# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_mono
_audit_block_doi                 10.5517/ccdc.csd.cc26ry0y
_database_code_depnum_ccdc_archive 'CCDC 2048790'
loop_
_audit_author_name
_audit_author_address
'Yang Zou'
;nanjing tech univ
China
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_audit_creation_date             2019-10-25
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H6 O16 P4 Zn2, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H30 N2 O16 P4 Zn2'
_chemical_formula_weight         664.96
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   8.4561(8)
_cell_length_b                   13.7954(14)
_cell_length_c                   10.1880(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.872(3)
_cell_angle_gamma                90
_cell_volume                     1188.3(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.49
_shelx_estimated_absorpt_T_max   0.834
_shelx_estimated_absorpt_T_min   0.650
_exptl_absorpt_coefficient_mu    2.361
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1448 before and 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.6057.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10899
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         1.476
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4097
_reflns_number_total             4215
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.86(2)
_refine_ls_extinction_coef       0.040(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4215
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0468
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0545P)²+5.3826P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1206
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.14(2)
 0.86(2)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
3.b Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4), O7(H7), O11(H11), O14(H14), O16(H16)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn -0.48941(10) -0.13092(6) -0.80912(9) 0.0175(3) Uani 1 1 d . . . . .
Zn2 Zn 0.01217(11) -0.42634(6) -0.69834(9) 0.0184(3) Uani 1 1 d . . . . .
P1 P -0.5188(3) -0.03725(16) -0.5182(2) 0.0224(5) Uani 1 1 d . . . . .
P2 P -0.1770(3) -0.22694(17) -0.7165(2) 0.0230(5) Uani 1 1 d . . . . .
P3 P -0.6767(3) -0.30620(16) -0.6876(2) 0.0223(5) Uani 1 1 d . . . . .
P4 P -0.0146(3) -0.61332(15) -0.8842(2) 0.0215(5) Uani 1 1 d . . . . .
O1 O -0.5415(10) 0.0646(5) -0.4695(7) 0.0316(16) Uani 1 1 d . . . . .
O2 O -0.6485(11) -0.0993(7) -0.4558(8) 0.047(2) Uani 1 1 d . . . . .
H2 H -0.676297 -0.141851 -0.507373 0.070 Uiso 1 1 calc GR . . . .
O3 O -0.5263(9) -0.0443(5) -0.6654(6) 0.0317(16) Uani 1 1 d . . . . .
O4 O -0.3555(11) -0.0759(7) -0.4634(8) 0.049(2) Uani 1 1 d . . . . .
H4 H -0.320016 -0.116252 -0.514234 0.073 Uiso 1 1 calc GR . . . .
O5 O -0.2703(8) -0.1734(5) -0.8215(7) 0.0350(17) Uani 1 1 d . . . . .
O6 O -0.1251(9) -0.3256(5) -0.7661(7) 0.0342(16) Uani 1 1 d . . . . .
O7 O -0.0263(8) -0.1600(5) -0.6874(9) 0.0351(17) Uani 1 1 d . . . . .
H7 H 0.041388 -0.191603 -0.647851 0.053 Uiso 1 1 calc GR . . . .
O8 O -0.2711(8) -0.2358(5) -0.5892(7) 0.0253(13) Uani 1 1 d . . . . .
O9 O -0.0305(10) -0.5549(5) -0.7607(7) 0.0320(16) Uani 1 1 d . . . . .
O10 O -0.0234(11) -0.5573(5) -1.0107(7) 0.0378(18) Uani 1 1 d . . . . .
O11 O -0.1482(11) -0.6908(6) -0.8790(7) 0.045(2) Uani 1 1 d . . . . .
H11 H -0.196425 -0.691751 -0.949423 0.067 Uiso 1 1 calc GR . . . .
O12 O 0.1447(10) -0.6710(6) -0.8720(7) 0.043(2) Uani 1 1 d . . . . .
O13 O -0.6218(9) -0.2448(5) -0.7992(6) 0.0301(15) Uani 1 1 d . . . . .
O14 O -0.7715(8) -0.2453(5) -0.5898(7) 0.0261(13) Uani 1 1 d . . . . .
