# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_datam_Compound_II
_audit_block_doi                 10.5517/cc5ct0b
_database_code_depnum_ccdc_archive 'CCDC 160301'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/b010001n 2001
_audit_update_record             
;
2001-03-13 deposited with the CCDC.	2023-03-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C H N O P Zn'
_chemical_formula_weight         139.37
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   5.2220(12)
_cell_length_b                   12.756(4)
_cell_length_c                   15.674(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1044.1(6)
_cell_formula_units_Z            10
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.217
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             670
_exptl_absorpt_coefficient_mu    6.067
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       ?
_diffrn_measurement_method       ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4365
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         23.25
_reflns_number_total             1491
_reflns_number_observed          1459
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
Refinement on F² for ALL reflections except for 1 with very negative F² 
or flagged by the user for potential systematic errors.  Weighted R-factors 
wR and all goodnesses of fit S are based on F², conventional R-factors R 
are based on F, with F set to zero for negative F². The observed criterion 
of F² > 2sigma(F²) is used only for calculating _R_factor_obs etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F² are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+0.9455P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(14)
_refine_ls_number_reflns         1490
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_obs          0.0221
_refine_ls_wR_factor_all         0.0572
_refine_ls_wR_factor_obs         0.0553
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_restrained_S_all      1.109
_refine_ls_restrained_S_obs      1.085
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zn1 Zn -0.11497(7) 1.12837(3) 0.54421(2) 0.01409(13) Uani 1 d . .
P1 P 0.1028(2) 0.91729(7) 0.63332(5) 0.0140(2) Uani 1 d . .
P2 P -0.1189(2) 1.37084(6) 0.56846(5) 0.0126(2) Uani 1 d . .
O1 O -0.0436(5) 1.0189(2) 0.6261(2) 0.0234(6) Uani 1 d . .
O2 O 0.0937(4) 1.1166(2) 0.44193(14) 0.0211(5) Uani 1 d . .
O3 O -0.4766(4) 1.1010(2) 0.51504(13) 0.0168(5) Uani 1 d . .
O4 O -0.0457(5) 1.2619(2) 0.60058(15) 0.0194(5) Uani 1 d . .
O5 O 0.2165(5) 0.9062(2) 0.72313(15) 0.0265(6) Uani 1 d . .
O6 O 0.3347(5) 0.9170(2) 0.56710(15) 0.0243(6) Uani 1 d . .
H30 H 0.4310(5) 0.9661(2) 0.57758(15) 0.037 Uiso 1 calc R .
O7 O -0.0565(4) 0.8217(2) 0.6083(2) 0.0226(6) Uani 1 d . .
O8 O -0.0231(5) 1.4525(2) 0.63672(15) 0.0186(5) Uani 1 d . .
H20 H -0.0950(5) 1.4415(2) 0.68235(15) 0.028 Uiso 1 calc R .
N1 N 0.2197(6) 0.6410(2) 0.5612(2) 0.0237(7) Uani 1 d . .
H3 H 0.2658(6) 0.6464(2) 0.5068(2) 0.036 Uiso 1 calc R .
H2 H 0.1113(6) 0.6925(2) 0.5742(2) 0.036 Uiso 1 calc R .
H1 H 0.1438(6) 0.5794(2) 0.5698(2) 0.036 Uiso 1 calc R .
N2 N 0.6576(6) 0.7833(3) 0.7624(2) 0.0275(7) Uani 1 d . .
H12 H 0.7841(6) 0.7988(3) 0.7982(2) 0.041 Uiso 1 calc R .
H11 H 0.5204(6) 0.8216(3) 0.7751(2) 0.041 Uiso 1 calc R .
H10 H 0.7067(6) 0.7971(3) 0.7092(2) 0.041 Uiso 1 calc R .
C1 C 0.4513(7) 0.6489(3) 0.6166(2) 0.0237(8) Uani 1 d . .
H4 H 0.5355(7) 0.7156(3) 0.6067(2) 0.028 Uiso 1 calc R .
H5 H 0.5706(7) 0.5935(3) 0.6019(2) 0.028 Uiso 1 calc R .
C2 C 0.3786(7) 0.6399(3) 0.7102(2) 0.0240(8) Uani 1 d . .
H6 H 0.2326(7) 0.6849(3) 0.7212(2) 0.029 Uiso 1 calc R .
H7 H 0.3268(7) 0.5683(3) 0.7219(2) 0.029 Uiso 1 calc R .
