# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1519627'
loop_
_audit_author_name
_audit_author_address
'Sandeep Kumar Gupta'
;Indian Institute of Technology Bombay, Mumbai
India
;
_audit_update_record             
;
2019-05-22 deposited with the CCDC.	2019-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H96 N4 O20 P4 S4 Zn4'
_chemical_formula_weight         1658.96

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_H-M_alt        'I b a 2'
_space_group_name_Hall           'I 2 -2c'

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

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

_cell_length_a                   21.231(8)
_cell_length_b                   21.328(8)
_cell_length_c                   20.064(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9085(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_F_000             3456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.261
_shelx_estimated_absorpt_T_min   0.667
_shelx_estimated_absorpt_T_max   0.884
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34447
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.022
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_full        24.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6093
_reflns_number_gt                5948
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_max     0.997
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0525P)²+153.9310P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1589 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6093
_refine_ls_number_parameters     444
_refine_ls_number_restraints     101
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0726
_refine_ls_wR_factor_ref         0.1710
_refine_ls_wR_factor_gt          0.1700
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4886(6) 0.7294(6) 0.3958(7) 0.032(3) Uani 1 1 d . . . . .
C2 C 0.4323(7) 0.7618(7) 0.3908(7) 0.043(4) Uani 1 1 d . U . . .
C3 C 0.4343(10) 0.8256(8) 0.3755(8) 0.062(5) Uani 1 1 d . U . . .
H3 H 0.3964 0.8490 0.3725 0.075 Uiso 1 1 calc R U . . .
C4 C 0.4945(12) 0.8562(6) 0.3643(9) 0.077(6) Uani 1 1 d D U . . .
C5 C 0.5447(10) 0.8221(7) 0.3670(12) 0.087(7) Uani 1 1 d . U . . .
H5 H 0.5838 0.8412 0.3562 0.104 Uiso 1 1 calc R U . . .
C6 C 0.5452(8) 0.7566(6) 0.3854(11) 0.067(6) Uani 1 1 d . . . . .
C10 C 0.6047(11) 0.7221(10) 0.4028(13) 0.094(7) Uani 1 1 d . U . . .
H10 H 0.5878 0.6814 0.4199 0.112 Uiso 1 1 calc R U . . .
C11 C 0.6443(10) 0.7010(10) 0.3465(11) 0.089(7) Uani 1 1 d . U . . .
H11A H 0.6172 0.6870 0.3098 0.134 Uiso 1 1 calc R U . . .
H11B H 0.6711 0.6662 0.3611 0.134 Uiso 1 1 calc R U . . .
H11C H 0.6708 0.7358 0.3313 0.134 Uiso 1 1 calc R U . . .
C12 C 0.6419(9) 0.7458(9) 0.4629(10) 0.073(5) Uani 1 1 d . U . . .
H12A H 0.6746 0.7152 0.4745 0.110 Uiso 1 1 calc R U . . .
H12B H 0.6134 0.7514 0.5008 0.110 Uiso 1 1 calc R U . . .
H12C H 0.6617 0.7860 0.4518 0.110 Uiso 1 1 calc R U . . .
C13 C 0.7322(3) 0.5045(3) 0.1651(5) 0.029(3) Uani 1 1 d G . . . .
C14 C 0.7594(3) 0.4468(3) 0.1796(4) 0.027(3) Uani 1 1 d G . . . .
C15 C 0.8237(4) 0.4427(3) 0.1918(5) 0.047(4) Uani 1 1 d G . . . .
H15 H 0.8422 0.4032 0.2018 0.056 Uiso 1 1 calc R U . . .
C16 C 0.8608(3) 0.4963(4) 0.1896(5) 0.050(4) Uani 1 1 d G . . . .
C17 C 0.8337(3) 0.5540(3) 0.1750(5) 0.047(4) Uani 1 1 d G . . . .
H17 H 0.8591 0.5906 0.1735 0.057 Uiso 1 1 calc R U . . .
C18 C 0.7694(4) 0.5581(3) 0.1628(5) 0.040(3) Uani 1 1 d G . . . .
C19 C 0.7189(7) 0.3886(6) 0.1742(9) 0.049(4) Uani 1 1 d . . . . .
H19 H 0.6759 0.4009 0.1586 0.058 Uiso 1 1 calc R U . . .
C20 C 0.7466(9) 0.3416(8) 0.1253(11) 0.072(6) Uani 1 1 d . . . . .
H20A H 0.7916 0.3500 0.1195 0.108 Uiso 1 1 calc R U . . .
H20B H 0.7251 0.3455 0.0823 0.108 Uiso 1 1 calc R U . . .
H20C H 0.7408 0.2990 0.1427 0.108 Uiso 1 1 calc R U . . .
C21 C 0.7140(8) 0.3625(7) 0.2463(8) 0.050(4) Uani 1 1 d . . . . .
H21A H 0.7370 0.3228 0.2493 0.076 Uiso 1 1 calc R U . . .
H21B H 0.6696 0.3555 0.2575 0.076 Uiso 1 1 calc R U . . .
H21C H 0.7322 0.3928 0.2775 0.076 Uiso 1 1 calc R U . . .
C22 C 0.7395(7) 0.6228(7) 0.1452(8) 0.048(4) Uani 1 1 d D . . . .
H22 H 0.6958 0.6158 0.1283 0.057 Uiso 1 1 calc R U . . .
C23 C 0.7364(9) 0.6624(6) 0.2061(10) 0.067(5) Uani 1 1 d . . . . .
H23A H 0.7193 0.6377 0.2431 0.101 Uiso 1 1 calc R U . . .
H23B H 0.7090 0.6985 0.1978 0.101 Uiso 1 1 calc R U . . .
H23C H 0.7787 0.6771 0.2176 0.101 Uiso 1 1 calc R U . . .
C24 C 0.7787(9) 0.6577(8) 0.0902(11) 0.079(7) Uani 1 1 d D . . . .
H24A H 0.7808 0.6316 0.0501 0.119 Uiso 1 1 calc R U . . .
H24B H 0.7584 0.6977 0.0795 0.119 Uiso 1 1 calc R U . . .
H24C H 0.8214 0.6655 0.1068 0.119 Uiso 1 1 calc R U . . .
C25 C 0.5926(8) 0.4509(7) 0.5145(7) 0.042(4) Uani 1 1 d . . . . .
H25A H 0.5871 0.4411 0.5619 0.064 Uiso 1 1 calc R U . . .
H25B H 0.6046 0.4128 0.4904 0.064 Uiso 1 1 calc R U . . .
H25C H 0.5529 0.4671 0.4964 0.064 Uiso 1 1 calc R U . . .
C26 C 0.6128(8) 0.5782(6) 0.5296(7) 0.038(4) Uani 1 1 d . . . . .
H26A H 0.5707 0.5779 0.5096 0.057 Uiso 1 1 calc R U . . .
H26B H 0.6357 0.6155 0.5146 0.057 Uiso 1 1 calc R U . . .
H26C H 0.6090 0.5790 0.5783 0.057 Uiso 1 1 calc R U . . .
C27 C 0.5583(9) 0.7418(10) 0.1735(11) 0.077(6) Uani 1 1 d . . . . .
H27A H 0.5710 0.7860 0.1738 0.115 Uiso 1 1 calc R U . . .
H27B H 0.5581 0.7256 0.2193 0.115 Uiso 1 1 calc R U . . .
H27C H 0.5882 0.7175 0.1467 0.115 Uiso 1 1 calc R U . . .
C28 C 0.4410(12) 0.7655(8) 0.2103(9) 0.092(8) Uani 1 1 d D . . . .
H28A H 0.4285 0.7308 0.2394 0.138 Uiso 1 1 calc R U . . .
H28B H 0.4032 0.7871 0.1940 0.138 Uiso 1 1 calc R U . . .
H28C H 0.4672 0.7950 0.2353 0.138 Uiso 1 1 calc R U . . .
N2 N 0.9257(5) 0.4931(6) 0.2077(8) 0.053(3) Uani 1 1 d . . . . .
H2A H 0.9286 0.4975 0.2520 0.063 Uiso 1 1 d R U . . .
H2B H 0.9427 0.4560 0.1975 0.063 Uiso 1 1 d R U . . .
O1 O 0.4851(4) 0.6654(4) 0.4141(4) 0.030(2) Uani 1 1 d . . . . .
O2 O 0.4989(4) 0.6389(3) 0.2928(4) 0.032(2) Uani 1 1 d . . . . .
O3 O 0.5371(4) 0.5652(4) 0.3862(4) 0.030(2) Uani 1 1 d . . . . .
O4 O 0.5790(4) 0.4203(3) 0.3641(4) 0.0257(17) Uani 1 1 d . . . . .
O5 O 0.6679(4) 0.5109(3) 0.1517(4) 0.0228(18) Uani 1 1 d . . . . .
O6 O 0.6408(4) 0.5263(4) 0.2732(5) 0.037(2) Uani 1 1 d . . . . .
O7 O 0.5755(5) 0.5738(4) 0.1815(4) 0.034(2) Uani 1 1 d . . . . .
O8 O 0.5730(4) 0.4589(4) 0.1982(5) 0.037(2) Uani 1 1 d . . . . .
O9 O 0.6639(4) 0.5178(4) 0.4311(5) 0.035(2) Uani 1 1 d . . . . .
O10 O 0.4676(5) 0.6670(4) 0.1407(5) 0.044(3) Uani 1 1 d . . . . .
P1 P 0.48547(15) 0.60984(13) 0.35963(19) 0.0262(7) Uani 1 1 d . . . . .
P2 P 0.61157(14) 0.51740(13) 0.20478(18) 0.0232(6) Uani 1 1 d . . . . .
S1 S 0.65431(16) 0.51008(14) 0.50498(17) 0.0308(7) Uani 1 1 d . . . . .
S2 S 0.48511(16) 0.73513(14) 0.14029(18) 0.0345(8) Uani 1 1 d D . . . .
Zn1 Zn 0.60086(6) 0.50837(5) 0.35706(8) 0.0224(3) Uani 1 1 d . . . . .
Zn2 Zn 0.49258(6) 0.60106(5) 0.20572(8) 0.0236(3) Uani 1 1 d . . . . .
C7 C 0.3731(12) 0.7235(17) 0.4229(12) 0.030(7) Uani 0.52(3) 1 d D U P A 1
H0AA H 0.3742 0.6797 0.4049 0.036 Uiso 0.52(3) 1 calc R U P A 1
C9 C 0.3087(14) 0.7526(17) 0.4037(18) 0.068(7) Uani 0.52(3) 1 d D U P A 1
H2AA H 0.3052 0.7547 0.3550 0.103 Uiso 0.52(3) 1 calc R U P A 1
H2AB H 0.2746 0.7266 0.4216 0.103 Uiso 0.52(3) 1 calc R U P A 1
H2AC H 0.3057 0.7950 0.4223 0.103 Uiso 0.52(3) 1 calc R U P A 1
C8 C 0.3803(15) 0.7195(16) 0.5001(12) 0.052(9) Uani 0.52(3) 1 d D U P A 1
H1AA H 0.4214 0.7012 0.5111 0.079 Uiso 0.52(3) 1 calc R U P A 1
H1AB H 0.3468 0.6931 0.5185 0.079 Uiso 0.52(3) 1 calc R U P A 1
H1AC H 0.3773 0.7617 0.5193 0.079 Uiso 0.52(3) 1 calc R U P A 1
C9A C 0.3177(16) 0.7773(17) 0.359(2) 0.068(7) Uani 0.48(3) 1 d D U P A 2
H2AD H 0.2936 0.8020 0.3908 0.103 Uiso 0.48(3) 1 calc R U P A 2
H2AE H 0.2894 0.7479 0.3358 0.103 Uiso 0.48(3) 1 calc R U P A 2
H2AF H 0.3370 0.8053 0.3257 0.103 Uiso 0.48(3) 1 calc R U P A 2
C7A C 0.3701(15) 0.7400(18) 0.396(2) 0.046(11) Uani 0.48(3) 1 d D U P A 2
H0AB H 0.3707 0.6980 0.3734 0.055 Uiso 0.48(3) 1 calc R U P A 2
C8A C 0.351(2) 0.726(2) 0.469(2) 0.079(14) Uani 0.48(3) 1 d D U P A 2
H1AD H 0.3550 0.6812 0.4774 0.119 Uiso 0.48(3) 1 calc R U P A 2
H1AE H 0.3075 0.7394 0.4760 0.119 Uiso 0.48(3) 1 calc R U P A 2
H1AF H 0.3790 0.7494 0.4988 0.119 Uiso 0.48(3) 1 calc R U P A 2
N1 N 0.4769(13) 0.9170(7) 0.3396(12) 0.035(4) Uani 0.58(3) 1 d D U P B 1
H1A H 0.4642 0.9160 0.2978 0.042 Uiso 0.58(3) 1 d R U P B 1
H1B H 0.4461 0.9314 0.3649 0.042 Uiso 0.58(3) 1 d R U P B 1
N1A N 0.5084(18) 0.9186(9) 0.3431(17) 0.035(4) Uani 0.42(3) 1 d D U P B 2
H1AG H 0.4725 0.9392 0.3367 0.042 Uiso 0.42(3) 1 d R U P B 2
H1AH H 0.5301 0.9371 0.3758 0.042 Uiso 0.42(3) 1 d R U P B 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
C1 C6 1.35(2) . ?
C1 C2 1.385(19) . ?
C1 O1 1.415(15) . ?
C2 C3 1.40(2) . ?
C2 C7A 1.40(4) . ?
C2 C7 1.63(3) . ?
C3 C4 1.45(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.29(3) . ?
C4 N1A 1.429(12) . ?
C4 N1 1.438(12) . ?
C5 C6 1.44(2) . ?
C5 H5 0.9500 . ?
C6 C10 1.50(3) . ?
C10 C11 1.48(3) . ?
C10 C12 1.53(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.3900 . ?
C13 C18 1.3900 . ?
C13 O5 1.399(9) . ?
C14 C15 1.3900 . ?
C14 C19 1.513(16) . ?
C15 C16 1.3900 . ?
C15 H15 0.9500 . ?
C16 C17 1.3900 . ?
C16 N2 1.427(13) . ?
C17 C18 1.3900 . ?
C17 H17 0.9500 . ?
C18 C22 1.559(15) . ?
C19 C20 1.52(2) . ?
C19 C21 1.55(2) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.49(2) . ?
C22 C24 1.570(18) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 S1 1.830(15) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 S1 1.771(14) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 S2 1.697(19) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 S2 1.808(16) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N2 H2A 0.8950 . ?
N2 H2B 0.8930 . ?
O1 P1 1.613(8) . ?
O2 P1 1.505(9) . ?
O2 Zn2 1.930(8) . ?
O3 P1 1.545(9) . ?
O3 Zn1 1.910(8) . ?
O4 P1 1.515(8) 2_665 ?
O4 Zn1 1.939(7) . ?
O5 P2 1.606(8) . ?
O6 P2 1.519(10) . ?
O6 Zn1 1.922(9) . ?
O7 P2 1.500(9) . ?
O7 Zn2 1.916(10) . ?
O8 P2 1.498(9) . ?
O8 Zn2 1.896(8) 2_665 ?
O9 S1 1.506(10) . ?
O9 Zn1 2.009(9) . ?
O10 S2 1.499(9) . ?
O10 Zn2 1.990(8) . ?
P1 O4 1.515(8) 2_665 ?
Zn2 O8 1.897(8) 2_665 ?
C7 C9 1.550(12) . ?
C7 C8 1.559(12) . ?
C7 H0AA 1.0000 . ?
C9 H2AA 0.9800 . ?
C9 H2AB 0.9800 . ?
C9 H2AC 0.9800 . ?
C8 H1AA 0.9800 . ?
C8 H1AB 0.9800 . ?
C8 H1AC 0.9800 . ?
C9A C7A 1.556(12) . ?
C9A H2AD 0.9800 . ?
C9A H2AE 0.9800 . ?
C9A H2AF 0.9800 . ?
C7A C8A 1.549(12) . ?
C7A H0AB 1.0000 . ?
C8A H1AD 0.9800 . ?
C8A H1AE 0.9800 . ?
C8A H1AF 0.9800 . ?
N1 H1A 0.8818 . ?
N1 H1B 0.8825 . ?
N1A H1AG 0.8892 . ?
N1A H1AH 0.8927 . ?

