# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_2ampyr31
_database_code_depnum_ccdc_archive 'CCDC 2154531'
loop_
_audit_author_name
_audit_author_address
'Daria Budzikur'
;University of Wroclaw
Poland
;
_audit_update_record             
;
2022-02-24 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C5 H7 N2), (H2 P2 O6), 2(H2 O)'
_chemical_formula_sum            'C10 H20 N4 O8 P2'
_chemical_formula_weight         386.24

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   7.574(2)
_cell_length_b                   21.682(4)
_cell_length_c                   5.1650(10)
_cell_angle_alpha                90
_cell_angle_beta                 94.22(2)
_cell_angle_gamma                90
_cell_volume                     845.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    2014
_cell_measurement_theta_min      4.0360
_cell_measurement_theta_max      70.9940

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_F_000             404
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.789
_shelx_estimated_absorpt_T_min   0.394
_shelx_estimated_absorpt_T_max   0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75513
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      80(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            4792
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         4.078
_diffrn_reflns_theta_max         71.347
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1607
_reflns_number_gt                1233
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0695P)²+0.2739P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1607
_refine_ls_number_parameters     134
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1257
_refine_ls_wR_factor_gt          0.1174
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.49339(10) 0.46131(3) 0.36558(14) 0.0213(2) Uani 1 1 d . . . . .
O1 O 0.4717(3) 0.40294(8) 0.5193(4) 0.0240(5) Uani 1 1 d . . . . .
O2 O 0.6558(3) 0.46353(8) 0.2119(4) 0.0248(5) Uani 1 1 d . . . . .
O3 O 0.3168(3) 0.47235(9) 0.1905(4) 0.0249(5) Uani 1 1 d . . . . .
H3P H 0.315(7) 0.495(2) 0.066(10) 0.076(16) Uiso 1 1 d . . . . .
N1 N 0.1824(3) 0.37147(10) 0.7498(5) 0.0240(5) Uani 1 1 d . . . . .
H1N H 0.279(5) 0.3852(16) 0.665(7) 0.044(10) Uiso 1 1 d . . . . .
C2 C 0.0164(4) 0.38940(12) 0.6694(6) 0.0247(6) Uani 1 1 d . . . . .
N2 N -0.0057(4) 0.42793(11) 0.4670(5) 0.0256(6) Uani 1 1 d . . . . .
H2N1 H 0.095(5) 0.4389(15) 0.396(7) 0.034(10) Uiso 1 1 d . . . . .
H2N2 H -0.112(5) 0.4385(14) 0.407(6) 0.023(8) Uiso 1 1 d . . . . .
C3 C -0.1258(4) 0.36656(13) 0.8032(6) 0.0276(7) Uani 1 1 d . . . . .
H3 H -0.244203 0.377840 0.750172 0.036(9) Uiso 1 1 calc R . . . .
C4 C -0.0909(4) 0.32794(13) 1.0102(6) 0.0291(7) Uani 1 1 d . . . . .
H4 H -0.186010 0.312537 1.101471 0.030(9) Uiso 1 1 calc R . . . .
C5 C 0.0840(4) 0.31070(13) 1.0901(6) 0.0280(7) Uani 1 1 d . . . . .
H5 H 0.107816 0.283717 1.233383 0.028(8) Uiso 1 1 calc R . . . .
C6 C 0.2175(4) 0.33349(12) 0.9579(6) 0.0265(7) Uani 1 1 d . . . . .
H6 H 0.336523 0.322945 1.010504 0.025(8) Uiso 1 1 calc R . . . .
O1W O 0.5484(3) 0.28003(9) 0.3958(4) 0.0314(5) Uani 1 1 d DG . . . .
H1W1 H 0.530181 0.317904 0.415369 0.036(10) Uiso 1 1 d DG . . . .
H1W2 H 0.545681 0.262857 0.541247 0.091(19) Uiso 1 1 d DG . . . .


_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 1.5096(19) . yes
P1 O2 1.513(2) . yes
P1 O3 1.577(2) . yes
P1 P1 2.1754(14) 3_666 yes
O3 H3P 0.81(5) . ?
N1 C2 1.352(4) . ?
N1 C6 1.365(4) . ?
N1 H1N 0.93(4) . ?
C2 N2 1.339(4) . ?
C2 C3 1.411(4) . ?
N2 H2N1 0.90(4) . ?
N2 H2N2 0.87(4) . ?
C3 C4 1.369(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.409(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.354(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
O1W H1W1 0.8400 . ?
O1W H1W2 0.8399 . ?

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 115.27(11) . . yes
O1 P1 O3 107.96(11) . . yes
O2 P1 O3 112.47(11) . . yes
O1 P1 P1 108.21(9) . 3_666 yes
O2 P1 P1 108.02(9) . 3_666 yes
O3 P1 P1 104.26(9) . 3_666 yes
P1 O3 H3P 121(4) . . ?
C2 N1 C6 122.6(3) . . ?
C2 N1 H1N 120(2) . . ?
C6 N1 H1N 117(2) . . ?
N2 C2 N1 118.6(3) . . ?
N2 C2 C3 123.0(3) . . ?
N1 C2 C3 118.4(3) . . ?
C2 N2 H2N1 115(2) . . ?
C2 N2 H2N2 120(2) . . ?
H2N1 N2 H2N2 125(3) . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 121.0(3) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 118.4(3) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
C5 C6 N1 120.5(3) . . ?
C5 C6 H6 119.7 . . ?
N1 C6 H6 119.7 . . ?
H1W1 O1W H1W2 108.1 . . ?

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
C6 N1 C2 N2 178.4(3) . . . . ?
C6 N1 C2 C3 -1.5(4) . . . . ?
N2 C2 C3 C4 -179.2(3) . . . . ?
N1 C2 C3 C4 0.8(4) . . . . ?
C2 C3 C4 C5 -0.2(4) . . . . ?
C3 C4 C5 C6 0.3(4) . . . . ?
C4 C5 C6 N1 -1.0(4) . . . . ?
C2 N1 C6 C5 1.7(4) . . . . ?
O1 P1 P1 O1 180.000(1) . . 3_666 3_666 yes
O2 P1 P1 O1 54.58(13) . . 3_666 3_666 yes
O3 P1 P1 O1 -65.25(13) . . 3_666 3_666 yes
O1 P1 P1 O2 -54.58(13) . . 3_666 3_666 yes
O2 P1 P1 O2 180.000(0) . . 3_666 3_666 yes
O3 P1 P1 O2 60.17(13) . . 3_666 3_666 yes
O1 P1 P1 O3 65.25(13) . . 3_666 3_666 yes
O2 P1 P1 O3 -60.17(13) . . 3_666 3_666 yes
O3 P1 P1 O3 180.000(1) . . 3_666 3_666 yes

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3P O2 0.81(5) 1.72(5) 2.522(3) 169(5) 3_665
N1 H1N O1 0.93(4) 1.73(4) 2.658(3) 173(3) .
N2 H2N1 O3 0.90(4) 2.18(4) 3.074(4) 173(3) .
N2 H2N2 O2 0.87(4) 2.04(4) 2.900(3) 171(3) 1_455
C3 H3 O1 0.95 2.44 3.377(4) 167.6 1_455
O1W H1W1 O1 0.84 1.98 2.811(3) 170.1 .
O1W H1W2 O1W 0.84 2.05 2.8922(19) 178.0 4_566

_refine_diff_density_max         0.450
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.077

####################################################################### 
# 
# 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_2amino61
_database_code_depnum_ccdc_archive 'CCDC 2154535'
loop_
_audit_author_name
_audit_author_address
'Daria Budzikur'
;University of Wroclaw
Poland
;
_audit_update_record             
;
2022-02-24 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C5 H7 N2), (H2 P2 O6), 2(C5 H6 N2)'
_chemical_formula_sum            'C20 H28 N8 O6 P2'
_chemical_formula_weight         538.44

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   10.060(2)
_cell_length_b                   11.679(3)
_cell_length_c                   11.180(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.07(2)
_cell_angle_gamma                90
_cell_volume                     1293.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5910
_cell_measurement_theta_min      4.4770
_cell_measurement_theta_max      77.2230

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_F_000             564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.977
_shelx_estimated_absorpt_T_min   0.648
_shelx_estimated_absorpt_T_max   0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.06367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur PX, Onyx'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Onyx
_diffrn_detector_area_resol_mean 8.1956
_diffrn_reflns_number            9914
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.464
_diffrn_reflns_theta_max         77.871
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2721
_reflns_number_gt                2473
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1065P)²+0.3305P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2721
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1557
_refine_ls_wR_factor_gt          0.1498
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.92031(4) 0.50731(4) 0.55443(4) 0.01464(19) Uani 1 1 d . . . . .
O1 O 0.91399(13) 0.39815(12) 0.62421(11) 0.0206(3) Uani 1 1 d . . . . .
O2 O 0.94752(12) 0.61712(11) 0.62749(10) 0.0180(3) Uani 1 1 d . . . . .
O3 O 0.78686(13) 0.52781(12) 0.45923(12) 0.0202(3) Uani 1 1 d . . . . .
H3P H 0.748(3) 0.468(3) 0.433(3) 0.036(7) Uiso 1 1 d . . . . .
N1A N 0.87098(15) 0.82920(14) 0.55340(13) 0.0183(3) Uani 1 1 d . . . . .
H1NA H 0.897(3) 0.760(3) 0.572(3) 0.053(9) Uiso 1 1 d . . . . .
C2A C 0.88344(17) 0.87320(16) 0.44429(15) 0.0180(4) Uani 1 1 d . . . . .
N2A N 0.94019(16) 0.81006(15) 0.36793(14) 0.0209(3) Uani 1 1 d . . . . .
H2A1 H 0.953(3) 0.842(3) 0.293(3) 0.034(7) Uiso 1 1 d . . . . .
H2A2 H 0.984(3) 0.745(3) 0.386(3) 0.044(8) Uiso 1 1 d . . . . .
C3A C 0.8340(2) 0.98522(16) 0.41537(17) 0.0214(4) Uani 1 1 d . . . . .
H3A H 0.841576 1.018702 0.339426 0.026 Uiso 1 1 calc R U . . .
C4A C 0.7753(2) 1.04463(17) 0.49749(17) 0.0260(4) Uani 1 1 d . . . . .
H4A H 0.741412 1.119536 0.478125 0.031 Uiso 1 1 calc R U . . .
C5A C 0.7644(2) 0.99582(17) 0.6111(2) 0.0270(5) Uani 1 1 d . . . . .
H5A H 0.722934 1.036683 0.668211 0.032 Uiso 1 1 calc R U . . .
C6A C 0.81456(19) 0.88927(18) 0.63624(16) 0.0230(4) Uani 1 1 d . . . . .
H6A H 0.810373 0.855830 0.712951 0.028 Uiso 1 1 calc R U . . .
N1B N 0.63803(14) 0.35749(14) 0.35381(13) 0.0188(3) Uani 1 1 d . . . . .
C2B C 0.66952(18) 0.27432(16) 0.28111(15) 0.0184(4) Uani 1 1 d . . . . .
N2B N 0.80203(17) 0.25318(15) 0.28202(15) 0.0228(4) Uani 1 1 d . . . . .
H2B1 H 0.828(3) 0.205(2) 0.225(2) 0.025(6) Uiso 1 1 d . . . . .
H2B2 H 0.861(3) 0.305(3) 0.318(2) 0.033(7) Uiso 1 1 d . . . . .
C3B C 0.5685(2) 0.21021(18) 0.20623(18) 0.0264(4) Uani 1 1 d . . . . .
H3B H 0.592390 0.152145 0.154361 0.032 Uiso 1 1 calc R U . . .
C4B C 0.4354(2) 0.2331(2) 0.20956(18) 0.0301(5) Uani 1 1 d . . . . .
H4B H 0.366118 0.191351 0.159288 0.036 Uiso 1 1 calc R U . . .
C5B C 0.40216(19) 0.31816(19) 0.28723(19) 0.0273(4) Uani 1 1 d . . . . .
H5B H 0.310736 0.334413 0.292138 0.033 Uiso 1 1 calc R U . . .
C6B C 0.50569(18) 0.37716(17) 0.35592(16) 0.0219(4) Uani 1 1 d . . . . .
H6B H 0.483506 0.435488 0.408298 0.026 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
P1 O1 1.5018(14) . yes
P1 O2 1.5195(13) . yes
P1 O3 1.5788(14) . yes
P1 P1 2.1824(9) 3_766 yes
O3 H3P 0.83(3) . ?
N1A C2A 1.350(2) . ?
N1A C6A 1.362(2) . ?
N1A H1NA 0.86(4) . ?
C2A N2A 1.330(2) . ?
C2A C3A 1.417(3) . ?
N2A H2A1 0.94(3) . ?
N2A H2A2 0.88(3) . ?
C3A C4A 1.365(3) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.414(3) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.354(3) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
N1B C2B 1.340(2) . ?
N1B C6B 1.355(2) . ?
C2B N2B 1.354(2) . ?
C2B C3B 1.413(3) . ?
N2B H2B1 0.93(3) . ?
N2B H2B2 0.89(3) . ?
C3B C4B 1.373(3) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.398(3) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.367(3) . ?
C5B H5B 0.9500 . ?
C6B H6B 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 P1 O2 117.21(8) . . yes
O1 P1 O3 111.76(8) . . yes
O2 P1 O3 106.64(7) . . yes
O1 P1 P1 108.98(6) . 3_766 yes
O2 P1 P1 106.56(6) . 3_766 yes
O3 P1 P1 104.89(6) . 3_766 yes
P1 O3 H3P 114(2) . . ?
C2A N1A C6A 122.27(17) . . ?
C2A N1A H1NA 120(2) . . ?
C6A N1A H1NA 117(2) . . ?
N2A C2A N1A 119.15(17) . . ?
N2A C2A C3A 122.59(17) . . ?
N1A C2A C3A 118.26(17) . . ?
C2A N2A H2A1 119.1(18) . . ?
C2A N2A H2A2 125.6(19) . . ?
H2A1 N2A H2A2 114(3) . . ?
C4A C3A C2A 119.47(18) . . ?
C4A C3A H3A 120.3 . . ?
C2A C3A H3A 120.3 . . ?
C3A C4A C5A 120.67(19) . . ?
C3A C4A H4A 119.7 . . ?
C5A C4A H4A 119.7 . . ?
C6A C5A C4A 118.20(19) . . ?
C6A C5A H5A 120.9 . . ?
C4A C5A H5A 120.9 . . ?
C5A C6A N1A 121.11(18) . . ?
C5A C6A H6A 119.4 . . ?
N1A C6A H6A 119.4 . . ?
C2B N1B C6B 118.08(16) . . ?
N1B C2B N2B 117.69(16) . . ?
N1B C2B C3B 121.46(17) . . ?
N2B C2B C3B 120.85(17) . . ?
C2B N2B H2B1 120.3(16) . . ?
C2B N2B H2B2 116.9(18) . . ?
H2B1 N2B H2B2 119(2) . . ?
C4B C3B C2B 118.99(18) . . ?
C4B C3B H3B 120.5 . . ?
C2B C3B H3B 120.5 . . ?
C3B C4B C5B 119.73(17) . . ?
C3B C4B H4B 120.1 . . ?
C5B C4B H4B 120.1 . . ?
C6B C5B C4B 117.75(18) . . ?
C6B C5B H5B 121.1 . . ?
C4B C5B H5B 121.1 . . ?
N1B C6B C5B 123.98(18) . . ?
N1B C6B H6B 118.0 . . ?
C5B C6B H6B 118.0 . . ?

