# Electronic Supplementary Material (ESI) for Materials Advances.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_ZOLE_Zn_form_2
_database_code_depnum_ccdc_archive 'CCDC 2120915'
loop_
_audit_author_name
_audit_author_address
'Vilmali Lopez-Mejias'
;University of Puerto Rico, Rio Piedras
Puerto Rico
;
_audit_update_record             
;
2021-11-08 deposited with the CCDC.	2022-02-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_ZOLE_Zn_form_2      
;
PROBLEM: Short Inter D-H..H-D       H9A      ..H9A      .       1.49 Ang.
RESPONSE: A high degree of disorder is presenetd by O9 (uncoordinated water molecule) wich hampers correct assigment of short contacts. 
;
_vrf_PLAT415_ZOLE_Zn_form_2      
;
PROBLEM: Short Inter D-H..H-X       H3       ..H9A      .       2.08 Ang.
RESPONSE: A high degree of disorder is presenetd by O9 (uncoordinated water molecule) wich hampers correct assigment of short contacts. 
;
# Added during the CSD deposition process: Monday 08 November 2021 06:37 PM
# end Validation Reply Form

_audit_creation_date             2020-03-28
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_chemical_name_common            ?
_chemical_name_systematic        'Zole-Zn form II'
_chemical_formula_moiety         'C10 H18 N4 O14 P4 Zn, 4(H2 O)'
_chemical_formula_sum            'C10 H26 N4 O18 P4 Zn'
_chemical_formula_weight         679.60
_chemical_melting_point          561.82
_chemical_oxdiff_formula         ZnC8H10N2O7P2
_chemical_oxdiff_usercomment     ZOLE_Zn_form_2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   4.96680(10)
_cell_length_b                   16.4043(3)
_cell_length_c                   14.4177(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.452(2)
_cell_angle_gamma                90
_cell_volume                     1172.58(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5634
_cell_measurement_temperature    101(1)
_cell_measurement_theta_max      68.7500
_cell_measurement_theta_min      4.0740
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.15e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11322
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.175
_diffrn_reflns_theta_min         4.086
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  45.00   0.50    3.00    --   11.59  82.00  69.00  118
  2  ω    -44.00  38.00   0.50    3.00    --   11.59 -82.00 -52.00  164
  3  ω     31.00 122.00   0.50   12.50    --   96.16 -82.00 -52.00  182
  4  ω     80.00 157.00   0.50   12.50    --   96.16  82.00  69.00  154
  5  ω    -45.00  15.00   0.50    3.00    --  -11.59 -82.00 -52.00  120
  6  ω    -20.00  55.00   0.50    3.00    --  -11.59  30.00  30.00  150
  7  ω    -37.00  53.00   0.50    3.00    --  -11.59  77.00   0.00  180
  8  ω    -37.00  45.00   0.50    3.00    --  -11.59  82.00  69.00  164
  9  ω      3.00  60.00   0.50    3.00    --   11.59-125.00-180.00  114
 10  ω     -2.00  74.00   0.50    3.00    --   11.59  45.00-150.00  152
 11  ω    -51.00  26.00   0.50    3.00    --   11.59 -45.00-120.00  154
 12  ω      3.00  60.00   0.50    3.00    --   11.59-125.00-150.00  114
 13  ω     30.00 124.00   0.50   12.50    --   96.16 -87.00  90.00  188
 14  ω     31.00 105.00   0.50   12.50    --   96.16 -33.00 -90.00  148
 15  ω     32.00 117.00   0.50   12.50    --   96.16-117.00 -60.00  170
 16  ω     75.00 157.00   0.50   12.50    --   96.16  68.00   0.00  164
 17  ω     82.00 157.00   0.50   12.50    --   96.16  17.00 120.00  150
 18  ω     78.00 157.00   0.50   12.50    --   96.16  59.00-150.00  158
 19  ω     71.00 157.00   0.50   12.50    --   96.16  77.00 -30.00  172
 20  ω     71.00 157.00   0.50   12.50    --   96.16  77.00  30.00  172
 21  ω     28.00 105.00   0.50   12.50    --   96.16 -25.00  60.00  154
 22  ω     88.00 157.00   0.50   12.50    --   96.16  25.00 -60.00  138
 23  ω     82.00 157.00   0.50   12.50    --   96.16  17.00-180.00  150
 24  ω    -83.00   5.00   0.50    3.00    --  -11.59 -15.00-150.00  176
 25  ω    -75.00   8.00   0.50    3.00    --  -11.59 -61.00  60.00  166
 26  ω    -83.00   5.00   0.50    3.00    --  -11.59 -15.00 -60.00  176
 27  ω    -75.00   8.00   0.50    3.00    --  -11.59 -61.00 -30.00  166
 28  ω      3.00  60.00   0.50    3.00    --   11.59-125.00 -60.00  114
 29  ω     -8.00  75.00   0.50    3.00    --   11.59  61.00 -60.00  166
 30  ω    -14.00  76.00   0.50    3.00    --   11.59  77.00-120.00  180
 31  ω      3.00  60.00   0.50    3.00    --   11.59-125.00  60.00  114
 32  ω    -52.00  31.00   0.50    3.00    --   11.59 -61.00-180.00  166
 33  ω     71.00 157.00   0.50   12.50    --   96.16  77.00 120.00  172
 34  ω     71.00 157.00   0.50   12.50    --   96.16  77.00 -60.00  172
 35  ω     71.00 157.00   0.50   12.50    --   96.16  77.00-180.00  172
 36  ω     33.00 115.00   0.50   12.50    --   96.16 -59.00  90.00  164
 37  ω     32.00 117.00   0.50   12.50    --   96.16-117.00 -90.00  170
 38  ω     75.00 157.00   0.50   12.50    --   96.16  68.00-120.00  164
 39  ω     71.00 157.00   0.50   12.50    --   96.16  77.00  60.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0740806000
_diffrn_orient_matrix_UB_12      0.0804428000
_diffrn_orient_matrix_UB_13      0.0474611000
_diffrn_orient_matrix_UB_21      -0.2339005000
_diffrn_orient_matrix_UB_22      0.0127009000
_diffrn_orient_matrix_UB_23      -0.0737270000
_diffrn_orient_matrix_UB_31      -0.1906345000
_diffrn_orient_matrix_UB_32      -0.0467960000
_diffrn_orient_matrix_UB_33      0.0614031000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1925
_reflns_number_total             2152
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2152
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0511
_refine_ls_restrained_S_all      1.108
_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)+(0.0620P)²+4.2160P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1321
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O9(H9A,H9B), O8(H8A,H8B)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2B,H2C)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2A), C3(H3), C4(H4), C5(H5A)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O5(H5), O7(H7)
;
_atom_sites_solution_hydrogens   mixed
_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 1.000000 0.500000 0.500000 0.0145(2) Uani 1 2 d S T P . .
P1 P 0.5099(2) 0.47473(6) 0.34615(7) 0.0135(3) Uani 1 1 d . . . . .
P2 P 0.7421(2) 0.64623(6) 0.36691(7) 0.0121(3) Uani 1 1 d . . . . .
O1 O 0.7245(6) 0.43991(17) 0.41184(19) 0.0151(6) Uani 1 1 d . . . . .
O2 O 0.4345(6) 0.41035(17) 0.2663(2) 0.0175(6) Uani 1 1 d . . . . .
H2 H 0.572146 0.395629 0.242478 0.026 Uiso 1 1 calc GR . . . .
O3 O 0.2526(6) 0.50236(18) 0.3839(2) 0.0186(7) Uani 1 1 d . . . . .
O4 O 0.8417(6) 0.61143(16) 0.4587(2) 0.0160(6) Uani 1 1 d . . . . .
O5 O 0.9738(6) 0.69525(17) 0.3211(2) 0.0159(6) Uani 1 1 d . . . . .
H5 H 1.116931 0.687940 0.351297 0.024 Uiso 1 1 calc GR . . . .
O6 O 0.5013(6) 0.70198(16) 0.3658(2) 0.0149(6) Uani 1 1 d . . . . .
O7 O 0.8949(6) 0.52971(17) 0.2451(2) 0.0171(6) Uani 1 1 d . . . . .
H7 H 1.010421 0.519802 0.286588 0.026 Uiso 1 1 calc GR . . . .
N1 N 0.5750(8) 0.6571(2) 0.1510(2) 0.0172(8) Uani 1 1 d . . . . .
N2 N 0.6205(11) 0.7773(2) 0.0959(3) 0.0366(11) Uani 1 1 d . . . . .
H2A H 0.595675 0.828397 0.085043 0.044 Uiso 1 1 calc R . . . .
C1 C 0.6601(8) 0.5616(2) 0.2846(3) 0.0127(8) Uani 1 1 d . . . . .
C2 C 0.4673(8) 0.5885(2) 0.2032(3) 0.0146(8) Uani 1 1 d . . . . .
H2B H 0.434109 0.542764 0.161401 0.017 Uiso 1 1 calc R . . . .
H2C H 0.296213 0.604360 0.226861 0.017 Uiso 1 1 calc R . . . .
C3 C 0.7857(10) 0.6543(3) 0.0938(3) 0.0236(10) Uani 1 1 d . . . . .
H3 H 0.889940 0.608858 0.081571 0.028 Uiso 1 1 calc R . . . .
C4 C 0.8132(12) 0.7303(3) 0.0584(3) 0.0329(12) Uani 1 1 d . . . . .
H4 H 0.938380 0.747053 0.016943 0.039 Uiso 1 1 calc R . . . .
C5 C 0.4785(11) 0.7328(3) 0.1509(3) 0.0271(11) Uani 1 1 d . . . . .
H5A H 0.335340 0.751052 0.184064 0.032 Uiso 1 1 calc R . . . .
O9 O 0.7493(10) 0.9600(2) 0.4875(3) 0.0416(10) Uani 1 1 d . . . . .
H9A H 0.618129 0.991376 0.472001 0.062 Uiso 1 1 d G . . . .
H9B H 0.769971 0.925649 0.444375 0.062 Uiso 1 1 d G . . . .
O8 O 0.8687(7) 0.36147(19) 0.1742(2) 0.0252(7) Uani 1 1 d . . . . .
H8A H 0.900570 0.311741 0.162387 0.038 Uiso 1 1 d G . . . .
H8B H 1.012968 0.384341 0.195549 0.038 Uiso 1 1 d G . . . .


_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 2.062(3) 3_766 ?
Zn1 O1 2.062(3) . ?
Zn1 O3 2.152(3) 1_655 ?
Zn1 O3 2.152(3) 3_666 ?
Zn1 O4 2.063(3) . ?
Zn1 O4 2.063(3) 3_766 ?
P1 O1 1.496(3) . ?
P1 O2 1.590(3) . ?
P1 O3 1.489(3) . ?
P1 C1 1.859(4) . ?
P2 O4 1.498(3) . ?
P2 O5 1.581(3) . ?
P2 O6 1.505(3) . ?
P2 C1 1.856(4) . ?
O2 H2 0.8200 . ?
O5 H5 0.8200 . ?
O7 H7 0.8200 . ?
O7 C1 1.428(5) . ?
N1 C2 1.472(5) . ?
N1 C3 1.372(6) . ?
N1 C5 1.331(6) . ?
N2 H2A 0.8600 . ?
N2 C4 1.365(8) . ?
N2 C5 1.314(7) . ?
C1 C2 1.535(5) . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 H3 0.9300 . ?
C3 C4 1.358(7) . ?
C4 H4 0.9300 . ?
C5 H5A 0.9300 . ?
O9 H9A 0.8498 . ?
O9 H9B 0.8503 . ?
O8 H8A 0.8502 . ?
O8 H8B 0.8497 . ?

