# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

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

data_1_tr72
_audit_block_doi                 10.5517/ccdc.csd.cc1qd4mw
_database_code_depnum_ccdc_archive 'CCDC 1590598'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-01 downloaded from the CCDC.
;
#####################################################################

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H14 N2 O7 P2, H2 O'
_chemical_formula_sum            'C8 H16 N2 O8 P2'
_chemical_formula_weight         330.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   7.695(3)
_cell_length_b                   7.920(3)
_cell_length_c                   10.362(3)
_cell_angle_alpha                96.36(3)
_cell_angle_beta                 99.93(3)
_cell_angle_gamma                91.11(3)
_cell_volume                     617.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7692
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      36.70

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_F_000             344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.395
_shelx_estimated_absorpt_T_min   0.792
_shelx_estimated_absorpt_T_max   0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Kuma MK4-CCD, Sapphire2, large Be window'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            9051
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.061
_diffrn_reflns_theta_max         36.790
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.720
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4465
_reflns_number_gt                4016
_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       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_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)+(0.0860P)²+0.1188P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4465
_refine_ls_number_parameters     185
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1209
_refine_ls_wR_factor_gt          0.1186
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.080
_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 0.16567(4) 0.03814(3) 0.19982(3) 0.00881(8) Uani 1 1 d . . . . .
O1 O 0.19993(11) -0.02164(11) 0.06484(8) 0.01155(16) Uani 1 1 d . . . . .
O2 O 0.33766(12) 0.03244(11) 0.30124(9) 0.01269(17) Uani 1 1 d . . . . .
H2 H 0.3125 0.0247 0.3762 0.019 Uiso 1 1 calc R U . . .
O3 O 0.01656(12) -0.06835(11) 0.23984(10) 0.01453(17) Uani 1 1 d . . . . .
H3 H -0.0644 -0.0044 0.2568 0.022 Uiso 1 1 calc R U . . .
P2 P -0.04194(4) 0.30083(4) 0.34070(3) 0.00885(8) Uani 1 1 d . . . . .
O4 O 0.07175(12) 0.30451(11) 0.47481(8) 0.01204(16) Uani 1 1 d . . . . .
O5 O -0.18362(11) 0.15897(11) 0.30598(9) 0.01224(16) Uani 1 1 d . . . . .
O6 O -0.13204(12) 0.47386(11) 0.32234(8) 0.01183(16) Uani 1 1 d . . . . .
H6 H -0.0999 0.5426 0.3905 0.018 Uiso 1 1 calc R U . . .
O7 O -0.02453(11) 0.28799(10) 0.08948(8) 0.01039(16) Uani 1 1 d . . . . .
H7 H -0.0608 0.1932 0.0479 0.016 Uiso 1 1 calc R U . . .
N1 N 0.34415(13) 0.33598(12) 0.10110(9) 0.00972(17) Uani 1 1 d . . . . .
N2 N 0.51916(14) 0.20823(13) -0.01672(10) 0.01282(19) Uani 1 1 d D . . . .
H2N H 0.6098 0.1525 -0.0383 0.015 Uiso 1 1 d DR U . . .
C1 C 0.09428(14) 0.26272(13) 0.20751(10) 0.00842(18) Uani 1 1 d . . . . .
C2 C 0.25512(15) 0.38919(13) 0.21438(10) 0.00925(19) Uani 1 1 d . . . . .
C3 C 0.20821(16) 0.57894(13) 0.21904(11) 0.0112(2) Uani 1 1 d . . . . .
H3A H 0.2570 0.6401 0.1541 0.013 Uiso 1 1 calc R U . . .
H3B H 0.0805 0.5976 0.2140 0.013 Uiso 1 1 calc R U . . .
C4 C 0.31598(17) 0.61219(15) 0.36081(12) 0.0143(2) Uani 1 1 d . . . . .
H4A H 0.4093 0.7030 0.3715 0.017 Uiso 1 1 calc R U . . .
H4B H 0.2419 0.6317 0.4298 0.017 Uiso 1 1 calc R U . . .
C5 C 0.38624(16) 0.43051(14) 0.34709(11) 0.0114(2) Uani 1 1 d . . . . .
H5A H 0.3628 0.3619 0.4170 0.014 Uiso 1 1 calc R U . . .
H5B H 0.5120 0.4274 0.3375 0.014 Uiso 1 1 calc R U . . .
C21 C 0.48793(15) 0.24353(14) 0.10572(11) 0.0112(2) Uani 1 1 d . . . . .
H21 H 0.5562 0.2089 0.1830 0.013 Uiso 1 1 calc R U . . .
C41 C 0.39280(16) 0.28099(16) -0.10239(12) 0.0147(2) Uani 1 1 d . . . . .
H41 H 0.3842 0.2755 -0.1953 0.018 Uiso 1 1 calc R U . . .
C51 C 0.28309(16) 0.36201(15) -0.02858(11) 0.0127(2) Uani 1 1 d . . . . .
H51 H 0.1835 0.4246 -0.0599 0.015 Uiso 1 1 calc R U . . .
O1W O 0.30527(13) 0.06708(12) 0.54064(9) 0.01577(18) Uani 1 1 d D . . . .
H1W H 0.2844 -0.0179 0.5783 0.024 Uiso 1 1 d DR U . . .
H2W H 0.2258 0.1378 0.5454 0.024 Uiso 1 1 d DR 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 1.4951(10) . yes
P1 O2 1.5463(11) . yes
P1 O3 1.5505(10) . yes
P1 C1 1.8690(13) . yes
O2 H2 0.8400 . ?
O3 H3 0.8400 . ?
P2 O4 1.5060(11) . yes
P2 O5 1.5192(10) . yes
P2 O6 1.5633(11) . yes
P2 C1 1.8744(12) . yes
O6 H6 0.8400 . ?
O7 C1 1.4309(15) . ?
O7 H7 0.8400 . ?
N1 C21 1.3355(17) . ?
N1 C51 1.3843(16) . ?
N1 C2 1.4845(15) . ?
N2 C21 1.3322(15) . ?
N2 C41 1.3794(18) . ?
N2 H2N 0.8801 . ?
C1 C2 1.5640(15) . ?
C2 C3 1.5498(17) . ?
C2 C5 1.5572(17) . ?
C3 C4 1.5495(18) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.5473(18) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C21 H21 0.9500 . ?
C41 C51 1.3582(17) . ?
C41 H41 0.9500 . ?
C51 H51 0.9500 . ?
O1W H1W 0.8408 . ?
O1W H2W 0.8415 . ?

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 109.39(6) . . yes
O1 P1 O3 112.68(6) . . yes
O2 P1 O3 109.76(6) . . yes
O1 P1 C1 110.29(6) . . yes
O2 P1 C1 108.04(6) . . yes
O3 P1 C1 106.55(6) . . yes
P1 O2 H2 109.5 . . ?
P1 O3 H3 109.5 . . ?
O4 P2 O5 115.28(6) . . yes
O4 P2 O6 111.67(6) . . yes
O5 P2 O6 108.39(6) . . yes
O4 P2 C1 110.69(6) . . yes
O5 P2 C1 103.59(5) . . yes
O6 P2 C1 106.60(6) . . yes
P2 O6 H6 109.5 . . ?
C1 O7 H7 109.5 . . ?
C21 N1 C51 108.81(10) . . ?
C21 N1 C2 125.61(10) . . ?
C51 N1 C2 125.38(10) . . ?
C21 N2 C41 109.10(11) . . ?
C21 N2 H2N 125.0 . . ?
C41 N2 H2N 125.8 . . ?
O7 C1 C2 105.52(9) . . ?
O7 C1 P1 110.36(7) . . ?
C2 C1 P1 110.89(8) . . ?
O7 C1 P2 104.09(8) . . ?
C2 C1 P2 116.78(7) . . ?
P1 C1 P2 108.86(6) . . ?
N1 C2 C3 111.44(9) . . ?
N1 C2 C5 113.14(10) . . ?
C3 C2 C5 89.68(9) . . ?
N1 C2 C1 107.93(8) . . yes
C3 C2 C1 114.62(10) . . ?
C5 C2 C1 119.14(9) . . ?
C4 C3 C2 89.61(9) . . ?
C4 C3 H3A 113.7 . . ?
C2 C3 H3A 113.7 . . ?
C4 C3 H3B 113.7 . . ?
C2 C3 H3B 113.7 . . ?
H3A C3 H3B 111.0 . . ?
C5 C4 C3 90.06(9) . . ?
C5 C4 H4A 113.6 . . ?
C3 C4 H4A 113.6 . . ?
C5 C4 H4B 113.6 . . ?
C3 C4 H4B 113.6 . . ?
H4A C4 H4B 110.9 . . ?
C4 C5 C2 89.41(10) . . ?
C4 C5 H5A 113.7 . . ?
C2 C5 H5A 113.7 . . ?
C4 C5 H5B 113.7 . . ?
C2 C5 H5B 113.7 . . ?
H5A C5 H5B 111.0 . . ?
N2 C21 N1 108.27(11) . . ?
N2 C21 H21 125.9 . . ?
N1 C21 H21 125.9 . . ?
C51 C41 N2 106.96(11) . . ?
C51 C41 H41 126.5 . . ?
N2 C41 H41 126.5 . . ?
C41 C51 N1 106.86(12) . . ?
C41 C51 H51 126.6 . . ?
N1 C51 H51 126.6 . . ?
H1W O1W H2W 110.1 . . ?

