# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_tr83ab
_database_code_depnum_ccdc_archive 'CCDC 1526910'
_audit_update_record             
;
2017-01-11 deposited with the CCDC.
2017-04-24 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         'C7 H14 N2 O7 P2'
_chemical_formula_sum            'C7 H14 N2 O7 P2'
_chemical_formula_weight         300.14

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                   7.947(3)
_cell_length_b                   7.954(3)
_cell_length_c                   9.044(3)
_cell_angle_alpha                104.08(3)
_cell_angle_beta                 90.23(3)
_cell_angle_gamma                91.08(3)
_cell_volume                     554.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      36.81

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_F_000             312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    0.424
_shelx_estimated_absorpt_T_min   0.873
_shelx_estimated_absorpt_T_max   0.931
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_T_max  0.942
_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 KM4-CCD, Sapphire2, large Be window'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            10837
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.063
_diffrn_reflns_theta_max         36.898
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4882
_reflns_number_gt                4506
_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)+(0.0781P)²+0.1361P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         4882
_refine_ls_number_parameters     173
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.1093
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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 0.50087(3) 0.67526(3) 0.25084(3) 0.00845(6) Uani 1 1 d . . . . .
O1 O 0.53615(9) 0.78596(9) 0.14393(9) 0.01372(13) Uani 1 1 d . . . . .
O2 O 0.54921(9) 0.75548(9) 0.41619(8) 0.01196(12) Uani 1 1 d . . . . .
H2 H 0.570(5) 0.691(5) 0.506(4) 0.096(11) Uiso 1 1 d . . . . .
O3 O 0.59368(9) 0.49794(9) 0.18856(8) 0.01301(12) Uani 1 1 d . . . . .
H3 H 0.5705 0.4299 0.2439 0.020 Uiso 1 1 calc R U . . .
P2 P 0.22994(3) 0.48351(3) 0.38256(2) 0.00808(6) Uani 1 1 d . . . . .
O4 O 0.20114(9) 0.59497(9) 0.54024(8) 0.01178(12) Uani 1 1 d . . . . .
O5 O 0.38381(9) 0.36844(9) 0.36996(8) 0.01109(11) Uani 1 1 d . . . . .
O6 O 0.07423(9) 0.36553(8) 0.32000(8) 0.01146(12) Uani 1 1 d . . . . .
H6 H -0.0085 0.3967 0.3770 0.017 Uiso 1 1 calc R U . . .
O7 O 0.23449(9) 0.49996(8) 0.09790(7) 0.00987(11) Uani 1 1 d . . . . .
H7 H 0.2955 0.5250 0.0304 0.052(7) Uiso 1 1 calc R . . . .
N1 N 0.17772(9) 0.85646(9) 0.12888(8) 0.00881(12) Uani 1 1 d . . . . .
N2 N 0.26965(10) 1.01705(10) -0.01719(10) 0.01246(13) Uani 1 1 d D . . . .
H2N H 0.3215 1.0958 -0.0549 0.015 Uiso 1 1 d DR U . . .
C1 C 0.27235(10) 0.61735(10) 0.24231(9) 0.00791(13) Uani 1 1 d . . . . .
C2 C 0.15655(10) 0.78195(10) 0.26443(9) 0.00877(13) Uani 1 1 d . . . . .
C3 C -0.02944(11) 0.72835(11) 0.26814(11) 0.01156(14) Uani 1 1 d . . . . .
H3A H -0.1001 0.8257 0.2608 0.017 Uiso 1 1 calc R U . . .
H3B H -0.0527 0.6958 0.3639 0.017 Uiso 1 1 calc R U . . .
H3C H -0.0544 0.6293 0.1821 0.017 Uiso 1 1 calc R U . . .
C4 C 0.20190(12) 0.92423(11) 0.40682(10) 0.01222(14) Uani 1 1 d . . . . .
H4A H 0.3218 0.9549 0.4051 0.018 Uiso 1 1 calc R U . . .
H4B H 0.1783 0.8822 0.4980 0.018 Uiso 1 1 calc R U . . .
H4C H 0.1347 1.0268 0.4086 0.018 Uiso 1 1 calc R U . . .
C21 C 0.27058(11) 0.99771(11) 0.12417(10) 0.01102(14) Uani 1 1 d . . . . .
H21 H 0.3277 1.0717 0.2085 0.013 Uiso 1 1 calc R U . . .
C41 C 0.17325(12) 0.88532(12) -0.10785(11) 0.01279(15) Uani 1 1 d . . . . .
H41 H 0.1525 0.8679 -0.2141 0.015 Uiso 1 1 calc R U . . .
C51 C 0.11361(11) 0.78530(11) -0.01678(10) 0.01100(14) Uani 1 1 d . . . . .