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 180.0 3_766 . ?
O1 Zn1 O3 94.28(12) . 3_666 ?
O1 Zn1 O3 94.28(12) 3_766 1_655 ?
O1 Zn1 O3 85.72(12) . 1_655 ?
O1 Zn1 O3 85.72(12) 3_766 3_666 ?
O1 Zn1 O4 91.05(11) 3_766 3_766 ?
O1 Zn1 O4 88.95(11) . 3_766 ?
O1 Zn1 O4 88.95(11) 3_766 . ?
O1 Zn1 O4 91.05(11) . . ?
O3 Zn1 O3 180.0 1_655 3_666 ?
O4 Zn1 O3 90.61(11) 3_766 1_655 ?
O4 Zn1 O3 90.61(11) . 3_666 ?
O4 Zn1 O3 89.39(11) . 1_655 ?
O4 Zn1 O3 89.39(11) 3_766 3_666 ?
O4 Zn1 O4 180.0 3_766 . ?
O1 P1 O2 109.42(16) . . ?
O1 P1 C1 107.68(17) . . ?
O2 P1 C1 104.33(17) . . ?
O3 P1 O1 118.65(18) . . ?
O3 P1 O2 107.25(18) . . ?
O3 P1 C1 108.60(18) . . ?
O4 P2 O5 110.69(17) . . ?
O4 P2 O6 117.45(17) . . ?
O4 P2 C1 109.14(17) . . ?
O5 P2 C1 104.51(17) . . ?
O6 P2 O5 106.53(16) . . ?
O6 P2 C1 107.71(17) . . ?
P1 O1 Zn1 128.98(17) . . ?
P1 O2 H2 109.5 . . ?
P1 O3 Zn1 146.28(18) . 1_455 ?
P2 O4 Zn1 133.83(17) . . ?
P2 O5 H5 109.5 . . ?
C1 O7 H7 109.5 . . ?
C3 N1 C2 126.5(4) . . ?
C5 N1 C2 124.9(4) . . ?
C5 N1 C3 108.6(4) . . ?
C4 N2 H2A 125.1 . . ?
C5 N2 H2A 125.1 . . ?
C5 N2 C4 109.8(4) . . ?
P2 C1 P1 110.3(2) . . ?
O7 C1 P1 105.7(3) . . ?
O7 C1 P2 112.1(3) . . ?
O7 C1 C2 106.7(3) . . ?
C2 C1 P1 109.6(3) . . ?
C2 C1 P2 112.1(3) . . ?
N1 C2 C1 112.4(3) . . ?
N1 C2 H2B 109.1 . . ?
N1 C2 H2C 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C1 C2 H2C 109.1 . . ?
H2B C2 H2C 107.9 . . ?
N1 C3 H3 126.5 . . ?
C4 C3 N1 107.0(4) . . ?
C4 C3 H3 126.5 . . ?
N2 C4 H4 126.8 . . ?
C3 C4 N2 106.4(5) . . ?
C3 C4 H4 126.8 . . ?
N1 C5 H5A 125.9 . . ?
N2 C5 N1 108.2(5) . . ?
N2 C5 H5A 125.9 . . ?
H9A O9 H9B 109.4 . . ?
H8A O8 H8B 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
P1 C1 C2 N1 -179.7(3) . . . . ?
P2 C1 C2 N1 57.4(4) . . . . ?
O1 P1 O3 Zn1 -14.5(4) . . . 1_455 ?
O1 P1 C1 P2 -67.3(2) . . . . ?
O1 P1 C1 O7 54.1(3) . . . . ?
O1 P1 C1 C2 168.8(3) . . . . ?
O2 P1 O1 Zn1 156.7(2) . . . . ?
O2 P1 O3 Zn1 110.0(3) . . . 1_455 ?
O2 P1 C1 P2 176.53(19) . . . . ?
O2 P1 C1 O7 -62.1(3) . . . . ?
O2 P1 C1 C2 52.6(3) . . . . ?
O3 P1 O1 Zn1 -79.9(3) . . . . ?
O3 P1 C1 P2 62.4(2) . . . . ?
O3 P1 C1 O7 -176.2(2) . . . . ?
O3 P1 C1 C2 -61.6(3) . . . . ?
O4 P2 C1 P1 37.0(3) . . . . ?
O4 P2 C1 O7 -80.5(3) . . . . ?
O4 P2 C1 C2 159.5(3) . . . . ?
O5 P2 O4 Zn1 -94.4(3) . . . . ?
O5 P2 C1 P1 155.46(19) . . . . ?
O5 P2 C1 O7 37.9(3) . . . . ?
O5 P2 C1 C2 -82.1(3) . . . . ?
O6 P2 O4 Zn1 142.9(2) . . . . ?
O6 P2 C1 P1 -91.5(2) . . . . ?
O6 P2 C1 O7 151.0(3) . . . . ?
O6 P2 C1 C2 31.0(3) . . . . ?
O7 C1 C2 N1 -65.7(4) . . . . ?
N1 C3 C4 N2 0.6(6) . . . . ?
C1 P1 O1 Zn1 43.9(3) . . . . ?
C1 P1 O3 Zn1 -137.8(3) . . . 1_455 ?
C1 P2 O4 Zn1 20.0(3) . . . . ?
C2 N1 C3 C4 178.6(4) . . . . ?
C2 N1 C5 N2 -179.0(4) . . . . ?
C3 N1 C2 C1 71.1(5) . . . . ?
C3 N1 C5 N2 0.0(5) . . . . ?
C4 N2 C5 N1 0.4(6) . . . . ?
C5 N1 C2 C1 -110.0(5) . . . . ?
C5 N1 C3 C4 -0.4(5) . . . . ?
C5 N2 C4 C3 -0.6(6) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.305
_oxdiff_exptl_absorpt_empirical_full_min 0.775
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_ZOLE_Mg_form_2
_database_code_depnum_ccdc_archive 'CCDC 2120916'
loop_
_audit_author_name
_audit_author_address
'Vilmali Lopez-Mejias'
;University of Puerto Rico, Rio Piedras
Puerto Rico
;
_audit_update_record             
;
2021-11-08 deposited with the CCDC.	2022-02-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_ZOLE_Mg_form_2      
;
PROBLEM: Short Inter D-H..H-D       H9A      ..H9A      .       1.47 Ang.
RESPONSE: A high degree of disorder is presenetd by O9 (uncoordinated water molecule) wich hampers correct assigment of short contacts. 
;
_vrf_PLAT415_ZOLE_Mg_form_2      
;
PROBLEM: Short Inter D-H..H-X       H5       ..H9A      .       2.03 Ang.
RESPONSE: A high degree of disorder is presenetd by O9 (uncoordinated water molecule) wich hampers correct assigment of short contacts. 
;
# Added during the CSD deposition process: Monday 08 November 2021 06:42 PM
# end Validation Reply Form

_audit_creation_date             2021-07-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Zole-Mg form II'
_chemical_formula_moiety         'C10 H18 Mg N4 O14 P4, 4(H2 O)'
_chemical_formula_sum            'C10 H26 Mg N4 O18 P4'
_chemical_formula_weight         638.54
_chemical_melting_point          566.67
_chemical_oxdiff_formula         MgC5H10N2O7P2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   4.96400(10)
_cell_length_b                   16.3671(3)
_cell_length_c                   14.4253(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.241(2)
_cell_angle_gamma                90
_cell_volume                     1170.13(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8185
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.8010
_cell_measurement_theta_min      3.0830
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65636
_exptl_absorpt_correction_type   multi-scan
_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   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.0336
_exptl_crystal_size_min          0.0245
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11655
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.593
_diffrn_reflns_theta_min         4.089
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -81.00  13.00   0.50    0.50    --  -41.89 107.00-165.00  188
  2  ω     79.00 158.00   0.50    1.78    --   96.54 107.00-165.00  158
  3  ω     26.00 112.00   0.50    1.78    --   96.54-107.00  96.00  172
  4  ω   -110.00 -30.00   0.50    0.50    --  -41.89 -32.00 -30.00  160
  5  ω   -107.00 -19.00   0.50    0.50    --  -41.89 -65.00-150.00  176
  6  ω     26.00 107.00   0.50    0.50    --   41.89  43.00 120.00  162
  7  ω    -34.00  74.00   0.50    0.50    --   41.89 -11.00  30.00  216
  8  ω     26.00 107.00   0.50    0.50    --   41.89  43.00-150.00  162
  9  ω    -13.00  81.00   0.50    0.50    --   41.89-107.00  96.00  188
 10  ω     30.00 110.00   0.50    0.50    --   41.89  32.00 -90.00  160
 11  ω     77.00 158.00   0.50    1.78    --   96.54  50.00 120.00  162
 12  ω     61.00 158.00   0.50    1.78    --   96.54 145.00 -30.00  194
 13  ω     31.00 112.00   0.50    1.78    --   96.54 -42.00   0.00  162
 14  ω     23.00 118.00   0.50    1.78    --   96.54 -17.00  30.00  190
 15  ω     29.00 109.00   0.50    1.78    --   96.54 -33.00 150.00  160
 16  ω     77.00 158.00   0.50    1.78    --   96.54  50.00-180.00  162
 17  ω     84.00 158.00   0.50    1.78    --   96.54  33.00   0.00  148
 18  ω     61.00 158.00   0.50    1.78    --   96.54 145.00 120.00  194
 19  ω     84.00 158.00   0.50    1.78    --   96.54  33.00-180.00  148
 20  ω     30.00 123.00   0.50    1.78    --   96.54 -77.00  90.00  186
 21  ω     23.00 110.00   0.50    1.78    --   96.54 -96.00 -90.00  174
 22  ω     15.00 108.00   0.50    0.50    --   41.89  77.00 -30.00  186
 23  ω    -23.00  61.00   0.50    0.50    --   41.89 -54.00 -90.00  168
 24  ω     22.00 107.00   0.50    0.50    --   41.89  54.00 -30.00  170
 25  ω     15.00 108.00   0.50    0.50    --   41.89  77.00  30.00  186
 26  ω     15.00 108.00   0.50    0.50    --   41.89  77.00  60.00  186
 27  ω     15.00 108.00   0.50    0.50    --   41.89  77.00-150.00  186
 28  ω    -23.00  58.00   0.50    0.50    --   41.89 -43.00 120.00  162
 29  ω     19.00 107.00   0.50    0.50    --   41.89  65.00 150.00  176
 30  ω     31.00 106.00   0.50    1.78    --   96.54 -59.00 -90.00  150
 31  ω     84.00 158.00   0.50    1.78    --   96.54  25.00 -60.00  148
 32  ω     73.00 158.00   0.50    1.78    --   96.54  68.00  60.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0715572000
_diffrn_orient_matrix_UB_12      0.0758013000
_diffrn_orient_matrix_UB_13      0.0569743000
_diffrn_orient_matrix_UB_21      0.0255385000
_diffrn_orient_matrix_UB_22      -0.0511086000
_diffrn_orient_matrix_UB_23      0.0897537000
_diffrn_orient_matrix_UB_31      0.3014134000
_diffrn_orient_matrix_UB_32      0.0223128000
_diffrn_orient_matrix_UB_33      0.0119488000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2010
_reflns_number_total             2146
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.662
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.289
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_gt           0.1210
_refine_ls_restrained_S_all      1.094
_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)+(0.1201P)²+53.8326P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3380
_refine_ls_wR_factor_ref         0.3388
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H,H) groups
2.a Free rotating group:
 O8(H3,H4,H8A,H8B), O9(H9A,H9B)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3A), C4(H4A), C5(H5)
2.d Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_atom_sites_solution_hydrogens   mixed
_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
P1 P 0.7427(5) 0.64627(14) 0.36708(17) 0.0110(7) Uani 1 1 d . . . . .
P2 P 0.5086(5) 0.47498(14) 0.34747(17) 0.0110(7) Uani 1 1 d . . . . .
Mg1 Mg 1.000000 0.500000 0.500000 0.0107(10) Uani 1 2 d S . P . .
O1 O 0.8448(15) 0.6105(4) 0.4578(5) 0.0139(15) Uani 1 1 d . . . . .
O2 O 0.5023(15) 0.7025(4) 0.3668(5) 0.0144(15) Uani 1 1 d . . . . .
O3 O 0.9738(15) 0.6956(4) 0.3205(5) 0.0144(15) Uani 1 1 d . . . . .
O4 O 0.8966(15) 0.5289(4) 0.2455(5) 0.0145(15) Uani 1 1 d . . . . .
O5 O 0.7273(13) 0.4410(4) 0.4129(5) 0.0109(14) Uani 1 1 d . . . . .
O6 O 0.2491(15) 0.5006(4) 0.3852(5) 0.0169(16) Uani 1 1 d . . . . .
O7 O 0.4335(15) 0.4103(4) 0.2678(5) 0.0149(15) Uani 1 1 d . . . . .
H7 H 0.572171 0.390415 0.249161 0.022 Uiso 1 1 calc R U . . .
N1 N 0.5777(18) 0.6569(5) 0.1515(6) 0.0126(17) Uani 1 1 d . . . . .
N2 N 0.622(2) 0.7784(6) 0.0968(7) 0.029(2) Uani 1 1 d . . . . .
H2 H 0.596051 0.829532 0.085822 0.035 Uiso 1 1 calc R U . . .
C1 C 0.658(2) 0.5610(6) 0.2848(7) 0.013(2) Uani 1 1 d . . . . .
C2 C 0.467(2) 0.5880(6) 0.2033(7) 0.015(2) Uani 1 1 d . . . . .
H2A H 0.434528 0.542164 0.161437 0.018 Uiso 1 1 calc R U . . .
H2B H 0.295229 0.603985 0.226631 0.018 Uiso 1 1 calc R U . . .
C3 C 0.481(2) 0.7328(7) 0.1516(7) 0.020(2) Uani 1 1 d . . . . .
H3A H 0.336717 0.750624 0.184851 0.024 Uiso 1 1 calc R U . . .
C4 C 0.818(3) 0.7309(7) 0.0602(8) 0.028(3) Uani 1 1 d . . . . .
H4A H 0.945126 0.748090 0.019519 0.033 Uiso 1 1 calc R U . . .
C5 C 0.791(3) 0.6543(7) 0.0945(8) 0.022(2) Uani 1 1 d . . . . .
H5 H 0.896230 0.609055 0.081927 0.027 Uiso 1 1 calc R U . . .
O8 O 0.8635(17) 0.3617(4) 0.1737(5) 0.0220(18) Uani 1 1 d G . . . .
H3 H 1.170100 0.690701 0.351095 0.033 Uiso 1 1 d G U . . .
H4 H 1.009231 0.525004 0.293978 0.033 Uiso 1 1 d G U . . .
H8A H 0.857489 0.309810 0.172847 0.033 Uiso 1 1 d G U . . .
H8B H 1.026480 0.372849 0.190096 0.033 Uiso 1 1 d G U . . .
O9 O 0.750(2) 0.4600(6) 0.0121(6) 0.040(3) Uani 1 1 d G . . . .
H9A H 0.863809 0.498772 0.017471 0.060 Uiso 1 1 d G U . . .
H9B H 0.768633 0.434374 0.063318 0.060 Uiso 1 1 d G 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
P1 O1 1.496(7) . ?
P1 O2 1.507(7) . ?
P1 O3 1.583(8) . ?
P1 C1 1.865(11) . ?
P2 O5 1.504(7) . ?
P2 O6 1.487(7) . ?
P2 O7 1.592(7) . ?
P2 C1 1.851(10) . ?
Mg1 O1 2.044(7) 3_766 ?
Mg1 O1 2.044(7) . ?
Mg1 O5 2.038(7) . ?
Mg1 O5 2.038(7) 3_766 ?
Mg1 O6 2.122(7) 3_666 ?
Mg1 O6 2.122(7) 1_655 ?
O3 H3 1.0500 . ?
O4 C1 1.442(12) . ?
O4 H4 0.8726 . ?
O7 H7 0.8200 . ?
N1 C2 1.476(13) . ?
N1 C3 1.332(14) . ?
N1 C5 1.378(14) . ?
N2 H2 0.8600 . ?
N2 C3 1.318(16) . ?
N2 C4 1.373(18) . ?
C1 C2 1.532(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C4 C5 1.356(16) . ?
C5 H5 0.9300 . ?
O8 H8A 0.8500 . ?
O8 H8B 0.8499 . ?
O9 H9A 0.8500 . ?
O9 H9B 0.8501 . ?

