# 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_ZnNH33tetraborato_E1
_database_code_depnum_ccdc_archive 'CCDC 1532489'
_audit_update_record             
;
2017-02-13 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_ZnNH33tetraborato_E1 
;
PROBLEM: D-H Without Acceptor       N2     --  H2A    ...     Please Check
RESPONSE: H2A does not participate in the H-bond network for sterical reasons, still it shows short contacts (H...O) with O4 and O1W at 2.86 and 2.85 A respectively
;
_vrf_PLAT911_ZnNH33tetraborato_E1 
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600          4 Report
RESPONSE: Some low-angle reflections were not collected because they were blocked by the beam-stop.
;
_vrf_PLAT915_ZnNH33tetraborato_E1 
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         64 %
RESPONSE: This non-centrosymmetric structure is obtained from inversion twinned crystals because there are no chiral precursos in the mother solution therefore the absolute structure is not relevant for the structure determination.
;
_vrf_PLAT934_ZnNH33tetraborato_E1 
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW &gt; 10 Outliers ....          1 Check
RESPONSE:  This isolate wrong reflection must have been affected by an integration error or noise in data collection.
;
_vrf_PLAT976_ZnNH33tetraborato_E1 
;
PROBLEM: Check Calcd Residual Density  0.68A From     O1W      -0.40 eA-3
RESPONSE: This residual density seems to be caused by rounding errors since an H-atom placed in this position would not form suitable H-bonds and would be only 2.06 A from H2A.
;
# Added during the CSD deposition process: Monday 13 February 2017 05:16 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Zn 2+, (N H3)3, B4 O9 H4 2-, H2 O'
_chemical_formula_sum            'B4 H15 N3 O10 Zn'
_chemical_formula_weight         325.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

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

_cell_length_a                   12.215(4)
_cell_length_b                   7.845(3)
_cell_length_c                   12.172(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.323(15)
_cell_angle_gamma                90
_cell_volume                     1113.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2185
_cell_measurement_theta_min      3.135
_cell_measurement_theta_max      24.974

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_F_000             664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.166
_exptl_absorpt_coefficient_mu    2.256
_shelx_estimated_absorpt_T_min   0.641
_shelx_estimated_absorpt_T_max   0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo Sealed Tube'
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       '\j and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            5167
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.130
_diffrn_reflns_theta_max         33.199
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3344
_reflns_number_gt                3033
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_max     0.925
_reflns_Friedel_fraction_full    0.996