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
C6A N1A C2A N2A 179.65(16) . . . . ?
C6A N1A C2A C3A -0.9(3) . . . . ?
N2A C2A C3A C4A 179.15(18) . . . . ?
N1A C2A C3A C4A -0.3(3) . . . . ?
C2A C3A C4A C5A 0.5(3) . . . . ?
C3A C4A C5A C6A 0.5(3) . . . . ?
C4A C5A C6A N1A -1.7(3) . . . . ?
C2A N1A C6A C5A 1.9(3) . . . . ?
C6B N1B C2B N2B -178.25(16) . . . . ?
C6B N1B C2B C3B 1.5(3) . . . . ?
N1B C2B C3B C4B -0.8(3) . . . . ?
N2B C2B C3B C4B 178.91(18) . . . . ?
C2B C3B C4B C5B -0.6(3) . . . . ?
C3B C4B C5B C6B 1.2(3) . . . . ?
C2B N1B C6B C5B -0.8(3) . . . . ?
C4B C5B C6B N1B -0.5(3) . . . . ?
O1 P1 P1 O1 180.000(0) . . 3_766 3_766 yes
O2 P1 P1 O1 -52.65(9) . . 3_766 3_766 yes
O3 P1 P1 O1 60.19(8) . . 3_766 3_766 yes
O1 P1 P1 O2 52.65(9) . . 3_766 3_766 yes
O2 P1 P1 O2 180.000(0) . . 3_766 3_766 yes
O3 P1 P1 O2 -67.16(8) . . 3_766 3_766 yes
O1 P1 P1 O3 -60.19(8) . . 3_766 3_766 yes
O2 P1 P1 O3 67.16(8) . . 3_766 3_766 yes
O3 P1 P1 O3 180.000(0) . . 3_766 3_766 yes

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3P N1B 0.83(3) 1.83(3) 2.640(2) 168(3) .
N1A H1NA O2 0.86(4) 1.83(4) 2.682(2) 174(3) .
N2A H2A1 O2 0.94(3) 1.91(3) 2.833(2) 167(3) 4_575
N2A H2A2 O1 0.88(3) 1.98(4) 2.833(2) 163(3) 3_766
N2B H2B1 O1 0.93(3) 1.95(3) 2.864(2) 170(2) 4_565
N2B H2B2 O2 0.89(3) 2.13(3) 2.962(2) 157(2) 3_766

_refine_diff_density_max         0.770
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_2ampyr11
_database_code_depnum_ccdc_archive 'CCDC 2154532'
loop_
_audit_author_name
_audit_author_address
'Daria Budzikur'
;University of Wroclaw
Poland
;
_audit_update_record             
;
2022-02-24 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C5 H7 N2), 2(H3 P2 O6), (H2 P2 O6), 2(H2 O)'
_chemical_formula_sum            'C20 H40 N8 O20 P6'
_chemical_formula_weight         898.42

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   15.716(2)
_cell_length_b                   17.045(2)
_cell_length_c                   13.827(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.460(10)
_cell_angle_gamma                90
_cell_volume                     3642.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    19071
_cell_measurement_theta_min      2.8560
_cell_measurement_theta_max      75.3940

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    3.577
_shelx_estimated_absorpt_T_min   0.716
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      80(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            37627
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.859
_diffrn_reflns_theta_max         75.963
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7508
_reflns_number_gt                6952
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+3.3496P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7508
_refine_ls_number_parameters     583
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_ref         0.0797
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1A P 0.81204(2) 0.52337(2) 0.24869(3) 0.01012(9) Uani 1 1 d . . . . .
O1A O 0.86864(7) 0.47093(7) 0.20008(8) 0.0131(2) Uani 1 1 d . . . . .
O2A O 0.84089(7) 0.53564(7) 0.35784(8) 0.0136(2) Uani 1 1 d . . . . .
O3A O 0.80269(7) 0.60708(7) 0.19869(9) 0.0130(2) Uani 1 1 d . . . . .
H3PA H 0.7981(17) 0.6043(16) 0.138(2) 0.044(8) Uiso 1 1 d . . . . .
P2A P 0.68137(2) 0.47535(2) 0.22237(3) 0.01095(9) Uani 1 1 d . . . . .
O4A O 0.62340(7) 0.52999(7) 0.26575(9) 0.0146(2) Uani 1 1 d . . . . .
O5A O 0.65476(7) 0.45621(7) 0.11457(8) 0.0158(2) Uani 1 1 d . . . . .
O6A O 0.69303(7) 0.39402(7) 0.27871(9) 0.0141(2) Uani 1 1 d . . . . .
H6PA H 0.7004(16) 0.3999(15) 0.340(2) 0.038(7) Uiso 1 1 d . . . . .
P1B P 0.78528(2) 0.53690(2) 0.59105(3) 0.01120(9) Uani 1 1 d . . . . .
O1B O 0.87520(7) 0.51073(7) 0.63363(8) 0.0144(2) Uani 1 1 d . . . . .
O2B O 0.73987(7) 0.58604(7) 0.66085(9) 0.0159(2) Uani 1 1 d . . . . .
H2PB H 0.7610(19) 0.5900(17) 0.722(2) 0.054(9) Uiso 1 1 d . . . . .
O3B O 0.77825(7) 0.58929(7) 0.49783(9) 0.0147(2) Uani 1 1 d . . . . .
H3PB H 0.799(2) 0.568(2) 0.448(2) 0.074(11) Uiso 1 1 d . . . . .
P2B P 0.70232(2) 0.43490(2) 0.55191(3) 0.01093(9) Uani 1 1 d . . . . .
O4B O 0.73168(7) 0.39443(7) 0.46686(8) 0.0144(2) Uani 1 1 d . . . . .
O5B O 0.70664(7) 0.38642(7) 0.64401(8) 0.0131(2) Uani 1 1 d . . . . .
O6B O 0.60874(7) 0.46826(7) 0.51640(9) 0.0143(2) Uani 1 1 d . . . . .
H6PB H 0.5873(17) 0.4748(16) 0.565(2) 0.042(8) Uiso 1 1 d . . . . .
P1C P 0.72645(2) 0.46278(2) 0.89296(3) 0.01167(9) Uani 1 1 d . . . . .
O1C O 0.63571(7) 0.48892(7) 0.85574(8) 0.0146(2) Uani 1 1 d . . . . .
O2C O 0.76934(7) 0.41473(7) 0.81975(9) 0.0163(2) Uani 1 1 d . . . . .
H2PC H 0.7435(19) 0.4079(17) 0.761(2) 0.054(9) Uiso 1 1 d . . . . .
O3C O 0.73806(8) 0.40935(7) 0.98553(9) 0.0156(2) Uani 1 1 d . . . . .
H3PC H 0.708(2) 0.4257(19) 1.027(2) 0.065(10) Uiso 1 1 d . . . . .
P2C P 0.80683(2) 0.56684(2) 0.92831(3) 0.01187(9) Uani 1 1 d . . . . .
O4C O 0.77468(7) 0.60875(7) 1.01084(8) 0.0137(2) Uani 1 1 d . . . . .
O5C O 0.79951(7) 0.61402(7) 0.83458(8) 0.0161(2) Uani 1 1 d . . . . .
O6C O 0.90135(7) 0.53789(7) 0.96580(9) 0.0167(2) Uani 1 1 d . . . . .
H6PC H 0.9225(19) 0.5215(18) 0.916(2) 0.061(9) Uiso 1 1 d . . . . .
N1A N 0.92343(9) 0.32226(8) 0.19742(10) 0.0141(3) Uani 1 1 d . . . . .
H1NA H 0.8998(14) 0.3711(14) 0.2001(16) 0.024(6) Uiso 1 1 d . . . . .
C2A C 0.87372(11) 0.25752(10) 0.19095(12) 0.0135(3) Uani 1 1 d . . . . .
N2A N 0.78913(9) 0.26429(9) 0.19281(11) 0.0168(3) Uani 1 1 d . . . . .
H2A1 H 0.7563(15) 0.2202(15) 0.1818(17) 0.032(6) Uiso 1 1 d . . . . .
H2A2 H 0.7666(16) 0.3080(16) 0.2039(18) 0.036(7) Uiso 1 1 d . . . . .
C3A C 0.91333(10) 0.18391(10) 0.18159(12) 0.0143(3) Uani 1 1 d . . . . .
H3A H 0.880112 0.137080 0.177751 0.018(5) Uiso 1 1 calc R . . . .
C4A C 0.99972(11) 0.18071(10) 0.17810(12) 0.0163(3) Uani 1 1 d . . . . .
H4A H 1.026361 0.131475 0.171318 0.012(5) Uiso 1 1 calc R . . . .
C5A C 1.04929(11) 0.24974(11) 0.18448(12) 0.0170(3) Uani 1 1 d . . . . .
H5A H 1.109274 0.247737 0.182047 0.022(5) Uiso 1 1 calc R . . . .
C6A C 1.00975(11) 0.31935(10) 0.19419(12) 0.0166(3) Uani 1 1 d . . . . .
H6A H 1.042426 0.366525 0.198796 0.023(6) Uiso 1 1 calc R . . . .
N1B N 0.88412(9) 0.32044(9) 0.44170(10) 0.0145(3) Uani 1 1 d . . . . .
H1NB H 0.8420(15) 0.3527(14) 0.4493(17) 0.027(6) Uiso 1 1 d . . . . .
C2B C 0.96331(10) 0.34840(10) 0.43381(11) 0.0136(3) Uani 1 1 d . . . . .
N2B N 0.97528(10) 0.42537(9) 0.42974(11) 0.0169(3) Uani 1 1 d . . . . .
H2B1 H 0.9291(15) 0.4584(14) 0.4204(17) 0.028(6) Uiso 1 1 d . . . . .
H2B2 H 1.0256(17) 0.4426(15) 0.4171(19) 0.039(7) Uiso 1 1 d . . . . .
C3B C 1.02983(10) 0.29304(10) 0.43077(12) 0.0162(3) Uani 1 1 d . . . . .
H3B H 1.086356 0.310386 0.425962 0.019(5) Uiso 1 1 calc R . . . .
C4B C 1.01279(11) 0.21475(11) 0.43473(13) 0.0185(3) Uani 1 1 d . . . . .
H4B H 1.057436 0.177799 0.431439 0.026(6) Uiso 1 1 calc R . . . .
C5B C 0.92951(11) 0.18801(11) 0.44369(13) 0.0197(4) Uani 1 1 d . . . . .
H5B H 0.917607 0.133518 0.446800 0.025(6) Uiso 1 1 calc R . . . .
C6B C 0.86703(11) 0.24204(11) 0.44772(12) 0.0173(3) Uani 1 1 d . . . . .
H6B H 0.810809 0.225344 0.454794 0.015(5) Uiso 1 1 calc R . . . .
N1C N 0.56695(9) 0.67401(9) 0.20236(11) 0.0169(3) Uani 1 1 d . . . . .
H1NC H 0.5922(15) 0.6289(14) 0.2179(17) 0.027(6) Uiso 1 1 d . . . . .
C2C C 0.61207(11) 0.74163(10) 0.21621(14) 0.0191(4) Uani 1 1 d . . . . .
N2C N 0.69798(10) 0.73849(10) 0.24847(15) 0.0278(4) Uani 1 1 d . . . . .
H2C1 H 0.7269(16) 0.6929(16) 0.2452(19) 0.039(7) Uiso 1 1 d . . . . .
H2C2 H 0.7270(16) 0.7824(16) 0.2635(18) 0.037(7) Uiso 1 1 d . . . . .
C3C C 0.56677(12) 0.81280(11) 0.19621(14) 0.0218(4) Uani 1 1 d . . . . .
H3C H 0.596697 0.861403 0.205807 0.024(6) Uiso 1 1 calc R . . . .
C4C C 0.47932(12) 0.81139(11) 0.16285(14) 0.0216(4) Uani 1 1 d . . . . .
H4C H 0.448733 0.859287 0.148471 0.027(6) Uiso 1 1 calc R . . . .
C5C C 0.43426(12) 0.73983(11) 0.14961(13) 0.0215(4) Uani 1 1 d . . . . .
H5C H 0.373474 0.738840 0.126930 0.034(6) Uiso 1 1 calc R . . . .
C6C C 0.47956(11) 0.67211(11) 0.16999(13) 0.0184(3) Uani 1 1 d . . . . .
H6C H 0.450268 0.623148 0.161653 0.029(6) Uiso 1 1 calc R . . . .
N1D N 0.62276(9) 0.69154(9) 0.96497(11) 0.0159(3) Uani 1 1 d . . . . .
H1ND H 0.6655(16) 0.6583(15) 0.9783(19) 0.038(7) Uiso 1 1 d . . . . .
C2D C 0.53997(10) 0.66582(10) 0.94189(12) 0.0148(3) Uani 1 1 d . . . . .
N2D N 0.52365(10) 0.58912(9) 0.94520(12) 0.0185(3) Uani 1 1 d . . . . .
H2D1 H 0.4687(17) 0.5744(15) 0.9282(18) 0.035(7) Uiso 1 1 d . . . . .
H2D2 H 0.5671(18) 0.5572(16) 0.9425(19) 0.044(7) Uiso 1 1 d . . . . .
C3D C 0.47472(11) 0.72298(10) 0.91719(13) 0.0170(3) Uani 1 1 d . . . . .
H3D H 0.415818 0.707419 0.900858 0.022(5) Uiso 1 1 calc R . . . .
C4D C 0.49596(11) 0.80037(11) 0.91670(13) 0.0197(4) Uani 1 1 d . . . . .
H4D H 0.451697 0.838332 0.898489 0.022(5) Uiso 1 1 calc R . . . .
C5D C 0.58292(12) 0.82504(11) 0.94289(13) 0.0205(4) Uani 1 1 d . . . . .
H5D H 0.597673 0.879125 0.944265 0.020(5) Uiso 1 1 calc R . . . .
C6D C 0.64470(11) 0.76915(11) 0.96602(13) 0.0190(4) Uani 1 1 d . . . . .
H6D H 0.703754 0.784097 0.983097 0.018(5) Uiso 1 1 calc R . . . .
O1W O 0.53517(8) 0.49533(7) 0.66794(9) 0.0172(2) Uiso 1 1 d DG . . . .
H1W1 H 0.483277 0.489264 0.673822 0.081(11) Uiso 1 1 d DG . . . .
H1W2 H 0.565477 0.496645 0.724628 0.045(7) Uiso 1 1 d DG . . . .
O2W O 0.96907(8) 0.48178(7) 0.82535(9) 0.0159(2) Uiso 1 1 d DG . . . .
H2W1 H 0.940267 0.489968 0.768896 0.037(7) Uiso 1 1 d DG . . . .
H2W2 H 1.020290 0.496098 0.825596 0.070(10) Uiso 1 1 d DG . . . .


_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
P1A O1A 1.5030(11) . yes
P1A O2A 1.5096(12) . yes
P1A O3A 1.5807(12) . yes
P1A P2A 2.1790(6) . yes
O3A H3PA 0.82(3) . ?
P2A O4A 1.5019(12) . yes
P2A O5A 1.5088(12) . yes
P2A O6A 1.5844(12) . yes
O6A H6PA 0.83(3) . ?
P1B O1B 1.4968(12) . yes
P1B O2B 1.5468(12) . yes
P1B O3B 1.5555(12) . yes
P1B P2B 2.1815(6) . yes
O2B H2PB 0.85(3) . ?
O3B H3PB 0.89(3) . ?
P2B O4B 1.5062(12) . yes
P2B O5B 1.5093(12) . yes
P2B O6B 1.5700(12) . yes
O6B H6PB 0.81(3) . ?
P1C O1C 1.4936(12) . yes
P1C O2C 1.5484(12) . yes
P1C O3C 1.5544(12) . yes
P1C P2C 2.1810(6) . yes
O2C H2PC 0.85(3) . ?
O3C H3PC 0.86(3) . ?
P2C O4C 1.5091(12) . yes
P2C O5C 1.5117(12) . yes
P2C O6C 1.5618(12) . yes
O6C H6PC 0.86(3) . ?
N1A C2A 1.346(2) . ?
N1A C6A 1.366(2) . ?
N1A H1NA 0.91(2) . ?
C2A N2A 1.339(2) . ?
C2A C3A 1.417(2) . ?
N2A H2A1 0.91(3) . ?
N2A H2A2 0.85(3) . ?
C3A C4A 1.368(2) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.405(2) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.357(2) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
N1B C2B 1.355(2) . ?
N1B C6B 1.369(2) . ?
N1B H1NB 0.88(2) . ?
C2B N2B 1.328(2) . ?
C2B C3B 1.415(2) . ?
N2B H2B1 0.91(2) . ?
N2B H2B2 0.89(3) . ?
C3B C4B 1.364(3) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.412(2) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.355(3) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
N1C C2C 1.349(2) . ?
N1C C6C 1.365(2) . ?
N1C H1NC 0.87(2) . ?
C2C N2C 1.344(2) . ?
C2C C3C 1.408(2) . ?
N2C H2C1 0.91(3) . ?
N2C H2C2 0.88(3) . ?
C3C C4C 1.368(3) . ?
C3C H3C 0.9500 . ?
C4C C5C 1.406(3) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.359(3) . ?
C5C H5C 0.9500 . ?
C6C H6C 0.9500 . ?
N1D C2D 1.355(2) . ?
N1D C6D 1.366(2) . ?
N1D H1ND 0.87(3) . ?
C2D N2D 1.335(2) . ?
C2D C3D 1.411(2) . ?
N2D H2D1 0.89(3) . ?
N2D H2D2 0.88(3) . ?
C3D C4D 1.361(3) . ?
C3D H3D 0.9500 . ?
C4D C5D 1.413(3) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.356(3) . ?
C5D H5D 0.9500 . ?
C6D H6D 0.9500 . ?
O1W H1W1 0.8405 . ?
O1W H1W2 0.8404 . ?
O2W H2W1 0.8399 . ?
O2W H2W2 0.8406 . ?