C3 C 0.5928(8) 0.6694(3) 0.7701(2) 0.0269(8) Uani 1 d . .
H9 H 0.5419(8) 0.6542(3) 0.8283(2) 0.032 Uiso 1 calc R .
H8 H 0.7432(8) 0.6277(3) 0.7571(2) 0.032 Uiso 1 calc R .

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
Zn1 0.0120(2) 0.0149(2) 0.0153(2) 0.0006(2) -0.00058(15) -0.0006(2)
P1 0.0144(4) 0.0149(4) 0.0126(4) 0.0022(3) 0.0014(4) 0.0004(4)
P2 0.0110(4) 0.0147(4) 0.0121(4) 0.0006(3) -0.0008(3) 0.0000(4)
O1 0.0256(14) 0.0233(12) 0.0212(13) 0.0066(11) 0.0049(12) 0.0049(11)
O2 0.0100(11) 0.0344(13) 0.0189(12) -0.0005(11) -0.0006(9) -0.0016(11)
O3 0.0129(12) 0.0242(13) 0.0134(11) 0.0041(10) -0.0026(9) -0.0041(10)
O4 0.0247(13) 0.0162(12) 0.0175(12) 0.0011(10) -0.0053(11) 0.0008(11)
O5 0.0286(14) 0.0328(14) 0.0182(12) 0.0008(12) -0.0039(11) 0.0107(12)
O6 0.0235(13) 0.0220(12) 0.0275(13) -0.0006(11) 0.0097(11) -0.0013(11)
O7 0.0192(14) 0.0213(12) 0.0274(13) -0.0015(11) -0.0002(11) -0.0024(11)
O8 0.0203(13) 0.0208(13) 0.0148(12) -0.0011(10) -0.0012(11) -0.0052(11)
N1 0.023(2) 0.024(2) 0.024(2) -0.0033(14) -0.0015(13) -0.0047(14)
N2 0.019(2) 0.039(2) 0.024(2) -0.0064(15) -0.0020(14) -0.0056(15)
C1 0.022(2) 0.026(2) 0.023(2) -0.001(2) -0.0032(14) -0.001(2)
C2 0.023(2) 0.024(2) 0.025(2) 0.0038(15) -0.002(2) -0.005(2)
C3 0.025(2) 0.033(2) 0.022(2) 0.007(2) -0.001(2) -0.001(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.933(2) . ?
Zn1 O2 1.944(2) . ?
Zn1 O4 1.953(2) . ?
Zn1 O3 1.974(2) . ?
P1 O1 1.510(3) . ?
P1 O7 1.527(3) . ?
P1 O5 1.534(2) . ?
P1 O6 1.595(2) . ?
P2 O2 1.518(2) 4_476 ?
P2 O4 1.526(2) . ?
P2 O3 1.547(2) 4_576 ?
P2 O8 1.575(2) . ?
O2 P2 1.518(2) 4_576 ?
O3 P2 1.547(2) 4_476 ?
O6 H30 0.82 . ?
O8 H20 0.82 . ?
N1 C1 1.492(5) . ?
N1 H3 0.89 . ?
N1 H2 0.89 . ?
N1 H1 0.89 . ?
N2 C3 1.496(5) . ?
N2 H12 0.89 . ?
N2 H11 0.89 . ?
N2 H10 0.89 . ?
C1 C2 1.520(5) . ?
C1 H4 0.97 . ?
C1 H5 0.97 . ?
C2 C3 1.508(5) . ?
C2 H6 0.97 . ?
C2 H7 0.97 . ?
C3 H9 0.97 . ?
C3 H8 0.97 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O2 112.58(10) . . ?
O1 Zn1 O4 107.09(11) . . ?
O2 Zn1 O4 109.67(10) . . ?
O1 Zn1 O3 102.16(10) . . ?
O2 Zn1 O3 109.37(9) . . ?
O4 Zn1 O3 115.85(10) . . ?
O1 P1 O7 112.98(14) . . ?
O1 P1 O5 110.11(15) . . ?
O7 P1 O5 111.89(15) . . ?
O1 P1 O6 109.75(14) . . ?
O7 P1 O6 104.17(13) . . ?
O5 P1 O6 107.65(15) . . ?
O2 P2 O4 112.27(14) 4_476 . ?
O2 P2 O3 111.09(13) 4_476 4_576 ?
O4 P2 O3 111.68(14) . 4_576 ?
O2 P2 O8 108.51(14) 4_476 . ?
O4 P2 O8 107.37(13) . . ?