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
O1 P1 C1 O7 40.74(8) . . . . ?
O2 P1 C1 O7 160.26(7) . . . . ?
O3 P1 C1 O7 -81.86(8) . . . . ?
O1 P1 C1 C2 -75.82(9) . . . . ?
O2 P1 C1 C2 43.70(9) . . . . ?
O3 P1 C1 C2 161.58(7) . . . . ?
O1 P1 C1 P2 154.39(5) . . . . ?
O2 P1 C1 P2 -86.09(7) . . . . ?
O3 P1 C1 P2 31.79(7) . . . . ?
O4 P2 C1 O7 -171.61(6) . . . . ?
O5 P2 C1 O7 64.27(8) . . . . ?
O6 P2 C1 O7 -49.98(7) . . . . ?
O4 P2 C1 C2 -55.78(10) . . . . ?
O5 P2 C1 C2 -179.90(8) . . . . ?
O6 P2 C1 C2 65.85(10) . . . . ?
O4 P2 C1 P1 70.70(7) . . . . ?
O5 P2 C1 P1 -53.42(7) . . . . ?
O6 P2 C1 P1 -167.68(5) . . . . ?
C21 N1 C2 C3 134.85(11) . . . . ?
C51 N1 C2 C3 -50.91(13) . . . . ?
C21 N1 C2 C5 35.56(14) . . . . ?
C51 N1 C2 C5 -150.20(10) . . . . ?
C21 N1 C2 C1 -98.46(12) . . . . ?
C51 N1 C2 C1 75.79(13) . . . . ?
O7 C1 C2 N1 -65.15(11) . . . . yes
P1 C1 C2 N1 54.34(11) . . . . yes
P2 C1 C2 N1 179.81(8) . . . . yes
O7 C1 C2 C3 59.67(11) . . . . yes
P1 C1 C2 C3 179.16(7) . . . . yes
P2 C1 C2 C3 -55.37(12) . . . . yes
O7 C1 C2 C5 164.06(9) . . . . yes
P1 C1 C2 C5 -76.45(11) . . . . yes
P2 C1 C2 C5 49.02(13) . . . . yes
N1 C2 C3 C4 -123.21(10) . . . . ?
C5 C2 C3 C4 -8.38(8) . . . . ?
C1 C2 C3 C4 113.84(10) . . . . ?
C2 C3 C4 C5 8.43(8) . . . . ?
C3 C4 C5 C2 -8.39(8) . . . . ?
N1 C2 C5 C4 121.67(9) . . . . ?
C3 C2 C5 C4 8.39(8) . . . . ?
C1 C2 C5 C4 -109.90(11) . . . . ?
C41 N2 C21 N1 0.45(12) . . . . ?
C51 N1 C21 N2 -0.71(12) . . . . ?
C2 N1 C21 N2 174.33(9) . . . . ?
C21 N2 C41 C51 -0.01(13) . . . . ?
N2 C41 C51 N1 -0.42(12) . . . . ?
C21 N1 C51 C41 0.70(12) . . . . ?
C2 N1 C51 C41 -174.36(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O1W 0.84 1.71 2.5211(14) 161.3 .
O3 H3 O5 0.84 1.68 2.5064(16) 165.5 .
O6 H6 O4 0.84 1.72 2.5553(15) 169.8 2_566
O7 H7 O1 0.84 1.88 2.6882(16) 162.3 2
N2 H2N O1 0.88 1.85 2.7271(17) 172.8 2_655
O1W H1W O5 0.84 1.97 2.7723(15) 160.0 2_556
O1W H2W O4 0.84 1.91 2.6876(17) 152.5 .
C3 H3B O6 0.99 2.39 3.1262(18) 130.6 .
C5 H5A O4 0.99 2.46 3.1476(18) 125.9 .
C21 H21 O5 0.95 2.25 3.116(2) 151.6 1_655

_refine_diff_density_max         0.668
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.115

####################################################################### 
# 
# 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_1a_tr01044ab
_database_code_depnum_ccdc_archive 'CCDC 1590600'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-01 downloaded from the CCDC.
;
##################################################################### 

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H34 Co3 N4 O20 P4, 6(H2 O)'
_chemical_formula_sum            'C16 H46 Co3 N4 O26 P4'
_chemical_formula_weight         1011.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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                   10.288(3)
_cell_length_b                   9.956(3)
_cell_length_c                   10.170(3)
_cell_angle_alpha                80.59(3)
_cell_angle_beta                 72.36(3)
_cell_angle_gamma                61.94(3)
_cell_volume                     875.7(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5103
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      28.80