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
O1A P1A O2A 115.77(7) . . yes
O1A P1A O3A 110.91(6) . . yes
O2A P1A O3A 107.42(7) . . yes
O1A P1A P2A 108.55(5) . . yes
O2A P1A P2A 108.78(5) . . yes
O3A P1A P2A 104.84(5) . . yes
P1A O3A H3PA 111.9(19) . . ?
O4A P2A O5A 116.69(7) . . yes
O4A P2A O6A 111.75(7) . . yes
O5A P2A O6A 106.44(7) . . yes
O4A P2A P1A 108.78(5) . . yes
O5A P2A P1A 109.27(5) . . yes
O6A P2A P1A 103.02(5) . . yes
P2A O6A H6PA 111.9(18) . . ?
O1B P1B O2B 115.19(7) . . yes
O1B P1B O3B 114.65(7) . . yes
O2B P1B O3B 103.58(7) . . yes
O1B P1B P2B 109.82(5) . . yes
O2B P1B P2B 105.28(5) . . yes
O3B P1B P2B 107.62(5) . . yes
P1B O2B H2PB 121(2) . . ?
P1B O3B H3PB 115(2) . . ?
O4B P2B O5B 115.77(7) . . yes
O4B P2B O6B 108.90(7) . . yes
O5B P2B O6B 111.00(7) . . yes
O4B P2B P1B 107.73(5) . . yes
O5B P2B P1B 107.08(5) . . yes
O6B P2B P1B 105.83(5) . . yes
P2B O6B H6PB 107.2(19) . . ?
O1C P1C O2C 115.74(7) . . yes
O1C P1C O3C 114.87(7) . . yes
O2C P1C O3C 103.21(7) . . yes
O1C P1C P2C 108.21(5) . . yes
O2C P1C P2C 105.87(5) . . yes
O3C P1C P2C 108.38(5) . . yes
P1C O2C H2PC 121(2) . . ?
P1C O3C H3PC 112(2) . . ?
O4C P2C O5C 114.37(7) . . yes
O4C P2C O6C 109.11(7) . . yes
O5C P2C O6C 111.87(7) . . yes
O4C P2C P1C 107.13(5) . . yes
O5C P2C P1C 106.84(5) . . yes
O6C P2C P1C 107.14(5) . . yes
P2C O6C H6PC 109(2) . . ?
C2A N1A C6A 122.41(15) . . ?
C2A N1A H1NA 120.9(14) . . ?
C6A N1A H1NA 116.5(14) . . ?
N2A C2A N1A 119.63(15) . . ?
N2A C2A C3A 122.15(15) . . ?
N1A C2A C3A 118.22(15) . . ?
C2A N2A H2A1 117.4(15) . . ?
C2A N2A H2A2 121.7(17) . . ?
H2A1 N2A H2A2 121(2) . . ?
C4A C3A C2A 119.59(15) . . ?
C4A C3A H3A 120.2 . . ?
C2A C3A H3A 120.2 . . ?
C3A C4A C5A 120.44(16) . . ?
C3A C4A H4A 119.8 . . ?
C5A C4A H4A 119.8 . . ?
C6A C5A C4A 118.66(15) . . ?
C6A C5A H5A 120.7 . . ?
C4A C5A H5A 120.7 . . ?
C5A C6A N1A 120.67(16) . . ?
C5A C6A H6A 119.7 . . ?
N1A C6A H6A 119.7 . . ?
C2B N1B C6B 122.78(15) . . ?
C2B N1B H1NB 120.8(15) . . ?
C6B N1B H1NB 116.2(15) . . ?
N2B C2B N1B 119.34(15) . . ?
N2B C2B C3B 123.13(15) . . ?
N1B C2B C3B 117.53(15) . . ?
C2B N2B H2B1 120.1(14) . . ?
C2B N2B H2B2 118.2(17) . . ?
H2B1 N2B H2B2 119(2) . . ?
C4B C3B C2B 119.99(16) . . ?
C4B C3B H3B 120.0 . . ?
C2B C3B H3B 120.0 . . ?
C3B C4B C5B 120.72(16) . . ?
C3B C4B H4B 119.6 . . ?
C5B C4B H4B 119.6 . . ?
C6B C5B C4B 118.32(17) . . ?
C6B C5B H5B 120.8 . . ?
C4B C5B H5B 120.8 . . ?
C5B C6B N1B 120.63(16) . . ?
C5B C6B H6B 119.7 . . ?
N1B C6B H6B 119.7 . . ?
C2C N1C C6C 122.58(16) . . ?
C2C N1C H1NC 120.9(15) . . ?
C6C N1C H1NC 116.4(15) . . ?
N2C C2C N1C 118.93(16) . . ?
N2C C2C C3C 122.76(17) . . ?
N1C C2C C3C 118.32(16) . . ?
C2C N2C H2C1 120.1(16) . . ?
C2C N2C H2C2 119.4(16) . . ?
H2C1 N2C H2C2 120(2) . . ?
C4C C3C C2C 119.48(17) . . ?
C4C C3C H3C 120.3 . . ?
C2C C3C H3C 120.3 . . ?
C3C C4C C5C 120.71(17) . . ?
C3C C4C H4C 119.6 . . ?
C5C C4C H4C 119.6 . . ?
C6C C5C C4C 118.53(17) . . ?
C6C C5C H5C 120.7 . . ?
C4C C5C H5C 120.7 . . ?
C5C C6C N1C 120.39(16) . . ?
C5C C6C H6C 119.8 . . ?
N1C C6C H6C 119.8 . . ?
C2D N1D C6D 123.06(15) . . ?
C2D N1D H1ND 120.6(17) . . ?
C6D N1D H1ND 116.3(17) . . ?
N2D C2D N1D 119.42(15) . . ?
N2D C2D C3D 123.31(16) . . ?
N1D C2D C3D 117.26(16) . . ?
C2D N2D H2D1 116.8(16) . . ?
C2D N2D H2D2 116.6(18) . . ?
H2D1 N2D H2D2 123(2) . . ?
C4D C3D C2D 120.16(16) . . ?
C4D C3D H3D 119.9 . . ?
C2D C3D H3D 119.9 . . ?
C3D C4D C5D 120.92(16) . . ?
C3D C4D H4D 119.5 . . ?
C5D C4D H4D 119.5 . . ?
C6D C5D C4D 117.98(17) . . ?
C6D C5D H5D 121.0 . . ?
C4D C5D H5D 121.0 . . ?
C5D C6D N1D 120.59(16) . . ?
C5D C6D H6D 119.7 . . ?
N1D C6D H6D 119.7 . . ?
H1W1 O1W H1W2 108.0 . . ?
H2W1 O2W H2W2 108.0 . . ?

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
O1A P1A P2A O4A -176.76(7) . . . . yes
O2A P1A P2A O4A 56.48(7) . . . . yes
O3A P1A P2A O4A -58.18(7) . . . . yes
O1A P1A P2A O5A -48.33(7) . . . . yes
O2A P1A P2A O5A -175.09(7) . . . . yes
O3A P1A P2A O5A 70.24(7) . . . . yes
O1A P1A P2A O6A 64.54(7) . . . . yes
O2A P1A P2A O6A -62.22(7) . . . . yes
O3A P1A P2A O6A -176.89(6) . . . . yes
O1B P1B P2B O4B -68.12(7) . . . . yes
O2B P1B P2B O4B 167.30(7) . . . . yes
O3B P1B P2B O4B 57.30(7) . . . . yes
O1B P1B P2B O5B 57.03(7) . . . . yes
O2B P1B P2B O5B -67.54(7) . . . . yes
O3B P1B P2B O5B -177.54(7) . . . . yes
O1B P1B P2B O6B 175.50(7) . . . . yes
O2B P1B P2B O6B 50.93(7) . . . . yes
O3B P1B P2B O6B -59.07(7) . . . . yes
O1C P1C P2C O4C 63.67(7) . . . . yes
O2C P1C P2C O4C -171.66(7) . . . . yes
O3C P1C P2C O4C -61.49(7) . . . . yes
O1C P1C P2C O5C -59.31(7) . . . . yes
O2C P1C P2C O5C 65.36(7) . . . . yes
O3C P1C P2C O5C 175.53(7) . . . . yes
O1C P1C P2C O6C -179.35(7) . . . . yes
O2C P1C P2C O6C -54.68(7) . . . . yes
O3C P1C P2C O6C 55.49(7) . . . . yes
C6A N1A C2A N2A -178.81(15) . . . . ?
C6A N1A C2A C3A 0.7(2) . . . . ?
N2A C2A C3A C4A 178.67(16) . . . . ?
N1A C2A C3A C4A -0.8(2) . . . . ?
C2A C3A C4A C5A 0.5(2) . . . . ?
C3A C4A C5A C6A 0.0(2) . . . . ?
C4A C5A C6A N1A -0.2(2) . . . . ?
C2A N1A C6A C5A -0.2(2) . . . . ?
C6B N1B C2B N2B -179.03(15) . . . . ?
C6B N1B C2B C3B 0.7(2) . . . . ?
N2B C2B C3B C4B -179.64(16) . . . . ?
N1B C2B C3B C4B 0.7(2) . . . . ?
C2B C3B C4B C5B -1.2(3) . . . . ?
C3B C4B C5B C6B 0.3(3) . . . . ?
C4B C5B C6B N1B 1.0(3) . . . . ?
C2B N1B C6B C5B -1.5(3) . . . . ?
C6C N1C C2C N2C 179.86(17) . . . . ?
C6C N1C C2C C3C -0.1(3) . . . . ?
N2C C2C C3C C4C 179.52(19) . . . . ?
N1C C2C C3C C4C -0.6(3) . . . . ?
C2C C3C C4C C5C 0.8(3) . . . . ?
C3C C4C C5C C6C -0.5(3) . . . . ?
C4C C5C C6C N1C -0.1(3) . . . . ?
C2C N1C C6C C5C 0.4(3) . . . . ?
C6D N1D C2D N2D -178.15(16) . . . . ?
C6D N1D C2D C3D 0.6(2) . . . . ?
N2D C2D C3D C4D 179.01(17) . . . . ?
N1D C2D C3D C4D 0.3(2) . . . . ?
C2D C3D C4D C5D -1.5(3) . . . . ?
C3D C4D C5D C6D 1.7(3) . . . . ?
C4D C5D C6D N1D -0.8(3) . . . . ?
C2D N1D C6D C5D -0.4(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3A H3PA O4C 0.82(3) 1.74(3) 2.5547(16) 171(3) 1_554
O6A H6PA O4B 0.83(3) 1.74(3) 2.5620(17) 167(3) .
O2B H2PB O5C 0.85(3) 1.62(3) 2.4616(17) 170(3) .
O3B H3PB O2A 0.89(3) 1.61(3) 2.4988(16) 175(3) .
O6B H6PB O1W 0.81(3) 1.80(3) 2.6115(17) 176(3) .
O2C H2PC O5B 0.85(3) 1.65(3) 2.4978(17) 171(3) .
O3C H3PC O5A 0.86(3) 1.67(3) 2.5266(17) 176(3) 1_556
O6C H6PC O2W 0.86(3) 1.70(3) 2.5630(17) 174(3) .
N1A H1NA O1A 0.91(2) 1.77(2) 2.6788(18) 171(2) .
N2A H2A1 O5B 0.91(3) 2.01(3) 2.9013(19) 167(2) 4_565
N2A H2A2 O6A 0.85(3) 2.23(3) 3.0385(19) 158(2) .
C3A H3A O1B 0.95 2.59 3.415(2) 145.4 4_565
N1B H1NB O4B 0.88(2) 1.93(2) 2.7846(18) 163(2) .
N2B H2B1 O2A 0.91(2) 1.99(2) 2.8669(19) 161(2) .
N2B H2B2 O1B 0.89(3) 1.99(3) 2.8676(19) 169(2) 3_766
N1C H1NC O4A 0.87(2) 1.84(2) 2.7017(19) 166(2) .
N2C H2C1 O3A 0.91(3) 2.06(3) 2.934(2) 162(2) .
N2C H2C2 O5C 0.88(3) 2.23(3) 3.097(2) 168(2) 4_575
C3C H3C O2B 0.95 2.60 3.331(2) 134.0 4_575
C3C H3C O1W 0.95 2.64 3.320(2) 128.6 4_575
C6C H6C O1C 0.95 2.33 3.272(2) 173.3 3_666
N1D H1ND O4C 0.87(3) 1.89(3) 2.7468(18) 166(2) .
N2D H2D1 O5A 0.89(3) 1.99(3) 2.8811(19) 178(2) 3_666
N2D H2D2 O1C 0.88(3) 2.10(3) 2.8878(19) 148(2) .
C4D H4D O5B 0.95 2.58 3.468(2) 154.8 2_656
C6D H6D O3B 0.95 2.45 3.176(2) 133.5 4_576
O1W H1W1 O4A 0.84 2.03 2.8403(17) 161.4 3_666
O1W H1W2 O1C 0.84 1.95 2.7861(17) 174.6 .
O2W H2W1 O1B 0.84 1.99 2.8333(17) 178.2 .
O2W H2W2 O1A 0.84 1.93 2.7577(16) 169.3 3_766

_refine_diff_density_max         0.439
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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_2aminopyr12
_database_code_depnum_ccdc_archive 'CCDC 2154533'
loop_
_audit_author_name
_audit_author_address
'Daria Budzikur'
;University of Wroclaw
Poland
;
_audit_update_record             
;
2022-02-24 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C5 H7 N2), (H2P2O6), (H4 P2 O6)'
_chemical_formula_sum            'C10 H20 N4 O12 P4'
_chemical_formula_weight         512.18

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.528(2)
_cell_length_b                   8.333(2)
_cell_length_c                   9.306(3)
_cell_angle_alpha                107.37(3)
_cell_angle_beta                 105.74(2)
_cell_angle_gamma                102.95(2)
_cell_volume                     505.8(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13147
_cell_measurement_theta_min      5.8340
_cell_measurement_theta_max      72.926

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_F_000             264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    4.107
_shelx_estimated_absorpt_T_min   0.248
_shelx_estimated_absorpt_T_max   0.494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.37154
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            16674
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         5.898
_diffrn_reflns_theta_max         73.410
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1922
_reflns_number_gt                1921
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0577P)²+0.5199P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1922
_refine_ls_number_parameters     145
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0991
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1A P 0.00610(7) 0.37853(6) 0.51916(6) 0.01201(17) Uani 1 1 d . . . . .
O1A O -0.0425(2) 0.38950(18) 0.66892(16) 0.0156(3) Uani 1 1 d . . . . .
O2A O 0.2096(2) 0.37023(18) 0.53432(17) 0.0152(3) Uani 1 1 d . . . . .
O3A O -0.1447(2) 0.22204(18) 0.36189(17) 0.0167(3) Uani 1 1 d D . . . .
H3PA H -0.261807 0.193793 0.355403 0.025 Uiso 1 1 d DR U . . .
P1B P -0.39471(7) -0.00270(6) 0.60486(6) 0.01281(17) Uani 1 1 d . . . . .
O1B O -0.4966(2) -0.11556(19) 0.67519(18) 0.0181(3) Uani 1 1 d . . . . .
O2B O -0.2379(2) -0.06186(19) 0.54654(18) 0.0185(3) Uani 1 1 d D . . . .
H2PB H -0.236292 -0.166969 0.517487 0.028 Uiso 1 1 d DR U . . .
O3B O -0.2921(2) 0.19500(18) 0.72305(16) 0.0164(3) Uani 1 1 d D . . . .
H3PB H -0.214638 0.257922 0.695459 0.025 Uiso 1 1 d DR U . . .
N1 N 0.5202(3) 0.5985(2) 0.8162(2) 0.0156(4) Uani 1 1 d . . . . .
H1N H 0.432(4) 0.534(4) 0.737(3) 0.019 Uiso 1 1 d . U . . .
C2 C 0.4933(3) 0.6765(3) 0.9544(2) 0.0150(4) Uani 1 1 d . . . . .
N2 N 0.3132(3) 0.6346(2) 0.9589(2) 0.0189(4) Uani 1 1 d . . . . .
H2N1 H 0.221(4) 0.563(4) 0.875(4) 0.023 Uiso 1 1 d . U . . .
H2N2 H 0.306(4) 0.687(3) 1.057(3) 0.023 Uiso 1 1 d . U . . .
C3 C 0.6588(3) 0.7996(3) 1.0895(3) 0.0199(4) Uani 1 1 d . . . . .
H3 H 0.645476 0.857052 1.188848 0.024 Uiso 1 1 calc R U . . .
C4 C 0.8388(3) 0.8352(3) 1.0761(3) 0.0229(5) Uani 1 1 d . . . . .
H4 H 0.950448 0.917863 1.166870 0.027 Uiso 1 1 calc R U . . .
C5 C 0.8607(3) 0.7512(3) 0.9295(3) 0.0224(5) Uani 1 1 d . . . . .
H5 H 0.985656 0.775715 0.920256 0.027 Uiso 1 1 calc R U . . .
C6 C 0.6986(3) 0.6342(3) 0.8017(3) 0.0193(4) Uani 1 1 d . . . . .
H6 H 0.709714 0.576734 0.701300 0.023 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
P1A O1A 1.5167(15) . yes
P1A O2A 1.5192(14) . yes
P1A O3A 1.5579(16) . yes
P1A P1A 2.1750(11) 2_566 yes
O3A H3PA 0.8400 . ?
P1B O1B 1.4894(15) . yes
P1B O2B 1.5425(15) . yes
P1B O3B 1.5515(16) . yes
P1B P1B 2.1748(12) 2_456 yes
O2B H2PB 0.8400 . ?
O3B H3PB 0.8400 . ?
N1 C2 1.348(3) . ?
N1 C6 1.362(3) . ?
N1 H1N 0.78(3) . ?
C2 N2 1.337(3) . ?
C2 C3 1.412(3) . ?
N2 H2N1 0.83(3) . ?
N2 H2N2 0.91(3) . ?
C3 C4 1.368(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.408(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.356(3) . ?
C5 H5 0.9500 . ?
C6 H6 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
O1A P1A O2A 114.30(8) . . yes
O1A P1A O3A 113.99(8) . . yes
O2A P1A O3A 108.45(8) . . yes
O1A P1A P1A 106.62(7) . 2_566 yes
O2A P1A P1A 107.04(7) . 2_566 yes
O3A P1A P1A 105.86(7) . 2_566 yes
P1A O3A H3PA 116.5 . . ?
O1B P1B O2B 116.13(9) . . yes
O1B P1B O3B 112.85(8) . . yes
O2B P1B O3B 105.95(8) . . yes
O1B P1B P1B 110.06(7) . 2_456 yes
O2B P1B P1B 105.73(7) . 2_456 yes
O3B P1B P1B 105.33(7) . 2_456 yes
P1B O2B H2PB 124.4 . . ?
P1B O3B H3PB 115.4 . . ?
C2 N1 C6 122.96(19) . . ?
C2 N1 H1N 121(2) . . ?
C6 N1 H1N 116(2) . . ?
N2 C2 N1 119.36(19) . . ?
N2 C2 C3 122.71(19) . . ?
N1 C2 C3 117.93(19) . . ?
C2 N2 H2N1 118.1(19) . . ?
C2 N2 H2N2 115.0(17) . . ?
H2N1 N2 H2N2 127(2) . . ?
C4 C3 C2 119.4(2) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.9(2) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 118.3(2) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
C5 C6 N1 120.5(2) . . ?
C5 C6 H6 119.7 . . ?
N1 C6 H6 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N1 C2 N2 179.86(19) . . . . ?
C6 N1 C2 C3 -0.5(3) . . . . ?
N2 C2 C3 C4 179.7(2) . . . . ?
N1 C2 C3 C4 0.1(3) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 C6 0.2(3) . . . . ?
C4 C5 C6 N1 -0.6(3) . . . . ?
C2 N1 C6 C5 0.8(3) . . . . ?
O1A P1A P1A O1A 180.000(1) . . 2_566 2_566 yes
O2A P1A P1A O1A 57.27(9) . . 2_566 2_566 yes
O3A P1A P1A O1A -58.27(9) . . 2_566 2_566 yes
O1A P1A P1A O2A -57.27(9) . . 2_566 2_566 yes
O2A P1A P1A O2A 180.000(0) . . 2_566 2_566 yes
O3A P1A P1A O2A 64.45(9) . . 2_566 2_566 yes
O1A P1A P1A O3A 58.27(9) . . 2_566 2_566 yes
O2A P1A P1A O3A -64.45(9) . . 2_566 2_566 yes
O3A P1A P1A O3A 180.000(0) . . 2_566 2_566 yes
O1B P1B P1B O1B 180.000(0) . . 2_456 2_456 yes
O2B P1B P1B O1B -53.84(10) . . 2_456 2_456 yes
O3B P1B P1B O1B 58.08(10) . . 2_456 2_456 yes
O1B P1B P1B O2B 53.84(10) . . 2_456 2_456 yes
O2B P1B P1B O2B 180.000(0) . . 2_456 2_456 yes
O3B P1B P1B O2B -68.08(9) . . 2_456 2_456 yes
O1B P1B P1B O3B -58.08(10) . . 2_456 2_456 yes
O2B P1B P1B O3B 68.08(9) . . 2_456 2_456 yes
O3B P1B P1B O3B 180.000(0) . . 2_456 2_456 yes