O3 P2 O8 105.58(13) 4_576 . ?
P1 O1 Zn1 140.1(2) . . ?
P2 O2 Zn1 129.39(14) 4_576 . ?
P2 O3 Zn1 127.93(13) 4_476 . ?
P2 O4 Zn1 126.76(14) . . ?
P1 O6 H30 109.47(10) . . ?
P2 O8 H20 109.47(9) . . ?
C1 N1 H3 109.5(2) . . ?
C1 N1 H2 109.5(2) . . ?
H3 N1 H2 109.5 . . ?
C1 N1 H1 109.5(2) . . ?
H3 N1 H1 109.5 . . ?
H2 N1 H1 109.5 . . ?
C3 N2 H12 109.5(2) . . ?
C3 N2 H11 109.5(2) . . ?
H12 N2 H11 109.5 . . ?
C3 N2 H10 109.5(2) . . ?
H12 N2 H10 109.5 . . ?
H11 N2 H10 109.5 . . ?
N1 C1 C2 110.7(3) . . ?
N1 C1 H4 109.5(2) . . ?
C2 C1 H4 109.5(2) . . ?
N1 C1 H5 109.5(2) . . ?
C2 C1 H5 109.5(2) . . ?
H4 C1 H5 108.1 . . ?
C3 C2 C1 113.4(3) . . ?
C3 C2 H6 108.9(2) . . ?
C1 C2 H6 108.9(2) . . ?
C3 C2 H7 108.9(2) . . ?
C1 C2 H7 108.9(2) . . ?
H6 C2 H7 107.7 . . ?
N2 C3 C2 111.1(3) . . ?
N2 C3 H9 109.4(2) . . ?
C2 C3 H9 109.4(2) . . ?
N2 C3 H8 109.4(2) . . ?
C2 C3 H8 109.4(2) . . ?
H9 C3 H8 108.0 . . ?

_refine_diff_density_max         0.370
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.175
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC) in cooperation with FIZ Karlsruhe.
# 
# Please note that these data are only for research purposes or private use.
# For detailed information please see under Terms & Conditions.
# Full information about CCDC and FIZ Karlsruhe 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 FIZ Karlsruhe. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_160301-ICSD
_database_code_depnum_ccdc_archive 'CCDC 1676719'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.jssc.2007.10.021 2007
_audit_update_record             
;
2018-02-27 deposited with the CCDC.	2023-03-20 downloaded from the CCDC.
;
_database_code_ICSD              160301
_chemical_name_systematic        'Strontium Dialuminate - Ht'
_chemical_formula_sum            'Al2 O4 Sr1'
_cell_length_a                   5.1765
_cell_length_b                   5.1765
_cell_length_c                   8.5758
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     199.01
_cell_formula_units_Z            2
_symmetry_space_group_name_H-M   'P 63 2 2'
_symmetry_Int_Tables_number      182
_symmetry_cell_setting           hexagonal
_refine_ls_R_factor_all          0.0238
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 'x, x-y, -z+1/2'
2 '-x+y, y, -z+1/2'
3 '-y, -x, -z+1/2'
4 'x-y, x, z+1/2'
5 'y, -x+y, z+1/2'
6 '-x, -y, z+1/2'
7 '-x, -x+y, -z'
8 'x-y, -y, -z'
9 'y, x, -z'
10 '-x+y, -x, z'
11 '-y, x-y, z'
12 'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Sr1 Sr2+ 0 0 0.25
Al1 Al3+ 0.3333 0.6667 0.9451
O1 O2- 0.6057 0.2114 0.25
O2 O2- 0.3591 0 0

#End of data_160301-ICSD


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC) in cooperation with FIZ Karlsruhe.
# 
# Please note that these data are only for research purposes or private use.
# For detailed information please see under Terms & Conditions.
# Full information about CCDC and FIZ Karlsruhe 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 FIZ Karlsruhe. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_151538-ICSD
_database_code_depnum_ccdc_archive 'CCDC 1668367'
loop_
_citation_id
_citation_doi
_citation_year
1 10.4028/www.scientific.net/MSF.443-444.263 2004
_audit_update_record             
;
2018-02-27 deposited with the CCDC.	2023-03-20 downloaded from the CCDC.