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
'Refined as a 2-component inversion twin., Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0396P)²+0.3392P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.281(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3344
_refine_ls_number_parameters     171
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_ref         0.0738
_refine_ls_wR_factor_gt          0.0707
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.562
_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
Zn01 Zn 0.48532(3) 0.69468(4) 0.55679(3) 0.01876(9) Uani 1 1 d . . . . .
N1 N 0.3228(3) 0.6740(4) 0.4549(3) 0.0246(6) Uani 1 1 d . . . . .
H1A H 0.3101 0.7507 0.3986 0.037 Uiso 1 1 calc R U . . .
H1B H 0.2749 0.6923 0.4963 0.037 Uiso 1 1 calc R U . . .
H1C H 0.3114 0.5698 0.4248 0.037 Uiso 1 1 calc R U . . .
N2 N 0.4997(5) 0.8245(5) 0.7050(4) 0.0411(10) Uani 1 1 d . . . . .
H2A H 0.4329 0.8219 0.7204 0.062 Uiso 1 1 calc R U . . .
H2B H 0.5189 0.9321 0.6969 0.062 Uiso 1 1 calc R U . . .
H2C H 0.5535 0.7762 0.7625 0.062 Uiso 1 1 calc R U . . .
N3 N 0.5876(3) 0.8305(4) 0.4835(3) 0.0236(6) Uani 1 1 d . . . . .
H3A H 0.6607 0.8147 0.5236 0.035 Uiso 1 1 calc R U . . .
H3B H 0.5704 0.9408 0.4835 0.035 Uiso 1 1 calc R U . . .
H3C H 0.5762 0.7953 0.4115 0.035 Uiso 1 1 calc R U . . .
O1 O 0.52672(19) 0.4553(3) 0.5929(2) 0.0142(4) Uani 1 1 d . . . . .
B1 B 0.5696(3) 0.3384(5) 0.5176(3) 0.0132(6) Uani 1 1 d . . . . .
B2 B 0.4749(3) 0.3544(4) 0.6692(3) 0.0134(6) Uani 1 1 d . . . . .
O2 O 0.60064(19) 0.4298(3) 0.4293(2) 0.0210(5) Uani 1 1 d . . . . .
H2 H 0.6659 0.4675 0.4553 0.031 Uiso 1 1 calc R U . . .
B3 B 0.3878(3) 0.1861(4) 0.4972(3) 0.0150(6) Uani 1 1 d . . . . .
O3 O 0.4796(2) 0.2161(3) 0.4594(2) 0.0190(5) Uani 1 1 d . . . . .
O4 O 0.4323(2) 0.4585(3) 0.7433(2) 0.0194(5) Uani 1 1 d . . . . .
H4 H 0.4851 0.4844 0.8003 0.029 Uiso 1 1 calc R U . . .
B4 B 0.6553(3) 0.1871(4) 0.6972(3) 0.0160(6) Uani 1 1 d . . . . .
O5 O 0.6684(2) 0.2442(3) 0.5954(2) 0.0192(5) Uani 1 1 d . . . . .
O8 O 0.7321(2) 0.0769(4) 0.7658(2) 0.0293(6) Uani 1 1 d . . . . .
H8 H 0.7974 0.1121 0.7748 0.044 Uiso 1 1 calc R U . . .
O7 O 0.3746(2) 0.2575(4) 0.5943(2) 0.0185(5) Uani 1 1 d . . . . .
O6 O 0.3041(2) 0.0743(4) 0.4393(2) 0.0265(6) Uani 1 1 d . . . . .
H6 H 0.3173 0.0425 0.3803 0.040 Uiso 1 1 calc R U . . .
O9 O 0.5631(2) 0.2317(3) 0.7332(2) 0.0179(5) Uani 1 1 d . . . . .
O1W O 0.2724(3) -0.0798(5) 0.2322(3) 0.0515(10) Uani 1 1 d D . . . .
H1WA H 0.3096 -0.1389 0.1975 0.077 Uiso 1 1 d DR U . . .
H1WB H 0.2130 -0.0346 0.1810 0.077 Uiso 1 1 d DR 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
Zn01 O1 1.961(2) . ?
Zn01 N1 2.010(3) . ?
Zn01 N2 2.033(4) . ?
Zn01 N3 2.038(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
O1 B1 1.497(4) . ?
O1 B2 1.497(4) . ?
B1 O2 1.434(4) . ?
B1 O3 1.472(4) . ?
B1 O5 1.489(4) . ?
B2 O4 1.425(4) . ?
B2 O9 1.481(4) . ?
B2 O7 1.498(4) . ?
O2 H2 0.8200 . ?
B3 O3 1.353(4) . ?
B3 O7 1.360(4) . ?
B3 O6 1.372(4) . ?
O4 H4 0.8200 . ?
B4 O8 1.363(4) . ?
B4 O9 1.369(4) . ?
B4 O5 1.371(4) . ?
O8 H8 0.8200 . ?
O6 H6 0.8200 . ?
O1W H1WA 0.8456 . ?
O1W H1WB 0.8782 . ?