H51 H 0.0418 0.6858 -0.0468 0.013 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 1.4819(8) . ?
P1 O2 1.5208(9) . ?
P1 O3 1.5832(10) . ?
P1 C1 1.8618(11) . ?
O2 H2 1.08(4) . ?
O3 H3 0.8400 . ?
P2 O4 1.5057(9) . ?
P2 O5 1.5293(9) . ?
P2 O6 1.5570(9) . ?
P2 C1 1.8715(10) . ?
O6 H6 0.8400 . ?
O7 C1 1.4357(12) . ?
O7 H7 0.8400 . ?
N1 C21 1.3420(12) . ?
N1 C51 1.3915(13) . ?
N1 C2 1.4945(12) . ?
N2 C21 1.3243(13) . ?
N2 C41 1.3798(14) . ?
N2 H2N 0.8796 . ?
C1 C2 1.5876(13) . ?
C2 C4 1.5300(14) . ?
C2 C3 1.5334(13) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C21 H21 0.9500 . ?
C41 C51 1.3579(13) . ?
C41 H41 0.9500 . ?
C51 H51 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 115.12(5) . . ?
O1 P1 O3 107.44(5) . . ?
O2 P1 O3 110.94(5) . . ?
O1 P1 C1 109.18(5) . . ?
O2 P1 C1 108.34(5) . . ?
O3 P1 C1 105.38(5) . . ?
P1 O2 H2 128(2) . . ?
P1 O3 H3 109.5 . . ?
O4 P2 O5 114.18(5) . . ?
O4 P2 O6 112.18(5) . . ?
O5 P2 O6 108.09(5) . . ?
O4 P2 C1 111.70(5) . . ?
O5 P2 C1 103.80(5) . . ?
O6 P2 C1 106.26(5) . . ?
P2 O6 H6 109.5 . . ?
C1 O7 H7 109.5 . . ?
C21 N1 C51 108.06(8) . . ?
C21 N1 C2 125.87(8) . . ?
C51 N1 C2 125.95(7) . . ?
C21 N2 C41 109.03(8) . . ?
C21 N2 H2N 129.3 . . ?
C41 N2 H2N 121.7 . . ?
O7 C1 C2 109.45(7) . . ?
O7 C1 P1 108.97(6) . . ?
C2 C1 P1 112.64(6) . . ?
O7 C1 P2 103.42(6) . . ?
C2 C1 P2 113.55(6) . . ?
P1 C1 P2 108.34(5) . . ?
N1 C2 C4 107.88(7) . . ?
N1 C2 C3 106.84(7) . . ?
C4 C2 C3 110.08(8) . . ?
N1 C2 C1 108.15(7) . . ?
C4 C2 C1 113.22(7) . . ?
C3 C2 C1 110.41(7) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C21 N1 108.87(8) . . ?
N2 C21 H21 125.6 . . ?
N1 C21 H21 125.6 . . ?
C51 C41 N2 107.16(9) . . ?
C51 C41 H41 126.4 . . ?
N2 C41 H41 126.4 . . ?
C41 C51 N1 106.87(8) . . ?
C41 C51 H51 126.6 . . ?
N1 C51 H51 126.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 P1 C1 O7 69.87(7) . . . . ?
O2 P1 C1 O7 -164.06(5) . . . . ?
O3 P1 C1 O7 -45.26(6) . . . . ?
O1 P1 C1 C2 -51.78(7) . . . . ?
O2 P1 C1 C2 74.29(7) . . . . ?
O3 P1 C1 C2 -166.92(6) . . . . ?
O1 P1 C1 P2 -178.26(4) . . . . ?
O2 P1 C1 P2 -52.18(5) . . . . ?
O3 P1 C1 P2 66.61(5) . . . . ?
O4 P2 C1 O7 -159.41(5) . . . . ?
O5 P2 C1 O7 77.10(7) . . . . ?
O6 P2 C1 O7 -36.78(6) . . . . ?
O4 P2 C1 C2 -40.90(7) . . . . ?
O5 P2 C1 C2 -164.39(6) . . . . ?
O6 P2 C1 C2 81.74(7) . . . . ?
O4 P2 C1 P1 85.04(6) . . . . ?
O5 P2 C1 P1 -38.45(5) . . . . ?
O6 P2 C1 P1 -152.33(4) . . . . ?
C21 N1 C2 C4 20.34(11) . . . . ?
C51 N1 C2 C4 -164.10(8) . . . . ?
C21 N1 C2 C3 138.68(9) . . . . ?
C51 N1 C2 C3 -45.76(11) . . . . ?
C21 N1 C2 C1 -102.46(10) . . . . ?
C51 N1 C2 C1 73.10(10) . . . . ?