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3A H3PA O1B 0.84 1.70 2.536(2) 173.6 2_456
O2B H2PB O2A 0.84 1.69 2.528(2) 174.6 2_556
O3B H3PB O1A 0.84 1.62 2.459(2) 171.6 .
N1 H1N O2A 0.78(3) 1.99(3) 2.769(3) 179(3) .
N2 H2N1 O1A 0.83(3) 2.17(3) 2.993(3) 173(3) .
N2 H2N2 O3B 0.91(3) 2.04(3) 2.941(3) 180(3) 2_567
C6 H6 O2A 0.95 2.56 3.372(3) 143.6 2_666

_refine_diff_density_max         0.469
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.082

####################################################################### 
# 
# 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_2am31_deh_em
_database_code_depnum_ccdc_archive 'CCDC 2154537'
loop_
_audit_author_name
_audit_author_address
'Daria Budzikur'
;University of Wroclaw
Poland
;
_audit_update_record             
;
2022-02-24 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C5 H7 N2), (H2 P2 O6)'
_chemical_formula_sum            'C10 H16 N4 O6 P2'
_chemical_formula_weight         350.21

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   14.254(2)
_cell_length_b                   14.405(2)
_cell_length_c                   11.118(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.81(2)
_cell_angle_gamma                90
_cell_volume                     2281.7(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4217
_cell_measurement_theta_min      4.332
_cell_measurement_theta_max      63.444

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_F_000             1092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.081
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.043
_exptl_absorpt_coefficient_mu    2.941
_shelx_estimated_absorpt_T_min   0.797
_shelx_estimated_absorpt_T_max   0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            39050
_diffrn_reflns_av_unetI/netI     0.1109
_diffrn_reflns_av_R_equivalents  0.1924
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.102
_diffrn_reflns_theta_max         64.981
_diffrn_reflns_theta_full        64.981
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3862
_reflns_number_gt                2179
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1270P)²+2.2392P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3862
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1580
_refine_ls_R_factor_gt           0.0844
_refine_ls_wR_factor_ref         0.2437
_refine_ls_wR_factor_gt          0.2148
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1A P 0.91954(12) 0.89166(12) 0.57239(16) 0.0223(5) Uani 1 1 d . . . . .
O1A O 0.9366(3) 0.9848(3) 0.6392(4) 0.0264(12) Uani 1 1 d . . . . .
H1PA H 0.973119 1.018009 0.599752 0.040 Uiso 1 1 calc R U . . .
O2A O 0.9747(3) 0.8852(3) 0.4573(4) 0.0251(11) Uani 1 1 d . . . . .
O3A O 0.9382(3) 0.8115(3) 0.6576(4) 0.0258(11) Uani 1 1 d . . . . .
P2A P 0.77061(12) 0.88219(13) 0.52089(17) 0.0261(5) Uani 1 1 d . . . . .
O4A O 0.7547(3) 0.9701(4) 0.4387(4) 0.0338(13) Uani 1 1 d . . . . .
H4PA H 0.721506 1.008847 0.474449 0.051 Uiso 1 1 calc R U . . .
O5A O 0.7110(3) 0.8867(4) 0.6313(4) 0.0315(12) Uani 1 1 d . . . . .
O6A O 0.7608(3) 0.7953(3) 0.4467(4) 0.0313(12) Uani 1 1 d . . . . .
P1B P 0.48616(13) 0.92571(13) 0.50178(19) 0.0293(5) Uani 1 1 d . . . . .
O1B O 0.5309(3) 0.8922(4) 0.6247(4) 0.0330(13) Uani 1 1 d . . . . .
H1PB H 0.589667 0.892843 0.620978 0.049 Uiso 1 1 calc R U . . .
O2B O 0.3809(3) 0.9145(3) 0.5099(5) 0.0338(13) Uani 1 1 d . . . . .
O3B O 0.5293(3) 0.8788(3) 0.3967(5) 0.0345(13) Uani 1 1 d . . . . .
N1A N 0.9058(4) 0.6348(4) 0.5960(5) 0.0262(14) Uani 1 1 d . . . . .
H1NA H 0.919370 0.691460 0.620524 0.031 Uiso 1 1 calc R U . . .
C2A C 0.9171(4) 0.6145(5) 0.4790(6) 0.0235(16) Uani 1 1 d . . . . .
N2A N 0.9513(4) 0.6783(4) 0.4057(5) 0.0297(15) Uani 1 1 d . . . . .
H2A1 H 0.966443 0.733638 0.433696 0.036 Uiso 1 1 calc R U . . .
H2A2 H 0.958724 0.665157 0.329343 0.036 Uiso 1 1 calc R U . . .
C3A C 0.8938(5) 0.5236(5) 0.4414(7) 0.0346(19) Uani 1 1 d . . . . .
H3A H 0.900976 0.505929 0.359887 0.041 Uiso 1 1 calc R U . . .
C4A C 0.8610(5) 0.4612(5) 0.5221(7) 0.0350(19) Uani 1 1 d . . . . .
H4A H 0.843298 0.400847 0.495662 0.042 Uiso 1 1 calc R U . . .
C5A C 0.8529(5) 0.4852(5) 0.6447(7) 0.0350(19) Uani 1 1 d . . . . .
H5A H 0.832732 0.440995 0.701821 0.042 Uiso 1 1 calc R U . . .
C6A C 0.8749(5) 0.5736(6) 0.6781(7) 0.0330(18) Uani 1 1 d . . . . .
H6A H 0.868554 0.592425 0.759288 0.040 Uiso 1 1 calc R U . . .
N1B N 0.6741(4) 0.6356(5) 0.5057(6) 0.0422(18) Uani 1 1 d . . . . .
H1NB H 0.698501 0.689814 0.488021 0.051 Uiso 1 1 calc R U . . .
C2B C 0.6521(5) 0.6185(6) 0.6179(8) 0.041(2) Uani 1 1 d . . . . .
N2B N 0.6662(5) 0.6885(5) 0.7026(6) 0.0432(18) Uani 1 1 d . . . . .
H2B1 H 0.689097 0.742409 0.680775 0.052 Uiso 1 1 calc R U . . .
H2B2 H 0.652126 0.678874 0.778141 0.052 Uiso 1 1 calc R U . . .
C3B C 0.6144(6) 0.5311(6) 0.6480(8) 0.045(2) Uani 1 1 d . . . . .
H3B H 0.597236 0.518046 0.728102 0.054 Uiso 1 1 calc R U . . .
C4B C 0.6032(6) 0.4656(7) 0.5594(10) 0.059(3) Uani 1 1 d . . . . .
H4B H 0.580136 0.405740 0.578742 0.070 Uiso 1 1 calc R U . . .
C5B C 0.6259(5) 0.4867(6) 0.4379(9) 0.048(2) Uani 1 1 d . . . . .
H5B H 0.617387 0.442974 0.374492 0.057 Uiso 1 1 calc R U . . .
C6B C 0.6604(6) 0.5737(7) 0.4190(8) 0.047(2) Uani 1 1 d . . . . .
H6B H 0.675486 0.590673 0.339314 0.057 Uiso 1 1 calc R U . . .
N1C N 0.2909(4) 0.8287(4) 0.3251(6) 0.0320(16) Uani 1 1 d . . . . .
H1NC H 0.328296 0.860215 0.374627 0.038 Uiso 1 1 calc R U . . .
C2C C 0.3288(5) 0.7664(5) 0.2499(7) 0.0331(19) Uani 1 1 d . . . . .
N2C N 0.4222(4) 0.7548(5) 0.2521(6) 0.0440(19) Uani 1 1 d . . . . .
H2C1 H 0.458050 0.787488 0.302100 0.053 Uiso 1 1 calc R U . . .
H2C2 H 0.447721 0.714384 0.203458 0.053 Uiso 1 1 calc R U . . .
C3C C 0.2666(6) 0.7170(6) 0.1733(7) 0.038(2) Uani 1 1 d . . . . .
H3C H 0.289545 0.671519 0.119807 0.046 Uiso 1 1 calc R U . . .
C4C C 0.1717(5) 0.7354(6) 0.1768(7) 0.039(2) Uani 1 1 d . . . . .
H4C H 0.129933 0.702952 0.123351 0.047 Uiso 1 1 calc R U . . .
C5C C 0.1352(5) 0.7994(5) 0.2555(8) 0.037(2) Uani 1 1 d . . . . .
H5C H 0.069643 0.810749 0.258350 0.045 Uiso 1 1 calc R U . . .
C6C C 0.1964(5) 0.8443(6) 0.3269(8) 0.039(2) Uani 1 1 d . . . . .
H6C H 0.173576 0.889126 0.381424 0.047 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
P1A O3A 1.512(5) . yes
P1A O2A 1.525(5) . yes
P1A O1A 1.549(5) . yes
P1A P2A 2.185(3) . yes
O1A H1PA 0.8400 . ?
P2A O6A 1.503(5) . yes
P2A O5A 1.516(5) . yes
P2A O4A 1.573(5) . yes
O4A H4PA 0.8400 . ?
P1B O3B 1.499(5) . yes
P1B O2B 1.514(5) . yes
P1B O1B 1.566(5) . yes
P1B P1B 2.177(4) 3_676 yes
O1B H1PB 0.8400 . ?
N1A C2A 1.348(8) . ?
N1A C6A 1.353(9) . ?
N1A H1NA 0.8800 . ?
C2A N2A 1.330(8) . ?
C2A C3A 1.411(10) . ?
N2A H2A1 0.8800 . ?
N2A H2A2 0.8800 . ?
C3A C4A 1.364(10) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.414(10) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.361(11) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
N1B C2B 1.319(10) . ?
N1B C6B 1.324(10) . ?
N1B H1NB 0.8800 . ?
C2B N2B 1.390(11) . ?
C2B C3B 1.413(12) . ?
N2B H2B1 0.8800 . ?
N2B H2B2 0.8800 . ?
C3B C4B 1.370(12) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.432(13) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.365(12) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
N1C C2C 1.352(9) . ?
N1C C6C 1.366(9) . ?
N1C H1NC 0.8800 . ?
C2C N2C 1.341(9) . ?
C2C C3C 1.403(11) . ?
N2C H2C1 0.8800 . ?
N2C H2C2 0.8800 . ?
C3C C4C 1.381(11) . ?
C3C H3C 0.9500 . ?
C4C C5C 1.384(11) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.329(11) . ?
C5C H5C 0.9500 . ?
C6C H6C 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
O3A P1A O2A 113.2(3) . . yes
O3A P1A O1A 109.8(3) . . yes
O2A P1A O1A 112.2(3) . . yes
O3A P1A P2A 105.5(2) . . yes
O2A P1A P2A 107.4(2) . . yes
O1A P1A P2A 108.5(2) . . yes
P1A O1A H1PA 109.5 . . ?
O6A P2A O5A 115.8(3) . . yes
O6A P2A O4A 110.0(3) . . yes
O5A P2A O4A 111.2(3) . . yes
O6A P2A P1A 105.6(2) . . yes
O5A P2A P1A 110.5(2) . . yes
O4A P2A P1A 102.9(2) . . yes
P2A O4A H4PA 109.5 . . ?
O3B P1B O2B 115.5(3) . . yes
O3B P1B O1B 112.0(3) . . yes
O2B P1B O1B 107.0(3) . . yes
O3B P1B P1B 110.5(2) . 3_676 yes
O2B P1B P1B 106.7(2) . 3_676 yes
O1B P1B P1B 104.5(2) . 3_676 yes
P1B O1B H1PB 109.5 . . ?
C2A N1A C6A 124.2(6) . . ?
C2A N1A H1NA 117.9 . . ?
C6A N1A H1NA 117.9 . . ?
N2A C2A N1A 119.9(6) . . ?
N2A C2A C3A 123.2(7) . . ?
N1A C2A C3A 116.9(6) . . ?
C2A N2A H2A1 120.0 . . ?
C2A N2A H2A2 120.0 . . ?
H2A1 N2A H2A2 120.0 . . ?
C4A C3A C2A 120.0(7) . . ?
C4A C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C3A C4A C5A 120.9(7) . . ?
C3A C4A H4A 119.5 . . ?
C5A C4A H4A 119.5 . . ?
C6A C5A C4A 117.8(7) . . ?
C6A C5A H5A 121.1 . . ?
C4A C5A H5A 121.1 . . ?
N1A C6A C5A 120.2(7) . . ?
N1A C6A H6A 119.9 . . ?
C5A C6A H6A 119.9 . . ?
C2B N1B C6B 122.0(8) . . ?
C2B N1B H1NB 119.0 . . ?
C6B N1B H1NB 119.0 . . ?
N1B C2B N2B 118.2(8) . . ?
N1B C2B C3B 119.6(9) . . ?
N2B C2B C3B 122.3(8) . . ?
C2B N2B H2B1 120.0 . . ?
C2B N2B H2B2 120.0 . . ?
H2B1 N2B H2B2 120.0 . . ?
C4B C3B C2B 118.7(9) . . ?
C4B C3B H3B 120.6 . . ?
C2B C3B H3B 120.6 . . ?
C3B C4B C5B 120.5(9) . . ?
C3B C4B H4B 119.7 . . ?
C5B C4B H4B 119.7 . . ?
C6B C5B C4B 115.7(9) . . ?
C6B C5B H5B 122.2 . . ?
C4B C5B H5B 122.2 . . ?
N1B C6B C5B 123.5(9) . . ?
N1B C6B H6B 118.3 . . ?
C5B C6B H6B 118.3 . . ?
C2C N1C C6C 122.2(7) . . ?
C2C N1C H1NC 118.9 . . ?
C6C N1C H1NC 118.9 . . ?
N2C C2C N1C 119.2(7) . . ?
N2C C2C C3C 123.8(7) . . ?
N1C C2C C3C 117.0(7) . . ?
C2C N2C H2C1 120.0 . . ?
C2C N2C H2C2 120.0 . . ?
H2C1 N2C H2C2 120.0 . . ?
C4C C3C C2C 119.2(7) . . ?
C4C C3C H3C 120.4 . . ?
C2C C3C H3C 120.4 . . ?
C3C C4C C5C 122.2(8) . . ?
C3C C4C H4C 118.9 . . ?
C5C C4C H4C 118.9 . . ?
C6C C5C C4C 116.7(7) . . ?
C6C C5C H5C 121.7 . . ?
C4C C5C H5C 121.7 . . ?
C5C C6C N1C 122.7(8) . . ?
C5C C6C H6C 118.6 . . ?
N1C C6C H6C 118.6 . . ?