_exptl_crystal_description       column
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_F_000             519
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    1.691
_shelx_estimated_absorpt_T_min   0.622
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
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)
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Kuma MK4-CCD, Sapphire2, large Be window'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            7949
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.091
_diffrn_reflns_theta_max         28.863
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4166
_reflns_number_gt                3380
_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       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_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)+(0.0988P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4166
_refine_ls_number_parameters     262
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1367
_refine_ls_wR_factor_gt          0.1319
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      0.999
_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
Co1 Co 1.0000 0.0000 0.5000 0.00905(15) Uani 1 2 d S . P . .
Co2 Co 0.46085(5) 0.29135(4) 0.46205(4) 0.01048(14) Uani 1 1 d . . . . .
P1 P 0.78236(9) 0.10521(8) 0.28905(8) 0.00906(18) Uani 1 1 d . . . . .
P2 P 0.73295(9) 0.34693(9) 0.47723(8) 0.00918(18) Uani 1 1 d . . . . .
O1 O 0.7831(3) 0.0719(2) 0.1504(2) 0.0129(4) Uani 1 1 d . . . . .
O2 O 0.9363(2) 0.0103(2) 0.3220(2) 0.0113(4) Uani 1 1 d . . . . .
O3 O 0.6511(2) 0.0912(2) 0.4052(2) 0.0115(4) Uani 1 1 d . . . . .
O4 O 0.7161(2) 0.5060(2) 0.4785(2) 0.0105(4) Uani 1 1 d . . . . .
O5 O 0.8781(3) 0.2301(2) 0.5151(2) 0.0126(4) Uani 1 1 d . . . . .
O6 O 0.5900(3) 0.3319(3) 0.5676(2) 0.0130(4) Uani 1 1 d . . . . .
O7 O 0.5804(2) 0.3968(2) 0.2912(2) 0.0101(4) Uani 1 1 d . . . . .
H7O H 0.5422 0.4816 0.3274 0.015 Uiso 1 1 calc R U . . .
N1 N 0.8264(3) 0.3317(3) 0.0419(3) 0.0107(5) Uani 1 1 d . . . . .
N2 N 0.8776(3) 0.2279(3) -0.1504(3) 0.0172(6) Uani 1 1 d D . . . .
H2N H 0.9307 0.1573 -0.2132 0.021 Uiso 1 1 d DR U . . .
C1 C 0.7390(3) 0.3100(3) 0.2973(3) 0.0112(6) Uani 1 1 d . . . . .
C2 C 0.8398(4) 0.3614(3) 0.1739(3) 0.0115(6) Uani 1 1 d . . . . .
C3 C 0.8142(4) 0.5294(4) 0.1742(3) 0.0179(7) Uani 1 1 d . . . . .
H3A H 0.8081 0.5839 0.0840 0.021 Uiso 1 1 calc R U . . .
H3B H 0.7276 0.5905 0.2495 0.021 Uiso 1 1 calc R U . . .
C4 C 0.9711(4) 0.4675(5) 0.2038(4) 0.0253(8) Uani 1 1 d . . . . .
H4A H 0.9646 0.4837 0.2995 0.030 Uiso 1 1 calc R U . . .
H4B H 1.0403 0.5046 0.1365 0.030 Uiso 1 1 calc R U . . .
C5 C 1.0074(4) 0.3034(4) 0.1786(3) 0.0186(7) Uani 1 1 d . . . . .
H5A H 1.0350 0.2315 0.2564 0.022 Uiso 1 1 calc R U . . .
H5B H 1.0834 0.2622 0.0902 0.022 Uiso 1 1 calc R U . . .
C21 C 0.9274(4) 0.2156(4) -0.0410(3) 0.0148(6) Uani 1 1 d . . . . .
H21 H 1.0199 0.1369 -0.0242 0.018 Uiso 1 1 calc R U . . .
C41 C 0.7402(4) 0.3570(4) -0.1386(4) 0.0203(7) Uani 1 1 d . . . . .
H41 H 0.6798 0.3936 -0.2030 0.024 Uiso 1 1 calc R U . . .
C51 C 0.7075(4) 0.4218(4) -0.0183(3) 0.0158(6) Uani 1 1 d . . . . .
H51 H 0.6196 0.5120 0.0180 0.019 Uiso 1 1 calc R U . . .
O1W O 0.7959(3) -0.0261(3) 0.6160(3) 0.0232(6) Uani 1 1 d D . . . .
H1W H 0.7366 -0.0030 0.5656 0.035 Uiso 1 1 d DR U . . .
H2W H 0.7508 0.0263 0.6873 0.035 Uiso 1 1 d DR U . . .
O2W O 0.3529(3) 0.1816(3) 0.6230(2) 0.0226(6) Uani 1 1 d D . . . .
H3W H 0.3712 0.0938 0.6057 0.034 Uiso 1 1 d DR U . . .
H4W H 0.2775 0.2158 0.6917 0.034 Uiso 1 1 d DR U . . .
O3W O 0.3508(3) 0.2677(3) 0.3321(3) 0.0267(6) Uani 1 1 d D . . . .
H5W H 0.2567 0.2971 0.3661 0.040 Uiso 1 1 d DR U . . .
H6W H 0.3766 0.2403 0.2506 0.040 Uiso 1 1 d DR U . . .
O4W O 0.5261(6) 0.1713(7) 0.0835(5) 0.0257(19) Uani 0.512(10) 1 d D . P A 1
H7W H 0.5259 0.0860 0.0926 0.039 Uiso 0.512(10) 1 d DR U P A 1
H8W H 0.6013 0.1650 0.1054 0.039 Uiso 0.512(10) 1 d DR U P A 1
O4X O 0.5331(6) 0.0664(7) 0.1271(5) 0.0213(17) Uani 0.488(10) 1 d D . P A 2
H7X H 0.5032 0.1136 0.0574 0.032 Uiso 0.488(10) 1 d DR U P A 2
H8X H 0.6133 0.0692 0.1276 0.032 Uiso 0.488(10) 1 d DR U P A 2
O5W O 0.5607(5) 0.1612(5) 0.8103(4) 0.0201(14) Uani 0.527(9) 1 d D . P B 1
H9W H 0.5293 0.0960 0.8154 0.030 Uiso 0.527(9) 1 d DR U P B 1
H10W H 0.5428 0.2201 0.7418 0.030 Uiso 0.527(9) 1 d DR U P B 1
O5X O 0.5094(7) 0.0904(7) 0.8471(6) 0.0269(18) Uani 0.473(9) 1 d D . P B 2
H9X H 0.4697 0.0306 0.8629 0.040 Uiso 0.473(9) 1 d DR U P B 2
H10X H 0.5466 0.0854 0.9118 0.040 Uiso 0.473(9) 1 d DR U P B 2
O6W O 0.0764(3) 0.3381(3) 0.5184(3) 0.0194(5) Uani 1 1 d D . . . .
H11W H 0.0113 0.3127 0.5121 0.029 Uiso 1 1 d DR U . . .
H12W H 0.1011 0.3046 0.5930 0.029 Uiso 1 1 d DR 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
Co1 O5 2.035(2) 2_756 yes
Co1 O5 2.035(2) . yes
Co1 O2 2.077(2) 2_756 yes
Co1 O2 2.077(2) . yes
Co1 O1W 2.186(2) 2_756 yes
Co1 O1W 2.186(3) . yes
Co2 O4 2.007(2) 2_666 yes
Co2 O3 2.039(2) . yes
Co2 O3W 2.084(2) . yes
Co2 O2W 2.136(2) . yes
Co2 O6 2.143(2) . yes
Co2 O7 2.226(2) . yes
P1 O1 1.498(2) . yes
P1 O2 1.524(2) . yes
P1 O3 1.547(2) . yes
P1 C1 1.881(3) . yes
P2 O4 1.512(2) . yes
P2 O5 1.516(2) . yes
P2 O6 1.540(2) . yes
P2 C1 1.902(3) . yes
O4 Co2 2.007(2) 2_666 ?
O7 C1 1.460(4) . ?
O7 H7O 0.8400 . ?
N1 C21 1.336(4) . ?
N1 C51 1.386(4) . ?
N1 C2 1.479(4) . ?
N2 C21 1.325(4) . ?
N2 C41 1.380(4) . ?
N2 H2N 0.8802 . ?
C1 C2 1.554(4) . ?
C2 C5 1.554(4) . ?
C2 C3 1.567(4) . ?
C3 C4 1.541(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.543(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C21 H21 0.9500 . ?
C41 C51 1.353(5) . ?
C41 H41 0.9500 . ?
C51 H51 0.9500 . ?
O1W H1W 0.8402 . ?
O1W H2W 0.8398 . ?
O2W H3W 0.8402 . ?
O2W H4W 0.8401 . ?
O3W H5W 0.8398 . ?
O3W H6W 0.8397 . ?
O4W H7W 0.8400 . ?
O4W H8W 0.8401 . ?
O4X O5X 1.771(9) 2_656 ?
O4X H7X 0.8400 . ?
O4X H8X 0.8401 . ?
O5W H9W 0.8399 . ?
O5W H10W 0.8400 . ?
O5X O4X 1.771(9) 2_656 ?
O5X H9X 0.8400 . ?
O5X H10X 0.8400 . ?
O6W H11W 0.8399 . ?
O6W H12W 0.8397 . ?

