# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1522056
_database_code_depnum_ccdc_archive 'CCDC 1522056'
_audit_update_record             
;
2017-01-12 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H20 Br2 N2 Si2 Zn'
_chemical_formula_weight         497.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

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

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

_cell_length_a                   13.6038(4)
_cell_length_b                   25.6130(7)
_cell_length_c                   11.8630(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4133.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9912
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      23.87

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_F_000             1968
_exptl_transmission_factor_min   0.000
_exptl_transmission_factor_max   0.000
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.410
_exptl_absorpt_coefficient_mu    5.166
_shelx_estimated_absorpt_T_min   0.148
_shelx_estimated_absorpt_T_max   0.226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.148
_exptl_absorpt_correction_T_max  0.226
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Breeze CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            66112
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.590
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4291
_reflns_number_gt                3662
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker AEPX2'
_computing_cell_refinement       'Bruker AEPX2'
_computing_data_reduction        'Bruker AEPX2'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0285P)²+4.8231P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4291
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0710
_refine_ls_wR_factor_gt          0.0677
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.2500 0.5000 0.55836(3) 0.02744(11) Uani 1 2 d S T P . .
Zn2 Zn 0.04868(3) 0.2500 -0.2500 0.03229(12) Uani 1 2 d S T P . .
Br1 Br 0.24320(2) 0.58104(2) 0.65026(3) 0.04727(10) Uani 1 1 d . . . . .
Br2 Br -0.03960(3) 0.32385(2) -0.30905(3) 0.04629(10) Uani 1 1 d . . . . .
Si1 Si 0.06221(7) 0.38288(4) 0.21611(8) 0.0452(2) Uani 1 1 d . . . . .
Si2 Si 0.18183(6) 0.39754(3) 0.07929(6) 0.03172(18) Uani 1 1 d . . . . .
N1 N 0.13700(16) 0.49705(8) 0.44346(17) 0.0250(4) Uani 1 1 d . . . . .
N2 N 0.14531(18) 0.26990(9) -0.1263(2) 0.0336(5) Uani 1 1 d . . . . .
C1 C 0.1263(2) 0.45255(10) 0.3854(2) 0.0297(6) Uani 1 1 d . . . . .
H1A H 0.1682 0.4242 0.4040 0.036 Uiso 1 1 calc R U . . .
C2 C 0.0582(2) 0.44522(11) 0.3003(2) 0.0307(6) Uani 1 1 d . . . . .
C3 C -0.0028(2) 0.48725(11) 0.2775(2) 0.0326(6) Uani 1 1 d . . . . .
H3A H -0.0519 0.4842 0.2209 0.039 Uiso 1 1 calc R U . . .
C4 C 0.0070(2) 0.53353(11) 0.3363(2) 0.0319(6) Uani 1 1 d . . . . .
H4A H -0.0348 0.5623 0.3203 0.038 Uiso 1 1 calc R U . . .
C5 C 0.0781(2) 0.53723(10) 0.4183(2) 0.0271(6) Uani 1 1 d . . . . .
H5A H 0.0856 0.5692 0.4582 0.033 Uiso 1 1 calc R U . . .
C6 C 0.0988(5) 0.32823(15) 0.3117(4) 0.102(2) Uani 1 1 d . . . . .
H6A H 0.1621 0.3364 0.3470 0.123 Uiso 1 1 calc R U . . .
H6B H 0.0487 0.3237 0.3702 0.123 Uiso 1 1 calc R U . . .
H6C H 0.1049 0.2959 0.2679 0.123 Uiso 1 1 calc R U . . .
C7 C -0.0576(3) 0.3696(2) 0.1464(5) 0.107(2) Uani 1 1 d . . . . .
H7A H -0.0747 0.3989 0.0970 0.129 Uiso 1 1 calc R U . . .
H7B H -0.0525 0.3375 0.1016 0.129 Uiso 1 1 calc R U . . .
H7C H -0.1087 0.3653 0.2038 0.129 Uiso 1 1 calc R U . . .