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 Zn01 N1 101.67(11) . . ?
O1 Zn01 N2 109.43(14) . . ?
N1 Zn01 N2 113.35(18) . . ?
O1 Zn01 N3 116.61(11) . . ?
N1 Zn01 N3 113.19(14) . . ?
N2 Zn01 N3 102.96(15) . . ?
Zn01 N1 H1A 109.5 . . ?
Zn01 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
Zn01 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Zn01 N2 H2A 109.5 . . ?
Zn01 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
Zn01 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
Zn01 N3 H3A 109.5 . . ?
Zn01 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
Zn01 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
B1 O1 B2 110.2(2) . . ?
B1 O1 Zn01 124.31(19) . . ?
B2 O1 Zn01 121.14(17) . . ?
O2 B1 O3 107.0(3) . . ?
O2 B1 O5 112.3(3) . . ?
O3 B1 O5 109.3(3) . . ?
O2 B1 O1 111.8(3) . . ?
O3 B1 O1 110.2(2) . . ?
O5 B1 O1 106.2(3) . . ?
O4 B2 O9 112.7(3) . . ?
O4 B2 O1 113.0(3) . . ?
O9 B2 O1 107.1(2) . . ?
O4 B2 O7 106.8(2) . . ?
O9 B2 O7 109.0(3) . . ?
O1 B2 O7 108.1(3) . . ?
B1 O2 H2 109.5 . . ?
O3 B3 O7 123.2(3) . . ?
O3 B3 O6 120.2(3) . . ?
O7 B3 O6 116.5(3) . . ?
B3 O3 B1 121.7(3) . . ?
B2 O4 H4 109.5 . . ?
O8 B4 O9 116.6(3) . . ?
O8 B4 O5 121.1(3) . . ?
O9 B4 O5 122.3(3) . . ?
B4 O5 B1 116.5(2) . . ?
B4 O8 H8 109.5 . . ?
B3 O7 B2 116.8(2) . . ?
B3 O6 H6 109.5 . . ?
B4 O9 B2 122.5(2) . . ?
H1WA O1W H1WB 108.6 . . ?

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
B2 O1 B1 O2 169.4(2) . . . . ?
Zn01 O1 B1 O2 12.7(4) . . . . ?
B2 O1 B1 O3 50.6(4) . . . . ?
Zn01 O1 B1 O3 -106.1(3) . . . . ?
B2 O1 B1 O5 -67.7(3) . . . . ?
Zn01 O1 B1 O5 135.5(2) . . . . ?
B1 O1 B2 O4 -180.0(2) . . . . ?
Zn01 O1 B2 O4 -22.4(4) . . . . ?
B1 O1 B2 O9 55.3(3) . . . . ?
Zn01 O1 B2 O9 -147.1(2) . . . . ?
B1 O1 B2 O7 -62.0(3) . . . . ?
Zn01 O1 B2 O7 95.6(3) . . . . ?
O7 B3 O3 B1 -3.9(5) . . . . ?
O6 B3 O3 B1 178.4(3) . . . . ?
O2 B1 O3 B3 -139.6(3) . . . . ?
O5 B1 O3 B3 98.6(3) . . . . ?
O1 B1 O3 B3 -17.8(4) . . . . ?
O8 B4 O5 B1 169.4(3) . . . . ?
O9 B4 O5 B1 -8.1(5) . . . . ?
O2 B1 O5 B4 165.0(3) . . . . ?
O3 B1 O5 B4 -76.5(4) . . . . ?
O1 B1 O5 B4 42.4(4) . . . . ?
O3 B3 O7 B2 -8.4(5) . . . . ?
O6 B3 O7 B2 169.3(3) . . . . ?
O4 B2 O7 B3 162.7(3) . . . . ?
O9 B2 O7 B3 -75.3(4) . . . . ?
O1 B2 O7 B3 40.8(4) . . . . ?
O8 B4 O9 B2 178.0(3) . . . . ?
O5 B4 O9 B2 -4.4(5) . . . . ?
O4 B2 O9 B4 -144.3(3) . . . . ?
O1 B2 O9 B4 -19.3(4) . . . . ?
O7 B2 O9 B4 97.4(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O6 0.89 2.59 3.150(4) 121.6 1_565
N1 H1A O1W 0.89 2.35 3.235(5) 171.9 1_565
N1 H1B O5 0.89 2.06 2.950(4) 177.4 3_455
N1 H1C O8 0.89 2.21 2.980(4) 144.4 4_454
N2 H2B O9 0.89 2.42 3.281(4) 162.3 1_565
N2 H2C O2 0.89 2.52 3.308(5) 147.5 2_565
N3 H3A O7 0.89 2.54 3.410(4) 167.3 3
N3 H3B O3 0.89 2.41 3.278(4) 166.6 1_565
N3 H3C O9 0.89 2.14 3.012(4) 166.7 2_564
O2 H2 O6 0.82 1.95 2.701(3) 152.7 3
O4 H4 O2 0.82 1.89 2.711(4) 173.5 2_565
O8 H8 O4 0.82 2.17 2.704(3) 123.3 3_545
O6 H6 O1W 0.82 1.97 2.717(4) 151.1 .
O1W H1WA O7 0.85 1.92 2.752(4) 169.7 2_554
O1W H1WB O1 0.88 2.29 3.131(4) 159.4 4_454
O1W H1WB O5 0.88 2.50 3.171(5) 134.1 4_454