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
O5 Co1 O5 180.0 2_756 . yes
O5 Co1 O2 90.06(9) 2_756 2_756 yes
O5 Co1 O2 89.94(9) . 2_756 yes
O5 Co1 O2 89.94(9) 2_756 . yes
O5 Co1 O2 90.06(9) . . yes
O2 Co1 O2 180.0 2_756 . yes
O5 Co1 O1W 90.00(10) 2_756 2_756 yes
O5 Co1 O1W 90.00(10) . 2_756 yes
O2 Co1 O1W 87.38(9) 2_756 2_756 yes
O2 Co1 O1W 92.62(9) . 2_756 yes
O5 Co1 O1W 90.00(10) 2_756 . yes
O5 Co1 O1W 90.00(10) . . yes
O2 Co1 O1W 92.62(9) 2_756 . yes
O2 Co1 O1W 87.38(9) . . yes
O1W Co1 O1W 180.0 2_756 . yes
O4 Co2 O3 175.56(9) 2_666 . yes
O4 Co2 O3W 90.32(10) 2_666 . yes
O3 Co2 O3W 93.65(10) . . yes
O4 Co2 O2W 89.80(10) 2_666 . yes
O3 Co2 O2W 92.28(10) . . yes
O3W Co2 O2W 88.55(11) . . yes
O4 Co2 O6 89.94(9) 2_666 . yes
O3 Co2 O6 85.83(9) . . yes
O3W Co2 O6 170.88(10) . . yes
O2W Co2 O6 100.57(9) . . yes
O4 Co2 O7 92.43(9) 2_666 . yes
O3 Co2 O7 85.52(9) . . ?yes
O3W Co2 O7 91.18(10) . . yes
O2W Co2 O7 177.76(8) . . yes
O6 Co2 O7 79.70(8) . . yes
O1 P1 O2 112.50(13) . . yes
O1 P1 O3 112.11(13) . . yes
O2 P1 O3 111.78(13) . . yes
O1 P1 C1 110.88(13) . . yes
O2 P1 C1 106.08(13) . . yes
O3 P1 C1 102.92(13) . . yes
O4 P2 O5 110.58(13) . . yes
O4 P2 O6 111.93(13) . . yes
O5 P2 O6 112.90(13) . . yes
O4 P2 C1 108.65(13) . . yes
O5 P2 C1 109.70(13) . . yes
O6 P2 C1 102.73(13) . . yes
P1 O2 Co1 129.74(13) . . ?
P1 O3 Co2 115.22(12) . . ?
P2 O4 Co2 134.31(14) . 2_666 ?
P2 O5 Co1 134.06(13) . . ?
P2 O6 Co2 116.54(12) . . ?
C1 O7 Co2 102.75(16) . . ?
C1 O7 H7O 109.5 . . ?
Co2 O7 H7O 97.0 . . ?
C21 N1 C51 108.1(3) . . ?
C21 N1 C2 126.2(3) . . ?
C51 N1 C2 125.7(3) . . ?
C21 N2 C41 108.6(3) . . ?
C21 N2 H2N 119.6 . . ?
C41 N2 H2N 131.7 . . ?
O7 C1 C2 108.6(2) . . ?
O7 C1 P1 104.70(19) . . ?
C2 C1 P1 113.1(2) . . ?
O7 C1 P2 103.57(19) . . ?
C2 C1 P2 116.8(2) . . ?
P1 C1 P2 108.93(15) . . ?
N1 C2 C5 113.4(3) . . ?
N1 C2 C1 110.2(2) . . yes
C5 C2 C1 115.8(3) . . ?
N1 C2 C3 110.0(2) . . ?
C5 C2 C3 89.5(2) . . ?
C1 C2 C3 116.6(3) . . ?
C4 C3 C2 88.9(3) . . ?
C4 C3 H3A 113.8 . . ?
C2 C3 H3A 113.8 . . ?
C4 C3 H3B 113.8 . . ?
C2 C3 H3B 113.8 . . ?
H3A C3 H3B 111.1 . . ?
C3 C4 C5 90.9(3) . . ?
C3 C4 H4A 113.5 . . ?
C5 C4 H4A 113.5 . . ?
C3 C4 H4B 113.5 . . ?
C5 C4 H4B 113.5 . . ?
H4A C4 H4B 110.8 . . ?
C4 C5 C2 89.3(3) . . ?
C4 C5 H5A 113.8 . . ?
C2 C5 H5A 113.8 . . ?
C4 C5 H5B 113.8 . . ?
C2 C5 H5B 113.8 . . ?
H5A C5 H5B 111.0 . . ?
N2 C21 N1 109.0(3) . . ?
N2 C21 H21 125.5 . . ?
N1 C21 H21 125.5 . . ?
C51 C41 N2 107.2(3) . . ?
C51 C41 H41 126.4 . . ?
N2 C41 H41 126.4 . . ?
C41 C51 N1 107.0(3) . . ?
C41 C51 H51 126.5 . . ?
N1 C51 H51 126.5 . . ?
Co1 O1W H1W 110.3 . . ?
Co1 O1W H2W 111.7 . . ?
H1W O1W H2W 110.5 . . ?
Co2 O2W H3W 115.3 . . ?
Co2 O2W H4W 132.0 . . ?
H3W O2W H4W 110.4 . . ?
Co2 O3W H5W 114.0 . . ?
Co2 O3W H6W 135.3 . . ?
H5W O3W H6W 110.5 . . ?
H7W O4W H8W 110.4 . . ?
O5X O4X H7X 105.1 2_656 . ?
O5X O4X H8X 129.6 2_656 . ?
H7X O4X H8X 110.4 . . ?
H9W O5W H10W 110.5 . . ?
O4X O5X H9X 12.4 2_656 . ?
O4X O5X H10X 106.1 2_656 . ?
H9X O5X H10X 110.5 . . ?
H11W O6W H12W 110.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 P1 O2 Co1 -176.85(14) . . . . ?
O3 P1 O2 Co1 -49.68(19) . . . . ?
C1 P1 O2 Co1 61.76(19) . . . . ?
O1 P1 O3 Co2 -97.67(15) . . . . ?
O2 P1 O3 Co2 134.96(13) . . . . ?
C1 P1 O3 Co2 21.53(16) . . . . ?
O5 P2 O4 Co2 -141.69(17) . . . 2_666 ?
O6 P2 O4 Co2 -14.9(2) . . . 2_666 ?
C1 P2 O4 Co2 97.86(19) . . . 2_666 ?
O4 P2 O5 Co1 -165.75(16) . . . . ?
O6 P2 O5 Co1 68.0(2) . . . . ?
C1 P2 O5 Co1 -45.9(2) . . . . ?
O4 P2 O6 Co2 113.40(14) . . . . ?
O5 P2 O6 Co2 -121.05(14) . . . . ?
C1 P2 O6 Co2 -2.98(16) . . . . ?
Co2 O7 C1 C2 174.79(18) . . . . ?
Co2 O7 C1 P1 53.69(17) . . . . ?
Co2 O7 C1 P2 -60.41(16) . . . . ?
O1 P1 C1 O7 67.8(2) . . . . ?
O2 P1 C1 O7 -169.74(17) . . . . ?
O3 P1 C1 O7 -52.2(2) . . . . ?
O1 P1 C1 C2 -50.3(2) . . . . ?
O2 P1 C1 C2 72.1(2) . . . . ?
O3 P1 C1 C2 -170.3(2) . . . . ?
O1 P1 C1 P2 178.10(13) . . . . ?
O2 P1 C1 P2 -59.48(18) . . . . ?
O3 P1 C1 P2 58.05(17) . . . . ?
C21 N1 C2 C5 30.1(4) . . . . ?
C51 N1 C2 C5 -148.7(3) . . . . ?
C21 N1 C2 C1 -101.5(3) . . . . ?
C51 N1 C2 C1 79.7(4) . . . . ?
C21 N1 C2 C3 128.6(3) . . . . ?
C51 N1 C2 C3 -50.2(4) . . . . ?
O7 C1 C2 N1 -60.6(3) . . . . yes
P1 C1 C2 N1 55.2(3) . . . . yes
P2 C1 C2 N1 -177.22(19) . . . . yes
O7 C1 C2 C5 169.0(2) . . . . yes
P1 C1 C2 C5 -75.2(3) . . . . yes
P2 C1 C2 C5 52.4(3) . . . . yes
O7 C1 C2 C3 65.7(3) . . . . yes
P1 C1 C2 C3 -178.6(2) . . . . yes
P2 C1 C2 C3 -50.9(3) . . . . yes
N1 C2 C3 C4 -123.9(3) . . . . ?
C5 C2 C3 C4 -9.1(2) . . . . ?
C1 C2 C3 C4 109.8(3) . . . . ?
C2 C3 C4 C5 9.1(2) . . . . ?
C3 C4 C5 C2 -9.2(2) . . . . ?
N1 C2 C5 C4 120.7(3) . . . . ?
C1 C2 C5 C4 -110.5(3) . . . . ?
C3 C2 C5 C4 9.0(2) . . . . ?
C41 N2 C21 N1 0.4(4) . . . . ?
C51 N1 C21 N2 -0.2(3) . . . . ?
C2 N1 C21 N2 -179.2(3) . . . . ?
C21 N2 C41 C51 -0.5(4) . . . . ?
N2 C41 C51 N1 0.4(4) . . . . ?
C21 N1 C51 C41 -0.2(4) . . . . ?
C2 N1 C51 C41 178.8(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
O7 H7O O6 0.84 1.96 2.778(3) 165.7 2_666
N2 H2N O2 0.88 1.85 2.719(4) 169.3 2_755
O1W H1W O3 0.84 1.98 2.767(3) 156.4 .
O1W H2W O5W 0.84 1.95 2.702(5) 149.1 .
O1W H2W O5X 0.84 2.37 3.006(6) 132.9 .
O2W H3W O3 0.84 1.98 2.798(3) 162.7 2_656
O3W H5W O6W 0.84 1.94 2.717(4) 153.5 .
O3W H6W O4W 0.84 1.88 2.639(5) 150.1 .
O3W H6W O4X 0.84 2.01 2.709(6) 140.6 .
O4W H8W O1 0.84 1.82 2.616(6) 157.1 .
O4X H7X O5X 0.84 2.17 2.893(8) 144.6 1_554
O4X H8X O1 0.84 1.84 2.680(6) 173.5 .
O5W H10W O6 0.84 1.99 2.780(5) 156.8 .
O5X H9X O4X 0.84 0.97 1.771(9) 156.9 2_656
O5X H10X O4X 0.84 2.13 2.893(8) 150.1 1_556
O6W H11W O5 0.84 1.89 2.727(3) 171.3 1_455
O6W H12W O2W 0.84 2.38 2.962(4) 126.8 .
C3 H3B O4 0.99 2.33 2.957(4) 120.3 .
C3 H3B O2W 0.99 2.46 3.259(4) 137.4 2_666
C5 H5A O1W 0.99 2.46 3.392(4) 156.9 2_756
C21 H21 O1 0.95 2.33 3.052(4) 132.9 2_755

_refine_diff_density_max         0.746
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.155

####################################################################### 
# 
# 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_2a_tomeka
_database_code_depnum_ccdc_archive 'CCDC 1590601'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-01 downloaded from the CCDC.
;
##################################################################### 

