# 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_ZG-3N-L
_audit_block_doi                 10.5517/ccdc.csd.cc1pd4y5
_database_code_depnum_ccdc_archive 'CCDC 1560817'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ZG-3N-L
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C0.83 H3.31 Ga0.38 N0.62 O4 P Zn0.62'
_chemical_formula_weight         183.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           214
_space_group_name_H-M_alt        'I 41 3 2'
_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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'

_cell_length_a                   18.0307(4)
_cell_length_b                   18.0307(4)
_cell_length_c                   18.0307(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5861.9(4)
_cell_formula_units_Z            48
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    20676
_cell_measurement_theta_min      3.196
_cell_measurement_theta_max      28.286


_exptl_crystal_description       Cube
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.501
_exptl_crystal_F_000             4319
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.490
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8465
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            28819
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.597
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1223
_reflns_number_gt                1196
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.648
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Organic species, N3C4H16 (protonated diethylenetriamine) were disordered and could not be located on difference maps. Unassigned electron densities were removed by using SQUEEZE in PLATON software package. Since the atom numbers of Zn and Ga are too close, the occupancy of them could not be properly refined. The fixed occupancy factors were obtained from ICP-AES data.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0224P)²+5.0349P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.012(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1223
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0145
_refine_ls_R_factor_gt           0.0138
_refine_ls_wR_factor_ref         0.0426
_refine_ls_wR_factor_gt          0.0424
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ga1 Ga 0.74199(2) 0.65207(2) 0.88881(2) 0.01821(10) Uani 0.38 1 d . . P . .
Zn1 Zn 0.74199(2) 0.65207(2) 0.88881(2) 0.01821(10) Uani 0.62 1 d . . P . .
P1 P 0.84801(4) 0.61481(3) 0.75662(3) 0.01781(16) Uani 1 1 d . . . . .
O1 O 0.77477(11) 0.60914(12) 0.79946(10) 0.0289(5) Uani 1 1 d . . . . .
O2 O 0.69597(10) 0.74516(11) 0.87054(12) 0.0287(4) Uani 1 1 d . . . . .
O3 O 0.82625(11) 0.66157(11) 0.95190(11) 0.0264(4) Uani 1 1 d . . . . .
O4 O 0.67324(11) 0.58476(11) 0.93146(10) 0.0254(4) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.01505(15) 0.02322(17) 0.01637(16) -0.00046(10) 0.00102(10) 0.00311(10)
Zn1 0.01505(15) 0.02322(17) 0.01637(16) -0.00046(10) 0.00102(10) 0.00311(10)
P1 0.0234(3) 0.0159(3) 0.0141(3) -0.0001(2) 0.0033(2) 0.0010(2)
O1 0.0267(10) 0.0409(12) 0.0192(9) -0.0061(8) 0.0053(8) -0.0007(8)
O2 0.0157(8) 0.0245(10) 0.0460(12) 0.0000(9) -0.0008(8) 0.0018(7)
O3 0.0222(9) 0.0294(10) 0.0278(10) 0.0000(8) -0.0057(8) 0.0016(8)
O4 0.0263(10) 0.0325(10) 0.0175(8) 0.0014(8) 0.0058(7) -0.0024(8)

_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
Ga1 O1 1.8825(19) . ?
Ga1 O4 1.898(2) . ?
Ga1 O2 1.9012(19) . ?
Ga1 O3 1.9058(19) . ?
P1 O2 1.5327(19) 5 ?
P1 O1 1.533(2) . ?
P1 O3 1.535(2) 37_446 ?
P1 O4 1.5376(19) 15_564 ?
O2 P1 1.5327(19) 9 ?
O3 P1 1.535(2) 37_446 ?
O4 P1 1.5376(19) 16_645 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ga1 O4 106.80(9) . . ?
O1 Ga1 O2 110.60(9) . . ?
O4 Ga1 O2 110.47(9) . . ?
O1 Ga1 O3 107.30(9) . . ?
O4 Ga1 O3 109.65(9) . . ?
O2 Ga1 O3 111.84(9) . . ?
O2 P1 O1 111.09(12) 5 . ?
O2 P1 O3 107.47(12) 5 37_446 ?
O1 P1 O3 111.56(11) . 37_446 ?
O2 P1 O4 110.38(11) 5 15_564 ?
O1 P1 O4 106.29(11) . 15_564 ?
O3 P1 O4 110.08(12) 37_446 15_564 ?
P1 O1 Ga1 132.39(13) . . ?
P1 O2 Ga1 125.57(12) 9 . ?
P1 O3 Ga1 125.79(13) 37_446 . ?
P1 O4 Ga1 123.32(12) 16_645 . ?

_refine_diff_density_max         0.253
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.054

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL 1 in I4(1)32
CELL 0.71073  18.03070  18.03070  18.03070  90.0000  90.0000  90.0000
ZERR   48.00   0.00040   0.00040   0.00040   0.0000   0.0000   0.0000
LATT -2
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SYMM 0.75+Y, 0.25+X, 0.25-Z
SYMM 0.75-Y, 0.75-X, 0.75-Z
SYMM 0.25+Y, 0.25-X, 0.75+Z
SYMM 0.25-Y, 0.75+X, 0.25+Z
SYMM 0.75+X, 0.25+Z, 0.25-Y
SYMM 0.25-X, 0.75+Z, 0.25+Y
SYMM 0.75-X, 0.75-Z, 0.75-Y
SYMM 0.25+X, 0.25-Z, 0.75+Y
SYMM 0.75+Z, 0.25+Y, 0.25-X
SYMM 0.25+Z, 0.25-Y, 0.75+X
SYMM 0.25-Z, 0.75+Y, 0.25+X
SYMM 0.75-Z, 0.75-Y, 0.75-X
SFAC O P GA ZN C N H
UNIT 192 48 18.24 29.76 39.68 29.76 158.72

TEMP 23.000

L.S. 5 0   15
ACTA
BOND
FMAP 2
PLAN 20
EADP GA1 ZN1
EXYZ GA1 ZN1
TWIN
WGHT    0.022400    5.034900
BASF   0.01223
FVAR       0.41418
GA1   3    0.741987    0.652069    0.888808    10.38000    0.01505    0.02322 =
         0.01637   -0.00046    0.00102    0.00311
ZN1   4    0.741987    0.652069    0.888808    10.62000    0.01505    0.02322 =
         0.01637   -0.00046    0.00102    0.00311
P1    2    0.848006    0.614808    0.756624    11.00000    0.02341    0.01594 =
         0.01408   -0.00010    0.00333    0.00104
O1    1    0.774768    0.609141    0.799463    11.00000    0.02670    0.04092 =
         0.01916   -0.00612    0.00527   -0.00065
O2    1    0.695965    0.745165    0.870539    11.00000    0.01570    0.02451 =
         0.04600    0.00004   -0.00078    0.00183
O3    1    0.826253    0.661570    0.951899    11.00000    0.02216    0.02936 =
         0.02782   -0.00005   -0.00571    0.00163
O4    1    0.673243    0.584764    0.931462    11.00000    0.02627    0.03252 =
         0.01745    0.00143    0.00578   -0.00239
HKLF 4

REM  1 in I4(1)32
REM R1 =  0.0138 for    1196 Fo > 4sig(Fo)  and  0.0145 for all    1223 data
REM     56 parameters refined using      0 restraints

END

WGHT      0.0224      5.0304

REM Highest difference peak  0.253,  deepest hole -0.192,  1-sigma level  0.054
Q1    1   0.7500  0.8750  1.0000  10.25000  0.05    0.25
Q2    1   0.6664  0.7467  0.8642  11.00000  0.05    0.23
Q3    1   0.7588  0.6292  0.8372  11.00000  0.05    0.23
Q4    1   0.6612  0.5975  0.9628  11.00000  0.05    0.21
Q5    1   0.8750  0.8242  0.9258  10.50000  0.05    0.19
Q6    1   0.7887  0.6281  0.9154  11.00000  0.05    0.19
Q7    1   0.6557  0.5813  0.9469  11.00000  0.05    0.18
Q8    1   0.6615  0.5674  0.9377  11.00000  0.05    0.18
Q9    1   0.7052  0.7763  0.8547  11.00000  0.05    0.16
Q10   1   0.8079  0.8187  0.8566  11.00000  0.05    0.15
Q11   1   0.7858  0.8383  0.8402  11.00000  0.05    0.15
Q12   1   0.7891  0.8019  0.8767  11.00000  0.05    0.14
Q13   1   0.6528  0.7141  0.9049  11.00000  0.05    0.14
Q14   1   0.8042  0.8103  0.8731  11.00000  0.05    0.13
Q15   1   0.6609  0.5484  0.7104  11.00000  0.05    0.13
Q16   1   0.7994  0.8280  0.8396  11.00000  0.05    0.13
Q17   1   0.6903  0.7312  0.8303  11.00000  0.05    0.12
Q18   1   0.9235  0.7539  0.9103  11.00000  0.05    0.12
Q19   1   0.8126  0.6132  0.7966  11.00000  0.05    0.12
Q20   1   0.7722  0.6711  0.7994  11.00000  0.05    0.12
;
_shelx_res_checksum              50220

# SQUEEZE RESULTS (Version =  30715)
# 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 -0.028 0.214 0.627 950 313 ' '
2 0.010 0.233 0.125 994 332 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The integral electron density in the voids is 645 electrons. The elctron density for N3C4H16 (protonated diethylenetriamine) calculated from the formula (N3C4H16)0.21(Zn0.62Ga0.38PO4) is 615 electrons.
;
####################################################################### 
# 
# 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_ZG-5N-H
_audit_block_doi                 10.5517/ccdc.csd.cc1pd53c
_database_code_depnum_ccdc_archive 'CCDC 1560822'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ZG-5N-H
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C0.96 H3.36 Ga0.40 N0.60 O4 P Zn0.60'
_chemical_formula_weight         185.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           214
_space_group_name_H-M_alt        'I 41 3 2'
_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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'