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 P1 O2 118.1(4) . . ?
O1 P1 O3 110.7(4) . . ?
O1 P1 C1 108.5(4) . . ?
O2 P1 O3 106.3(4) . . ?
O2 P1 C1 107.7(4) . . ?
O3 P1 C1 104.7(4) . . ?
O5 P2 O7 109.8(4) . . ?
O5 P2 C1 107.1(4) . . ?
O6 P2 O5 118.9(4) . . ?
O6 P2 O7 106.2(4) . . ?
O6 P2 C1 110.1(4) . . ?
O7 P2 C1 103.7(4) . . ?
O1 Mg1 O1 180.0 . 3_766 ?
O1 Mg1 O6 90.6(3) 3_766 1_655 ?
O1 Mg1 O6 89.4(3) . 1_655 ?
O1 Mg1 O6 89.4(3) 3_766 3_666 ?
O1 Mg1 O6 90.6(3) . 3_666 ?
O5 Mg1 O1 89.5(3) . 3_766 ?
O5 Mg1 O1 89.5(3) 3_766 . ?
O5 Mg1 O1 90.5(3) 3_766 3_766 ?
O5 Mg1 O1 90.5(3) . . ?
O5 Mg1 O5 180.0 3_766 . ?
O5 Mg1 O6 85.2(3) . 1_655 ?
O5 Mg1 O6 85.2(3) 3_766 3_666 ?
O5 Mg1 O6 94.8(3) 3_766 1_655 ?
O5 Mg1 O6 94.8(3) . 3_666 ?
O6 Mg1 O6 180.0 3_666 1_655 ?
P1 O1 Mg1 135.2(4) . . ?
P1 O3 H3 117.4 . . ?
C1 O4 H4 102.5 . . ?
P2 O5 Mg1 130.0(4) . . ?
P2 O6 Mg1 147.1(4) . 1_455 ?
P2 O7 H7 109.5 . . ?
C3 N1 C2 124.5(9) . . ?
C3 N1 C5 108.6(9) . . ?
C5 N1 C2 126.9(9) . . ?
C3 N2 H2 125.6 . . ?
C3 N2 C4 108.8(10) . . ?
C4 N2 H2 125.6 . . ?
P2 C1 P1 109.9(5) . . ?
O4 C1 P1 111.2(7) . . ?
O4 C1 P2 106.0(6) . . ?
O4 C1 C2 106.9(8) . . ?
C2 C1 P1 112.4(7) . . ?
C2 C1 P2 110.3(7) . . ?
N1 C2 C1 112.1(8) . . ?
N1 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N1 C3 H3A 125.6 . . ?
N2 C3 N1 108.8(10) . . ?
N2 C3 H3A 125.6 . . ?
N2 C4 H4A 126.4 . . ?
C5 C4 N2 107.3(11) . . ?
C5 C4 H4A 126.4 . . ?
N1 C5 H5 126.8 . . ?
C4 C5 N1 106.5(11) . . ?
C4 C5 H5 126.8 . . ?
H8A O8 H8B 104.5 . . ?
H9A O9 H9B 104.5 . . ?

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
P1 C1 C2 N1 56.7(10) . . . . ?
P2 C1 C2 N1 179.7(7) . . . . ?
O1 P1 C1 P2 37.4(6) . . . . ?
O1 P1 C1 O4 -79.6(7) . . . . ?
O1 P1 C1 C2 160.6(7) . . . . ?
O2 P1 O1 Mg1 142.3(6) . . . . ?
O2 P1 C1 P2 -91.5(5) . . . . ?
O2 P1 C1 O4 151.5(6) . . . . ?
O2 P1 C1 C2 31.7(8) . . . . ?
O3 P1 O1 Mg1 -94.9(7) . . . . ?
O3 P1 C1 P2 155.6(5) . . . . ?
O3 P1 C1 O4 38.6(7) . . . . ?
O3 P1 C1 C2 -81.1(8) . . . . ?
O4 C1 C2 N1 -65.5(10) . . . . ?
O5 P2 O6 Mg1 -11.4(11) . . . 1_455 ?
O5 P2 C1 P1 -66.9(6) . . . . ?
O5 P2 C1 O4 53.3(7) . . . . ?
O5 P2 C1 C2 168.6(7) . . . . ?
O6 P2 O5 Mg1 -80.5(6) . . . . ?
O6 P2 C1 P1 63.7(6) . . . . ?
O6 P2 C1 O4 -176.1(6) . . . . ?
O6 P2 C1 C2 -60.8(8) . . . . ?
O7 P2 O5 Mg1 157.0(5) . . . . ?
O7 P2 O6 Mg1 112.9(9) . . . 1_455 ?
O7 P2 C1 P1 177.0(5) . . . . ?
O7 P2 C1 O4 -62.8(7) . . . . ?
O7 P2 C1 C2 52.5(8) . . . . ?
N2 C4 C5 N1 0.1(13) . . . . ?
C1 P1 O1 Mg1 19.5(8) . . . . ?
C1 P2 O5 Mg1 45.0(6) . . . . ?
C1 P2 O6 Mg1 -135.4(9) . . . 1_455 ?
C2 N1 C3 N2 -178.7(10) . . . . ?
C2 N1 C5 C4 178.7(10) . . . . ?
C3 N1 C2 C1 -110.1(11) . . . . ?
C3 N1 C5 C4 -0.3(13) . . . . ?
C3 N2 C4 C5 0.1(14) . . . . ?
C4 N2 C3 N1 -0.3(13) . . . . ?
C5 N1 C2 C1 71.1(13) . . . . ?
C5 N1 C3 N2 0.3(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.358
_oxdiff_exptl_absorpt_empirical_full_min 0.664
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_ZOLE_Zn_form_1
_database_code_depnum_ccdc_archive 'CCDC 2120920'
loop_
_audit_author_name
_audit_author_address
'Vilmali Lopez-Mejias'
;University of Puerto Rico, Rio Piedras
Puerto Rico
;
_audit_update_record             
;
2021-11-08 deposited with the CCDC.	2022-02-16 downloaded from the CCDC.
;
_audit_creation_date             2021-10-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Zole-Zin form I'
_chemical_formula_moiety         'C5 H11 N2 O8 P2 Zn0.5'
_chemical_formula_sum            'C5 H11 N2 O8 P2 Zn0.50'
_chemical_formula_weight         321.78
_chemical_melting_point          504.65
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.3868(5)
_cell_length_b                   8.4456(5)
_cell_length_c                   9.7191(6)
_cell_angle_alpha                105.3330(10)
_cell_angle_beta                 111.2460(10)
_cell_angle_gamma                97.4060(10)
_cell_volume                     527.70(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3439
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.215
_cell_measurement_theta_min      2.388
_shelx_estimated_absorpt_T_max   0.985
_shelx_estimated_absorpt_T_min   0.746
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9101
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.470
_diffrn_reflns_theta_min         2.388
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker AXS SMART APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2715
_reflns_number_total             3066
_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 v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3066
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0304
_refine_ls_restrained_S_all      1.051
_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)+(0.0431P)²+0.0572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0787
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 Zn1-H8A \\sim Zn1-H8B
 with sigma of 0.02
3.a Free rotating group:
 O8(H8A,H8B)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C5(H5)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O7(H7)
3.e Idealised tetrahedral OH refined as rotating group with stretchable bonds:
 O4(H4)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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 1.000000 0.500000 1.000000 0.00806(9) Uani 1 2 d DS . P . .
P1 P 0.62656(6) 0.22699(6) 0.97810(5) 0.00753(10) Uani 1 1 d . . . . .
P2 P 0.65688(7) 0.22146(6) 0.66878(5) 0.00821(10) Uani 1 1 d . . . . .
O1 O 0.78659(18) 0.39031(16) 1.05672(14) 0.0099(2) Uani 1 1 d . . . . .
O2 O 0.47450(18) 0.21222(16) 1.04719(15) 0.0102(3) Uani 1 1 d . . . . .
O3 O 0.72856(18) 0.07434(16) 0.97783(15) 0.0100(3) Uani 1 1 d . . . . .
H3 H 0.647140 -0.011143 0.968590 0.015 Uiso 1 1 calc R U . . .
O4 O 0.34100(18) 0.04358(16) 0.69269(16) 0.0111(3) Uani 1 1 d . . . . .
H4 H 0.3857(18) -0.027(2) 0.650(3) 0.017 Uiso 1 1 calc R U . . .
O5 O 0.81266(18) 0.38774(16) 0.76088(14) 0.0108(3) Uani 1 1 d . . . . .
O6 O 0.53295(18) 0.19657(16) 0.49949(15) 0.0104(3) Uani 1 1 d . . . . .
O7 O 0.76796(19) 0.07523(16) 0.68411(15) 0.0111(3) Uani 1 1 d . . . . .
H7 H 0.686019 -0.019110 0.627845 0.017 Uiso 1 1 calc R U . . .
O8 O 1.11437(19) 0.28252(17) 1.01117(17) 0.0156(3) Uani 1 1 d G . . . .
H8A H 1.232722 0.269052 1.021012 0.023 Uiso 1 1 d DG U . . .
H8B H 1.037543 0.180021 0.969453 0.023 Uiso 1 1 d DG U . . .
N1 N 0.2480(2) 0.34629(19) 0.61711(18) 0.0103(3) Uani 1 1 d . . . . .
N2 N 0.1435(2) 0.4109(2) 0.40615(19) 0.0148(3) Uani 1 1 d . . . . .
H2 H 0.139(3) 0.467(3) 0.336(3) 0.022 Uiso 1 1 d . U . . .
C1 C 0.4883(2) 0.2036(2) 0.7687(2) 0.0087(3) Uani 1 1 d . . . . .
C2 C 0.3759(3) 0.3450(2) 0.7726(2) 0.0104(3) Uani 1 1 d . . . . .
H2A H 0.291669 0.331640 0.830163 0.013 Uiso 1 1 calc R U . . .
H2B H 0.475436 0.455915 0.831705 0.013 Uiso 1 1 calc R U . . .
C3 C 0.0714(3) 0.2273(2) 0.5131(2) 0.0130(4) Uani 1 1 d . . . . .
H3A H 0.007072 0.134857 0.531019 0.016 Uiso 1 1 calc R U . . .
C4 C 0.0075(3) 0.2677(2) 0.3804(2) 0.0154(4) Uani 1 1 d . . . . .
H4A H -0.109629 0.207981 0.287053 0.019 Uiso 1 1 calc R U . . .
C5 C 0.2881(3) 0.4576(2) 0.5503(2) 0.0133(4) Uani 1 1 d . . . . .
H5 H 0.400029 0.553135 0.597252 0.016 Uiso 1 1 calc R 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 O1 2.0422(12) 2_767 ?
Zn1 O1 2.0422(12) . ?
Zn1 O5 2.0930(13) . ?
Zn1 O5 2.0930(13) 2_767 ?
Zn1 O8 2.1303(13) . ?
Zn1 O8 2.1303(13) 2_767 ?
P1 O1 1.5004(13) . ?
P1 O2 1.5109(13) . ?
P1 O3 1.5747(13) . ?
P1 C1 1.8585(18) . ?
P2 O5 1.5065(13) . ?
P2 O6 1.5051(13) . ?
P2 O7 1.5781(13) . ?
P2 C1 1.8494(18) . ?
O3 H3 0.8400 . ?
O4 H4 0.81(2) . ?
O4 C1 1.438(2) . ?
O7 H7 0.8400 . ?
O8 H8A 0.8701 . ?
O8 H8B 0.8700 . ?
N1 C2 1.468(2) . ?
N1 C3 1.379(2) . ?
N1 C5 1.336(2) . ?
N2 H2 0.92(2) . ?
N2 C4 1.371(2) . ?
N2 C5 1.332(2) . ?
C1 C2 1.540(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9500 . ?
C3 C4 1.355(3) . ?
C4 H4A 0.9500 . ?
C5 H5 0.9500 . ?

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 180.00(7) 2_767 . ?
O1 Zn1 O5 89.18(5) 2_767 . ?
O1 Zn1 O5 90.82(5) . . ?
O1 Zn1 O5 90.82(5) 2_767 2_767 ?
O1 Zn1 O5 89.18(5) . 2_767 ?
O1 Zn1 O8 85.45(5) . . ?
O1 Zn1 O8 94.55(5) 2_767 . ?
O1 Zn1 O8 85.45(5) 2_767 2_767 ?
O1 Zn1 O8 94.55(5) . 2_767 ?
O5 Zn1 O5 180.0 . 2_767 ?
O5 Zn1 O8 86.92(5) 2_767 . ?
O5 Zn1 O8 93.08(5) . . ?
O5 Zn1 O8 86.92(5) . 2_767 ?
O5 Zn1 O8 93.08(5) 2_767 2_767 ?
O8 Zn1 O8 180.0 . 2_767 ?
O1 P1 O2 115.18(7) . . ?
O1 P1 O3 109.10(7) . . ?
O1 P1 C1 108.53(8) . . ?
O2 P1 O3 110.09(7) . . ?
O2 P1 C1 107.67(8) . . ?
O3 P1 C1 105.85(8) . . ?
O5 P2 O7 107.46(7) . . ?
O5 P2 C1 107.84(8) . . ?
O6 P2 O5 115.63(7) . . ?
O6 P2 O7 110.99(7) . . ?
O6 P2 C1 109.07(8) . . ?
O7 P2 C1 105.33(8) . . ?
P1 O1 Zn1 133.57(8) . . ?
P1 O3 H3 109.5 . . ?
C1 O4 H4 109.5 . . ?
P2 O5 Zn1 131.94(8) . . ?
P2 O7 H7 109.5 . . ?
Zn1 O8 H8A 128.9 . . ?
Zn1 O8 H8B 122.7 . . ?
H8A O8 H8B 104.5 . . ?
C3 N1 C2 125.31(15) . . ?
C5 N1 C2 125.68(15) . . ?
C5 N1 C3 108.94(15) . . ?
C4 N2 H2 126.4(15) . . ?
C5 N2 H2 124.3(15) . . ?
C5 N2 C4 109.26(16) . . ?
P2 C1 P1 112.52(9) . . ?
O4 C1 P1 108.18(11) . . ?
O4 C1 P2 111.42(12) . . ?
O4 C1 C2 107.77(13) . . ?
C2 C1 P1 104.49(12) . . ?
C2 C1 P2 112.10(12) . . ?
N1 C2 C1 114.08(14) . . ?
N1 C2 H2A 108.7 . . ?
N1 C2 H2B 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N1 C3 H3A 126.6 . . ?
C4 C3 N1 106.79(17) . . ?
C4 C3 H3A 126.6 . . ?
N2 C4 H4A 126.4 . . ?
C3 C4 N2 107.12(17) . . ?
C3 C4 H4A 126.4 . . ?
N1 C5 H5 126.1 . . ?
N2 C5 N1 107.88(16) . . ?
N2 C5 H5 126.1 . . ?