O7 C1 C2 N1 -53.81(8) . . . . ?
P1 C1 C2 N1 67.58(8) . . . . ?
P2 C1 C2 N1 -168.80(5) . . . . ?
O7 C1 C2 C4 -173.30(7) . . . . ?
P1 C1 C2 C4 -51.91(8) . . . . ?
P2 C1 C2 C4 71.71(8) . . . . ?
O7 C1 C2 C3 62.76(9) . . . . ?
P1 C1 C2 C3 -175.85(6) . . . . ?
P2 C1 C2 C3 -52.23(8) . . . . ?
C41 N2 C21 N1 0.17(10) . . . . ?
C51 N1 C21 N2 -0.84(10) . . . . ?
C2 N1 C21 N2 175.37(8) . . . . ?
C21 N2 C41 C51 0.59(11) . . . . ?
N2 C41 C51 N1 -1.08(10) . . . . ?
C21 N1 C51 C41 1.19(10) . . . . ?
C2 N1 C51 C41 -175.02(8) . . . . ?

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 O5 1.08(4) 1.37(4) 2.4361(12) 170(4) 2_666
O3 H3 O5 0.84 2.00 2.7043(13) 141.0 .
O6 H6 O4 0.84 1.70 2.5180(14) 163.1 2_566
O7 H7 O3 0.84 2.14 2.9369(14) 158.7 2_665
N2 H2N O1 0.88 1.77 2.6358(14) 165.7 2_675
C4 H4A O2 0.98 2.44 3.1016(16) 124.0 .
C4 H4B O4 0.98 2.42 3.1388(16) 130.2 .
C21 H21 O5 0.95 2.49 3.3378(18) 149.2 1_565
C41 H41 O6 0.95 2.57 3.0805(17) 113.9 2_565
C51 H51 O6 0.95 2.57 3.0801(17) 114.0 2_565
C51 H51 O7 0.95 2.60 3.5037(18) 159.2 2_565

_refine_diff_density_max         0.612
_refine_diff_density_min         -0.580
_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_tr14012
_database_code_depnum_ccdc_archive 'CCDC 1526912'
_audit_update_record             
;
2017-01-20 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H34 Co3 N4 O20 P4, 6(H2 O)'
_chemical_formula_sum            'C14 H46 Co3 N4 O26 P4'
_chemical_formula_weight         987.22

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                   9.609(3)
_cell_length_b                   9.850(3)
_cell_length_c                   10.253(3)
_cell_angle_alpha                82.94(3)
_cell_angle_beta                 74.54(3)
_cell_angle_gamma                64.73(3)
_cell_volume                     845.8(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    2812
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      28.79

_exptl_crystal_description       column
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_F_000             507
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.748
_shelx_estimated_absorpt_T_min   0.527
_shelx_estimated_absorpt_T_max   0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      80(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, Ruby'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            7550
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.775
_diffrn_reflns_theta_max         28.852
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3888
_reflns_number_gt                3187
_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 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0445P)²+0.9017P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3888
_refine_ls_number_parameters     235
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1066
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.056
_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 0.01360(17) Uani 1 2 d S . P . .
Co2 Co 0.44392(6) 0.29745(5) 0.46687(5) 0.01361(14) Uani 1 1 d . . . . .
P1 P 0.77053(11) 0.11301(10) 0.28612(9) 0.0122(2) Uani 1 1 d . . . . .
P2 P 0.74227(11) 0.34748(10) 0.47438(9) 0.0120(2) Uani 1 1 d . . . . .
O1 O 0.7648(3) 0.0810(3) 0.1488(2) 0.0164(5) Uani 1 1 d . . . . .
O2 O 0.9304(3) 0.0145(3) 0.3197(2) 0.0135(5) Uani 1 1 d . . . . .
O3 O 0.6325(3) 0.1012(3) 0.3996(2) 0.0125(5) Uani 1 1 d . . . . .
O4 O 0.7361(3) 0.5043(3) 0.4740(2) 0.0146(5) Uani 1 1 d . . . . .
O5 O 0.8919(3) 0.2301(3) 0.5117(2) 0.0141(5) Uani 1 1 d . . . . .
O6 O 0.5896(3) 0.3397(3) 0.5639(2) 0.0130(5) Uani 1 1 d . . . . .
O7 O 0.5701(3) 0.3981(3) 0.2936(2) 0.0133(5) Uani 1 1 d . . . . .
H7 H 0.5397 0.4880 0.3140 0.020 Uiso 1 1 calc R U . . .
N1 N 0.8381(3) 0.3249(3) 0.0465(3) 0.0126(6) Uani 1 1 d . . . . .
N2 N 0.8942(4) 0.2067(4) -0.1386(3) 0.0189(7) Uani 1 1 d D . . . .