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
C6 C1 C2 123.0(13) . . ?
C6 C1 O1 120.1(12) . . ?
C2 C1 O1 116.9(12) . . ?
C1 C2 C3 118.3(15) . . ?
C1 C2 C7A 130.1(18) . . ?
C3 C2 C7A 111.5(19) . . ?
C1 C2 C7 112.8(15) . . ?
C3 C2 C7 126.8(17) . . ?
C2 C3 C4 120.0(15) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 N1A 111(2) . . ?
C5 C4 N1 137(2) . . ?
C5 C4 C3 117.8(13) . . ?
N1A C4 C3 130(2) . . ?
N1 C4 C3 103.4(19) . . ?
C4 C5 C6 124.1(17) . . ?
C4 C5 H5 117.9 . . ?
C6 C5 H5 117.9 . . ?
C1 C6 C5 116.6(16) . . ?
C1 C6 C10 120.2(16) . . ?
C5 C6 C10 122.5(17) . . ?
C11 C10 C6 117(2) . . ?
C11 C10 C12 114(2) . . ?
C6 C10 C12 117.2(17) . . ?
C11 C10 H10 101.6 . . ?
C6 C10 H10 101.6 . . ?
C12 C10 H10 101.6 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 120.0 . . ?
C14 C13 O5 122.1(6) . . ?
C18 C13 O5 117.9(6) . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C19 118.4(8) . . ?
C15 C14 C19 121.2(7) . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 N2 119.7(8) . . ?
C15 C16 N2 120.0(8) . . ?
C16 C17 C18 120.0 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C13 120.0 . . ?
C17 C18 C22 119.7(8) . . ?
C13 C18 C22 120.3(8) . . ?
C14 C19 C20 111.6(12) . . ?
C14 C19 C21 105.4(12) . . ?
C20 C19 C21 113.0(14) . . ?
C14 C19 H19 108.9 . . ?
C20 C19 H19 108.9 . . ?
C21 C19 H19 108.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C18 109.6(12) . . ?
C23 C22 C24 109.4(14) . . ?
C18 C22 C24 111.3(11) . . ?
C23 C22 H22 108.9 . . ?
C18 C22 H22 108.9 . . ?
C24 C22 H22 108.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
S1 C25 H25A 109.5 . . ?
S1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
S1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
S1 C26 H26A 109.5 . . ?
S1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
S1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
S2 C27 H27A 109.5 . . ?
S2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
S2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
S2 C28 H28A 109.5 . . ?
S2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
S2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C16 N2 H2A 108.3 . . ?
C16 N2 H2B 111.9 . . ?
H2A N2 H2B 107.1 . . ?
C1 O1 P1 122.2(8) . . ?
P1 O2 Zn2 128.4(5) . . ?
P1 O3 Zn1 142.0(6) . . ?
P1 O4 Zn1 128.6(4) 2_665 . ?
C13 O5 P2 127.5(7) . . ?
P2 O6 Zn1 125.9(5) . . ?
P2 O7 Zn2 129.3(6) . . ?
P2 O8 Zn2 162.9(6) . 2_665 ?
S1 O9 Zn1 128.8(6) . . ?
S2 O10 Zn2 128.5(6) . . ?
O2 P1 O4 113.6(5) . 2_665 ?
O2 P1 O3 115.2(5) . . ?
O4 P1 O3 111.0(5) 2_665 . ?
O2 P1 O1 107.6(5) . . ?
O4 P1 O1 105.5(5) 2_665 . ?
O3 P1 O1 102.8(5) . . ?
O8 P2 O7 111.2(5) . . ?
O8 P2 O6 114.0(5) . . ?
O7 P2 O6 112.9(5) . . ?
O8 P2 O5 106.1(5) . . ?
O7 P2 O5 104.0(5) . . ?
O6 P2 O5 107.8(5) . . ?
O9 S1 C26 104.7(6) . . ?
O9 S1 C25 106.0(6) . . ?
C26 S1 C25 100.4(7) . . ?
O10 S2 C27 107.8(8) . . ?
O10 S2 C28 102.4(8) . . ?
C27 S2 C28 98.0(12) . . ?
O3 Zn1 O6 117.0(4) . . ?
O3 Zn1 O4 115.0(3) . . ?
O6 Zn1 O4 111.3(4) . . ?
O3 Zn1 O9 100.5(4) . . ?
O6 Zn1 O9 109.5(4) . . ?
O4 Zn1 O9 101.7(4) . . ?
O8 Zn2 O7 116.7(4) 2_665 . ?
O8 Zn2 O2 113.9(4) 2_665 . ?
O7 Zn2 O2 107.0(4) . . ?
O8 Zn2 O10 103.2(4) 2_665 . ?
O7 Zn2 O10 107.0(4) . . ?
O2 Zn2 O10 108.4(4) . . ?
C9 C7 C8 110.8(12) . . ?
C9 C7 C2 112(2) . . ?
C8 C7 C2 110(2) . . ?
C9 C7 H0AA 107.8 . . ?
C8 C7 H0AA 107.8 . . ?
C2 C7 H0AA 107.8 . . ?
C7 C9 H2AA 109.5 . . ?
C7 C9 H2AB 109.5 . . ?
H2AA C9 H2AB 109.5 . . ?
C7 C9 H2AC 109.5 . . ?
H2AA C9 H2AC 109.5 . . ?
H2AB C9 H2AC 109.5 . . ?
C7 C8 H1AA 109.5 . . ?
C7 C8 H1AB 109.5 . . ?
H1AA C8 H1AB 109.5 . . ?
C7 C8 H1AC 109.5 . . ?
H1AA C8 H1AC 109.5 . . ?
H1AB C8 H1AC 109.5 . . ?
C7A C9A H2AD 109.5 . . ?
C7A C9A H2AE 109.5 . . ?
H2AD C9A H2AE 109.5 . . ?
C7A C9A H2AF 109.5 . . ?
H2AD C9A H2AF 109.5 . . ?
H2AE C9A H2AF 109.5 . . ?
C2 C7A C8A 112(3) . . ?
C2 C7A C9A 118(2) . . ?
C8A C7A C9A 111.3(12) . . ?
C2 C7A H0AB 104.7 . . ?
C8A C7A H0AB 104.7 . . ?
C9A C7A H0AB 104.7 . . ?
C7A C8A H1AD 109.5 . . ?
C7A C8A H1AE 109.5 . . ?
H1AD C8A H1AE 109.5 . . ?
C7A C8A H1AF 109.5 . . ?
H1AD C8A H1AF 109.5 . . ?
H1AE C8A H1AF 109.5 . . ?
C4 N1 H1A 112.6 . . ?
C4 N1 H1B 107.9 . . ?
H1A N1 H1B 109.2 . . ?
C4 N1A H1AG 109.0 . . ?
C4 N1A H1AH 107.5 . . ?
H1AG N1A H1AH 109.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -1(2) . . . . ?
O1 C1 C2 C3 177.4(12) . . . . ?
C6 C1 C2 C7A 175(3) . . . . ?
O1 C1 C2 C7A -6(3) . . . . ?
C6 C1 C2 C7 -166.1(17) . . . . ?
O1 C1 C2 C7 12.5(18) . . . . ?
C1 C2 C3 C4 1(2) . . . . ?
C7A C2 C3 C4 -176(2) . . . . ?
C7 C2 C3 C4 163.4(17) . . . . ?
C2 C3 C4 C5 2(3) . . . . ?
C2 C3 C4 N1A 174(2) . . . . ?
C2 C3 C4 N1 170.8(16) . . . . ?
N1A C4 C5 C6 -179(2) . . . . ?
N1 C4 C5 C6 -169(3) . . . . ?
C3 C4 C5 C6 -5(3) . . . . ?
C2 C1 C6 C5 -1(3) . . . . ?
O1 C1 C6 C5 -179.8(15) . . . . ?
C2 C1 C6 C10 169.5(16) . . . . ?
O1 C1 C6 C10 -9(3) . . . . ?
C4 C5 C6 C1 5(3) . . . . ?
C4 C5 C6 C10 -166(2) . . . . ?
C1 C6 C10 C11 110(2) . . . . ?
C5 C6 C10 C11 -80(3) . . . . ?
C1 C6 C10 C12 -109(2) . . . . ?
C5 C6 C10 C12 61(3) . . . . ?
C18 C13 C14 C15 0.0 . . . . ?
O5 C13 C14 C15 179.3(9) . . . . ?
C18 C13 C14 C19 -173.4(10) . . . . ?
O5 C13 C14 C19 5.9(11) . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C19 C14 C15 C16 173.2(10) . . . . ?
C14 C15 C16 C17 0.0 . . . . ?
C14 C15 C16 N2 174.6(12) . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
N2 C16 C17 C18 -174.6(12) . . . . ?
C16 C17 C18 C13 0.0 . . . . ?
C16 C17 C18 C22 -178.8(10) . . . . ?
C14 C13 C18 C17 0.0 . . . . ?
O5 C13 C18 C17 -179.3(9) . . . . ?
C14 C13 C18 C22 178.8(11) . . . . ?
O5 C13 C18 C22 -0.5(11) . . . . ?
C13 C14 C19 C20 122.0(13) . . . . ?
C15 C14 C19 C20 -51.2(17) . . . . ?
C13 C14 C19 C21 -115.0(11) . . . . ?
C15 C14 C19 C21 71.7(12) . . . . ?
C17 C18 C22 C23 -73.6(13) . . . . ?
C13 C18 C22 C23 107.6(13) . . . . ?
C17 C18 C22 C24 47.5(15) . . . . ?
C13 C18 C22 C24 -131.3(12) . . . . ?
C6 C1 O1 P1 -85.3(16) . . . . ?
C2 C1 O1 P1 96.1(13) . . . . ?
C14 C13 O5 P2 83.3(9) . . . . ?
C18 C13 O5 P2 -97.3(8) . . . . ?
Zn2 O2 P1 O4 -52.7(8) . . . 2_665 ?
Zn2 O2 P1 O3 76.9(8) . . . . ?
Zn2 O2 P1 O1 -169.1(6) . . . . ?
Zn1 O3 P1 O2 -30.1(10) . . . . ?
Zn1 O3 P1 O4 100.7(9) . . . 2_665 ?
Zn1 O3 P1 O1 -146.9(8) . . . . ?
C1 O1 P1 O2 7.7(11) . . . . ?
C1 O1 P1 O4 -113.9(10) . . . 2_665 ?
C1 O1 P1 O3 129.7(9) . . . . ?
Zn2 O8 P2 O7 -56(2) 2_665 . . . ?
Zn2 O8 P2 O6 73(2) 2_665 . . . ?
Zn2 O8 P2 O5 -168(2) 2_665 . . . ?
Zn2 O7 P2 O8 50.9(8) . . . . ?
Zn2 O7 P2 O6 -78.7(8) . . . . ?
Zn2 O7 P2 O5 164.6(6) . . . . ?
Zn1 O6 P2 O8 -39.8(8) . . . . ?
Zn1 O6 P2 O7 88.3(7) . . . . ?
Zn1 O6 P2 O5 -157.3(5) . . . . ?
C13 O5 P2 O8 -113.2(8) . . . . ?
C13 O5 P2 O7 129.5(7) . . . . ?
C13 O5 P2 O6 9.4(8) . . . . ?
Zn1 O9 S1 C26 -74.5(9) . . . . ?
Zn1 O9 S1 C25 31.1(9) . . . . ?
Zn2 O10 S2 C27 31.9(12) . . . . ?
Zn2 O10 S2 C28 -70.8(12) . . . . ?
C1 C2 C7 C9 -167.4(18) . . . . ?
C3 C2 C7 C9 29(3) . . . . ?
C1 C2 C7 C8 69(2) . . . . ?
C3 C2 C7 C8 -95(2) . . . . ?
C1 C2 C7A C8A 76(4) . . . . ?
C3 C2 C7A C8A -108(3) . . . . ?
C1 C2 C7A C9A -153(2) . . . . ?
C3 C2 C7A C9A 23(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C25 H25A O7 0.98 2.43 3.411(16) 175.1 4_565
C25 H25B O4 0.98 2.60 3.101(17) 112.1 .
C26 H26A O3 0.98 2.59 3.308(17) 130.1 .
C26 H26C O8 0.98 2.65 3.575(16) 157.4 4_565