H14 H -0.772048 -0.272617 -0.518358 0.039 Uiso 1 1 calc GR . . . .
O15 O -0.7700(8) -0.3940(5) -0.7317(8) 0.0310(15) Uani 1 1 d . . . . .
O16 O -0.5267(9) -0.3472(5) -0.6072(8) 0.0359(17) Uani 1 1 d . . . . .
H16 H -0.446310 -0.320197 -0.632368 0.054 Uiso 1 1 calc GR . . . .
N1 N -0.9942(11) -0.1130(6) -0.1012(8) 0.0286(18) Uani 1 1 d . . . . .
C1 C -1.1538(16) -0.0986(12) -0.1653(16) 0.059(4) Uani 1 1 d . . . . .
H1A H -1.223440 -0.067870 -0.104480 0.089 Uiso 1 1 calc GR . . . .
H1B H -1.196725 -0.160367 -0.190736 0.089 Uiso 1 1 calc GR . . . .
H1C H -1.143156 -0.058445 -0.241578 0.089 Uiso 1 1 calc GR . . . .
C2 C -0.9826(15) -0.0458(9) 0.0162(11) 0.040(3) Uani 1 1 d . . . . .
H2A H -0.989133 0.020251 -0.012977 0.061 Uiso 1 1 calc GR . . . .
H2B H -0.883432 -0.056009 0.061291 0.061 Uiso 1 1 calc GR . . . .
H2C H -1.067794 -0.059083 0.074774 0.061 Uiso 1 1 calc GR . . . .
C3 C -0.8708(18) -0.0917(10) -0.1959(13) 0.052(3) Uani 1 1 d . . . . .
H3A H -0.891986 -0.126600 -0.275775 0.078 Uiso 1 1 calc GR . . . .
H3B H -0.769961 -0.111152 -0.160286 0.078 Uiso 1 1 calc GR . . . .
H3C H -0.869527 -0.023405 -0.213814 0.078 Uiso 1 1 calc GR . . . .
C4 C -0.9801(19) -0.2142(9) -0.0541(13) 0.053(4) Uani 1 1 d . . . . .
H4A H -1.068665 -0.229427 0.000050 0.080 Uiso 1 1 calc GR . . . .
H4B H -0.883874 -0.221358 -0.003858 0.080 Uiso 1 1 calc GR . . . .
H4C H -0.978732 -0.257377 -0.127944 0.080 Uiso 1 1 calc GR . . . .
N2 N -0.4949(12) -0.6215(6) -0.6372(9) 0.035(2) Uani 1 1 d . . . . .
C5 C -0.6409(17) -0.5934(10) -0.5683(14) 0.052(3) Uani 1 1 d . . . . .
H5A H -0.653584 -0.633922 -0.492529 0.078 Uiso 1 1 calc GR . . . .
H5B H -0.730406 -0.601271 -0.626382 0.078 Uiso 1 1 calc GR . . . .
H5C H -0.633243 -0.526920 -0.541255 0.078 Uiso 1 1 calc GR . . . .
C6 C -0.3524(19) -0.5981(15) -0.5514(19) 0.075(5) Uani 1 1 d . . . . .
H6A H -0.338628 -0.529080 -0.547121 0.112 Uiso 1 1 calc GR . . . .
H6B H -0.259847 -0.627227 -0.587844 0.112 Uiso 1 1 calc GR . . . .
H6C H -0.368447 -0.623068 -0.464626 0.112 Uiso 1 1 calc GR . . . .
C7 C -0.4839(17) -0.5661(9) -0.7615(13) 0.049(3) Uani 1 1 d . . . . .
H7A H -0.583035 -0.569620 -0.808359 0.073 Uiso 1 1 calc GR . . . .
H7B H -0.401969 -0.593296 -0.814369 0.073 Uiso 1 1 calc GR . . . .
H7C H -0.459448 -0.499655 -0.742128 0.073 Uiso 1 1 calc GR . . . .
C8 C -0.507(2) -0.7261(9) -0.6725(19) 0.072(5) Uani 1 1 d . . . . .
H8A H -0.494338 -0.764831 -0.594884 0.109 Uiso 1 1 calc GR . . . .
