# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_8PhBr
_database_code_depnum_ccdc_archive 'CCDC 1869188'
_audit_update_record             
;
2018-09-22 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_1_8PhBr             
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.933 Why?
RESPONSE: Low quality of the crystal
;
_vrf_PLAT990_1_8PhBr             
;
PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE Job ...          ! Note
RESPONSE:  SHELXL-97 (Sheldrick, 1997) program was used for the SQUEEZE Job
;
# Added during the CSD deposition process: Saturday 22 September 2018 06:22 PM
# end Validation Reply Form


_audit_creation_date             2018-09-22T18:47:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C138 H148 Br8 Cl4 N12 Zn2'
_chemical_formula_weight         2886.5

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.6822(15)
_cell_length_b                   17.7483(17)
_cell_length_c                   25.194(3)
_cell_angle_alpha                78.121(7)
_cell_angle_beta                 77.607(10)
_cell_angle_gamma                60.899(8)
_cell_volume                     6699.7(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    175
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      20.03
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.48
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2936
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 5 -5 0.371
4 -1 -1 0.335
1 -17 8 0.332
-9 1 3 0.3
-3 -2 -11 0.317
3 -1 16 0.273
1 4 -2 0.477
-5 -9 -6 0.458

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_T_max  0.604

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.1856
_diffrn_reflns_number            63267
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.043
_diffrn_reflns_theta_max         24.787
_diffrn_reflns_theta_full        24.787
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.933
_reflns_Friedel_coverage         0
_reflns_number_total             21472
_reflns_number_gt                9508
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1053P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         21472
_refine_ls_number_parameters     1225
_refine_ls_number_restraints     42
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.0739
_refine_ls_wR_factor_ref         0.2083
_refine_ls_wR_factor_gt          0.1788
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_restrained_S_all      0.857
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.102


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.030 0.304 0.229 8 0 ' '
2 0.057 0.118 0.963 11 1 ' '
3 0.500 0.517 0.000 1540 461 ' '
4 0.943 0.882 0.037 11 1 ' '
5 0.970 0.696 0.771 8 1 ' '
_platon_squeeze_details          
;
There are 8 PhBr per molecular compound, four of them 
presented severe disorder and it was not possible to get a 
chemical sensible model for it, so Squeeze procedure was used to remove 
its contribution to the structure factors.
;