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
P1 C1 C2 N1 -177.58(12) . . . . ?
P2 C1 C2 N1 60.29(17) . . . . ?
O1 P1 C1 P2 54.08(11) . . . . ?
O1 P1 C1 O4 177.60(10) . . . . ?
O1 P1 C1 C2 -67.78(12) . . . . ?
O2 P1 O1 Zn1 -168.54(9) . . . . ?
O2 P1 C1 P2 179.36(8) . . . . ?
O2 P1 C1 O4 -57.11(13) . . . . ?
O2 P1 C1 C2 57.51(13) . . . . ?
O3 P1 O1 Zn1 67.10(12) . . . . ?
O3 P1 C1 P2 -62.92(10) . . . . ?
O3 P1 C1 O4 60.61(12) . . . . ?
O3 P1 C1 C2 175.23(11) . . . . ?
O4 C1 C2 N1 -62.67(18) . . . . ?
O5 P2 C1 P1 -55.17(11) . . . . ?
O5 P2 C1 O4 -176.88(11) . . . . ?
O5 P2 C1 C2 62.25(13) . . . . ?
O6 P2 O5 Zn1 172.03(9) . . . . ?
O6 P2 C1 P1 178.53(8) . . . . ?
O6 P2 C1 O4 56.83(13) . . . . ?
O6 P2 C1 C2 -64.04(14) . . . . ?
O7 P2 O5 Zn1 -63.40(11) . . . . ?
O7 P2 C1 P1 59.35(11) . . . . ?
O7 P2 C1 O4 -62.36(13) . . . . ?
O7 P2 C1 C2 176.77(11) . . . . ?
N1 C3 C4 N2 -0.8(2) . . . . ?
C1 P1 O1 Zn1 -47.79(12) . . . . ?
C1 P2 O5 Zn1 49.69(12) . . . . ?
C2 N1 C3 C4 -175.93(16) . . . . ?
C2 N1 C5 N2 176.08(15) . . . . ?
C3 N1 C2 C1 70.8(2) . . . . ?
C3 N1 C5 N2 -0.9(2) . . . . ?
C4 N2 C5 N1 0.4(2) . . . . ?
C5 N1 C2 C1 -105.7(2) . . . . ?
C5 N1 C3 C4 1.1(2) . . . . ?
C5 N2 C4 C3 0.3(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_ZOLE_Ca_form_1
_database_code_depnum_ccdc_archive 'CCDC 2120919'
loop_
_audit_author_name
_audit_author_address
'Vilmali Lopez-Mejias'
;University of Puerto Rico, Rio Piedras
Puerto Rico
;
_audit_update_record             
;
2021-11-08 deposited with the CCDC.	2022-02-16 downloaded from the CCDC.
;
_audit_creation_date             2019-10-09
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_chemical_name_common            ?
_chemical_name_systematic        'Zole-Ca form I'
_chemical_formula_moiety         'C10 H22 Ca N4 O16 P4'
_chemical_formula_sum            'C10 H22 Ca N4 O16 P4'
_chemical_formula_weight         618.27
_chemical_melting_point          571.57
_chemical_oxdiff_formula         'C10 H28 Ca1 N6 O14 P4'
_chemical_oxdiff_usercomment     ZOLE_Ca_form_1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.3520(2)
_cell_length_b                   8.9793(2)
_cell_length_c                   9.5484(2)
_cell_angle_alpha                105.677(2)
_cell_angle_beta                 108.739(2)
_cell_angle_gamma                97.937(2)
_cell_volume                     556.97(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    11413
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      68.9060
_cell_measurement_theta_min      5.1810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.977
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.15e (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             318
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 0 -1 0.1003
0 -4 5 0.0596
-4 1 0 0.1096
0 4 -5 0.0903
4 0 1 0.0992
0 -6 1 0.0288
0 6 -1 0.0393
1 3 4 0.1010
4 -3 0 0.0775
2 -4 -3 0.0481
-3 0 -2 0.0928
-3 4 3 0.0816

_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.071
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.6635 -0.2308 -1.0887 0.4082 -0.0114 0.9128
-0.3877 -4.4438 5.1227 -0.9272 0.0234 0.3739
-4.4330 1.4242 -0.3236 -0.1469 0.0048 -0.9891
0.4064 4.4421 -5.1262 0.9287 -0.0234 -0.3702
4.1911 -0.4278 0.7872 0.1924 0.2016 0.9604
-0.1465 -5.6552 1.0252 -0.6826 -0.7203 0.1232
0.0089 5.6959 -1.0560 0.6795 0.7170 -0.1554
0.5151 2.8171 3.5363 0.0244 0.9375 0.3472
4.2861 -2.7488 0.3677 -0.0043 -0.2049 0.9788
2.2297 -4.1930 -2.8743 -0.0241 -0.9512 0.3076
-3.4781 0.4419 -2.2830 -0.0106 -0.3805 -0.9247
-2.7936 4.2623 2.5016 0.0224 0.8888 -0.4577

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12816
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.940
_diffrn_reflns_theta_min         5.192
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -40.00  32.00   0.50    0.20    --  -11.59  88.00   0.00  144
  2  ω    -32.00  40.00   0.50    0.20    --   11.59 -88.00-116.00  144
  3  ω     79.00 157.00   0.50    0.20    --   96.16  88.00   0.00  156
  4  ω     30.00 124.00   0.50    0.20    --   96.16 -88.00-116.00  188
  5  ω    -76.00  14.00   0.50    0.20    --  -11.59 -77.00  30.00  180
  6  ω    -20.00  55.00   0.50    0.20    --  -11.59  30.00 -60.00  150
  7  ω    -76.00  14.00   0.50    0.20    --  -11.59 -77.00  90.00  180
  8  ω    -31.00  52.00   0.50    0.20    --  -11.59  61.00 -30.00  166
  9  ω    -31.00  16.00   0.50    0.20    --  -11.59 -88.00-116.00   94
 10  ω    -55.00  20.00   0.50    0.20    --   11.59 -30.00  90.00  150
 11  ω      3.00  60.00   0.50    0.20    --   11.59-125.00-120.00  114
 12  ω    -55.00  20.00   0.50    0.20    --   11.59 -30.00 150.00  150
 13  ω    -15.00  31.00   0.50    0.20    --   11.59  88.00   0.00   92
 14  ω      3.00  60.00   0.50    0.20    --   11.59-125.00 120.00  114
 15  ω     33.00 112.00   0.50    0.20    --   96.16 -50.00 -60.00  158
 16  ω     32.00 117.00   0.50    0.20    --   96.16-117.00-120.00  170
 17  ω     71.00 157.00   0.50    0.20    --   96.16  77.00-120.00  172
 18  ω     32.00 118.00   0.50    0.20    --   96.16 -68.00 150.00  172
 19  ω     33.00 109.00   0.50    0.20    --   96.16 -42.00-120.00  152
 20  ω     87.00 157.00   0.50    0.20    --   96.16  33.00 -60.00  140
 21  ω     87.00 157.00   0.50    0.20    --   96.16  33.00-150.00  140
 22  ω     33.00 115.00   0.50    0.20    --   96.16 -59.00-150.00  164
 23  ω     26.00 109.00   0.50    0.20    --   96.16 -96.00   0.00  166
 24  ω     81.00 157.00   0.50    0.20    --   96.16  96.00 -60.00  152
 25  ω     62.00 157.00   0.50    0.20    --   96.16 145.00-180.00  190
 26  ω     87.00 157.00   0.50    0.20    --   96.16  33.00  30.00  140
 27  ω     31.00 105.00   0.50    0.20    --   96.16 -33.00-150.00  148
 28  ω     66.00 157.00   0.50    0.20    --   96.16   8.00-180.00  182
 29  ω     32.00 117.00   0.50    0.20    --   96.16-117.00-180.00  170
 30  ω     26.00 109.00   0.50    0.20    --   96.16 -96.00  60.00  166
 31  ω     31.00 105.00   0.50    0.20    --   96.16 -33.00  30.00  148
 32  ω     32.00 117.00   0.50    0.20    --   96.16-117.00 -60.00  170
 33  ω     33.00 109.00   0.50    0.20    --   96.16 -42.00  60.00  152
 34  ω     32.00 117.00   0.50    0.20    --   96.16-117.00 -30.00  170
 35  ω     32.00 118.00   0.50    0.20    --   96.16 -68.00  60.00  172
 36  ω    -60.00  -3.00   0.50    0.20    --  -11.59 125.00  60.00  114
 37  ω    -75.00   8.00   0.50    0.20    --  -11.59 -61.00 -90.00  166
 38  ω    -76.00  14.00   0.50    0.20    --  -11.59 -77.00 150.00  180
 39  ω    -75.00   8.00   0.50    0.20    --  -11.59 -61.00 -30.00  166
 40  ω    -83.00   5.00   0.50    0.20    --  -11.59 -15.00  30.00  176
 41  ω    -74.00   2.00   0.50    0.20    --  -11.59 -45.00-180.00  152
 42  ω    -76.00  14.00   0.50    0.20    --  -11.59 -77.00 -30.00  180
 43  ω    -20.00  55.00   0.50    0.20    --  -11.59  30.00  60.00  150
 44  ω      4.00  78.00   0.50    0.20    --   11.59  30.00 150.00  148
 45  ω      3.00  60.00   0.50    0.20    --   11.59-125.00-180.00  114
 46  ω      3.00  60.00   0.50    0.20    --   11.59-125.00   0.00  114
 47  ω      4.00  78.00   0.50    0.20    --   11.59  30.00-120.00  148
 48  ω     71.00 157.00   0.50    0.20    --   96.16  77.00 150.00  172
 49  ω     78.00 157.00   0.50    0.20    --   96.16  59.00  30.00  158
 50  ω     71.00 157.00   0.50    0.20    --   96.16  77.00 -30.00  172
 51  ω     88.00 157.00   0.50    0.20    --   96.16  25.00  90.00  138
 52  ω     78.00 157.00   0.50    0.20    --   96.16  59.00  90.00  158
 53  ω     71.00 157.00   0.50    0.20    --   96.16  77.00 -90.00  172
 54  ω     71.00 157.00   0.50    0.20    --   96.16  77.00-180.00  172
 55  ω     71.00 157.00   0.50    0.20    --   96.16  77.00  60.00  172
 56  ω     75.00 157.00   0.50    0.20    --   96.16  68.00 -60.00  164
 57  ω     71.00 157.00   0.50    0.20    --   96.16  77.00   0.00  172
 58  ω     71.00 157.00   0.50    0.20    --   96.16  77.00 120.00  172
 59  ω     78.00 157.00   0.50    0.20    --   96.16  59.00 120.00  158
 60  ω     78.00 157.00   0.50    0.20    --   96.16  59.00 -90.00  158
 61  ω     71.00 157.00   0.50    0.20    --   96.16  77.00 -60.00  172
 62  ω     71.00 157.00   0.50    0.20    --   96.16  77.00-150.00  172
 63  ω     80.00 157.00   0.50    0.20    --   96.16  50.00 150.00  154
 64  ω     78.00 157.00   0.50    0.20    --   96.16  59.00 -30.00  158
 65  ω     78.00 157.00   0.50    0.20    --   96.16  59.00   0.00  158
 66  ω     78.00 157.00   0.50    0.20    --   96.16  59.00-150.00  158
 67  ω     80.00 157.00   0.50    0.20    --   96.16  50.00-120.00  154
 68  ω     71.00 157.00   0.50    0.20    --   96.16  77.00  30.00  172
 69  ω     80.00 157.00   0.50    0.20    --   96.16  50.00-180.00  154
 70  ω     78.00 157.00   0.50    0.20    --   96.16  59.00  60.00  158
 71  ω     71.00 157.00   0.50    0.20    --   96.16  77.00  90.00  172
 72  ω    -60.00  -3.00   0.50    0.20    --  -11.59 125.00 150.00  114
 73  ω    -75.00   8.00   0.50    0.20    --  -11.59 -61.00-180.00  166
 74  ω    -75.00   8.00   0.50    0.20    --  -11.59 -61.00 120.00  166
 75  ω    -83.00  60.00   0.50    0.20    --  -11.59   0.00-180.00  286
 76  ω    -83.00  60.00   0.50    0.20    --  -11.59   0.00-150.00  286
 77  ω    -83.00  60.00   0.50    0.20    --  -11.59   0.00-120.00  286
 78  ω    -83.00  60.00   0.50    0.20    --  -11.59   0.00 -90.00  286
 79  ω    -83.00  60.00   0.50    0.20    --  -11.59   0.00 -60.00  286
 80  ω    -83.00  60.00   0.50    0.20    --  -11.59   0.00 -30.00  286
 81  ω    -83.00  60.00   0.50    0.20    --  -11.59   0.00   0.00  286
 82  ω    -74.00   2.00   0.50    0.20    --  -11.59 -45.00-120.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0725794000
_diffrn_orient_matrix_UB_12      0.1032521000
_diffrn_orient_matrix_UB_13      -0.0859321000
_diffrn_orient_matrix_UB_21      0.0374827000
_diffrn_orient_matrix_UB_22      0.1515759000
_diffrn_orient_matrix_UB_23      0.1388928000
_diffrn_orient_matrix_UB_31      0.2132150000
_diffrn_orient_matrix_UB_32      -0.0132239000
_diffrn_orient_matrix_UB_33      0.0776588000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2047
_reflns_number_total             2057
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0133(6)
_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   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2057
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0224
_refine_ls_restrained_S_all      1.084
_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)+(0.0313P)²+0.4276P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0609
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2B,H2C)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2A), C3(H3), C4(H4A), C5(H5)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4), O6(H6)
;
_atom_sites_solution_hydrogens   mixed
_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
Ca1 Ca 1.000000 0.500000 1.000000 0.00740(13) Uani 1 2 d S T P . .
P1 P 0.63835(6) 0.21512(4) 0.65809(4) 0.00785(12) Uani 1 1 d . . . . .
P2 P 0.60441(6) 0.21768(4) 0.97557(4) 0.00683(12) Uani 1 1 d . . . . .
O1 O 0.78087(17) 0.37751(13) 0.74135(12) 0.0113(2) Uani 1 1 d . . . . .
O2 O 0.76326(16) 0.08797(13) 0.67866(13) 0.0109(2) Uani 1 1 d . . . . .
H2 H 0.691473 -0.001960 0.627693 0.016 Uiso 1 1 calc GR . . . .
O3 O 0.51448(16) 0.18095(12) 0.48810(12) 0.0104(2) Uani 1 1 d . . . . .
O4 O 0.33189(16) 0.03958(13) 0.69020(13) 0.0107(2) Uani 1 1 d . . . . .
H4 H 0.386022 -0.027643 0.656050 0.016 Uiso 1 1 calc GR . . . .
O5 O 0.44916(16) 0.19005(12) 1.04436(12) 0.0094(2) Uani 1 1 d . . . . .
O6 O 0.72270(16) 0.08496(12) 0.97645(13) 0.0099(2) Uani 1 1 d . . . . .
H6 H 0.652394 0.003229 0.972080 0.015 Uiso 1 1 calc GR . . . .
O7 O 0.74837(16) 0.37803(12) 1.05326(12) 0.0093(2) Uani 1 1 d . . . . .
O8 O 1.1057(2) 0.26966(14) 1.02180(15) 0.0149(3) Uani 1 1 d . . . . .
H8A H 1.208(4) 0.241(3) 1.025(3) 0.030(6) Uiso 1 1 d . . . . .
H8B H 1.021(4) 0.190(3) 0.990(3) 0.041(8) Uiso 1 1 d . . . . .
N1 N 0.2474(2) 0.33723(15) 0.61958(15) 0.0099(3) Uani 1 1 d . . . . .
N2 N 0.1813(2) 0.43014(17) 0.42813(16) 0.0146(3) Uani 1 1 d . . . . .
H2A H 0.187590 0.491461 0.373607 0.018 Uiso 1 1 calc R . . . .
C1 C 0.4714(2) 0.19270(18) 0.76553(17) 0.0083(3) Uani 1 1 d . . . . .
C2 C 0.3498(2) 0.31923(19) 0.77114(18) 0.0111(3) Uani 1 1 d . . . . .
H2B H 0.252031 0.291717 0.814084 0.013 Uiso 1 1 calc R . . . .
H2C H 0.437912 0.421431 0.842630 0.013 Uiso 1 1 calc R . . . .
C3 C 0.3021(2) 0.45857(19) 0.57475(19) 0.0126(3) Uani 1 1 d . . . . .
H3 H 0.406999 0.547855 0.635750 0.015 Uiso 1 1 calc R . . . .
C4 C 0.0448(3) 0.2872(2) 0.37727(19) 0.0153(3) Uani 1 1 d . . . . .
H4A H -0.056169 0.239527 0.278755 0.018 Uiso 1 1 calc R . . . .
C5 C 0.0847(2) 0.22889(19) 0.49749(19) 0.0129(3) Uani 1 1 d . . . . .
H5 H 0.015919 0.134041 0.497833 0.016 Uiso 1 1 calc R . . . .