C8 C 0.1350(3) 0.44451(12) -0.0287(3) 0.0509(9) Uani 1 1 d . . . . .
H8A H 0.0737 0.4311 -0.0611 0.061 Uiso 1 1 calc R U . . .
H8B H 0.1227 0.4784 0.0069 0.061 Uiso 1 1 calc R U . . .
H8C H 0.1841 0.4486 -0.0886 0.061 Uiso 1 1 calc R U . . .
C9 C 0.2985(3) 0.42171(13) 0.1429(3) 0.0487(8) Uani 1 1 d . . . . .
H9A H 0.3219 0.3966 0.1991 0.058 Uiso 1 1 calc R U . . .
H9B H 0.3483 0.4257 0.0837 0.058 Uiso 1 1 calc R U . . .
H9C H 0.2869 0.4555 0.1791 0.058 Uiso 1 1 calc R U . . .
C10 C 0.2024(2) 0.33220(10) 0.0102(2) 0.0296(6) Uani 1 1 d . . . . .
C11 C 0.2694(2) 0.29533(11) 0.0476(3) 0.0384(7) Uani 1 1 d . . . . .
H11A H 0.3123 0.3036 0.1083 0.046 Uiso 1 1 calc R U . . .
C12 C 0.2745(2) 0.24698(12) -0.0021(3) 0.0452(8) Uani 1 1 d . . . . .
H12A H 0.3215 0.2220 0.0226 0.054 Uiso 1 1 calc R U . . .
C13 C 0.2106(2) 0.23534(11) -0.0878(3) 0.0422(7) Uani 1 1 d . . . . .
H13A H 0.2129 0.2016 -0.1210 0.051 Uiso 1 1 calc R U . . .
C14 C 0.1428(2) 0.31703(10) -0.0784(2) 0.0317(6) Uani 1 1 d . . . . .
H14A H 0.0972 0.3418 -0.1071 0.038 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 2.056(2) 2_565 ?
Zn1 N1 2.056(2) . ?
Zn1 Br1 2.3464(4) 2_565 ?
Zn1 Br1 2.3464(4) . ?
Zn2 N2 2.035(2) 4_554 ?
Zn2 N2 2.035(2) . ?
Zn2 Br2 2.3475(4) 4_554 ?
Zn2 Br2 2.3475(4) . ?
Si1 C7 1.859(4) . ?
Si1 C6 1.869(5) . ?
Si1 C2 1.884(3) . ?
Si1 Si2 2.3288(13) . ?
Si2 C9 1.864(3) . ?
Si2 C8 1.870(3) . ?
Si2 C10 1.884(3) . ?
N1 C5 1.338(3) . ?
N1 C1 1.339(3) . ?
N2 C14 1.335(3) . ?
N2 C13 1.335(4) . ?
C1 C2 1.383(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.386(4) . ?
C3 C4 1.382(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.376(4) . ?
C4 H4A 0.9500 . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C14 1.383(4) . ?
C10 C11 1.386(4) . ?
C11 C12 1.373(4) . ?
C11 H11A 0.9500 . ?
C12 C13 1.371(5) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 N1 96.94(12) 2_565 . ?
N1 Zn1 Br1 108.12(6) 2_565 2_565 ?
N1 Zn1 Br1 107.76(6) . 2_565 ?
N1 Zn1 Br1 107.76(6) 2_565 . ?
N1 Zn1 Br1 108.12(6) . . ?
Br1 Zn1 Br1 124.63(3) 2_565 . ?
N2 Zn2 N2 99.53(14) 4_554 . ?
N2 Zn2 Br2 110.11(6) 4_554 4_554 ?
N2 Zn2 Br2 108.48(7) . 4_554 ?
N2 Zn2 Br2 108.48(7) 4_554 . ?
N2 Zn2 Br2 110.11(6) . . ?
Br2 Zn2 Br2 118.46(3) 4_554 . ?
C7 Si1 C6 111.5(3) . . ?
C7 Si1 C2 111.48(19) . . ?
C6 Si1 C2 108.71(16) . . ?
C7 Si1 Si2 109.39(17) . . ?
C6 Si1 Si2 110.9(2) . . ?
C2 Si1 Si2 104.67(9) . . ?
C9 Si2 C8 110.72(17) . . ?
C9 Si2 C10 110.15(14) . . ?
C8 Si2 C10 108.92(13) . . ?
C9 Si2 Si1 111.52(13) . . ?
C8 Si2 Si1 110.08(13) . . ?
C10 Si2 Si1 105.28(9) . . ?
C5 N1 C1 118.3(2) . . ?
C5 N1 Zn1 124.55(18) . . ?
C1 N1 Zn1 116.97(18) . . ?
C14 N2 C13 118.1(3) . . ?
C14 N2 Zn2 121.14(19) . . ?
C13 N2 Zn2 120.69(19) . . ?
N1 C1 C2 124.3(3) . . ?
N1 C1 H1A 117.8 . . ?
C2 C1 H1A 117.8 . . ?
C1 C2 C3 116.0(3) . . ?
C1 C2 Si1 118.9(2) . . ?
C3 C2 Si1 124.9(2) . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C5 C4 C3 118.9(3) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
N1 C5 C4 121.7(2) . . ?
N1 C5 H5A 119.1 . . ?
C4 C5 H5A 119.1 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C14 C10 C11 116.0(3) . . ?
C14 C10 Si2 119.5(2) . . ?
C11 C10 Si2 124.3(2) . . ?
C12 C11 C10 120.7(3) . . ?
C12 C11 H11A 119.7 . . ?
C10 C11 H11A 119.7 . . ?
C13 C12 C11 118.9(3) . . ?
C13 C12 H12A 120.6 . . ?
C11 C12 H12A 120.6 . . ?
N2 C13 C12 122.1(3) . . ?
N2 C13 H13A 118.9 . . ?
C12 C13 H13A 118.9 . . ?
N2 C14 C10 124.2(3) . . ?
N2 C14 H14A 117.9 . . ?
C10 C14 H14A 117.9 . . ?