H2N H 0.9439 0.1387 -0.2026 0.023 Uiso 1 1 d DR U . . .
C1 C 0.7364(4) 0.3141(4) 0.2992(3) 0.0126(7) Uani 1 1 d . . . . .
C2 C 0.8456(4) 0.3660(4) 0.1800(4) 0.0140(7) Uani 1 1 d . . . . .
C3 C 0.7929(5) 0.5366(4) 0.1724(4) 0.0200(8) Uani 1 1 d . . . . .
H3A H 0.8541 0.5634 0.0887 0.030 Uiso 1 1 calc R U . . .
H3B H 0.8109 0.5696 0.2503 0.030 Uiso 1 1 calc R U . . .
H3C H 0.6799 0.5859 0.1733 0.030 Uiso 1 1 calc R U . . .
C4 C 1.0186(4) 0.2899(4) 0.1919(4) 0.0179(8) Uani 1 1 d . . . . .
H4A H 1.0526 0.1808 0.1975 0.027 Uiso 1 1 calc R U . . .
H4B H 1.0273 0.3250 0.2736 0.027 Uiso 1 1 calc R U . . .
H4C H 1.0864 0.3155 0.1122 0.027 Uiso 1 1 calc R U . . .
C21 C 0.9461(4) 0.2095(4) -0.0321(4) 0.0161(7) Uani 1 1 d . . . . .
H21 H 1.0446 0.1406 -0.0142 0.019 Uiso 1 1 calc R U . . .
C41 C 0.7478(5) 0.3246(5) -0.1298(4) 0.0231(9) Uani 1 1 d . . . . .
H41 H 0.6841 0.3494 -0.1932 0.028 Uiso 1 1 calc R U . . .
C51 C 0.7119(4) 0.3979(4) -0.0152(4) 0.0180(8) Uani 1 1 d . . . . .
H51 H 0.6178 0.4838 0.0178 0.022 Uiso 1 1 calc R U . . .
O1W O 0.7777(3) -0.0202(3) 0.6055(3) 0.0173(6) Uani 1 1 d D . . . .
H1W H 0.7229 0.0155 0.5479 0.026 Uiso 1 1 d DR U . . .
H2W H 0.7226 0.0117 0.6830 0.026 Uiso 1 1 d DR U . . .
O2W O 0.3528(3) 0.1812(3) 0.6286(3) 0.0170(6) Uani 1 1 d D . . . .
H3W H 0.3627 0.0952 0.6135 0.025 Uiso 1 1 d DR U . . .
H4W H 0.4021 0.1764 0.6867 0.025 Uiso 1 1 d DR U . . .
O3W O 0.3007(3) 0.2787(3) 0.3483(3) 0.0193(6) Uani 1 1 d D . . . .
H5W H 0.2719 0.2110 0.3854 0.029 Uiso 1 1 d DR U . . .
H6W H 0.3328 0.2665 0.2642 0.029 Uiso 1 1 d DR U . . .
O4W O 0.4832(3) 0.1692(3) 0.0979(3) 0.0258(6) Uani 1 1 d D . . . .
H7W H 0.4552 0.2563 0.0644 0.039 Uiso 1 1 d DR U . . .
H8W H 0.5720 0.1409 0.1156 0.039 Uiso 1 1 d DR U . . .
O5W O 0.5256(3) 0.1085(3) 0.8285(3) 0.0276(7) Uani 1 1 d D . . . .
H9W H 0.5547 0.1404 0.8840 0.041 Uiso 1 1 d DR U . . .
H10W H 0.5156 0.0289 0.8575 0.041 Uiso 1 1 d DR U . . .
O6W O -0.0245(6) 0.4483(6) 0.6112(5) 0.0244(16) Uiso 0.554(9) 1 d D . P A 1
H11W H -0.0281 0.3850 0.6734 0.037 Uiso 0.554(9) 1 d DR U P A 1
H12W H 0.0678 0.4214 0.5619 0.037 Uiso 0.554(9) 1 d DR U P A 1
O6X O 0.0540(7) 0.3400(7) 0.6307(6) 0.0218(19) Uiso 0.446(9) 1 d D . P A 2
H11X H -0.0120 0.4132 0.6800 0.033 Uiso 0.446(9) 1 d DR U P A 2
H12X H 0.0258 0.3426 0.5593 0.033 Uiso 0.446(9) 1 d DR U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O5 2.055(3) . ?
Co1 O5 2.055(3) 2_756 ?
Co1 O2 2.097(2) 2_756 ?
Co1 O2 2.097(2) . ?
Co1 O1W 2.203(3) 2_756 ?
Co1 O1W 2.203(3) . ?
Co2 O4 2.005(3) 2_666 ?
Co2 O3 2.041(3) . ?