_cell_length_a                   18.0053(7)
_cell_length_b                   18.0053(7)
_cell_length_c                   18.0053(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5837.2(7)
_cell_formula_units_Z            48
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    19587
_cell_measurement_theta_min      3.195
_cell_measurement_theta_max      28.317

_exptl_crystal_description       Cube
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.532
_exptl_crystal_F_000             4355
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.527
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8759
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            29923
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.599
_diffrn_reflns_theta_max         28.380
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1227
_reflns_number_gt                1202
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Organic species, N5C8H28 (protonated tetraethylenepentamine) were disordered and could not be located on difference maps. Unassigned electron densities were removed by using SQUEEZE in PLATON software package. Since the atom numbers of Zn and Ga are too close, the occupancy of them could not be properly refined. The fixed occupancy factors were obtained from ICP-AES data.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0151P)²+4.2551P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.017(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1227
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0138
_refine_ls_R_factor_gt           0.0131
_refine_ls_wR_factor_ref         0.0359
_refine_ls_wR_factor_gt          0.0357
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ga1 Ga 0.75819(2) 0.65206(2) 0.11114(2) 0.01844(8) Uani 0.4 1 d . . P . .
Zn1 Zn 0.75819(2) 0.65206(2) 0.11114(2) 0.01844(8) Uani 0.6 1 d . . P . .
P1 P 0.65222(3) 0.61498(3) 0.24329(3) 0.01833(14) Uani 1 1 d . . . . .
O1 O 0.72552(10) 0.60869(11) 0.20051(9) 0.0292(4) Uani 1 1 d . . . . .
O2 O 0.80377(9) 0.74574(10) 0.12984(11) 0.0288(4) Uani 1 1 d . . . . .
O3 O 0.67368(9) 0.66163(10) 0.04787(10) 0.0264(4) Uani 1 1 d . . . . .
O4 O 0.82704(10) 0.58448(10) 0.06865(9) 0.0259(4) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.01517(13) 0.02365(15) 0.01652(14) 0.00065(10) 0.00127(10) -0.00302(10)
Zn1 0.01517(13) 0.02365(15) 0.01652(14) 0.00065(10) 0.00127(10) -0.00302(10)
P1 0.0244(3) 0.0160(3) 0.0146(3) 0.0000(2) 0.0039(2) -0.0013(2)
O1 0.0262(9) 0.0410(11) 0.0206(8) 0.0060(7) 0.0060(7) 0.0004(8)
O2 0.0158(8) 0.0245(9) 0.0462(11) -0.0010(8) -0.0011(8) -0.0016(6)
O3 0.0218(8) 0.0292(9) 0.0283(9) 0.0008(7) -0.0062(7) -0.0019(7)
O4 0.0258(9) 0.0332(10) 0.0187(8) -0.0020(7) 0.0065(7) 0.0024(7)

_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
Ga1 O1 1.8829(17) . ?
Ga1 O4 1.8980(18) . ?
Ga1 O2 1.9059(17) . ?
Ga1 O3 1.9087(17) . ?
P1 O2 1.5301(17) 6_566 ?
P1 O1 1.5324(18) . ?
P1 O3 1.5346(18) 38_554 ?
P1 O4 1.5379(17) 16_645 ?
O2 P1 1.5301(17) 12_664 ?
O3 P1 1.5347(18) 38_554 ?
O4 P1 1.5379(17) 15_564 ?

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 Ga1 O4 106.42(8) . . ?
O1 Ga1 O2 110.52(8) . . ?
O4 Ga1 O2 110.94(8) . . ?
O1 Ga1 O3 107.36(8) . . ?
O4 Ga1 O3 109.76(8) . . ?
O2 Ga1 O3 111.65(8) . . ?
O2 P1 O1 111.24(11) 6_566 . ?
O2 P1 O3 107.38(11) 6_566 38_554 ?
O1 P1 O3 111.64(10) . 38_554 ?
O2 P1 O4 110.60(10) 6_566 16_645 ?
O1 P1 O4 106.05(10) . 16_645 ?
O3 P1 O4 109.95(11) 38_554 16_645 ?
P1 O1 Ga1 131.92(12) . . ?
P1 O2 Ga1 124.92(11) 12_664 . ?
P1 O3 Ga1 125.61(11) 38_554 . ?
P1 O4 Ga1 123.08(11) 15_564 . ?

_refine_diff_density_max         0.227
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.045

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL 1 in I4(1)32
CELL 0.71073  18.00530  18.00530  18.00530  90.0000  90.0000  90.0000
ZERR   48.00   0.00070   0.00070   0.00070   0.0000   0.0000   0.0000
LATT -2
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SYMM 0.75+Y, 0.25+X, 0.25-Z
SYMM 0.75-Y, 0.75-X, 0.75-Z
SYMM 0.25+Y, 0.25-X, 0.75+Z
SYMM 0.25-Y, 0.75+X, 0.25+Z
SYMM 0.75+X, 0.25+Z, 0.25-Y
SYMM 0.25-X, 0.75+Z, 0.25+Y
SYMM 0.75-X, 0.75-Z, 0.75-Y
SYMM 0.25+X, 0.25-Z, 0.75+Y
SYMM 0.75+Z, 0.25+Y, 0.25-X
SYMM 0.25+Z, 0.25-Y, 0.75+X
SYMM 0.25-Z, 0.75+Y, 0.25+X
SYMM 0.75-Z, 0.75-Y, 0.75-X
SFAC O P GA ZN C N H
UNIT 192 48 19.2 28.8 46.08 28.8 161.28
TEMP 23.000

L.S. 5 0   16
ACTA
BOND
FMAP 2
PLAN 20

EADP ZN1 GA1
EXYZ ZN1 GA1
TWIN
WGHT    0.015100    4.255100
BASF   0.01675
FVAR       0.42301
GA1   3    0.758192    0.652059    0.111135    10.40000    0.01517    0.02365 =
         0.01652    0.00065    0.00127   -0.00302
ZN1   4    0.758192    0.652059    0.111135    10.60000    0.01517    0.02365 =
         0.01652    0.00065    0.00127   -0.00302
P1    2    0.652216    0.614982    0.243293    11.00000    0.02440    0.01601 =
         0.01458    0.00003    0.00392   -0.00134
O1    1    0.725518    0.608687    0.200508    11.00000    0.02617    0.04097 =
         0.02061    0.00603    0.00597    0.00037
O2    1    0.803770    0.745743    0.129845    11.00000    0.01577    0.02453 =
         0.04617   -0.00102   -0.00112   -0.00160
O3    1    0.673677    0.661631    0.047869    11.00000    0.02178    0.02922 =
         0.02831    0.00084   -0.00622   -0.00191
O4    1    0.827038    0.584479    0.068652    11.00000    0.02583    0.03316 =
         0.01874   -0.00198    0.00645    0.00237
HKLF 4

REM  1 in I4(1)32
REM R1 =  0.0131 for    1202 Fo > 4sig(Fo)  and  0.0138 for all    1227 data
REM     56 parameters refined using      0 restraints

END

WGHT      0.0151      4.2551

REM Highest difference peak  0.227,  deepest hole -0.192,  1-sigma level  0.045
Q1    1   0.8391  0.7462  0.1342  11.00000  0.05    0.23
Q2    1   0.7369  0.6317  0.1617  11.00000  0.05    0.21
Q3    1   0.7139  0.6318  0.0784  11.00000  0.05    0.17
Q4    1   0.7403  0.6481  0.1696  11.00000  0.05    0.17
Q5    1   0.7074  0.6328  0.0880  11.00000  0.05    0.17
Q6    1   0.8408  0.5918  0.0354  11.00000  0.05    0.16
Q7    1   0.8452  0.7119  0.0997  11.00000  0.05    0.14
Q8    1   0.6987  0.6021  0.2050  11.00000  0.05    0.14
Q9    1   0.8075  0.7201  0.0994  11.00000  0.05    0.13
Q10   1   0.8354  0.5742  0.0510  11.00000  0.05    0.13
Q11   1   0.8421  0.5744  0.0839  11.00000  0.05    0.13
Q12   1   0.8174  0.7052  0.0944  11.00000  0.05    0.13
Q13   1   0.7075  0.6242  0.2248  11.00000  0.05    0.12
Q14   1   0.7923  0.7717  0.1398  11.00000  0.05    0.12
Q15   1   0.7747  0.7290  0.1489  11.00000  0.05    0.11
Q16   1   0.7500  0.8750  0.0000  10.25000  0.05    0.11
Q17   1   0.7169  0.8196  0.1097  11.00000  0.05    0.11
Q18   1   0.8003  0.7628  0.1366  11.00000  0.05    0.11
Q19   1   0.7010  0.8438  0.1568  11.00000  0.05    0.11
Q20   1   0.7500  0.7624  0.0000  10.50000  0.05    0.11
;
_shelx_res_checksum              71401