_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
Ca1 P1 3.5075(4) . ?
Ca1 P1 3.5075(4) 2_767 ?
Ca1 P2 3.4854(4) . ?
Ca1 P2 3.4854(4) 2_767 ?
Ca1 O1 2.3218(11) . ?
Ca1 O1 2.3218(11) 2_767 ?
Ca1 O7 2.2862(11) 2_767 ?
Ca1 O7 2.2862(11) . ?
Ca1 O8 2.3446(12) . ?
Ca1 O8 2.3446(12) 2_767 ?
Ca1 H8B 2.78(3) 2_767 ?
Ca1 H8B 2.78(3) . ?
P1 O1 1.5075(11) . ?
P1 O2 1.5749(11) . ?
P1 O3 1.5040(11) . ?
P1 C1 1.8580(15) . ?
P2 O5 1.5124(11) . ?
P2 O6 1.5696(11) . ?
P2 O7 1.4970(11) . ?
P2 C1 1.8614(15) . ?
O2 H2 0.8200 . ?
O4 H4 0.8200 . ?
O4 C1 1.4358(18) . ?
O6 H6 0.8200 . ?
O8 H8A 0.82(3) . ?
O8 H8B 0.79(3) . ?
N1 C2 1.4654(19) . ?
N1 C3 1.332(2) . ?
N1 C5 1.380(2) . ?
N2 H2A 0.8600 . ?
N2 C3 1.326(2) . ?
N2 C4 1.373(2) . ?
C1 C2 1.540(2) . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 H3 0.9300 . ?
C4 H4A 0.9300 . ?
C4 C5 1.352(2) . ?
C5 H5 0.9300 . ?

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
P1 Ca1 P1 180.000(11) . 2_767 ?
P1 Ca1 H8B 68.3(6) 2_767 2_767 ?
P1 Ca1 H8B 111.7(6) 2_767 . ?
P1 Ca1 H8B 111.7(6) . 2_767 ?
P1 Ca1 H8B 68.3(6) . . ?
P2 Ca1 P1 52.900(9) . . ?
P2 Ca1 P1 127.100(9) . 2_767 ?
P2 Ca1 P1 127.100(9) 2_767 . ?
P2 Ca1 P1 52.900(9) 2_767 2_767 ?
P2 Ca1 P2 180.0 . 2_767 ?
P2 Ca1 H8B 57.3(6) 2_767 2_767 ?
P2 Ca1 H8B 122.7(6) 2_767 . ?
P2 Ca1 H8B 57.3(6) . . ?
P2 Ca1 H8B 122.7(6) . 2_767 ?
O1 Ca1 P1 18.78(3) . . ?
O1 Ca1 P1 161.22(3) 2_767 . ?
O1 Ca1 P1 18.78(3) 2_767 2_767 ?
O1 Ca1 P1 161.22(3) . 2_767 ?
O1 Ca1 P2 110.66(3) 2_767 . ?
O1 Ca1 P2 69.34(3) . . ?
O1 Ca1 P2 69.34(3) 2_767 2_767 ?
O1 Ca1 P2 110.66(3) . 2_767 ?
O1 Ca1 O1 180.0 . 2_767 ?
O1 Ca1 O8 85.50(4) 2_767 . ?
O1 Ca1 O8 94.50(4) 2_767 2_767 ?
O1 Ca1 O8 94.50(4) . . ?
O1 Ca1 O8 85.50(4) . 2_767 ?
O1 Ca1 H8B 84.3(6) 2_767 2_767 ?
O1 Ca1 H8B 84.3(6) . . ?
O1 Ca1 H8B 95.7(6) . 2_767 ?
O1 Ca1 H8B 95.7(6) 2_767 . ?
O7 Ca1 P1 68.92(3) . . ?
O7 Ca1 P1 68.92(3) 2_767 2_767 ?
O7 Ca1 P1 111.08(3) . 2_767 ?
O7 Ca1 P1 111.08(3) 2_767 . ?
O7 Ca1 P2 161.74(3) 2_767 . ?
O7 Ca1 P2 161.74(3) . 2_767 ?
O7 Ca1 P2 18.26(3) . . ?
O7 Ca1 P2 18.26(3) 2_767 2_767 ?
O7 Ca1 O1 83.29(4) 2_767 2_767 ?
O7 Ca1 O1 83.29(4) . . ?
O7 Ca1 O1 96.71(4) 2_767 . ?
O7 Ca1 O1 96.71(4) . 2_767 ?
O7 Ca1 O7 180.00(3) . 2_767 ?
O7 Ca1 O8 80.71(4) . . ?
O7 Ca1 O8 80.71(4) 2_767 2_767 ?
O7 Ca1 O8 99.29(4) . 2_767 ?
O7 Ca1 O8 99.29(4) 2_767 . ?
O7 Ca1 H8B 68.9(6) . . ?
O7 Ca1 H8B 68.9(6) 2_767 2_767 ?
O7 Ca1 H8B 111.1(6) 2_767 . ?
O7 Ca1 H8B 111.1(6) . 2_767 ?
O8 Ca1 P1 80.39(3) 2_767 2_767 ?
O8 Ca1 P1 99.61(3) 2_767 . ?
O8 Ca1 P1 99.61(3) . 2_767 ?
O8 Ca1 P1 80.39(3) . . ?
O8 Ca1 P2 71.14(3) 2_767 2_767 ?
O8 Ca1 P2 71.14(3) . . ?
O8 Ca1 P2 108.86(3) . 2_767 ?
O8 Ca1 P2 108.86(3) 2_767 . ?
O8 Ca1 O8 180.0 2_767 . ?
O8 Ca1 H8B 14.8(6) . . ?
O8 Ca1 H8B 165.2(6) . 2_767 ?
O8 Ca1 H8B 14.8(6) 2_767 2_767 ?
O8 Ca1 H8B 165.2(6) 2_767 . ?
H8B Ca1 H8B 180.0 . 2_767 ?
O1 P1 Ca1 29.72(4) . . ?
O1 P1 O2 107.12(6) . . ?
O1 P1 C1 108.33(6) . . ?
O2 P1 Ca1 90.02(4) . . ?
O2 P1 C1 105.10(6) . . ?
O3 P1 Ca1 145.29(4) . . ?
O3 P1 O1 115.60(6) . . ?
O3 P1 O2 111.23(6) . . ?
O3 P1 C1 108.92(7) . . ?
C1 P1 Ca1 90.37(5) . . ?
O5 P2 Ca1 143.89(4) . . ?
O5 P2 O6 110.15(6) . . ?
O5 P2 C1 107.31(7) . . ?
O6 P2 Ca1 93.34(4) . . ?
O6 P2 C1 106.23(6) . . ?
O7 P2 Ca1 28.59(4) . . ?
O7 P2 O5 115.42(6) . . ?
O7 P2 O6 108.93(6) . . ?
O7 P2 C1 108.37(6) . . ?
C1 P2 Ca1 91.00(5) . . ?
P1 O1 Ca1 131.51(6) . . ?
P1 O2 H2 109.5 . . ?
C1 O4 H4 109.5 . . ?
P2 O6 H6 109.5 . . ?
P2 O7 Ca1 133.14(6) . . ?
Ca1 O8 H8A 134.2(17) . . ?
Ca1 O8 H8B 116(2) . . ?
H8A O8 H8B 106(3) . . ?
C3 N1 C2 125.20(14) . . ?
C3 N1 C5 108.76(13) . . ?
C5 N1 C2 125.98(13) . . ?
C3 N2 H2A 125.4 . . ?
C3 N2 C4 109.15(14) . . ?
C4 N2 H2A 125.4 . . ?
P1 C1 P2 113.74(8) . . ?
O4 C1 P1 110.46(10) . . ?
O4 C1 P2 108.80(10) . . ?
O4 C1 C2 106.85(12) . . ?
C2 C1 P1 112.50(10) . . ?
C2 C1 P2 104.08(10) . . ?
N1 C2 C1 115.09(12) . . ?
N1 C2 H2B 108.5 . . ?
N1 C2 H2C 108.5 . . ?
C1 C2 H2B 108.5 . . ?
C1 C2 H2C 108.5 . . ?
H2B C2 H2C 107.5 . . ?
N1 C3 H3 125.9 . . ?
N2 C3 N1 108.24(14) . . ?
N2 C3 H3 125.9 . . ?
N2 C4 H4A 126.5 . . ?
C5 C4 N2 107.05(14) . . ?
C5 C4 H4A 126.5 . . ?
N1 C5 H5 126.6 . . ?
C4 C5 N1 106.79(14) . . ?
C4 C5 H5 126.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 P1 C1 P2 -33.42(7) . . . . ?
Ca1 P1 C1 O4 -156.09(9) . . . . ?
Ca1 P1 C1 C2 84.60(10) . . . . ?
Ca1 P2 C1 P1 33.67(7) . . . . ?
Ca1 P2 C1 O4 157.25(9) . . . . ?
Ca1 P2 C1 C2 -89.11(9) . . . . ?
P1 C1 C2 N1 49.69(16) . . . . ?
P2 C1 C2 N1 173.27(11) . . . . ?
O1 P1 C1 P2 -57.54(9) . . . . ?
O1 P1 C1 O4 179.80(9) . . . . ?
O1 P1 C1 C2 60.49(12) . . . . ?
O2 P1 O1 Ca1 -57.40(10) . . . . ?
O2 P1 C1 P2 56.70(9) . . . . ?
O2 P1 C1 O4 -65.97(11) . . . . ?
O2 P1 C1 C2 174.73(10) . . . . ?
O3 P1 O1 Ca1 178.01(7) . . . . ?
O3 P1 C1 P2 175.97(7) . . . . ?
O3 P1 C1 O4 53.30(11) . . . . ?
O3 P1 C1 C2 -66.00(12) . . . . ?
O4 C1 C2 N1 -71.70(16) . . . . ?
O5 P2 O7 Ca1 -175.53(7) . . . . ?
O5 P2 C1 P1 -177.92(7) . . . . ?
O5 P2 C1 O4 -54.34(11) . . . . ?
O5 P2 C1 C2 59.30(11) . . . . ?
O6 P2 O7 Ca1 59.97(10) . . . . ?
O6 P2 C1 P1 -60.11(9) . . . . ?
O6 P2 C1 O4 63.47(11) . . . . ?
O6 P2 C1 C2 177.12(9) . . . . ?
O7 P2 C1 P1 56.81(9) . . . . ?
O7 P2 C1 O4 -179.61(9) . . . . ?
O7 P2 C1 C2 -65.96(11) . . . . ?
N2 C4 C5 N1 -0.65(18) . . . . ?
C1 P1 O1 Ca1 55.50(10) . . . . ?
C1 P2 O7 Ca1 -55.19(10) . . . . ?
C2 N1 C3 N2 176.66(13) . . . . ?
C2 N1 C5 C4 -176.47(14) . . . . ?
C3 N1 C2 C1 -105.71(17) . . . . ?
C3 N1 C5 C4 0.81(18) . . . . ?
C3 N2 C4 C5 0.27(18) . . . . ?
C4 N2 C3 N1 0.24(18) . . . . ?
C5 N1 C2 C1 71.15(19) . . . . ?
C5 N1 C3 N2 -0.65(18) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.847
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_ZOLE_Mg_form_1
_database_code_depnum_ccdc_archive 'CCDC 2120917'
loop_
_audit_author_name
_audit_author_address
'Vilmali Lopez-Mejias'
;University of Puerto Rico, Rio Piedras
Puerto Rico
;
_audit_update_record             
;
2021-11-08 deposited with the CCDC.	2022-02-16 downloaded from the CCDC.
;
_audit_creation_date             2020-03-28
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_chemical_name_common            ?
_chemical_name_systematic        'Zole-Mg form I'
_chemical_formula_moiety         'C5 H11 Mg0.5 N2 O8 P2'
_chemical_formula_sum            'C5 H11 Mg0.50 N2 O8 P2'
_chemical_formula_weight         301.25
_chemical_melting_point          571.17
_chemical_oxdiff_formula         MgC5H10N2O7P2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4070(2)
_cell_length_b                   8.40350(10)
_cell_length_c                   9.7306(2)
_cell_angle_alpha                105.249(2)
_cell_angle_beta                 111.368(2)
_cell_angle_gamma                97.085(2)
_cell_volume                     527.74(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6892
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      68.5620
_cell_measurement_theta_min      5.1640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65450
_exptl_absorpt_correction_type   multi-scan
_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   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10206
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.816
_diffrn_reflns_theta_min         5.177
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -97.00  -8.00   0.50    0.50    --  -41.24 134.00-153.00  178
  2  ω    -97.00  -8.00   0.50    0.50    --  -41.24 135.00  25.00  178
  3  ω      8.00  97.00   0.50    0.50    --   41.24-135.00 -40.00  178
  4  ω      8.00  97.00   0.50    0.50    --   41.24-134.00 139.00  178
  5  ω     32.00 124.00   0.50    0.50    --   96.95-134.00 139.00  184
  6  ω     32.00 125.00   0.50    0.50    --   96.95-135.00 -40.00  186
  7  ω     67.00 158.00   0.50    0.50    --   96.95 134.00-153.00  182
  8  ω    -57.00  24.00   0.50    0.50    --  -41.24  43.00-150.00  162
  9  ω     25.00 106.00   0.50    0.50    --   41.24  43.00-120.00  162
 10  ω     15.00 108.00   0.50    0.50    --   41.24  77.00  30.00  186
 11  ω     29.00 109.00   0.50    0.50    --   41.24  32.00 150.00  160
 12  ω    -31.00  58.00   0.50    0.50    --   41.24 -21.00-120.00  178
 13  ω     29.00 109.00   0.50    0.50    --   41.24  32.00  30.00  160
 14  ω     25.00 106.00   0.50    0.50    --   41.24  43.00-180.00  162
 15  ω     61.00 158.00   0.50    0.50    --   96.95 145.00 -90.00  194
 16  ω     31.00 132.00   0.50    0.50    --   96.95-145.00 -60.00  202
 17  ω     73.00 158.00   0.50    0.50    --   96.95  68.00  60.00  170
 18  ω     70.00 158.00   0.50    0.50    --   96.95  77.00  90.00  176
 19  ω     32.00 118.00   0.50    0.50    --   96.95 -59.00 -90.00  172
 20  ω     28.00 127.00   0.50    0.50    --   96.95 -87.00 -60.00  198
 21  ω     26.00 110.00   0.50    0.50    --   96.95 -25.00-150.00  168
 22  ω     28.00 127.00   0.50    0.50    --   96.95 -87.00  90.00  198
 23  ω     32.00 118.00   0.50    0.50    --   96.95 -59.00   0.00  172
 24  ω     81.00 158.00   0.50    0.50    --   96.95  42.00-180.00  154
 25  ω     84.00 158.00   0.50    0.50    --   96.95  33.00-150.00  148
 26  ω     26.00 110.00   0.50    0.50    --   96.95 -25.00 -60.00  168
 27  ω     29.00 109.00   0.50    0.50    --   96.95 -33.00 120.00  160
 28  ω     84.00 158.00   0.50    0.50    --   96.95  33.00  30.00  148
 29  ω     30.00 113.00   0.50    0.50    --   96.95-117.00 -30.00  166
 30  ω     73.00 158.00   0.50    0.50    --   96.95  68.00-120.00  170
 31  ω     32.00 118.00   0.50    0.50    --   96.95 -59.00  90.00  172
 32  ω     84.00 158.00   0.50    0.50    --   96.95  33.00 150.00  148
 33  ω     80.00 158.00   0.50    0.50    --   96.95  96.00 -90.00  156
 34  ω     77.00 158.00   0.50    0.50    --   96.95 117.00 -30.00  162
 35  ω     67.00 158.00   0.50    0.50    --   96.95 135.00  25.00  182
 36  ω   -108.00 -15.00   0.50    0.50    --  -41.24 -77.00  90.00  186
 37  ω    -57.00  24.00   0.50    0.50    --  -41.24  43.00  60.00  162
 38  ω   -113.00 -25.00   0.50    0.50    --  -41.24 -21.00 -60.00  176
 39  ω   -108.00 -15.00   0.50    0.50    --  -41.24 -77.00  60.00  186
 40  ω     18.00 107.00   0.50    0.50    --   41.24  65.00   0.00  178
 41  ω     15.00 108.00   0.50    0.50    --   41.24  77.00  90.00  186
 42  ω     15.00 108.00   0.50    0.50    --   41.24  77.00 -60.00  186
 43  ω     15.00 108.00   0.50    0.50    --   41.24  77.00-150.00  186
 44  ω     15.00 108.00   0.50    0.50    --   41.24  77.00-120.00  186
 45  ω     15.00 108.00   0.50    0.50    --   41.24  77.00 -90.00  186
 46  ω     18.00 107.00   0.50    0.50    --   41.24  65.00-180.00  178
 47  ω     73.00 158.00   0.50    0.50    --   96.95  68.00-150.00  170
 48  ω     70.00 158.00   0.50    0.50    --   96.95  77.00 -90.00  176
 49  ω     73.00 158.00   0.50    0.50    --   96.95  68.00  30.00  170
 50  ω     70.00 158.00   0.50    0.50    --   96.95  77.00 -30.00  176
 51  ω     73.00 158.00   0.50    0.50    --   96.95  68.00  90.00  170
 52  ω     70.00 158.00   0.50    0.50    --   96.95  77.00-120.00  176
 53  ω     73.00 158.00   0.50    0.50    --   96.95  68.00 150.00  170
 54  ω     73.00 158.00   0.50    0.50    --   96.95  68.00   0.00  170
 55  ω     70.00 158.00   0.50    0.50    --   96.95  77.00-180.00  176
 56  ω     70.00 158.00   0.50    0.50    --   96.95  77.00 120.00  176
 57  ω     70.00 148.00   0.50    0.50    --   96.95  77.00  30.00  156
 58  ω     70.00 158.00   0.50    0.50    --   96.95  77.00 -60.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1093737000
_diffrn_orient_matrix_UB_12      0.0857645000
_diffrn_orient_matrix_UB_13      0.1788551000
_diffrn_orient_matrix_UB_21      0.0943795000
_diffrn_orient_matrix_UB_22      0.1594758000
_diffrn_orient_matrix_UB_23      -0.0228672000
_diffrn_orient_matrix_UB_31      -0.1793521000
_diffrn_orient_matrix_UB_32      0.0748461000
_diffrn_orient_matrix_UB_33      0.0010773000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1897
_reflns_number_total             1946
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0035(6)
_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   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1946
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0272
_refine_ls_restrained_S_all      1.054
_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)+(0.0363P)²+0.5521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0732
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3A), C4(H4A), C5(H5)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O7(H7)
;
_atom_sites_solution_hydrogens   mixed
_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
P1 P 0.62652(6) 0.22691(5) 0.97753(5) 0.01027(15) Uani 1 1 d . . . . .
P2 P 0.65706(6) 0.22187(5) 0.66972(5) 0.01144(15) Uani 1 1 d . . . . .
Mg1 Mg 1.000000 0.500000 1.000000 0.0112(2) Uani 1 2 d S T P . .
O1 O 0.78783(18) 0.38784(15) 1.05411(14) 0.0129(3) Uani 1 1 d . . . . .
O2 O 0.47601(18) 0.21470(15) 1.04765(14) 0.0133(3) Uani 1 1 d . . . . .
O3 O 0.72637(18) 0.07241(15) 0.97671(14) 0.0138(3) Uani 1 1 d . . . . .
H3 H 0.647290 -0.010161 0.969292 0.021 Uiso 1 1 calc GR . . . .
O4 O 0.34139(19) 0.04306(16) 0.69236(15) 0.0159(3) Uani 1 1 d . . . . .
H4 H 0.388933 -0.029977 0.653428 0.024 Uiso 1 1 calc GR . . . .
O5 O 0.81333(19) 0.38633(16) 0.76348(14) 0.0153(3) Uani 1 1 d . . . . .
O6 O 0.53470(19) 0.19938(15) 0.50065(14) 0.0150(3) Uani 1 1 d . . . . .
O7 O 0.76541(19) 0.07312(16) 0.68333(14) 0.0151(3) Uani 1 1 d . . . . .
H7 H 0.685385 -0.018246 0.626428 0.023 Uiso 1 1 calc GR . . . .
O8 O 0.8862(2) 0.71558(17) 0.99322(17) 0.0190(3) Uani 1 1 d . . . . .
N1 N 0.2470(2) 0.34643(19) 0.61616(17) 0.0148(3) Uani 1 1 d . . . . .
N2 N 0.1429(2) 0.4115(2) 0.40557(18) 0.0195(4) Uani 1 1 d . . . . .
H2 H 0.136225 0.463471 0.339314 0.023 Uiso 1 1 calc R . . . .
C1 C 0.4882(3) 0.2037(2) 0.7686(2) 0.0129(4) Uani 1 1 d . . . . .
C2 C 0.3743(3) 0.3449(2) 0.7715(2) 0.0153(4) Uani 1 1 d . . . . .
H2A H 0.291761 0.331372 0.827412 0.018 Uiso 1 1 calc R . . . .
H2B H 0.470483 0.454093 0.829322 0.018 Uiso 1 1 calc R . . . .
C3 C 0.0712(3) 0.2283(2) 0.5124(2) 0.0179(4) Uani 1 1 d . . . . .
H3A H 0.008608 0.137675 0.530118 0.021 Uiso 1 1 calc R . . . .
C4 C 0.0064(3) 0.2689(2) 0.3796(2) 0.0206(4) Uani 1 1 d . . . . .
H4A H -0.108219 0.211225 0.288638 0.025 Uiso 1 1 calc R . . . .
C5 C 0.2870(3) 0.4570(2) 0.5489(2) 0.0180(4) Uani 1 1 d . . . . .
H5 H 0.396647 0.549845 0.594337 0.022 Uiso 1 1 calc R . . . .
H8A H 0.967(5) 0.811(4) 1.026(4) 0.047(8) Uiso 1 1 d . . . . .
H8B H 0.783(5) 0.732(4) 0.984(3) 0.041(8) Uiso 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
P1 O1 1.4947(12) . ?
P1 O2 1.5106(12) . ?
P1 O3 1.5711(12) . ?
P1 C1 1.8563(18) . ?
P2 O5 1.5016(13) . ?
P2 O6 1.5070(12) . ?
P2 O7 1.5752(13) . ?
P2 C1 1.8496(18) . ?
Mg1 O1 2.0333(12) . ?
Mg1 O1 2.0333(12) 2_767 ?
Mg1 O5 2.0784(12) 2_767 ?
Mg1 O5 2.0784(12) . ?
Mg1 O8 2.0965(14) 2_767 ?
Mg1 O8 2.0966(14) . ?
O3 H3 0.8200 . ?
O4 H4 0.8200 . ?
O4 C1 1.442(2) . ?
O7 H7 0.8200 . ?
O8 H8A 0.84(3) . ?
O8 H8B 0.77(3) . ?
N1 C2 1.466(2) . ?
N1 C3 1.377(2) . ?
N1 C5 1.331(2) . ?
N2 H2 0.8600 . ?
N2 C4 1.370(3) . ?
N2 C5 1.328(3) . ?
C1 C2 1.538(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9300 . ?
C3 C4 1.355(3) . ?
C4 H4A 0.9300 . ?
C5 H5 0.9300 . ?

