24A 120.7 . . ?
C23 C24 H24A 120.7 . . ?
C2 C25 N26 112.7(2) . . ?
C2 C25 H25A 109.1 . . ?
N26 C25 H25A 109.1 . . ?
C2 C25 H25B 109.1 . . ?
N26 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
C33 C28 C29 123.1(4) . . ?
C33 C28 N26 119.6(4) . . ?
C29 C28 N26 117.3(4) . . ?
C30 C29 C28 116.7(6) . . ?
C30 C29 H29A 121.6 . . ?
C28 C29 H29A 121.6 . . ?
C31 C30 C29 121.5(6) . . ?
C31 C30 H30A 119.3 . . ?
C29 C30 H30A 119.3 . . ?
C30 C31 C32 119.9(5) . . ?
C30 C31 H31A 120.0 . . ?
C32 C31 H31A 120.0 . . ?
C33 C32 C31 120.5(6) . . ?
C33 C32 H32A 119.7 . . ?
C31 C32 H32A 119.7 . . ?
C28 C33 C32 118.2(6) . . ?
C28 C33 H33A 120.9 . . ?
C32 C33 H33A 120.9 . . ?
Cl4 Cu1 Cl3 98.71(5) . . ?
Cl4 Cu1 Cl1 97.29(4) . . ?
Cl3 Cu1 Cl1 134.54(5) . . ?
Cl4 Cu1 Cl2 133.16(5) . . ?
Cl3 Cu1 Cl2 99.88(5) . . ?
Cl1 Cu1 Cl2 99.42(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.4(4) . . . . ?
C7 C1 C2 C3 -179.9(3) . . . . ?
C6 C1 C2 C25 -178.2(3) . . . . ?
C7 C1 C2 C25 0.6(4) . . . . ?
C1 C2 C3 C4 -4.8(4) . . . . ?
C25 C2 C3 C4 174.8(3) . . . . ?
C1 C2 C3 C9 176.2(3) . . . . ?
C25 C2 C3 C9 -4.2(4) . . . . ?
C2 C3 C4 C5 2.8(4) . . . . ?
C9 C3 C4 C5 -178.2(3) . . . . ?
C2 C3 C4 C10 177.9(3) . . . . ?
C9 C3 C4 C10 -3.1(4) . . . . ?
C3 C4 C5 C6 2.6(4) . . . . ?
C10 C4 C5 C6 -172.6(3) . . . . ?
C3 C4 C5 C8 -179.0(3) . . . . ?
C10 C4 C5 C8 5.9(4) . . . . ?
C4 C5 C6 C1 -6.1(4) . . . . ?
C8 C5 C6 C1 175.5(3) . . . . ?
C4 C5 C6 C18 170.1(3) . . . . ?
C8 C5 C6 C18 -8.3(4) . . . . ?
C2 C1 C6 C5 4.1(4) . . . . ?
C7 C1 C6 C5 -174.7(3) . . . . ?
C2 C1 C6 C18 -172.0(3) . . . . ?
C7 C1 C6 C18 9.2(4) . . . . ?
C5 C4 C10 N11 77.1(3) . . . . ?
C3 C4 C10 N11 -98.1(3) . . . . ?
C12 N11 C10 C4 -142.6(3) . . . . ?
C10 N11 C12 C17 117.0(3) . . . . ?
C10 N11 C12 C13 -62.2(4) . . . . ?
C17 C12 C13 C14 1.4(5) . . . . ?
N11 C12 C13 C14 -179.4(3) . . . . ?
C12 C13 C14 C15 -1.1(5) . . . . ?
C13 C14 C15 C16 0.2(5) . . . . ?
C14 C15 C16 C17 0.4(5) . . . . ?
C13 C12 C17 C16 -0.8(5) . . . . ?
N11 C12 C17 C16 180.0(3) . . . . ?
C15 C16 C17 C12 -0.1(5) . . . . ?
C5 C6 C18 N19 -81.1(3) . . . . ?
C1 C6 C18 N19 95.1(3) . . . . ?
C19 N19 C18 C6 -96.8(3) . . . . ?
C18 N19 C19 C24 -66.6(4) . . . . ?
C18 N19 C19 C20 113.9(4) . . . . ?
C24 C19 C20 C21 0.3(7) . . . . ?
N19 C19 C20 C21 179.9(4) . . . . ?
C19 C20 C21 C22 -1.2(8) . . . . ?
C20 C21 C22 C23 1.5(9) . . . . ?
C21 C22 C23 C24 -1.0(10) . . . . ?
C20 C19 C24 C23 0.2(8) . . . . ?
N19 C19 C24 C23 -179.4(5) . . . . ?
C22 C23 C24 C19 0.2(10) . . . . ?
C3 C2 C25 N26 90.0(3) . . . . ?
C1 C2 C25 N26 -90.4(3) . . . . ?
C28 N26 C25 C2 110.1(3) . . . . ?
C25 N26 C28 C33 -108.4(3) . . . . ?
C25 N26 C28 C29 70.2(4) . . . . ?
C33 C28 C29 C30 1.0(6) . . . . ?
N26 C28 C29 C30 -177.5(3) . . . . ?
C28 C29 C30 C31 -1.6(7) . . . . ?
C29 C30 C31 C32 1.8(8) . . . . ?
C30 C31 C32 C33 -1.3(8) . . . . ?
C29 C28 C33 C32 -0.6(6) . . . . ?
N26 C28 C33 C32 177.9(3) . . . . ?
C31 C32 C33 C28 0.7(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         1.823
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.067