_refine_diff_density_max         0.963
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.080

####################################################################### 
# 
# 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_1522055
_database_code_depnum_ccdc_archive 'CCDC 1522055'
_audit_update_record             
;
2017-01-12 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H73 Cl3 N6 O20 Si6 Zn3'
_chemical_formula_weight         1453.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           230
_space_group_name_H-M_alt        'I a -3 d'
_space_group_name_Hall           '-I 4bd 2c 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'z, x, y'
'-x+1/4, z+3/4, y+1/4'
'-z+1/2, -x, y+1/2'
'x+1/4, -z+1/4, y+3/4'
'z, -x, -y+1/2'
'x+1/4, z+3/4, -y+3/4'
'-z+1/2, x, -y'
'-x+1/4, -z+1/4, -y+1/4'
'y, z, x'
'-z+1/4, -y+1/4, -x+1/4'
'-z+3/4, y+1/4, x+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'y, -z, -x+1/2'
'-y, -z+1/2, x'
'-y, z+1/2, -x+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'z+1/2, x+1/2, y+1/2'
'-x+3/4, z+5/4, y+3/4'
'-z+1, -x+1/2, y+1'
'x+3/4, -z+3/4, y+5/4'
'z+1/2, -x+1/2, -y+1'
'x+3/4, z+5/4, -y+5/4'
'-z+1, x+1/2, -y+1/2'
'-x+3/4, -z+3/4, -y+3/4'
'y+1/2, z+1/2, x+1/2'
'-z+3/4, -y+3/4, -x+3/4'
'-z+5/4, y+3/4, x+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'y+1/2, -z+1/2, -x+1'
'-y+1/2, -z+1, x+1/2'
'-y+1/2, z+1, -x+1'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-z, -x, -y'
'x-1/4, -z-3/4, -y-1/4'
'z-1/2, x, -y-1/2'
'-x-1/4, z-1/4, -y-3/4'
'-z, x, y-1/2'
'-x-1/4, -z-3/4, y-3/4'
'z-1/2, -x, y'
'x-1/4, z-1/4, y-1/4'
'-y, -z, -x'
'z-1/4, y-1/4, x-1/4'
'z-3/4, -y-1/4, -x-3/4'
'-z-3/4, -y-1/4, x-1/4'
'-z-1/4, y-1/4, -x-3/4'
'-y, z, x-1/2'
'y, z-1/2, -x'
'y, -z-1/2, x-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'
'-z+1/2, -x+1/2, -y+1/2'
'x+1/4, -z-1/4, -y+1/4'
'z, x+1/2, -y'
'-x+1/4, z+1/4, -y-1/4'
'-z+1/2, x+1/2, y'
'-x+1/4, -z-1/4, y-1/4'
'z, -x+1/2, y+1/2'
'x+1/4, z+1/4, y+1/4'
'-y+1/2, -z+1/2, -x+1/2'
'z+1/4, y+1/4, x+1/4'
'z-1/4, -y+1/4, -x-1/4'
'-z-1/4, -y+1/4, x+1/4'
'-z+1/4, y+1/4, -x-1/4'
'-y+1/2, z+1/2, x'
'y+1/2, z, -x+1/2'
'y+1/2, -z, x'

_cell_length_a                   30.7561(2)
_cell_length_b                   30.7561(2)
_cell_length_c                   30.7561(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     29093.4(6)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9909
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      27.06