_refine_diff_density_max         0.333
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.079

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 'vapour diffusion '
####################################################################### 
# 
# 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_ZnNH34tetraborato_E2_final
_database_code_depnum_ccdc_archive 'CCDC 1532490'
_audit_update_record             
;
2017-02-13 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_ZnNH34tetraborato_E2_final 
;
PROBLEM: D-H Without Acceptor       N4     --  H4B    ...     Please Check
RESPONSE: H4B does not participate in the H-bond network for sterical reasons, still it shows short contacts (H...O) with O1 and O2 and O4W  at 2.71, 2.68 and 2.86 A respectively
;
# Added during the CSD deposition process: Monday 13 February 2017 05:16 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Zn 2+, (N H3)4, B4 O9 H4 2-, (H2 O)4'
_chemical_formula_sum            'B4 H24 N4 O13 Zn'
_chemical_formula_weight         396.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-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                   15.0796(9)
_cell_length_b                   11.8853(5)
_cell_length_c                   16.7606(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3003.9(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9955
_cell_measurement_theta_min      2.784
_cell_measurement_theta_max      30.195

_exptl_crystal_description       'capped octahedra'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_F_000             1648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.195
_exptl_absorpt_coefficient_mu    1.705
_shelx_estimated_absorpt_T_min   0.693
_shelx_estimated_absorpt_T_max   0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo Sealed Tube'
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       '\j and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            100416
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.200
_diffrn_reflns_theta_max         30.616
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4605
_reflns_number_gt                3806
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0298P)²+2.0035P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4605
_refine_ls_number_parameters     233
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0725
_refine_ls_wR_factor_gt          0.0658
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      3.564
_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
Zn01 Zn 0.64100(2) 0.81241(2) 0.61493(2) 0.02704(6) Uani 1 1 d . . . . .
N1 N 0.75516(10) 0.88183(12) 0.57680(8) 0.0310(3) Uani 1 1 d . . . . .
H1A H 0.7766 0.8418 0.5363 0.047 Uiso 1 1 calc R U . . .
H1B H 0.7943 0.8824 0.6165 0.047 Uiso 1 1 calc R U . . .
H1C H 0.7450 0.9520 0.5607 0.047 Uiso 1 1 calc R U . . .
N2 N 0.53783(10) 0.89410(13) 0.56541(9) 0.0365(3) Uani 1 1 d . . . . .
H2A H 0.5438 0.9677 0.5735 0.055 Uiso 1 1 calc R U . . .
H2B H 0.4876 0.8704 0.5876 0.055 Uiso 1 1 calc R U . . .
H2C H 0.5365 0.8803 0.5132 0.055 Uiso 1 1 calc R U . . .
N3 N 0.63415(9) 0.64769(12) 0.59063(8) 0.0276(3) Uani 1 1 d . . . . .