_refine_diff_density_max         1.009
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.125



####################################################################### 
# 
# 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_KS_2_MeOH
_database_code_depnum_ccdc_archive 'CCDC 1519628'
loop_
_audit_author_name
_audit_author_address
'Sandeep Kumar Gupta'
;Indian Institute of Technology Bombay, Mumbai
India
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H20 N O5 P Zn, C H4 O'
_chemical_formula_sum            'C15 H24 N O6 P Zn'
_chemical_formula_weight         410.69

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   16.942(5)
_cell_length_b                   16.942(5)
_cell_length_c                   15.489(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4446(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5457
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      31.3

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_F_000             1712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.201
_shelx_estimated_absorpt_T_min   0.795
_shelx_estimated_absorpt_T_max   0.813
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            16615
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.630
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_full        24.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3890
_reflns_number_gt                3669
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       
;
CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0409P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1505 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3890
_refine_ls_number_parameters     225
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0715
_refine_ls_wR_factor_gt          0.0708
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
C1 C 0.8368(2) 0.3192(2) 0.5412(3) 0.0280(9) Uani 1 1 d . . . . .
C2 C 0.8291(2) 0.3660(2) 0.4679(3) 0.0311(10) Uani 1 1 d . . . . .
C3 C 0.7532(3) 0.3707(3) 0.4305(3) 0.0391(11) Uani 1 1 d . . . . .
H3 H 0.7449 0.4031 0.3812 0.047 Uiso 1 1 calc R U . . .
C4 C 0.6910(3) 0.3286(3) 0.4650(3) 0.0388(11) Uani 1 1 d . . . . .
C5 C 0.7007(3) 0.2823(3) 0.5382(3) 0.0411(12) Uani 1 1 d . . . . .
H5 H 0.6569 0.2543 0.5612 0.049 Uiso 1 1 calc R U . . .
C6 C 0.7743(3) 0.2765(2) 0.5785(3) 0.0365(11) Uani 1 1 d . . . . .
C7 C 0.7837(3) 0.2292(3) 0.6600(4) 0.0532(13) Uani 1 1 d . . . . .
H7 H 0.8412 0.2209 0.6716 0.064 Uiso 1 1 calc R U . . .
C8 C 0.7430(5) 0.1501(4) 0.6567(5) 0.091(2) Uani 1 1 d . . . . .
H8A H 0.7589 0.1220 0.6042 0.137 Uiso 1 1 calc R U . . .
H8B H 0.6857 0.1579 0.6562 0.137 Uiso 1 1 calc R U . . .
H8C H 0.7578 0.1189 0.7074 0.137 Uiso 1 1 calc R U . . .
C9 C 0.7465(4) 0.2751(4) 0.7370(4) 0.078(2) Uani 1 1 d . . . . .
H9A H 0.6897 0.2815 0.7271 0.117 Uiso 1 1 calc R U . . .
H9B H 0.7712 0.3272 0.7417 0.117 Uiso 1 1 calc R U . . .
H9C H 0.7550 0.2456 0.7906 0.117 Uiso 1 1 calc R U . . .
C10 C 0.8982(3) 0.4054(3) 0.4258(3) 0.0422(11) Uani 1 1 d . . . . .
H10 H 0.9376 0.4169 0.4721 0.051 Uiso 1 1 calc R U . . .
C11 C 0.8769(4) 0.4828(4) 0.3841(4) 0.077(2) Uani 1 1 d . . . . .
H11A H 0.8438 0.5136 0.4236 0.116 Uiso 1 1 calc R U . . .
H11B H 0.8479 0.4728 0.3305 0.116 Uiso 1 1 calc R U . . .
H11C H 0.9252 0.5123 0.3712 0.116 Uiso 1 1 calc R U . . .
C12 C 0.9372(3) 0.3488(4) 0.3620(4) 0.075(2) Uani 1 1 d . . . . .
H12A H 0.9044 0.3442 0.3102 0.113 Uiso 1 1 calc R U . . .
H12B H 0.9431 0.2968 0.3889 0.113 Uiso 1 1 calc R U . . .
H12C H 0.9894 0.3692 0.3460 0.113 Uiso 1 1 calc R U . . .
C13 C 0.5701(2) 0.2768(2) 0.4020(3) 0.0334(10) Uani 1 1 d . . . . .
C14 C 0.4939(2) 0.2953(3) 0.3569(4) 0.0463(13) Uani 1 1 d . . . . .
H14A H 0.4533 0.2575 0.3749 0.069 Uiso 1 1 calc R U . . .
H14B H 0.5015 0.2916 0.2943 0.069 Uiso 1 1 calc R U . . .
H14C H 0.4770 0.3489 0.3720 0.069 Uiso 1 1 calc R U . . .
C15 C 0.6436(5) 0.5340(5) 0.2993(8) 0.151(5) Uani 1 1 d . . . . .
H15A H 0.6825 0.5319 0.3460 0.226 Uiso 1 1 calc R U . . .
H15B H 0.6115 0.5818 0.3053 0.226 Uiso 1 1 calc R U . . .
H15C H 0.6709 0.5349 0.2435 0.226 Uiso 1 1 calc R U . . .
N1 N 0.6155(2) 0.3362(2) 0.4243(3) 0.0506(11) Uani 1 1 d . . . . .
H1 H 0.5982 0.3842 0.4134 0.061 Uiso 1 1 calc R U . . .
O1 O 0.91163(15) 0.31116(15) 0.57853(19) 0.0288(7) Uani 1 1 d . . . . .
O2 O 0.9086(2) 0.45068(17) 0.6280(2) 0.0448(9) Uani 1 1 d . . . . .
O3 O 0.9301(3) 0.3433(2) 0.7329(2) 0.0677(13) Uani 1 1 d . . . . .
O4 O 0.6278(2) 0.03300(18) 0.3746(3) 0.0840(18) Uani 1 1 d . . . . .
O5 O 0.58928(17) 0.20750(16) 0.4177(2) 0.0331(7) Uani 1 1 d . . . . .
O6 O 0.5959(4) 0.4689(5) 0.3034(6) 0.171(4) Uani 1 1 d . . . . .
H6 H 0.5647 0.4690 0.2613 0.257 Uiso 1 1 calc R U . . .
P1 P 0.94703(6) 0.37481(5) 0.64523(6) 0.0246(2) Uani 1 1 d . . . . .
Zn1 Zn 0.55734(2) 0.11573(2) 0.34672(3) 0.02467(14) Uani 1 1 d . . . . .


_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
C1 C2 1.392(6) . ?
C1 O1 1.400(5) . ?
C1 C6 1.406(6) . ?
C2 C3 1.413(6) . ?
C2 C10 1.496(6) . ?
C3 C4 1.380(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(7) . ?
C4 N1 1.431(5) . ?
C5 C6 1.397(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.504(7) . ?
C7 C8 1.508(7) . ?
C7 C9 1.557(9) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.505(8) . ?
C10 C12 1.527(7) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O5 1.242(5) . ?
C13 N1 1.314(5) . ?
C13 C14 1.502(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O6 1.367(10) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N1 H1 0.8800 . ?
O1 P1 1.609(3) . ?
O2 P1 1.466(3) . ?
O2 Zn1 1.895(3) 4_656 ?
O3 P1 1.486(4) . ?
O3 Zn1 1.907(3) 7_655 ?
O4 P1 1.489(3) 4_646 ?
O4 Zn1 1.891(3) . ?
O5 Zn1 1.979(3) . ?
O6 H6 0.8400 . ?
P1 O4 1.489(3) 2_666 ?
Zn1 O2 1.894(3) 2_566 ?
Zn1 O3 1.907(3) 7_654 ?