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_F_000             12032
_exptl_transmission_factor_min   0.000
_exptl_transmission_factor_max   0.002
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.252
_shelx_estimated_absorpt_T_min   0.721
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Breeze CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            216020
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.622
_diffrn_reflns_theta_max         25.986
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2393
_reflns_number_gt                2094
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0698P)²+678.7322P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2393
_refine_ls_number_parameters     133
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0940
_refine_ls_wR_factor_ref         0.2630
_refine_ls_wR_factor_gt          0.2576
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_restrained_S_all      1.228
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.17146(3) 0.1250 0.07854(3) 0.0362(4) Uani 1 2 d S T P . .
Cl1 Cl -0.00285(8) 0.1250 0.25285(8) 0.0814(15) Uani 1 2 d S T P . .
O1 O 0.16664(18) 0.08336(18) 0.1250 0.044(2) Uani 1 2 d S T P . .
H1B H 0.1885 0.0615 0.1250 0.053 Uiso 1 2 calc R U P . .
O2 O 0.0394(3) 0.1091(3) 0.2571(4) 0.104(3) Uani 1 1 d . . . . .
O3 O -0.0314(5) 0.0944(9) 0.2591(7) 0.330(19) Uani 1 1 d . . . . .
N1 N 0.2279(2) 0.1588(2) 0.0822(2) 0.0389(16) Uani 1 1 d . . . . .
C1 C 0.2308(3) 0.1984(3) 0.0636(4) 0.056(3) Uani 1 1 d . . . . .
H1A H 0.2068 0.2091 0.0473 0.067 Uiso 1 1 calc R U . . .
C2 C 0.2669(4) 0.2232(4) 0.0676(5) 0.073(3) Uani 1 1 d . . . . .
H2A H 0.2680 0.2509 0.0540 0.087 Uiso 1 1 calc R U . . .
C3 C 0.3022(3) 0.2084(3) 0.0915(3) 0.052(2) Uani 1 1 d . . . . .
H3A H 0.3275 0.2259 0.0943 0.063 Uiso 1 1 calc R U . . .
C4 C 0.3006(3) 0.1678(3) 0.1112(3) 0.0380(18) Uani 1 1 d . . . . .
C5 C 0.2619(3) 0.1446(2) 0.1051(3) 0.0383(18) Uani 1 1 d . . . . .
H5A H 0.2597 0.1168 0.1182 0.046 Uiso 1 1 calc R U . . .
C6 C 0.3246(5) 0.1079(5) 0.1857(4) 0.089(4) Uani 1 1 d . . . . .
H6A H 0.3086 0.0841 0.1719 0.107 Uiso 1 1 calc R U . . .
H6B H 0.3485 0.0959 0.2031 0.107 Uiso 1 1 calc R U . . .
H6C H 0.3050 0.1244 0.2045 0.107 Uiso 1 1 calc R U . . .
C7 C 0.3778(5) 0.1897(4) 0.1687(5) 0.095(5) Uani 1 1 d . . . . .
H7A H 0.3895 0.2087 0.1460 0.114 Uiso 1 1 calc R U . . .
H7B H 0.3582 0.2064 0.1875 0.114 Uiso 1 1 calc R U . . .
H7C H 0.4017 0.1779 0.1861 0.114 Uiso 1 1 calc R U . . .
Si1 Si 0.34709(9) 0.14424(8) 0.14314(8) 0.0491(7) Uani 1 1 d . . . . .
O5 O 0.3427(10) -0.001(4) 0.255(3) 0.19(2) Uani 0.5 1 d . . P A -1
H5B H 0.3164 0.0051 0.2580 0.233 Uiso 0.5 1 d R U P A -1
H5C H 0.3491 -0.0222 0.2711 0.233 Uiso 0.5 1 d R U P A -1