# SQUEEZE RESULTS (Version =  30715)
# 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 0.010 0.233 0.126 988 348 ' '
2 -0.025 0.216 0.625 939 319 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The integral electron density in the voids is 667 electrons. The elctron density for N5C8H28 (protonated tetraethylenepentamine) calculated from the formula (N5C8H28)0.12(Zn0.6Ga0.4PO4) is 639 electrons.
;
####################################################################### 
# 
# 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_ZG-3N-H
_audit_block_doi                 10.5517/ccdc.csd.cc1pd4z6
_database_code_depnum_ccdc_archive 'CCDC 1560818'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ZG-3N-H
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C0.84 H3.36 Ga0.37 N0.63 O4 P Zn0.63'
_chemical_formula_weight         184.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           214
_space_group_name_H-M_alt        'I 41 3 2'
_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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'

_cell_length_a                   18.0121(3)
_cell_length_b                   18.0121(3)
_cell_length_c                   18.0121(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5843.8(3)
_cell_formula_units_Z            48
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    18932
_cell_measurement_theta_min      2.769
_cell_measurement_theta_max      28.255

_exptl_crystal_description       Cube
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_F_000             4329
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.502
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7683
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            28518
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.599
_diffrn_reflns_theta_max         28.262
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1216
_reflns_number_gt                1187
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.648
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Organic species, N3C4H16 (protonated diethylenetriamine) were disordered and could not be located on difference maps. Unassigned electron densities were removed by using SQUEEZE in PLATON software package. Since the atom numbers of Zn and Ga are too close, the occupancy of them could not be properly refined. The fixed occupancy factors were obtained from ICP-AES data.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0265P)²+5.6574P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.009(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1216
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0152
_refine_ls_wR_factor_ref         0.0482
_refine_ls_wR_factor_gt          0.0480
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_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
Ga1 Ga 0.25796(2) 0.34786(2) 0.11120(2) 0.01821(11) Uani 0.37 1 d . . P . .
Zn1 Zn 0.25796(2) 0.34786(2) 0.11120(2) 0.01821(11) Uani 0.63 1 d . . P . .
P1 P 0.15205(4) 0.38521(4) 0.24340(4) 0.01804(18) Uani 1 1 d . . . . .
O1 O 0.22517(12) 0.39101(14) 0.20054(12) 0.0292(5) Uani 1 1 d . . . . .
O2 O 0.30406(11) 0.25452(12) 0.12952(14) 0.0292(5) Uani 1 1 d . . . . .
O3 O 0.17374(12) 0.33847(12) 0.04813(12) 0.0264(5) Uani 1 1 d . . . . .
O4 O 0.32678(12) 0.41551(12) 0.06835(11) 0.0258(4) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.01525(17) 0.02319(19) 0.01619(18) -0.00036(12) 0.00094(12) 0.00322(12)
Zn1 0.01525(17) 0.02319(19) 0.01619(18) -0.00036(12) 0.00094(12) 0.00322(12)
P1 0.0237(4) 0.0161(4) 0.0143(3) 0.0000(3) 0.0035(3) 0.0014(3)
O1 0.0256(11) 0.0420(14) 0.0201(10) -0.0054(9) 0.0052(9) -0.0003(9)
O2 0.0173(10) 0.0233(11) 0.0472(14) 0.0003(10) -0.0007(9) 0.0013(8)
O3 0.0215(10) 0.0286(11) 0.0290(12) -0.0004(9) -0.0047(9) 0.0008(8)
O4 0.0258(11) 0.0337(12) 0.0180(10) 0.0020(9) 0.0056(8) -0.0024(9)

_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
Ga1 O1 1.882(2) . ?
Ga1 O4 1.902(2) . ?
Ga1 O3 1.903(2) . ?
Ga1 O2 1.904(2) . ?
P1 O2 1.530(2) 5 ?
P1 O1 1.530(2) . ?
P1 O4 1.533(2) 39_454 ?
P1 O3 1.534(2) 13_455 ?
O2 P1 1.530(2) 9 ?
O3 P1 1.534(2) 13_455 ?
O4 P1 1.533(2) 40_544 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ga1 O4 106.68(10) . . ?
O1 Ga1 O3 107.28(10) . . ?
O4 Ga1 O3 109.53(10) . . ?
O1 Ga1 O2 110.69(10) . . ?
O4 Ga1 O2 110.60(10) . . ?
O3 Ga1 O2 111.88(10) . . ?
O2 P1 O1 111.07(14) 5 . ?
O2 P1 O4 110.69(12) 5 39_454 ?
O1 P1 O4 106.12(12) . 39_454 ?
O2 P1 O3 107.34(13) 5 13_455 ?
O1 P1 O3 111.45(13) . 13_455 ?
O4 P1 O3 110.21(13) 39_454 13_455 ?
P1 O1 Ga1 132.32(14) . . ?
P1 O2 Ga1 125.32(13) 9 . ?
P1 O3 Ga1 125.83(14) 13_455 . ?
P1 O4 Ga1 123.17(14) 40_544 . ?

_refine_diff_density_max         0.229
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.075

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL 1 in I4(1)32
CELL 0.71073  18.01210  18.01210  18.01210  90.0000  90.0000  90.0000
ZERR   48.00   0.00030   0.00030   0.00030   0.0000   0.0000   0.0000
LATT -2
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SYMM 0.75+Y, 0.25+X, 0.25-Z
SYMM 0.75-Y, 0.75-X, 0.75-Z
SYMM 0.25+Y, 0.25-X, 0.75+Z
SYMM 0.25-Y, 0.75+X, 0.25+Z
SYMM 0.75+X, 0.25+Z, 0.25-Y
SYMM 0.25-X, 0.75+Z, 0.25+Y
SYMM 0.75-X, 0.75-Z, 0.75-Y
SYMM 0.25+X, 0.25-Z, 0.75+Y
SYMM 0.75+Z, 0.25+Y, 0.25-X
SYMM 0.25+Z, 0.25-Y, 0.75+X
SYMM 0.25-Z, 0.75+Y, 0.25+X
SYMM 0.75-Z, 0.75-Y, 0.75-X
SFAC O P GA ZN C N H
UNIT 192 48 17.76 30.24 40.32 30.24 161.28
TEMP 23.000

L.S. 5 0   14
ACTA
BOND
FMAP 2
PLAN 20
EADP ZN1 GA1
EXYZ ZN1 GA1
TWIN
WGHT    0.026500    5.657400
BASF   0.00905
FVAR       0.40554
GA1   3    0.257965    0.347865    0.111201    10.37000    0.01525    0.02319 =
         0.01619   -0.00036    0.00094    0.00322
ZN1   4    0.257965    0.347865    0.111201    10.63000    0.01525    0.02319 =
         0.01619   -0.00036    0.00094    0.00322
P1    2    0.152050    0.385213    0.243400    11.00000    0.02374    0.01608 =
         0.01429   -0.00005    0.00348    0.00142
O1    1    0.225171    0.391014    0.200543    11.00000    0.02558    0.04197 =
         0.02011   -0.00537    0.00518   -0.00032
O2    1    0.304063    0.254516    0.129519    11.00000    0.01729    0.02326 =
         0.04716    0.00033   -0.00068    0.00129
O3    1    0.173741    0.338471    0.048127    11.00000    0.02146    0.02865 =
         0.02904   -0.00037   -0.00466    0.00077
O4    1    0.326776    0.415509    0.068353    11.00000    0.02584    0.03371 =
         0.01798    0.00203    0.00562   -0.00240
HKLF 4

REM  1 in I4(1)32
REM R1 =  0.0152 for    1187 Fo > 4sig(Fo)  and  0.0159 for all    1216 data
REM     56 parameters refined using      0 restraints

END

WGHT      0.0265      5.6574

REM Highest difference peak  0.229,  deepest hole -0.301,  1-sigma level  0.075
Q1    1   0.3249  0.2601  0.1371  11.00000  0.05    0.23
Q2    1   0.2070  0.3268  0.0940  11.00000  0.05    0.21
Q3    1   0.2447  0.2933  0.0660  11.00000  0.05    0.21
Q4    1   0.3475  0.4107  0.0328  11.00000  0.05    0.21
Q5    1   0.2425  0.2634  0.2108  11.00000  0.05    0.21
Q6    1   0.3013  0.2723  0.1534  11.00000  0.05    0.20
Q7    1   0.3081  0.2795  0.0623  11.00000  0.05    0.19
Q8    1   0.3406  0.2564  0.1282  11.00000  0.05    0.18
Q9    1   0.2882  0.2586  0.1759  11.00000  0.05    0.18
Q10   1   0.2851  0.2526  0.1873  11.00000  0.05    0.18
Q11   1   0.2054  0.3110  0.0823  11.00000  0.05    0.18
Q12   1   0.2222  0.2711  0.1975  11.00000  0.05    0.18
Q13   1   0.3213  0.2857  0.0608  11.00000  0.05    0.17
Q14   1   0.2419  0.4646  0.2657  11.00000  0.05    0.17
Q15   1   0.3016  0.5516  0.1250  10.50000  0.05    0.15
Q16   1   0.2972  0.4766  0.0441  11.00000  0.05    0.15
Q17   1   0.3484  0.4186  0.0504  11.00000  0.05    0.15
Q18   1   0.1250  0.2154  0.0346  10.50000  0.05    0.15
Q19   1   0.2853  0.4686  0.0660  11.00000  0.05    0.14
Q20   1   0.3426  0.2984  0.0520  11.00000  0.05    0.14
;
_shelx_res_checksum              14029

# SQUEEZE RESULTS (Version =  30715)
# 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 0.015 0.227 0.131 947 277 ' '
2 -0.020 0.223 0.616 989 315 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The integral electron density in the voids is 592 electrons. The elctron density for N3C4H16 (protonated diethylenetriamine) calculated from from the formula (N3C4H16)0.21(Zn0.63Ga0.37PO4) is 614 electrons.
;
####################################################################### 
# 
# 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_ZG-4N-H
_audit_block_doi                 10.5517/ccdc.csd.cc1pd519
_database_code_depnum_ccdc_archive 'CCDC 1560820'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ZG-4N-H
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C0.90 H3.30 Ga0.40 N0.60 O4 P Zn0.60'
_chemical_formula_weight         184.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           214
_space_group_name_H-M_alt        'I 41 3 2'
_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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'