H3A H 0.6617 0.6338 0.5447 0.041 Uiso 1 1 calc R U . . .
H3B H 0.5776 0.6271 0.5867 0.041 Uiso 1 1 calc R U . . .
H3C H 0.6601 0.6090 0.6296 0.041 Uiso 1 1 calc R U . . .
N4 N 0.62220(9) 0.83981(14) 0.73239(8) 0.0331(3) Uani 1 1 d . . . . .
H4A H 0.6733 0.8308 0.7582 0.050 Uiso 1 1 calc R U . . .
H4B H 0.5825 0.7911 0.7511 0.050 Uiso 1 1 calc R U . . .
H4C H 0.6025 0.9096 0.7398 0.050 Uiso 1 1 calc R U . . .
O1 O 0.43022(6) 0.73177(8) 0.67617(6) 0.01678(18) Uani 1 1 d . . . . .
O2 O 0.41881(7) 0.85883(9) 0.79030(6) 0.0232(2) Uani 1 1 d D . . . .
H2 H 0.4328(12) 0.9164(13) 0.7716(5) 0.035 Uiso 1 1 calc DR U . . .
O3 O 0.31594(7) 0.71137(8) 0.77535(6) 0.01855(19) Uani 1 1 d . . . . .
O4 O 0.43175(7) 0.60471(9) 0.56323(6) 0.0255(2) Uani 1 1 d . . . . .
H4 H 0.4309 0.5392 0.5786 0.038 Uiso 1 1 calc DR U . . .
B1 B 0.37278(9) 0.79241(12) 0.73115(8) 0.0152(3) Uani 1 1 d . . . . .
B2 B 0.37859(10) 0.67322(12) 0.61597(9) 0.0164(3) Uani 1 1 d . . . . .
B3 B 0.28770(10) 0.61942(12) 0.73447(9) 0.0169(3) Uani 1 1 d . . . . .
O5 O 0.31279(7) 0.86890(8) 0.68358(6) 0.01938(19) Uani 1 1 d . . . . .
O6 O 0.23341(8) 0.54600(9) 0.77387(6) 0.0268(2) Uani 1 1 d D . . . .
H6 H 0.2172(12) 0.4977(14) 0.7436(7) 0.040 Uiso 1 1 calc DR U . . .
O9 O 0.32908(7) 0.75723(9) 0.56589(6) 0.0208(2) Uani 1 1 d . . . . .
O7 O 0.31055(7) 0.59981(8) 0.65626(6) 0.0208(2) Uani 1 1 d . . . . .
B4 B 0.29605(10) 0.84939(13) 0.60460(9) 0.0171(3) Uani 1 1 d . . . . .
O8 O 0.24367(8) 0.92187(9) 0.56194(6) 0.0270(2) Uani 1 1 d D . . . .
H8 H 0.2270(12) 0.9724(14) 0.5908(6) 0.041 Uiso 1 1 calc DR U . . .
O1W O 0.52439(8) 0.86655(11) 0.92272(7) 0.0313(3) Uani 1 1 d D . . . .
H1WA H 0.4935(14) 0.858(2) 0.8860(10) 0.047 Uiso 1 1 d D U . . .
H1WB H 0.4940(13) 0.871(2) 0.9596(10) 0.047 Uiso 1 1 d D U . . .
O2W O 0.49068(10) 1.06004(11) 0.73426(9) 0.0416(3) Uani 1 1 d D . . . .
H2WA H 0.4609(16) 1.092(2) 0.7020(13) 0.062 Uiso 1 1 d D U . . .
H2WB H 0.5095(17) 1.1108(17) 0.7596(14) 0.062 Uiso 1 1 d D U . . .
O3W O 0.38695(14) 0.62417(15) 0.92194(8) 0.0585(5) Uani 1 1 d D . . . .
H3WA H 0.371(2) 0.652(3) 0.8825(13) 0.088 Uiso 1 1 d D U . . .
H3WB H 0.368(2) 0.660(3) 0.9564(16) 0.088 Uiso 1 1 d D U . . .
O4W O 0.38569(12) 1.16406(16) 0.60684(11) 0.0542(4) Uani 1 1 d D . . . .
H4WA H 0.3347(11) 1.161(3) 0.5993(19) 0.081 Uiso 1 1 d D U . . .
H4WB H 0.4032(19) 1.2206(19) 0.5896(19) 0.081 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn01 N3 2.0023(14) . ?
Zn01 N2 2.0131(15) . ?
Zn01 N1 2.0132(14) . ?
Zn01 N4 2.0154(14) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
O1 B2 1.4520(17) . ?
O1 B1 1.4556(17) . ?
O2 B1 1.4451(17) . ?
O2 H2 0.782(15) . ?
O3 B3 1.3584(17) . ?
O3 B1 1.4870(17) . ?
O4 B2 1.4447(17) . ?
O4 H4 0.8200 . ?
B1 O5 1.5101(17) . ?
B2 O9 1.5030(18) . ?
B2 O7 1.5067(17) . ?
B3 O6 1.3667(17) . ?
B3 O7 1.3752(17) . ?
O5 B4 1.3675(17) . ?
O6 H6 0.804(15) . ?
O9 B4 1.3671(18) . ?
B4 O8 1.3702(18) . ?
O8 H8 0.811(15) . ?
O1W H1WA 0.779(14) . ?
O1W H1WB 0.772(14) . ?
O2W H2WA 0.796(15) . ?
O2W H2WB 0.791(15) . ?
O3W H3WA 0.776(16) . ?
O3W H3WB 0.773(16) . ?
O4W H4WA 0.779(16) . ?
O4W H4WB 0.778(16) . ?