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.93729(4) 0.16039(4) 0.24655(3) 0.02186(19) Uani 1 1 d . . . . .
Zn2 Zn 0.37196(5) 0.18544(5) 0.78538(4) 0.0392(2) Uani 1 1 d . . . . .
Cl1 Cl 0.44633(14) 0.22492(13) 0.82657(10) 0.0665(7) Uani 1 1 d . . . . .
Cl6 Cl 0.22900(12) 0.23980(12) 0.82217(8) 0.0474(5) Uani 1 1 d . . . . .
Cl7 Cl 0.43502(13) 0.03851(12) 0.79191(11) 0.0664(7) Uani 1 1 d . . . . .
Cl8 Cl 0.37912(16) 0.23930(14) 0.69534(9) 0.0675(6) Uani 1 1 d . . . . .
N1 N 0.8598(3) 0.1032(3) 0.29419(19) 0.0196(11) Uani 1 1 d . . . . .
N2 N 0.9300(3) 0.0640(3) 0.2114(2) 0.0212(12) Uani 1 1 d . . . . .
N3 N 0.8475(3) -0.0689(3) 0.3032(2) 0.0271(13) Uani 1 1 d . . . . .
N4 N 0.7961(3) -0.0115(3) 0.2253(2) 0.0295(13) Uani 1 1 d . . . . .
N6 N 0.7124(4) 0.4747(3) 0.2837(2) 0.0323(14) Uani 1 1 d . . . . .
N7 N 0.8052(4) 0.4782(3) 0.2132(2) 0.0309(13) Uani 1 1 d . . . . .
N8 N 1.2730(3) 0.0159(3) 0.1939(2) 0.0234(12) Uani 1 1 d . . . . .
N9 N 1.2365(3) 0.1083(3) 0.2518(2) 0.0254(12) Uani 1 1 d . . . . .
N11 N 0.8561(3) 0.2810(3) 0.2219(2) 0.0220(12) Uani 1 1 d . . . . .
N12 N 0.8697(3) 0.2876(3) 0.3073(2) 0.0235(12) Uani 1 1 d . . . . .
N13 N 1.0766(3) 0.1474(3) 0.1721(2) 0.0242(12) Uani 1 1 d . . . . .
N14 N 1.0581(3) 0.1058(3) 0.2634(2) 0.0212(12) Uani 1 1 d . . . . .
C1 C 0.8777(4) 0.0548(4) 0.2552(3) 0.0216(14) Uani 1 1 d . . . . .
C2 C 0.8406(4) -0.0074(4) 0.2616(2) 0.0215(14) Uani 1 1 d . . . . .
C3 C 0.8055(5) -0.1120(5) 0.2923(3) 0.047(2) Uani 1 1 d . . . . .
H3 H 0.800187 -0.159322 0.315268 0.056 Uiso 1 1 calc R U . . .
C4 C 0.7745(5) -0.0779(5) 0.2458(3) 0.0424(19) Uani 1 1 d . . . . .
H4 H 0.743123 -0.095463 0.229171 0.051 Uiso 1 1 calc R U . . .
C5 C 0.7845(4) 0.4259(4) 0.2536(2) 0.0253(15) Uani 1 1 d . . . . .
C6 C 0.7425(5) 0.5628(4) 0.2205(3) 0.046(2) Uani 1 1 d . . . . .
H6 H 0.740559 0.613735 0.198205 0.055 Uiso 1 1 calc R U . . .
C7 C 0.6861(5) 0.5605(4) 0.2638(3) 0.0414(19) Uani 1 1 d . . . . .
H7 H 0.636658 0.609069 0.278373 0.05 Uiso 1 1 calc R U . . .
C8 C 1.1102(4) 0.1112(4) 0.2178(3) 0.0198(14) Uani 1 1 d . . . . .
C9 C 1.2048(4) 0.0790(4) 0.2206(3) 0.0251(15) Uani 1 1 d . . . . .
C10 C 1.3261(4) 0.0625(4) 0.2444(3) 0.0344(17) Uani 1 1 d . . . . .
H10 H 1.364994 0.069614 0.261328 0.041 Uiso 1 1 calc R U . . .
C11 C 0.7826(4) 0.1290(3) 0.3323(2) 0.0184(13) Uani 1 1 d . . . . .
C12 C 0.7021(4) 0.1571(5) 0.3166(3) 0.0388(18) Uani 1 1 d . . . . .
H12 H 0.698349 0.157998 0.279391 0.047 Uiso 1 1 calc R U . . .
C13 C 0.6267(4) 0.1840(5) 0.3538(3) 0.049(2) Uani 1 1 d . . . . .
H13 H 0.572208 0.200436 0.342555 0.059 Uiso 1 1 calc R U . . .
C14 C 0.6312(5) 0.1869(5) 0.4078(3) 0.0437(19) Uani 1 1 d . . . . .
C15 C 0.5465(5) 0.2193(6) 0.4494(3) 0.063(2) Uani 1 1 d . . . . .
H15A H 0.496403 0.234768 0.431075 0.094 Uiso 1 1 calc R U . . .
H15B H 0.551358 0.173129 0.479602 0.094 Uiso 1 1 calc R U . . .
H15C H 0.538325 0.270391 0.463786 0.094 Uiso 1 1 calc R U . . .
C16 C 0.7105(5) 0.1611(4) 0.4224(3) 0.0374(18) Uani 1 1 d . . . . .
H16 H 0.714094 0.162545 0.459221 0.045 Uiso 1 1 calc R U . . .
C17 C 0.7867(4) 0.1328(4) 0.3854(3) 0.0280(15) Uani 1 1 d . . . . .
H17 H 0.841098 0.116134 0.396766 0.034 Uiso 1 1 calc R U . . .
C20 C 1.3487(4) 0.0051(4) 0.2083(3) 0.0322(16) Uani 1 1 d . . . . .
H20 H 1.406488 -0.035208 0.195446 0.039 Uiso 1 1 calc R U . . .
C21 C 0.9781(4) 0.0022(4) 0.1742(2) 0.0237(15) Uani 1 1 d . . . . .
C22 C 0.9825(5) 0.0345(4) 0.1191(3) 0.0400(19) Uani 1 1 d . . . . .
H22 H 0.952883 0.09522 0.108157 0.048 Uiso 1 1 calc R U . . .
C23 C 1.0316(5) -0.0241(5) 0.0792(3) 0.044(2) Uani 1 1 d . . . . .
H23 H 1.03393 -0.002271 0.041454 0.053 Uiso 1 1 calc R U . . .
C24 C 1.0765(5) -0.1132(5) 0.0950(3) 0.048(2) Uani 1 1 d . . . . .
C25 C 1.1292(7) -0.1752(6) 0.0529(4) 0.077(3) Uani 1 1 d . . . . .
H25A H 1.125545 -0.142607 0.016237 0.116 Uiso 1 1 calc R U . . .
H25B H 1.190354 -0.207154 0.059542 0.116 Uiso 1 1 calc R U . . .
H25C H 1.106168 -0.216288 0.055417 0.116 Uiso 1 1 calc R U . . .
C26 C 1.0703(5) -0.1417(5) 0.1500(3) 0.050(2) Uani 1 1 d . . . . .
H26 H 1.099661 -0.20228 0.161532 0.06 Uiso 1 1 calc R U . . .
C27 C 1.0222(4) -0.0848(4) 0.1898(3) 0.0334(17) Uani 1 1 d . . . . .
H27 H 1.020444 -0.106794 0.227477 0.04 Uiso 1 1 calc R U . . .
C31 C 0.8927(4) -0.0909(4) 0.3514(3) 0.0303(16) Uani 1 1 d . . . . .
C32 C 0.9703(5) -0.1807(4) 0.3517(3) 0.0412(18) Uani 1 1 d . . . . .
H32A H 1.011087 -0.183711 0.31755 0.049 Uiso 1 1 calc R U . . .
H32B H 0.95001 -0.224349 0.353253 0.049 Uiso 1 1 calc R U . . .
C33 C 1.0174(5) -0.2014(5) 0.4007(3) 0.059(2) Uani 1 1 d . . . . .
H33A H 1.043716 -0.162166 0.396766 0.07 Uiso 1 1 calc R U . . .
H33B H 1.06514 -0.261826 0.401752 0.07 Uiso 1 1 calc R U . . .
C34 C 0.9551(5) -0.1910(5) 0.4544(3) 0.058(2) Uani 1 1 d . . . . .
H34A H 0.98663 -0.200201 0.485121 0.07 Uiso 1 1 calc R U . . .
H34B H 0.934875 -0.235687 0.460878 0.07 Uiso 1 1 calc R U . . .
C35 C 0.8760(5) -0.1006(5) 0.4530(3) 0.048(2) Uani 1 1 d . . . . .
H35A H 0.834855 -0.096842 0.487055 0.057 Uiso 1 1 calc R U . . .
H35B H 0.895353 -0.056069 0.450495 0.057 Uiso 1 1 calc R U . . .
C36 C 0.8304(5) -0.0837(5) 0.4040(3) 0.0409(18) Uani 1 1 d . . . . .
H36A H 0.808196 -0.126307 0.407573 0.049 Uiso 1 1 calc R U . . .
H36B H 0.779966 -0.024845 0.40283 0.049 Uiso 1 1 calc R U . . .
C40 C 0.8385(4) 0.3294(3) 0.2612(2) 0.0215(14) Uani 1 1 d . . . . .
C41 C 0.7723(5) 0.0457(5) 0.1737(3) 0.0345(17) Uani 1 1 d . . . . .
C42 C 0.8048(6) -0.0104(6) 0.1280(3) 0.058(2) Uani 1 1 d . . . . .
H42A H 0.776636 -0.048561 0.134762 0.069 Uiso 1 1 calc R U . . .
H42B H 0.868793 -0.047369 0.12589 0.069 Uiso 1 1 calc R U . . .
C43 C 0.7811(7) 0.0520(7) 0.0727(3) 0.077(3) Uani 1 1 d . . . . .
H43A H 0.813638 0.086149 0.064909 0.093 Uiso 1 1 calc R U . . .
H43B H 0.799455 0.016589 0.042299 0.093 Uiso 1 1 calc R U . . .
C44 C 0.6866(6) 0.1119(7) 0.0754(4) 0.071(3) Uani 1 1 d . . . . .
H44A H 0.654488 0.078075 0.078544 0.086 Uiso 1 1 calc R U . . .
H44B H 0.675103 0.15228 0.041154 0.086 Uiso 1 1 calc R U . . .
C45 C 0.6524(6) 0.1647(6) 0.1247(3) 0.063(2) Uani 1 1 d . . . . .
H45A H 0.679032 0.204028 0.119319 0.075 Uiso 1 1 calc R U . . .
H45B H 0.588304 0.200915 0.126607 0.075 Uiso 1 1 calc R U . . .
C46 C 0.6740(5) 0.1055(5) 0.1780(3) 0.0420(19) Uani 1 1 d . . . . .
H46A H 0.642463 0.070319 0.185524 0.05 Uiso 1 1 calc R U . . .
H46B H 0.655116 0.140727 0.208539 0.05 Uiso 1 1 calc R U . . .
C61 C 0.6675(4) 0.4423(4) 0.3317(3) 0.0345(17) Uani 1 1 d . . . . .
C62 C 0.5765(5) 0.4653(5) 0.3222(3) 0.0457(19) Uani 1 1 d . . . . .
H62A H 0.580059 0.441476 0.289002 0.055 Uiso 1 1 calc R U . . .
H62B H 0.541225 0.529201 0.31638 0.055 Uiso 1 1 calc R U . . .
C63 C 0.5324(5) 0.4281(6) 0.3715(3) 0.060(2) Uani 1 1 d . . . . .
H63A H 0.472166 0.445881 0.365365 0.072 Uiso 1 1 calc R U . . .
H63B H 0.564724 0.363903 0.374915 0.072 Uiso 1 1 calc R U . . .
C64 C 0.5290(5) 0.4585(6) 0.4241(3) 0.061(2) Uani 1 1 d . . . . .
H64A H 0.505206 0.428595 0.455315 0.073 Uiso 1 1 calc R U . . .
H64B H 0.489559 0.521712 0.422992 0.073 Uiso 1 1 calc R U . . .
C65 C 0.6201(5) 0.4394(5) 0.4323(3) 0.055(2) Uani 1 1 d . . . . .
H65A H 0.657605 0.375762 0.437578 0.066 Uiso 1 1 calc R U . . .
H65B H 0.616041 0.463238 0.465577 0.066 Uiso 1 1 calc R U . . .
C66 C 0.6616(5) 0.4793(5) 0.3830(3) 0.0394(18) Uani 1 1 d . . . . .
H66A H 0.720669 0.46575 0.388946 0.047 Uiso 1 1 calc R U . . .
H66B H 0.625726 0.543232 0.378428 0.047 Uiso 1 1 calc R U . . .
C71 C 0.8846(5) 0.4514(4) 0.1715(3) 0.0332(17) Uani 1 1 d . . . . .
C72 C 0.8564(6) 0.4780(5) 0.1158(3) 0.051(2) Uani 1 1 d . . . . .
H72A H 0.824022 0.542113 0.108846 0.061 Uiso 1 1 calc R U . . .
H72B H 0.817506 0.453834 0.113278 0.061 Uiso 1 1 calc R U . . .
C73 C 0.9401(7) 0.4426(6) 0.0725(3) 0.070(3) Uani 1 1 d . . . . .
H73A H 0.970417 0.378373 0.078408 0.084 Uiso 1 1 calc R U . . .
H73B H 0.92302 0.460839 0.035217 0.084 Uiso 1 1 calc R U . . .
C74 C 1.0020(7) 0.4779(6) 0.0777(4) 0.073(3) Uani 1 1 d . . . . .
H74A H 1.056531 0.45147 0.052256 0.088 Uiso 1 1 calc R U . . .
H74B H 0.974143 0.54152 0.067068 0.088 Uiso 1 1 calc R U . . .
C75 C 1.0242(5) 0.4584(5) 0.1359(3) 0.054(2) Uani 1 1 d . . . . .
H75A H 1.059899 0.486265 0.138397 0.065 Uiso 1 1 calc R U . . .
H75B H 1.05902 0.394912 0.144983 0.065 Uiso 1 1 calc R U . . .
C76 C 0.9412(5) 0.4920(5) 0.1766(3) 0.0404(18) Uani 1 1 d . . . . .
H76A H 0.908389 0.556039 0.169252 0.048 Uiso 1 1 calc R U . . .
H76B H 0.956453 0.477122 0.214277 0.048 Uiso 1 1 calc R U . . .
C81 C 1.2687(4) -0.0347(4) 0.1555(2) 0.0251(15) Uani 1 1 d . . . . .
C82 C 1.3067(5) -0.1290(4) 0.1774(3) 0.0413(18) Uani 1 1 d . . . . .
H82A H 1.272567 -0.136893 0.212793 0.05 Uiso 1 1 calc R U . . .
H82B H 1.367654 -0.150519 0.183608 0.05 Uiso 1 1 calc R U . . .
C83 C 1.3047(5) -0.1811(5) 0.1360(3) 0.050(2) Uani 1 1 d . . . . .
H83A H 1.333289 -0.243675 0.149709 0.06 Uiso 1 1 calc R U . . .
H83B H 1.243199 -0.163829 0.133383 0.06 Uiso 1 1 calc R U . . .
C84 C 1.3497(6) -0.1668(5) 0.0802(3) 0.056(2) Uani 1 1 d . . . . .
H84A H 1.341228 -0.196398 0.054402 0.067 Uiso 1 1 calc R U . . .
H84B H 1.413193 -0.192592 0.081529 0.067 Uiso 1 1 calc R U . . .
C85 C 1.3143(5) -0.0710(5) 0.0599(3) 0.052(2) Uani 1 1 d . . . . .
H85A H 1.34866 -0.063491 0.024493 0.062 Uiso 1 1 calc R U . . .
H85B H 1.253009 -0.047331 0.053552 0.062 Uiso 1 1 calc R U . . .
C86 C 1.3178(5) -0.0211(5) 0.0995(3) 0.0399(18) Uani 1 1 d . . . . .
H86A H 1.291189 0.04152 0.085556 0.048 Uiso 1 1 calc R U . . .
H86B H 1.379395 -0.04042 0.103163 0.048 Uiso 1 1 calc R U . . .
C91 C 1.1844(4) 0.1774(4) 0.2874(3) 0.0347(17) Uani 1 1 d . . . . .
C92 C 1.2027(5) 0.2547(4) 0.2658(3) 0.0402(18) Uani 1 1 d . . . . .
H92A H 1.188516 0.276395 0.227868 0.048 Uiso 1 1 calc R U . . .
H92B H 1.265304 0.236527 0.26532 0.048 Uiso 1 1 calc R U . . .
C93 C 1.1465(5) 0.3269(5) 0.3029(3) 0.051(2) Uani 1 1 d . . . . .
H93A H 1.161149 0.375434 0.28998 0.061 Uiso 1 1 calc R U . . .
H93B H 1.084266 0.349121 0.299417 0.061 Uiso 1 1 calc R U . . .
C94 C 1.1584(6) 0.2986(5) 0.3609(3) 0.055(2) Uani 1 1 d . . . . .
H94A H 1.117243 0.346716 0.382713 0.066 Uiso 1 1 calc R U . . .
H94B H 1.218561 0.283715 0.365395 0.066 Uiso 1 1 calc R U . . .
C95 C 1.1431(6) 0.2217(5) 0.3813(3) 0.056(2) Uani 1 1 d . . . . .
H95A H 1.080902 0.238696 0.38098 0.068 Uiso 1 1 calc R U . . .
H95B H 1.155486 0.201608 0.419641 0.068 Uiso 1 1 calc R U . . .
C96 C 1.2020(5) 0.1456(4) 0.3456(3) 0.0386(18) Uani 1 1 d . . . . .
H96A H 1.264302 0.12541 0.347802 0.046 Uiso 1 1 calc R U . . .
H96B H 1.188829 0.096269 0.359315 0.046 Uiso 1 1 calc R U . . .
C110 C 0.8107(4) 0.3053(3) 0.1766(3) 0.0236(15) Uani 1 1 d . . . . .
C111 C 0.7201(4) 0.3562(4) 0.1791(3) 0.0318(16) Uani 1 1 d . . . . .
H111 H 0.68621 0.378458 0.212265 0.038 Uiso 1 1 calc R U . . .
C112 C 0.6796(4) 0.3740(4) 0.1334(3) 0.0373(18) Uani 1 1 d . . . . .
H112 H 0.618098 0.408971 0.135849 0.045 Uiso 1 1 calc R U . . .
C113 C 0.7257(5) 0.3427(4) 0.0843(3) 0.0358(17) Uani 1 1 d . . . . .
C114 C 0.8165(5) 0.2923(4) 0.0836(3) 0.0370(18) Uani 1 1 d . . . . .
H114 H 0.850579 0.269137 0.050742 0.044 Uiso 1 1 calc R U . . .
C115 C 0.8584(4) 0.2748(4) 0.1277(2) 0.0235(14) Uani 1 1 d . . . . .
H115 H 0.920159 0.241774 0.124678 0.028 Uiso 1 1 calc R U . . .
C116 C 0.6819(5) 0.3593(5) 0.0353(3) 0.056(2) Uani 1 1 d . . . . .
H11A H 0.726078 0.33167 0.004961 0.084 Uiso 1 1 calc R U . . .
H11B H 0.640728 0.335111 0.044422 0.084 Uiso 1 1 calc R U . . .
H11C H 0.650361 0.422036 0.024518 0.084 Uiso 1 1 calc R U . . .
C120 C 0.8763(4) 0.3271(4) 0.3483(2) 0.0228(14) Uani 1 1 d . . . . .
C121 C 0.9038(4) 0.3908(4) 0.3363(3) 0.0283(15) Uani 1 1 d . . . . .
H121 H 0.914502 0.412789 0.299314 0.034 Uiso 1 1 calc R U . . .
C122 C 0.9154(4) 0.4222(4) 0.3787(3) 0.0328(16) Uani 1 1 d . . . . .
H122 H 0.932895 0.466656 0.370006 0.039 Uiso 1 1 calc R U . . .
C123 C 0.9024(4) 0.3908(4) 0.4327(3) 0.0309(16) Uani 1 1 d . . . . .
C124 C 0.8728(4) 0.3275(4) 0.4450(3) 0.0322(16) Uani 1 1 d . . . . .
H124 H 0.860478 0.30645 0.481906 0.039 Uiso 1 1 calc R U . . .
C125 C 0.8618(4) 0.2960(4) 0.4023(3) 0.0277(15) Uani 1 1 d . . . . .
H125 H 0.843855 0.251949 0.410771 0.033 Uiso 1 1 calc R U . . .
C126 C 0.9202(5) 0.4227(5) 0.4787(3) 0.046(2) Uani 1 1 d . . . . .
H12A H 0.907257 0.393093 0.514059 0.069 Uiso 1 1 calc R U . . .
H12B H 0.981743 0.409784 0.473 0.069 Uiso 1 1 calc R U . . .
H12C H 0.883066 0.485497 0.478238 0.069 Uiso 1 1 calc R U . . .
C130 C 1.1199(4) 0.1729(4) 0.1237(2) 0.0261(15) Uani 1 1 d . . . . .
C131 C 1.1113(4) 0.1577(4) 0.0744(3) 0.0362(17) Uani 1 1 d . . . . .
H131 H 1.07992 0.126971 0.074077 0.043 Uiso 1 1 calc R U . . .
C132 C 1.1468(5) 0.1858(5) 0.0264(3) 0.049(2) Uani 1 1 d . . . . .
H132 H 1.139619 0.173707 -0.006652 0.058 Uiso 1 1 calc R U . . .
C133 C 1.1933(5) 0.2313(5) 0.0233(3) 0.051(2) Uani 1 1 d . . . . .
C134 C 1.2035(5) 0.2463(5) 0.0724(3) 0.051(2) Uani 1 1 d . . . . .
H134 H 1.234951 0.27701 0.072467 0.061 Uiso 1 1 calc R U . . .
C135 C 1.1674(4) 0.2159(4) 0.1223(3) 0.0356(17) Uani 1 1 d . . . . .
H135 H 1.176122 0.225431 0.155759 0.043 Uiso 1 1 calc R U . . .
C136 C 1.2314(6) 0.2639(7) -0.0317(4) 0.089(3) Uani 1 1 d . . . . .
H13A H 1.217637 0.247274 -0.061715 0.134 Uiso 1 1 calc R U . . .
H13B H 1.206104 0.327328 -0.035112 0.134 Uiso 1 1 calc R U . . .
H13C H 1.294974 0.23805 -0.03335 0.134 Uiso 1 1 calc R U . . .