_cell_length_a                   17.9625(5)
_cell_length_b                   17.9625(5)
_cell_length_c                   17.9625(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5795.6(5)
_cell_formula_units_Z            48
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    20358
_cell_measurement_theta_min      2.776
_cell_measurement_theta_max      28.276

_exptl_crystal_description       Cube
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.539
_exptl_crystal_F_000             4334
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.566
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7662
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            28170
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.603
_diffrn_reflns_theta_max         28.293
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1214
_reflns_number_gt                1188
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.649
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Organic species, N4C6H22 (protonated triethylenetetramine) were disordered and could not be located on difference maps. Unassigned electron densities were removed by using SQUEEZE in PLATON software package. Since the atom numbers of Zn and Ga are too close, the occupancy of them could not be properly refined. The fixed occupancy factors were obtained from ICP-AES data.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0257P)²+4.7992P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.014(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1214
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0152
_refine_ls_wR_factor_ref         0.0452
_refine_ls_wR_factor_gt          0.0450
_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
Ga1 Ga 0.24176(2) 0.34761(2) 0.88867(2) 0.01723(10) Uani 0.4 1 d . . P . .
Zn1 Zn 0.24176(2) 0.34761(2) 0.88867(2) 0.01723(10) Uani 0.6 1 d . . P . .
P1 P 0.34803(4) 0.38503(4) 0.75694(4) 0.01747(17) Uani 1 1 d . . . . .
O1 O 0.27477(12) 0.39184(13) 0.79982(11) 0.0276(5) Uani 1 1 d . . . . .
O2 O 0.19638(11) 0.25365(11) 0.87022(13) 0.0280(5) Uani 1 1 d . . . . .
O3 O 0.32654(11) 0.33774(12) 0.95181(12) 0.0255(4) Uani 1 1 d . . . . .
O4 O 0.17302(12) 0.41536(12) 0.93154(11) 0.0255(4) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.01406(16) 0.02200(18) 0.01562(17) 0.00088(11) 0.00100(11) -0.00282(11)
Zn1 0.01406(16) 0.02200(18) 0.01562(17) 0.00088(11) 0.00100(11) -0.00282(11)
P1 0.0237(4) 0.0152(3) 0.0135(3) -0.0002(2) 0.0043(3) -0.0016(2)
O1 0.0248(11) 0.0386(13) 0.0193(10) 0.0048(8) 0.0053(8) -0.0002(9)
O2 0.0156(9) 0.0225(10) 0.0458(13) -0.0021(10) 0.0005(9) -0.0007(7)
O3 0.0210(10) 0.0274(10) 0.0282(11) 0.0018(9) -0.0066(8) -0.0002(8)
O4 0.0246(10) 0.0331(11) 0.0189(9) -0.0028(9) 0.0060(8) 0.0016(9)

_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
Ga1 O1 1.879(2) . ?
Ga1 O4 1.897(2) . ?
Ga1 O2 1.903(2) . ?
Ga1 O3 1.907(2) . ?
P1 O2 1.528(2) 6_456 ?
P1 O1 1.530(2) . ?
P1 O3 1.535(2) 14_556 ?
P1 O4 1.536(2) 40_544 ?
O2 P1 1.527(2) 12_565 ?
O3 P1 1.535(2) 14_556 ?
O4 P1 1.536(2) 39_454 ?

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 Ga1 O4 106.19(9) . . ?
O1 Ga1 O2 111.24(10) . . ?
O4 Ga1 O2 111.15(9) . . ?
O1 Ga1 O3 107.00(9) . . ?
O4 Ga1 O3 109.76(9) . . ?
O2 Ga1 O3 111.29(9) . . ?
O2 P1 O1 111.33(13) 6_456 . ?
O2 P1 O3 107.14(13) 6_456 14_556 ?
O1 P1 O3 111.56(12) . 14_556 ?
O2 P1 O4 110.87(12) 6_456 40_544 ?
O1 P1 O4 105.89(12) . 40_544 ?
O3 P1 O4 110.10(12) 14_556 40_544 ?
P1 O1 Ga1 131.71(14) . . ?
P1 O2 Ga1 124.46(13) 12_565 . ?
P1 O3 Ga1 125.19(13) 14_556 . ?
P1 O4 Ga1 123.14(13) 39_454 . ?

_refine_diff_density_max         0.241
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.063

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL 1 in I4(1)32
CELL 0.71073  17.96250  17.96250  17.96250  90.0000  90.0000  90.0000
ZERR   48.00   0.00050   0.00050   0.00050   0.0000   0.0000   0.0000
LATT -2
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SYMM 0.75+Y, 0.25+X, 0.25-Z
SYMM 0.75-Y, 0.75-X, 0.75-Z
SYMM 0.25+Y, 0.25-X, 0.75+Z
SYMM 0.25-Y, 0.75+X, 0.25+Z
SYMM 0.75+X, 0.25+Z, 0.25-Y
SYMM 0.25-X, 0.75+Z, 0.25+Y
SYMM 0.75-X, 0.75-Z, 0.75-Y
SYMM 0.25+X, 0.25-Z, 0.75+Y
SYMM 0.75+Z, 0.25+Y, 0.25-X
SYMM 0.25+Z, 0.25-Y, 0.75+X
SYMM 0.25-Z, 0.75+Y, 0.25+X
SYMM 0.75-Z, 0.75-Y, 0.75-X
SFAC O P GA ZN C N H
UNIT 192 48 19.2 28.8 43.2 28.8 158.4
TEMP 23.000

L.S. 5 0   17
ACTA
BOND
FMAP 2
PLAN 20

EADP ZN1 GA1
EXYZ ZN1 GA1
TWIN

WGHT    0.025700    4.799200
BASF   0.01360
FVAR       0.41515
GA1   3    0.241760    0.347608    0.888673    10.40000    0.01406    0.02200 =
         0.01562    0.00088    0.00100   -0.00282
ZN1   4    0.241760    0.347608    0.888673    10.60000    0.01406    0.02200 =
         0.01562    0.00088    0.00100   -0.00282
P1    2    0.348034    0.385029    0.756944    11.00000    0.02373    0.01523 =
         0.01346   -0.00024    0.00427   -0.00160
O1    1    0.274773    0.391845    0.799824    11.00000    0.02484    0.03861 =
         0.01931    0.00483    0.00528   -0.00020
O2    1    0.196383    0.253653    0.870217    11.00000    0.01562    0.02250 =
         0.04579   -0.00206    0.00048   -0.00066
O3    1    0.326540    0.337742    0.951812    11.00000    0.02098    0.02743 =
         0.02818    0.00177   -0.00663   -0.00019
O4    1    0.173022    0.415358    0.931536    11.00000    0.02460    0.03311 =
         0.01892   -0.00275    0.00601    0.00162
HKLF 4

REM  1 in I4(1)32
REM R1 =  0.0152 for    1188 Fo > 4sig(Fo)  and  0.0159 for all    1214 data
REM     56 parameters refined using      0 restraints

END

WGHT      0.0257      4.7924

REM Highest difference peak  0.241,  deepest hole -0.232,  1-sigma level  0.063
Q1    1   0.3750  0.1250  0.8750  10.16667  0.05    0.24
Q2    1   0.2508  0.2975  0.9502  11.00000  0.05    0.20
Q3    1   0.1571  0.2590  0.8777  11.00000  0.05    0.20
Q4    1   0.1742  0.5248  0.8519  11.00000  0.05    0.20
Q5    1   0.1953  0.2820  0.9352  11.00000  0.05    0.18
Q6    1   0.2845  0.3566  0.9263  11.00000  0.05    0.18
Q7    1   0.3095  0.3333  0.9097  11.00000  0.05    0.18
Q8    1   0.2965  0.3401  0.9349  11.00000  0.05    0.17
Q9    1   0.1962  0.4414  0.9298  11.00000  0.05    0.17
Q10   1   0.3815  0.2137  0.9536  11.00000  0.05    0.16
Q11   1   0.2341  0.4285  0.9826  11.00000  0.05    0.16
Q12   1   0.3726  0.2740  0.9112  11.00000  0.05    0.16
Q13   1   0.1696  0.4071  0.9520  11.00000  0.05    0.16
Q14   1   0.3998  0.2996  0.9274  11.00000  0.05    0.16
Q15   1   0.1507  0.4251  0.9304  11.00000  0.05    0.15
Q16   1   0.4217  0.2938  0.9263  11.00000  0.05    0.15
Q17   1   0.1922  0.3908  0.9373  11.00000  0.05    0.15
Q18   1   0.1633  0.4025  0.9623  11.00000  0.05    0.15
Q19   1   0.1359  0.4678  0.7556  11.00000  0.05    0.14
Q20   1   0.2305  0.4852  0.9588  11.00000  0.05    0.13
;
_shelx_res_checksum              4904

# SQUEEZE RESULTS (Version =  30715)
# 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 0.015 0.225 0.133 932 349 ' '
2 -0.020 0.224 0.624 989 367 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The integral electron density in the voids is 716 electrons. The elctron density for N4C6H22 (protonated triethylenetetramine) calculated from the formula (N4C6H22)0.15(Zn0.6Ga0.4PO4) is 619 electrons.
;
####################################################################### 
# 
# 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_ZG-5N-L
_audit_block_doi                 10.5517/ccdc.csd.cc1pd52b
_database_code_depnum_ccdc_archive 'CCDC 1560821'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ZG-5N-L
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C0.91 H3.19 Ga0.43 N0.57 O4 P Zn0.57'
_chemical_formula_weight         184.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           214
_space_group_name_H-M_alt        'I 41 3 2'
_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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'