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
O3A P1A P2A O6A -67.7(3) . . . . yes
O2A P1A P2A O6A 53.3(3) . . . . yes
O1A P1A P2A O6A 174.7(3) . . . . yes
O3A P1A P2A O5A 58.2(3) . . . . yes
O2A P1A P2A O5A 179.2(3) . . . . yes
O1A P1A P2A O5A -59.4(3) . . . . yes
O3A P1A P2A O4A 177.0(3) . . . . yes
O2A P1A P2A O4A -62.1(3) . . . . yes
O1A P1A P2A O4A 59.3(3) . . . . yes
C6A N1A C2A N2A -177.5(6) . . . . ?
C6A N1A C2A C3A 0.8(10) . . . . ?
N2A C2A C3A C4A 178.6(7) . . . . ?
N1A C2A C3A C4A 0.4(10) . . . . ?
C2A C3A C4A C5A -2.2(11) . . . . ?
C3A C4A C5A C6A 2.9(11) . . . . ?
C2A N1A C6A C5A -0.1(11) . . . . ?
C4A C5A C6A N1A -1.7(11) . . . . ?
C6B N1B C2B N2B -178.1(7) . . . . ?
C6B N1B C2B C3B 1.1(11) . . . . ?
N1B C2B C3B C4B 1.1(12) . . . . ?
N2B C2B C3B C4B -179.7(7) . . . . ?
C2B C3B C4B C5B -2.4(12) . . . . ?
C3B C4B C5B C6B 1.4(12) . . . . ?
C2B N1B C6B C5B -2.2(13) . . . . ?
C4B C5B C6B N1B 0.9(13) . . . . ?
C6C N1C C2C N2C 179.6(7) . . . . ?
C6C N1C C2C C3C -0.6(11) . . . . ?
N2C C2C C3C C4C -178.9(7) . . . . ?
N1C C2C C3C C4C 1.3(11) . . . . ?
C2C C3C C4C C5C -1.6(12) . . . . ?
C3C C4C C5C C6C 1.2(12) . . . . ?
C4C C5C C6C N1C -0.5(12) . . . . ?
C2C N1C C6C C5C 0.3(12) . . . . ?
O1B P1B P1B O1B 180.000(1) . . 3_676 3_676 yes
O2B P1B P1B O1B -66.9(3) . . 3_676 3_676 yes
O3B P1B P1B O1B 59.3(3) . . 3_676 3_676 yes
O1B P1B P1B O2B 66.9(3) . . 3_676 3_676 yes
O2B P1B P1B O2B 180.000(0) . . 3_676 3_676 yes
O3B P1B P1B O2B -53.8(4) . . 3_676 3_676 yes
O1B P1B P1B O3B -59.3(3) . . 3_676 3_676 yes
O2B P1B P1B O3B 53.8(4) . . 3_676 3_676 yes
O3B P1B P1B O3B 180.000(2) . . 3_676 3_676 yes

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1A H1PA O2A 0.84 1.71 2.517(6) 160.1 3_776
O4A H4PA O2B 0.84 1.84 2.627(6) 154.5 3_676
O1B H1PB O5A 0.84 1.73 2.567(6) 172.5 .
N1A H1NA O3A 0.88 1.80 2.672(7) 173.6 .
N2A H2A2 O3A 0.88 1.95 2.763(8) 152.7 4_575
N2A H2A1 O2A 0.88 2.20 3.052(7) 162.2 .
C3A H3A O1A 0.95 2.52 3.436(9) 160.7 4_575
N1B H1NB O6A 0.88 1.83 2.702(9) 173.7 .
N2B H2B2 O6A 0.88 2.42 3.000(9) 123.7 4_576
N2B H2B1 O5A 0.88 2.18 3.038(9) 166.2 .
C6B H6B O5A 0.95 2.41 3.350(10) 172.7 4_575
N1C H1NC O2B 0.88 1.83 2.688(8) 163.0 .
N2C H2C2 O1B 0.88 2.14 3.004(8) 165.6 4_575
N2C H2C1 O3B 0.88 1.95 2.820(9) 169.9 .
C3C H3C O2B 0.95 2.20 3.119(9) 163.6 4_575
C6C H6C O1A 0.95 2.41 3.137(9) 133.4 3_676

_refine_diff_density_max         0.769
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.130

####################################################################### 
# 
# 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_exp_452
_database_code_depnum_ccdc_archive 'CCDC 2154534'
loop_
_audit_author_name
_audit_author_address
'Daria Budzikur'
;University of Wroclaw
Poland
;
_audit_update_record             
;
2022-02-24 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'4(C5 H7 N2), 2(H3 P2 O6), (H2 P2 O6), 0.40 (H2 O)'
_chemical_formula_sum            'C20 H36.80 N8 O18.40 P6'
_chemical_formula_weight         869.59

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   13.737(5)
_cell_length_b                   10.658(3)
_cell_length_c                   24.822(9)
_cell_angle_alpha                90
_cell_angle_beta                 97.50(3)
_cell_angle_gamma                90
_cell_volume                     3603(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18276
_cell_measurement_theta_min      3.2050
_cell_measurement_theta_max      75.4430

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_F_000             1800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    3.561
_shelx_estimated_absorpt_T_min   0.249
_shelx_estimated_absorpt_T_max   0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            34209
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.245
_diffrn_reflns_theta_max         76.088
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7396
_reflns_number_gt                6098
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1861P)²+6.3481P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7396
_refine_ls_number_parameters     514
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0949
_refine_ls_wR_factor_ref         0.2951
_refine_ls_wR_factor_gt          0.2841
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1A P 0.22800(9) 0.75563(11) 0.32688(5) 0.0390(3) Uani 1 1 d . . . . .
O1A O 0.2179(3) 0.6226(3) 0.30877(13) 0.0491(8) Uani 1 1 d . . . . .
O2A O 0.3081(2) 0.8345(3) 0.30389(13) 0.0428(7) Uani 1 1 d . . . . .
H2PA H 0.358670 0.790541 0.303239 0.064 Uiso 1 1 calc R U . . .
O3A O 0.1351(2) 0.8383(3) 0.31086(13) 0.0441(7) Uani 1 1 d . . . . .
H3PA H 0.084434 0.795256 0.312896 0.066 Uiso 1 1 calc R U . . .
P2A P 0.26213(9) 0.75374(10) 0.41518(5) 0.0384(3) Uani 1 1 d . . . . .
O4A O 0.1684(3) 0.7480(3) 0.43958(14) 0.0460(8) Uani 1 1 d . . . . .
O5A O 0.3287(2) 0.6423(3) 0.42672(13) 0.0445(7) Uani 1 1 d . . . . .
O6A O 0.3174(2) 0.8791(3) 0.43247(13) 0.0431(7) Uani 1 1 d . . . . .
H6PA H 0.376902 0.871828 0.428476 0.065 Uiso 1 1 calc R U . . .
P1B P 0.57529(9) 0.74034(10) 0.33227(5) 0.0375(3) Uani 1 1 d . . . . .
O1B O 0.4725(2) 0.7330(3) 0.30253(13) 0.0424(7) Uani 1 1 d . . . . .
O2B O 0.6371(2) 0.8493(3) 0.31817(12) 0.0427(7) Uani 1 1 d . . . . .
O3B O 0.6267(2) 0.6118(3) 0.32296(12) 0.0411(7) Uani 1 1 d . . . . .
H3PB H 0.687870 0.620610 0.329112 0.062 Uiso 1 1 calc R U . . .
P2B P 0.56737(9) 0.75703(10) 0.41908(5) 0.0372(3) Uani 1 1 d . . . . .
O4B O 0.6690(2) 0.7567(3) 0.44917(13) 0.0428(7) Uani 1 1 d . . . . .
O5B O 0.5055(2) 0.8722(3) 0.42496(12) 0.0408(7) Uani 1 1 d . . . . .
O6B O 0.5156(2) 0.6361(3) 0.43683(13) 0.0414(7) Uani 1 1 d . . . . .
H6PB H 0.454728 0.648446 0.434085 0.062 Uiso 1 1 calc R U . . .
P1C P 0.91724(9) 0.77078(12) 0.42956(5) 0.0438(3) Uani 1 1 d . . . . .
O1C O 0.9347(3) 0.6483(3) 0.45753(16) 0.0601(10) Uani 1 1 d . . . . .
O2C O 0.8349(2) 0.8541(3) 0.44776(14) 0.0465(7) Uani 1 1 d . . . . .
H2PC H 0.785254 0.809835 0.450540 0.070 Uiso 1 1 calc R U . . .
O3C O 1.0061(2) 0.8625(3) 0.43727(14) 0.0474(8) Uani 1 1 d . . . . .
H3PC H 1.058478 0.821734 0.437756 0.071 Uiso 1 1 calc R U . . .
P2C P 0.88107(9) 0.73492(11) 0.34264(5) 0.0440(3) Uani 1 1 d . . . . .
O4C O 0.9739(3) 0.7225(4) 0.31843(17) 0.0581(9) Uani 1 1 d . . . . .
O5C O 0.8144(2) 0.6221(3) 0.33798(14) 0.0483(8) Uani 1 1 d . . . . .
O6C O 0.8243(2) 0.8532(3) 0.31803(14) 0.0472(8) Uani 1 1 d . . . . .
H6PC H 0.764091 0.844646 0.320153 0.071 Uiso 1 1 calc R U . . .
N1A N 0.2927(3) 0.3967(4) 0.36026(15) 0.0439(8) Uani 1 1 d . . . . .
H1NA H 0.288505 0.478974 0.361930 0.053 Uiso 1 1 calc R U . . .
C2A C 0.2970(3) 0.3305(4) 0.40698(18) 0.0414(9) Uani 1 1 d . . . . .
N2A N 0.2940(3) 0.3909(4) 0.45359(15) 0.0462(9) Uani 1 1 d . . . . .
H2A1 H 0.289146 0.473188 0.453856 0.055 Uiso 1 1 calc R U . . .
H2A2 H 0.296751 0.348497 0.484183 0.055 Uiso 1 1 calc R U . . .
C3A C 0.3017(3) 0.1976(5) 0.40291(19) 0.0462(10) Uani 1 1 d . . . . .
H3A H 0.303843 0.147157 0.434591 0.055 Uiso 1 1 calc R U . . .
C4A C 0.3031(3) 0.1429(5) 0.3534(2) 0.0477(11) Uani 1 1 d . . . . .
H4A H 0.306160 0.054117 0.350837 0.057 Uiso 1 1 calc R U . . .
C5A C 0.3000(4) 0.2156(5) 0.3062(2) 0.0487(11) Uani 1 1 d . . . . .
H5A H 0.301787 0.177335 0.271765 0.058 Uiso 1 1 calc R U . . .
C6A C 0.2944(4) 0.3426(5) 0.3110(2) 0.0487(11) Uani 1 1 d . . . . .
H6A H 0.291744 0.393790 0.279488 0.058 Uiso 1 1 calc R U . . .
N1B N 0.5466(3) 1.1091(4) 0.39103(15) 0.0420(8) Uani 1 1 d . . . . .
H1NB H 0.544359 1.026813 0.393389 0.050 Uiso 1 1 calc R U . . .
C2B C 0.5470(3) 1.1609(4) 0.34161(17) 0.0406(9) Uani 1 1 d . . . . .
N2B N 0.5449(3) 1.0891(4) 0.29793(15) 0.0454(9) Uani 1 1 d . . . . .
H2B1 H 0.543203 1.006928 0.301082 0.054 Uiso 1 1 calc R U . . .
H2B2 H 0.545177 1.123616 0.265741 0.054 Uiso 1 1 calc R U . . .
C3B C 0.5494(4) 1.2946(5) 0.33875(19) 0.0447(10) Uani 1 1 d . . . . .
H3B H 0.549383 1.335429 0.304718 0.054 Uiso 1 1 calc R U . . .
C4B C 0.5517(4) 1.3630(5) 0.3849(2) 0.0477(10) Uani 1 1 d . . . . .
H4B H 0.553162 1.451948 0.382878 0.057 Uiso 1 1 calc R U . . .
C5B C 0.5519(4) 1.3050(5) 0.4358(2) 0.0479(11) Uani 1 1 d . . . . .
H5B H 0.553653 1.353591 0.467964 0.058 Uiso 1 1 calc R U . . .
C6B C 0.5494(3) 1.1774(5) 0.43762(19) 0.0457(10) Uani 1 1 d . . . . .
H6B H 0.549704 1.135906 0.471501 0.055 Uiso 1 1 calc R U . . .
N1C N 0.8152(3) 0.3827(4) 0.37212(15) 0.0427(8) Uani 1 1 d . . . . .
H1NC H 0.824299 0.463968 0.369040 0.051 Uiso 1 1 calc R U . . .
C2C C 0.8163(3) 0.3334(4) 0.42232(18) 0.0427(10) Uani 1 1 d . . . . .
N2C N 0.8342(3) 0.4094(4) 0.46512(15) 0.0475(9) Uani 1 1 d . . . . .
H2C1 H 0.844825 0.489773 0.460310 0.057 Uiso 1 1 calc R U . . .
H2C2 H 0.835257 0.379160 0.498185 0.057 Uiso 1 1 calc R U . . .
C3C C 0.8002(3) 0.2027(5) 0.42634(19) 0.0444(10) Uani 1 1 d . . . . .
H3C H 0.799165 0.164517 0.460859 0.053 Uiso 1 1 calc R U . . .
C4C C 0.7861(3) 0.1326(5) 0.3804(2) 0.0479(11) Uani 1 1 d . . . . .
H4C H 0.775551 0.044867 0.383260 0.057 Uiso 1 1 calc R U . . .
C5C C 0.7868(4) 0.1862(5) 0.3288(2) 0.0486(11) Uani 1 1 d . . . . .
H5C H 0.777906 0.136276 0.296806 0.058 Uiso 1 1 calc R U . . .
C6C C 0.8006(3) 0.3126(5) 0.32639(19) 0.0472(11) Uani 1 1 d . . . . .
H6C H 0.799926 0.352044 0.292035 0.057 Uiso 1 1 calc R U . . .
N1D N 0.9486(5) 0.8155(8) 0.1744(3) 0.0554(17) Uani 0.742(10) 1 d D . P A 1
H1ND H 0.947475 0.865610 0.202480 0.067 Uiso 0.742(10) 1 calc R U P A 1
N2D N 0.9473(5) 0.9884(7) 0.1145(3) 0.068(2) Uani 0.742(10) 1 d D . P A 1
H2D1 H 0.947222 1.020088 0.081733 0.082 Uiso 0.742(10) 1 calc R U P A 1
H2D2 H 0.946554 1.038660 0.142569 0.082 Uiso 0.742(10) 1 calc R U P A 1
C2D C 0.9486(7) 0.8664(10) 0.1214(4) 0.050(2) Uani 0.742(10) 1 d D . P A 1
C3D C 0.9499(6) 0.7814(8) 0.0797(3) 0.0410(15) Uani 0.742(10) 1 d D . P A 1
H3D H 0.948342 0.811452 0.043566 0.049 Uiso 0.742(10) 1 calc R U P A 1
C4D C 0.9532(6) 0.6575(11) 0.0888(4) 0.0520(18) Uani 0.742(10) 1 d D . P A 1
H4D H 0.955663 0.602328 0.059008 0.062 Uiso 0.742(10) 1 calc R U P A 1
C5D C 0.9532(6) 0.6075(9) 0.1399(4) 0.059(2) Uani 0.742(10) 1 d D . P A 1
H5D H 0.955276 0.519391 0.145670 0.071 Uiso 0.742(10) 1 calc R U P A 1
C6D C 0.9502(6) 0.6884(10) 0.1813(4) 0.0533(18) Uani 0.742(10) 1 d D . P A 1
H6D H 0.949261 0.655681 0.216832 0.064 Uiso 0.742(10) 1 calc R U P A 1
N1E N 0.9511(19) 0.7347(17) 0.1925(9) 0.052(6) Uiso 0.258(10) 1 d D . P A 2
H1NE H 0.953743 0.705329 0.225780 0.063 Uiso 0.258(10) 1 calc R U P A 2
N2E N 0.9314(12) 0.9409(15) 0.2231(6) 0.051(5) Uiso 0.258(10) 1 d D . P A 2
H2E1 H 0.924528 1.022139 0.217524 0.061 Uiso 0.258(10) 1 calc R U P A 2
H2E2 H 0.932078 0.910167 0.256042 0.061 Uiso 0.258(10) 1 calc R U P A 2
C2E C 0.941(2) 0.8656(16) 0.1823(8) 0.059(8) Uiso 0.258(10) 1 d D . P A 2
C3E C 0.941(3) 0.901(2) 0.1289(8) 0.056(10) Uiso 0.258(10) 1 d D . P A 2
H3E H 0.936008 0.988260 0.120731 0.067 Uiso 0.258(10) 1 calc R U P A 2
C4E C 0.947(2) 0.8215(19) 0.0877(9) 0.044(7) Uiso 0.258(10) 1 d D . P A 2
H4E H 0.944542 0.851956 0.051628 0.052 Uiso 0.258(10) 1 calc R U P A 2
C5E C 0.956(4) 0.695(2) 0.0983(10) 0.11(2) Uiso 0.258(10) 1 d D . P A 2
H5E H 0.962248 0.637243 0.069818 0.127 Uiso 0.258(10) 1 calc R U P A 2
C6E C 0.957(3) 0.655(2) 0.1498(11) 0.069(10) Uiso 0.258(10) 1 d D . P A 2
H6E H 0.962049 0.567873 0.156886 0.083 Uiso 0.258(10) 1 calc R U P A 2
O1W O 0.9249(6) 0.9909(9) 0.2494(4) 0.045(3) Uiso 0.367(11) 1 d DG . P B 1
H1W1 H 0.897188 0.961097 0.274799 0.068 Uiso 0.367(11) 1 d DG U P B 1
H1W2 H 0.886148 1.041999 0.232069 0.068 Uiso 0.367(11) 1 d DG U P B 1