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
C2 C1 O1 118.5(4) . . ?
C2 C1 C6 123.9(4) . . ?
O1 C1 C6 117.6(4) . . ?
C1 C2 C3 116.9(4) . . ?
C1 C2 C10 122.5(4) . . ?
C3 C2 C10 120.5(4) . . ?
C4 C3 C2 120.5(5) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 121.1(4) . . ?
C3 C4 N1 117.7(4) . . ?
C5 C4 N1 121.1(4) . . ?
C4 C5 C6 120.7(4) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 116.9(4) . . ?
C5 C6 C7 120.5(4) . . ?
C1 C6 C7 122.6(4) . . ?
C6 C7 C8 113.3(5) . . ?
C6 C7 C9 109.5(4) . . ?
C8 C7 C9 106.6(6) . . ?
C6 C7 H7 109.1 . . ?
C8 C7 H7 109.1 . . ?
C9 C7 H7 109.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 C11 112.8(4) . . ?
C2 C10 C12 110.0(4) . . ?
C11 C10 C12 111.9(5) . . ?
C2 C10 H10 107.3 . . ?
C11 C10 H10 107.3 . . ?
C12 C10 H10 107.3 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O5 C13 N1 121.3(4) . . ?
O5 C13 C14 120.9(4) . . ?
N1 C13 C14 117.7(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O6 C15 H15A 109.5 . . ?
O6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 N1 C4 124.7(4) . . ?
C13 N1 H1 117.6 . . ?
C4 N1 H1 117.6 . . ?
C1 O1 P1 122.5(2) . . ?
P1 O2 Zn1 153.6(2) . 4_656 ?
P1 O3 Zn1 133.8(2) . 7_655 ?
P1 O4 Zn1 131.3(2) 4_646 . ?
C13 O5 Zn1 124.2(3) . . ?
C15 O6 H6 109.5 . . ?
O2 P1 O3 113.3(2) . . ?
O2 P1 O4 115.0(2) . 2_666 ?
O3 P1 O4 111.5(3) . 2_666 ?
O2 P1 O1 107.76(16) . . ?
O3 P1 O1 105.89(17) . . ?
O4 P1 O1 102.28(18) 2_666 . ?
O4 Zn1 O2 113.18(17) . 2_566 ?
O4 Zn1 O3 114.2(2) . 7_654 ?
O2 Zn1 O3 112.15(17) 2_566 7_654 ?
O4 Zn1 O5 106.44(13) . . ?
O2 Zn1 O5 108.45(13) 2_566 . ?
O3 Zn1 O5 101.38(13) 7_654 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 178.0(4) . . . . ?
C6 C1 C2 C3 0.8(6) . . . . ?
O1 C1 C2 C10 2.4(6) . . . . ?
C6 C1 C2 C10 -174.8(4) . . . . ?
C1 C2 C3 C4 -1.6(6) . . . . ?
C10 C2 C3 C4 174.1(4) . . . . ?
C2 C3 C4 C5 1.6(7) . . . . ?
C2 C3 C4 N1 179.7(4) . . . . ?
C3 C4 C5 C6 -0.7(7) . . . . ?
N1 C4 C5 C6 -178.7(4) . . . . ?
C4 C5 C6 C1 -0.1(7) . . . . ?
C4 C5 C6 C7 177.2(5) . . . . ?
C2 C1 C6 C5 0.0(7) . . . . ?
O1 C1 C6 C5 -177.2(4) . . . . ?
C2 C1 C6 C7 -177.2(4) . . . . ?
O1 C1 C6 C7 5.5(6) . . . . ?
C5 C6 C7 C8 44.9(8) . . . . ?
C1 C6 C7 C8 -138.0(6) . . . . ?
C5 C6 C7 C9 -73.9(6) . . . . ?
C1 C6 C7 C9 103.2(6) . . . . ?
C1 C2 C10 C11 -148.2(5) . . . . ?
C3 C2 C10 C11 36.3(6) . . . . ?
C1 C2 C10 C12 86.1(6) . . . . ?
C3 C2 C10 C12 -89.4(6) . . . . ?
O5 C13 N1 C4 2.3(8) . . . . ?
C14 C13 N1 C4 -177.8(5) . . . . ?
C3 C4 N1 C13 130.9(5) . . . . ?
C5 C4 N1 C13 -51.0(7) . . . . ?
C2 C1 O1 P1 83.8(4) . . . . ?
C6 C1 O1 P1 -98.8(4) . . . . ?
N1 C13 O5 Zn1 -150.7(4) . . . . ?
C14 C13 O5 Zn1 29.4(6) . . . . ?
Zn1 O2 P1 O3 53.6(6) 4_656 . . . ?
Zn1 O2 P1 O4 -76.3(6) 4_656 . . 2_666 ?
Zn1 O2 P1 O1 170.4(5) 4_656 . . . ?
Zn1 O3 P1 O2 -55.6(4) 7_655 . . . ?
Zn1 O3 P1 O4 76.1(4) 7_655 . . 2_666 ?
Zn1 O3 P1 O1 -173.5(3) 7_655 . . . ?
C1 O1 P1 O2 -25.2(4) . . . . ?
C1 O1 P1 O3 96.4(4) . . . . ?
C1 O1 P1 O4 -146.8(4) . . . 2_666 ?
P1 O4 Zn1 O2 48.5(5) 4_646 . . 2_566 ?
P1 O4 Zn1 O3 -81.4(5) 4_646 . . 7_654 ?
P1 O4 Zn1 O5 167.6(4) 4_646 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O6 0.88 2.23 2.944(7) 138.3 .
N1 H1 O6 0.88 2.23 2.944(7) 138.3 .
N1 H1 O6 0.88 2.23 2.944(7) 138.3 .

_refine_diff_density_max         0.340
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.046



####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1541652'
_audit_update_record             
;
2017-04-02 deposited with the CCDC.	2019-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H43 N8 O8 P2 Zn2'
_chemical_formula_sum            'C36 H43 N8 O8 P2 Zn2'
_chemical_formula_weight         908.46

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

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

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

_cell_length_a                   18.2767(4)
_cell_length_b                   18.2767(4)
_cell_length_c                   30.7812(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10282.1(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    396(2)
_cell_measurement_reflns_used    11122
_cell_measurement_theta_min      2.286
_cell_measurement_theta_max      28.669