_cell_length_a                   18.0228(13)
_cell_length_b                   18.0228(13)
_cell_length_c                   18.0228(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5854.2(13)
_cell_formula_units_Z            48
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    17342
_cell_measurement_theta_min      3.195
_cell_measurement_theta_max      28.303

_exptl_crystal_description       Cube
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.510
_exptl_crystal_F_000             4324
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.528
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8345
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            27922
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.598
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1224
_reflns_number_gt                1188
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Organic species, N5C8H28 (protonated tetraethylenepentamine) were disordered and could not be located on difference maps. Unassigned electron densities were removed by using SQUEEZE in PLATON software package. Since the atom numbers of Zn and Ga are too close, the occupancy of them could not be properly refined. The fixed occupancy factors were obtained from ICP-AES data.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0193P)²+4.0977P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.028(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1224
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0147
_refine_ls_wR_factor_ref         0.0400
_refine_ls_wR_factor_gt          0.0397
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_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
Ga1 Ga 0.25826(2) 0.34809(2) 0.11109(2) 0.01903(9) Uani 0.43 1 d . . P . .
Zn1 Zn 0.25826(2) 0.34809(2) 0.11109(2) 0.01903(9) Uani 0.57 1 d . . P . .
P1 P 0.38503(4) 0.24327(3) 0.15222(4) 0.01841(16) Uani 1 1 d . . . . .
O1 O 0.30388(10) 0.25416(11) 0.12949(12) 0.0292(4) Uani 1 1 d . . . . .
O2 O 0.22532(11) 0.39117(12) 0.20064(10) 0.0299(5) Uani 1 1 d . . . . .
O3 O 0.17376(11) 0.33856(11) 0.04786(11) 0.0268(4) Uani 1 1 d . . . . .
O4 O 0.32717(11) 0.41564(11) 0.06859(10) 0.0265(4) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.01576(15) 0.02453(17) 0.01679(16) -0.00067(11) 0.00109(11) 0.00294(11)
Zn1 0.01576(15) 0.02453(17) 0.01679(16) -0.00067(11) 0.00109(11) 0.00294(11)
P1 0.0162(3) 0.0146(3) 0.0244(3) 0.0037(3) 0.0017(2) -0.0001(2)
O1 0.0166(9) 0.0240(10) 0.0468(13) 0.0002(10) -0.0007(9) 0.0012(7)
O2 0.0256(10) 0.0430(13) 0.0210(9) -0.0067(9) 0.0059(8) 0.0000(9)
O3 0.0227(10) 0.0298(10) 0.0281(10) -0.0015(8) -0.0061(8) 0.0016(8)
O4 0.0269(10) 0.0341(11) 0.0185(9) 0.0039(8) 0.0057(8) -0.0010(8)

_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
Ga1 O2 1.8868(19) . ?
Ga1 O4 1.900(2) . ?
Ga1 O3 1.9098(19) . ?
Ga1 O1 1.9110(19) . ?
P1 O2 1.529(2) 9 ?
P1 O1 1.5315(19) . ?
P1 O3 1.534(2) 20_554 ?
P1 O4 1.5380(19) 42_544 ?
O2 P1 1.529(2) 5 ?
O3 P1 1.534(2) 17_455 ?
O4 P1 1.5380(19) 42_544 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ga1 O4 106.67(9) . . ?
O2 Ga1 O3 107.25(9) . . ?
O4 Ga1 O3 109.77(9) . . ?
O2 Ga1 O1 110.58(9) . . ?
O4 Ga1 O1 110.88(8) . . ?
O3 Ga1 O1 111.53(9) . . ?
O2 P1 O1 111.34(12) 9 . ?
O2 P1 O3 111.64(12) 9 20_554 ?
O1 P1 O3 107.25(12) . 20_554 ?
O2 P1 O4 106.01(11) 9 42_544 ?
O1 P1 O4 110.61(11) . 42_544 ?
O3 P1 O4 110.04(12) 20_554 42_544 ?
P1 O1 Ga1 124.80(12) . . ?
P1 O2 Ga1 132.15(13) 5 . ?
P1 O3 Ga1 125.73(13) 17_455 . ?
P1 O4 Ga1 122.99(12) 42_544 . ?

_refine_diff_density_max         0.259
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.051

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL 1 in I4(1)32
CELL 0.71073  18.02280  18.02280  18.02280  90.0000  90.0000  90.0000
ZERR   48.00   0.00130   0.00130   0.00130   0.0000   0.0000   0.0000
LATT -2
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SYMM 0.75+Y, 0.25+X, 0.25-Z
SYMM 0.75-Y, 0.75-X, 0.75-Z
SYMM 0.25+Y, 0.25-X, 0.75+Z
SYMM 0.25-Y, 0.75+X, 0.25+Z
SYMM 0.75+X, 0.25+Z, 0.25-Y
SYMM 0.25-X, 0.75+Z, 0.25+Y
SYMM 0.75-X, 0.75-Z, 0.75-Y
SYMM 0.25+X, 0.25-Z, 0.75+Y
SYMM 0.75+Z, 0.25+Y, 0.25-X
SYMM 0.25+Z, 0.25-Y, 0.75+X
SYMM 0.25-Z, 0.75+Y, 0.25+X
SYMM 0.75-Z, 0.75-Y, 0.75-X
SFAC O P GA ZN C N H
UNIT 192 48 20.64 27.36 43.776 27.36 153.216
TEMP 23.000

L.S. 5 0   16
ACTA
BOND
FMAP 2
PLAN 20

EADP ZN1 GA1
EXYZ ZN1 GA1
TWIN

WGHT    0.019300    4.097700
BASF   0.02793
FVAR       0.41505
GA1   3    0.258261    0.348092    0.111091    10.43000    0.01576    0.02453 =
         0.01679   -0.00067    0.00109    0.00294
ZN1   4    0.258261    0.348092    0.111091    10.57000    0.01576    0.02453 =
         0.01679   -0.00067    0.00109    0.00294
P1    2    0.385033    0.243269    0.152215    11.00000    0.01623    0.01460 =
         0.02439    0.00371    0.00170   -0.00013
O1    1    0.303876    0.254156    0.129494    11.00000    0.01665    0.02402 =
         0.04680    0.00023   -0.00070    0.00120
O2    1    0.225317    0.391173    0.200642    11.00000    0.02565    0.04298 =
         0.02101   -0.00674    0.00591   -0.00001
O3    1    0.173764    0.338562    0.047860    11.00000    0.02268    0.02978 =
         0.02807   -0.00151   -0.00613    0.00159
O4    1    0.327169    0.415643    0.068592    11.00000    0.02689    0.03410 =
         0.01854    0.00390    0.00574   -0.00104
HKLF 4

REM  1 in I4(1)32
REM R1 =  0.0147 for    1188 Fo > 4sig(Fo)  and  0.0158 for all    1224 data
REM     56 parameters refined using      0 restraints

END

WGHT      0.0193      4.0978

REM Highest difference peak  0.259,  deepest hole -0.187,  1-sigma level  0.051
Q1    1   0.3446  0.2550  0.1316  11.00000  0.05    0.26
Q2    1   0.3399  0.4121  0.0345  11.00000  0.05    0.20
Q3    1   0.3230  0.5219  0.1622  11.00000  0.05    0.18
Q4    1   0.2321  0.3561  0.1621  11.00000  0.05    0.17
Q5    1   0.1999  0.3453  0.0994  11.00000  0.05    0.17
Q6    1   0.3068  0.2725  0.1580  11.00000  0.05    0.17
Q7    1   0.1864  0.3282  0.0986  11.00000  0.05    0.17
Q8    1   0.3476  0.4158  0.0502  11.00000  0.05    0.17
Q9    1   0.3750  0.5000  0.2500  10.25000  0.05    0.13
Q10   1   0.2839  0.5339  0.1250  10.50000  0.05    0.13
Q11   1   0.0811  0.2968  0.0791  11.00000  0.05    0.13
Q12   1   0.2442  0.2990  0.0564  11.00000  0.05    0.13
Q13   1   0.3188  0.5074  0.1831  11.00000  0.05    0.12
Q14   1   0.3318  0.5188  0.1398  11.00000  0.05    0.12
Q15   1   0.1581  0.3507  0.0721  11.00000  0.05    0.12
Q16   1   0.2628  0.2969  0.0960  11.00000  0.05    0.12
Q17   1   0.2250  0.3070  0.0556  11.00000  0.05    0.12
Q18   1   0.3521  0.5264  0.1212  11.00000  0.05    0.12
Q19   1   0.1676  0.3366  0.0881  11.00000  0.05    0.12
Q20   1   0.2541  0.4327  0.0579  11.00000  0.05    0.12
;
_shelx_res_checksum              7354

# SQUEEZE RESULTS (Version =  30715)
# 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 0.015 0.227 0.131 944 329 ' '
2 -0.020 0.223 0.616 990 354 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The integral electron density in the voids is 683 electrons. The elctron density for N5C8H28 (protonated tetraethylenepentamine) calculated from the formula (N5C8H28)0.114(Zn0.57Ga0.43PO4) is 607 electrons.
;
####################################################################### 
# 
# 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_ZG-6N-H
_audit_block_doi                 10.5517/ccdc.csd.cc1pd54d
_database_code_depnum_ccdc_archive 'CCDC 1560823'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ZG-6N-H
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C0.93 H3.17 Ga0.44 N0.56 O4 P Zn0.56'
_chemical_formula_weight         184.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           214
_space_group_name_H-M_alt        'I 41 3 2'
_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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'