Co2 O2W 2.108(3) . ?
Co2 O6 2.113(2) . ?
Co2 O3W 2.138(2) . ?
Co2 O7 2.248(3) . ?
P1 O1 1.500(2) . ?
P1 O2 1.532(3) . ?
P1 O3 1.550(3) . ?
P1 C1 1.881(3) . ?
P2 O4 1.520(2) . ?
P2 O5 1.522(3) . ?
P2 O6 1.537(3) . ?
P2 C1 1.884(3) . ?
O4 Co2 2.005(3) 2_666 ?
O7 C1 1.466(4) . ?
O7 H7 0.8400 . ?
N1 C21 1.338(5) . ?
N1 C51 1.393(5) . ?
N1 C2 1.502(4) . ?
N2 C21 1.324(5) . ?
N2 C41 1.378(5) . ?
N2 H2N 0.8800 . ?
C1 C2 1.573(5) . ?
C2 C3 1.533(5) . ?
C2 C4 1.537(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C21 H21 0.9500 . ?
C41 C51 1.342(5) . ?
C41 H41 0.9500 . ?
C51 H51 0.9500 . ?
O1W H1W 0.8401 . ?
O1W H2W 0.8397 . ?
O2W H3W 0.8401 . ?
O2W H4W 0.8400 . ?
O3W H5W 0.8397 . ?
O3W H6W 0.8394 . ?
O4W H7W 0.8400 . ?
O4W H8W 0.8400 . ?
O5W H9W 0.8396 . ?
O5W H10W 0.8400 . ?
O6W H11W 0.8401 . ?
O6W H12W 0.8403 . ?
O6X H11X 0.8401 . ?
O6X H12X 0.8402 . ?

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 ?
O5 Co1 O2 90.85(10) . 2_756 ?
O5 Co1 O2 89.14(10) 2_756 2_756 ?
O5 Co1 O2 89.15(10) . . ?
O5 Co1 O2 90.85(10) 2_756 . ?
O2 Co1 O2 180.0 2_756 . ?
O5 Co1 O1W 88.08(10) . 2_756 ?
O5 Co1 O1W 91.92(10) 2_756 2_756 ?
O2 Co1 O1W 86.89(10) 2_756 2_756 ?
O2 Co1 O1W 93.11(10) . 2_756 ?
O5 Co1 O1W 91.92(10) . . ?
O5 Co1 O1W 88.08(10) 2_756 . ?
O2 Co1 O1W 93.11(10) 2_756 . ?
O2 Co1 O1W 86.89(10) . . ?
O1W Co1 O1W 180.0 2_756 . ?
O4 Co2 O3 177.14(10) 2_666 . ?
O4 Co2 O2W 92.64(11) 2_666 . ?
O3 Co2 O2W 90.19(10) . . ?
O4 Co2 O6 91.45(10) 2_666 . ?
O3 Co2 O6 87.80(10) . . ?
O2W Co2 O6 97.21(9) . . ?
O4 Co2 O3W 85.94(10) 2_666 . ?
O3 Co2 O3W 94.42(10) . . ?
O2W Co2 O3W 90.64(10) . . ?
O6 Co2 O3W 171.84(10) . . ?
O4 Co2 O7 93.78(10) 2_666 . ?
O3 Co2 O7 83.37(10) . . ?
O2W Co2 O7 172.99(10) . . ?
O6 Co2 O7 79.83(9) . . ?
O3W Co2 O7 92.62(9) . . ?
O1 P1 O2 112.34(15) . . ?
O1 P1 O3 112.57(14) . . ?
O2 P1 O3 110.72(14) . . ?
O1 P1 C1 111.32(15) . . ?
O2 P1 C1 107.19(14) . . ?
O3 P1 C1 102.12(15) . . ?
O4 P2 O5 111.03(14) . . ?
O4 P2 O6 111.06(15) . . ?
O5 P2 O6 113.29(14) . . ?
O4 P2 C1 106.99(15) . . ?
O5 P2 C1 110.76(15) . . ?
O6 P2 C1 103.28(14) . . ?
P1 O2 Co1 129.02(15) . . ?
P1 O3 Co2 117.03(14) . . ?
P2 O4 Co2 131.86(16) . 2_666 ?
P2 O5 Co1 133.05(13) . . ?
P2 O6 Co2 117.25(14) . . ?
C1 O7 Co2 102.51(19) . . ?
C1 O7 H7 109.5 . . ?
Co2 O7 H7 106.1 . . ?
C21 N1 C51 107.4(3) . . ?
C21 N1 C2 127.1(3) . . ?
C51 N1 C2 125.5(3) . . ?
C21 N2 C41 108.6(3) . . ?
C21 N2 H2N 125.3 . . ?