H8B H -0.426511 -0.742224 -0.733926 0.109 Uiso 1 1 calc GR . . . .
H8C H -0.609428 -0.738506 -0.711592 0.109 Uiso 1 1 calc GR . . . .


_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 1.918(7) 2_554 ?
Zn1 O3 1.919(6) . ?
Zn1 O5 1.949(7) . ?
Zn1 O13 1.933(7) . ?
Zn2 O6 1.932(7) . ?
Zn2 O9 1.916(6) . ?
Zn2 O10 1.953(7) 2_545 ?
Zn2 O15 1.931(7) 1_655 ?
P1 O1 1.503(7) . ?
P1 O2 1.536(8) . ?
P1 O3 1.503(7) . ?
P1 O4 1.575(9) . ?
P2 O5 1.512(7) . ?
P2 O6 1.519(7) . ?
P2 O7 1.597(8) . ?
P2 O8 1.538(7) . ?
P3 O13 1.497(7) . ?
P3 O14 1.539(7) . ?
P3 O15 1.510(7) . ?
P3 O16 1.602(8) . ?
P4 O9 1.502(7) . ?
P4 O10 1.504(7) . ?
P4 O11 1.557(8) . ?
P4 O12 1.567(8) . ?
N1 C1 1.504(16) . ?
N1 C2 1.515(13) . ?
N1 C3 1.462(14) . ?
N1 C4 1.480(14) . ?
N2 C5 1.481(16) . ?
N2 C6 1.513(19) . ?
N2 C7 1.483(15) . ?
N2 C8 1.490(17) . ?

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 O3 108.4(3) 2_554 . ?
O1 Zn1 O5 107.1(3) 2_554 . ?
O1 Zn1 O13 107.8(3) 2_554 . ?
O3 Zn1 O5 113.7(3) . . ?
O3 Zn1 O13 111.4(3) . . ?
O13 Zn1 O5 108.1(3) . . ?
O6 Zn2 O10 109.4(3) . 2_545 ?
O9 Zn2 O6 116.0(3) . . ?
O9 Zn2 O10 100.8(3) . 2_545 ?
O9 Zn2 O15 109.3(3) . 1_655 ?
O15 Zn2 O6 109.9(3) 1_655 . ?
O15 Zn2 O10 111.1(4) 1_655 2_545 ?
O1 P1 O2 106.8(5) . . ?
O1 P1 O3 112.7(4) . . ?
O1 P1 O4 108.4(5) . . ?
O2 P1 O4 107.0(6) . . ?
O3 P1 O2 110.9(5) . . ?
O3 P1 O4 110.8(5) . . ?
O5 P2 O6 110.7(4) . . ?
O5 P2 O7 104.8(4) . . ?
O5 P2 O8 111.4(4) . . ?
O6 P2 O7 110.3(4) . . ?
O6 P2 O8 111.4(4) . . ?
O8 P2 O7 108.1(4) . . ?
O13 P3 O14 110.7(4) . . ?
O13 P3 O15 113.2(4) . . ?
O13 P3 O16 109.6(4) . . ?
O14 P3 O16 106.1(4) . . ?
O15 P3 O14 110.9(4) . . ?
O15 P3 O16 105.9(4) . . ?
O9 P4 O10 116.0(4) . . ?
O9 P4 O11 105.4(4) . . ?
O9 P4 O12 107.1(4) . . ?
O10 P4 O11 110.8(5) . . ?
O10 P4 O12 111.1(5) . . ?
O11 P4 O12 105.8(5) . . ?
P1 O1 Zn1 134.3(5) . 2 ?
P1 O3 Zn1 142.8(5) . . ?
P2 O5 Zn1 126.0(4) . . ?
P2 O6 Zn2 134.5(5) . . ?
P4 O9 Zn2 139.1(4) . . ?
P4 O10 Zn2 140.6(5) . 2_544 ?
P3 O13 Zn1 133.3(4) . . ?
P3 O15 Zn2 128.9(4) . 1_455 ?
C1 N1 C2 108.0(9) . . ?
C3 N1 C1 109.4(11) . . ?
C3 N1 C2 111.1(9) . . ?
C3 N1 C4 110.4(10) . . ?
C4 N1 C1 109.4(11) . . ?