_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
P1A O1A 1.488(3) . yes
P1A O2A 1.551(3) . yes
P1A O3A 1.559(3) . yes
P1A P2A 2.1808(18) . yes
O2A H2PA 0.8400 . ?
O3A H3PA 0.8400 . ?
P2A O4A 1.494(4) . yes
P2A O5A 1.503(3) . yes
P2A O6A 1.568(3) . yes
O6A H6PA 0.8400 . ?
P1B O2B 1.507(3) . yes
P1B O1B 1.508(3) . yes
P1B O3B 1.572(3) . yes
P1B P2B 2.1790(19) . yes
O3B H3PB 0.8400 . ?
P2B O4B 1.495(3) . yes
P2B O5B 1.511(3) . yes
P2B O6B 1.563(3) . yes
O6B H6PB 0.8400 . ?
P1C O1C 1.484(4) . yes
P1C O2C 1.551(3) . yes
P1C O3C 1.556(3) . yes
P1C P2C 2.184(2) . yes
O2C H2PC 0.8400 . ?
O3C H3PC 0.8400 . ?
P2C O4C 1.485(4) . yes
P2C O5C 1.507(3) . yes
P2C O6C 1.564(3) . yes
O6C H6PC 0.8400 . ?
N1A C2A 1.352(6) . ?
N1A C6A 1.355(6) . ?
N1A H1NA 0.8800 . ?
C2A N2A 1.329(6) . ?
C2A C3A 1.422(7) . ?
N2A H2A1 0.8800 . ?
N2A H2A2 0.8800 . ?
C3A C4A 1.363(7) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.400(7) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.362(7) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
N1B C2B 1.345(6) . ?
N1B C6B 1.363(6) . ?
N1B H1NB 0.8800 . ?
C2B N2B 1.324(6) . ?
C2B C3B 1.428(6) . ?
N2B H2B1 0.8800 . ?
N2B H2B2 0.8800 . ?
C3B C4B 1.355(7) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.404(7) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.361(7) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
N1C C2C 1.351(6) . ?
N1C C6C 1.352(6) . ?
N1C H1NC 0.8800 . ?
C2C N2C 1.333(6) . ?
C2C C3C 1.417(7) . ?
N2C H2C1 0.8800 . ?
N2C H2C2 0.8800 . ?
C3C C4C 1.355(7) . ?
C3C H3C 0.9500 . ?
C4C C5C 1.404(7) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.363(7) . ?
C5C H5C 0.9500 . ?
C6C H6C 0.9500 . ?
N1D C6D 1.366(12) . ?
N1D C2D 1.421(10) . ?
N1D H1ND 0.8800 . ?
N2D C2D 1.312(12) . ?
N2D H2D1 0.8800 . ?
N2D H2D2 0.8800 . ?
C2D C3D 1.378(13) . ?
C3D C4D 1.340(12) . ?
C3D H3D 0.9500 . ?
C4D C5D 1.374(11) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.347(14) . ?
C5D H5D 0.9500 . ?
C6D H6D 0.9500 . ?
N1E C6E 1.366(12) . ?
N1E C2E 1.421(10) . ?
N1E H1NE 0.8800 . ?
N2E C2E 1.312(12) . ?
N2E H2E1 0.8800 . ?
N2E H2E2 0.8800 . ?
C2E C3E 1.378(13) . ?
C3E C4E 1.340(12) . ?
C3E H3E 0.9500 . ?
C4E C5E 1.374(11) . ?
C4E H4E 0.9500 . ?
C5E C6E 1.347(15) . ?
C5E H5E 0.9500 . ?
C6E H6E 0.9500 . ?
O1W H1W1 0.8400 . ?
O1W H1W2 0.8400 . ?

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
O1A P1A O2A 116.6(2) . . yes
O1A P1A O3A 114.83(19) . . yes
O2A P1A O3A 101.33(18) . . yes
O1A P1A P2A 107.10(14) . . yes
O2A P1A P2A 107.76(13) . . yes
O3A P1A P2A 108.85(14) . . yes
P1A O2A H2PA 109.5 . . ?
P1A O3A H3PA 109.5 . . ?
O4A P2A O5A 115.16(19) . . yes
O4A P2A O6A 109.64(19) . . yes
O5A P2A O6A 111.11(19) . . yes
O4A P2A P1A 108.91(15) . . yes
O5A P2A P1A 104.15(14) . . yes
O6A P2A P1A 107.46(13) . . yes
P2A O6A H6PA 109.5 . . ?
O2B P1B O1B 116.51(19) . . yes
O2B P1B O3B 111.14(18) . . yes
O1B P1B O3B 107.01(18) . . yes
O2B P1B P2B 105.61(13) . . yes
O1B P1B P2B 108.89(15) . . yes
O3B P1B P2B 107.33(13) . . yes
P1B O3B H3PB 109.5 . . ?
O4B P2B O5B 117.04(19) . . yes
O4B P2B O6B 106.68(18) . . yes
O5B P2B O6B 111.09(19) . . yes
O4B P2B P1B 109.26(15) . . yes
O5B P2B P1B 105.25(13) . . yes
O6B P2B P1B 107.14(13) . . yes
P2B O6B H6PB 109.5 . . ?
O1C P1C O2C 116.6(2) . . yes
O1C P1C O3C 114.8(2) . . yes
O2C P1C O3C 101.18(19) . . yes
O1C P1C P2C 108.09(18) . . yes
O2C P1C P2C 107.92(14) . . yes
O3C P1C P2C 107.77(15) . . yes
P1C O2C H2PC 109.5 . . ?
P1C O3C H3PC 109.5 . . ?
O4C P2C O5C 116.3(2) . . yes
O4C P2C O6C 108.9(2) . . yes
O5C P2C O6C 110.24(19) . . yes
O4C P2C P1C 108.59(18) . . yes
O5C P2C P1C 105.85(16) . . yes
O6C P2C P1C 106.41(15) . . yes
P2C O6C H6PC 109.5 . . ?
C2A N1A C6A 123.2(4) . . ?
C2A N1A H1NA 118.4 . . ?
C6A N1A H1NA 118.4 . . ?
N2A C2A N1A 119.4(4) . . ?
N2A C2A C3A 123.4(4) . . ?
N1A C2A C3A 117.1(4) . . ?
C2A N2A H2A1 120.0 . . ?
C2A N2A H2A2 120.0 . . ?
H2A1 N2A H2A2 120.0 . . ?
C4A C3A C2A 119.7(4) . . ?
C4A C3A H3A 120.1 . . ?
C2A C3A H3A 120.1 . . ?
C3A C4A C5A 121.0(5) . . ?
C3A C4A H4A 119.5 . . ?
C5A C4A H4A 119.5 . . ?
C6A C5A C4A 118.2(5) . . ?
C6A C5A H5A 120.9 . . ?
C4A C5A H5A 120.9 . . ?
N1A C6A C5A 120.6(4) . . ?
N1A C6A H6A 119.7 . . ?
C5A C6A H6A 119.7 . . ?
C2B N1B C6B 123.5(4) . . ?
C2B N1B H1NB 118.3 . . ?
C6B N1B H1NB 118.3 . . ?
N2B C2B N1B 120.5(4) . . ?
N2B C2B C3B 122.3(4) . . ?
N1B C2B C3B 117.2(4) . . ?
C2B N2B H2B1 120.0 . . ?
C2B N2B H2B2 120.0 . . ?
H2B1 N2B H2B2 120.0 . . ?
C4B C3B C2B 119.5(4) . . ?
C4B C3B H3B 120.2 . . ?
C2B C3B H3B 120.2 . . ?
C3B C4B C5B 121.4(5) . . ?
C3B C4B H4B 119.3 . . ?
C5B C4B H4B 119.3 . . ?
C6B C5B C4B 118.2(4) . . ?
C6B C5B H5B 120.9 . . ?
C4B C5B H5B 120.9 . . ?
C5B C6B N1B 120.2(4) . . ?
C5B C6B H6B 119.9 . . ?
N1B C6B H6B 119.9 . . ?
C2C N1C C6C 122.8(4) . . ?
C2C N1C H1NC 118.6 . . ?
C6C N1C H1NC 118.6 . . ?
N2C C2C N1C 118.6(4) . . ?
N2C C2C C3C 123.8(4) . . ?
N1C C2C C3C 117.7(4) . . ?
C2C N2C H2C1 120.0 . . ?
C2C N2C H2C2 120.0 . . ?
H2C1 N2C H2C2 120.0 . . ?
C4C C3C C2C 119.3(4) . . ?
C4C C3C H3C 120.3 . . ?
C2C C3C H3C 120.3 . . ?
C3C C4C C5C 121.8(5) . . ?
C3C C4C H4C 119.1 . . ?
C5C C4C H4C 119.1 . . ?
C6C C5C C4C 117.3(4) . . ?
C6C C5C H5C 121.3 . . ?
C4C C5C H5C 121.3 . . ?
N1C C6C C5C 121.1(4) . . ?
N1C C6C H6C 119.5 . . ?
C5C C6C H6C 119.5 . . ?
C6D N1D C2D 119.5(8) . . ?
C6D N1D H1ND 120.2 . . ?
C2D N1D H1ND 120.2 . . ?
C2D N2D H2D1 120.0 . . ?
C2D N2D H2D2 120.0 . . ?
H2D1 N2D H2D2 120.0 . . ?
N2D C2D C3D 123.6(8) . . ?
N2D C2D N1D 119.9(9) . . ?
C3D C2D N1D 116.5(8) . . ?
C4D C3D C2D 121.6(8) . . ?
C4D C3D H3D 119.2 . . ?
C2D C3D H3D 119.2 . . ?
C3D C4D C5D 122.3(11) . . ?
C3D C4D H4D 118.8 . . ?
C5D C4D H4D 118.8 . . ?
C6D C5D C4D 117.3(9) . . ?
C6D C5D H5D 121.3 . . ?
C4D C5D H5D 121.3 . . ?
C5D C6D N1D 122.7(7) . . ?
C5D C6D H6D 118.6 . . ?
N1D C6D H6D 118.6 . . ?
C6E N1E C2E 118.9(16) . . ?
C6E N1E H1NE 120.5 . . ?
C2E N1E H1NE 120.5 . . ?
C2E N2E H2E1 120.0 . . ?
C2E N2E H2E2 120.0 . . ?
H2E1 N2E H2E2 120.0 . . ?
N2E C2E C3E 125.9(17) . . ?
N2E C2E N1E 118.7(16) . . ?
C3E C2E N1E 115.4(15) . . ?
C4E C3E C2E 124(2) . . ?
C4E C3E H3E 117.8 . . ?
C2E C3E H3E 117.8 . . ?
C3E C4E C5E 119(2) . . ?
C3E C4E H4E 120.3 . . ?
C5E C4E H4E 120.3 . . ?
C6E C5E C4E 118.6(19) . . ?
C6E C5E H5E 120.7 . . ?
C4E C5E H5E 120.7 . . ?
C5E C6E N1E 123(2) . . ?
C5E C6E H6E 118.4 . . ?
N1E C6E H6E 118.4 . . ?
H1W1 O1W H1W2 108.1 . . ?

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
O1A P1A P2A O4A -86.0(2) . . . . yes
O2A P1A P2A O4A 147.8(2) . . . . yes
O3A P1A P2A O4A 38.7(2) . . . . yes
O1A P1A P2A O5A 37.4(2) . . . . yes
O2A P1A P2A O5A -88.8(2) . . . . yes
O3A P1A P2A O5A 162.10(19) . . . . yes
O1A P1A P2A O6A 155.3(2) . . . . yes
O2A P1A P2A O6A 29.1(2) . . . . yes
O3A P1A P2A O6A -79.96(19) . . . . yes
O2B P1B P2B O4B -57.5(2) . . . . yes
O1B P1B P2B O4B 176.7(2) . . . . yes
O3B P1B P2B O4B 61.14(19) . . . . yes
O2B P1B P2B O5B 69.0(2) . . . . yes
O1B P1B P2B O5B -56.9(2) . . . . yes
O3B P1B P2B O5B -172.39(17) . . . . yes
O2B P1B P2B O6B -172.72(17) . . . . yes
O1B P1B P2B O6B 61.4(2) . . . . yes
O3B P1B P2B O6B -54.1(2) . . . . yes
O1C P1C P2C O4C -84.7(2) . . . . yes
O2C P1C P2C O4C 148.4(2) . . . . yes
O3C P1C P2C O4C 39.9(2) . . . . yes
O1C P1C P2C O5C 40.8(2) . . . . yes
O2C P1C P2C O5C -86.0(2) . . . . yes
O3C P1C P2C O5C 165.45(19) . . . . yes
O1C P1C P2C O6C 158.1(2) . . . . yes
O2C P1C P2C O6C 31.3(2) . . . . yes
O3C P1C P2C O6C -77.3(2) . . . . yes
C6A N1A C2A N2A -179.4(4) . . . . ?
C6A N1A C2A C3A -1.3(7) . . . . ?
N2A C2A C3A C4A 179.0(5) . . . . ?
N1A C2A C3A C4A 1.0(6) . . . . ?
C2A C3A C4A C5A 0.0(7) . . . . ?
C3A C4A C5A C6A -0.8(7) . . . . ?
C2A N1A C6A C5A 0.5(7) . . . . ?
C4A C5A C6A N1A 0.5(7) . . . . ?
C6B N1B C2B N2B 179.5(4) . . . . ?
C6B N1B C2B C3B -0.8(6) . . . . ?
N2B C2B C3B C4B -179.9(5) . . . . ?
N1B C2B C3B C4B 0.4(6) . . . . ?
C2B C3B C4B C5B 0.1(7) . . . . ?
C3B C4B C5B C6B -0.2(7) . . . . ?
C4B C5B C6B N1B -0.2(7) . . . . ?
C2B N1B C6B C5B 0.7(7) . . . . ?
C6C N1C C2C N2C 178.1(4) . . . . ?
C6C N1C C2C C3C -0.8(6) . . . . ?
N2C C2C C3C C4C -177.6(5) . . . . ?
N1C C2C C3C C4C 1.2(6) . . . . ?
C2C C3C C4C C5C -0.3(7) . . . . ?
C3C C4C C5C C6C -1.0(7) . . . . ?
C2C N1C C6C C5C -0.5(7) . . . . ?
C4C C5C C6C N1C 1.4(7) . . . . ?
C6D N1D C2D N2D -179.8(7) . . . . ?
C6D N1D C2D C3D 0.3(12) . . . . ?
N2D C2D C3D C4D 178.6(8) . . . . ?
N1D C2D C3D C4D -1.5(13) . . . . ?
C2D C3D C4D C5D 1.6(13) . . . . ?
C3D C4D C5D C6D -0.3(13) . . . . ?
C4D C5D C6D N1D -0.9(12) . . . . ?
C2D N1D C6D C5D 0.9(12) . . . . ?
C6E N1E C2E N2E 178(3) . . . . ?
C6E N1E C2E C3E -2(5) . . . . ?
N2E C2E C3E C4E -178(3) . . . . ?
N1E C2E C3E C4E 2(5) . . . . ?
C2E C3E C4E C5E -2(6) . . . . ?
C3E C4E C5E C6E 1(7) . . . . ?
C4E C5E C6E N1E -2(7) . . . . ?
C2E N1E C6E C5E 2(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2A H2PA O1B 0.84 1.68 2.508(4) 167.5 .
O3A H3PA O4C 0.84 1.73 2.563(5) 173.6 1_455
O6A H6PA O5B 0.84 1.78 2.616(5) 173.3 .
O3B H3PB O5C 0.84 1.72 2.560(4) 173.3 .
O6B H6PB O5A 0.84 1.72 2.548(5) 168.8 .
O2C H2PC O4B 0.84 1.69 2.509(5) 164.2 .
O3C H3PC O4A 0.84 1.70 2.537(5) 176.3 1_655
O6C H6PC O2B 0.84 1.74 2.572(5) 170.6 .
N1A H1NA O1A 0.88 2.17 2.854(5) 134.6 .
N1A H1NA O5A 0.88 2.39 3.100(5) 138.4 .
N2A H2A1 O5A 0.88 2.02 2.818(5) 149.6 .
N2A H2A2 O4B 0.88 2.00 2.870(5) 168.2 3_666
N1B H1NB O5B 0.88 1.93 2.744(5) 153.1 .
N2B H2B1 O2B 0.88 2.13 2.867(5) 141.4 .
N2B H2B2 O1B 0.88 2.05 2.911(5) 167.5 2_655
C5B H5B O6B 0.95 2.66 3.467(6) 142.8 3_676
N1C H1NC O5C 0.88 1.85 2.688(5) 158.3 .
N2C H2C1 O1C 0.88 2.10 2.914(5) 153.8 .
N2C H2C2 O4A 0.88 2.06 2.904(5) 160.2 3_666
C3C H3C O4A 0.95 2.62 3.341(6) 132.6 3_666
C5C H5C O1A 0.95 2.63 3.474(6) 147.8 2_645
C6C H6C O2A 0.95 2.64 3.388(6) 135.7 2_645
N1D H1ND O1W 0.88 1.83 2.688(13) 166.3 .
N2D H2D1 O1C 0.88 2.42 3.079(9) 131.9 2_755
N2D H2D2 O4C 0.88 2.39 3.114(8) 140.2 2_755
C3D H3D O1C 0.95 2.16 3.104(8) 171.0 4_575
C5D H5D O3A 0.95 2.60 3.404(10) 142.1 2_645
C6D H6D O4C 0.95 2.60 3.396(10) 141.6 .
C6D H6D O1W 0.95 2.53 3.092(13) 118.1 2_745
N1E H1NE O4C 0.88 2.29 3.10(2) 154.2 .
N2E H2E1 O1A 0.88 2.25 2.856(17) 125.8 2_655
N2E H2E2 O4C 0.88 2.55 3.316(17) 146.2 .
N2E H2E2 O6C 0.88 2.35 3.082(16) 140.6 .
O1W H1W1 O6C 0.84 1.94 2.754(10) 163.2 .
O1W H1W2 O1A 0.84 1.85 2.677(9) 166.8 2_655