C41 N2 H2N 126.1 . . ?
O7 C1 C2 109.9(3) . . ?
O7 C1 P1 103.3(2) . . ?
C2 C1 P1 113.4(2) . . ?
O7 C1 P2 104.9(2) . . ?
C2 C1 P2 115.2(2) . . ?
P1 C1 P2 109.14(18) . . ?
N1 C2 C3 104.9(3) . . ?
N1 C2 C4 108.6(3) . . ?
C3 C2 C4 109.2(3) . . ?
N1 C2 C1 110.0(2) . . ?
C3 C2 C1 113.2(3) . . ?
C4 C2 C1 110.6(3) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C21 N1 109.2(3) . . ?
N2 C21 H21 125.4 . . ?
N1 C21 H21 125.4 . . ?
C51 C41 N2 107.4(3) . . ?
C51 C41 H41 126.3 . . ?
N2 C41 H41 126.3 . . ?
C41 C51 N1 107.4(3) . . ?
C41 C51 H51 126.3 . . ?
N1 C51 H51 126.3 . . ?
Co1 O1W H1W 102.0 . . ?
Co1 O1W H2W 126.6 . . ?
H1W O1W H2W 110.5 . . ?
Co2 O2W H3W 117.8 . . ?
Co2 O2W H4W 102.8 . . ?
H3W O2W H4W 110.4 . . ?
Co2 O3W H5W 106.0 . . ?
Co2 O3W H6W 121.8 . . ?
H5W O3W H6W 110.5 . . ?
H7W O4W H8W 110.4 . . ?
H9W O5W H10W 110.5 . . ?
H11W O6W H12W 110.4 . . ?
H11X O6X H12X 110.4 . . ?

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 -175.44(15) . . . . ?
O3 P1 O2 Co1 -48.6(2) . . . . ?
C1 P1 O2 Co1 62.0(2) . . . . ?
O1 P1 O3 Co2 -100.06(16) . . . . ?
O2 P1 O3 Co2 133.27(14) . . . . ?
C1 P1 O3 Co2 19.41(18) . . . . ?
O5 P2 O4 Co2 -141.83(18) . . . 2_666 ?
O6 P2 O4 Co2 -14.8(2) . . . 2_666 ?
C1 P2 O4 Co2 97.2(2) . . . 2_666 ?
O4 P2 O5 Co1 -167.14(18) . . . . ?
O6 P2 O5 Co1 67.1(2) . . . . ?
C1 P2 O5 Co1 -48.4(2) . . . . ?
O4 P2 O6 Co2 114.62(15) . . . . ?
O5 P2 O6 Co2 -119.62(15) . . . . ?
C1 P2 O6 Co2 0.25(18) . . . . ?
Co2 O7 C1 C2 177.96(19) . . . . ?
Co2 O7 C1 P1 56.65(19) . . . . ?
Co2 O7 C1 P2 -57.66(18) . . . . ?
O1 P1 C1 O7 68.0(2) . . . . ?
O2 P1 C1 O7 -168.8(2) . . . . ?
O3 P1 C1 O7 -52.3(2) . . . . ?
O1 P1 C1 C2 -50.9(3) . . . . ?
O2 P1 C1 C2 72.3(3) . . . . ?
O3 P1 C1 C2 -171.3(2) . . . . ?
O1 P1 C1 P2 179.23(16) . . . . ?
O2 P1 C1 P2 -57.6(2) . . . . ?
O3 P1 C1 P2 58.9(2) . . . . ?
O4 P2 C1 O7 -77.2(2) . . . . ?
O5 P2 C1 O7 161.69(18) . . . . ?
O6 P2 C1 O7 40.1(2) . . . . ?
O4 P2 C1 C2 43.8(3) . . . . ?
O5 P2 C1 C2 -77.3(3) . . . . ?
O6 P2 C1 C2 161.1(2) . . . . ?
O4 P2 C1 P1 172.68(16) . . . . ?
O5 P2 C1 P1 51.5(2) . . . . ?
O6 P2 C1 P1 -70.1(2) . . . . ?
C21 N1 C2 C3 135.7(4) . . . . ?
C51 N1 C2 C3 -47.2(4) . . . . ?
C21 N1 C2 C4 19.0(4) . . . . ?
C51 N1 C2 C4 -163.9(3) . . . . ?
C21 N1 C2 C1 -102.2(4) . . . . ?
C51 N1 C2 C1 74.9(4) . . . . ?
O7 C1 C2 N1 -65.3(3) . . . . ?
P1 C1 C2 N1 49.8(3) . . . . ?
P2 C1 C2 N1 176.5(2) . . . . ?
O7 C1 C2 C3 51.8(3) . . . . ?
P1 C1 C2 C3 166.8(2) . . . . ?