;
_database_code_ICSD              151538
_chemical_name_systematic        'Thulium Magnesium (5/24)'
_chemical_formula_sum            'Mg24 Tm5'
_cell_length_a                   11.215
_cell_length_b                   11.215
_cell_length_c                   11.215
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1410.58
_cell_formula_units_Z            2
_symmetry_space_group_name_H-M   'I -4 3 m'
_symmetry_Int_Tables_number      217
_symmetry_cell_setting           cubic
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 '-z, -y, x'
2 '-y, -x, z'
3 '-x, -z, y'
4 '-z, -x, y'
5 '-y, -z, x'
6 '-x, -y, z'
7 '-z, y, -x'
8 '-y, x, -z'
9 '-x, z, -y'
10 '-z, x, -y'
11 '-y, z, -x'
12 '-x, y, -z'
13 'z, -y, -x'
14 'y, -x, -z'
15 'x, -z, -y'
16 'z, -x, -y'
17 'y, -z, -x'
18 'x, -y, -z'
19 'z, y, x'
20 'y, x, z'
21 'x, z, y'
22 'z, x, y'
23 'y, z, x'
24 'x, y, z'
25 '-z+1/2, -y+1/2, x+1/2'
26 '-y+1/2, -x+1/2, z+1/2'
27 '-x+1/2, -z+1/2, y+1/2'
28 '-z+1/2, -x+1/2, y+1/2'
29 '-y+1/2, -z+1/2, x+1/2'
30 '-x+1/2, -y+1/2, z+1/2'
31 '-z+1/2, y+1/2, -x+1/2'
32 '-y+1/2, x+1/2, -z+1/2'
33 '-x+1/2, z+1/2, -y+1/2'
34 '-z+1/2, x+1/2, -y+1/2'
35 '-y+1/2, z+1/2, -x+1/2'
36 '-x+1/2, y+1/2, -z+1/2'
37 'z+1/2, -y+1/2, -x+1/2'
38 'y+1/2, -x+1/2, -z+1/2'
39 'x+1/2, -z+1/2, -y+1/2'
40 'z+1/2, -x+1/2, -y+1/2'
41 'y+1/2, -z+1/2, -x+1/2'
42 'x+1/2, -y+1/2, -z+1/2'
43 'z+1/2, y+1/2, x+1/2'
44 'y+1/2, x+1/2, z+1/2'
45 'x+1/2, z+1/2, y+1/2'
46 'z+1/2, x+1/2, y+1/2'
47 'y+1/2, z+1/2, x+1/2'
48 'x+1/2, y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Tm1 Tm0+ 0 0 0
Tm2 Tm0+ 0.3152 0.3152 0.3152
Mg1 Mg0+ 0.3568 0.3568 0.0342
Mg2 Mg0+ 0.0915 0.0915 0.2778

#End of data_151538-ICSD


####################################################################### 
# 
# 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_compoundI
_audit_block_doi                 10.5517/cc52pb7
_database_code_depnum_ccdc_archive 'CCDC 151538'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/ic000366c 2000
2 10.1039/b010001n 2001
_audit_update_record             
;
2000-10-24 deposited with the CCDC.	2023-03-20 downloaded from the CCDC.
;
_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C3 H13 N2 O8 P2 Zn'
_chemical_formula_weight         332.46
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   5.2677(5)
_cell_length_b                   13.3025(13)
_cell_length_c                   14.7833(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.0490(10)
_cell_angle_gamma                90.00
_cell_volume                     1030.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    571(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      571(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4104
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         23.26
_reflns_number_total             1463
_reflns_number_observed          1291
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       'Siemens XSCANS'
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'

_refine_special_details          
; 
Refinement on F² for ALL reflections except for 0 with very negative F² 
or flagged by the user for potential systematic errors.  Weighted R-factors 
wR and all goodnesses of fit S are based on F², conventional R-factors R 
are based on F, with F set to zero for negative F². The observed criterion 
of F² > 2sigma(F²) is used only for calculating _R_factor_obs etc. and
is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F² are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.7829P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1463
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_obs          0.0290
_refine_ls_wR_factor_all         0.0916
_refine_ls_wR_factor_obs         0.0783
_refine_ls_goodness_of_fit_all   1.127
_refine_ls_goodness_of_fit_obs   1.033
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.033
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zn1 Zn 0.25553(9) 0.98159(4) 0.11203(3) 0.0167(2) Uani 1 d . .
P1 P 0.5196(2) 0.93323(8) 0.30328(7) 0.0169(3) Uani 1 d . .
P2 P 0.2485(2) 0.89066(8) -0.08934(7) 0.0156(3) Uani 1 d . .
O1 O 0.2075(7) 0.8919(2) 0.0105(2) 0.0276(8) Uani 1 d . .