C140 C 1.0847(4) 0.0508(4) 0.3117(2) 0.0214(14) Uani 1 1 d . . . . .
C141 C 1.0364(4) 0.0812(4) 0.3610(3) 0.0289(16) Uani 1 1 d . . . . .
H141 H 0.988485 0.138012 0.36089 0.035 Uiso 1 1 calc R U . . .
C142 C 1.0576(5) 0.0293(4) 0.4101(3) 0.0397(18) Uani 1 1 d . . . . .
H142 H 1.023357 0.051622 0.443178 0.048 Uiso 1 1 calc R U . . .
C143 C 1.1266(4) -0.0536(4) 0.4131(3) 0.0355(17) Uani 1 1 d . . . . .
C144 C 1.1758(5) -0.0842(5) 0.3631(3) 0.0422(19) Uani 1 1 d . . . . .
H144 H 1.224341 -0.140629 0.363123 0.051 Uiso 1 1 calc R U . . .
C145 C 1.1535(4) -0.0320(4) 0.3133(3) 0.0317(16) Uani 1 1 d . . . . .
H145 H 1.186487 -0.054227 0.279971 0.038 Uiso 1 1 calc R U . . .
C146 C 1.1475(5) -0.1095(5) 0.4678(3) 0.057(2) Uani 1 1 d . . . . .
H14A H 1.198282 -0.165756 0.461598 0.086 Uiso 1 1 calc R U . . .
H14B H 1.16045 -0.080162 0.490889 0.086 Uiso 1 1 calc R U . . .
H14C H 1.097154 -0.118411 0.48601 0.086 Uiso 1 1 calc R U . . .
Br1 Br 0.18456(8) 0.60509(9) 0.20343(5) 0.1056(4) Uani 1 1 d . . . . .
Br2 Br 0.86436(6) 0.47123(7) 0.63901(5) 0.0810(3) Uani 1 1 d . . . . .
Br3 Br 0.30866(7) 0.46682(8) 0.45655(6) 0.1006(4) Uani 1 1 d . . . . .
C1D C 0.0361(6) 0.6778(6) 0.1474(4) 0.064(2) Uani 1 1 d . . . . .
H1D H 0.004528 0.702498 0.180263 0.077 Uiso 1 1 calc R U . . .
C2D C -0.0042(6) 0.6938(5) 0.1046(4) 0.060(2) Uani 1 1 d . . . . .
H2D H -0.065734 0.729016 0.107287 0.072 Uiso 1 1 calc R U . . .
C3D C 0.0428(7) 0.6591(6) 0.0551(4) 0.073(3) Uani 1 1 d . . . . .
H3D H 0.013566 0.673116 0.024257 0.088 Uiso 1 1 calc R U . . .
C4D C 0.1320(6) 0.6046(5) 0.0520(4) 0.062(2) Uani 1 1 d . . . . .
H4D H 0.164327 0.579929 0.019207 0.074 Uiso 1 1 calc R U . . .
C5D C 0.1723(6) 0.5871(5) 0.0964(5) 0.070(3) Uani 1 1 d . . . . .
H5D H 0.233124 0.548946 0.095 0.084 Uiso 1 1 calc R U . . .
C6D C 0.1264(6) 0.6235(6) 0.1429(4) 0.059(2) Uani 1 1 d . . . . .
C7D C 0.2887(6) 0.3193(6) 0.4618(4) 0.068(3) Uani 1 1 d . . . . .
H7D H 0.26358 0.348366 0.429114 0.082 Uiso 1 1 calc R U . . .
C8D C 0.3523(6) 0.3209(8) 0.5354(4) 0.068(3) Uani 1 1 d . . . . .
H8D H 0.368851 0.350917 0.553935 0.082 Uiso 1 1 calc R U . . .
C9D C 0.3618(6) 0.2380(9) 0.5553(4) 0.090(4) Uani 1 1 d . . . . .
H9D H 0.388242 0.209775 0.587677 0.108 Uiso 1 1 calc R U . . .
C11D C 0.9837(5) 0.4198(5) 0.6479(4) 0.048(2) Uani 1 1 d . . . . .
C12D C 1.0093(6) 0.4067(5) 0.6983(4) 0.058(2) Uani 1 1 d . . . . .
H12D H 0.967051 0.42567 0.729545 0.07 Uiso 1 1 calc R U . . .
C13D C 1.0959(7) 0.3662(6) 0.7027(4) 0.065(3) Uani 1 1 d . . . . .
H13D H 1.113898 0.356082 0.737481 0.078 Uiso 1 1 calc R U . . .
C14D C 1.1569(6) 0.3401(5) 0.6588(5) 0.064(3) Uani 1 1 d . . . . .
H14D H 1.217181 0.313151 0.662426 0.077 Uiso 1 1 calc R U . . .
C15D C 1.1311(7) 0.3528(6) 0.6093(5) 0.075(3) Uani 1 1 d . . . . .
H15D H 1.174257 0.33332 0.578515 0.09 Uiso 1 1 calc R U . . .
C16D C 1.0445(7) 0.3931(5) 0.6025(3) 0.054(2) Uani 1 1 d . . . . .
H16D H 1.027177 0.402309 0.567538 0.065 Uiso 1 1 calc R U . . .
C19D C 0.3176(5) 0.3560(6) 0.4877(4) 0.061(2) Uani 1 1 d . . . . .
C17D C 0.2960(7) 0.2305(8) 0.4849(5) 0.091(3) Uani 1 1 d . . . . .
H17D H 0.274429 0.202635 0.468295 0.109 Uiso 1 1 calc R U . . .
C18D C 0.3343(7) 0.1942(7) 0.5298(4) 0.085(3) Uani 1 1 d . . . . .
H18D H 0.343271 0.137285 0.544994 0.102 Uiso 1 1 calc R U . . .
Br4 Br 0.57306(11) 0.01985(13) 0.37714(8) 0.1522(7) Uani 1 1 d . . . . .
C20D C 0.4788(6) -0.0055(5) 0.3965(4) 0.072(3) Uani 1 1 d D . . . .
C21D C 0.4625(5) -0.0444(4) 0.3613(4) 0.063(2) Uani 1 1 d D . . . .
H21D H 0.497147 -0.057768 0.326794 0.076 Uiso 1 1 calc R U . . .
C22D C 0.3926(6) -0.0631(6) 0.3791(5) 0.092(3) Uani 1 1 d D . . . .
H22D H 0.380473 -0.088679 0.35454 0.11 Uiso 1 1 calc R U . . .
C23D C 0.3386(6) -0.0481(6) 0.4291(5) 0.079(3) Uani 1 1 d D . . . .
H23D H 0.294102 -0.065753 0.438028 0.094 Uiso 1 1 calc R U . . .
C24D C 0.4274(6) 0.0141(6) 0.4459(4) 0.082(3) Uani 1 1 d D . . . .
H24D H 0.439383 0.041948 0.469076 0.098 Uiso 1 1 calc R U . . .
C25D C 0.3501(6) -0.0080(6) 0.4649(4) 0.086(3) Uani 1 1 d D . . . .
H25D H 0.313767 0.00551 0.498888 0.103 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N11 1.968(4) . ?
Zn1 N14 1.972(5) . ?
Zn1 N1 2.120(5) . ?
Zn1 N2 2.149(5) . ?
Zn1 C1 2.514(6) . ?
Zn2 Cl1 2.254(2) . ?
Zn2 Cl7 2.268(2) . ?
Zn2 Cl6 2.274(2) . ?
Zn2 Cl8 2.275(2) . ?
N1 C1 1.323(7) . ?
N1 C11 1.417(7) . ?
N2 C1 1.317(7) . ?
N2 C21 1.407(7) . ?
N3 C2 1.327(7) . ?
N3 C3 1.394(8) . ?
N3 C31 1.477(8) . ?
N4 C2 1.360(7) . ?
N4 C4 1.380(8) . ?
N4 C41 1.473(8) . ?
N6 C5 1.316(8) . ?
N6 C7 1.373(8) . ?
N6 C61 1.473(8) . ?
N7 C5 1.347(8) . ?
N7 C6 1.388(8) . ?
N7 C71 1.491(8) . ?
N8 C9 1.345(8) . ?
N8 C20 1.376(8) . ?
N8 C81 1.485(7) . ?
N9 C9 1.358(7) . ?
N9 C10 1.374(8) . ?
N9 C91 1.469(8) . ?
N11 C40 1.330(7) . ?
N11 C110 1.411(8) . ?
N12 C40 1.313(7) . ?
N12 C120 1.416(7) . ?
N13 C8 1.308(7) . ?
N13 C130 1.411(8) . ?
N14 C8 1.327(7) . ?
N14 C140 1.403(7) . ?
C1 C2 1.505(8) . ?
C3 C4 1.303(10) . ?
C5 C40 1.495(8) . ?
C6 C7 1.318(10) . ?
C8 C9 1.494(8) . ?
C10 C20 1.361(9) . ?
C11 C17 1.373(8) . ?
C11 C12 1.378(9) . ?
C12 C13 1.383(9) . ?
C13 C14 1.393(10) . ?
C14 C16 1.356(10) . ?
C14 C15 1.552(10) . ?
C16 C17 1.390(9) . ?
C21 C27 1.363(9) . ?
C21 C22 1.389(9) . ?
C22 C23 1.422(9) . ?
C23 C24 1.395(11) . ?
C24 C26 1.375(10) . ?
C24 C25 1.505(9) . ?
C26 C27 1.400(9) . ?
C31 C36 1.513(9) . ?
C31 C32 1.515(9) . ?
C32 C33 1.520(10) . ?
C33 C34 1.530(11) . ?
C34 C35 1.532(10) . ?
C35 C36 1.517(10) . ?
C41 C42 1.510(10) . ?
C41 C46 1.527(10) . ?
C42 C43 1.584(12) . ?
C43 C44 1.477(13) . ?
C44 C45 1.546(12) . ?
C45 C46 1.518(10) . ?
C61 C62 1.516(10) . ?
C61 C66 1.531(9) . ?
C62 C63 1.527(10) . ?
C63 C64 1.510(11) . ?
C64 C65 1.529(11) . ?
C65 C66 1.527(10) . ?
C71 C72 1.497(10) . ?
C71 C76 1.527(9) . ?
C72 C73 1.567(11) . ?
C73 C74 1.540(12) . ?
C74 C75 1.526(12) . ?
C75 C76 1.522(10) . ?
C81 C82 1.497(9) . ?
C81 C86 1.529(9) . ?
C82 C83 1.544(10) . ?
C83 C84 1.498(10) . ?
C84 C85 1.513(10) . ?
C85 C86 1.493(10) . ?
C91 C96 1.499(9) . ?
C91 C92 1.526(9) . ?
C92 C93 1.536(9) . ?
C93 C94 1.469(10) . ?
C94 C95 1.487(10) . ?
C95 C96 1.565(10) . ?
C110 C115 1.381(8) . ?
C110 C111 1.400(8) . ?
C111 C112 1.387(9) . ?
C112 C113 1.382(9) . ?
C113 C114 1.406(9) . ?
C113 C116 1.500(9) . ?
C114 C115 1.365(9) . ?
C120 C125 1.378(8) . ?
C120 C121 1.391(8) . ?
C121 C122 1.396(9) . ?
C122 C123 1.376(9) . ?
C123 C124 1.412(9) . ?
C123 C126 1.535(9) . ?
C124 C125 1.394(8) . ?
C130 C135 1.374(9) . ?
C130 C131 1.378(9) . ?
C131 C132 1.355(10) . ?
C132 C133 1.386(11) . ?
C133 C134 1.383(10) . ?
C133 C136 1.536(11) . ?
C134 C135 1.412(10) . ?
C140 C145 1.379(8) . ?
C140 C141 1.391(8) . ?
C141 C142 1.385(9) . ?
C142 C143 1.381(9) . ?
C143 C144 1.411(10) . ?
C143 C146 1.522(9) . ?
C144 C145 1.402(9) . ?
Br1 C6D 1.906(9) . ?
Br2 C11D 1.892(8) . ?
Br3 C19D 1.904(9) . ?
C1D C2D 1.325(12) . ?
C1D C6D 1.401(12) . ?
C2D C3D 1.414(12) . ?
C3D C4D 1.386(13) . ?
C4D C5D 1.358(12) . ?
C5D C6D 1.356(12) . ?
C7D C19D 1.324(11) . ?
C7D C17D 1.515(14) . ?
C8D C19D 1.357(12) . ?
C8D C9D 1.391(14) . ?
C9D C18D 1.400(15) . ?
C11D C12D 1.376(11) . ?
C11D C16D 1.376(11) . ?
C12D C13D 1.357(12) . ?
C13D C14D 1.346(13) . ?
C14D C15D 1.357(13) . ?
C15D C16D 1.373(13) . ?
C17D C18D 1.326(13) . ?
Br4 C20D 1.873(10) . ?
C20D C24D 1.372(5) . ?
C20D C21D 1.379(12) . ?
C21D C22D 1.391(5) . ?
C22D C23D 1.395(14) . ?
C23D C25D 1.359(5) . ?
C24D C25D 1.554(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
N11 Zn1 N14 132.19(19) . . ?
N11 Zn1 N1 106.68(19) . . ?
N14 Zn1 N1 114.69(19) . . ?
N11 Zn1 N2 114.46(19) . . ?
N14 Zn1 N2 105.06(19) . . ?
N1 Zn1 N2 63.32(17) . . ?
N11 Zn1 C1 114.02(19) . . ?
N14 Zn1 C1 113.75(19) . . ?
N1 Zn1 C1 31.74(18) . . ?
N2 Zn1 C1 31.58(18) . . ?
Cl1 Zn2 Cl7 109.62(8) . . ?
Cl1 Zn2 Cl6 111.67(8) . . ?
Cl7 Zn2 Cl6 110.25(8) . . ?
Cl1 Zn2 Cl8 108.16(10) . . ?
Cl7 Zn2 Cl8 108.71(9) . . ?
Cl6 Zn2 Cl8 108.35(9) . . ?
C1 N1 C11 123.5(5) . . ?
C1 N1 Zn1 90.8(3) . . ?
C11 N1 Zn1 137.3(3) . . ?
C1 N2 C21 124.5(5) . . ?
C1 N2 Zn1 89.7(3) . . ?
C21 N2 Zn1 141.1(4) . . ?
C2 N3 C3 106.5(6) . . ?
C2 N3 C31 128.0(5) . . ?
C3 N3 C31 125.5(6) . . ?
C2 N4 C4 108.0(5) . . ?
C2 N4 C41 126.8(5) . . ?
C4 N4 C41 125.2(5) . . ?
C5 N6 C7 109.5(6) . . ?
C5 N6 C61 125.3(5) . . ?
C7 N6 C61 125.3(6) . . ?
C5 N7 C6 107.0(6) . . ?
C5 N7 C71 126.7(5) . . ?
C6 N7 C71 126.1(5) . . ?
C9 N8 C20 108.5(5) . . ?
C9 N8 C81 126.5(5) . . ?
C20 N8 C81 125.0(5) . . ?
C9 N9 C10 108.5(5) . . ?
C9 N9 C91 126.1(5) . . ?
C10 N9 C91 125.5(5) . . ?
C40 N11 C110 126.5(5) . . ?
C40 N11 Zn1 108.1(4) . . ?
C110 N11 Zn1 123.9(4) . . ?
C40 N12 C120 124.6(5) . . ?
C8 N13 C130 124.5(5) . . ?
C8 N14 C140 125.9(5) . . ?
C8 N14 Zn1 109.0(4) . . ?
C140 N14 Zn1 123.0(4) . . ?
N2 C1 N1 116.2(5) . . ?
N2 C1 C2 122.6(5) . . ?
N1 C1 C2 121.3(5) . . ?
N2 C1 Zn1 58.7(3) . . ?
N1 C1 Zn1 57.5(3) . . ?
C2 C1 Zn1 178.7(4) . . ?
N3 C2 N4 108.6(5) . . ?
N3 C2 C1 125.4(5) . . ?
N4 C2 C1 126.0(5) . . ?
C4 C3 N3 110.0(6) . . ?
C3 C4 N4 107.0(6) . . ?
N6 C5 N7 108.2(5) . . ?
N6 C5 C40 128.4(6) . . ?
N7 C5 C40 123.4(5) . . ?
C7 C6 N7 108.3(6) . . ?
C6 C7 N6 107.0(6) . . ?
N13 C8 N14 118.9(5) . . ?
N13 C8 C9 121.9(5) . . ?
N14 C8 C9 119.2(5) . . ?
N8 C9 N9 108.1(5) . . ?
N8 C9 C8 126.8(5) . . ?
N9 C9 C8 125.2(5) . . ?
C20 C10 N9 107.3(5) . . ?
C17 C11 C12 118.8(6) . . ?
C17 C11 N1 119.2(5) . . ?
C12 C11 N1 121.8(5) . . ?
C11 C12 C13 121.5(7) . . ?
C12 C13 C14 119.5(7) . . ?
C16 C14 C13 118.4(7) . . ?
C16 C14 C15 121.8(7) . . ?
C13 C14 C15 119.8(7) . . ?
C14 C16 C17 122.4(7) . . ?
C11 C17 C16 119.4(6) . . ?
C10 C20 N8 107.7(6) . . ?
C27 C21 C22 120.1(5) . . ?
C27 C21 N2 123.5(6) . . ?
C22 C21 N2 116.4(5) . . ?
C21 C22 C23 119.5(6) . . ?
C24 C23 C22 120.6(7) . . ?
C26 C24 C23 117.6(6) . . ?
C26 C24 C25 121.7(7) . . ?
C23 C24 C25 120.7(7) . . ?
C24 C26 C27 122.5(7) . . ?
C21 C27 C26 119.8(6) . . ?
N3 C31 C36 111.0(5) . . ?
N3 C31 C32 111.2(5) . . ?
C36 C31 C32 110.7(5) . . ?
C31 C32 C33 110.5(6) . . ?
C32 C33 C34 111.5(7) . . ?
C33 C34 C35 111.2(6) . . ?
C36 C35 C34 109.8(6) . . ?
C31 C36 C35 110.6(6) . . ?
N12 C40 N11 116.4(5) . . ?
N12 C40 C5 121.9(5) . . ?
N11 C40 C5 121.7(5) . . ?
N4 C41 C42 108.3(6) . . ?
N4 C41 C46 111.0(5) . . ?
C42 C41 C46 112.2(6) . . ?
C41 C42 C43 107.7(7) . . ?
C44 C43 C42 111.8(7) . . ?
C43 C44 C45 111.8(7) . . ?
C46 C45 C44 111.2(7) . . ?
C45 C46 C41 109.4(6) . . ?
N6 C61 C62 111.1(6) . . ?
N6 C61 C66 111.0(5) . . ?
C62 C61 C66 109.4(6) . . ?
C61 C62 C63 110.2(6) . . ?
C64 C63 C62 112.2(7) . . ?
C63 C64 C65 110.6(7) . . ?
C64 C65 C66 111.1(7) . . ?
C65 C66 C61 109.1(6) . . ?
N7 C71 C72 108.6(6) . . ?
N7 C71 C76 111.5(5) . . ?
C72 C71 C76 110.3(6) . . ?
C71 C72 C73 108.3(7) . . ?
C74 C73 C72 110.0(6) . . ?
C75 C74 C73 111.9(7) . . ?
C74 C75 C76 110.5(7) . . ?
C75 C76 C71 109.7(6) . . ?
N8 C81 C82 110.2(5) . . ?
N8 C81 C86 109.3(5) . . ?
C82 C81 C86 110.9(5) . . ?
C81 C82 C83 109.6(6) . . ?
C84 C83 C82 112.6(6) . . ?
C83 C84 C85 111.1(6) . . ?
C86 C85 C84 112.2(6) . . ?
C85 C86 C81 110.5(6) . . ?
N9 C91 C96 111.6(5) . . ?
N9 C91 C92 109.7(5) . . ?
C96 C91 C92 110.8(5) . . ?
C91 C92 C93 109.1(6) . . ?
C94 C93 C92 113.7(7) . . ?
C93 C94 C95 111.0(6) . . ?
C94 C95 C96 111.7(6) . . ?
C91 C96 C95 108.9(6) . . ?
C115 C110 C111 118.7(6) . . ?
C115 C110 N11 117.8(5) . . ?
C111 C110 N11 123.5(5) . . ?
C112 C111 C110 120.1(6) . . ?
C113 C112 C111 122.3(6) . . ?
C112 C113 C114 115.6(6) . . ?
C112 C113 C116 122.4(6) . . ?
C114 C113 C116 121.9(6) . . ?
C115 C114 C113 123.5(6) . . ?
C114 C115 C110 119.8(6) . . ?
C125 C120 C121 118.8(6) . . ?
C125 C120 N12 118.5(5) . . ?
C121 C120 N12 122.6(5) . . ?
C120 C121 C122 119.7(6) . . ?
C123 C122 C121 122.1(6) . . ?
C122 C123 C124 118.1(6) . . ?
C122 C123 C126 121.4(6) . . ?
C124 C123 C126 120.5(6) . . ?
C125 C124 C123 119.5(6) . . ?
C120 C125 C124 121.8(6) . . ?
C135 C130 C131 117.5(6) . . ?
C135 C130 N13 123.9(6) . . ?
C131 C130 N13 118.5(6) . . ?
C132 C131 C130 121.0(7) . . ?
C131 C132 C133 123.2(7) . . ?
C134 C133 C132 116.6(7) . . ?
C134 C133 C136 121.2(8) . . ?
C132 C133 C136 122.2(8) . . ?
C133 C134 C135 120.1(7) . . ?
C130 C135 C134 121.6(7) . . ?
C145 C140 C141 118.2(6) . . ?
C145 C140 N14 124.3(5) . . ?
C141 C140 N14 117.5(5) . . ?
C142 C141 C140 120.4(6) . . ?
C143 C142 C141 122.6(6) . . ?
C142 C143 C144 116.8(6) . . ?
C142 C143 C146 121.3(6) . . ?
C144 C143 C146 121.8(6) . . ?
C145 C144 C143 120.4(6) . . ?
C140 C145 C144 121.4(6) . . ?
C2D C1D C6D 118.3(9) . . ?
C1D C2D C3D 121.0(9) . . ?
C4D C3D C2D 119.5(9) . . ?
C5D C4D C3D 118.9(9) . . ?
C4D C5D C6D 120.6(9) . . ?
C5D C6D C1D 121.6(9) . . ?
C5D C6D Br1 120.4(7) . . ?
C1D C6D Br1 117.9(7) . . ?
C19D C7D C17D 119.4(9) . . ?
C19D C8D C9D 115.6(9) . . ?
C8D C9D C18D 123.0(10) . . ?
C12D C11D C16D 120.8(8) . . ?
C12D C11D Br2 121.5(7) . . ?
C16D C11D Br2 117.6(7) . . ?
C13D C12D C11D 118.9(8) . . ?
C14D C13D C12D 121.5(9) . . ?
C13D C14D C15D 119.2(9) . . ?
C14D C15D C16D 121.8(9) . . ?
C15D C16D C11D 117.7(9) . . ?
C7D C19D C8D 124.8(10) . . ?
C7D C19D Br3 117.8(8) . . ?
C8D C19D Br3 117.4(8) . . ?
C18D C17D C7D 115.8(11) . . ?
C17D C18D C9D 121.3(12) . . ?
C24D C20D C21D 120.9(9) . . ?
C24D C20D Br4 119.4(8) . . ?
C21D C20D Br4 119.7(6) . . ?
C20D C21D C22D 116.4(9) . . ?
C23D C22D C21D 126.8(11) . . ?
C25D C23D C22D 119.4(9) . . ?
C20D C24D C25D 121.6(10) . . ?
C23D C25D C24D 114.8(9) . . ?