P2 C1 C2 C3 -66.4(3) . . . . ?
O7 C1 C2 C4 174.7(2) . . . . ?
P1 C1 C2 C4 -70.2(3) . . . . ?
P2 C1 C2 C4 56.5(3) . . . . ?
C41 N2 C21 N1 0.4(4) . . . . ?
C51 N1 C21 N2 -0.1(4) . . . . ?
C2 N1 C21 N2 177.4(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 -177.7(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 H7 O6 0.84 1.97 2.740(4) 151.9 2_666
N2 H2N O2 0.88 1.81 2.688(4) 171.2 2_755
C3 H3B O4 0.98 2.31 2.994(5) 126.0 .
C3 H3B O2W 0.98 2.54 3.225(4) 126.9 2_666
C3 H3B O6X 0.98 2.46 3.381(7) 156.0 2_666
C4 H4A O2 0.98 2.45 3.208(4) 134.3 .
C21 H21 O1 0.95 2.45 3.101(5) 125.7 2_755
O1W H1W O3 0.84 1.88 2.712(4) 169.5 .
O1W H2W O5W 0.84 2.01 2.801(4) 157.6 .
O2W H3W O3 0.84 1.94 2.772(3) 172.9 2_656
O2W H4W O5W 0.84 1.99 2.812(4) 164.7 .
O3W H5W O1W 0.84 2.11 2.903(3) 156.5 2_656
O3W H6W O4W 0.84 1.95 2.738(4) 154.9 .
O4W H8W O1 0.84 1.80 2.643(4) 178.4 .
O5W H9W O4W 0.84 2.13 2.783(4) 134.3 1_556
O5W H10W O4W 0.84 1.94 2.778(4) 171.8 2_656
O6W H11W N2 0.84 2.62 3.446(6) 166.8 1_456
O6W H12W O4 0.84 2.23 2.894(6) 136.3 2_666
O6X H12X O5 0.84 2.19 2.804(6) 129.7 1_455

_refine_diff_density_max         0.860
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.128

####################################################################### 
# 
# 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_tr22023ab
_database_code_depnum_ccdc_archive 'CCDC 1526913'
_audit_update_record             
;
2017-01-20 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H30 Co3 N4 O20 P4, 6(H2 O)'
_chemical_formula_sum            'C14 H42 Co3 N4 O26 P4'
_chemical_formula_weight         983.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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                   10.177(3)
_cell_length_b                   9.884(3)
_cell_length_c                   10.001(3)
_cell_angle_alpha                80.66(3)
_cell_angle_beta                 71.08(3)
_cell_angle_gamma                63.18(3)
_cell_volume                     849.1(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    2089
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      28.74

_exptl_crystal_description       plate
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_F_000             503
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.741
_shelx_estimated_absorpt_T_min   0.722
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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      130(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, Ruby'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            6388
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.691
_diffrn_reflns_theta_max         28.800
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             3783
_reflns_number_gt                2832
_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 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0263P)²+0.5221P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3783
_refine_ls_number_parameters     233
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.0879
_refine_ls_wR_factor_gt          0.0785
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.033
_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 0.00748(16) Uani 1 2 d S . P . .
Co2 Co 0.46081(5) 0.29125(5) 0.46004(5) 0.00767(13) Uani 1 1 d . . . . .
P1 P 0.78679(10) 0.10457(10) 0.28814(10) 0.0084(2) Uani 1 1 d . . . . .
P2 P 0.73163(10) 0.34422(10) 0.48655(10) 0.0066(2) Uani 1 1 d . . . . .
O1 O 0.7885(3) 0.0770(3) 0.1444(3) 0.0114(5) Uani 1 1 d . . . . .
O2 O 0.9403(3) 0.0071(3) 0.3199(3) 0.0104(5) Uani 1 1 d . . . . .
O3 O 0.6517(3) 0.0882(3) 0.4056(3) 0.0092(5) Uani 1 1 d . . . . .
O4 O 0.7156(3) 0.5036(3) 0.4881(3) 0.0092(5) Uani 1 1 d . . . . .
O5 O 0.8732(3) 0.2287(3) 0.5276(3) 0.0093(5) Uani 1 1 d . . . . .
O6 O 0.5826(3) 0.3302(3) 0.5760(2) 0.0080(5) Uani 1 1 d . . . . .
O7 O 0.5915(3) 0.3938(3) 0.2894(3) 0.0081(5) Uani 1 1 d . . . . .
H7 H 0.5523 0.4787 0.3266 0.012 Uiso 1 1 calc R U . . .
N1 N 0.8474(3) 0.3431(3) 0.0411(3) 0.0098(6) Uani 1 1 d . . . . .
N2 N 0.8894(4) 0.2522(4) -0.1575(3) 0.0205(8) Uani 1 1 d D . . . .