_cell_length_a                   17.9470(2)
_cell_length_b                   17.9470(2)
_cell_length_c                   17.9470(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5780.64(19)
_cell_formula_units_Z            48
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    18531
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      28.219

_exptl_crystal_description       Cube
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.544
_exptl_crystal_F_000             4326
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.604
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7494
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            29004
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.605
_diffrn_reflns_theta_max         28.212
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1207
_reflns_number_gt                1184
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Organic species, N6C10H34 (protonated pentaethylenehexamine) were disordered and could not be located on difference maps. Unassigned electron densities were removed by using SQUEEZE in PLATON software package. Since the atom numbers of Zn and Ga are too close, the occupancy of them could not be properly refined. The fixed occupancy factors were obtained from ICP-AES data.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0243P)²+5.6150P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.027(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1207
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0160
_refine_ls_R_factor_gt           0.0155
_refine_ls_wR_factor_ref         0.0441
_refine_ls_wR_factor_gt          0.0439
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ga1 Ga 0.74193(2) 0.65241(2) 0.88871(2) 0.01180(10) Uani 0.44 1 d . . P . .
Zn1 Zn 0.74193(2) 0.65241(2) 0.88871(2) 0.01180(10) Uani 0.56 1 d . . P . .
P1 P 0.84759(4) 0.61479(4) 0.75663(4) 0.01233(16) Uani 1 1 d . . . . .
O1 O 0.77411(11) 0.60778(12) 0.79959(11) 0.0196(4) Uani 1 1 d . . . . .
O2 O 0.69668(11) 0.74587(11) 0.86961(12) 0.0203(4) Uani 1 1 d . . . . .
O3 O 0.82618(11) 0.66197(11) 0.95215(11) 0.0178(4) Uani 1 1 d . . . . .
O4 O 0.67317(12) 0.58428(11) 0.93090(11) 0.0176(4) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.00908(15) 0.01569(17) 0.01063(17) -0.00094(11) 0.00074(11) 0.00177(11)
Zn1 0.00908(15) 0.01569(17) 0.01063(17) -0.00094(11) 0.00074(11) 0.00177(11)
P1 0.0165(3) 0.0101(3) 0.0104(3) -0.0003(2) 0.0029(3) 0.0011(2)
O1 0.0172(10) 0.0290(12) 0.0126(9) -0.0038(8) 0.0026(7) 0.0001(8)
O2 0.0099(9) 0.0178(10) 0.0333(12) 0.0014(9) 0.0005(8) 0.0007(7)
O3 0.0134(9) 0.0199(10) 0.0199(10) -0.0013(8) -0.0041(8) 0.0012(8)
O4 0.0172(10) 0.0238(11) 0.0117(9) 0.0020(8) 0.0044(7) -0.0011(8)

_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
Ga1 O1 1.880(2) . ?
Ga1 O2 1.895(2) . ?
Ga1 O4 1.895(2) . ?
Ga1 O3 1.9005(19) . ?
P1 O1 1.533(2) . ?
P1 O2 1.534(2) 5 ?
P1 O3 1.537(2) 37_446 ?
P1 O4 1.539(2) 15_564 ?
O2 P1 1.534(2) 9 ?
O3 P1 1.537(2) 37_446 ?
O4 P1 1.539(2) 16_645 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ga1 O2 110.79(9) . . ?
O1 Ga1 O4 105.37(9) . . ?
O2 Ga1 O4 111.37(9) . . ?
O1 Ga1 O3 107.69(9) . . ?
O2 Ga1 O3 111.69(9) . . ?
O4 Ga1 O3 109.69(9) . . ?
O1 P1 O2 111.32(12) . 5 ?
O1 P1 O3 111.57(12) . 37_446 ?
O2 P1 O3 107.39(12) 5 37_446 ?
O1 P1 O4 105.92(11) . 15_564 ?
O2 P1 O4 110.66(11) 5 15_564 ?
O3 P1 O4 110.00(12) 37_446 15_564 ?
P1 O1 Ga1 131.10(13) . . ?
P1 O2 Ga1 124.66(12) 9 . ?
P1 O3 Ga1 125.39(13) 37_446 . ?
P1 O4 Ga1 122.76(12) 16_645 . ?

_refine_diff_density_max         0.322
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.064

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL 1 in I4(1)32
CELL 0.71073  17.94700  17.94700  17.94700  90.0000  90.0000  90.0000
ZERR   48.00   0.00020   0.00020   0.00020   0.0000   0.0000   0.0000
LATT -2
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SYMM 0.75+Y, 0.25+X, 0.25-Z
SYMM 0.75-Y, 0.75-X, 0.75-Z
SYMM 0.25+Y, 0.25-X, 0.75+Z
SYMM 0.25-Y, 0.75+X, 0.25+Z
SYMM 0.75+X, 0.25+Z, 0.25-Y
SYMM 0.25-X, 0.75+Z, 0.25+Y
SYMM 0.75-X, 0.75-Z, 0.75-Y
SYMM 0.25+X, 0.25-Z, 0.75+Y
SYMM 0.75+Z, 0.25+Y, 0.25-X
SYMM 0.25+Z, 0.25-Y, 0.75+X
SYMM 0.25-Z, 0.75+Y, 0.25+X
SYMM 0.75-Z, 0.75-Y, 0.75-X
SFAC O P GA ZN C N H
UNIT 192 48 21.12 26.88 44.8 26.88 152.32
TEMP 23.000

L.S. 5 0   16
ACTA
BOND
FMAP 2
PLAN 20

EADP GA1 ZN1
EXYZ GA1 ZN1
TWIN
WGHT    0.024300    5.615000
BASF   0.02688
FVAR       0.32673
GA1   3    0.741933    0.652411    0.888712    10.44000    0.00908    0.01569 =
         0.01063   -0.00094    0.00074    0.00177
ZN1   4    0.741933    0.652411    0.888712    10.56000    0.00908    0.01569 =
         0.01063   -0.00094    0.00074    0.00177
P1    2    0.847587    0.614790    0.756634    11.00000    0.01650    0.01014 =
         0.01037   -0.00033    0.00286    0.00107
O1    1    0.774110    0.607779    0.799587    11.00000    0.01715    0.02903 =
         0.01260   -0.00378    0.00255    0.00010
O2    1    0.696684    0.745867    0.869607    11.00000    0.00992    0.01781 =
         0.03326    0.00139    0.00051    0.00075
O3    1    0.826183    0.661967    0.952150    11.00000    0.01341    0.01994 =
         0.01994   -0.00134   -0.00405    0.00121
O4    1    0.673171    0.584282    0.930904    11.00000    0.01724    0.02382 =
         0.01168    0.00199    0.00443   -0.00106
HKLF 4

REM  1 in I4(1)32
REM R1 =  0.0155 for    1184 Fo > 4sig(Fo)  and  0.0160 for all    1207 data
REM     56 parameters refined using      0 restraints

END

WGHT      0.0243      5.6150

REM Highest difference peak  0.322,  deepest hole -0.312,  1-sigma level  0.064
Q1    1   0.7500  0.8750  1.0000  10.25000  0.05    0.32
Q2    1   0.6250  0.3750  0.8750  10.16667  0.05    0.27
Q3    1   0.8048  0.8821  0.9105  11.00000  0.05    0.25
Q4    1   0.6143  0.3857  0.8857  10.33333  0.05    0.24
Q5    1   0.8124  0.8203  0.8755  11.00000  0.05    0.23
Q6    1   0.6583  0.5944  0.9608  11.00000  0.05    0.21
Q7    1   0.8411  0.6954  0.9459  11.00000  0.05    0.21
Q8    1   0.8924  0.8065  0.8940  11.00000  0.05    0.20
Q9    1   0.6617  0.7456  0.8738  11.00000  0.05    0.20
Q10   1   0.8759  0.8074  0.9108  11.00000  0.05    0.19
Q11   1   0.7608  0.5683  0.7988  11.00000  0.05    0.18
Q12   1   0.7957  0.6352  0.9140  11.00000  0.05    0.18
Q13   1   0.6641  0.5612  0.6949  11.00000  0.05    0.17
Q14   1   0.6464  0.7127  0.9017  11.00000  0.05    0.17
Q15   1   0.7575  0.6322  0.8296  11.00000  0.05    0.17
Q16   1   0.6594  0.5704  0.9288  11.00000  0.05    0.17
Q17   1   0.7069  0.8166  0.8882  11.00000  0.05    0.17
Q18   1   0.8627  0.8006  0.9250  11.00000  0.05    0.17
Q19   1   0.7144  0.7808  0.8563  11.00000  0.05    0.16
Q20   1   0.6595  0.5702  0.7148  11.00000  0.05    0.15
;
_shelx_res_checksum              66894

# SQUEEZE RESULTS (Version =  30715)
# 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 -0.026 0.215 0.632 931 345 ' '
2 0.010 0.233 0.126 977 350 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The integral electron density in the voids is 695 electrons. The elctron density for N6C10H34 (protonated pentaethylenehexamine) calculated from the formula (N6C10H34)0.093(Zn0.56Ga0.44PO4) is 607 electrons.
;
####################################################################### 
# 
# 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_ZG-4N-L
_audit_block_doi                 10.5517/ccdc.csd.cc1pd508
_database_code_depnum_ccdc_archive 'CCDC 1560819'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ZG-4N-L
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C0.90 H3.30 Ga0.40 N0.60 O4 P Zn0.60'
_chemical_formula_weight         184.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           214
_space_group_name_H-M_alt        'I 41 3 2'
_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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'