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 P1 O2 115.67(7) . . ?
O1 P1 O3 108.63(7) . . ?
O1 P1 C1 108.46(7) . . ?
O2 P1 O3 110.22(7) . . ?
O2 P1 C1 107.76(8) . . ?
O3 P1 C1 105.61(7) . . ?
O5 P2 O6 115.98(7) . . ?
O5 P2 O7 107.39(7) . . ?
O5 P2 C1 107.80(8) . . ?
O6 P2 O7 110.71(7) . . ?
O6 P2 C1 109.20(8) . . ?
O7 P2 C1 105.19(7) . . ?
O1 Mg1 O1 180.0 . 2_767 ?
O1 Mg1 O5 89.66(5) . . ?
O1 Mg1 O5 90.34(5) 2_767 . ?
O1 Mg1 O5 90.34(5) . 2_767 ?
O1 Mg1 O5 89.66(5) 2_767 2_767 ?
O1 Mg1 O8 85.85(5) . 2_767 ?
O1 Mg1 O8 94.15(5) . . ?
O1 Mg1 O8 94.15(5) 2_767 2_767 ?
O1 Mg1 O8 85.86(5) 2_767 . ?
O5 Mg1 O5 180.0 2_767 . ?
O5 Mg1 O8 88.21(5) 2_767 2_767 ?
O5 Mg1 O8 91.79(5) . 2_767 ?
O5 Mg1 O8 91.79(5) 2_767 . ?
O5 Mg1 O8 88.21(5) . . ?
O8 Mg1 O8 180.0 2_767 . ?
P1 O1 Mg1 135.40(7) . . ?
P1 O3 H3 109.5 . . ?
C1 O4 H4 109.5 . . ?
P2 O5 Mg1 133.60(7) . . ?
P2 O7 H7 109.5 . . ?
Mg1 O8 H8A 119(2) . . ?
Mg1 O8 H8B 132(2) . . ?
H8A O8 H8B 107(3) . . ?
C3 N1 C2 125.52(15) . . ?
C5 N1 C2 125.72(16) . . ?
C5 N1 C3 108.68(15) . . ?
C4 N2 H2 125.3 . . ?
C5 N2 H2 125.3 . . ?
C5 N2 C4 109.48(16) . . ?
P2 C1 P1 112.13(9) . . ?
O4 C1 P1 108.43(11) . . ?
O4 C1 P2 111.52(11) . . ?
O4 C1 C2 107.39(14) . . ?
C2 C1 P1 104.75(11) . . ?
C2 C1 P2 112.26(12) . . ?
N1 C2 C1 114.19(14) . . ?
N1 C2 H2A 108.7 . . ?
N1 C2 H2B 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N1 C3 H3A 126.4 . . ?
C4 C3 N1 107.15(17) . . ?
C4 C3 H3A 126.4 . . ?
N2 C4 H4A 126.7 . . ?
C3 C4 N2 106.61(17) . . ?
C3 C4 H4A 126.7 . . ?
N1 C5 H5 126.0 . . ?
N2 C5 N1 108.07(17) . . ?
N2 C5 H5 126.0 . . ?