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
N3 Zn01 N2 110.35(6) . . ?
N3 Zn01 N1 112.35(6) . . ?
N2 Zn01 N1 109.41(6) . . ?
N3 Zn01 N4 110.45(6) . . ?
N2 Zn01 N4 102.48(6) . . ?
N1 Zn01 N4 111.35(6) . . ?
Zn01 N1 H1A 109.5 . . ?
Zn01 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
Zn01 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
Zn01 N2 H2A 109.5 . . ?
Zn01 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
Zn01 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
Zn01 N3 H3A 109.5 . . ?
Zn01 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
Zn01 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Zn01 N4 H4A 109.5 . . ?
Zn01 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
Zn01 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
B2 O1 B1 110.98(10) . . ?
B1 O2 H2 109.5 . . ?
B3 O3 B1 116.78(10) . . ?
B2 O4 H4 109.5 . . ?
O2 B1 O1 114.77(11) . . ?
O2 B1 O3 106.79(11) . . ?
O1 B1 O3 109.74(10) . . ?
O2 B1 O5 108.73(11) . . ?
O1 B1 O5 108.69(10) . . ?
O3 B1 O5 107.92(10) . . ?
O4 B2 O1 113.44(12) . . ?
O4 B2 O9 107.96(11) . . ?
O1 B2 O9 109.64(11) . . ?
O4 B2 O7 109.01(11) . . ?
O1 B2 O7 109.34(10) . . ?
O9 B2 O7 107.26(11) . . ?
O3 B3 O6 117.24(12) . . ?
O3 B3 O7 122.58(12) . . ?
O6 B3 O7 120.16(12) . . ?
B4 O5 B1 121.30(11) . . ?
B3 O6 H6 109.5 . . ?
B4 O9 B2 116.63(10) . . ?
B3 O7 B2 119.98(11) . . ?
O9 B4 O5 121.88(12) . . ?
O9 B4 O8 117.78(12) . . ?
O5 B4 O8 120.33(12) . . ?
B4 O8 H8 109.5 . . ?
H1WA O1W H1WB 107(2) . . ?
H2WA O2W H2WB 102(2) . . ?
H3WA O3W H3WB 107(3) . . ?
H4WA O4W H4WB 108(2) . . ?