_cell_length_a                   17.9925(6)
_cell_length_b                   17.9925(6)
_cell_length_c                   17.9925(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5824.7(6)
_cell_formula_units_Z            48
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    19721
_cell_measurement_theta_min      3.201
_cell_measurement_theta_max      28.292

_exptl_crystal_description       Cube
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.526
_exptl_crystal_F_000             4334
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.538
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8523
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            28114
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.601
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1214
_reflns_number_gt                1191
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.649
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Organic species, N4C6H22 (protonated triethylenetetramine) were disordered and could not be located on difference maps. Unassigned electron densities were removed by using SQUEEZE in PLATON software package. Since the atom numbers of Zn and Ga are too close, the occupancy of them could not be properly refined. The fixed occupancy factors were obtained from ICP-AES data.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0177P)²+3.1693P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.014(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1214
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0131
_refine_ls_R_factor_gt           0.0125
_refine_ls_wR_factor_ref         0.0362
_refine_ls_wR_factor_gt          0.0360
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_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
Ga1 Ga 0.24167(2) 0.34778(2) 0.88867(2) 0.01782(8) Uani 0.4 1 d . . P . .
Zn1 Zn 0.24167(2) 0.34778(2) 0.88867(2) 0.01782(8) Uani 0.6 1 d . . P . .
P1 P 0.34814(3) 0.38503(3) 0.75695(3) 0.01767(13) Uani 1 1 d . . . . .
O1 O 0.27483(10) 0.39158(11) 0.79981(9) 0.0281(4) Uani 1 1 d . . . . .
O2 O 0.19634(9) 0.25380(9) 0.87054(11) 0.0282(4) Uani 1 1 d . . . . .
O3 O 0.32644(9) 0.33774(10) 0.95187(10) 0.0263(4) Uani 1 1 d . . . . .
O4 O 0.17302(10) 0.41524(10) 0.93149(9) 0.0259(4) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.01459(13) 0.02271(15) 0.01617(14) 0.00076(9) 0.00103(9) -0.00309(9)
Zn1 0.01459(13) 0.02271(15) 0.01617(14) 0.00076(9) 0.00103(9) -0.00309(9)
P1 0.0241(3) 0.0155(3) 0.0134(2) -0.0004(2) 0.0038(2) -0.0015(2)
O1 0.0256(9) 0.0397(10) 0.0191(8) 0.0048(7) 0.0059(7) 0.0001(7)
O2 0.0163(7) 0.0224(8) 0.0458(11) -0.0019(8) -0.0002(7) -0.0014(6)
O3 0.0211(8) 0.0290(9) 0.0286(9) 0.0020(7) -0.0058(7) -0.0008(7)
O4 0.0265(9) 0.0328(9) 0.0184(8) -0.0033(7) 0.0055(7) 0.0011(7)

_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
Ga1 O1 1.8796(17) . ?
Ga1 O4 1.8954(17) . ?
Ga1 O2 1.9055(16) . ?
Ga1 O3 1.9111(16) . ?
P1 O2 1.5308(17) 6_456 ?
P1 O1 1.5325(17) . ?
P1 O3 1.5364(18) 14_556 ?
P1 O4 1.5390(17) 40_544 ?
O2 P1 1.5308(17) 12_565 ?
O3 P1 1.5365(18) 14_556 ?
O4 P1 1.5389(17) 39_454 ?

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 Ga1 O4 106.51(8) . . ?
O1 Ga1 O2 111.24(8) . . ?
O4 Ga1 O2 111.04(7) . . ?
O1 Ga1 O3 107.00(8) . . ?
O4 Ga1 O3 109.81(8) . . ?
O2 Ga1 O3 111.07(7) . . ?
O2 P1 O1 111.32(10) 6_456 . ?
O2 P1 O3 107.15(10) 6_456 14_556 ?
O1 P1 O3 111.64(10) . 14_556 ?
O2 P1 O4 110.77(10) 6_456 40_544 ?
O1 P1 O4 105.97(9) . 40_544 ?
O3 P1 O4 110.04(10) 14_556 40_544 ?
P1 O1 Ga1 131.99(11) . . ?
P1 O2 Ga1 124.51(10) 12_565 . ?
P1 O3 Ga1 125.17(11) 14_556 . ?
P1 O4 Ga1 123.21(11) 39_454 . ?

_refine_diff_density_max         0.251
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.047

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL 1 in I4(1)32
CELL 0.71073  17.99250  17.99250  17.99250  90.0000  90.0000  90.0000
ZERR   48.00   0.00060   0.00060   0.00060   0.0000   0.0000   0.0000
LATT -2
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SYMM 0.75+Y, 0.25+X, 0.25-Z
SYMM 0.75-Y, 0.75-X, 0.75-Z
SYMM 0.25+Y, 0.25-X, 0.75+Z
SYMM 0.25-Y, 0.75+X, 0.25+Z
SYMM 0.75+X, 0.25+Z, 0.25-Y
SYMM 0.25-X, 0.75+Z, 0.25+Y
SYMM 0.75-X, 0.75-Z, 0.75-Y
SYMM 0.25+X, 0.25-Z, 0.75+Y
SYMM 0.75+Z, 0.25+Y, 0.25-X
SYMM 0.25+Z, 0.25-Y, 0.75+X
SYMM 0.25-Z, 0.75+Y, 0.25+X
SYMM 0.75-Z, 0.75-Y, 0.75-X
SFAC O P GA ZN C N H
UNIT 192 48 19.2 28.8 43.2 28.8 158.4
TEMP 23.000

L.S. 5 0   15
ACTA
BOND
FMAP 2
PLAN 20
TWIN
EADP ZN1 GA1
EXYZ ZN1 GA1
WGHT    0.017700    3.169300
BASF   0.01380
FVAR       0.41669
GA1   3    0.241669    0.347784    0.888667    10.40000    0.01459    0.02271 =
         0.01617    0.00076    0.00103   -0.00309
ZN1   4    0.241669    0.347784    0.888667    10.60000    0.01459    0.02271 =
         0.01617    0.00076    0.00103   -0.00309
P1    2    0.348144    0.385031    0.756946    11.00000    0.02413    0.01550 =
         0.01338   -0.00038    0.00384   -0.00154
O1    1    0.274831    0.391579    0.799810    11.00000    0.02562    0.03971 =
         0.01906    0.00484    0.00588    0.00007
O2    1    0.196343    0.253803    0.870538    11.00000    0.01625    0.02243 =
         0.04584   -0.00186   -0.00023   -0.00144
O3    1    0.326442    0.337735    0.951867    11.00000    0.02113    0.02900 =
         0.02863    0.00200   -0.00584   -0.00084
O4    1    0.173017    0.415245    0.931488    11.00000    0.02646    0.03278 =
         0.01839   -0.00329    0.00550    0.00111
HKLF 4

REM  1 in I4(1)32
REM R1 =  0.0125 for    1191 Fo > 4sig(Fo)  and  0.0131 for all    1214 data
REM     56 parameters refined using      0 restraints

END

WGHT      0.0177      3.1693

REM Highest difference peak  0.251,  deepest hole -0.169,  1-sigma level  0.047
Q1    1   0.1590  0.2542  0.8693  11.00000  0.05    0.25
Q2    1   0.1590  0.4094  0.9664  11.00000  0.05    0.22
Q3    1   0.2883  0.3588  0.9171  11.00000  0.05    0.18
Q4    1   0.1708  0.2499  0.8969  11.00000  0.05    0.17
Q5    1   0.2961  0.3457  0.9003  11.00000  0.05    0.15
Q6    1   0.2652  0.3655  0.8373  11.00000  0.05    0.14
Q7    1   0.3750  0.2131  0.9631  10.50000  0.05    0.13
Q8    1   0.3750  0.1250  0.8750  10.16667  0.05    0.13
Q9    1   0.3073  0.3269  0.9011  11.00000  0.05    0.13
Q10   1   0.2200  0.2893  0.8972  11.00000  0.05    0.12
Q11   1   0.2075  0.2810  0.8500  11.00000  0.05    0.12
Q12   1   0.2853  0.3562  0.9358  11.00000  0.05    0.12
Q13   1   0.2098  0.2286  0.8639  11.00000  0.05    0.12
Q14   1   0.1968  0.3863  0.9188  11.00000  0.05    0.11
Q15   1   0.1250  0.4853  0.7353  10.50000  0.05    0.11
Q16   1   0.2977  0.3841  0.7957  11.00000  0.05    0.11
Q17   1   0.2696  0.3843  0.7756  11.00000  0.05    0.11
Q18   1   0.1731  0.5286  0.8477  11.00000  0.05    0.11
Q19   1   0.1944  0.4445  0.9253  11.00000  0.05    0.11
Q20   1   0.2560  0.2615  0.7826  11.00000  0.05    0.11
;
_shelx_res_checksum              90962

# SQUEEZE RESULTS (Version =  30715)
# 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 0.014 0.226 0.133 939 314 ' '
2 -0.020 0.224 0.624 995 341 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The integral electron density in the voids is 655 electrons. The elctron density for N4C6H22 (protonated triethylenetetramine) calculated from the formula (N4C6H22)0.15(Zn0.6Ga0.4PO4) is 619 electrons.
;
####################################################################### 
# 
# 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_ZG-6N-L
_audit_block_doi                 10.5517/ccdc.csd.cc1pd55f
_database_code_depnum_ccdc_archive 'CCDC 1560824'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ZG-6N-L
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C0.90 H3.06 Ga0.46 N0.54 O4 P Zn0.54'
_chemical_formula_weight         183.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           214
_space_group_name_H-M_alt        'I 41 3 2'
_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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'