O2 O 0.4765(6) 1.0961(2) 0.1066(2) 0.0270(8) Uani 1 d . .
O3 O 0.3911(6) 0.8941(2) 0.2127(2) 0.0232(7) Uani 1 d . .
O4 O -0.0724(6) 1.0347(2) 0.1439(2) 0.0234(7) Uani 1 d . .
O5 O 0.4290(7) 1.0365(2) 0.3272(2) 0.0286(8) Uani 1 d . .
O6 O 0.4975(6) 0.8574(2) 0.3787(2) 0.0243(7) Uani 1 d . .
O7 O 0.8170(6) 0.9381(3) 0.2944(2) 0.0273(8) Uani 1 d . .
H20 H 0.8439(6) 0.9781(3) 0.2543(2) 0.041 Uiso 1 calc R .
O8 O 0.1610(6) 0.7842(2) -0.1278(2) 0.0247(8) Uani 1 d . .
H30 H 0.2507(6) 0.7405(2) -0.1014(2) 0.037 Uiso 1 calc R .
N1 N 0.7463(8) 0.7849(3) 0.7276(3) 0.0285(10) Uani 1 d . .
H1 H 0.8185(8) 0.7792(3) 0.7846(3) 0.043 Uiso 1 calc R .
H2 H 0.6321(8) 0.7361(3) 0.7160(3) 0.043 Uiso 1 calc R .
H3 H 0.6690(8) 0.8443(3) 0.7205(3) 0.043 Uiso 1 calc R .
N2 N 0.8019(8) 0.8912(3) 0.5333(3) 0.0286(10) Uani 1 d . .
H10 H 0.6874(8) 0.8897(3) 0.4836(3) 0.034 Uiso 1 calc R .
H11 H 0.7319(8) 0.9265(3) 0.5763(3) 0.034 Uiso 1 calc R .
C3 C 1.0315(9) 0.9456(4) 0.5101(3) 0.0308(12) Uani 1 d . .
H9 H 1.0943(9) 0.9146(4) 0.4573(3) 0.037 Uiso 1 calc R .
H8 H 1.1647(9) 0.9412(4) 0.5605(3) 0.037 Uiso 1 calc R .
C1 C 0.9451(12) 0.7769(5) 0.6641(4) 0.0466(15) Uani 1 d . .
H4 H 1.0312(12) 0.7127(5) 0.6737(4) 0.056 Uiso 1 calc R .
H5 H 1.0709(12) 0.8293(5) 0.6785(4) 0.056 Uiso 1 calc R .
C2 C 0.8450(13) 0.7855(4) 0.5669(4) 0.047(2) Uani 1 d . .
H6 H 0.6847(13) 0.7493(4) 0.5573(4) 0.057 Uiso 1 calc R .
H7 H 0.9641(13) 0.7530(4) 0.5305(4) 0.057 Uiso 1 calc R .

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
Zn1 0.0174(3) 0.0182(3) 0.0148(3) -0.0003(2) 0.0027(2) 0.0000(2)
P1 0.0223(7) 0.0153(6) 0.0134(6) 0.0004(5) 0.0033(5) 0.0006(5)
P2 0.0164(6) 0.0156(6) 0.0152(6) -0.0007(5) 0.0031(5) -0.0008(5)
O1 0.046(2) 0.023(2) 0.015(2) -0.0023(13) 0.0070(15) -0.006(2)
O2 0.019(2) 0.023(2) 0.040(2) 0.0035(15) 0.0063(15) 0.0007(14)
O3 0.031(2) 0.022(2) 0.015(2) 0.0008(13) -0.0030(14) -0.0013(14)
O4 0.020(2) 0.028(2) 0.023(2) 0.0064(14) 0.0082(14) 0.0057(14)
O5 0.043(2) 0.022(2) 0.022(2) -0.0002(14) 0.010(2) 0.008(2)
O6 0.033(2) 0.021(2) 0.019(2) 0.0061(13) 0.0023(14) -0.0043(14)
O7 0.025(2) 0.037(2) 0.020(2) 0.0054(15) 0.0048(14) 0.000(2)
O8 0.023(2) 0.021(2) 0.029(2) -0.0066(14) 0.0002(14) -0.0009(14)
N1 0.039(3) 0.021(2) 0.025(2) 0.003(2) 0.003(2) 0.001(2)
N2 0.039(3) 0.034(2) 0.014(2) -0.002(2) 0.005(2) 0.010(2)
C3 0.026(3) 0.044(3) 0.022(3) -0.009(2) 0.000(2) 0.007(2)
C1 0.056(4) 0.042(4) 0.042(3) 0.006(3) 0.009(3) 0.011(3)
C2 0.075(5) 0.031(3) 0.039(3) 0.000(3) 0.014(3) 0.015(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.913(3) . ?