_exptl_crystal_description       needle
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_F_000             3752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.042
_shelx_estimated_absorpt_T_min   0.819
_shelx_estimated_absorpt_T_max   0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.19772
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            73345
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_av_R_equivalents  0.1350
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.229
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4541
_reflns_number_gt                2543
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       
;
CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1020P)²+26.3254P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4541
_refine_ls_number_parameters     279
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0955
_refine_ls_wR_factor_ref         0.2683
_refine_ls_wR_factor_gt          0.2324
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.33222(5) 0.66544(5) 0.20027(2) 0.0591(4) Uani 1 1 d . . . . .
P1 P 0.34390(12) 0.65942(12) 0.29991(5) 0.0612(6) Uani 1 1 d . . . . .
O1 O 0.3632(3) 0.6305(3) 0.25562(15) 0.0791(16) Uani 1 1 d . . . . .
O2 O 0.3685(4) 0.7635(3) 0.19476(15) 0.0863(18) Uani 1 1 d . . . . .
O3 O 0.2325(3) 0.6463(3) 0.18676(17) 0.0913(19) Uani 1 1 d . . . . .
O4 O 0.3960(3) 0.6139(3) 0.33221(15) 0.0684(14) Uani 1 1 d . . . . .
N1 N 0.3797(4) 0.6133(4) 0.14918(19) 0.0714(17) Uani 1 1 d . . . . .
N2 N 0.5432(6) 0.5445(6) 0.0264(3) 0.139(4) Uani 1 1 d . . . . .
N3 N 0.4294(6) 0.4808(6) 0.0098(3) 0.126(3) Uani 1 1 d . . . . .
C13 C 0.4504(6) 0.6189(6) 0.1411(3) 0.102(3) Uani 1 1 d . . . . .
H13 H 0.4791 0.6435 0.1614 0.122 Uiso 1 1 calc R U . . .
C14 C 0.4840(6) 0.5917(6) 0.1059(3) 0.113(4) Uani 1 1 d . . . . .
H14 H 0.5342 0.5974 0.1021 0.135 Uiso 1 1 calc R U . . .
C15 C 0.4429(7) 0.5556(5) 0.0758(3) 0.091(3) Uani 1 1 d . . . . .
C16 C 0.3691(6) 0.5465(5) 0.0834(2) 0.095(3) Uani 1 1 d . . . . .
H16 H 0.3404 0.5196 0.0642 0.113 Uiso 1 1 calc R U . . .
C17 C 0.3383(5) 0.5781(5) 0.1199(3) 0.084(3) Uani 1 1 d . . . . .
H17 H 0.2881 0.5749 0.1242 0.101 Uiso 1 1 calc R U . . .
C18 C 0.4737(8) 0.5249(8) 0.0340(3) 0.117(4) Uani 1 1 d . . . . .
C1 C 0.3705(5) 0.5745(4) 0.3683(3) 0.069(2) Uani 1 1 d . . . . .
C2 C 0.3544(5) 0.5024(6) 0.3629(3) 0.085(3) Uani 1 1 d . . . . .
C3 C 0.3308(6) 0.4613(6) 0.3988(3) 0.110(3) Uani 1 1 d . . . . .
H3 H 0.3194 0.4120 0.3960 0.132 Uiso 1 1 calc R U . . .
N4 N 0.2953(8) 0.4546(7) 0.4748(4) 0.176(5) Uani 1 1 d D . . . .
C5 C 0.3248(6) 0.4963(8) 0.4387(4) 0.114(4) Uani 1 1 d D . . . .
C6 C 0.3663(6) 0.6092(6) 0.4089(2) 0.095(3) Uani 1 1 d . . . . .
C7 C 0.3607(6) 0.4643(5) 0.3187(3) 0.095(3) Uani 1 1 d . . . . .
H7 H 0.3628 0.5033 0.2969 0.113 Uiso 1 1 calc R U . . .
C9 C 0.2983(8) 0.4160(11) 0.3058(5) 0.231(10) Uani 1 1 d . . . . .
H9A H 0.3020 0.3702 0.3209 0.347 Uiso 1 1 calc R U . . .
H9B H 0.3000 0.4074 0.2751 0.347 Uiso 1 1 calc R U . . .
H9C H 0.2530 0.4393 0.3132 0.347 Uiso 1 1 calc R U . . .
C8 C 0.4321(8) 0.4238(9) 0.3155(4) 0.195(7) Uani 1 1 d . . . . .
H8A H 0.4719 0.4577 0.3187 0.293 Uiso 1 1 calc R U . . .
H8B H 0.4353 0.4002 0.2877 0.293 Uiso 1 1 calc R U . . .
H8C H 0.4346 0.3877 0.3381 0.293 Uiso 1 1 calc R U . . .
C10 C 0.3898(7) 0.6876(5) 0.4125(3) 0.113(4) Uani 1 1 d D . . . .
H10 H 0.3887 0.7189 0.3866 0.135 Uiso 0.5 1 calc R U P A 1
C0AA C 0.3427(6) 0.5656(8) 0.4424(3) 0.109(4) Uani 1 1 d . . . . .
H0AA H 0.3392 0.5868 0.4698 0.131 Uiso 1 1 calc R U . . .
C2AA C 0.3708(11) 0.7211(10) 0.4574(4) 0.133(8) Uani 0.635(19) 1 d D U P B 1
H2AA H 0.3187 0.7216 0.4612 0.199 Uiso 0.635(19) 1 calc R U P B 1
H2AB H 0.3892 0.7702 0.4589 0.199 Uiso 0.635(19) 1 calc R U P B 1
H2AC H 0.3928 0.6921 0.4799 0.199 Uiso 0.635(19) 1 calc R U P B 1
C1AA C 0.4438(19) 0.706(2) 0.4498(11) 0.162(7) Uani 0.316(15) 1 d D U P B 1
H1AA H 0.4932 0.7009 0.4394 0.243 Uiso 0.316(15) 1 calc R U P B 1
H2AD H 0.4360 0.6726 0.4735 0.243 Uiso 0.316(15) 1 calc R U P B 1
H2AE H 0.4358 0.7550 0.4594 0.243 Uiso 0.316(15) 1 calc R U P B 1
C2AB C 0.3150(13) 0.728(2) 0.4202(13) 0.19(2) Uani 0.365(19) 1 d D U P B 2
H2AF H 0.2832 0.7188 0.3960 0.283 Uiso 0.365(19) 1 calc R U P B 2
H2AG H 0.3234 0.7793 0.4231 0.283 Uiso 0.365(19) 1 calc R U P B 2
H2AH H 0.2928 0.7093 0.4463 0.283 Uiso 0.365(19) 1 calc R U P B 2
C1AB C 0.4761(8) 0.6896(11) 0.4070(6) 0.162(7) Uani 0.684(15) 1 d D U P B 2
H1AB H 0.4977 0.6520 0.4246 0.243 Uiso 0.684(15) 1 calc R U P B 2
H1AC H 0.4943 0.7365 0.4160 0.243 Uiso 0.684(15) 1 calc R U P B 2
H1AD H 0.4885 0.6814 0.3771 0.243 Uiso 0.684(15) 1 calc R U P B 2
H4A H 0.275(7) 0.489(2) 0.493(3) 0.194 Uiso 1 1 d D U . . .
H4B H 0.331(4) 0.420(5) 0.480(3) 0.194 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O3 1.902(5) . ?
Zn1 O1 1.906(5) . ?
Zn1 O2 1.919(6) . ?
Zn1 N1 2.033(6) . ?
P1 O3 1.476(6) 15_656 ?
P1 O2 1.488(6) 13_576 ?
P1 O1 1.504(5) . ?
P1 O4 1.608(5) . ?
O2 P1 1.488(6) 13_576 ?
O3 P1 1.475(6) 15_656 ?
O4 C1 1.404(9) . ?
N1 C13 1.319(11) . ?
N1 C17 1.341(9) . ?
N2 N3 1.308(10) 9_665 ?
N2 C18 1.341(15) . ?
N3 N2 1.308(10) 9_665 ?
N3 C18 1.363(15) . ?
C13 C14 1.342(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.364(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.378(13) . ?
C15 C18 1.512(12) . ?