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H34 Co3 N4 O18 P4, 2(H2 O)'
_chemical_formula_sum            'C18 H38 Co3 N4 O20 P4'
_chemical_formula_weight         931.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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                   7.9658(17)
_cell_length_b                   9.4269(19)
_cell_length_c                   9.9867(19)
_cell_angle_alpha                92.69(5)
_cell_angle_beta                 95.66(5)
_cell_angle_gamma                101.35(5)
_cell_volume                     730.0(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3046
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      30.76

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_F_000             475
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    2.004
_shelx_estimated_absorpt_T_min   0.781
_shelx_estimated_absorpt_T_max   0.906
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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)
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Technologies, Xcalibur R, Ruby'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            6688
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.913
_diffrn_reflns_theta_max         30.828
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4079
_reflns_number_gt                3323
_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, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_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)+(0.0343P)²+0.4734P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4079
_refine_ls_number_parameters     224
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.0903
_refine_ls_wR_factor_gt          0.0842
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.036
_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
Co1 Co 0.5000 0.5000 0.5000 0.00645(12) Uani 1 2 d S . P . .
Co2 Co -0.09684(5) 0.34365(4) 0.51722(4) 0.00684(10) Uani 1 1 d . . . . .
P1 P 0.23060(9) 0.43999(7) 0.71916(7) 0.00482(14) Uani 1 1 d . . . . .
O1 O 0.1961(3) 0.4676(2) 0.86190(19) 0.0084(4) Uani 1 1 d . . . . .
O2 O 0.4160(2) 0.4997(2) 0.69202(19) 0.0075(4) Uani 1 1 d . . . . .
O3 O 0.1028(2) 0.4939(2) 0.61739(19) 0.0068(4) Uani 1 1 d . . . . .
P2 P 0.22011(9) 0.20255(7) 0.49112(7) 0.00446(14) Uani 1 1 d . . . . .
O4 O 0.1967(2) 0.04243(19) 0.45512(19) 0.0070(4) Uani 1 1 d . . . . .
O5 O 0.4010(2) 0.28434(19) 0.47274(18) 0.0065(4) Uani 1 1 d . . . . .
O6 O 0.0831(2) 0.2713(2) 0.41357(18) 0.0060(4) Uani 1 1 d . . . . .
O7 O -0.0051(2) 0.2036(2) 0.67321(19) 0.0068(4) Uani 1 1 d . . . . .
H7O H -0.0431 0.1165 0.6457 0.010 Uiso 1 1 calc R U . . .
N1 N 0.2797(3) 0.2021(2) 0.9147(2) 0.0067(4) Uani 1 1 d . . . . .
N2 N 0.3752(3) 0.3178(2) 1.1089(2) 0.0094(5) Uani 1 1 d D . . . .
H2N H 0.4491 0.3800 1.1652 0.011 Uiso 1 1 d DR U . . .
C1 C 0.1818(3) 0.2378(3) 0.6723(3) 0.0060(5) Uani 1 1 d . . . . .
C2 C 0.2678(3) 0.1426(3) 0.7708(3) 0.0056(5) Uani 1 1 d . . . . .
C3 C 0.1664(4) -0.0142(3) 0.7647(3) 0.0073(5) Uani 1 1 d . . . . .
H3A H 0.1305 -0.0524 0.6700 0.009 Uiso 1 1 calc R U . . .
H3B H 0.0624 -0.0199 0.8126 0.009 Uiso 1 1 calc R U . . .
C4 C 0.2908(4) -0.1003(3) 0.8344(3) 0.0108(5) Uani 1 1 d . . . . .
H4A H 0.2699 -0.2006 0.7930 0.013 Uiso 1 1 calc R U . . .
H4B H 0.2771 -0.1043 0.9317 0.013 Uiso 1 1 calc R U . . .
C5 C 0.4738(4) -0.0165(3) 0.8134(3) 0.0110(5) Uani 1 1 d . . . . .
H5A H 0.5453 0.0100 0.9011 0.013 Uiso 1 1 calc R U . . .
H5B H 0.5315 -0.0768 0.7566 0.013 Uiso 1 1 calc R U . . .
C6 C 0.4480(3) 0.1208(3) 0.7428(3) 0.0076(5) Uani 1 1 d . . . . .
H6A H 0.5374 0.2056 0.7800 0.009 Uiso 1 1 calc R U . . .
H6B H 0.4541 0.1073 0.6446 0.009 Uiso 1 1 calc R U . . .
C21 C 0.4184(4) 0.2829(3) 0.9887(3) 0.0090(5) Uani 1 1 d . . . . .
H21 H 0.5295 0.3106 0.9596 0.011 Uiso 1 1 calc R U . . .
C41 C 0.2031(4) 0.2599(3) 1.1130(3) 0.0104(5) Uani 1 1 d . . . . .
H41 H 0.1386 0.2685 1.1870 0.013 Uiso 1 1 calc R U . . .
C51 C 0.1433(4) 0.1886(3) 0.9918(3) 0.0093(5) Uani 1 1 d . . . . .
H51 H 0.0285 0.1383 0.9645 0.011 Uiso 1 1 calc R U . . .
O1W O 0.2579(2) 0.5382(2) 0.37888(19) 0.0080(4) Uani 1 1 d D . . . .
H1W H 0.1923 0.4563 0.3761 0.012 Uiso 1 1 d DR U . . .
H2W H 0.2625 0.5677 0.3010 0.012 Uiso 1 1 d DR U . . .
O2W O -0.3075(2) 0.1905(2) 0.4695(2) 0.0098(4) Uani 1 1 d D . . . .
H3W H -0.4077 0.2066 0.4665 0.015 Uiso 1 1 d DR U . . .
H4W H -0.3054 0.1071 0.4950 0.015 Uiso 1 1 d DR U . . .
O3W O -0.1815(3) 0.3982(2) 0.8859(2) 0.0154(4) Uani 1 1 d D . . . .
H5W H -0.1933 0.4390 0.9599 0.023 Uiso 1 1 d DR U . . .
H6W H -0.0767 0.4026 0.8778 0.023 Uiso 1 1 d DR 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
Co1 O5 2.026(2) . yes
Co1 O5 2.026(2) 2_666 yes
Co1 O2 2.092(2) . yes
Co1 O2 2.092(2) 2_666 yes
Co1 O1W 2.273(2) 2_666 yes
Co1 O1W 2.273(2) . yes
Co2 O2W 1.988(2) . yes
Co2 O3 2.050(2) . yes
Co2 O6 2.050(2) . yes
Co2 O3 2.089(2) 2_566 yes
Co2 O1W 2.163(2) 2_566 yes
Co2 O7 2.247(2) . ?
P1 O1 1.499(2) . yes
P1 O2 1.529(2) . yes
P1 O3 1.542(2) . yes
P1 C1 1.895(3) . yes
O3 Co2 2.089(2) 2_566 ?
P2 O4 1.5058(19) . yes
P2 O5 1.528(2) . yes
P2 O6 1.539(2) . yes
P2 C1 1.889(3) . yes
O7 C1 1.461(3) . ?
O7 H7O 0.8400 . ?
N1 C21 1.342(4) . ?
N1 C51 1.381(3) . ?
N1 C2 1.505(3) . ?
N2 C21 1.325(3) . ?
N2 C41 1.378(4) . ?
N2 H2N 0.8800 . ?
C1 C2 1.560(4) . ?
C2 C3 1.534(4) . ?
C2 C6 1.540(4) . ?
C3 C4 1.537(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.554(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.541(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C21 H21 0.9500 . ?