O4 O 0.233(2) 0.1935(16) 0.218(2) 0.30(4) Uani 0.3333 1 d . . P . .
H4A H 0.2057 0.2057 0.2057 0.360 Uiso 1 3 d R U P . .
H4B H 0.2575 0.2102 0.2190 0.360 Uiso 0.3333 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.924(3) 9 ?
Zn1 O1 1.924(3) . ?
Zn1 N1 2.027(7) 18 ?
Zn1 N1 2.027(7) . ?
Cl1 O3 1.303(16) 18 ?
Cl1 O3 1.303(16) . ?
Cl1 O2 1.394(9) 18 ?
Cl1 O2 1.394(9) . ?
O1 Zn1 1.924(3) 8 ?
O1 H1B 0.9500 . ?
N1 C5 1.334(10) . ?
N1 C1 1.347(11) . ?
C1 C2 1.353(14) . ?
C1 H1A 0.9500 . ?
C2 C3 1.389(14) . ?
C2 H2A 0.9500 . ?
C3 C4 1.389(12) . ?
C3 H3A 0.9500 . ?
C4 C5 1.399(11) . ?
C4 Si1 1.880(9) . ?
C5 H5A 0.9500 . ?
C6 Si1 1.855(13) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 Si1 1.861(11) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
Si1 Si1 2.327(6) 21_554 ?
O5 H5B 0.8400 . ?
O5 H5C 0.8400 . ?
O4 O4 1.50(8) 9 ?
O4 O4 1.50(8) 17 ?
O4 H4A 0.9980 . ?
O4 H4B 0.9122 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O1 109.2(4) 9 . ?
O1 Zn1 N1 111.5(2) 9 18 ?
O1 Zn1 N1 106.9(2) . 18 ?
O1 Zn1 N1 106.9(2) 9 . ?
O1 Zn1 N1 111.5(2) . . ?
N1 Zn1 N1 110.9(4) 18 . ?
O3 Cl1 O3 109(2) 18 . ?
O3 Cl1 O2 111.2(11) 18 18 ?
O3 Cl1 O2 109.2(9) . 18 ?
O3 Cl1 O2 109.2(9) 18 . ?
O3 Cl1 O2 111.2(11) . . ?
O2 Cl1 O2 107.3(10) 18 . ?
Zn1 O1 Zn1 130.8(4) 8 . ?
Zn1 O1 H1B 114.6 8 . ?
Zn1 O1 H1B 114.6 . . ?
C5 N1 C1 117.9(7) . . ?
C5 N1 Zn1 122.1(6) . . ?
C1 N1 Zn1 119.7(6) . . ?
N1 C1 C2 121.6(9) . . ?
N1 C1 H1A 119.2 . . ?
C2 C1 H1A 119.2 . . ?
C1 C2 C3 120.3(10) . . ?
C1 C2 H2A 119.8 . . ?
C3 C2 H2A 119.8 . . ?
C4 C3 C2 119.8(9) . . ?
C4 C3 H3A 120.1 . . ?
C2 C3 H3A 120.1 . . ?
C3 C4 C5 115.5(8) . . ?
C3 C4 Si1 123.1(7) . . ?
C5 C4 Si1 121.4(6) . . ?
N1 C5 C4 124.8(7) . . ?
N1 C5 H5A 117.6 . . ?
C4 C5 H5A 117.6 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 Si1 C7 110.1(7) . . ?
C6 Si1 C4 108.5(5) . . ?
C7 Si1 C4 108.5(5) . . ?
C6 Si1 Si1 110.5(5) . 21_554 ?
C7 Si1 Si1 109.3(5) . 21_554 ?
C4 Si1 Si1 110.0(3) . 21_554 ?
H5B O5 H5C 109.5 . . ?
O4 O4 O4 59.998(11) 9 17 ?
O4 O4 H4A 41.1 9 . ?
O4 O4 H4A 41.1 17 . ?
O4 O4 H4B 78.8 9 . ?
O4 O4 H4B 112.0 17 . ?
H4A O4 H4B 119.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 0.4(16) . . . . ?
Zn1 N1 C1 C2 175.7(10) . . . . ?
N1 C1 C2 C3 0(2) . . . . ?
C1 C2 C3 C4 0.2(19) . . . . ?
C2 C3 C4 C5 0.0(15) . . . . ?
C2 C3 C4 Si1 178.6(9) . . . . ?
C1 N1 C5 C4 -0.3(13) . . . . ?
Zn1 N1 C5 C4 -175.5(6) . . . . ?
C3 C4 C5 N1 0.1(13) . . . . ?
Si1 C4 C5 N1 -178.6(6) . . . . ?
C3 C4 Si1 C6 150.4(9) . . . . ?
C5 C4 Si1 C6 -31.0(9) . . . . ?
C3 C4 Si1 C7 30.8(10) . . . . ?
C5 C4 Si1 C7 -150.6(9) . . . . ?
C3 C4 Si1 Si1 -88.7(8) . . . 21_554 ?
C5 C4 Si1 Si1 89.9(7) . . . 21_554 ?

_refine_diff_density_max         0.864
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.139