C16 C17 1.384(11) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C1 C2 1.360(12) . ?
C1 C6 1.404(11) . ?
C2 C3 1.404(12) . ?
C2 C7 1.533(11) . ?
C3 C5 1.388(15) . ?
C3 H3 0.9300 . ?
N4 C5 1.452(14) . ?
N4 H4A 0.91(2) . ?
N4 H4B 0.92(2) . ?
C5 C0AA 1.313(15) . ?
C6 C0AA 1.372(13) . ?
C6 C10 1.501(13) . ?
C7 C9 1.495(15) . ?
C7 C8 1.503(14) . ?
C7 H7 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 C1AA 1.549(10) . ?
C10 C2AA 1.551(9) . ?
C10 C2AB 1.568(10) . ?
C10 C1AB 1.586(9) . ?
C10 H10 0.9800 . ?
C0AA H0AA 0.9300 . ?
C2AA H2AA 0.9600 . ?
C2AA H2AB 0.9600 . ?
C2AA H2AC 0.9600 . ?
C1AA H1AA 0.9600 . ?
C1AA H2AD 0.9600 . ?
C1AA H2AE 0.9600 . ?
C2AB H2AF 0.9600 . ?
C2AB H2AG 0.9600 . ?
C2AB H2AH 0.9600 . ?
C1AB H1AB 0.9600 . ?
C1AB H1AC 0.9600 . ?
C1AB H1AD 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
O3 Zn1 O1 114.7(2) . . ?
O3 Zn1 O2 119.0(3) . . ?
O1 Zn1 O2 106.8(2) . . ?
O3 Zn1 N1 98.8(3) . . ?
O1 Zn1 N1 114.1(3) . . ?
O2 Zn1 N1 102.8(2) . . ?
O3 P1 O2 114.2(4) 15_656 13_576 ?
O3 P1 O1 114.6(3) 15_656 . ?
O2 P1 O1 111.2(3) 13_576 . ?
O3 P1 O4 107.7(3) 15_656 . ?
O2 P1 O4 104.0(3) 13_576 . ?
O1 P1 O4 103.9(3) . . ?
P1 O1 Zn1 128.5(4) . . ?
P1 O2 Zn1 140.3(4) 13_576 . ?
P1 O3 Zn1 144.7(3) 15_656 . ?
C1 O4 P1 123.9(5) . . ?
C13 N1 C17 117.6(7) . . ?
C13 N1 Zn1 121.8(6) . . ?
C17 N1 Zn1 120.2(6) . . ?
N3 N2 C18 114.6(10) 9_665 . ?
N2 N3 C18 116.6(10) 9_665 . ?
N1 C13 C14 124.8(10) . . ?
N1 C13 H13 117.6 . . ?
C14 C13 H13 117.6 . . ?
C13 C14 C15 118.5(10) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C14 C15 C16 118.8(8) . . ?
C14 C15 C18 123.5(11) . . ?
C16 C15 C18 117.7(11) . . ?
C15 C16 C17 119.1(8) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
N1 C17 C16 121.1(8) . . ?
N1 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
N2 C18 N3 128.8(9) . . ?
N2 C18 C15 113.7(13) . . ?
N3 C18 C15 117.5(13) . . ?
C2 C1 C6 122.4(8) . . ?
C2 C1 O4 118.2(7) . . ?
C6 C1 O4 119.4(8) . . ?
C1 C2 C3 119.2(9) . . ?
C1 C2 C7 122.2(8) . . ?
C3 C2 C7 118.6(10) . . ?
C5 C3 C2 118.3(11) . . ?
C5 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C5 N4 H4A 104(2) . . ?
C5 N4 H4B 104(2) . . ?
H4A N4 H4B 130(10) . . ?
C0AA C5 C3 120.1(10) . . ?
C0AA C5 N4 122.2(13) . . ?
C3 C5 N4 117.6(13) . . ?
C0AA C6 C1 115.1(10) . . ?
C0AA C6 C10 126.1(9) . . ?
C1 C6 C10 118.8(8) . . ?
C9 C7 C8 110.7(11) . . ?
C9 C7 C2 116.5(10) . . ?
C8 C7 C2 110.3(8) . . ?
C9 C7 H7 106.2 . . ?
C8 C7 H7 106.2 . . ?
C2 C7 H7 106.2 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C10 C1AA 116.2(19) . . ?
C6 C10 C2AA 112.2(10) . . ?
C1AA C10 C2AA 53.0(14) . . ?
C6 C10 C2AB 101.9(18) . . ?
C6 C10 C1AB 107.3(11) . . ?
C2AB C10 C1AB 150.7(19) . . ?
C6 C10 H10 119.4 . . ?
C1AA C10 H10 119.4 . . ?
C2AA C10 H10 119.4 . . ?
C5 C0AA C6 124.9(11) . . ?
C5 C0AA H0AA 117.5 . . ?
C6 C0AA H0AA 117.5 . . ?
C10 C2AA H2AA 109.5 . . ?
C10 C2AA H2AB 109.5 . . ?
H2AA C2AA H2AB 109.5 . . ?
C10 C2AA H2AC 109.5 . . ?
H2AA C2AA H2AC 109.5 . . ?
H2AB C2AA H2AC 109.5 . . ?
C10 C1AA H1AA 109.5 . . ?
C10 C1AA H2AD 109.5 . . ?
H1AA C1AA H2AD 109.5 . . ?
C10 C1AA H2AE 109.5 . . ?
H1AA C1AA H2AE 109.5 . . ?
H2AD C1AA H2AE 109.5 . . ?
C10 C2AB H2AF 109.5 . . ?
C10 C2AB H2AG 109.5 . . ?
H2AF C2AB H2AG 109.5 . . ?
C10 C2AB H2AH 109.5 . . ?
H2AF C2AB H2AH 109.5 . . ?
H2AG C2AB H2AH 109.5 . . ?
C10 C1AB H1AB 109.5 . . ?
C10 C1AB H1AC 109.5 . . ?
H1AB C1AB H1AC 109.5 . . ?
C10 C1AB H1AD 109.5 . . ?
H1AB C1AB H1AD 109.5 . . ?
H1AC C1AB H1AD 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 P1 O1 Zn1 70.5(5) 15_656 . . . ?
O2 P1 O1 Zn1 -60.9(5) 13_576 . . . ?
O4 P1 O1 Zn1 -172.2(4) . . . . ?
O3 P1 O4 C1 -4.7(7) 15_656 . . . ?
O2 P1 O4 C1 116.9(6) 13_576 . . . ?
O1 P1 O4 C1 -126.6(6) . . . . ?
C17 N1 C13 C14 -0.3(15) . . . . ?
Zn1 N1 C13 C14 -173.5(9) . . . . ?
N1 C13 C14 C15 0.1(17) . . . . ?
C13 C14 C15 C16 -1.9(16) . . . . ?
C13 C14 C15 C18 177.7(10) . . . . ?
C14 C15 C16 C17 3.8(14) . . . . ?
C18 C15 C16 C17 -175.8(9) . . . . ?
C13 N1 C17 C16 2.3(13) . . . . ?
Zn1 N1 C17 C16 175.6(7) . . . . ?
C15 C16 C17 N1 -4.1(14) . . . . ?
N3 N2 C18 N3 2(2) 9_665 . . . ?
N3 N2 C18 C15 -179.3(8) 9_665 . . . ?
N2 N3 C18 N2 -2(2) 9_665 . . . ?
N2 N3 C18 C15 179.3(9) 9_665 . . . ?
C14 C15 C18 N2 -8.1(15) . . . . ?
C16 C15 C18 N2 171.5(10) . . . . ?
C14 C15 C18 N3 170.6(10) . . . . ?
C16 C15 C18 N3 -9.8(14) . . . . ?
P1 O4 C1 C2 92.7(8) . . . . ?
P1 O4 C1 C6 -90.8(9) . . . . ?
C6 C1 C2 C3 1.9(13) . . . . ?
O4 C1 C2 C3 178.2(7) . . . . ?
C6 C1 C2 C7 -178.6(8) . . . . ?
O4 C1 C2 C7 -2.3(12) . . . . ?
C1 C2 C3 C5 -0.1(14) . . . . ?
C7 C2 C3 C5 -179.7(9) . . . . ?
C2 C3 C5 C0AA -1.6(17) . . . . ?
C2 C3 C5 N4 175.6(10) . . . . ?
C2 C1 C6 C0AA -1.9(14) . . . . ?
O4 C1 C6 C0AA -178.2(8) . . . . ?
C2 C1 C6 C10 175.9(9) . . . . ?
O4 C1 C6 C10 -0.4(13) . . . . ?
C1 C2 C7 C9 -134.5(12) . . . . ?
C3 C2 C7 C9 45.0(15) . . . . ?
C1 C2 C7 C8 98.2(12) . . . . ?
C3 C2 C7 C8 -82.3(13) . . . . ?
C0AA C6 C10 C1AA 47(2) . . . . ?
C1 C6 C10 C1AA -130(2) . . . . ?
C0AA C6 C10 C2AA -11.2(16) . . . . ?
C1 C6 C10 C2AA 171.2(10) . . . . ?
C0AA C6 C10 C2AB -72.5(19) . . . . ?
C1 C6 C10 C2AB 110.0(18) . . . . ?
C0AA C6 C10 C1AB 107.3(13) . . . . ?
C1 C6 C10 C1AB -70.3(12) . . . . ?
C3 C5 C0AA C6 1.6(19) . . . . ?
N4 C5 C0AA C6 -175.4(11) . . . . ?
C1 C6 C0AA C5 0.1(17) . . . . ?
C10 C6 C0AA C5 -177.5(12) . . . . ?