# END of CIF
_refine_special_details          SQUEEZE
####################################################################### 
# 
# 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_LHCl
_database_code_depnum_ccdc_archive 'CCDC 1869191'
_audit_update_record             
;
2018-09-22 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_date             2018-08-02T20:41:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C33 H42 Cl10 N4'
_chemical_formula_weight         849.2

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.0787(16)
_cell_length_b                   21.553(3)
_cell_length_c                   24.176(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.498(9)
_cell_angle_gamma                90
_cell_volume                     8352.1(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    34
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      19.83
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.36
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3504
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 0 1 0.297
-8 -2 -3 0.348
2 -19 -1 0.311
-1 7 0 0.218
-6 -2 -1 0.273
13 12 3 0.247
10 -12 1 0.271
-1 2 0 0.247
-1 -2 -2 0.166
1 2 2 0.228
6 5 -8 0.227
-8 -5 9 0.283
2 -3 2 0.258


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_number            26951
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.073
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_Friedel_coverage         0
_reflns_number_total             7326
_reflns_number_gt                5441
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0927P)²+21.5535P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7326
_refine_ls_number_parameters     446
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.1988
_refine_ls_wR_factor_gt          0.1865
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.07

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.93526(16) 0.11267(13) 0.51180(10) 0.0313(6) Uani 1 1 d . . . . .
N2 N 0.84333(16) 0.07693(13) 0.57459(11) 0.0289(6) Uani 1 1 d . . . . .
N3 N 1.01098(16) 0.07113(13) 0.64520(10) 0.0299(6) Uani 1 1 d . . . . .
N4 N 0.99265(16) 0.17019(13) 0.63352(11) 0.0304(6) Uani 1 1 d . . . . .
Cl1 Cl 0.80519(5) 0.10429(4) 0.69854(3) 0.0354(2) Uani 1 1 d . . . . .
C1 C 0.91674(18) 0.10150(15) 0.56135(12) 0.0262(7) Uani 1 1 d . . . . .
C2 C 0.97346(18) 0.11453(15) 0.61216(12) 0.0266(7) Uani 1 1 d . . . . .
C3 C 1.0428(2) 0.16190(18) 0.68172(14) 0.0372(8) Uani 1 1 d . . . . .
H3 H 1.065287 0.193811 0.705537 0.045 Uiso 1 1 calc R U . . .
C4 C 1.0543(2) 0.10059(18) 0.68909(13) 0.0367(8) Uani 1 1 d . . . . .
H4 H 1.086328 0.081204 0.718958 0.044 Uiso 1 1 calc R U . . .
C11 C 1.01674(19) 0.13179(16) 0.50106(12) 0.0287(7) Uani 1 1 d . . . . .
C12 C 1.0860(2) 0.09464(17) 0.51329(14) 0.0349(8) Uani 1 1 d . . . . .
H12 H 1.080476 0.056696 0.532661 0.042 Uiso 1 1 calc R U . . .
C13 C 1.1633(2) 0.11256(18) 0.49740(14) 0.0388(8) Uani 1 1 d . . . . .
H13 H 1.210188 0.086419 0.505831 0.047 Uiso 1 1 calc R U . . .
C14 C 1.1738(2) 0.16757(18) 0.46959(14) 0.0387(8) Uani 1 1 d . . . . .
C15 C 1.1040(2) 0.20420(17) 0.45684(15) 0.0402(8) Uani 1 1 d . . . . .
H15 H 1.109635 0.241987 0.43725 0.048 Uiso 1 1 calc R U . . .
C16 C 1.0264(2) 0.18676(16) 0.47208(14) 0.0340(8) Uani 1 1 d . . . . .
H16 H 0.979381 0.212424 0.462739 0.041 Uiso 1 1 calc R U . . .
C17 C 1.2587(3) 0.1852(2) 0.45121(19) 0.0573(11) Uani 1 1 d . . . . .
H17A H 1.254851 0.225428 0.432223 0.086 Uiso 1 1 calc R U . . .
H17B H 1.298939 0.188128 0.483732 0.086 Uiso 1 1 calc R U . . .
H17C H 1.277241 0.153569 0.425806 0.086 Uiso 1 1 calc R U . . .
C21 C 0.77899(19) 0.05004(15) 0.53967(13) 0.0282(7) Uani 1 1 d . . . . .
C22 C 0.7739(2) 0.05227(18) 0.48209(13) 0.0354(8) Uani 1 1 d . . . . .
H22 H 0.814668 0.074081 0.463354 0.042 Uiso 1 1 calc R U . . .
C23 C 0.7086(2) 0.02230(19) 0.45232(14) 0.0394(8) Uani 1 1 d . . . . .
H23 H 0.705735 0.023842 0.412949 0.047 Uiso 1 1 calc R U . . .
C24 C 0.6475(2) -0.00982(17) 0.47765(15) 0.0372(8) Uani 1 1 d . . . . .
C25 C 0.6525(2) -0.01015(17) 0.53490(15) 0.0392(8) Uani 1 1 d . . . . .
H25 H 0.610689 -0.03091 0.553502 0.047 Uiso 1 1 calc R U . . .
C26 C 0.7173(2) 0.01916(17) 0.56582(14) 0.0356(8) Uani 1 1 d . . . . .
H26 H 0.719468 0.018112 0.605191 0.043 Uiso 1 1 calc R U . . .
C27 C 0.5791(2) -0.0442(2) 0.44406(18) 0.0542(11) Uani 1 1 d . . . . .
H27A H 0.585802 -0.038572 0.404434 0.081 Uiso 1 1 calc R U . . .
H27B H 0.582239 -0.088464 0.453217 0.081 Uiso 1 1 calc R U . . .
H27C H 0.524708 -0.027844 0.452721 0.081 Uiso 1 1 calc R U . . .
C31 C 1.0082(2) 0.00305(15) 0.63610(13) 0.0297(7) Uani 1 1 d . . . . .
C32 C 1.0947(2) -0.02464(18) 0.64841(15) 0.0382(8) Uani 1 1 d . . . . .
H32A H 1.13414 -0.004927 0.624285 0.046 Uiso 1 1 calc R U . . .
H32B H 1.114489 -0.016144 0.687487 0.046 Uiso 1 1 calc R U . . .
C33 C 1.0931(2) -0.09435(18) 0.63842(15) 0.0425(9) Uani 1 1 d . . . . .
H33A H 1.148993 -0.111915 0.648962 0.051 Uiso 1 1 calc R U . . .
H33B H 1.079433 -0.102643 0.598467 0.051 Uiso 1 1 calc R U . . .
C34 C 1.0287(3) -0.12587(19) 0.67213(16) 0.0471(10) Uani 1 1 d . . . . .
H34A H 1.02601 -0.1706 0.662865 0.057 Uiso 1 1 calc R U . . .
H34B H 1.04611 -0.121909 0.712167 0.057 Uiso 1 1 calc R U . . .
C35 C 0.9430(2) -0.09717(18) 0.66034(16) 0.0439(9) Uani 1 1 d . . . . .
H35A H 0.92292 -0.105428 0.621277 0.053 Uiso 1 1 calc R U . . .
H35B H 0.903541 -0.116811 0.684443 0.053 Uiso 1 1 calc R U . . .
C36 C 0.9445(2) -0.02761(16) 0.67041(14) 0.0349(8) Uani 1 1 d . . . . .
H36A H 0.958867 -0.019212 0.710277 0.042 Uiso 1 1 calc R U . . .
H36B H 0.888509 -0.010007 0.660186 0.042 Uiso 1 1 calc R U . . .
C41 C 0.9632(2) 0.23111(16) 0.61144(16) 0.0360(8) Uani 1 1 d . . . . .
C42 C 1.0374(3) 0.27195(18) 0.60047(19) 0.0498(10) Uani 1 1 d . . . . .
H42A H 1.072406 0.278801 0.635469 0.06 Uiso 1 1 calc R U . . .
H42B H 1.071926 0.251115 0.573853 0.06 Uiso 1 1 calc R U . . .
C43 C 1.0064(3) 0.3338(2) 0.5769(2) 0.0702(14) Uani 1 1 d . . . . .
H43A H 0.975831 0.326957 0.540219 0.084 Uiso 1 1 calc R U . . .
H43B H 1.054725 0.360953 0.57144 0.084 Uiso 1 1 calc R U . . .
C44 C 0.9493(3) 0.3657(2) 0.6152(3) 0.0819(17) Uani 1 1 d . . . . .
H44A H 0.92836 0.404963 0.598056 0.098 Uiso 1 1 calc R U . . .
H44B H 0.981065 0.375781 0.650773 0.098 Uiso 1 1 calc R U . . .
C45 C 0.8752(3) 0.3236(2) 0.6262(3) 0.0719(14) Uani 1 1 d . . . . .
H45A H 0.839986 0.344366 0.65241 0.086 Uiso 1 1 calc R U . . .
H45B H 0.840691 0.316403 0.591011 0.086 Uiso 1 1 calc R U . . .
C46 C 0.9062(3) 0.26140(19) 0.65043(19) 0.0502(10) Uani 1 1 d . . . . .
H46A H 0.93676 0.268148 0.687094 0.06 Uiso 1 1 calc R U . . .
H46B H 0.858066 0.233929 0.655602 0.06 Uiso 1 1 calc R U . . .
H31 H 0.9944(19) -0.0004(14) 0.5996(14) 0.019(8) Uiso 1 1 d . . . . .
H2 H 0.834(2) 0.0777(16) 0.6081(15) 0.026(9) Uiso 1 1 d . . . . .
H41 H 0.933(2) 0.2222(18) 0.5746(16) 0.041(10) Uiso 1 1 d . . . . .
C1D C 0.7071(3) 0.1812(3) 0.8045(2) 0.0794(16) Uani 1 1 d . . . . .
H1D H 0.726405 0.154468 0.774193 0.095 Uiso 1 1 calc R U . . .
Cl2 Cl 0.74662(10) 0.15063(8) 0.86823(6) 0.0926(5) Uani 1 1 d . . . . .
Cl3 Cl 0.74755(14) 0.25696(8) 0.79693(8) 0.1086(6) Uani 1 1 d . . . . .
Cl4 Cl 0.59934(12) 0.18117(17) 0.79967(11) 0.1658(12) Uani 1 1 d . . . . .
C2D C 0.8348(3) 0.3155(2) 0.39182(19) 0.0551(11) Uani 1 1 d . . . . .
H2D H 0.798004 0.34823 0.373721 0.066 Uiso 1 1 calc R U . . .
Cl5 Cl 0.83357(10) 0.25190(8) 0.34838(8) 0.1026(6) Uani 1 1 d . . . . .
Cl6 Cl 0.79458(12) 0.29418(9) 0.45406(7) 0.1040(6) Uani 1 1 d . . . . .
Cl7 Cl 0.93366(11) 0.34533(9) 0.40346(10) 0.1217(8) Uani 1 1 d . . . . .
C3D C 0.6737(3) -0.0140(2) 0.72671(18) 0.0617(12) Uani 1 1 d . . . . .
H3D H 0.711558 0.020987 0.718335 0.074 Uiso 1 1 calc R U . A 1
Cl8 Cl 0.57962(11) 0.00098(13) 0.68984(7) 0.1257(8) Uani 1 1 d . . . . .
Cl10 Cl 0.66247(14) -0.01033(13) 0.79698(6) 0.1369(9) Uani 1 1 d . . . . .
Cl9 Cl 0.7325(12) -0.0813(4) 0.7232(16) 0.149(6) Uani 0.46(4) 1 d . . P B 1
Cl9' Cl 0.7006(13) -0.0851(4) 0.6960(6) 0.118(4) Uani 0.54(4) 1 d . . P B 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 1.280(4) . ?
N1 C11 1.417(4) . ?
N2 C1 1.355(4) . ?
N2 C21 1.408(4) . ?
N3 C2 1.342(4) . ?
N3 C4 1.378(4) . ?
N3 C31 1.484(4) . ?
N4 C2 1.332(4) . ?
N4 C3 1.376(4) . ?
N4 C41 1.481(5) . ?
C1 C2 1.498(4) . ?
C3 C4 1.344(5) . ?
C11 C12 1.385(5) . ?
C11 C16 1.391(5) . ?
C12 C13 1.385(5) . ?
C13 C14 1.380(5) . ?
C14 C15 1.387(5) . ?
C14 C17 1.517(5) . ?
C15 C16 1.380(5) . ?
C21 C22 1.389(5) . ?
C21 C26 1.387(5) . ?
C22 C23 1.385(5) . ?
C23 C24 1.384(5) . ?
C24 C25 1.380(5) . ?
C24 C27 1.510(5) . ?
C25 C26 1.386(5) . ?
C31 C36 1.519(5) . ?
C31 C32 1.521(5) . ?
C32 C33 1.522(5) . ?
C33 C34 1.526(5) . ?
C34 C35 1.516(6) . ?
C35 C36 1.519(5) . ?
C41 C46 1.514(5) . ?
C41 C42 1.522(5) . ?
C42 C43 1.518(6) . ?
C43 C44 1.519(8) . ?
C44 C45 1.536(7) . ?
C45 C46 1.531(6) . ?
C1D Cl4 1.728(6) . ?
C1D Cl2 1.748(6) . ?
C1D Cl3 1.773(6) . ?
C2D Cl7 1.717(5) . ?
C2D Cl5 1.726(5) . ?
C2D Cl6 1.745(5) . ?
C3D Cl8 1.725(5) . ?
C3D Cl10 1.724(5) . ?
C3D Cl9 1.738(12) . ?
C3D Cl9' 1.770(9) . ?

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 C11 120.8(3) . . ?
C1 N2 C21 129.2(3) . . ?
C2 N3 C4 108.3(3) . . ?
C2 N3 C31 126.5(3) . . ?
C4 N3 C31 125.3(3) . . ?
C2 N4 C3 108.3(3) . . ?
C2 N4 C41 126.9(3) . . ?
C3 N4 C41 124.7(3) . . ?
N1 C1 N2 124.5(3) . . ?
N1 C1 C2 124.1(3) . . ?
N2 C1 C2 111.4(3) . . ?
N4 C2 N3 108.5(3) . . ?
N4 C2 C1 126.5(3) . . ?
N3 C2 C1 125.0(3) . . ?
C4 C3 N4 107.8(3) . . ?
C3 C4 N3 107.1(3) . . ?
C12 C11 C16 118.7(3) . . ?
C12 C11 N1 122.2(3) . . ?
C16 C11 N1 118.8(3) . . ?
C13 C12 C11 120.3(3) . . ?
C14 C13 C12 121.4(3) . . ?
C13 C14 C15 118.0(3) . . ?
C13 C14 C17 120.4(4) . . ?
C15 C14 C17 121.6(4) . . ?
C16 C15 C14 121.2(3) . . ?
C15 C16 C11 120.4(3) . . ?
C22 C21 C26 119.0(3) . . ?
C22 C21 N2 124.7(3) . . ?
C26 C21 N2 116.2(3) . . ?
C21 C22 C23 119.2(3) . . ?
C24 C23 C22 122.6(3) . . ?
C25 C24 C23 117.3(3) . . ?
C25 C24 C27 121.3(3) . . ?
C23 C24 C27 121.4(3) . . ?
C24 C25 C26 121.4(3) . . ?
C25 C26 C21 120.4(3) . . ?
N3 C31 C36 111.3(3) . . ?
N3 C31 C32 110.0(3) . . ?
C36 C31 C32 111.6(3) . . ?
C33 C32 C31 110.6(3) . . ?
C32 C33 C34 111.0(3) . . ?
C35 C34 C33 111.2(3) . . ?
C36 C35 C34 111.7(3) . . ?
C35 C36 C31 110.1(3) . . ?
N4 C41 C46 110.5(3) . . ?
N4 C41 C42 110.1(3) . . ?
C46 C41 C42 112.4(3) . . ?
C43 C42 C41 109.5(3) . . ?
C42 C43 C44 111.4(4) . . ?
C43 C44 C45 110.6(4) . . ?
C46 C45 C44 110.5(4) . . ?
C41 C46 C45 109.5(4) . . ?
Cl4 C1D Cl2 110.7(3) . . ?
Cl4 C1D Cl3 111.5(4) . . ?
Cl2 C1D Cl3 109.1(3) . . ?
Cl7 C2D Cl5 111.3(3) . . ?
Cl7 C2D Cl6 111.0(3) . . ?
Cl5 C2D Cl6 109.2(3) . . ?
Cl8 C3D Cl10 110.2(3) . . ?
Cl8 C3D Cl9 126.1(12) . . ?
Cl10 C3D Cl9 100.8(12) . . ?
Cl8 C3D Cl9' 100.3(8) . . ?
Cl10 C3D Cl9' 120.0(5) . . ?