C41 C51 1.352(4) . ?
C41 H41 0.9500 . ?
C51 H51 0.9500 . ?
O1W Co2 2.163(2) 2_566 ?
O1W H1W 0.8400 . ?
O1W H2W 0.8399 . ?
O2W H3W 0.8397 . ?
O2W H4W 0.8399 . ?
O3W H5W 0.8399 . ?
O3W H6W 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
O5 Co1 O5 180.00(10) . 2_666 yes
O5 Co1 O2 89.22(9) . . yes
O5 Co1 O2 90.78(9) 2_666 . yes
O5 Co1 O2 90.78(9) . 2_666 yes
O5 Co1 O2 89.22(9) 2_666 2_666 yes
O2 Co1 O2 180.0 . 2_666 yes
O5 Co1 O1W 91.81(9) . 2_666 yes
O5 Co1 O1W 88.18(9) 2_666 2_666 yes
O2 Co1 O1W 81.16(8) . 2_666 yes
O2 Co1 O1W 98.84(8) 2_666 2_666 yes
O5 Co1 O1W 88.19(9) . . yes
O5 Co1 O1W 91.81(9) 2_666 . yes
O2 Co1 O1W 98.85(8) . . yes
O2 Co1 O1W 81.15(8) 2_666 . yes
O1W Co1 O1W 180.0 2_666 . yes
O2W Co2 O3 164.70(8) . . yes
O2W Co2 O6 103.27(8) . . yes
O3 Co2 O6 87.09(8) . . yes
O2W Co2 O3 107.97(9) . 2_566 yes
O3 Co2 O3 83.07(9) . 2_566 yes
O6 Co2 O3 89.22(8) . 2_566 yes
O2W Co2 O1W 86.54(8) . 2_566 yes
O3 Co2 O1W 84.46(8) . 2_566 yes
O6 Co2 O1W 168.73(7) . 2_566 yes
O3 Co2 O1W 82.38(8) 2_566 2_566 yes
O2W Co2 O7 89.00(8) . . yes
O3 Co2 O7 81.24(8) . . yes
O6 Co2 O7 81.95(8) . . yes
O3 Co2 O7 162.34(7) 2_566 . yes
O1W Co2 O7 104.04(8) 2_566 . yes
O1 P1 O2 114.24(12) . . yes
O1 P1 O3 111.93(11) . . yes
O2 P1 O3 110.45(11) . . yes
O1 P1 C1 109.85(12) . . yes
O2 P1 C1 107.60(12) . . yes
O3 P1 C1 101.97(12) . . yes
P1 O2 Co1 123.87(12) . . ?
P1 O3 Co2 118.09(11) . . ?
P1 O3 Co2 140.07(12) . 2_566 ?
Co2 O3 Co2 96.92(9) . 2_566 ?
O4 P2 O5 112.02(12) . . yes
O4 P2 O6 112.68(12) . . yes
O5 P2 O6 110.54(11) . . yes
O4 P2 C1 110.96(12) . . yes
O5 P2 C1 107.93(12) . . yes
O6 P2 C1 102.20(11) . . yes
P2 O5 Co1 128.84(12) . . ?
P2 O6 Co2 118.98(11) . . ?
C1 O7 Co2 102.95(15) . . ?
C1 O7 H7O 109.5 . . ?
Co2 O7 H7O 108.0 . . ?
C21 N1 C51 107.8(2) . . ?
C21 N1 C2 127.2(2) . . ?
C51 N1 C2 124.9(2) . . ?
C21 N2 C41 108.7(2) . . ?
C21 N2 H2N 119.6 . . ?
C41 N2 H2N 131.0 . . ?
O7 C1 C2 110.0(2) . . ?
O7 C1 P2 105.44(17) . . ?
C2 C1 P2 112.81(17) . . ?
O7 C1 P1 101.05(16) . . ?
C2 C1 P1 116.28(18) . . ?
P2 C1 P1 110.04(14) . . ?
N1 C2 C3 106.6(2) . . ?
N1 C2 C6 108.0(2) . . ?
C3 C2 C6 101.9(2) . . ?
N1 C2 C1 111.1(2) . . yes
C3 C2 C1 112.6(2) . . ?
C6 C2 C1 115.9(2) . . ?
C2 C3 C4 105.4(2) . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3B 110.7 . . ?
C4 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
C3 C4 C5 105.1(2) . . ?
C3 C4 H4A 110.7 . . ?
C5 C4 H4A 110.7 . . ?
C3 C4 H4B 110.7 . . ?
C5 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
C6 C5 C4 106.2(2) . . ?
C6 C5 H5A 110.5 . . ?
C4 C5 H5A 110.5 . . ?
C6 C5 H5B 110.5 . . ?
C4 C5 H5B 110.5 . . ?
H5A C5 H5B 108.7 . . ?
C2 C6 C5 105.5(2) . . ?
C2 C6 H6A 110.6 . . ?
C5 C6 H6A 110.6 . . ?
C2 C6 H6B 110.6 . . ?
C5 C6 H6B 110.6 . . ?
H6A C6 H6B 108.8 . . ?
N2 C21 N1 108.9(2) . . ?
N2 C21 H21 125.5 . . ?
N1 C21 H21 125.5 . . ?
C51 C41 N2 107.1(3) . . ?
C51 C41 H41 126.5 . . ?
N2 C41 H41 126.5 . . ?
C41 C51 N1 107.5(3) . . ?
C41 C51 H51 126.3 . . ?
N1 C51 H51 126.3 . . ?
Co2 O1W Co1 116.89(9) 2_566 . ?
Co2 O1W H1W 96.6 2_566 . ?
Co1 O1W H1W 102.0 . . ?
Co2 O1W H2W 107.8 2_566 . ?
Co1 O1W H2W 120.1 . . ?
H1W O1W H2W 110.4 . . ?
Co2 O2W H3W 123.3 . . ?
Co2 O2W H4W 117.6 . . ?
H3W O2W H4W 110.5 . . ?
H5W O3W H6W 110.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 P1 O2 Co1 -172.97(11) . . . . ?
O3 P1 O2 Co1 -45.74(16) . . . . ?
C1 P1 O2 Co1 64.78(16) . . . . ?
O1 P1 O3 Co2 -101.68(14) . . . . ?
O2 P1 O3 Co2 129.82(12) . . . . ?
C1 P1 O3 Co2 15.68(14) . . . . ?
O1 P1 O3 Co2 110.05(18) . . . 2_566 ?
O2 P1 O3 Co2 -18.5(2) . . . 2_566 ?
C1 P1 O3 Co2 -132.59(18) . . . 2_566 ?
O4 P2 O5 Co1 177.79(12) . . . . ?
O6 P2 O5 Co1 51.24(17) . . . . ?
C1 P2 O5 Co1 -59.76(17) . . . . ?
O4 P2 O6 Co2 111.30(13) . . . . ?
O5 P2 O6 Co2 -122.51(12) . . . . ?
C1 P2 O6 Co2 -7.84(14) . . . . ?
Co2 O7 C1 C2 -176.94(16) . . . . ?
Co2 O7 C1 P2 -55.01(15) . . . . ?
Co2 O7 C1 P1 59.59(14) . . . . ?
O4 P2 C1 O7 -76.60(18) . . . . ?
O5 P2 C1 O7 160.31(15) . . . . ?
O6 P2 C1 O7 43.74(17) . . . . ?
O4 P2 C1 C2 43.5(2) . . . . ?
O5 P2 C1 C2 -79.6(2) . . . . ?
O6 P2 C1 C2 163.88(18) . . . . ?
O4 P2 C1 P1 175.20(12) . . . . ?
O5 P2 C1 P1 52.10(16) . . . . ?
O6 P2 C1 P1 -64.46(15) . . . . ?
O1 P1 C1 O7 67.57(18) . . . . ?
O2 P1 C1 O7 -167.50(14) . . . . ?
O3 P1 C1 O7 -51.27(17) . . . . ?
O1 P1 C1 C2 -51.5(2) . . . . ?
O2 P1 C1 C2 73.4(2) . . . . ?
O3 P1 C1 C2 -170.35(18) . . . . ?
O1 P1 C1 P2 178.67(12) . . . . ?
O2 P1 C1 P2 -56.40(16) . . . . ?
O3 P1 C1 P2 59.83(15) . . . . ?
C21 N1 C2 C3 136.9(3) . . . . ?
C51 N1 C2 C3 -47.0(3) . . . . ?
C21 N1 C2 C6 28.0(3) . . . . ?
C51 N1 C2 C6 -155.8(2) . . . . ?
C21 N1 C2 C1 -100.2(3) . . . . ?
C51 N1 C2 C1 76.0(3) . . . . ?
O7 C1 C2 N1 -79.1(3) . . . . yes
P2 C1 C2 N1 163.49(17) . . . . yes
P1 C1 C2 N1 35.0(3) . . . . yes
O7 C1 C2 C3 40.4(3) . . . . yes
P2 C1 C2 C3 -77.0(2) . . . . yes
P1 C1 C2 C3 154.47(18) . . . . yes
O7 C1 C2 C6 157.2(2) . . . . yes
P2 C1 C2 C6 39.7(3) . . . . yes
P1 C1 C2 C6 -88.8(2) . . . . yes
N1 C2 C3 C4 -73.4(2) . . . . ?
C6 C2 C3 C4 39.6(3) . . . . ?
C1 C2 C3 C4 164.5(2) . . . . ?
C2 C3 C4 C5 -27.6(3) . . . . ?
C3 C4 C5 C6 4.5(3) . . . . ?
N1 C2 C6 C5 75.5(3) . . . . ?
C3 C2 C6 C5 -36.6(3) . . . . ?
C1 C2 C6 C5 -159.1(2) . . . . ?
C4 C5 C6 C2 20.1(3) . . . . ?
C41 N2 C21 N1 -0.8(3) . . . . ?
C51 N1 C21 N2 1.2(3) . . . . ?
C2 N1 C21 N2 177.8(2) . . . . ?
C21 N2 C41 C51 0.1(3) . . . . ?
N2 C41 C51 N1 0.6(3) . . . . ?
C21 N1 C51 C41 -1.1(3) . . . . ?
C2 N1 C51 C41 -177.9(2) . . . . ?