_refine_diff_density_max         0.706
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.083



####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1921274'
loop_
_audit_author_name
_audit_author_address
'Sandeep Kumar Gupta'
;Indian Institute of Technology Bombay, Mumbai
India
;
_audit_update_record             
;
2019-06-05 deposited with the CCDC.	2019-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H20 N O5 P Zn, 2(H2 O), O [+ solvent]'
_chemical_formula_sum            'C14 H24 N O8 P Zn'
_chemical_formula_weight         430.68

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   16.7211(2)
_cell_length_b                   16.7211(2)
_cell_length_c                   15.5352(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4343.57(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    24287
_cell_measurement_theta_min      1.8490
_cell_measurement_theta_max      30.7650

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    1.239
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80128
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49457
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.436
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3810
_reflns_number_gt                3619
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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_cell_refinement       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0645P)²+2.9211P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1614 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3810
_refine_ls_number_parameters     232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1067
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn -0.61770(3) -0.44358(3) -0.59579(4) 0.0264(2) Uani 1 1 d . . . . .
P1 P -0.55004(8) -0.62907(8) -0.60595(9) 0.0277(3) Uani 1 1 d . . . . .
O1 O -0.5877(2) -0.6915(2) -0.6730(3) 0.0302(9) Uani 1 1 d . . . . .
O5 O -0.9111(3) -0.7892(2) -0.8348(3) 0.0373(10) Uani 1 1 d . . . . .
O4 O -0.4616(2) -0.6340(3) -0.6268(3) 0.0459(12) Uani 1 1 d . . . . .
O3 O -0.5679(3) -0.6605(3) -0.5179(3) 0.0469(12) Uani 1 1 d . . . . .
O2 O -0.5865(2) -0.5496(2) -0.6236(3) 0.0367(10) Uani 1 1 d . . . . .
N1 N -0.8892(3) -0.6590(3) -0.8213(5) 0.0490(15) Uani 1 1 d . . . . .
H1 H -0.9076 -0.6115 -0.8288 0.059 Uiso 1 1 calc R U . . .
C5 C -0.8029(4) -0.7136(3) -0.7075(5) 0.0385(15) Uani 1 1 d . . . . .
H5 H -0.8469 -0.7393 -0.6835 0.046 Uiso 1 1 calc R U . . .
C6 C -0.7288(3) -0.7219(3) -0.6695(4) 0.0334(13) Uani 1 1 d . . . . .
C3 C -0.7499(4) -0.6273(4) -0.8166(5) 0.0403(15) Uani 1 1 d . . . . .
H3 H -0.7580 -0.5954 -0.8649 0.048 Uiso 1 1 calc R U . . .
C2 C -0.6731(3) -0.6333(4) -0.7812(4) 0.0352(14) Uani 1 1 d . . . . .
C10 C -0.7184(4) -0.7707(4) -0.5891(5) 0.0435(15) Uani 1 1 d . . . . .
H10 H -0.6610 -0.7773 -0.5786 0.052 Uiso 1 1 calc R U . . .
C1 C -0.6647(3) -0.6812(3) -0.7078(4) 0.0291(12) Uani 1 1 d . . . . .
C4 C -0.8129(3) -0.6673(4) -0.7814(5) 0.0393(15) Uani 1 1 d . . . . .
C13 C -0.9332(4) -0.7199(3) -0.8473(4) 0.0355(14) Uani 1 1 d . . . . .
C11 C -0.7552(5) -0.7250(5) -0.5118(5) 0.0538(19) Uani 1 1 d . . . . .
H11A H -0.7367 -0.6706 -0.5122 0.081 Uiso 1 1 calc R U . . .
H11B H -0.7391 -0.7503 -0.4590 0.081 Uiso 1 1 calc R U . . .
H11C H -0.8124 -0.7258 -0.5162 0.081 Uiso 1 1 calc R U . . .
C7 C -0.6022(4) -0.5940(4) -0.8250(4) 0.0413(15) Uani 1 1 d . . . . .
H7 H -0.5605 -0.5871 -0.7813 0.050 Uiso 1 1 calc R U . . .
C8 C -0.6218(5) -0.5117(5) -0.8604(6) 0.070(2) Uani 1 1 d . . . . .
H8A H -0.6582 -0.5169 -0.9079 0.104 Uiso 1 1 calc R U . . .
H8B H -0.5735 -0.4863 -0.8796 0.104 Uiso 1 1 calc R U . . .
H8C H -0.6461 -0.4799 -0.8161 0.104 Uiso 1 1 calc R U . . .
C14 C -1.0113(3) -0.7024(4) -0.8937(6) 0.0471(18) Uani 1 1 d . . . . .
H14A H -1.0045 -0.7110 -0.9543 0.071 Uiso 1 1 calc R U . . .
H14B H -1.0265 -0.6478 -0.8836 0.071 Uiso 1 1 calc R U . . .
H14C H -1.0524 -0.7373 -0.8723 0.071 Uiso 1 1 calc R U . . .
C12 C -0.7564(5) -0.8535(4) -0.5946(6) 0.064(2) Uani 1 1 d . . . . .
H12A H -0.8121 -0.8483 -0.6087 0.095 Uiso 1 1 calc R U . . .
H12B H -0.7510 -0.8802 -0.5402 0.095 Uiso 1 1 calc R U . . .
H12C H -0.7300 -0.8842 -0.6385 0.095 Uiso 1 1 calc R U . . .
C9 C -0.5683(5) -0.6496(7) -0.8948(7) 0.086(3) Uani 1 1 d . . . . .
H9A H -0.5503 -0.6985 -0.8688 0.129 Uiso 1 1 calc R U . . .
H9B H -0.5242 -0.6238 -0.9230 0.129 Uiso 1 1 calc R U . . .
H9C H -0.6092 -0.6613 -0.9363 0.129 Uiso 1 1 calc R U . . .
O6 O -0.7231(3) -0.8885(3) -0.8268(4) 0.0708(16) Uani 1 1 d G . . . .
H6A H -0.7308 -0.8391 -0.8369 0.106 Uiso 1 1 d G U . . .
H6B H -0.7687 -0.9100 -0.8346 0.106 Uiso 1 1 d G U . . .
O7 O -0.6101(4) -0.9726(5) -0.7227(5) 0.109(3) Uani 1 1 d G . . . .
H7A H -0.6431 -0.9985 -0.7536 0.164 Uiso 1 1 d G U . . .
H7B H -0.6123 -0.9251 -0.7419 0.164 Uiso 1 1 d G U . . .
O8 O -0.5709(6) -0.8852(8) -0.9247(7) 0.153(4) Uani 1 1 d . . . . .