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
B2 O1 B1 O2 -176.41(11) . . . . ?
B2 O1 B1 O3 63.35(13) . . . . ?
B2 O1 B1 O5 -54.45(13) . . . . ?
B3 O3 B1 O2 -160.58(11) . . . . ?
B3 O3 B1 O1 -35.61(15) . . . . ?
B3 O3 B1 O5 82.67(13) . . . . ?
B1 O1 B2 O4 -175.66(11) . . . . ?
B1 O1 B2 O9 63.58(13) . . . . ?
B1 O1 B2 O7 -53.75(13) . . . . ?
B1 O3 B3 O6 -178.22(12) . . . . ?
B1 O3 B3 O7 0.73(19) . . . . ?
O2 B1 O5 B4 147.01(12) . . . . ?
O1 B1 O5 B4 21.44(16) . . . . ?
O3 B1 O5 B4 -97.51(14) . . . . ?
O4 B2 O9 B4 -161.41(12) . . . . ?
O1 B2 O9 B4 -37.37(16) . . . . ?
O7 B2 O9 B4 81.25(14) . . . . ?
O3 B3 O7 B2 8.2(2) . . . . ?
O6 B3 O7 B2 -172.91(12) . . . . ?
O4 B2 O7 B3 143.11(12) . . . . ?
O1 B2 O7 B3 18.58(17) . . . . ?
O9 B2 O7 B3 -100.24(14) . . . . ?
B2 O9 B4 O5 4.8(2) . . . . ?
B2 O9 B4 O8 -174.03(12) . . . . ?
B1 O5 B4 O9 3.2(2) . . . . ?
B1 O5 B4 O8 -177.92(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O9 0.89 2.22 3.1134(17) 179.3 4_566
N1 H1B O2 0.89 2.46 3.3355(19) 168.9 6_657
N1 H1C O8 0.89 2.55 3.2940(18) 141.6 5_676
N2 H2A O3W 0.89 2.13 2.968(2) 155.7 3_656
N2 H2B O1 0.89 2.38 3.1308(19) 142.1 .
N2 H2C O4W 0.89 2.39 3.185(3) 149.1 5_676
N3 H3A O8 0.89 2.27 3.1543(18) 171.3 4_566
N3 H3B O4 0.89 2.25 3.1284(18) 169.2 .
N3 H3C O6 0.89 2.10 2.9764(17) 169.3 6_657
N4 H4A O5 0.89 2.36 3.2191(18) 161.5 6_657
N4 H4C O2W 0.89 2.46 3.284(2) 154.3 .
O2 H2 O2W 0.78 2.02 2.7886(17) 169.2 .
O4 H4 O1W 0.82 2.16 2.9163(17) 153.3 3_646
O6 H6 O5 0.80 1.89 2.6843(14) 171.3 8_655
O8 H8 O7 0.81 1.95 2.7642(14) 177.0 8_665
O1W H1WA O2 0.779(14) 1.960(15) 2.7329(15) 172(3) .
O1W H1WB O4 0.772(14) 1.994(15) 2.7594(15) 171(2) 7_576
O2W H2WA O4W 0.796(15) 2.138(15) 2.932(2) 174(3) .
O2W H2WB O1 0.791(15) 2.013(15) 2.8005(16) 174(3) 3_656
O3W H3WA O3 0.776(16) 2.102(17) 2.8736(18) 173(4) .
O3W H3WB O9 0.773(16) 2.163(18) 2.9273(18) 170(4) 7_576
O4W H4WA O7 0.779(16) 2.50(2) 3.166(2) 145(3) 8_665
O4W H4WB O1W 0.778(16) 2.060(18) 2.806(2) 161(3) 3_656

_refine_diff_density_max         0.260
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.067

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: diluted ammonium hydroxide in water'