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
P1 C1 C2 N1 -177.82(12) . . . . ?
P2 C1 C2 N1 60.26(18) . . . . ?
O1 P1 C1 P2 52.64(11) . . . . ?
O1 P1 C1 O4 176.21(10) . . . . ?
O1 P1 C1 C2 -69.36(13) . . . . ?
O2 P1 O1 Mg1 -167.70(9) . . . . ?
O2 P1 C1 P2 178.55(8) . . . . ?
O2 P1 C1 O4 -57.88(13) . . . . ?
O2 P1 C1 C2 56.55(13) . . . . ?
O3 P1 O1 Mg1 67.78(12) . . . . ?
O3 P1 C1 P2 -63.65(10) . . . . ?
O3 P1 C1 O4 59.92(12) . . . . ?
O3 P1 C1 C2 174.35(11) . . . . ?
O4 C1 C2 N1 -62.67(18) . . . . ?
O5 P2 C1 P1 -54.01(11) . . . . ?
O5 P2 C1 O4 -175.82(11) . . . . ?
O5 P2 C1 C2 63.61(13) . . . . ?
O6 P2 O5 Mg1 171.77(9) . . . . ?
O6 P2 C1 P1 179.20(8) . . . . ?
O6 P2 C1 O4 57.38(13) . . . . ?
O6 P2 C1 C2 -63.19(14) . . . . ?
O7 P2 O5 Mg1 -63.84(12) . . . . ?
O7 P2 C1 P1 60.35(10) . . . . ?
O7 P2 C1 O4 -61.47(13) . . . . ?
O7 P2 C1 C2 177.96(11) . . . . ?
N1 C3 C4 N2 -0.5(2) . . . . ?
C1 P1 O1 Mg1 -46.54(13) . . . . ?
C1 P2 O5 Mg1 49.04(13) . . . . ?
C2 N1 C3 C4 -176.27(17) . . . . ?
C2 N1 C5 N2 176.40(16) . . . . ?
C3 N1 C2 C1 71.5(2) . . . . ?
C3 N1 C5 N2 -0.5(2) . . . . ?
C4 N2 C5 N1 0.2(2) . . . . ?
C5 N1 C2 C1 -104.9(2) . . . . ?
C5 N1 C3 C4 0.7(2) . . . . ?
C5 N2 C4 C3 0.2(2) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.417
_oxdiff_exptl_absorpt_empirical_full_min 0.733
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_ZOLE_Ca_form_2
_database_code_depnum_ccdc_archive 'CCDC 2120918'
loop_
_audit_author_name
_audit_author_address
'Vilmali Lopez-Mejias'
;University of Puerto Rico, Rio Piedras
Puerto Rico
;
_audit_update_record             
;
2021-11-08 deposited with the CCDC.	2022-02-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_ZOLE_Ca_form_2      
;
PROBLEM: Short Inter D-H..H-D       H2       ..H17A     .       1.99 Ang.
RESPONSE: A high degree of disorder is presenetd by O9 (uncoordinated water molecule) wich hampers correct assigment of short contacts. 
;
_vrf_PLAT417_ZOLE_Ca_form_2_2    
;
PROBLEM: Short Inter D-H..H-D       H16B     ..H17A     .       2.10 Ang.
RESPONSE: A high degree of disorder is presenetd by O9 (uncoordinated water molecule) wich hampers correct assigment of short contacts. 
;
# Added during the CSD deposition process: Monday 08 November 2021 06:48 PM
# end Validation Reply Form

_audit_creation_date             2020-03-28
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_chemical_name_common            ?
_chemical_name_systematic        'Zole-Ca form II'
_chemical_formula_moiety         'C10 H18 Ca N4 O14 P4, 3(H2 O)'
_chemical_formula_sum            'C10 H24 Ca N4 O17 P4'
_chemical_formula_weight         636.29
_chemical_melting_point          539.60
_chemical_oxdiff_formula         C5H10N2O7P2Ca
_chemical_oxdiff_usercomment     ZOLE_Ca_form_2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   10.2301(2)
_cell_length_b                   20.8833(5)
_cell_length_c                   22.4723(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4801.0(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7787
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.6790
_cell_measurement_theta_min      3.9390
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.002
_diffrn_reflns_theta_min         3.934
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -62.00 -36.00   0.50   12.00    --  -11.59 -38.00-155.00   52
  2  ω    -74.00 -49.00   0.50   12.00    --  -11.59 148.00-135.00   50
  3  ω    -49.00  -2.00   0.50   12.00    --  -11.59 123.00  60.00   94
  4  ω    -35.00   7.00   0.50   12.00    --  -11.59  84.00 173.00   84
  5  ω     34.00  59.00   0.50   12.00    --   11.59-123.00 -19.00   50
  6  ω      7.00  32.00   0.50   12.00    --   11.59-123.00 -19.00   50
  7  ω     17.00  43.00   0.50   12.00    --   11.59-148.00 177.00   52
  8  ω      4.00  29.00   0.50   12.00    --   11.59  84.00 173.00   50
  9  ω    -51.00 -15.00   0.50   12.00    --   11.59 -38.00-155.00   72
 10  ω    -10.00  17.00   0.50   12.00    --   11.59 -38.00-155.00   54
 11  ω     32.00  75.00   0.50   51.50    --   96.16 -84.00  53.00   86
 12  ω     78.00 117.00   0.50   51.50    --   96.16 123.00  60.00   78
 13  ω    112.00 151.00   0.50   51.50    --   96.16  84.00 173.00   78
 14  ω     48.00  86.00   0.50   51.50    --   96.16 -38.00-155.00   76
 15  ω     83.00 123.00   0.50   51.50    --   96.16  38.00  -0.00   80
 16  ω    127.00 157.00   0.50   51.50    --   96.16 148.00-135.00   60
 17  ω     24.00  50.00   0.50   12.00    --   11.59  30.00  60.00   52
 18  ω     -6.00  21.00   0.50   12.00    --   11.59 -84.00  53.00   54
 19  ω     13.00  38.00   0.50   12.00    --   11.59  38.00  -0.00   50
 20  ω      7.00  32.00   0.50   12.00    --   11.59-125.00-180.00   50
 21  ω      5.00  56.00   0.50   12.00    --   11.59-125.00 -60.00  102
 22  ω     35.00  60.00   0.50   51.50    --   96.16-117.00-180.00   50
 23  ω     82.00 157.00   0.50   51.50    --   96.16  17.00  90.00  150
 24  ω     82.00 107.00   0.50   51.50    --   96.16  17.00-180.00   50
 25  ω     88.00 144.00   0.50   51.50    --   96.16  33.00 -30.00  112
 26  ω    124.00 156.00   0.50   51.50    --   96.16  17.00-180.00   64
 27  ω     91.00 117.00   0.50   51.50    --   96.16-117.00-180.00   52
 28  ω     36.00 109.00   0.50   51.50    --   96.16 -42.00  60.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0147314000
_diffrn_orient_matrix_UB_12      0.0685624000
_diffrn_orient_matrix_UB_13      -0.0242647000
_diffrn_orient_matrix_UB_21      0.0716191000
_diffrn_orient_matrix_UB_22      0.0263320000
_diffrn_orient_matrix_UB_23      0.0551521000
_diffrn_orient_matrix_UB_31      0.1317973000
_diffrn_orient_matrix_UB_32      -0.0067669000
_diffrn_orient_matrix_UB_33      -0.0325997000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3712
_reflns_number_total             4427
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0448
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0670P)²+5.7530P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1211
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O17(H17A,H17B), O16(H16A,H16B), O15(H15A,H15B)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C8(H8), C9(H9A), C10(H10)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O6(H6), O7(H7), O9(H9), O13(H13), O14(H14)
;
_atom_sites_solution_hydrogens   mixed
_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
Ca1 Ca 0.45342(6) 0.61481(3) 0.25055(3) 0.01432(16) Uani 1 1 d . . . . .
P1 P 0.71574(8) 0.72837(4) 0.23038(4) 0.01452(19) Uani 1 1 d . . . . .
P2 P 0.69808(8) 0.66525(4) 0.35107(3) 0.01427(19) Uani 1 1 d . . . . .
P3 P 0.32403(8) 0.52680(4) 0.37267(4) 0.01622(19) Uani 1 1 d . . . . .
P4 P 0.02629(8) 0.51060(4) 0.37428(4) 0.01613(19) Uani 1 1 d . . . . .
O1 O 0.6233(2) 0.67562(11) 0.21287(10) 0.0194(5) Uani 1 1 d . . . . .
O2 O 0.6731(2) 0.79376(11) 0.20391(11) 0.0226(5) Uani 1 1 d . . . . .
H2 H 0.701773 0.797209 0.169977 0.034 Uiso 1 1 calc GR . . . .
O3 O 0.8580(2) 0.71347(11) 0.21977(10) 0.0183(5) Uani 1 1 d . . . . .
O4 O 0.5700(2) 0.63261(11) 0.33903(10) 0.0183(5) Uani 1 1 d . . . . .
O5 O 0.8198(2) 0.63008(11) 0.33221(10) 0.0175(5) Uani 1 1 d . . . . .
O6 O 0.7047(2) 0.68163(12) 0.41883(10) 0.0206(5) Uani 1 1 d . . . . .
H6 H 0.781259 0.682141 0.429648 0.031 Uiso 1 1 calc GR . . . .
O7 O 0.5733(2) 0.77422(10) 0.32418(10) 0.0180(5) Uani 1 1 d . . . . .
H7 H 0.512302 0.751141 0.314214 0.027 Uiso 1 1 calc GR . . . .
O8 O 0.3279(2) 0.54939(11) 0.30949(10) 0.0196(5) Uani 1 1 d . . . . .
O9 O 0.4357(2) 0.56046(11) 0.40979(10) 0.0198(5) Uani 1 1 d . . . . .
H9 H 0.468046 0.589387 0.389993 0.030 Uiso 1 1 calc GR . . . .
O10 O 0.3358(2) 0.45636(11) 0.38479(11) 0.0228(5) Uani 1 1 d . . . . .
O11 O 0.0188(2) 0.52634(11) 0.30861(10) 0.0178(5) Uani 1 1 d . . . . .
O12 O 0.0334(2) 0.44187(11) 0.39120(11) 0.0242(5) Uani 1 1 d . . . . .
O13 O -0.0944(2) 0.54225(11) 0.40689(10) 0.0199(5) Uani 1 1 d . . . . .
H13 H -0.116575 0.574651 0.388922 0.030 Uiso 1 1 calc GR . . . .
O14 O 0.1507(2) 0.62163(11) 0.39634(10) 0.0186(5) Uani 1 1 d . . . . .
H14 H 0.153156 0.629081 0.360533 0.028 Uiso 1 1 calc GR . . . .
N1 N 0.8802(3) 0.92940(14) 0.25972(14) 0.0232(6) Uani 1 1 d . . . . .
H1 H 0.923(4) 0.955(2) 0.235(2) 0.036(12) Uiso 1 1 d . . . . .
N2 N 0.8142(3) 0.84843(13) 0.31066(12) 0.0170(6) Uani 1 1 d . . . . .
N3 N 0.4513(3) 0.57831(15) 0.55565(13) 0.0222(6) Uani 1 1 d . . . . .
H3 H 0.520(5) 0.567(2) 0.577(2) 0.056(16) Uiso 1 1 d . . . . .
N4 N 0.2697(3) 0.57269(13) 0.50692(12) 0.0188(6) Uani 1 1 d . . . . .
C1 C 0.6951(3) 0.74255(15) 0.31121(14) 0.0162(6) Uani 1 1 d . . . . .
C2 C 0.8056(3) 0.78371(15) 0.33663(15) 0.0177(7) Uani 1 1 d . . . . .
H2A H 0.793284 0.787673 0.379265 0.021 Uiso 1 1 calc R . . . .
H2B H 0.888004 0.761812 0.330101 0.021 Uiso 1 1 calc R . . . .
C3 C 0.7279(3) 0.89729(17) 0.32079(17) 0.0238(7) Uani 1 1 d . . . . .
H3A H 0.654767 0.895838 0.345315 0.029 Uiso 1 1 calc R . . . .
C4 C 0.7688(3) 0.94796(17) 0.28854(18) 0.0274(8) Uani 1 1 d . . . . .
H4 H 0.728845 0.987885 0.286339 0.033 Uiso 1 1 calc R . . . .
C5 C 0.9059(3) 0.86916(16) 0.27315(15) 0.0205(7) Uani 1 1 d . . . . .
H5 H 0.975888 0.845267 0.258885 0.025 Uiso 1 1 calc R . . . .
C6 C 0.1685(3) 0.55439(15) 0.40617(14) 0.0164(6) Uani 1 1 d . . . . .
C7 C 0.1600(3) 0.54468(16) 0.47392(14) 0.0184(7) Uani 1 1 d . . . . .
H7A H 0.079220 0.563579 0.488193 0.022 Uiso 1 1 calc R . . . .
H7B H 0.156428 0.499135 0.482239 0.022 Uiso 1 1 calc R . . . .
C8 C 0.3601(3) 0.53894(17) 0.53630(15) 0.0209(7) Uani 1 1 d . . . . .
H8 H 0.358730 0.494855 0.542129 0.025 Uiso 1 1 calc R . . . .
C9 C 0.4212(4) 0.63948(17) 0.53793(15) 0.0240(7) Uani 1 1 d . . . . .
H9A H 0.470279 0.676127 0.545186 0.029 Uiso 1 1 calc R . . . .
C10 C 0.3065(3) 0.63647(17) 0.50791(16) 0.0223(7) Uani 1 1 d . . . . .
H10 H 0.261229 0.670644 0.491187 0.027 Uiso 1 1 calc R . . . .
O17 O 0.7265(3) 0.83424(13) 0.10295(13) 0.0352(7) Uani 1 1 d . . . . .
H17A H 0.809206 0.836729 0.105767 0.053 Uiso 1 1 d G . . . .
H17B H 0.693830 0.871652 0.103654 0.053 Uiso 1 1 d G . . . .
O16 O 0.9875(3) 0.67574(13) 0.56640(12) 0.0340(6) Uani 1 1 d . . . . .
H16A H 1.022230 0.698341 0.593620 0.051 Uiso 1 1 d G . . . .
H16B H 0.994737 0.636410 0.575162 0.051 Uiso 1 1 d G . . . .
O15 O 0.9490(2) 0.69980(13) 0.44958(11) 0.0272(6) Uani 1 1 d . . . . .
H15A H 0.955275 0.694723 0.487003 0.041 Uiso 1 1 d G . . . .
H15B H 1.005938 0.676960 0.432133 0.041 Uiso 1 1 d G . . . .