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
O7 H7O O4 0.84 1.91 2.701(3) 156.2 2_556
N2 H2N O2 0.88 1.88 2.753(3) 170.4 2_667
O1W H1W O6 0.84 1.86 2.680(3) 164.5 .
O1W H2W O3W 0.84 1.98 2.774(3) 158.5 2_566
O2W H3W O5 0.84 1.82 2.645(3) 166.6 1_455
O2W H4W O4 0.84 1.86 2.637(3) 153.9 2_556
O3W H5W O1 0.84 1.95 2.789(3) 174.0 2_567
O3W H6W O1 0.84 2.16 2.985(3) 166.7 .
C3 H3A O4 0.99 2.43 3.187(3) 132.9 .
C3 H3A O6 0.99 2.46 3.162(4) 127.9 2_556
C3 H3A O2W 0.99 2.56 3.223(4) 124.1 2_556
C6 H6B O5 0.99 2.51 3.195(3) 125.9 .
C21 H21 O3W 0.95 2.48 3.432(4) 176.6 1_655
C41 H41 O6 0.95 2.35 3.242(3) 156.7 1_556

_refine_diff_density_max         0.609
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.121

####################################################################### 
# 
# 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_2_tr33
_database_code_depnum_ccdc_archive 'CCDC 1590599'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-01 downloaded from the CCDC.
;
##################################################################### 

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H16 N2 O7 P2, 4(H2 O)'
_chemical_formula_sum            'C9 H24 N2 O11 P2'
_chemical_formula_weight         398.24

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                   6.895(2)
_cell_length_b                   16.818(6)
_cell_length_c                   14.457(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.27(3)
_cell_angle_gamma                90
_cell_volume                     1676.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6382
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      77.83