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

data_2_ZnCl2_3CH2Cl2
_database_code_depnum_ccdc_archive 'CCDC 1869189'
_audit_update_record             
;
2018-09-22 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_2_ZnCl2_3CH2Cl2     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Low quality of the crystal
;
_vrf_PLAT220_2_ZnCl2_3CH2Cl2     
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        6.2 Ratio
RESPONSE: There is one disordered carbon atom that was not treated
;
_vrf_PLAT990_2_ZnCl2_3CH2Cl2     
;
PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE Job ...          ! Note
RESPONSE: Shelxl 97 version was used for the Squeeze Job
;
# Added during the CSD deposition process: Saturday 22 September 2018 06:22 PM
# end Validation Reply Form


_audit_creation_date             2018-08-03T16:17:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C64 H80 Cl12 N8 Zn2'
_chemical_formula_sum            'C64 H80 Cl12 N8 Zn2'
_chemical_formula_weight         1517.5

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_Int_Tables_number      61
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   21.712(2)
_cell_length_b                   13.037(2)
_cell_length_c                   54.215(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15346(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    105
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      19.76
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6272

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_T_max  0.770

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.1419
_diffrn_reflns_av_unetI/netI     0.1645
_diffrn_reflns_number            59272
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_theta_min         3.006
_diffrn_reflns_theta_max         23.707
_diffrn_reflns_theta_full        23.707
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_Friedel_coverage         0
_reflns_number_total             11612
_reflns_number_gt                5166
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-2008 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1225P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         11612
_refine_ls_number_parameters     721
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1887
_refine_ls_R_factor_gt           0.0848
_refine_ls_wR_factor_ref         0.2526
_refine_ls_wR_factor_gt          0.2178
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.981
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.088

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.013 -0.009 0.000 951 229 ' '
2 0.896 0.066 0.211 152 34 ' '
3 0.396 0.066 0.289 152 33 ' '
4 0.542 0.009 0.500 951 230 ' '
5 0.604 -0.066 0.711 153 35 ' '
6 0.104 -0.066 0.789 152 33 ' '
7 0.896 0.434 0.711 152 36 ' '
8 0.396 0.434 0.789 152 34 ' '
9 0.604 0.566 0.211 152 34 ' '
10 0.104 0.566 0.289 152 32 ' '
_platon_squeeze_details          
;
There is 3 dichlorometane molecules per molecular compound, two of them 
presented severe disorder and it was not possible to get a 
chemical sensible model for it, so Squeeze procedure was used to remove 
its contribution to the structure factors.
;

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.57710(5) 0.65091(8) 0.11284(2) 0.0589(4) Uani 1 1 d . . . . .
Zn2 Zn 0.44174(5) 0.73143(8) 0.12824(2) 0.0619(4) Uani 1 1 d . . . . .
Cl3 Cl 0.62367(9) 0.53727(18) 0.13706(4) 0.0573(7) Uani 1 1 d . . . . .
Cl4 Cl 0.39208(12) 0.85436(19) 0.10845(5) 0.0801(9) Uani 1 1 d . . . . .
Cl5 Cl 0.47708(11) 0.60289(18) 0.10108(5) 0.0759(9) Uani 1 1 d . . . . .
Cl6 Cl 0.39099(12) 0.6596(2) 0.15869(6) 0.0886(10) Uani 1 1 d . . . . .
Cl7 Cl 0.54128(11) 0.7830(2) 0.13865(6) 0.0850(9) Uani 1 1 d . . . . .
Cl8 Cl 0.63074(13) 0.7083(2) 0.08153(5) 0.0890(9) Uani 1 1 d . . . . .
N1 N 1.1719(3) 0.7146(5) 0.15847(12) 0.0370(16) Uani 1 1 d . . . . .
N2 N 1.1931(3) 0.8276(5) 0.12996(12) 0.0382(17) Uani 1 1 d . . . . .
N3 N 0.8005(3) 0.6996(5) 0.12034(12) 0.0373(17) Uani 1 1 d . . . . .
N4 N 0.8473(3) 0.6212(5) 0.09038(12) 0.0388(17) Uani 1 1 d . . . . .
N5 N 1.0468(3) 0.8195(5) 0.12490(11) 0.0351(17) Uani 1 1 d . . . . .
N6 N 1.0627(3) 0.8648(5) 0.16583(13) 0.0413(18) Uani 1 1 d . . . . .
N7 N 0.9384(3) 0.7859(5) 0.12607(12) 0.0395(17) Uani 1 1 d . . . . .
N8 N 0.9071(3) 0.8425(6) 0.08698(13) 0.0490(19) Uani 1 1 d . . . . .
C1 C 0.9844(3) 0.8674(6) 0.12607(15) 0.037(2) Uani 1 1 d . . . . .
H1A H 0.980546 0.909128 0.141249 0.044 Uiso 1 1 calc R U . . .
H1B H 0.978128 0.912886 0.111663 0.044 Uiso 1 1 calc R U . . .
C2 C 0.9000(3) 0.7793(6) 0.10502(15) 0.035(2) Uani 1 1 d . . . . .
C3 C 1.0825(3) 0.8255(6) 0.14541(16) 0.035(2) Uani 1 1 d . . . . .
C4 C 1.1478(3) 0.7850(6) 0.14329(15) 0.033(2) Uani 1 1 d . . . . .
C5 C 1.2475(4) 0.7823(6) 0.13716(16) 0.042(2) Uani 1 1 d . . . . .
H5 H 1.287316 0.797689 0.130943 0.051 Uiso 1 1 calc R U . . .
C6 C 1.2343(4) 0.7133(7) 0.15429(15) 0.044(2) Uani 1 1 d . . . . .
H6 H 1.263185 0.670086 0.162352 0.053 Uiso 1 1 calc R U . . .
C7 C 0.8517(3) 0.6984(6) 0.10635(14) 0.032(2) Uani 1 1 d . . . . .
C8 C 0.7928(4) 0.5736(7) 0.09385(17) 0.057(3) Uani 1 1 d . . . . .
H8 H 0.777625 0.516944 0.084673 0.069 Uiso 1 1 calc R U . . .
C9 C 0.7636(4) 0.6213(7) 0.11287(16) 0.053(2) Uani 1 1 d . . . . .
H9 H 0.724721 0.603351 0.119646 0.064 Uiso 1 1 calc R U . . .
C11 C 1.1375(4) 0.6438(6) 0.17490(14) 0.042(2) Uani 1 1 d . . . . .
C12 C 1.1414(4) 0.5363(6) 0.16563(16) 0.051(2) Uani 1 1 d . . . . .
H12A H 1.125415 0.533063 0.148545 0.061 Uiso 1 1 calc R U . . .
H12B H 1.184955 0.513887 0.165417 0.061 Uiso 1 1 calc R U . . .
C13 C 1.1037(4) 0.4643(7) 0.18226(18) 0.059(3) Uani 1 1 d . . . . .
H13A H 1.059471 0.482443 0.181057 0.071 Uiso 1 1 calc R U . . .
H13B H 1.108608 0.39276 0.176496 0.071 Uiso 1 1 calc R U . . .
C14 C 1.1236(5) 0.4719(8) 0.2081(2) 0.076(3) Uani 1 1 d . . . . .
H14A H 1.164927 0.4406 0.209623 0.091 Uiso 1 1 calc R U . . .
H14B H 1.094908 0.431546 0.218441 0.091 Uiso 1 1 calc R U . . .
C15 C 1.1263(5) 0.5831(8) 0.21816(17) 0.078(3) Uani 1 1 d . . . . .
H15A H 1.084162 0.611582 0.219546 0.093 Uiso 1 1 calc R U . . .
H15B H 1.14535 0.583571 0.234748 0.093 Uiso 1 1 calc R U . . .
C16 C 1.1639(4) 0.6472(7) 0.20072(16) 0.062(3) Uani 1 1 d . . . . .
H16A H 1.164654 0.719073 0.206612 0.074 Uiso 1 1 calc R U . . .
H16B H 1.206785 0.621504 0.200446 0.074 Uiso 1 1 calc R U . . .
C21 C 1.1860(4) 0.9060(6) 0.11022(15) 0.043(2) Uani 1 1 d . . . . .
C22 C 1.2244(4) 1.0024(7) 0.11666(17) 0.059(3) Uani 1 1 d . . . . .
H22A H 1.209034 1.033676 0.132129 0.071 Uiso 1 1 calc R U . . .
H22B H 1.268139 0.983604 0.11899 0.071 Uiso 1 1 calc R U . . .
C23 C 1.2180(5) 1.0789(7) 0.09520(16) 0.062(3) Uani 1 1 d . . . . .
H23A H 1.243889 1.139684 0.098659 0.074 Uiso 1 1 calc R U . . .
H23B H 1.174634 1.102156 0.094232 0.074 Uiso 1 1 calc R U . . .
C24 C 1.2365(5) 1.0341(7) 0.07056(18) 0.070(3) Uani 1 1 d . . . . .
H24A H 1.281323 1.019801 0.070629 0.084 Uiso 1 1 calc R U . . .
H24B H 1.22815 1.084727 0.057377 0.084 Uiso 1 1 calc R U . . .
C25 C 1.2022(5) 0.9371(8) 0.06521(17) 0.072(3) Uani 1 1 d . . . . .
H25A H 1.218403 0.906497 0.049815 0.087 Uiso 1 1 calc R U . . .
H25B H 1.158171 0.953584 0.062502 0.087 Uiso 1 1 calc R U . . .
C26 C 1.2074(4) 0.8589(6) 0.08596(14) 0.047(2) Uani 1 1 d . . . . .
H26A H 1.181841 0.798194 0.082057 0.056 Uiso 1 1 calc R U . . .
H26B H 1.250717 0.836194 0.08755 0.056 Uiso 1 1 calc R U . . .
C31 C 0.7875(4) 0.7729(6) 0.13986(15) 0.044(2) Uani 1 1 d . . . . .
C32 C 0.7307(4) 0.8390(7) 0.13322(17) 0.058(3) Uani 1 1 d . . . . .
H32A H 0.694251 0.794232 0.131131 0.07 Uiso 1 1 calc R U . . .
H32B H 0.738167 0.875034 0.117428 0.07 Uiso 1 1 calc R U . . .
C33 C 0.7184(5) 0.9172(8) 0.15356(17) 0.067(3) Uani 1 1 d . . . . .
H33A H 0.754634 0.962564 0.155518 0.081 Uiso 1 1 calc R U . . .
H33B H 0.682573 0.960238 0.14903 0.081 Uiso 1 1 calc R U . . .
C34 C 0.7054(5) 0.8615(9) 0.1779(2) 0.086(4) Uani 1 1 d . . . . .
H34A H 0.667311 0.820326 0.176237 0.103 Uiso 1 1 calc R U . . .
H34B H 0.699014 0.912414 0.191161 0.103 Uiso 1 1 calc R U . . .
C35 C 0.7590(5) 0.7917(8) 0.18452(17) 0.078(3) Uani 1 1 d . . . . .
H35A H 0.796009 0.834101 0.187566 0.093 Uiso 1 1 calc R U . . .
H35B H 0.749083 0.754811 0.199988 0.093 Uiso 1 1 calc R U . . .
C36 C 0.7736(4) 0.7115(7) 0.16383(15) 0.057(3) Uani 1 1 d . . . . .
H36A H 0.738003 0.66535 0.161273 0.068 Uiso 1 1 calc R U . . .
H36B H 0.809752 0.669457 0.168516 0.068 Uiso 1 1 calc R U . . .
C41 C 0.8930(4) 0.5891(7) 0.07149(15) 0.045(2) Uani 1 1 d . . . . .
C42 C 0.8659(4) 0.5910(8) 0.04616(15) 0.062(3) Uani 1 1 d . . . . .
H42A H 0.82964 0.544998 0.045529 0.074 Uiso 1 1 calc R U . . .
H42B H 0.851993 0.661362 0.042182 0.074 Uiso 1 1 calc R U . . .
C43 C 0.9134(5) 0.5563(9) 0.02726(19) 0.078(3) Uani 1 1 d . . . . .
H43A H 0.948068 0.605553 0.026882 0.093 Uiso 1 1 calc R U . . .
H43B H 0.894411 0.554632 0.010665 0.093 Uiso 1 1 calc R U . . .
C44 C 0.9375(4) 0.4491(8) 0.0339(2) 0.072(3) Uani 1 1 d . . . . .
H44A H 0.903561 0.399048 0.032053 0.087 Uiso 1 1 calc R U . . .
H44B H 0.970299 0.430022 0.022079 0.087 Uiso 1 1 calc R U . . .
C45 C 0.9625(4) 0.4414(7) 0.05929(18) 0.062(3) Uani 1 1 d . . . . .
H45A H 1.000938 0.481863 0.060486 0.075 Uiso 1 1 calc R U . . .
H45B H 0.972481 0.368948 0.062988 0.075 Uiso 1 1 calc R U . . .
C46 C 0.9164(4) 0.4808(7) 0.07801(15) 0.057(3) Uani 1 1 d . . . . .
H46A H 0.880975 0.433081 0.0788 0.068 Uiso 1 1 calc R U . . .
H46B H 0.935955 0.482395 0.094502 0.068 Uiso 1 1 calc R U . . .
C51 C 1.0620(3) 0.7638(6) 0.10322(14) 0.0299(19) Uani 1 1 d . . . . .
C52 C 1.0799(3) 0.6647(6) 0.10446(14) 0.034(2) Uani 1 1 d . . . . .
H52 H 1.082711 0.630802 0.119927 0.041 Uiso 1 1 calc R U . . .
C53 C 1.0942(3) 0.6125(7) 0.08248(18) 0.050(2) Uani 1 1 d . . . . .
H53 H 1.107571 0.543159 0.083318 0.059 Uiso 1 1 calc R U . . .
C54 C 1.0894(4) 0.6590(7) 0.05993(17) 0.044(2) Uani 1 1 d . . . . .
C55 C 1.0690(3) 0.7588(7) 0.05965(15) 0.047(2) Uani 1 1 d . . . . .
H55 H 1.064175 0.792426 0.044226 0.056 Uiso 1 1 calc R U . . .
C56 C 1.0552(3) 0.8122(6) 0.08113(14) 0.036(2) Uani 1 1 d . . . . .
H56 H 1.041191 0.881191 0.080419 0.043 Uiso 1 1 calc R U . . .
C57 C 1.1053(4) 0.6002(7) 0.03658(15) 0.058(3) Uani 1 1 d . . . . .
H57A H 1.099344 0.644764 0.022216 0.087 Uiso 1 1 calc R U . . .
H57B H 1.148383 0.577938 0.037295 0.087 Uiso 1 1 calc R U . . .
H57C H 1.078468 0.540086 0.035169 0.087 Uiso 1 1 calc R U . . .
C61 C 1.0983(4) 0.8831(6) 0.18715(15) 0.040(2) Uani 1 1 d . . . . .
C62 C 1.0742(4) 0.8596(7) 0.20943(16) 0.051(2) Uani 1 1 d . . . . .
H62 H 1.033515 0.83307 0.210283 0.061 Uiso 1 1 calc R U . . .
C63 C 1.1075(5) 0.8732(8) 0.23129(17) 0.067(3) Uani 1 1 d . . . . .
H63 H 1.089414 0.855402 0.246655 0.081 Uiso 1 1 calc R U . . .
C64 C 1.1668(4) 0.9124(8) 0.23064(17) 0.060(3) Uani 1 1 d . . . . .
C65 C 1.1907(4) 0.9414(7) 0.20779(18) 0.054(2) Uani 1 1 d . . . . .
H65 H 1.230737 0.970447 0.206894 0.065 Uiso 1 1 calc R U . . .
C66 C 1.1568(4) 0.9283(6) 0.18640(15) 0.041(2) Uani 1 1 d . . . . .
H66 H 1.173371 0.950097 0.171062 0.049 Uiso 1 1 calc R U . . .
C67 C 1.2055(4) 0.9223(8) 0.25381(16) 0.075(3) Uani 1 1 d . . . . .
H67A H 1.181577 0.898635 0.268059 0.112 Uiso 1 1 calc R U . . .
H67B H 1.242703 0.880394 0.252157 0.112 Uiso 1 1 calc R U . . .
H67C H 1.217077 0.99425 0.256203 0.112 Uiso 1 1 calc R U . . .
C71 C 0.9375(3) 0.7174(6) 0.14568(16) 0.038(2) Uani 1 1 d . . . . .
C72 C 0.9303(3) 0.7552(6) 0.17012(16) 0.044(2) Uani 1 1 d . . . . .
H72 H 0.925521 0.82674 0.172904 0.052 Uiso 1 1 calc R U . . .
C73 C 0.9301(4) 0.6902(8) 0.18915(15) 0.045(2) Uani 1 1 d . . . . .
H73 H 0.925369 0.717345 0.205296 0.054 Uiso 1 1 calc R U . . .
C74 C 0.9364(4) 0.5843(9) 0.18648(19) 0.059(3) Uani 1 1 d . . . . .
C75 C 0.9428(4) 0.5454(7) 0.1632(2) 0.056(3) Uani 1 1 d . . . . .
H75 H 0.946371 0.473528 0.160734 0.068 Uiso 1 1 calc R U . . .
C76 C 0.9441(3) 0.6139(7) 0.14263(16) 0.042(2) Uani 1 1 d . . . . .
H76 H 0.949552 0.586995 0.126497 0.05 Uiso 1 1 calc R U . . .
C77 C 0.9374(4) 0.5118(8) 0.20850(17) 0.073(3) Uani 1 1 d . . . . .
H77A H 0.942245 0.441073 0.202678 0.109 Uiso 1 1 calc R U . . .
H77B H 0.971947 0.529552 0.219326 0.109 Uiso 1 1 calc R U . . .
H77C H 0.898681 0.518053 0.217654 0.109 Uiso 1 1 calc R U . . .
C81 C 0.8665(4) 0.8470(7) 0.06652(16) 0.050(2) Uani 1 1 d . . . . .
C82 C 0.8948(5) 0.8638(10) 0.0441(2) 0.101(4) Uani 1 1 d . . . . .
H82 H 0.938366 0.869736 0.043017 0.122 Uiso 1 1 calc R U . . .
C83 C 0.8587(5) 0.8718(13) 0.02305(19) 0.132(6) Uani 1 1 d . . . . .
H83 H 0.878461 0.88152 0.007588 0.159 Uiso 1 1 calc R U . . .
C84 C 0.7947(5) 0.8662(12) 0.0237(2) 0.117(5) Uani 1 1 d . . . . .
C85 C 0.7700(5) 0.8511(9) 0.0466(2) 0.085(4) Uani 1 1 d . . . . .
H85 H 0.726428 0.848404 0.047803 0.102 Uiso 1 1 calc R U . . .
C86 C 0.8023(4) 0.8399(7) 0.06744(16) 0.058(3) Uani 1 1 d . . . . .
H86 H 0.781934 0.827318 0.082637 0.07 Uiso 1 1 calc R U . . .
C87 C 0.7579(6) 0.8781(15) 0.0009(2) 0.186(9) Uani 1 1 d . . . . .
H87A H 0.714015 0.871965 0.00488 0.28 Uiso 1 1 calc R U . . .
H87B H 0.765866 0.94571 -0.00633 0.28 Uiso 1 1 calc R U . . .
H87C H 0.769408 0.824593 -0.010914 0.28 Uiso 1 1 calc R U . . .
C1D C 0.6005(6) 0.1767(10) 0.2757(3) 0.123(5) Uani 1 1 d . . . . .
H1D1 H 0.601155 0.201338 0.293004 0.147 Uiso 1 1 calc R U . . .
H1D2 H 0.597024 0.101013 0.276187 0.147 Uiso 1 1 calc R U . . .
Cl1D Cl 0.5369(2) 0.2249(3) 0.26163(8) 0.1471(15) Uani 1 1 d . . . . .
Cl2D Cl 0.6673(2) 0.2075(3) 0.26246(12) 0.190(2) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 Cl8 2.190(3) . ?
Zn1 Cl3 2.223(3) . ?
Zn1 Cl5 2.348(2) . ?
Zn1 Cl7 2.351(3) . ?
Zn2 Cl6 2.194(3) . ?
Zn2 Cl4 2.209(3) . ?
Zn2 Cl7 2.333(3) . ?
Zn2 Cl5 2.359(3) . ?
N1 C4 1.340(9) . ?
N1 C6 1.373(9) . ?
N1 C11 1.484(10) . ?
N2 C4 1.342(9) . ?
N2 C5 1.376(9) . ?
N2 C21 1.488(10) . ?
N3 C7 1.346(9) . ?
N3 C9 1.359(10) . ?
N3 C31 1.454(10) . ?
N4 C7 1.331(9) . ?
N4 C8 1.349(10) . ?
N4 C41 1.486(10) . ?
N5 C3 1.358(9) . ?
N5 C51 1.420(9) . ?
N5 C1 1.493(9) . ?
N6 C3 1.293(9) . ?
N6 C61 1.411(10) . ?
N7 C71 1.389(10) . ?
N7 C2 1.417(9) . ?
N7 C1 1.458(9) . ?
N8 C2 1.288(9) . ?
N8 C81 1.417(10) . ?
C2 C7 1.489(10) . ?
C3 C4 1.516(10) . ?
C5 C6 1.324(10) . ?
C8 C9 1.362(11) . ?
C11 C16 1.513(11) . ?
C11 C12 1.491(11) . ?
C12 C13 1.538(11) . ?
C13 C14 1.468(12) . ?
C14 C15 1.551(14) . ?
C15 C16 1.502(12) . ?
C21 C26 1.524(11) . ?
C21 C22 1.548(11) . ?
C22 C23 1.538(11) . ?
C23 C24 1.513(12) . ?
C24 C25 1.497(12) . ?
C25 C26 1.522(11) . ?
C31 C32 1.545(11) . ?
C31 C36 1.555(11) . ?
C32 C33 1.526(11) . ?
C33 C34 1.530(13) . ?
C34 C35 1.520(13) . ?
C35 C36 1.566(11) . ?
C41 C46 1.542(12) . ?
C41 C42 1.494(11) . ?
C42 C43 1.523(12) . ?
C43 C44 1.535(13) . ?
C44 C45 1.482(13) . ?
C45 C46 1.514(11) . ?
C51 C52 1.350(10) . ?
C51 C56 1.362(10) . ?
C52 C53 1.407(11) . ?
C53 C54 1.369(11) . ?
C54 C55 1.375(11) . ?
C54 C57 1.519(11) . ?
C55 C56 1.390(11) . ?
C61 C62 1.352(11) . ?
C61 C66 1.400(11) . ?
C62 C63 1.400(12) . ?
C63 C64 1.385(12) . ?
C64 C65 1.395(12) . ?
C64 C67 1.516(11) . ?
C65 C66 1.384(11) . ?
C71 C76 1.366(11) . ?
C71 C72 1.422(11) . ?
C72 C73 1.336(11) . ?
C73 C74 1.394(13) . ?
C74 C75 1.367(12) . ?
C74 C77 1.523(12) . ?
C75 C76 1.430(11) . ?
C81 C86 1.397(11) . ?
C81 C82 1.382(12) . ?
C82 C83 1.387(13) . ?
C83 C84 1.393(14) . ?
C84 C87 1.477(14) . ?
C84 C85 1.367(13) . ?
C85 C86 1.339(12) . ?
C1D Cl2D 1.669(14) . ?
C1D Cl1D 1.699(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
Cl8 Zn1 Cl3 116.32(10) . . ?
Cl8 Zn1 Cl5 111.87(12) . . ?
Cl3 Zn1 Cl5 113.78(10) . . ?
Cl8 Zn1 Cl7 112.76(12) . . ?
Cl3 Zn1 Cl7 106.69(11) . . ?
Cl5 Zn1 Cl7 92.92(9) . . ?
Cl6 Zn2 Cl4 115.45(11) . . ?
Cl6 Zn2 Cl7 113.97(12) . . ?
Cl4 Zn2 Cl7 111.12(11) . . ?
Cl6 Zn2 Cl5 109.25(12) . . ?
Cl4 Zn2 Cl5 111.78(12) . . ?
Cl7 Zn2 Cl5 93.12(9) . . ?
Zn1 Cl5 Zn2 86.68(9) . . ?
Zn2 Cl7 Zn1 87.20(9) . . ?
C4 N1 C6 107.0(6) . . ?
C4 N1 C11 126.7(6) . . ?
C6 N1 C11 126.0(7) . . ?
C4 N2 C5 107.4(6) . . ?
C4 N2 C21 126.5(7) . . ?
C5 N2 C21 126.1(7) . . ?
C7 N3 C9 108.1(7) . . ?
C7 N3 C31 125.4(7) . . ?
C9 N3 C31 126.5(7) . . ?
C7 N4 C8 108.7(7) . . ?
C7 N4 C41 127.8(7) . . ?
C8 N4 C41 123.5(7) . . ?
C3 N5 C51 125.0(6) . . ?
C3 N5 C1 117.3(6) . . ?
C51 N5 C1 117.4(6) . . ?
C3 N6 C61 125.9(7) . . ?
C71 N7 C2 124.7(7) . . ?
C71 N7 C1 118.6(6) . . ?
C2 N7 C1 116.6(7) . . ?
C2 N8 C81 123.2(7) . . ?
N7 C1 N5 108.4(6) . . ?
N8 C2 N7 120.2(7) . . ?
N8 C2 C7 125.0(7) . . ?
N7 C2 C7 114.8(7) . . ?
N5 C3 N6 122.3(7) . . ?
N5 C3 C4 116.8(7) . . ?
N6 C3 C4 120.9(7) . . ?
N1 C4 N2 109.1(6) . . ?
N1 C4 C3 123.9(7) . . ?
N2 C4 C3 125.6(7) . . ?
C6 C5 N2 107.8(7) . . ?
C5 C6 N1 108.7(7) . . ?
N3 C7 N4 108.4(7) . . ?
N3 C7 C2 126.9(8) . . ?
N4 C7 C2 123.7(7) . . ?
C9 C8 N4 107.7(8) . . ?
C8 C9 N3 107.1(8) . . ?
N1 C11 C16 110.3(7) . . ?
N1 C11 C12 110.7(7) . . ?
C16 C11 C12 108.5(7) . . ?
C13 C12 C11 110.2(7) . . ?
C14 C13 C12 111.2(8) . . ?
C13 C14 C15 114.2(8) . . ?
C16 C15 C14 108.6(8) . . ?
C11 C16 C15 111.1(8) . . ?
N2 C21 C26 108.2(7) . . ?
N2 C21 C22 109.9(7) . . ?
C26 C21 C22 110.9(7) . . ?
C23 C22 C21 107.9(7) . . ?
C22 C23 C24 113.2(8) . . ?
C23 C24 C25 111.4(8) . . ?
C24 C25 C26 112.6(8) . . ?
C21 C26 C25 110.2(7) . . ?
N3 C31 C32 110.6(7) . . ?
N3 C31 C36 107.9(7) . . ?
C32 C31 C36 109.1(7) . . ?
C31 C32 C33 110.1(7) . . ?
C34 C33 C32 109.7(8) . . ?
C33 C34 C35 110.4(8) . . ?
C36 C35 C34 112.6(8) . . ?
C35 C36 C31 107.1(7) . . ?
N4 C41 C46 108.7(7) . . ?
N4 C41 C42 111.5(7) . . ?
C46 C41 C42 110.8(7) . . ?
C43 C42 C41 110.3(8) . . ?
C42 C43 C44 110.1(9) . . ?
C45 C44 C43 113.9(8) . . ?
C44 C45 C46 111.0(8) . . ?
C41 C46 C45 112.0(7) . . ?
C52 C51 C56 121.2(7) . . ?
C52 C51 N5 121.0(7) . . ?
C56 C51 N5 117.7(7) . . ?
C51 C52 C53 119.0(8) . . ?
C54 C53 C52 121.7(8) . . ?
C53 C54 C55 117.0(8) . . ?
C53 C54 C57 120.2(8) . . ?
C55 C54 C57 122.8(9) . . ?
C54 C55 C56 122.3(8) . . ?
C51 C56 C55 118.8(8) . . ?
C62 C61 N6 118.8(8) . . ?
C62 C61 C66 118.2(8) . . ?
N6 C61 C66 123.0(7) . . ?
C61 C62 C63 121.9(8) . . ?
C62 C63 C64 120.4(9) . . ?
C65 C64 C63 117.9(8) . . ?
C65 C64 C67 120.5(9) . . ?
C63 C64 C67 121.6(9) . . ?
C64 C65 C66 120.9(8) . . ?
C65 C66 C61 120.7(8) . . ?
C76 C71 N7 122.7(8) . . ?
C76 C71 C72 117.8(8) . . ?
N7 C71 C72 119.4(7) . . ?
C73 C72 C71 120.0(8) . . ?
C74 C73 C72 123.2(9) . . ?
C73 C74 C75 118.2(9) . . ?
C73 C74 C77 122.3(10) . . ?
C75 C74 C77 119.4(10) . . ?
C74 C75 C76 119.4(9) . . ?
C71 C76 C75 121.4(9) . . ?
C86 C81 N8 126.1(8) . . ?
C86 C81 C82 119.0(8) . . ?
N8 C81 C82 114.8(8) . . ?
C81 C82 C83 119.0(10) . . ?
C84 C83 C82 122.8(10) . . ?
C87 C84 C83 120.9(11) . . ?
C87 C84 C85 124.2(11) . . ?
C83 C84 C85 114.8(10) . . ?
C86 C85 C84 125.4(10) . . ?
C85 C86 C81 119.0(9) . . ?
Cl2D C1D Cl1D 115.1(8) . . ?