_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
Ca1 P1 3.4233(10) 6_556 ?
Ca1 P2 3.5323(10) . ?
Ca1 P3 3.5583(10) . ?
Ca1 O1 2.313(2) . ?
Ca1 O3 2.376(2) 6_556 ?
Ca1 O4 2.348(2) . ?
Ca1 O5 2.330(2) 6_556 ?
Ca1 O8 2.296(2) . ?
Ca1 O11 2.372(2) 6_656 ?
P1 O1 1.504(2) . ?
P1 O2 1.552(2) . ?
P1 O3 1.507(2) . ?
P1 C1 1.852(3) . ?
P2 O4 1.501(2) . ?
P2 O5 1.506(2) . ?
P2 O6 1.562(2) . ?
P2 C1 1.847(3) . ?
P3 O8 1.496(2) . ?
P3 O9 1.579(2) . ?
P3 O10 1.501(2) . ?
P3 C6 1.852(3) . ?
P4 O11 1.514(2) . ?
P4 O12 1.487(2) . ?
P4 O13 1.580(2) . ?
P4 C6 1.862(3) . ?
O2 H2 0.8200 . ?
O6 H6 0.8200 . ?
O7 H7 0.8200 . ?
O7 C1 1.441(4) . ?
O9 H9 0.8200 . ?
O13 H13 0.8200 . ?
O14 H14 0.8200 . ?
O14 C6 1.433(4) . ?
N1 H1 0.89(5) . ?
N1 C4 1.367(5) . ?
N1 C5 1.320(4) . ?
N2 C2 1.475(4) . ?
N2 C3 1.368(4) . ?
N2 C5 1.333(4) . ?
N3 H3 0.89(6) . ?
N3 C8 1.318(5) . ?
N3 C9 1.373(5) . ?
N4 C7 1.467(4) . ?
N4 C8 1.337(4) . ?
N4 C10 1.384(4) . ?
C1 C2 1.531(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9300 . ?
C3 C4 1.349(5) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.538(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8 0.9300 . ?
C9 H9A 0.9300 . ?
C9 C10 1.355(5) . ?
C10 H10 0.9300 . ?
O17 H17A 0.8503 . ?
O17 H17B 0.8498 . ?
O16 H16A 0.8502 . ?
O16 H16B 0.8478 . ?
O15 H15A 0.8500 . ?
O15 H15B 0.8487 . ?

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
P1 Ca1 P2 102.51(2) 6_556 . ?
P1 Ca1 P3 89.83(2) 6_556 . ?
P2 Ca1 P3 85.66(2) . . ?
O1 Ca1 P1 101.49(6) . 6_556 ?
O1 Ca1 P2 62.48(6) . . ?
O1 Ca1 P3 147.72(6) . . ?
O1 Ca1 O3 86.30(8) . 6_556 ?
O1 Ca1 O4 80.87(8) . . ?
O1 Ca1 O5 94.22(8) . 6_556 ?
O1 Ca1 O11 90.62(8) . 6_656 ?
O3 Ca1 P1 21.89(5) 6_556 6_556 ?
O3 Ca1 P2 81.55(6) 6_556 . ?
O3 Ca1 P3 94.50(6) 6_556 . ?
O4 Ca1 P1 98.35(6) . 6_556 ?
O4 Ca1 P2 18.44(5) . . ?
O4 Ca1 P3 67.52(6) . . ?
O4 Ca1 O3 80.44(8) . 6_556 ?
O4 Ca1 O11 117.03(8) . 6_656 ?
O5 Ca1 P1 65.70(6) 6_556 6_556 ?
O5 Ca1 P2 152.30(6) 6_556 . ?
O5 Ca1 P3 117.90(6) 6_556 . ?
O5 Ca1 O3 82.20(8) 6_556 6_556 ?
O5 Ca1 O4 162.21(8) 6_556 . ?
O5 Ca1 O11 79.91(8) 6_556 6_656 ?
O8 Ca1 P1 86.71(6) . 6_556 ?
O8 Ca1 P2 101.82(6) . . ?
O8 Ca1 P3 16.17(6) . . ?
O8 Ca1 O1 163.39(9) . . ?
O8 Ca1 O3 97.13(8) . 6_556 ?
O8 Ca1 O4 83.68(8) . . ?
O8 Ca1 O5 102.33(8) . 6_556 ?
O8 Ca1 O11 91.00(8) . 6_656 ?
O11 Ca1 P1 144.08(6) 6_656 6_556 ?
O11 Ca1 P2 113.01(6) 6_656 . ?
O11 Ca1 P3 97.74(6) 6_656 . ?
O11 Ca1 O3 161.56(8) 6_656 6_556 ?
O1 P1 Ca1 88.40(10) . 6_656 ?
O1 P1 O2 111.56(14) . . ?
O1 P1 O3 114.49(13) . . ?
O1 P1 C1 107.58(14) . . ?
O2 P1 Ca1 148.98(10) . 6_656 ?
O2 P1 C1 101.72(14) . . ?
O3 P1 Ca1 36.00(9) . 6_656 ?
O3 P1 O2 113.09(13) . . ?
O3 P1 C1 107.34(14) . . ?
C1 P1 Ca1 93.95(10) . 6_656 ?
O4 P2 Ca1 29.66(9) . . ?
O4 P2 O5 116.69(14) . . ?
O4 P2 O6 108.24(13) . . ?
O4 P2 C1 107.17(14) . . ?
O5 P2 Ca1 105.09(10) . . ?
O5 P2 O6 110.19(13) . . ?
O5 P2 C1 107.65(14) . . ?
O6 P2 Ca1 136.01(9) . . ?
O6 P2 C1 106.39(14) . . ?
C1 P2 Ca1 86.50(10) . . ?
O8 P3 Ca1 25.29(9) . . ?
O8 P3 O9 109.99(13) . . ?
O8 P3 O10 118.62(14) . . ?
O8 P3 C6 108.06(14) . . ?
O9 P3 Ca1 84.75(9) . . ?
O9 P3 C6 105.55(14) . . ?
O10 P3 Ca1 128.05(10) . . ?
O10 P3 O9 106.39(13) . . ?
O10 P3 C6 107.47(14) . . ?
C6 P3 Ca1 118.19(10) . . ?
O11 P4 O13 108.75(13) . . ?
O11 P4 C6 107.95(14) . . ?
O12 P4 O11 117.48(14) . . ?
O12 P4 O13 108.87(14) . . ?
O12 P4 C6 109.74(14) . . ?
O13 P4 C6 103.09(14) . . ?
P1 O1 Ca1 141.15(13) . . ?
P1 O2 H2 109.5 . . ?
P1 O3 Ca1 122.11(13) . 6_656 ?
P2 O4 Ca1 131.89(13) . . ?
P2 O5 Ca1 140.92(14) . 6_656 ?
P2 O6 H6 109.5 . . ?
C1 O7 H7 109.5 . . ?
P3 O8 Ca1 138.55(14) . . ?
P3 O9 H9 109.5 . . ?
P4 O11 Ca1 136.86(13) . 6_556 ?
P4 O13 H13 109.5 . . ?
C6 O14 H14 109.5 . . ?
C4 N1 H1 122(3) . . ?
C5 N1 H1 128(3) . . ?
C5 N1 C4 109.1(3) . . ?
C3 N2 C2 125.4(3) . . ?
C5 N2 C2 126.1(3) . . ?
C5 N2 C3 108.5(3) . . ?
C8 N3 H3 125(3) . . ?
C8 N3 C9 109.0(3) . . ?
C9 N3 H3 126(3) . . ?
C8 N4 C7 124.6(3) . . ?
C8 N4 C10 108.1(3) . . ?
C10 N4 C7 126.9(3) . . ?
P2 C1 P1 109.51(17) . . ?
O7 C1 P1 111.7(2) . . ?
O7 C1 P2 108.5(2) . . ?
O7 C1 C2 107.8(3) . . ?
C2 C1 P1 111.8(2) . . ?
C2 C1 P2 107.3(2) . . ?
N2 C2 C1 114.3(3) . . ?
N2 C2 H2A 108.7 . . ?
N2 C2 H2B 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N2 C3 H3A 126.4 . . ?
C4 C3 N2 107.2(3) . . ?
C4 C3 H3A 126.4 . . ?
N1 C4 H4 126.6 . . ?
C3 C4 N1 106.9(3) . . ?
C3 C4 H4 126.6 . . ?
N1 C5 N2 108.3(3) . . ?
N1 C5 H5 125.8 . . ?
N2 C5 H5 125.8 . . ?
P3 C6 P4 111.23(17) . . ?
O14 C6 P3 110.6(2) . . ?
O14 C6 P4 108.8(2) . . ?
O14 C6 C7 105.9(3) . . ?
C7 C6 P3 114.2(2) . . ?
C7 C6 P4 105.8(2) . . ?
N4 C7 C6 113.8(3) . . ?
N4 C7 H7A 108.8 . . ?
N4 C7 H7B 108.8 . . ?
C6 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N3 C8 N4 108.9(3) . . ?
N3 C8 H8 125.5 . . ?
N4 C8 H8 125.5 . . ?
N3 C9 H9A 126.4 . . ?
C10 C9 N3 107.2(3) . . ?
C10 C9 H9A 126.4 . . ?
N4 C10 H10 126.6 . . ?
C9 C10 N4 106.7(3) . . ?
C9 C10 H10 126.6 . . ?
H17A O17 H17B 109.5 . . ?
H16A O16 H16B 109.5 . . ?
H15A O15 H15B 109.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 P1 O1 Ca1 101.9(2) 6_656 . . . ?
Ca1 P1 C1 P2 -41.80(14) 6_656 . . . ?
Ca1 P1 C1 O7 -162.05(19) 6_656 . . . ?
Ca1 P1 C1 C2 77.0(2) 6_656 . . . ?
Ca1 P2 O5 Ca1 56.3(2) . . . 6_656 ?
Ca1 P2 C1 P1 -52.42(14) . . . . ?
Ca1 P2 C1 O7 69.78(19) . . . . ?
Ca1 P2 C1 C2 -174.0(2) . . . . ?
Ca1 P3 C6 P4 95.34(15) . . . . ?
Ca1 P3 C6 O14 -25.7(2) . . . . ?
Ca1 P3 C6 C7 -145.0(2) . . . . ?
P1 C1 C2 N2 61.7(3) . . . . ?
P2 C1 C2 N2 -178.2(2) . . . . ?
P3 C6 C7 N4 53.7(3) . . . . ?
P4 C6 C7 N4 176.4(2) . . . . ?
O1 P1 O3 Ca1 -47.22(19) . . . 6_656 ?
O1 P1 C1 P2 47.77(19) . . . . ?
O1 P1 C1 O7 -72.5(2) . . . . ?
O1 P1 C1 C2 166.6(2) . . . . ?
O2 P1 O1 Ca1 -102.5(2) . . . . ?
O2 P1 O3 Ca1 -176.51(13) . . . 6_656 ?
O2 P1 C1 P2 165.12(15) . . . . ?
O2 P1 C1 O7 44.9(2) . . . . ?
O2 P1 C1 C2 -76.0(2) . . . . ?
O3 P1 O1 Ca1 127.5(2) . . . . ?
O3 P1 C1 P2 -75.91(18) . . . . ?
O3 P1 C1 O7 163.8(2) . . . . ?
O3 P1 C1 C2 42.9(2) . . . . ?
O4 P2 O5 Ca1 85.7(2) . . . 6_656 ?
O4 P2 C1 P1 -73.97(18) . . . . ?
O4 P2 C1 O7 48.2(2) . . . . ?
O4 P2 C1 C2 164.5(2) . . . . ?
O5 P2 O4 Ca1 -72.9(2) . . . . ?
O5 P2 C1 P1 52.30(19) . . . . ?
O5 P2 C1 O7 174.51(19) . . . . ?
O5 P2 C1 C2 -69.3(2) . . . . ?
O6 P2 O4 Ca1 162.17(16) . . . . ?
O6 P2 O5 Ca1 -150.4(2) . . . 6_656 ?
O6 P2 C1 P1 170.41(14) . . . . ?
O6 P2 C1 O7 -67.4(2) . . . . ?
O6 P2 C1 C2 48.8(2) . . . . ?
O7 C1 C2 N2 -61.5(3) . . . . ?
O8 P3 C6 P4 70.07(19) . . . . ?
O8 P3 C6 O14 -51.0(2) . . . . ?
O8 P3 C6 C7 -170.3(2) . . . . ?
O9 P3 O8 Ca1 3.5(3) . . . . ?
O9 P3 C6 P4 -172.28(15) . . . . ?
O9 P3 C6 O14 66.7(2) . . . . ?
O9 P3 C6 C7 -52.7(3) . . . . ?
O10 P3 O8 Ca1 -119.2(2) . . . . ?
O10 P3 C6 P4 -59.0(2) . . . . ?
O10 P3 C6 O14 179.9(2) . . . . ?
O10 P3 C6 C7 60.6(3) . . . . ?
O11 P4 C6 P3 -63.43(19) . . . . ?
O11 P4 C6 O14 58.6(2) . . . . ?
O11 P4 C6 C7 172.0(2) . . . . ?
O12 P4 O11 Ca1 160.63(16) . . . 6_556 ?
O12 P4 C6 P3 65.7(2) . . . . ?
O12 P4 C6 O14 -172.2(2) . . . . ?
O12 P4 C6 C7 -58.8(3) . . . . ?
O13 P4 O11 Ca1 36.5(2) . . . 6_556 ?
O13 P4 C6 P3 -178.40(15) . . . . ?
O13 P4 C6 O14 -56.4(2) . . . . ?
O13 P4 C6 C7 57.1(2) . . . . ?
O14 C6 C7 N4 -68.2(3) . . . . ?
N2 C3 C4 N1 -0.6(4) . . . . ?
N3 C9 C10 N4 -1.1(4) . . . . ?
C1 P1 O1 Ca1 8.3(3) . . . . ?
C1 P1 O3 Ca1 72.11(17) . . . 6_656 ?
C1 P2 O4 Ca1 47.8(2) . . . . ?
C1 P2 O5 Ca1 -34.8(3) . . . 6_656 ?
C2 N2 C3 C4 -179.2(3) . . . . ?
C2 N2 C5 N1 179.8(3) . . . . ?
C3 N2 C2 C1 71.7(4) . . . . ?
C3 N2 C5 N1 0.3(4) . . . . ?
C4 N1 C5 N2 -0.7(4) . . . . ?
C5 N1 C4 C3 0.8(4) . . . . ?
C5 N2 C2 C1 -107.7(4) . . . . ?
C5 N2 C3 C4 0.2(4) . . . . ?
C6 P3 O8 Ca1 118.2(2) . . . . ?
C6 P4 O11 Ca1 -74.7(2) . . . 6_556 ?
C7 N4 C8 N3 173.6(3) . . . . ?
C7 N4 C10 C9 -172.7(3) . . . . ?
C8 N3 C9 C10 1.2(4) . . . . ?
C8 N4 C7 C6 -112.6(4) . . . . ?
C8 N4 C10 C9 0.6(4) . . . . ?
C9 N3 C8 N4 -0.8(4) . . . . ?
C10 N4 C7 C6 59.7(4) . . . . ?
C10 N4 C8 N3 0.1(4) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.642
_oxdiff_exptl_absorpt_empirical_full_min 0.705
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