_cell_length_a                   17.949(3)
_cell_length_b                   17.949(3)
_cell_length_c                   17.949(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5783(3)
_cell_formula_units_Z            48
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    22042
_cell_measurement_theta_min      3.208
_cell_measurement_theta_max      28.204

_exptl_crystal_description       Cube
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.533
_exptl_crystal_F_000             4306
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.614
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9053
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            28801
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.604
_diffrn_reflns_theta_max         28.209
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             1199
_reflns_number_gt                1183
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.652
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.997

_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       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Organic species, N6C10H34 (protonated pentaethylenehexamine) were disordered and could not be located on difference maps. Unassigned electron densities were removed by using SQUEEZE in PLATON software package. Since the atom numbers of Zn and Ga are too close, the occupancy of them could not be properly refined. The fixed occupancy factors were obtained from ICP-AES data.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0140P)²+4.3423P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.011(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1199
_refine_ls_number_parameters     57
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0118
_refine_ls_R_factor_gt           0.0115
_refine_ls_wR_factor_ref         0.0334
_refine_ls_wR_factor_gt          0.0333
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.125
_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
Ga1 Ga 0.25807(2) 0.34777(2) 0.11120(2) 0.01714(8) Uani 0.46 1 d . . P . .
Zn1 Zn 0.25807(2) 0.34777(2) 0.11120(2) 0.01714(8) Uani 0.54 1 d . . P . .
P1 P 0.15224(3) 0.38508(3) 0.24329(3) 0.01730(13) Uani 1 1 d . . . . .
O1 O 0.22561(9) 0.39152(10) 0.20040(9) 0.0281(4) Uani 1 1 d . . . . .
O2 O 0.30350(9) 0.25414(9) 0.12984(10) 0.0278(4) Uani 1 1 d . . . . .
O3 O 0.32691(9) 0.41551(9) 0.06870(9) 0.0250(3) Uani 1 1 d . . . . .
O4 O 0.17374(9) 0.33802(9) 0.04800(9) 0.0254(3) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.01412(12) 0.02157(14) 0.01573(13) -0.00062(9) 0.00128(9) 0.00244(8)
Zn1 0.01412(12) 0.02157(14) 0.01573(13) -0.00062(9) 0.00128(9) 0.00244(8)
P1 0.0225(3) 0.0154(3) 0.0140(2) 0.00004(19) 0.0039(2) 0.00152(19)
O1 0.0244(8) 0.0404(10) 0.0195(7) -0.0058(7) 0.0055(6) -0.0004(7)
O2 0.0156(7) 0.0224(8) 0.0455(10) 0.0016(8) -0.0001(7) 0.0011(6)
O3 0.0250(8) 0.0317(9) 0.0183(7) 0.0036(7) 0.0065(6) -0.0018(7)
O4 0.0205(8) 0.0269(8) 0.0290(9) -0.0009(7) -0.0064(7) 0.0010(6)

_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
Ga1 O1 1.8760(16) . ?
Ga1 O3 1.8939(17) . ?
Ga1 O2 1.8977(16) . ?
Ga1 O4 1.8997(16) . ?
P1 O1 1.5298(17) . ?
P1 O2 1.5308(16) 5 ?
P1 O3 1.5345(16) 39_454 ?
P1 O4 1.5360(17) 13_455 ?
O2 P1 1.5308(16) 9 ?
O3 P1 1.5344(16) 40_544 ?
O4 P1 1.5360(17) 13_455 ?

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 Ga1 O3 106.12(7) . . ?
O1 Ga1 O2 110.71(8) . . ?
O3 Ga1 O2 111.05(7) . . ?
O1 Ga1 O4 107.50(7) . . ?
O3 Ga1 O4 109.78(7) . . ?
O2 Ga1 O4 111.47(7) . . ?
O1 P1 O2 111.25(10) . 5 ?
O1 P1 O3 106.06(9) . 39_454 ?
O2 P1 O3 110.72(9) 5 39_454 ?
O1 P1 O4 111.66(10) . 13_455 ?
O2 P1 O4 107.24(10) 5 13_455 ?
O3 P1 O4 109.95(10) 39_454 13_455 ?
P1 O1 Ga1 131.69(11) . . ?
P1 O2 Ga1 124.75(10) 9 . ?
P1 O3 Ga1 123.08(10) 40_544 . ?
P1 O4 Ga1 125.38(10) 13_455 . ?

_refine_diff_density_max         0.233
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.044

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL 1 in I4(1)32
CELL 0.71073  17.94910  17.94910  17.94910  90.0000  90.0000  90.0000
ZERR   48.00   0.00270   0.00270   0.00270   0.0000   0.0000   0.0000
LATT -2
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SYMM 0.75+Y, 0.25+X, 0.25-Z
SYMM 0.75-Y, 0.75-X, 0.75-Z
SYMM 0.25+Y, 0.25-X, 0.75+Z
SYMM 0.25-Y, 0.75+X, 0.25+Z
SYMM 0.75+X, 0.25+Z, 0.25-Y
SYMM 0.25-X, 0.75+Z, 0.25+Y
SYMM 0.75-X, 0.75-Z, 0.75-Y
SYMM 0.25+X, 0.25-Z, 0.75+Y
SYMM 0.75+Z, 0.25+Y, 0.25-X
SYMM 0.25+Z, 0.25-Y, 0.75+X
SYMM 0.25-Z, 0.75+Y, 0.25+X
SYMM 0.75-Z, 0.75-Y, 0.75-X
SFAC O P GA ZN C N H
UNIT 192 48 22.08 25.92 43.2 25.92 146.88
TEMP 23.000

L.S. 5 0   14
ACTA
BOND
FMAP 2
PLAN 20
EADP ZN1 GA1
EXYZ ZN1 GA1
TWIN
WGHT    0.014000    4.342300
BASF   0.01067
FVAR       0.58491   0.62100
GA1   3    0.258073    0.347770    0.111203    10.46000    0.01412    0.02157 =
         0.01573   -0.00062    0.00128    0.00244
ZN1   4    0.258073    0.347770    0.111203    10.54000    0.01412    0.02157 =
         0.01573   -0.00062    0.00128    0.00244
P1    2    0.152238    0.385076    0.243286    11.00000    0.02251    0.01538 =
         0.01401    0.00004    0.00387    0.00152
O1    1    0.225613    0.391520    0.200403    11.00000    0.02435    0.04037 =
         0.01945   -0.00580    0.00549   -0.00045
O2    1    0.303505    0.254137    0.129840    11.00000    0.01556    0.02236 =
         0.04552    0.00163   -0.00015    0.00114
O3    1    0.326912    0.415507    0.068700    11.00000    0.02502    0.03173 =
         0.01827    0.00356    0.00646   -0.00184
O4    1    0.173740    0.338022    0.047997    11.00000    0.02046    0.02691 =
         0.02898   -0.00088   -0.00640    0.00103
HKLF 4

REM  1 in I4(1)32
REM R1 =  0.0115 for    1183 Fo > 4sig(Fo)  and  0.0118 for all    1199 data
REM     57 parameters refined using      0 restraints

END

WGHT      0.0140      4.3426

REM Highest difference peak  0.233,  deepest hole -0.168,  1-sigma level  0.044
Q1    1   0.3414  0.2564  0.1339  11.00000  0.05    0.23
Q2    1   0.3420  0.4057  0.0340  11.00000  0.05    0.21
Q3    1   0.2114  0.3599  0.0822  11.00000  0.05    0.17
Q4    1   0.2068  0.3655  0.0946  11.00000  0.05    0.16
Q5    1   0.2226  0.3570  0.0504  11.00000  0.05    0.14
Q6    1   0.3750  0.4066  0.1566  10.50000  0.05    0.14
Q7    1   0.2196  0.3796  0.2289  11.00000  0.05    0.12
Q8    1   0.1939  0.3850  0.2072  11.00000  0.05    0.12
Q9    1   0.3381  0.4282  0.0741  11.00000  0.05    0.12
Q10   1   0.3067  0.2986  0.1271  11.00000  0.05    0.12
Q11   1   0.2758  0.2996  0.0999  11.00000  0.05    0.11
Q12   1   0.2417  0.2992  0.0533  11.00000  0.05    0.11
Q13   1   0.2888  0.2334  0.1442  11.00000  0.05    0.11
Q14   1   0.2329  0.3658  0.1642  11.00000  0.05    0.11
Q15   1   0.2500  0.4519  0.0000  10.50000  0.05    0.11
Q16   1   0.1789  0.3486  0.0090  11.00000  0.05    0.11
Q17   1   0.2579  0.4385  0.0228  11.00000  0.05    0.11
Q18   1   0.3060  0.4431  0.0570  11.00000  0.05    0.10
Q19   1   0.3106  0.3845  0.0675  11.00000  0.05    0.10
Q20   1   0.2366  0.3815  0.2293  11.00000  0.05    0.10
;
_shelx_res_checksum              97510

# SQUEEZE RESULTS (Version =  30715)
# 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 0.015 0.225 0.133 930 271 ' '
2 -0.020 0.223 0.625 979 307 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The integral electron density in the voids is 578 electrons. The elctron density for N6C10H34 (protonated pentaethylenehexamine) calculated from the formula (N6C10H34)0.09(Zn0.54Ga0.46PO4) is 587 electrons.
;