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

data_2_2Cl_13CH2Cl2
_database_code_depnum_ccdc_archive 'CCDC 1869190'
_audit_update_record             
;
2018-09-22 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_2_2Cl_13CH2Cl2      
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Low quality of the crystal
;
_vrf_PLAT340_2_2Cl_13CH2Cl2      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01314 Ang.
RESPONSE: There is some disorder in the molecule
;
# Added during the CSD deposition process: Saturday 22 September 2018 06:22 PM
# end Validation Reply Form


_audit_creation_date             2018-08-02T14:14:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C74  H1020  N8  Cl28'
_chemical_formula_sum            'C74 H102 Cl28 N8'
_chemical_formula_weight         2096.23

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.838(6)
_cell_length_b                   15.476(15)
_cell_length_c                   27.491(9)
_cell_angle_alpha                98.93(4)
_cell_angle_beta                 92.92(3)
_cell_angle_gamma                110.32(5)
_cell_volume                     5028(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    23
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      18.79
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.28
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2156

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_T_max  0.908

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.1069
_diffrn_reflns_av_unetI/netI     0.2205
_diffrn_reflns_number            55323
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         23.2
_diffrn_reflns_theta_full        23.2
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_reflns_Laue_measured_fraction_full 0.99
_diffrn_reflns_Laue_measured_fraction_max 0.99
_diffrn_reflns_point_group_measured_fraction_full 0.99
_diffrn_reflns_point_group_measured_fraction_max 0.99
_reflns_Friedel_coverage         0
_reflns_number_total             14192
_reflns_number_gt                5675
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_reflns_reduction_process 
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1326P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         14192
_refine_ls_number_parameters     986
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.198
_refine_ls_R_factor_gt           0.094
_refine_ls_wR_factor_ref         0.2905
_refine_ls_wR_factor_gt          0.2284
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_restrained_S_all      0.919
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.096