_refine_diff_density_max         0.747
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.143

####################################################################### 
# 
# 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_2ampyr11-dehh
_database_code_depnum_ccdc_archive 'CCDC 2154536'
loop_
_audit_author_name
_audit_author_address
'Daria Budzikur'
;University of Wroclaw
Poland
;
_audit_update_record             
;
2022-02-24 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'4(C5 H7 N2), 2(H3 P2 O6), (H2 P2 O6), 0.1(H2 O)'
_chemical_formula_sum            'C20 H36.20 N8 O18.10 P6'
_chemical_formula_weight         864.19

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   13.706(5)
_cell_length_b                   10.656(4)
_cell_length_c                   24.802(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.61(3)
_cell_angle_gamma                90
_cell_volume                     3598(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13370
_cell_measurement_theta_min      3.2340
_cell_measurement_theta_max      64.3890

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_F_000             1788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.026
_exptl_absorpt_coefficient_mu    3.556
_shelx_estimated_absorpt_T_min   0.794
_shelx_estimated_absorpt_T_max   0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.56534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            86594
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_av_R_equivalents  0.1243
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.246
_diffrn_reflns_theta_max         74.824
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             7170
_reflns_number_gt                3580
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1198P)²+6.1134P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7170
_refine_ls_number_parameters     511
_refine_ls_number_restraints     446
_refine_ls_R_factor_all          0.1628
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_ref         0.2674
_refine_ls_wR_factor_gt          0.2169
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1A P 0.23089(13) 0.75264(16) 0.32986(7) 0.0529(5) Uani 1 1 d . U . . .
O1A O 0.2231(4) 0.6190(4) 0.31324(19) 0.0678(13) Uani 1 1 d . U . . .
O2A O 0.3116(3) 0.8309(4) 0.30642(18) 0.0579(12) Uani 1 1 d . U . . .
H2PA H 0.362814 0.787452 0.306578 0.087 Uiso 1 1 calc R U . . .
O3A O 0.1383(3) 0.8336(4) 0.31377(19) 0.0618(12) Uani 1 1 d . U . . .
H3PA H 0.087781 0.789328 0.314778 0.093 Uiso 1 1 calc R U . . .
P2A P 0.26250(13) 0.75488(17) 0.41852(7) 0.0529(5) Uani 1 1 d . U . . .
O4A O 0.1681(3) 0.7494(4) 0.44293(17) 0.0612(12) Uani 1 1 d . U . . .
O5A O 0.3299(3) 0.6449(4) 0.43143(17) 0.0594(12) Uani 1 1 d . U . . .
O6A O 0.3169(3) 0.8814(4) 0.43478(18) 0.0584(12) Uani 1 1 d . U . . .
H6PA H 0.376705 0.874376 0.430747 0.088 Uiso 1 1 calc R U . . .
P1B P 0.57859(13) 0.74120(16) 0.33288(6) 0.0503(4) Uani 1 1 d . U . . .
O1B O 0.4767(3) 0.7334(5) 0.30269(17) 0.0625(13) Uani 1 1 d . U . . .
O2B O 0.6414(3) 0.8495(4) 0.31910(17) 0.0575(12) Uani 1 1 d . U . . .
O3B O 0.6292(3) 0.6141(4) 0.32317(18) 0.0560(11) Uani 1 1 d . U . . .
H3PB H 0.689923 0.620473 0.332383 0.084 Uiso 1 1 calc R U . . .
P2B P 0.56772(12) 0.75822(16) 0.42021(6) 0.0488(4) Uani 1 1 d . U . . .
O4B O 0.6686(3) 0.7571(4) 0.45007(16) 0.0576(12) Uani 1 1 d . U . . .
O5B O 0.5062(3) 0.8736(4) 0.42587(16) 0.0518(11) Uani 1 1 d . U . . .
O6B O 0.5152(3) 0.6368(4) 0.43742(18) 0.0560(11) Uani 1 1 d . U . . .
H6PB H 0.454362 0.649356 0.435045 0.084 Uiso 1 1 calc R U . . .
P1C P 0.91630(13) 0.77380(18) 0.43177(8) 0.0579(5) Uani 1 1 d . U . . .
O1C O 0.9314(4) 0.6529(4) 0.4619(2) 0.0722(14) Uani 1 1 d . U . . .
O2C O 0.8328(3) 0.8571(4) 0.44790(19) 0.0606(12) Uani 1 1 d . U . . .
H2PC H 0.784242 0.812115 0.452742 0.091 Uiso 1 1 calc R U . . .
O3C O 1.0045(3) 0.8644(4) 0.4388(2) 0.0631(12) Uani 1 1 d . U . . .
H3PC H 1.056802 0.823694 0.438019 0.095 Uiso 1 1 calc R U . . .
P2C P 0.88440(14) 0.73104(18) 0.34467(8) 0.0599(5) Uani 1 1 d . U . . .
O4C O 0.9796(4) 0.7125(5) 0.3230(2) 0.0793(16) Uani 1 1 d . U . . .
O5C O 0.8168(3) 0.6203(4) 0.34067(19) 0.0622(12) Uani 1 1 d . U . . .
O6C O 0.8298(4) 0.8485(4) 0.31782(19) 0.0650(13) Uani 1 1 d . U . . .
H6PC H 0.769231 0.841643 0.319714 0.097 Uiso 1 1 calc R U . . .
N1A N 0.2950(4) 0.3937(5) 0.3595(2) 0.0611(15) Uani 1 1 d . U . . .
H1NA H 0.290978 0.476033 0.360681 0.073 Uiso 1 1 calc R U . . .
C2A C 0.2998(5) 0.3295(6) 0.4068(3) 0.0533(16) Uani 1 1 d . U . . .
N2A N 0.2961(4) 0.3917(5) 0.4525(2) 0.0578(14) Uani 1 1 d . U . . .
H2A1 H 0.290569 0.473960 0.451995 0.069 Uiso 1 1 calc R U . . .
H2A2 H 0.299226 0.350913 0.483518 0.069 Uiso 1 1 calc R U . . .
C3A C 0.3053(5) 0.1982(6) 0.4041(3) 0.0617(18) Uani 1 1 d . U . . .
H3A H 0.308713 0.149954 0.436488 0.074 Uiso 1 1 calc R U . . .
C5A C 0.3022(6) 0.2102(7) 0.3076(3) 0.070(2) Uani 1 1 d . U . . .
H5A H 0.304072 0.169456 0.273681 0.084 Uiso 1 1 calc R U . . .
C6A C 0.2960(6) 0.3373(8) 0.3098(3) 0.074(2) Uani 1 1 d . U . . .
H6A H 0.292471 0.386147 0.277642 0.089 Uiso 1 1 calc R U . . .
C4A C 0.3057(5) 0.1395(7) 0.3553(3) 0.0642(18) Uani 1 1 d . U . . .
H4A H 0.308295 0.050517 0.353641 0.077 Uiso 1 1 calc R U . . .
N1B N 0.5462(4) 1.1090(5) 0.3897(2) 0.0610(15) Uani 1 1 d . U . . .
H1NB H 0.543886 1.026756 0.392338 0.073 Uiso 1 1 calc R U . . .
C2B C 0.5457(5) 1.1613(6) 0.3403(3) 0.0575(17) Uani 1 1 d . U . . .
N2B N 0.5451(4) 1.0877(5) 0.2967(2) 0.0569(14) Uani 1 1 d . U . . .
H2B1 H 0.544933 1.005583 0.300356 0.068 Uiso 1 1 calc R U . . .
H2B2 H 0.544764 1.121336 0.264242 0.068 Uiso 1 1 calc R U . . .
C3B C 0.5487(6) 1.2931(7) 0.3363(3) 0.068(2) Uani 1 1 d . U . . .
H3B H 0.548922 1.332719 0.301972 0.082 Uiso 1 1 calc R U . . .
C4B C 0.5511(5) 1.3630(7) 0.3826(3) 0.0623(18) Uani 1 1 d . U . . .
H4B H 0.551926 1.451924 0.380165 0.075 Uiso 1 1 calc R U . . .
C5B C 0.5525(5) 1.3070(7) 0.4330(3) 0.0646(19) Uani 1 1 d . U . . .
H5B H 0.555108 1.356884 0.464850 0.077 Uiso 1 1 calc R U . . .
C6B C 0.5501(6) 1.1800(7) 0.4363(3) 0.070(2) Uani 1 1 d . U . . .
H6B H 0.551084 1.140141 0.470625 0.084 Uiso 1 1 calc R U . . .
N1C N 0.8150(4) 0.3779(5) 0.3678(2) 0.0546(14) Uani 1 1 d . U . . .
H1NC H 0.823235 0.459318 0.364256 0.066 Uiso 1 1 calc R U . . .
C2C C 0.8161(5) 0.3292(7) 0.4186(3) 0.0563(16) Uani 1 1 d . U . . .
N2C N 0.8343(4) 0.4057(5) 0.4610(2) 0.0583(14) Uani 1 1 d . U . . .
H2C1 H 0.845441 0.485909 0.455887 0.070 Uiso 1 1 calc R U . . .
H2C2 H 0.835341 0.376011 0.494187 0.070 Uiso 1 1 calc R U . . .
C3C C 0.8009(5) 0.1998(7) 0.4229(3) 0.0583(17) Uani 1 1 d . U . . .
H3C H 0.800728 0.162777 0.457720 0.070 Uiso 1 1 calc R U . . .
C4C C 0.7865(5) 0.1264(7) 0.3777(3) 0.0606(18) Uani 1 1 d . U . . .
H4C H 0.775481 0.038820 0.381019 0.073 Uiso 1 1 calc R U . . .
C5C C 0.7880(5) 0.1808(7) 0.3259(3) 0.0663(19) Uani 1 1 d . U . . .
H5C H 0.779430 0.130383 0.294106 0.080 Uiso 1 1 calc R U . . .
C6C C 0.8019(5) 0.3064(7) 0.3224(3) 0.0658(19) Uani 1 1 d . U . . .
H6C H 0.802362 0.344525 0.287839 0.079 Uiso 1 1 calc R U . . .
N1D N 0.9450(9) 0.8209(11) 0.1742(4) 0.094(3) Uani 0.760(11) 1 d D U P A 1
H1ND H 0.942071 0.872809 0.201562 0.113 Uiso 0.760(11) 1 calc R U P A 1
C2D C 0.9458(9) 0.8650(10) 0.1169(4) 0.064(3) Uani 0.760(11) 1 d D U P A 1
N2D N 0.9447(6) 0.9873(8) 0.1080(4) 0.091(3) Uani 0.760(11) 1 d D U P A 1
H2D1 H 0.944208 1.016149 0.074703 0.109 Uiso 0.760(11) 1 calc R U P A 1
H2D2 H 0.944603 1.039900 0.135329 0.109 Uiso 0.760(11) 1 calc R U P A 1
C3D C 0.9461(8) 0.7805(9) 0.0801(4) 0.050(2) Uani 0.760(11) 1 d D U P A 1
H3D H 0.943644 0.807719 0.043447 0.060 Uiso 0.760(11) 1 calc R U P A 1
C4D C 0.9497(10) 0.6525(11) 0.0898(5) 0.075(3) Uani 0.760(11) 1 d D U P A 1
H4D H 0.952387 0.595816 0.060492 0.090 Uiso 0.760(11) 1 calc R U P A 1
C5D C 0.9493(10) 0.6087(12) 0.1397(5) 0.082(3) Uani 0.760(11) 1 d D U P A 1
H5D H 0.949131 0.520829 0.146228 0.098 Uiso 0.760(11) 1 calc R U P A 1
C6D C 0.9493(11) 0.6896(13) 0.1808(5) 0.085(3) Uani 0.760(11) 1 d D U P A 1
H6D H 0.952399 0.656764 0.216611 0.102 Uiso 0.760(11) 1 calc R U P A 1
N1E N 0.954(3) 0.737(2) 0.1897(10) 0.081(6) Uiso 0.240(11) 1 d D U P A 2
H1NE H 0.951434 0.704418 0.222093 0.098 Uiso 0.240(11) 1 calc R U P A 2
C2E C 0.952(4) 0.876(2) 0.1795(10) 0.087(6) Uiso 0.240(11) 1 d D U P A 2
N2E N 0.937(2) 0.945(2) 0.2219(10) 0.095(9) Uiso 0.240(11) 1 d D U P A 2
H2E1 H 0.918159 1.023962 0.217280 0.114 Uiso 0.240(11) 1 calc R U P A 2
H2E2 H 0.946283 0.913241 0.254782 0.114 Uiso 0.240(11) 1 calc R U P A 2
C3E C 0.942(4) 0.904(3) 0.1289(10) 0.071(6) Uiso 0.240(11) 1 d D U P A 2
H3E H 0.930354 0.990725 0.121348 0.085 Uiso 0.240(11) 1 calc R U P A 2
C4E C 0.947(3) 0.830(3) 0.0836(10) 0.065(6) Uiso 0.240(11) 1 d D U P A 2
H4E H 0.944080 0.863968 0.048105 0.078 Uiso 0.240(11) 1 calc R U P A 2
C5E C 0.955(4) 0.707(3) 0.0926(11) 0.073(5) Uiso 0.240(11) 1 d D U P A 2
H5E H 0.957246 0.651268 0.062997 0.087 Uiso 0.240(11) 1 calc R U P A 2
C6E C 0.960(4) 0.663(3) 0.1431(11) 0.082(5) Uiso 0.240(11) 1 d D U P A 2
H6E H 0.968654 0.574953 0.148109 0.098 Uiso 0.240(11) 1 calc R U P A 2
O1W O 0.924(3) 0.993(4) 0.2501(17) 0.058(15) Uiso 0.106(12) 1 d D U P B 1
H1W1 H 0.907330 0.970049 0.280092 0.087 Uiso 0.106(12) 1 d DR U P B 1
H1W2 H 0.883196 1.046546 0.236695 0.087 Uiso 0.106(12) 1 d DR U P B 1