C4 N1 C2 108.5(9) . . ?
C5 N2 C6 109.4(12) . . ?
C5 N2 C7 109.5(10) . . ?
C5 N2 C8 108.1(11) . . ?
C7 N2 C6 108.9(11) . . ?
C7 N2 C8 107.3(10) . . ?
C8 N2 C6 113.6(13) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.14(2)
2 0.86(2)

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

data_1
_audit_block_doi                 10.5517/ccdc.csd.cc26ry1z
_database_code_depnum_ccdc_archive 'CCDC 2048791'
loop_
_audit_author_name
_audit_author_address
'Yang Zou'
;nanjing tech univ
China
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_audit_creation_date             2019-10-25
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(H24 O64 P16 Zn8), 2(C4 H7.98 N)'
_chemical_formula_sum            'C8 H22 N2 O16 P4 Zn2'
_chemical_formula_weight         656.89
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   15.987(14)
_cell_length_b                   9.949(8)
_cell_length_c                   15.258(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2427(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2633
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      27.661
_cell_measurement_theta_min      4.685
_shelx_estimated_absorpt_T_max   0.893
_shelx_estimated_absorpt_T_min   0.769
_exptl_absorpt_coefficient_mu    2.312
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1416 before and 0.0782 after correction.
The Ratio of minimum to maximum transmission is 0.6491.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5234
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.640
_diffrn_reflns_theta_min         5.101
_diffrn_ambient_temperature      301.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                1217
_reflns_number_total             1255
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.25(2)
_refine_ls_extinction_coef       0.019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1255
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0309
_refine_ls_restrained_S_all      1.185
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0566P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0896
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.75(2)
 0.25(2)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Others
 Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(H1'C)=Sof(C2')=Sof(H2'A)=Sof(H2'B)=Sof(H2'C)=
 1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(1)
 Fixed Sof: H4(0.5)
4.a Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C1'(H1'A,H1'B,H1'C), C2'(H2'A,H2'B,H2'C)
4.b Tetrahedral OH refined with riding coordinates:
 O3(H3), O4(H4)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.000000 0.500000 0.09211(3) 0.0269(4) Uani 1 2 d S T P . .
P1 P 0.12931(8) 0.53366(13) 0.24759(8) 0.0303(4) Uani 1 1 d . . . . .
O1 O 0.0410(3) 0.3591(5) 0.0158(3) 0.0501(11) Uani 1 1 d . . . . .
O2 O 0.0863(2) 0.5811(4) 0.1645(3) 0.0388(8) Uani 1 1 d . . . . .
O3 O 0.1478(4) 0.3785(4) 0.2388(3) 0.0546(12) Uani 1 1 d . . . . .
H3 H 0.180679 0.365981 0.198336 0.082 Uiso 1 1 calc R . . . .
O4 O 0.0713(3) 0.5430(5) 0.3287(3) 0.0478(11) Uani 1 1 d . . . . .
H4 H 0.027763 0.502002 0.318934 0.072 Uiso 0.5 1 calc R . . . .
N1 N 0.250000 0.750000 0.9834(5) 0.0463(19) Uani 1 2 d S T P . .
C1 C 0.272(2) 0.672(3) 1.062(2) 0.136(12) Uani 0.67(4) 1 d . . . A 1
C2 C 0.287(4) 0.847(7) 0.926(3) 0.29(5) Uani 0.67(4) 1 d . . . A 1
H2A H 0.313310 0.916355 0.960004 0.441 Uiso 0.67(4) 1 calc R . . A 1
H2B H 0.328025 0.804007 0.889634 0.441 Uiso 0.67(4) 1 calc R . . A 1
H2C H 0.244367 0.886207 0.889634 0.441 Uiso 0.67(4) 1 calc R . . A 1
C1' C 0.251(2) 0.612(3) 0.998(4) 0.095(17) Uani 0.33(4) 1 d . . . A 2
H1'A H 0.250773 0.565042 0.943151 0.142 Uiso 0.33(4) 1 calc R . . A 2
H1'B H 0.299709 0.587756 1.030948 0.142 Uiso 0.33(4) 1 calc R . . A 2
H1'C H 0.201652 0.586698 1.030948 0.142 Uiso 0.33(4) 1 calc R . . A 2
C2' C 0.350(2) 0.749(4) 0.972(4) 0.099(17) Uani 0.33(4) 1 d . . . A 2
H2'A H 0.368958 0.658676 0.960402 0.148 Uiso 0.33(4) 1 calc R . . A 2
H2'B H 0.365974 0.806029 0.924152 0.148 Uiso 0.33(4) 1 calc R . . A 2
H2'C H 0.376187 0.780661 1.024992 0.148 Uiso 0.33(4) 1 calc R . . A 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 1.937(4) 2_565 ?