_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 O2 1.898(4) . ?
Zn1 O3 1.916(4) 3_544 ?
Zn1 O4 1.917(4) 2_445 ?
Zn1 O5 1.970(4) 8_353 ?
P1 O2 1.487(4) . ?
P1 O3 1.495(5) . ?
P1 O4 1.516(4) . ?
P1 O1 1.603(4) . ?
O1 C1 1.406(7) . ?
O5 C13 1.230(7) . ?
O5 Zn1 1.970(4) 7_433 ?
O4 Zn1 1.917(4) 2_445 ?
O3 Zn1 1.916(4) 4_454 ?
N1 C13 1.320(8) . ?
N1 C4 1.424(8) . ?
C5 C6 1.380(9) . ?
C5 C4 1.394(10) . ?
C6 C1 1.404(8) . ?
C6 C10 1.501(9) . ?
C3 C4 1.364(9) . ?
C3 C2 1.402(9) . ?
C2 C1 1.400(9) . ?
C2 C7 1.516(9) . ?
C10 C12 1.526(9) . ?
C10 C11 1.552(10) . ?
C13 C14 1.521(9) . ?
C7 C8 1.518(11) . ?
C7 C9 1.537(11) . ?

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 Zn1 O3 113.9(2) . 3_544 ?
O2 Zn1 O4 112.64(19) . 2_445 ?
O3 Zn1 O4 115.0(2) 3_544 2_445 ?
O2 Zn1 O5 110.52(18) . 8_353 ?
O3 Zn1 O5 100.46(18) 3_544 8_353 ?
O4 Zn1 O5 102.88(17) 2_445 8_353 ?
O2 P1 O3 113.6(3) . . ?
O2 P1 O4 114.2(3) . . ?
O3 P1 O4 111.8(3) . . ?
O2 P1 O1 107.5(2) . . ?
O3 P1 O1 106.7(2) . . ?
O4 P1 O1 102.1(2) . . ?
C1 O1 P1 122.0(3) . . ?
C13 O5 Zn1 125.1(4) . 7_433 ?
P1 O4 Zn1 125.7(3) . 2_445 ?
P1 O3 Zn1 133.8(3) . 4_454 ?
P1 O2 Zn1 154.9(3) . . ?
C13 N1 C4 123.8(5) . . ?
C6 C5 C4 121.1(6) . . ?
C5 C6 C1 117.1(6) . . ?
C5 C6 C10 121.0(6) . . ?
C1 C6 C10 121.8(5) . . ?
C4 C3 C2 121.0(7) . . ?
C1 C2 C3 117.0(6) . . ?
C1 C2 C7 122.4(5) . . ?
C3 C2 C7 120.6(6) . . ?
C6 C10 C12 113.5(6) . . ?
C6 C10 C11 109.3(5) . . ?
C12 C10 C11 109.0(6) . . ?
C2 C1 C6 123.1(5) . . ?
C2 C1 O1 118.4(5) . . ?
C6 C1 O1 118.5(5) . . ?
C3 C4 C5 120.7(6) . . ?
C3 C4 N1 118.0(7) . . ?
C5 C4 N1 121.3(6) . . ?
O5 C13 N1 120.7(6) . . ?
O5 C13 C14 120.9(5) . . ?
N1 C13 C14 118.4(5) . . ?
C2 C7 C8 112.8(6) . . ?
C2 C7 C9 110.1(6) . . ?
C8 C7 C9 111.8(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P1 O1 C1 -27.9(5) . . . . ?
O3 P1 O1 C1 94.2(5) . . . . ?
O4 P1 O1 C1 -148.4(4) . . . . ?
O2 P1 O4 Zn1 46.1(5) . . . 2_445 ?
O3 P1 O4 Zn1 -84.6(4) . . . 2_445 ?
O1 P1 O4 Zn1 161.7(3) . . . 2_445 ?
O2 P1 O3 Zn1 -52.8(5) . . . 4_454 ?
O4 P1 O3 Zn1 78.2(5) . . . 4_454 ?
O1 P1 O3 Zn1 -171.0(4) . . . 4_454 ?
O3 P1 O2 Zn1 40.2(8) . . . . ?
O4 P1 O2 Zn1 -89.6(7) . . . . ?
O1 P1 O2 Zn1 158.0(6) . . . . ?
O3 Zn1 O2 P1 -40.6(7) 3_544 . . . ?
O4 Zn1 O2 P1 92.7(7) 2_445 . . . ?
O5 Zn1 O2 P1 -152.8(6) 8_353 . . . ?
C4 C5 C6 C1 0.7(9) . . . . ?
C4 C5 C6 C10 179.0(6) . . . . ?
C4 C3 C2 C1 -0.9(9) . . . . ?
C4 C3 C2 C7 175.0(6) . . . . ?
C5 C6 C10 C12 49.4(9) . . . . ?
C1 C6 C10 C12 -132.4(7) . . . . ?
C5 C6 C10 C11 -72.5(7) . . . . ?
C1 C6 C10 C11 105.8(7) . . . . ?
C3 C2 C1 C6 -0.2(8) . . . . ?
C7 C2 C1 C6 -176.0(5) . . . . ?
C3 C2 C1 O1 177.1(5) . . . . ?
C7 C2 C1 O1 1.3(8) . . . . ?
C5 C6 C1 C2 0.3(8) . . . . ?
C10 C6 C1 C2 -178.0(6) . . . . ?
C5 C6 C1 O1 -177.0(5) . . . . ?
C10 C6 C1 O1 4.7(8) . . . . ?
P1 O1 C1 C2 85.8(6) . . . . ?
P1 O1 C1 C6 -96.8(5) . . . . ?
C2 C3 C4 C5 1.9(9) . . . . ?
C2 C3 C4 N1 -179.4(6) . . . . ?
C6 C5 C4 C3 -1.8(9) . . . . ?
C6 C5 C4 N1 179.6(6) . . . . ?
C13 N1 C4 C3 125.5(7) . . . . ?
C13 N1 C4 C5 -55.9(10) . . . . ?
Zn1 O5 C13 N1 -155.0(5) 7_433 . . . ?
Zn1 O5 C13 C14 24.5(9) 7_433 . . . ?
C4 N1 C13 O5 3.1(11) . . . . ?
C4 N1 C13 C14 -176.5(7) . . . . ?
C1 C2 C7 C8 -143.7(7) . . . . ?
C3 C2 C7 C8 40.6(8) . . . . ?
C1 C2 C7 C9 90.6(8) . . . . ?
C3 C2 C7 C9 -85.1(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C14 H14A O3 0.96 2.66 3.277(9) 122.7 6_334
O6 H6B O4 0.85 1.94 2.779(7) 169.9 8_343
O7 H7B O6 0.85 2.36 2.858 118.3 .

_refine_diff_density_max         0.385
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.070