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.0187(5) 0.7325(4) 0.2700(2) 0.0356(17) Uani 1 1 d . . . . .
N2 N 0.1472(6) 0.8766(5) 0.2647(2) 0.0404(18) Uani 1 1 d . . . . .
N3 N 0.0840(5) 0.8350(4) 0.3828(2) 0.0355(17) Uani 1 1 d . . . . .
N4 N 0.0170(5) 0.9273(5) 0.3531(2) 0.0370(17) Uani 1 1 d . . . . .
N5 N -0.0613(5) 0.6811(4) 0.1852(2) 0.0371(17) Uani 1 1 d . . . . .
N6 N -0.1060(5) 0.5208(5) 0.1763(2) 0.0357(17) Uani 1 1 d . . . . .
N7 N -0.3297(5) 0.5282(4) 0.1294(2) 0.0379(17) Uani 1 1 d . . . . .
N8 N -0.2130(5) 0.6008(4) 0.0816(2) 0.0356(17) Uani 1 1 d . . . . .
Cl1 Cl 0.31839(17) 0.40128(15) 0.07321(7) 0.0465(6) Uani 1 1 d . . . . .
Cl2 Cl 0.08736(18) 0.87917(15) 0.54635(7) 0.0471(6) Uani 1 1 d . . . . .
C1 C 0.0370(6) 0.6969(6) 0.2201(3) 0.038(2) Uani 1 1 d . . . . .
H1A H 0.050043 0.637396 0.219616 0.046 Uiso 1 1 calc R U . . .
H1B H 0.104013 0.742737 0.210115 0.046 Uiso 1 1 calc R U . . .
C2 C 0.0805(7) 0.8248(6) 0.2902(3) 0.035(2) Uani 1 1 d . . . . .
C3 C 0.0573(6) 0.8594(6) 0.3410(3) 0.034(2) Uani 1 1 d . . . . .
C4 C 0.0185(7) 0.9469(6) 0.4041(3) 0.041(2) Uani 1 1 d . . . . .
H4 H -0.004638 0.992972 0.422477 0.049 Uiso 1 1 calc R U . . .
C5 C 0.0591(7) 0.8879(6) 0.4223(3) 0.041(2) Uani 1 1 d . . . . .
H5 H 0.068932 0.883556 0.456246 0.049 Uiso 1 1 calc R U . . .
C6 C -0.1272(7) 0.5889(6) 0.1639(3) 0.034(2) Uani 1 1 d . . . . .
C7 C -0.2225(7) 0.5787(6) 0.1253(3) 0.038(2) Uani 1 1 d . . . . .
C8 C -0.3186(7) 0.5662(6) 0.0550(3) 0.046(2) Uani 1 1 d . . . . .
H8 H -0.335834 0.572928 0.022158 0.055 Uiso 1 1 calc R U . . .
C9 C -0.3919(7) 0.5215(6) 0.0842(3) 0.040(2) Uani 1 1 d . . . . .
H9 H -0.470373 0.491214 0.076053 0.048 Uiso 1 1 calc R U . . .
C10 C -0.3347(8) 0.4887(6) 0.3593(3) 0.059(3) Uani 1 1 d . . . . .
H10A H -0.321199 0.430829 0.361562 0.089 Uiso 1 1 calc R U . . .
H10B H -0.336911 0.521044 0.392597 0.089 Uiso 1 1 calc R U . . .
H10C H -0.406231 0.473474 0.339255 0.089 Uiso 1 1 calc R U . . .
C11 C -0.0685(7) 0.6712(6) 0.2917(3) 0.035(2) Uani 1 1 d . . . . .
C12 C -0.0700(7) 0.5855(6) 0.2979(3) 0.039(2) Uani 1 1 d . . . . .
H12 H -0.010418 0.566517 0.287724 0.047 Uiso 1 1 calc R U . . .
C13 C -0.1539(8) 0.5257(6) 0.3181(3) 0.045(2) Uani 1 1 d . . . . .
H13 H -0.152612 0.465536 0.320617 0.054 Uiso 1 1 calc R U . . .
C14 C -0.2422(7) 0.5513(6) 0.3354(3) 0.044(2) Uani 1 1 d . . . . .
C15 C -0.2433(7) 0.6375(6) 0.3282(3) 0.043(2) Uani 1 1 d . . . . .
H15 H -0.30276 0.656199 0.338819 0.052 Uiso 1 1 calc R U . . .
C16 C -0.1591(7) 0.6984(6) 0.3057(3) 0.043(2) Uani 1 1 d . . . . .
C20 C 0.4317(8) 1.2597(7) 0.3305(3) 0.066(3) Uani 1 1 d . . . . .
H20A H 0.422138 1.294981 0.305036 0.098 Uiso 1 1 calc R U . . .
H20B H 0.409566 1.284557 0.361662 0.098 Uiso 1 1 calc R U . . .
H20C H 0.510189 1.265742 0.335517 0.098 Uiso 1 1 calc R U . . .
C21 C 0.2172(6) 0.9701(5) 0.2832(3) 0.034(2) Uani 1 1 d . . . . .
C22 C 0.2864(7) 0.9999(6) 0.3283(3) 0.046(2) Uani 1 1 d . . . . .
H22 H 0.285454 0.956348 0.349257 0.055 Uiso 1 1 calc R U . . .
C23 C 0.3553(7) 1.0915(6) 0.3420(3) 0.040(2) Uani 1 1 d . . . . .
H23 H 0.40243 1.109747 0.372408 0.048 Uiso 1 1 calc R U . . .
C24 C 0.3597(7) 1.1581(6) 0.3141(3) 0.042(2) Uani 1 1 d . . . . .
C25 C 0.2944(7) 1.1271(6) 0.2680(3) 0.047(2) Uani 1 1 d . . . . .
H25 H 0.297843 1.17027 0.246523 0.056 Uiso 1 1 calc R U . . .
C26 C 0.2257(7) 1.0354(6) 0.2535(3) 0.042(2) Uani 1 1 d . . . . .
H26 H 0.18255 1.016328 0.22202 0.05 Uiso 1 1 calc R U . . .
C31 C 0.1286(7) 0.7616(6) 0.3888(3) 0.040(2) Uani 1 1 d . . . . .
H31 H 0.12958 0.72677 0.35505 0.048 Uiso 1 1 calc R U . . .
C32 C 0.2500(7) 0.8029(6) 0.4151(3) 0.049(2) Uani 1 1 d . . . . .
H32A H 0.298687 0.846631 0.395799 0.058 Uiso 1 1 calc R U . . .
H32B H 0.25142 0.838521 0.448424 0.058 Uiso 1 1 calc R U . . .
C33 C 0.2935(8) 0.7256(7) 0.4196(4) 0.059(3) Uani 1 1 d . . . . .
H33A H 0.297583 0.693398 0.386127 0.07 Uiso 1 1 calc R U . . .
H33B H 0.369988 0.752882 0.437358 0.07 Uiso 1 1 calc R U . . .
C34 C 0.2202(8) 0.6558(7) 0.4470(4) 0.063(3) Uani 1 1 d . . . . .
H34A H 0.222964 0.686662 0.481627 0.076 Uiso 1 1 calc R U . . .
H34B H 0.249447 0.604586 0.447777 0.076 Uiso 1 1 calc R U . . .
C35 C 0.0983(8) 0.6137(7) 0.4234(4) 0.058(3) Uani 1 1 d . . . . .
H35A H 0.093206 0.574935 0.390491 0.069 Uiso 1 1 calc R U . . .
H35B H 0.05174 0.572947 0.444501 0.069 Uiso 1 1 calc R U . . .
C36 C 0.0554(8) 0.6918(6) 0.4177(3) 0.047(2) Uani 1 1 d . . . . .
H36A H 0.052164 0.725408 0.450974 0.056 Uiso 1 1 calc R U . . .
H36B H -0.021577 0.664141 0.400406 0.056 Uiso 1 1 calc R U . . .
C41 C -0.0250(7) 0.9778(5) 0.3194(3) 0.039(2) Uani 1 1 d . . . . .
H41 H -0.017475 0.952597 0.284567 0.047 Uiso 1 1 calc R U . . .
C42 C 0.0472(8) 1.0813(6) 0.3316(3) 0.050(2) Uani 1 1 d . . . . .
H42A H 0.040397 1.108328 0.365795 0.06 Uiso 1 1 calc R U . . .
H42B H 0.126602 1.089741 0.328909 0.06 Uiso 1 1 calc R U . . .
C43 C 0.0068(9) 1.1301(7) 0.2947(4) 0.066(3) Uani 1 1 d . . . . .
H43A H 0.014773 1.103314 0.260544 0.079 Uiso 1 1 calc R U . . .
H43B H 0.05308 1.197774 0.301334 0.079 Uiso 1 1 calc R U . . .
C44 C -0.1166(9) 1.1172(7) 0.2992(4) 0.069(3) Uani 1 1 d . . . . .
H44A H -0.142406 1.147721 0.274439 0.082 Uiso 1 1 calc R U . . .
H44B H -0.122914 1.148576 0.332512 0.082 Uiso 1 1 calc R U . . .
C45 C -0.1920(9) 1.0138(7) 0.2910(4) 0.064(3) Uani 1 1 d . . . . .
H45A H -0.268285 1.008821 0.29836 0.077 Uiso 1 1 calc R U . . .
H45B H -0.196535 0.984924 0.255802 0.077 Uiso 1 1 calc R U . . .
C46 C -0.1475(7) 0.9611(6) 0.3238(3) 0.042(2) Uani 1 1 d . . . . .
H46A H -0.156847 0.981671 0.358742 0.051 Uiso 1 1 calc R U . . .
H46B H -0.191519 0.89318 0.314371 0.051 Uiso 1 1 calc R U . . .
C50 C -0.1669(9) 0.9962(7) 0.1516(3) 0.064(3) Uani 1 1 d . . . . .
H50A H -0.102668 1.041445 0.14029 0.096 Uiso 1 1 calc R U . . .
H50B H -0.230568 0.973797 0.125786 0.096 Uiso 1 1 calc R U . . .
H50C H -0.186775 1.026455 0.181875 0.096 Uiso 1 1 calc R U . . .
C51 C -0.0875(7) 0.7599(5) 0.1784(3) 0.034(2) Uani 1 1 d . . . . .
C52 C -0.0086(7) 0.8343(6) 0.1631(3) 0.046(2) Uani 1 1 d . . . . .
H52 H 0.063423 0.832427 0.158306 0.055 Uiso 1 1 calc R U . . .
C53 C -0.0325(8) 0.9102(6) 0.1548(3) 0.050(2) Uani 1 1 d . . . . .
H53 H 0.022864 0.960123 0.14401 0.06 Uiso 1 1 calc R U . . .
C54 C -0.1378(8) 0.9161(6) 0.1620(3) 0.046(2) Uani 1 1 d . . . . .
C55 C -0.2155(8) 0.8409(6) 0.1789(3) 0.051(2) Uani 1 1 d . . . . .
H55 H -0.28698 0.842896 0.184692 0.061 Uiso 1 1 calc R U . . .
C56 C -0.1906(7) 0.7648(6) 0.1871(3) 0.042(2) Uani 1 1 d . . . . .
H56 H -0.244423 0.715244 0.198864 0.05 Uiso 1 1 calc R U . . .
C60 C -0.3013(8) 0.1312(6) 0.0945(3) 0.059(3) Uani 1 1 d . . . . .
H60A H -0.304625 0.096206 0.121535 0.089 Uiso 1 1 calc R U . . .
H60B H -0.376784 0.115069 0.077968 0.089 Uiso 1 1 calc R U . . .
H60C H -0.253965 0.11504 0.070547 0.089 Uiso 1 1 calc R U . . .
C61 C -0.1590(7) 0.4259(6) 0.1535(3) 0.038(2) Uani 1 1 d . . . . .
C62 C -0.1714(7) 0.3615(7) 0.1836(3) 0.048(2) Uani 1 1 d . . . . .
H62 H -0.146831 0.383099 0.217978 0.058 Uiso 1 1 calc R U . . .
C63 C -0.2177(8) 0.2673(6) 0.1662(3) 0.052(2) Uani 1 1 d . . . . .
H63 H -0.226189 0.224212 0.188172 0.062 Uiso 1 1 calc R U . . .
C64 C -0.2527(7) 0.2348(6) 0.1152(3) 0.044(2) Uani 1 1 d . . . . .
C65 C -0.2397(7) 0.2986(6) 0.0841(3) 0.039(2) Uani 1 1 d . . . . .
C66 C -0.1919(7) 0.3921(6) 0.1032(3) 0.044(2) Uani 1 1 d . . . . .
H66 H -0.180756 0.435561 0.081372 0.053 Uiso 1 1 calc R U . . .
C71 C -0.3814(7) 0.4911(5) 0.1720(3) 0.037(2) Uani 1 1 d . . . . .
H71 H -0.320784 0.503918 0.199465 0.045 Uiso 1 1 calc R U . . .
C72 C -0.4611(7) 0.5399(6) 0.1905(3) 0.045(2) Uani 1 1 d . . . . .
H72A H -0.520141 0.530358 0.163437 0.054 Uiso 1 1 calc R U . . .
H72B H -0.41941 0.608132 0.200712 0.054 Uiso 1 1 calc R U . . .
C73 C -0.5145(7) 0.5000(7) 0.2344(3) 0.050(2) Uani 1 1 d . . . . .
H73A H -0.456077 0.515862 0.262702 0.06 Uiso 1 1 calc R U . . .
H73B H -0.569596 0.52875 0.244729 0.06 Uiso 1 1 calc R U . . .
C74 C -0.5720(8) 0.3948(7) 0.2211(4) 0.060(3) Uani 1 1 d . . . . .
H74A H -0.636121 0.379678 0.19566 0.072 Uiso 1 1 calc R U . . .
H74B H -0.601666 0.370765 0.250891 0.072 Uiso 1 1 calc R U . . .
C75 C -0.4962(7) 0.3462(7) 0.2020(3) 0.056(3) Uani 1 1 d . . . . .
H75A H -0.539438 0.2783 0.191337 0.067 Uiso 1 1 calc R U . . .
H75B H -0.437438 0.353809 0.228817 0.067 Uiso 1 1 calc R U . . .
C76 C -0.4411(7) 0.3865(6) 0.1579(3) 0.045(2) Uani 1 1 d . . . . .
H76A H -0.387171 0.356599 0.147396 0.054 Uiso 1 1 calc R U . . .
H76B H -0.499113 0.372266 0.129683 0.054 Uiso 1 1 calc R U . . .
C81 C -0.1111(7) 0.6543(6) 0.0605(3) 0.039(2) Uani 1 1 d . . . . .
H81 H -0.047001 0.676867 0.087277 0.047 Uiso 1 1 calc R U . . .
C82 C -0.0826(7) 0.5968(6) 0.0182(3) 0.040(2) Uani 1 1 d . . . . .
H82A H -0.144701 0.573779 -0.009022 0.048 Uiso 1 1 calc R U . . .
H82B H -0.073038 0.541649 0.029019 0.048 Uiso 1 1 calc R U . . .
C83 C 0.0240(7) 0.6541(6) -0.0006(3) 0.045(2) Uani 1 1 d . . . . .
H83A H 0.086747 0.673738 0.02612 0.054 Uiso 1 1 calc R U . . .
H83B H 0.040801 0.614777 -0.028761 0.054 Uiso 1 1 calc R U . . .
C84 C 0.0141(8) 0.7395(7) -0.0169(3) 0.055(3) Uani 1 1 d . . . . .
H84A H -0.043201 0.720297 -0.045938 0.066 Uiso 1 1 calc R U . . .
H84B H 0.086364 0.777809 -0.026785 0.066 Uiso 1 1 calc R U . . .
C85 C -0.0186(7) 0.7969(6) 0.0252(3) 0.046(2) Uani 1 1 d . . . . .
H85A H -0.030574 0.850466 0.013461 0.056 Uiso 1 1 calc R U . . .
H85B H 0.043349 0.822509 0.052466 0.056 Uiso 1 1 calc R U . . .
C86 C -0.1245(7) 0.7389(6) 0.0447(3) 0.046(2) Uani 1 1 d . . . . .
H86A H -0.140776 0.777787 0.07331 0.055 Uiso 1 1 calc R U . . .
H86B H -0.188388 0.718614 0.018537 0.055 Uiso 1 1 calc R U . . .
C11D C 0.3969(9) 0.6529(8) 0.0848(4) 0.082(3) Uani 1 1 d . . . . .
H11A H 0.380802 0.588998 0.091882 0.098 Uiso 1 1 calc R U . . .
H11B H 0.342241 0.677541 0.099999 0.098 Uiso 1 1 calc R U . . .
Cl23 Cl 0.5334(3) 0.7255(2) 0.11215(11) 0.0920(10) Uani 1 1 d . . . . .
Cl24 Cl 0.3802(4) 0.6464(2) 0.02238(12) 0.1278(15) Uani 1 1 d . . . . .
C12D C 0.1295(8) 0.4831(7) 0.1362(3) 0.062(3) Uani 1 1 d . . . . .
H12A H 0.1712 0.449617 0.116572 0.075 Uiso 1 1 calc R U . . .
H12B H 0.054325 0.437189 0.138153 0.075 Uiso 1 1 calc R U . . .
Cl25 Cl 0.1162(2) 0.5706(2) 0.10658(9) 0.0704(8) Uani 1 1 d . . . . .
Cl26 Cl 0.2005(3) 0.5301(3) 0.19658(11) 0.1004(11) Uani 1 1 d . . . . .
C13D C 0.6157(8) 0.0155(7) 0.4394(4) 0.064(3) Uani 1 1 d . . . . .
H13A H 0.697518 0.04664 0.43993 0.077 Uiso 1 1 calc R U . . .
H13B H 0.602405 -0.031674 0.461204 0.077 Uiso 1 1 calc R U . . .
Cl27 Cl 0.5579(2) 0.0988(2) 0.46194(10) 0.0762(8) Uani 1 1 d . . . . .
Cl28 Cl 0.5563(3) -0.0410(2) 0.37840(11) 0.1012(11) Uani 1 1 d . . . . .
C4D C 0.1762(9) 0.3966(8) 0.2936(4) 0.077(3) Uani 1 1 d . . . . .
H4D1 H 0.195198 0.344483 0.303533 0.093 Uiso 1 1 calc R U . . .
H4D2 H 0.182687 0.394227 0.257768 0.093 Uiso 1 1 calc R U . . .
Cl9 Cl 0.0378(3) 0.3823(2) 0.30484(15) 0.1035(11) Uani 1 1 d . . . . .
Cl10 Cl 0.2692(3) 0.5022(2) 0.32645(12) 0.1083(12) Uani 1 1 d . . . . .
C5D C 0.7727(10) 0.2686(8) 0.4079(4) 0.078(3) Uani 1 1 d . . . . .
H5D1 H 0.715525 0.262173 0.431298 0.094 Uiso 1 1 calc R U . . .
H5D2 H 0.811585 0.225098 0.413303 0.094 Uiso 1 1 calc R U . . .
Cl11 Cl 0.8673(3) 0.3809(2) 0.42038(12) 0.0911(10) Uani 1 1 d . . . . .
Cl12 Cl 0.7059(3) 0.2363(3) 0.34675(14) 0.1144(12) Uani 1 1 d . . . . .
C6D C 0.1907(8) 0.1159(7) 0.5131(3) 0.065(3) Uani 1 1 d . . . . .
H6D1 H 0.152094 0.051759 0.519377 0.078 Uiso 1 1 calc R U . . .
H6D2 H 0.133431 0.137698 0.499376 0.078 Uiso 1 1 calc R U . . .
Cl13 Cl 0.2841(2) 0.1127(2) 0.46996(10) 0.0817(9) Uani 1 1 d . . . . .
Cl14 Cl 0.2570(3) 0.1893(3) 0.56831(12) 0.1234(16) Uani 1 1 d . . . . .
C7D C 0.1251(9) 0.3366(8) 0.4423(4) 0.083(3) Uani 1 1 d . . . . .
H7D1 H 0.097802 0.374569 0.422671 0.1 Uiso 1 1 calc R U . . .
H7D2 H 0.060983 0.279249 0.444116 0.1 Uiso 1 1 calc R U . . .
Cl15 Cl 0.2259(3) 0.3052(2) 0.41225(11) 0.0957(10) Uani 1 1 d . . . . .
Cl16 Cl 0.1755(3) 0.3996(3) 0.50096(15) 0.1488(19) Uani 1 1 d . . . . .
C8D C 0.5081(10) 0.0229(9) 0.2406(4) 0.081(4) Uani 1 1 d . . . . .
H8D1 H 0.426609 0.003207 0.242655 0.097 Uiso 1 1 calc R U . . .
H8D2 H 0.545487 0.028353 0.273879 0.097 Uiso 1 1 calc R U . . .
Cl17 Cl 0.5353(3) -0.0619(3) 0.19861(14) 0.1094(11) Uani 1 1 d . . . . .
Cl18 Cl 0.5544(3) 0.1283(3) 0.22261(14) 0.1182(13) Uani 1 1 d . . . . .
C9D C 0.4621(10) 0.3665(9) 0.5094(4) 0.096(4) Uani 1 1 d . . . . .
H9D1 H 0.413807 0.398675 0.497672 0.115 Uiso 1 1 calc R U . . .
H9D2 H 0.413305 0.302468 0.512333 0.115 Uiso 1 1 calc R U . . .
Cl19 Cl 0.5300(3) 0.4260(3) 0.56676(12) 0.1149(13) Uani 1 1 d . . . . .
Cl20 Cl 0.5528(3) 0.3588(3) 0.46609(11) 0.1061(12) Uani 1 1 d . . . . .
C10D C 0.6469(11) 0.8112(9) 0.9862(5) 0.100(4) Uani 1 1 d . . . . .
H10D H 0.675166 0.761626 0.972418 0.12 Uiso 1 1 calc R U . . .
H10E H 0.60852 0.792665 1.015307 0.12 Uiso 1 1 calc R U . . .
Cl21 Cl 0.7579(5) 0.9157(3) 1.0046(2) 0.207(3) Uani 1 1 d . . . . .
Cl22 Cl 0.5513(3) 0.8205(3) 0.94137(15) 0.1236(13) Uani 1 1 d . . . . .
C1D C 0.472(2) 0.732(2) 0.3131(10) 0.110(10) Uiso 0.516(19) 1 d . . P A 1
H1D1 H 0.500369 0.763042 0.347999 0.132 Uiso 0.516(19) 1 calc R U P A 1
H1D2 H 0.448845 0.66359 0.310277 0.132 Uiso 0.516(19) 1 calc R U P A 1
Cl4 Cl 0.5686(6) 0.7724(5) 0.2749(3) 0.065(3) Uiso 0.516(19) 1 d . . P A 1
Cl3 Cl 0.3398(6) 0.7719(6) 0.2857(4) 0.077(3) Uiso 0.516(19) 1 d . . P A 1
C1D' C 0.4249(16) 0.7265(14) 0.2532(7) 0.060(7) Uiso 0.484(19) 1 d . . P A 2
H1D3 H 0.440126 0.732279 0.218638 0.072 Uiso 0.484(19) 1 calc R U P A 2
H1D4 H 0.381672 0.659692 0.253203 0.072 Uiso 0.484(19) 1 calc R U P A 2
Cl4' Cl 0.5560(9) 0.7593(7) 0.2907(5) 0.104(4) Uiso 0.484(19) 1 d . . P A 2
Cl3' Cl 0.3434(6) 0.7901(6) 0.2709(4) 0.076(3) Uiso 0.484(19) 1 d . . P A 2
C2D C 0.1552(15) 0.2093(9) 0.1243(5) 0.123(6) Uani 1 1 d . . . . .
H2DA H 0.100788 0.17507 0.094779 0.148 Uiso 1 1 calc R U . B 3
H2DB H 0.211396 0.265364 0.115502 0.148 Uiso 1 1 calc R U . B 3
Cl5 Cl 0.0929(7) 0.2394(5) 0.1691(3) 0.122(3) Uiso 0.639(9) 1 d . . P C 3
Cl6 Cl 0.2152(4) 0.1426(4) 0.14318(19) 0.096(2) Uiso 0.639(9) 1 d . . P C 3
Cl5' Cl 0.0537(8) 0.2525(6) 0.1600(3) 0.063(3) Uiso 0.361(9) 1 d . . P C 4
Cl6' Cl 0.1155(9) 0.1155(7) 0.0870(4) 0.110(4) Uiso 0.361(9) 1 d . . P C 4
C3D C 0.3545(14) 0.9428(12) 0.0928(6) 0.058(5) Uiso 0.616(10) 1 d . . P D 5
H3D1 H 0.306388 0.972621 0.078452 0.07 Uiso 0.616(10) 1 calc R U P D 5
H3D2 H 0.412217 0.991618 0.117481 0.07 Uiso 0.616(10) 1 calc R U P D 5
Cl7 Cl 0.4174(7) 0.9016(5) 0.0476(2) 0.124(3) Uiso 0.616(10) 1 d . . P D 5
Cl8 Cl 0.2697(7) 0.8518(6) 0.1241(3) 0.150(4) Uiso 0.616(10) 1 d . . P D 5
C3D' C 0.358(8) 0.987(6) 0.070(3) 0.28(4) Uiso 0.384(10) 1 d . . P D 6
H3D3 H 0.43805 1.026682 0.07728 0.342 Uiso 0.384(10) 1 calc R U P D 6
H3D4 H 0.316883 1.010548 0.047669 0.342 Uiso 0.384(10) 1 calc R U P D 6
Cl7' Cl 0.3293(13) 0.8536(10) 0.0530(5) 0.150(6) Uiso 0.384(10) 1 d . . P D 6
Cl8' Cl 0.2798(11) 0.9522(10) 0.1337(5) 0.155(6) Uiso 0.384(10) 1 d . . P D 6