_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
P1A O1A 1.483(5) . yes
P1A O3A 1.549(5) . yes
P1A O2A 1.551(5) . yes
P1A P2A 2.192(2) . yes
O2A H2PA 0.8400 . ?
O3A H3PA 0.8400 . ?
P2A O4A 1.491(5) . yes
P2A O5A 1.504(4) . yes
P2A O6A 1.571(5) . yes
O6A H6PA 0.8400 . ?
P1B O2B 1.502(5) . yes
P1B O1B 1.509(4) . yes
P1B O3B 1.553(4) . yes
P1B P2B 2.196(2) . yes
O3B H3PB 0.8400 . ?
P2B O4B 1.492(4) . yes
P2B O5B 1.506(4) . yes
P2B O6B 1.564(4) . yes
O6B H6PB 0.8400 . ?
P1C O1C 1.492(5) . yes
P1C O2C 1.537(5) . yes
P1C O3C 1.542(5) . yes
P1C P2C 2.202(3) . yes
O2C H2PC 0.8400 . ?
O3C H3PC 0.8400 . ?
P2C O4C 1.481(5) . yes
P2C O5C 1.496(5) . yes
P2C O6C 1.567(5) . yes
O6C H6PC 0.8400 . ?
N1A C2A 1.353(8) . ?
N1A C6A 1.373(9) . ?
N1A H1NA 0.8800 . ?
C2A N2A 1.319(8) . ?
C2A C3A 1.403(9) . ?
N2A H2A1 0.8800 . ?
N2A H2A2 0.8800 . ?
C3A C4A 1.364(9) . ?
C3A H3A 0.9500 . ?
C5A C6A 1.358(10) . ?
C5A C4A 1.398(10) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
C4A H4A 0.9500 . ?
N1B C2B 1.346(8) . ?
N1B C6B 1.377(8) . ?
N1B H1NB 0.8800 . ?
C2B N2B 1.334(8) . ?
C2B C3B 1.409(9) . ?
N2B H2B1 0.8800 . ?
N2B H2B2 0.8800 . ?
C3B C4B 1.367(9) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.382(9) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.357(10) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
N1C C6C 1.353(8) . ?
N1C C2C 1.362(8) . ?
N1C H1NC 0.8800 . ?
C2C N2C 1.332(8) . ?
C2C C3C 1.400(9) . ?
N2C H2C1 0.8800 . ?
N2C H2C2 0.8800 . ?
C3C C4C 1.363(9) . ?
C3C H3C 0.9500 . ?
C4C C5C 1.411(9) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.356(10) . ?
C5C H5C 0.9500 . ?
C6C H6C 0.9500 . ?
N1D C6D 1.409(15) . ?
N1D C2D 1.499(14) . ?
N1D H1ND 0.8800 . ?
C2D C3D 1.283(13) . ?
C2D N2D 1.321(13) . ?
N2D H2D1 0.8800 . ?
N2D H2D2 0.8800 . ?
C3D C4D 1.385(13) . ?
C3D H3D 0.9500 . ?
C4D C5D 1.324(14) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.335(17) . ?
C5D H5D 0.9500 . ?
C6D H6D 0.9500 . ?
N1E C6E 1.409(15) . ?
N1E C2E 1.499(15) . ?
N1E H1NE 0.8800 . ?
C2E C3E 1.283(13) . ?
C2E N2E 1.321(13) . ?
N2E H2E1 0.8800 . ?
N2E H2E2 0.8800 . ?
C3E C4E 1.385(13) . ?
C3E H3E 0.9500 . ?
C4E C5E 1.323(14) . ?
C4E H4E 0.9500 . ?
C5E C6E 1.335(17) . ?
C5E H5E 0.9500 . ?
C6E H6E 0.9500 . ?
O1W H1W1 0.8405 . ?
O1W H1W2 0.8401 . ?

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
O1A P1A O3A 115.6(3) . . yes
O1A P1A O2A 116.4(3) . . yes
O3A P1A O2A 101.7(3) . . yes
O1A P1A P2A 106.8(2) . . yes
O3A P1A P2A 108.3(2) . . yes
O2A P1A P2A 107.6(2) . . yes
P1A O2A H2PA 109.5 . . ?
P1A O3A H3PA 109.5 . . ?
O4A P2A O5A 115.1(3) . . yes
O4A P2A O6A 109.7(3) . . yes
O5A P2A O6A 110.6(3) . . yes
O4A P2A P1A 109.0(2) . . yes
O5A P2A P1A 104.5(2) . . yes
O6A P2A P1A 107.46(19) . . yes
P2A O6A H6PA 109.5 . . ?
O2B P1B O1B 116.8(3) . . yes
O2B P1B O3B 110.9(3) . . yes
O1B P1B O3B 106.2(3) . . yes
O2B P1B P2B 105.47(19) . . yes
O1B P1B P2B 109.3(2) . . yes
O3B P1B P2B 107.89(19) . . yes
P1B O3B H3PB 109.5 . . ?
O4B P2B O5B 117.2(3) . . yes
O4B P2B O6B 106.7(3) . . yes
O5B P2B O6B 111.7(2) . . yes
O4B P2B P1B 108.94(19) . . yes
O5B P2B P1B 105.17(17) . . yes
O6B P2B P1B 106.65(19) . . yes
P2B O6B H6PB 109.5 . . ?
O1C P1C O2C 115.6(3) . . yes
O1C P1C O3C 115.0(3) . . yes
O2C P1C O3C 101.9(3) . . yes
O1C P1C P2C 108.3(2) . . yes
O2C P1C P2C 107.8(2) . . yes
O3C P1C P2C 107.8(2) . . yes
P1C O2C H2PC 109.5 . . ?
P1C O3C H3PC 109.5 . . ?
O4C P2C O5C 115.8(3) . . yes
O4C P2C O6C 110.5(3) . . yes
O5C P2C O6C 109.9(3) . . yes
O4C P2C P1C 107.4(2) . . yes
O5C P2C P1C 106.2(2) . . yes
O6C P2C P1C 106.4(2) . . yes
P2C O6C H6PC 109.5 . . ?
C2A N1A C6A 123.5(6) . . ?
C2A N1A H1NA 118.2 . . ?
C6A N1A H1NA 118.2 . . ?
N2A C2A N1A 119.2(6) . . ?
N2A C2A C3A 123.3(6) . . ?
N1A C2A C3A 117.4(6) . . ?
C2A N2A H2A1 120.0 . . ?
C2A N2A H2A2 120.0 . . ?
H2A1 N2A H2A2 120.0 . . ?
C4A C3A C2A 120.4(7) . . ?
C4A C3A H3A 119.8 . . ?
C2A C3A H3A 119.8 . . ?
C6A C5A C4A 119.9(7) . . ?
C6A C5A H5A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C5A C6A N1A 118.7(7) . . ?
C5A C6A H6A 120.6 . . ?
N1A C6A H6A 120.6 . . ?
C3A C4A C5A 120.0(7) . . ?
C3A C4A H4A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C2B N1B C6B 122.2(6) . . ?
C2B N1B H1NB 118.9 . . ?
C6B N1B H1NB 118.9 . . ?
N2B C2B N1B 119.6(6) . . ?
N2B C2B C3B 121.8(6) . . ?
N1B C2B C3B 118.6(6) . . ?
C2B N2B H2B1 120.0 . . ?
C2B N2B H2B2 120.0 . . ?
H2B1 N2B H2B2 120.0 . . ?
C4B C3B C2B 118.8(6) . . ?
C4B C3B H3B 120.6 . . ?
C2B C3B H3B 120.6 . . ?
C3B C4B C5B 121.4(7) . . ?
C3B C4B H4B 119.3 . . ?
C5B C4B H4B 119.3 . . ?
C6B C5B C4B 119.2(7) . . ?
C6B C5B H5B 120.4 . . ?
C4B C5B H5B 120.4 . . ?
C5B C6B N1B 119.7(7) . . ?
C5B C6B H6B 120.1 . . ?
N1B C6B H6B 120.1 . . ?
C6C N1C C2C 122.7(6) . . ?
C6C N1C H1NC 118.6 . . ?
C2C N1C H1NC 118.6 . . ?
N2C C2C N1C 118.6(6) . . ?
N2C C2C C3C 123.9(6) . . ?
N1C C2C C3C 117.4(6) . . ?
C2C N2C H2C1 120.0 . . ?
C2C N2C H2C2 120.0 . . ?
H2C1 N2C H2C2 120.0 . . ?
C4C C3C C2C 120.8(6) . . ?
C4C C3C H3C 119.6 . . ?
C2C C3C H3C 119.6 . . ?
C3C C4C C5C 119.8(7) . . ?
C3C C4C H4C 120.1 . . ?
C5C C4C H4C 120.1 . . ?
C6C C5C C4C 118.7(7) . . ?
C6C C5C H5C 120.7 . . ?
C4C C5C H5C 120.7 . . ?
N1C C6C C5C 120.6(7) . . ?
N1C C6C H6C 119.7 . . ?
C5C C6C H6C 119.7 . . ?
C6D N1D C2D 114.7(10) . . ?
C6D N1D H1ND 122.7 . . ?
C2D N1D H1ND 122.7 . . ?
C3D C2D N2D 125.0(12) . . ?
C3D C2D N1D 117.1(10) . . ?
N2D C2D N1D 117.9(10) . . ?
C2D N2D H2D1 120.0 . . ?
C2D N2D H2D2 120.0 . . ?
H2D1 N2D H2D2 120.0 . . ?
C2D C3D C4D 124.7(11) . . ?
C2D C3D H3D 117.6 . . ?
C4D C3D H3D 117.6 . . ?
C5D C4D C3D 120.5(11) . . ?
C5D C4D H4D 119.8 . . ?
C3D C4D H4D 119.8 . . ?
C4D C5D C6D 119.1(11) . . ?
C4D C5D H5D 120.4 . . ?
C6D C5D H5D 120.4 . . ?
C5D C6D N1D 123.8(12) . . ?
C5D C6D H6D 118.1 . . ?
N1D C6D H6D 118.1 . . ?
C6E N1E C2E 114.6(19) . . ?
C6E N1E H1NE 122.7 . . ?
C2E N1E H1NE 122.7 . . ?
C3E C2E N2E 130(3) . . ?
C3E C2E N1E 113(2) . . ?
N2E C2E N1E 115(2) . . ?
C2E N2E H2E1 120.0 . . ?
C2E N2E H2E2 120.0 . . ?
H2E1 N2E H2E2 120.0 . . ?
C2E C3E C4E 130(3) . . ?
C2E C3E H3E 114.8 . . ?
C4E C3E H3E 114.8 . . ?
C5E C4E C3E 116(2) . . ?
C5E C4E H4E 122.0 . . ?
C3E C4E H4E 122.0 . . ?
C4E C5E C6E 120(2) . . ?
C4E C5E H5E 119.9 . . ?
C6E C5E H5E 119.9 . . ?
C5E C6E N1E 125(2) . . ?
C5E C6E H6E 117.7 . . ?
N1E C6E H6E 117.7 . . ?
H1W1 O1W H1W2 108.1 . . ?

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
O1A P1A P2A O4A -86.4(3) . . . . yes
O3A P1A P2A O4A 38.7(3) . . . . yes
O2A P1A P2A O4A 148.0(3) . . . . yes
O1A P1A P2A O5A 37.2(3) . . . . yes
O3A P1A P2A O5A 162.3(3) . . . . yes
O2A P1A P2A O5A -88.5(3) . . . . yes
O1A P1A P2A O6A 154.7(3) . . . . yes
O3A P1A P2A O6A -80.1(3) . . . . yes
O2A P1A P2A O6A 29.1(3) . . . . yes
O2B P1B P2B O4B -57.5(3) . . . . yes
O1B P1B P2B O4B 176.2(3) . . . . yes
O3B P1B P2B O4B 61.1(3) . . . . yes
O2B P1B P2B O5B 69.0(3) . . . . yes
O1B P1B P2B O5B -57.4(3) . . . . yes
O3B P1B P2B O5B -172.5(3) . . . . yes
O2B P1B P2B O6B -172.3(3) . . . . yes
O1B P1B P2B O6B 61.4(3) . . . . yes
O3B P1B P2B O6B -53.7(3) . . . . yes
O1C P1C P2C O4C -83.4(3) . . . . yes
O2C P1C P2C O4C 150.9(3) . . . . yes
O3C P1C P2C O4C 41.6(3) . . . . yes
O1C P1C P2C O5C 41.1(3) . . . . yes
O2C P1C P2C O5C -84.6(3) . . . . yes
O3C P1C P2C O5C 166.1(3) . . . . yes
O1C P1C P2C O6C 158.2(3) . . . . yes
O2C P1C P2C O6C 32.5(3) . . . . yes
O3C P1C P2C O6C -76.8(3) . . . . yes
C6A N1A C2A N2A -178.5(6) . . . . ?
C6A N1A C2A C3A -0.6(10) . . . . ?
N2A C2A C3A C4A 177.8(7) . . . . ?
N1A C2A C3A C4A 0.1(10) . . . . ?
C4A C5A C6A N1A 1.1(12) . . . . ?
C2A N1A C6A C5A 0.0(11) . . . . ?
C2A C3A C4A C5A 1.0(11) . . . . ?
C6A C5A C4A C3A -1.6(12) . . . . ?
C6B N1B C2B N2B 177.8(7) . . . . ?
C6B N1B C2B C3B -0.5(11) . . . . ?
N2B C2B C3B C4B -178.7(7) . . . . ?
N1B C2B C3B C4B -0.5(11) . . . . ?
C2B C3B C4B C5B 1.1(12) . . . . ?
C3B C4B C5B C6B -0.8(12) . . . . ?
C4B C5B C6B N1B -0.1(11) . . . . ?
C2B N1B C6B C5B 0.8(11) . . . . ?
C6C N1C C2C N2C 176.7(6) . . . . ?
C6C N1C C2C C3C -1.2(10) . . . . ?
N2C C2C C3C C4C -177.3(7) . . . . ?
N1C C2C C3C C4C 0.4(10) . . . . ?
C2C C3C C4C C5C 0.8(11) . . . . ?
C3C C4C C5C C6C -1.4(11) . . . . ?
C2C N1C C6C C5C 0.6(11) . . . . ?
C4C C5C C6C N1C 0.7(11) . . . . ?
C6D N1D C2D C3D 2.8(16) . . . . ?
C6D N1D C2D N2D -178.1(11) . . . . ?
N2D C2D C3D C4D 178.3(11) . . . . ?
N1D C2D C3D C4D -2.7(18) . . . . ?
C2D C3D C4D C5D 3(2) . . . . ?
C3D C4D C5D C6D -3(2) . . . . ?
C4D C5D C6D N1D 3(2) . . . . ?
C2D N1D C6D C5D -3.1(19) . . . . ?
C6E N1E C2E C3E 9(7) . . . . ?
C6E N1E C2E N2E 174(4) . . . . ?
N2E C2E C3E C4E -172(5) . . . . ?
N1E C2E C3E C4E -9(9) . . . . ?
C2E C3E C4E C5E 5(9) . . . . ?
C3E C4E C5E C6E -1(8) . . . . ?
C4E C5E C6E N1E 2(8) . . . . ?
C2E N1E C6E C5E -6(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2A H2PA O1B 0.84 1.68 2.501(6) 166.2 .
O3A H3PA O4C 0.84 1.73 2.561(7) 172.4 1_455
O6A H6PA O5B 0.84 1.79 2.630(6) 174.3 .
O3B H3PB O5C 0.84 1.73 2.559(6) 169.9 .
O6B H6PB O5A 0.84 1.70 2.528(6) 169.2 .
O2C H2PC O4B 0.84 1.68 2.496(6) 161.9 .
O3C H3PC O4A 0.84 1.71 2.547(7) 173.6 1_655
O6C H6PC O2B 0.84 1.75 2.586(7) 171.4 .
N1A H1NA O1A 0.88 2.08 2.792(7) 137.6 .
N1A H1NA O5A 0.88 2.53 3.222(7) 136.4 .
N2A H2A1 O5A 0.88 1.98 2.797(7) 153.3 .
N2A H2A2 O4B 0.88 2.02 2.884(7) 168.5 3_666
N1B H1NB O5B 0.88 1.93 2.741(7) 152.7 .
N2B H2B1 O2B 0.88 2.14 2.886(7) 141.8 .
N2B H2B2 O1B 0.88 2.04 2.899(7) 165.4 2_655
N1C H1NC O5C 0.88 1.81 2.669(7) 164.4 .
N2C H2C1 O1C 0.88 2.13 2.950(7) 154.8 .
N2C H2C2 O4A 0.88 2.06 2.903(7) 160.4 3_666
C3C H3C O4A 0.95 2.62 3.350(8) 133.5 3_666
N1D H1ND O1W 0.88 1.79 2.67(5) 171.2 .
N2D H2D1 O1C 0.88 2.49 3.111(11) 127.9 2_755
N2D H2D2 O4C 0.88 2.30 3.058(11) 144.6 2_755
C3D H3D O1C 0.95 2.05 2.999(11) 173.5 4_575
C5D H5D O3A 0.95 2.58 3.418(13) 146.8 2_645
C6D H6D O4C 0.95 2.69 3.512(14) 145.2 .
C6D H6D O1W 0.95 2.50 3.11(4) 121.4 2_745
N1E H1NE O4C 0.88 2.49 3.30(3) 152.6 .
N2E H2E1 O1A 0.88 2.24 2.93(3) 134.8 2_655
N2E H2E2 O4C 0.88 2.73 3.53(3) 151.0 .
N2E H2E2 O6C 0.88 2.46 3.11(3) 131.6 .
O1W H1W1 O6C 0.84 1.98 2.71(4) 145.7 .
O1W H1W2 O1A 0.84 1.96 2.76(4) 158.5 2_655

_refine_diff_density_max         0.625
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.117