Zn1 O2 1.924(3) . ?
Zn1 O3 1.964(3) . ?
Zn1 O4 1.969(3) . ?
P1 O5 1.509(3) . ?
P1 O6 1.517(3) . ?
P1 O3 1.527(3) . ?
P1 O7 1.587(3) . ?
P2 O2 1.508(3) 3_675 ?
P2 O1 1.515(3) . ?
P2 O4 1.530(3) 3_575 ?
P2 O8 1.577(3) . ?
O2 P2 1.508(3) 3_675 ?
O4 P2 1.530(3) 3_575 ?
O7 H20 0.82 . ?
O8 H30 0.82 . ?
N1 C1 1.482(7) . ?
N1 H1 0.89 . ?
N1 H2 0.89 . ?
N1 H3 0.89 . ?
N2 C3 1.480(6) . ?
N2 C2 1.501(7) . ?
N2 H10 0.90 . ?
N2 H11 0.90 . ?
C3 C3 1.508(10) 3_776 ?
C3 H9 0.97 . ?
C3 H8 0.97 . ?
C1 C2 1.483(8) . ?
C1 H4 0.97 . ?
C1 H5 0.97 . ?
C2 H6 0.97 . ?
C2 H7 0.97 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O2 119.45(14) . . ?
O1 Zn1 O3 103.42(13) . . ?
O2 Zn1 O3 109.14(13) . . ?
O1 Zn1 O4 111.40(14) . . ?
O2 Zn1 O4 106.01(13) . . ?
O3 Zn1 O4 106.81(12) . . ?
O5 P1 O6 112.5(2) . . ?
O5 P1 O3 113.2(2) . . ?
O6 P1 O3 110.9(2) . . ?
O5 P1 O7 108.8(2) . . ?
O6 P1 O7 103.9(2) . . ?
O3 P1 O7 107.0(2) . . ?
O2 P2 O1 113.7(2) 3_675 . ?
O2 P2 O4 112.0(2) 3_675 3_575 ?
O1 P2 O4 111.5(2) . 3_575 ?
O2 P2 O8 107.1(2) 3_675 . ?
O1 P2 O8 107.1(2) . . ?
O4 P2 O8 104.8(2) 3_575 . ?
P2 O1 Zn1 138.6(2) . . ?
P2 O2 Zn1 134.1(2) 3_675 . ?
P1 O3 Zn1 123.7(2) . . ?
P2 O4 Zn1 127.2(2) 3_575 . ?
P1 O7 H20 109.47(12) . . ?
P2 O8 H30 109.47(12) . . ?
C1 N1 H1 109.5(3) . . ?
C1 N1 H2 109.5(3) . . ?
H1 N1 H2 109.5 . . ?
C1 N1 H3 109.5(3) . . ?
H1 N1 H3 109.5 . . ?
H2 N1 H3 109.5 . . ?
C3 N2 C2 115.8(4) . . ?
C3 N2 H10 108.3(2) . . ?
C2 N2 H10 108.3(3) . . ?
C3 N2 H11 108.3(2) . . ?
C2 N2 H11 108.3(3) . . ?
H10 N2 H11 107.4 . . ?
N2 C3 C3 110.3(5) . 3_776 ?
N2 C3 H9 109.6(2) . . ?
C3 C3 H9 109.6(4) 3_776 . ?
N2 C3 H8 109.6(2) . . ?
C3 C3 H8 109.6(4) 3_776 . ?
H9 C3 H8 108.1 . . ?
N1 C1 C2 113.9(5) . . ?
N1 C1 H4 108.8(3) . . ?
C2 C1 H4 108.8(3) . . ?
N1 C1 H5 108.8(3) . . ?
C2 C1 H5 108.8(3) . . ?
H4 C1 H5 107.7 . . ?
C1 C2 N2 114.8(5) . . ?
C1 C2 H6 108.6(4) . . ?
N2 C2 H6 108.6(3) . . ?
C1 C2 H7 108.6(3) . . ?
N2 C2 H7 108.6(3) . . ?
H6 C2 H7 107.5 . . ?

_refine_diff_density_max         0.877
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.153