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C2 1.379(10) . ?
N1 C11 1.419(10) . ?
N1 C1 1.458(10) . ?
N2 C2 1.275(9) . ?
N2 C21 1.407(10) . ?
N3 C3 1.326(10) . ?
N3 C5 1.377(10) . ?
N3 C31 1.466(11) . ?
N4 C3 1.329(10) . ?
N4 C4 1.384(10) . ?
N4 C41 1.492(10) . ?
N5 C6 1.394(10) . ?
N5 C51 1.409(10) . ?
N5 C1 1.471(10) . ?
N6 C6 1.267(10) . ?
N6 C61 1.411(10) . ?
N7 C7 1.347(9) . ?
N7 C9 1.410(10) . ?
N7 C71 1.473(10) . ?
N8 C7 1.300(10) . ?
N8 C8 1.390(10) . ?
N8 C81 1.486(10) . ?
C2 C3 1.499(11) . ?
C4 C5 1.343(11) . ?
C6 C7 1.525(12) . ?
C8 C9 1.344(11) . ?
C10 C14 1.502(11) . ?
C11 C12 1.357(11) . ?
C11 C16 1.419(12) . ?
C12 C13 1.361(11) . ?
C13 C14 1.406(12) . ?
C14 C15 1.384(12) . ?
C15 C16 1.408(11) . ?
C20 C24 1.502(12) . ?
C21 C26 1.376(11) . ?
C21 C22 1.400(11) . ?
C22 C23 1.365(11) . ?
C23 C24 1.364(11) . ?
C24 C25 1.402(11) . ?
C25 C26 1.366(11) . ?
C31 C36 1.523(11) . ?
C31 C32 1.552(11) . ?
C32 C33 1.504(13) . ?
C33 C34 1.496(13) . ?
C34 C35 1.534(13) . ?
C35 C36 1.517(13) . ?
C41 C46 1.517(11) . ?
C41 C42 1.519(12) . ?
C42 C43 1.525(13) . ?
C43 C44 1.540(14) . ?
C44 C45 1.529(14) . ?
C45 C46 1.519(13) . ?
C50 C54 1.475(13) . ?
C51 C52 1.383(11) . ?
C51 C56 1.383(11) . ?
C52 C53 1.361(12) . ?
C53 C54 1.407(13) . ?
C54 C55 1.405(12) . ?
C55 C56 1.370(12) . ?
C60 C64 1.506(12) . ?
C61 C62 1.366(11) . ?
C61 C66 1.387(11) . ?
C62 C63 1.364(12) . ?
C63 C64 1.408(12) . ?
C64 C65 1.377(11) . ?
C65 C66 1.364(11) . ?
C71 C76 1.506(11) . ?
C71 C72 1.532(12) . ?
C72 C73 1.526(11) . ?
C73 C74 1.510(13) . ?
C74 C75 1.493(13) . ?
C75 C76 1.540(12) . ?
C81 C82 1.493(11) . ?
C81 C86 1.502(12) . ?
C82 C83 1.515(11) . ?
C83 C84 1.505(12) . ?
C84 C85 1.514(12) . ?
C85 C86 1.524(11) . ?
C11D Cl24 1.701(11) . ?
C11D Cl23 1.771(11) . ?
C12D Cl25 1.736(11) . ?
C12D Cl26 1.769(10) . ?
C13D Cl28 1.764(10) . ?
C13D Cl27 1.749(11) . ?
C4D Cl10 1.729(11) . ?
C4D Cl9 1.763(12) . ?
C5D Cl11 1.710(11) . ?
C5D Cl12 1.762(11) . ?
C6D Cl13 1.737(10) . ?
C6D Cl14 1.727(10) . ?
C7D Cl16 1.714(12) . ?
C7D Cl15 1.736(12) . ?
C8D Cl18 1.693(12) . ?
C8D Cl17 1.750(12) . ?
C9D Cl19 1.716(11) . ?
C9D Cl20 1.727(13) . ?
C10D Cl22 1.752(13) . ?
C10D Cl21 1.725(14) . ?
C1D Cl4 1.68(3) . ?
C1D Cl3 2.14(3) . ?
C1D' Cl3' 1.71(2) . ?
C1D' Cl4' 1.80(2) . ?
C2D Cl6' 1.546(16) . ?
C2D Cl6 1.615(16) . ?
C2D Cl5 1.597(15) . ?
C2D Cl5' 1.908(18) . ?
C3D Cl7 1.678(17) . ?
C3D Cl8 1.820(18) . ?
C3D' Cl8' 2.10(8) . ?
C3D' Cl7' 1.94(9) . ?

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
C2 N1 C11 125.6(6) . . ?
C2 N1 C1 117.4(6) . . ?
C11 N1 C1 116.7(6) . . ?
C2 N2 C21 123.7(7) . . ?
C3 N3 C5 109.4(7) . . ?
C3 N3 C31 128.2(7) . . ?
C5 N3 C31 122.4(7) . . ?
C3 N4 C4 109.6(7) . . ?
C3 N4 C41 128.1(7) . . ?
C4 N4 C41 122.4(7) . . ?
C6 N5 C51 124.1(7) . . ?
C6 N5 C1 118.2(7) . . ?
C51 N5 C1 117.5(6) . . ?
C6 N6 C61 125.3(7) . . ?
C7 N7 C9 106.6(6) . . ?
C7 N7 C71 130.1(6) . . ?
C9 N7 C71 123.1(7) . . ?
C7 N8 C8 108.5(7) . . ?
C7 N8 C81 129.1(7) . . ?
C8 N8 C81 122.4(7) . . ?
N1 C1 N5 109.7(6) . . ?
N2 C2 N1 120.1(7) . . ?
N2 C2 C3 124.0(7) . . ?
N1 C2 C3 115.8(7) . . ?
N4 C3 N3 107.4(7) . . ?
N4 C3 C2 126.0(7) . . ?
N3 C3 C2 126.2(8) . . ?
C5 C4 N4 106.4(7) . . ?
C4 C5 N3 107.2(7) . . ?
N6 C6 N5 120.6(7) . . ?
N6 C6 C7 124.4(7) . . ?
N5 C6 C7 115.0(8) . . ?
N8 C7 N7 110.4(7) . . ?
N8 C7 C6 126.5(7) . . ?
N7 C7 C6 122.0(7) . . ?
C9 C8 N8 107.7(7) . . ?
C8 C9 N7 106.8(7) . . ?
C12 C11 C16 118.6(8) . . ?
C12 C11 N1 121.9(8) . . ?
C16 C11 N1 119.4(8) . . ?
C11 C12 C13 122.4(9) . . ?
C12 C13 C14 121.3(9) . . ?
C15 C14 C13 116.8(8) . . ?
C15 C14 C10 119.9(9) . . ?
C13 C14 C10 123.2(9) . . ?
C14 C15 C16 122.2(9) . . ?
C15 C16 C11 118.4(8) . . ?
C26 C21 C22 117.3(7) . . ?
C26 C21 N2 118.1(7) . . ?
C22 C21 N2 124.3(8) . . ?
C23 C22 C21 120.0(8) . . ?
C24 C23 C22 123.2(8) . . ?
C23 C24 C25 116.5(8) . . ?
C23 C24 C20 123.0(8) . . ?
C25 C24 C20 120.5(8) . . ?
C26 C25 C24 120.9(8) . . ?
C25 C26 C21 121.9(8) . . ?
N3 C31 C36 111.4(7) . . ?
N3 C31 C32 111.9(7) . . ?
C36 C31 C32 109.1(7) . . ?
C33 C32 C31 110.3(7) . . ?
C34 C33 C32 111.6(9) . . ?
C33 C34 C35 112.7(8) . . ?
C36 C35 C34 109.7(8) . . ?
C35 C36 C31 112.5(8) . . ?
N4 C41 C46 110.4(6) . . ?
N4 C41 C42 109.0(7) . . ?
C46 C41 C42 112.1(7) . . ?
C43 C42 C41 107.8(7) . . ?
C42 C43 C44 109.9(8) . . ?
C43 C44 C45 112.2(9) . . ?
C46 C45 C44 111.2(8) . . ?
C41 C46 C45 111.7(7) . . ?
C52 C51 C56 119.1(8) . . ?
C52 C51 N5 119.6(8) . . ?
C56 C51 N5 121.3(7) . . ?
C53 C52 C51 121.0(9) . . ?
C52 C53 C54 121.3(9) . . ?
C55 C54 C53 116.7(9) . . ?
C55 C54 C50 121.1(9) . . ?
C53 C54 C50 122.2(9) . . ?
C56 C55 C54 121.6(9) . . ?
C55 C56 C51 120.3(8) . . ?
C62 C61 C66 117.3(8) . . ?
C62 C61 N6 116.2(8) . . ?
C66 C61 N6 126.3(8) . . ?
C63 C62 C61 122.5(9) . . ?
C62 C63 C64 119.0(8) . . ?
C65 C64 C63 119.4(8) . . ?
C65 C64 C60 120.2(8) . . ?
C63 C64 C60 120.4(8) . . ?
C66 C65 C64 119.3(8) . . ?
C65 C66 C61 122.4(8) . . ?
N7 C71 C76 109.8(6) . . ?
N7 C71 C72 110.7(7) . . ?
C76 C71 C72 111.3(7) . . ?
C71 C72 C73 109.8(7) . . ?
C74 C73 C72 111.1(7) . . ?
C73 C74 C75 112.9(8) . . ?
C74 C75 C76 110.8(8) . . ?
C71 C76 C75 110.7(7) . . ?
N8 C81 C82 113.2(6) . . ?
N8 C81 C86 110.0(7) . . ?
C82 C81 C86 110.1(6) . . ?
C81 C82 C83 110.7(7) . . ?
C84 C83 C82 111.5(7) . . ?
C83 C84 C85 109.5(7) . . ?
C84 C85 C86 111.9(7) . . ?
C81 C86 C85 110.6(7) . . ?
Cl24 C11D Cl23 112.7(7) . . ?
Cl25 C12D Cl26 111.2(5) . . ?
Cl28 C13D Cl27 110.9(6) . . ?
Cl10 C4D Cl9 110.9(6) . . ?
Cl11 C5D Cl12 112.6(6) . . ?
Cl13 C6D Cl14 111.8(5) . . ?
Cl16 C7D Cl15 112.3(7) . . ?
Cl18 C8D Cl17 110.9(6) . . ?
Cl19 C9D Cl20 112.8(7) . . ?
Cl22 C10D Cl21 111.4(8) . . ?
Cl4 C1D Cl3 101.3(13) . . ?
Cl3' C1D' Cl4' 115.8(12) . . ?
Cl6 C2D Cl5 106.6(8) . . ?
Cl6' C2D Cl5' 122.1(11) . . ?
Cl7 C3D Cl8 112.8(10) . . ?
Cl8' C3D' Cl7' 85(3) . . ?


# END of CIF