_exptl_crystal_description       column
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    2.930
_shelx_estimated_absorpt_T_min   0.346
_shelx_estimated_absorpt_T_max   0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_T_max  1.0001
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
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                   'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur PX, Onyx'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.1956
_diffrn_reflns_number            9263
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.033
_diffrn_reflns_theta_max         77.976
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3505
_reflns_number_gt                3053
_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       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_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)+(0.1348P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3505
_refine_ls_number_parameters     221
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0605
_refine_ls_wR_factor_ref         0.1678
_refine_ls_wR_factor_gt          0.1628
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.050
_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 0.36208(7) 0.21703(3) 0.22984(3) 0.00984(19) Uani 1 1 d . . . . .
O1 O 0.4260(2) 0.17968(9) 0.14176(11) 0.0139(3) Uani 1 1 d . . . . .
O2 O 0.5193(2) 0.25598(10) 0.28880(10) 0.0136(3) Uani 1 1 d . . . . .
O3 O 0.2567(2) 0.15604(9) 0.29315(11) 0.0131(3) Uani 1 1 d . . . . .
H3 H 0.1971 0.1226 0.2600 0.020 Uiso 1 1 calc R U . . .
P2 P 0.01414(7) 0.31109(3) 0.30141(3) 0.01025(19) Uani 1 1 d . . . . .
O4 O -0.0968(2) 0.38740(9) 0.29512(10) 0.0136(3) Uani 1 1 d . . . . .
O5 O 0.1373(2) 0.30091(10) 0.39153(11) 0.0144(3) Uani 1 1 d . . . . .
H5 H 0.1713 0.3458 0.4115 0.022 Uiso 1 1 calc R U . . .
O6 O -0.1185(2) 0.23671(9) 0.29734(11) 0.0144(3) Uani 1 1 d . . . . .
H6 H -0.2321 0.2505 0.2826 0.022 Uiso 1 1 calc R U . . .
O7 O 0.0553(2) 0.26908(9) 0.12509(10) 0.0130(3) Uani 1 1 d . . . . .
H7 H 0.0002 0.2265 0.1396 0.020 Uiso 1 1 calc R U . . .
N1 N 0.4157(3) 0.35041(11) 0.09343(12) 0.0115(4) Uani 1 1 d . . . . .
N2 N 0.5256(3) 0.30077(12) -0.03350(13) 0.0169(4) Uani 1 1 d D . . . .
H2N H 0.5387 0.2802 -0.0890 0.020 Uiso 1 1 d DR U . . .
C1 C 0.1759(3) 0.29546(12) 0.20067(14) 0.0105(4) Uani 1 1 d . . . . .
C2 C 0.2719(3) 0.37352(13) 0.16478(14) 0.0119(4) Uani 1 1 d . . . . .
C3 C 0.1294(3) 0.43222(13) 0.11626(15) 0.0145(4) Uani 1 1 d . . . . .
H3A H 0.0896 0.4126 0.0542 0.017 Uiso 1 1 calc R U . . .
H3B H 0.0122 0.4403 0.1535 0.017 Uiso 1 1 calc R U . . .
C4 C 0.2471(4) 0.50989(14) 0.10911(18) 0.0214(5) Uani 1 1 d . . . . .
H4A H 0.1617 0.5567 0.1166 0.026 Uiso 1 1 calc R U . . .
H4B H 0.3094 0.5135 0.0482 0.026 Uiso 1 1 calc R U . . .
C5 C 0.4025(4) 0.50659(14) 0.18804(18) 0.0217(5) Uani 1 1 d . . . . .
H5A H 0.5345 0.5092 0.1626 0.026 Uiso 1 1 calc R U . . .
H5B H 0.3858 0.5515 0.2314 0.026 Uiso 1 1 calc R U . . .
C6 C 0.3709(3) 0.42671(14) 0.23746(15) 0.0154(4) Uani 1 1 d . . . . .
H6A H 0.4962 0.4036 0.2585 0.018 Uiso 1 1 calc R U . . .
H6B H 0.2872 0.4337 0.2917 0.018 Uiso 1 1 calc R U . . .
C21 C 0.3659(3) 0.32162(13) 0.00980(15) 0.0143(4) Uani 1 1 d . . . . .
H21 H 0.2372 0.3169 -0.0145 0.017 Uiso 1 1 calc R U . . .
C41 C 0.6837(3) 0.31613(14) 0.02341(17) 0.0181(5) Uani 1 1 d . . . . .
H41 H 0.8158 0.3069 0.0094 0.022 Uiso 1 1 calc R U . . .
C51 C 0.6162(3) 0.34686(13) 0.10314(16) 0.0159(4) Uani 1 1 d . . . . .
H51 H 0.6917 0.3629 0.1556 0.019 Uiso 1 1 calc R U . . .
O1W O 0.3162(2) 0.40145(10) 0.49172(11) 0.0172(3) Uani 1 1 d D . . . .
H1W H 0.4254 0.4112 0.4697 0.026 Uiso 1 1 d DR U . . .
H2W H 0.3286 0.3745 0.5404 0.026 Uiso 1 1 d DR U . . .
O2W O 0.6958(3) 0.43615(10) 0.44710(12) 0.0198(4) Uani 1 1 d D . . . .
H3W H 0.7588 0.4175 0.4030 0.030 Uiso 1 1 d DR U . . .
H4W H 0.7176 0.4851 0.4530 0.030 Uiso 1 1 d DR U . . .
O3W O 0.8057(2) 0.36222(10) 0.61263(11) 0.0167(3) Uani 1 1 d D . . . .
H5W H 0.6960 0.3478 0.6304 0.025 Uiso 1 1 d DR U . . .
H6W H 0.7980 0.3802 0.5585 0.025 Uiso 1 1 d DR U . . .
O4W O 0.0684(3) 0.04971(11) 0.20537(17) 0.0355(5) Uani 1 1 d D . . . .
H7W H -0.0339 0.0688 0.1819 0.053 Uiso 1 1 d DR U . . .
H8W H 0.0558 0.0007 0.2144 0.053 Uiso 1 1 d DR 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 1.4950(16) . yes
P1 O2 1.5133(16) . yes
P1 O3 1.5643(16) . yes
P1 C1 1.882(2) . yes
O3 H3 0.8400 . ?
P2 O4 1.4955(16) . yes
P2 O5 1.5489(18) . yes
P2 O6 1.5499(17) . yes
P2 C1 1.873(2) . yes
O5 H5 0.8400 . ?
O6 H6 0.8400 . ?
O7 C1 1.429(2) . ?
O7 H7 0.8400 . ?
N1 C21 1.340(3) . ?
N1 C51 1.387(3) . ?
N1 C2 1.498(3) . ?
N2 C21 1.326(3) . ?
N2 C41 1.375(3) . ?
N2 H2N 0.8802 . ?
C1 C2 1.564(3) . ?
C2 C6 1.529(3) . ?
C2 C3 1.550(3) . ?
C3 C4 1.542(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.549(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.539(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C21 H21 0.9500 . ?
C41 C51 1.355(3) . ?
C41 H41 0.9500 . ?
C51 H51 0.9500 . ?
O1W H1W 0.8404 . ?
O1W H2W 0.8402 . ?
O2W H3W 0.8403 . ?
O2W H4W 0.8402 . ?
O3W H5W 0.8400 . ?
O3W H6W 0.8400 . ?
O4W H7W 0.8400 . ?
O4W H8W 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
O1 P1 O2 116.15(10) . . yes
O1 P1 O3 111.85(9) . . yes
O2 P1 O3 106.88(9) . . yes
O1 P1 C1 108.42(9) . . yes
O2 P1 C1 107.42(9) . . yes
O3 P1 C1 105.52(9) . . yes
P1 O3 H3 109.5 . . ?
O4 P2 O5 114.59(9) . . yes
O4 P2 O6 112.94(9) . . yes
O5 P2 O6 104.76(9) . . yes
O4 P2 C1 112.69(9) . . yes
O5 P2 C1 108.29(10) . . yes
O6 P2 C1 102.61(9) . . yes
P2 O5 H5 109.5 . . ?
P2 O6 H6 109.5 . . ?
C1 O7 H7 109.5 . . ?
C21 N1 C51 108.10(19) . . ?
C21 N1 C2 123.68(18) . . ?
C51 N1 C2 127.93(19) . . ?
C21 N2 C41 108.9(2) . . ?
C21 N2 H2N 129.6 . . ?
C41 N2 H2N 121.6 . . ?
O7 C1 C2 104.50(16) . . ?
O7 C1 P2 106.97(14) . . ?
C2 C1 P2 113.83(14) . . ?
O7 C1 P1 109.64(14) . . ?
C2 C1 P1 111.77(14) . . ?
P2 C1 P1 109.83(10) . . ?
N1 C2 C6 109.46(17) . . ?
N1 C2 C3 106.05(16) . . ?
C6 C2 C3 101.95(17) . . ?
N1 C2 C1 107.59(16) . . yes
C6 C2 C1 116.66(17) . . ?
C3 C2 C1 114.57(17) . . ?
C4 C3 C2 103.91(18) . . ?
C4 C3 H3A 111.0 . . ?
C2 C3 H3A 111.0 . . ?
C4 C3 H3B 111.0 . . ?
C2 C3 H3B 111.0 . . ?
H3A C3 H3B 109.0 . . ?
C3 C4 C5 106.06(19) . . ?
C3 C4 H4A 110.5 . . ?
C5 C4 H4A 110.5 . . ?
C3 C4 H4B 110.5 . . ?
C5 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
C6 C5 C4 105.70(19) . . ?
C6 C5 H5A 110.6 . . ?
C4 C5 H5A 110.6 . . ?
C6 C5 H5B 110.6 . . ?
C4 C5 H5B 110.6 . . ?
H5A C5 H5B 108.7 . . ?
C2 C6 C5 104.90(18) . . ?
C2 C6 H6A 110.8 . . ?
C5 C6 H6A 110.8 . . ?
C2 C6 H6B 110.8 . . ?
C5 C6 H6B 110.8 . . ?
H6A C6 H6B 108.8 . . ?
N2 C21 N1 108.8(2) . . ?
N2 C21 H21 125.6 . . ?
N1 C21 H21 125.6 . . ?
C51 C41 N2 107.3(2) . . ?
C51 C41 H41 126.3 . . ?
N2 C41 H41 126.3 . . ?
C41 C51 N1 106.9(2) . . ?
C41 C51 H51 126.6 . . ?
N1 C51 H51 126.6 . . ?
H1W O1W H2W 110.4 . . ?
H3W O2W H4W 110.4 . . ?
H5W O3W H6W 110.5 . . ?
H7W O4W H8W 110.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 P2 C1 O7 -78.19(15) . . . . ?
O5 P2 C1 O7 153.99(13) . . . . ?
O6 P2 C1 O7 43.58(15) . . . . ?
O4 P2 C1 C2 36.71(17) . . . . ?
O5 P2 C1 C2 -91.11(16) . . . . ?
O6 P2 C1 C2 158.48(15) . . . . ?
O4 P2 C1 P1 162.89(10) . . . . ?
O5 P2 C1 P1 35.07(13) . . . . ?
O6 P2 C1 P1 -75.34(12) . . . . ?
O1 P1 C1 O7 37.32(16) . . . . ?
O2 P1 C1 O7 163.58(13) . . . . ?
O3 P1 C1 O7 -82.66(15) . . . . ?
O1 P1 C1 C2 -78.08(16) . . . . ?
O2 P1 C1 C2 48.18(16) . . . . ?
O3 P1 C1 C2 161.94(13) . . . . ?
O1 P1 C1 P2 154.58(10) . . . . ?
O2 P1 C1 P2 -79.16(12) . . . . ?
O3 P1 C1 P2 34.60(13) . . . . ?
C21 N1 C2 C6 -162.5(2) . . . . ?
C51 N1 C2 C6 24.4(3) . . . . ?
C21 N1 C2 C3 -53.2(3) . . . . ?
C51 N1 C2 C3 133.7(2) . . . . ?
C21 N1 C2 C1 69.8(2) . . . . ?
C51 N1 C2 C1 -103.3(2) . . . . ?
O7 C1 C2 N1 -71.03(19) . . . . yes
P2 C1 C2 N1 172.63(13) . . . . yes
P1 C1 C2 N1 47.48(19) . . . . yes
O7 C1 C2 C6 165.59(17) . . . . yes
P2 C1 C2 C6 49.2(2) . . . . yes
P1 C1 C2 C6 -75.9(2) . . . . yes
O7 C1 C2 C3 46.6(2) . . . . yes
P2 C1 C2 C3 -69.7(2) . . . . yes
P1 C1 C2 C3 165.12(14) . . . . yes
N1 C2 C3 C4 -74.4(2) . . . . ?
C6 C2 C3 C4 40.1(2) . . . . ?
C1 C2 C3 C4 167.05(17) . . . . ?
C2 C3 C4 C5 -25.2(2) . . . . ?
C3 C4 C5 C6 0.6(2) . . . . ?
N1 C2 C6 C5 72.0(2) . . . . ?
C3 C2 C6 C5 -40.0(2) . . . . ?
C1 C2 C6 C5 -165.58(18) . . . . ?
C4 C5 C6 C2 24.6(2) . . . . ?
C41 N2 C21 N1 0.2(3) . . . . ?
C51 N1 C21 N2 -0.4(2) . . . . ?
C2 N1 C21 N2 -174.72(18) . . . . ?
C21 N2 C41 C51 0.2(3) . . . . ?
N2 C41 C51 N1 -0.4(2) . . . . ?
C21 N1 C51 C41 0.5(2) . . . . ?
C2 N1 C51 C41 174.5(2) . . . . ?

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 H3 O4W 0.84 1.70 2.534(3) 173.0 .
O5 H5 O1W 0.84 1.78 2.530(2) 147.7 .
O6 H6 O2 0.84 1.72 2.519(2) 157.8 1_455
O7 H7 O3W 0.84 2.04 2.803(2) 151.2 4_465
N2 H2N O2 0.88 1.87 2.740(3) 169.2 4_565
O1W H1W O2W 0.84 1.95 2.772(3) 167.3 .
O1W H2W O1 0.84 1.84 2.658(2) 164.4 4_566
O2W H3W O4 0.84 1.94 2.772(2) 173.0 1_655
O2W H4W O1W 0.84 2.08 2.873(3) 156.1 3_666
O3W H5W O1 0.84 1.93 2.753(2) 166.7 4_566
O3W H6W O2W 0.84 1.98 2.787(3) 160.5 .
O4W H7W O3W 0.84 1.88 2.677(3) 158.7 4_465
O4W H8W O4 0.84 1.93 2.737(3) 160.4 2_545
C3 H3B O4 0.99 2.37 3.141(3) 134.2 .
C6 H6A O2 0.99 2.52 3.132(3) 119.4 .
C21 H21 O5 0.95 2.49 3.088(3) 120.8 4_565
C51 H51 O4 0.95 2.50 3.441(3) 172.8 1_655

_refine_diff_density_max         0.857
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.130