Zn1 O1 1.937(4) . ?
Zn1 O2 1.943(4) 2_565 ?
Zn1 O2 1.943(4) . ?
P1 O1 1.504(4) 4 ?
P1 O2 1.517(4) . ?
P1 O3 1.577(5) . ?
P1 O4 1.549(4) . ?
O3 H3 0.8200 . ?
O4 H4 0.8200 . ?
N1 C1 1.47(2) . ?
N1 C1 1.47(2) 14_565 ?
N1 C2 1.43(3) 14_565 ?
N1 C2 1.43(3) . ?
N1 C1' 1.40(3) . ?
N1 C1' 1.40(3) 14_565 ?
N1 C2' 1.62(4) . ?
N1 C2' 1.62(4) 14_565 ?
C1 C1 1.70(8) 14_565 ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C1' H1'A 0.9600 . ?
C1' H1'B 0.9600 . ?
C1' H1'C 0.9600 . ?
C2' H2'A 0.9600 . ?
C2' H2'B 0.9600 . ?
C2' H2'C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O1 106.1(3) 2_565 . ?
O1 Zn1 O2 113.70(18) . . ?
O1 Zn1 O2 106.39(19) 2_565 . ?
O1 Zn1 O2 113.70(18) 2_565 2_565 ?
O1 Zn1 O2 106.39(19) . 2_565 ?
O2 Zn1 O2 110.7(3) . 2_565 ?
O1 P1 O2 112.5(3) 4 . ?
O1 P1 O3 110.2(3) 4 . ?
O1 P1 O4 109.3(2) 4 . ?
O2 P1 O3 108.6(2) . . ?
O2 P1 O4 112.2(3) . . ?
O4 P1 O3 103.8(3) . . ?
P1 O1 Zn1 139.4(3) 8_544 . ?
P1 O2 Zn1 131.9(3) . . ?
P1 O3 H3 109.5 . . ?
P1 O4 H4 109.5 . . ?
C1 N1 C1 71(3) 14_565 . ?
C1 N1 C2' 81(2) 14_565 14_565 ?
C1 N1 C2' 109(2) . 14_565 ?
C2 N1 C1 104(3) . 14_565 ?
C2 N1 C1 139(3) . . ?
C2 N1 C1 139(3) 14_565 14_565 ?
C2 N1 C1 104(3) 14_565 . ?
C2 N1 C2 105(4) 14_565 . ?
C2 N1 C2' 62(3) 14_565 14_565 ?
C2 N1 C2' 110(4) . 14_565 ?
C1' N1 C1' 161(5) 14_565 . ?
C1' N1 C2' 90.2(19) 14_565 14_565 ?
C1' N1 C2' 92(2) 14_565 . ?
C1' N1 C2' 92(2) . 14_565 ?
C1' N1 C2' 90.2(19) . . ?
C2' N1 C2' 168(4) . 14_565 ?
N1 C1 C1 54.7(17) . 14_565 ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C1' H1'A 109.5 . . ?
N1 C1' H1'B 109.5 . . ?
N1 C1' H1'C 109.5 . . ?
H1'A C1' H1'B 109.5 . . ?
H1'A C1' H1'C 109.5 . . ?
H1'B C1' H1'C 109.5 . . ?
N1 C2' H2'A 109.5 . . ?
N1 C2' H2'B 109.5 . . ?
N1 C2' H2'C 109.5 . . ?
H2'A C2' H2'B 109.5 . . ?
H2'A C2' H2'C 109.5 . . ?
H2'B C2' H2'C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.75(2)
2 0.25(2)