H2N H 0.9406 0.1840 -0.2211 0.025 Uiso 1 1 d DR U . . .
C1 C 0.7479(4) 0.3065(4) 0.3025(4) 0.0083(7) Uani 1 1 d . . . . .
C2 C 0.8586(4) 0.3527(4) 0.1813(4) 0.0087(7) Uani 1 1 d . . . . .
C3 C 0.9005(4) 0.4789(4) 0.1889(4) 0.0166(9) Uani 1 1 d . . . . .
H3A H 0.9133 0.5432 0.1032 0.020 Uiso 1 1 calc R U . . .
H3B H 0.8570 0.5324 0.2795 0.020 Uiso 1 1 calc R U . . .
C4 C 1.0176(4) 0.3166(5) 0.1846(4) 0.0195(9) Uani 1 1 d . . . . .
H4A H 1.1024 0.2813 0.0963 0.023 Uiso 1 1 calc R U . . .
H4B H 1.0461 0.2705 0.2725 0.023 Uiso 1 1 calc R U . . .
C21 C 0.9365(4) 0.2250(4) -0.0437(4) 0.0152(8) Uani 1 1 d . . . . .
H21 H 1.0199 0.1361 -0.0253 0.018 Uiso 1 1 calc R U . . .
C41 C 0.7658(5) 0.3913(5) -0.1461(4) 0.0220(9) Uani 1 1 d . . . . .
H41 H 0.7098 0.4384 -0.2134 0.026 Uiso 1 1 calc R U . . .
C51 C 0.7388(4) 0.4484(4) -0.0216(4) 0.0163(9) Uani 1 1 d . . . . .
H51 H 0.6599 0.5431 0.0159 0.020 Uiso 1 1 calc R U . . .
O1W O 0.7964(3) -0.0359(3) 0.6193(3) 0.0125(6) Uani 1 1 d D . . . .
H1W H 0.7426 -0.0032 0.5629 0.019 Uiso 1 1 d DR U . . .
H2W H 0.7471 0.0090 0.6967 0.019 Uiso 1 1 d DR U . . .
O2W O 0.3402(3) 0.1896(3) 0.6267(3) 0.0146(6) Uani 1 1 d D . . . .
H3W H 0.3487 0.1053 0.6090 0.022 Uiso 1 1 d DR U . . .
H4W H 0.3620 0.1841 0.7021 0.022 Uiso 1 1 d DR U . . .
O3W O 0.3554(3) 0.2719(3) 0.3245(3) 0.0193(6) Uani 1 1 d D . . . .
H5W H 0.2690 0.2722 0.3650 0.029 Uiso 1 1 d DR U . . .
H6W H 0.3989 0.2192 0.2515 0.029 Uiso 1 1 d DR U . . .
O4W O 0.5442(3) 0.0875(4) 0.1017(3) 0.0409(9) Uani 1 1 d D . . . .
H7W H 0.5431 0.1114 0.0175 0.061 Uiso 1 1 d DR U . . .
H8W H 0.6214 0.0879 0.1150 0.061 Uiso 1 1 d DR U . . .
O5W O 0.5235(4) 0.1700(4) 0.8291(3) 0.0411(9) Uani 1 1 d D . . . .
H9W H 0.5344 0.2266 0.7582 0.062 Uiso 1 1 d DR U . . .
H10W H 0.5084 0.0998 0.8091 0.062 Uiso 1 1 d DR U . . .
O6W O 0.0744(3) 0.3456(3) 0.5195(3) 0.0222(7) Uani 1 1 d D . . . .
H11W H 0.0081 0.3119 0.5361 0.033 Uiso 1 1 d DR U . . .
H12W H 0.1193 0.3169 0.5829 0.033 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 2.047(3) 2_756 ?
Co1 O5 2.047(3) . ?
Co1 O2 2.061(2) 2_756 ?
Co1 O2 2.061(2) . ?
Co1 O1W 2.183(2) 2_756 ?
Co1 O1W 2.183(2) . ?
Co2 O4 2.014(3) 2_666 ?
Co2 O3W 2.059(3) . ?
Co2 O3 2.061(3) . ?
Co2 O2W 2.130(3) . ?
Co2 O6 2.130(2) . ?
Co2 O7 2.211(3) . ?
P1 O1 1.499(3) . ?
P1 O2 1.528(3) . ?
P1 O3 1.546(3) . ?
P1 C1 1.872(4) . ?
P2 O4 1.511(3) . ?
P2 O5 1.515(2) . ?
P2 O6 1.546(2) . ?
P2 C1 1.877(4) . ?
O4 Co2 2.014(3) 2_666 ?
O7 C1 1.468(4) . ?
O7 H7 0.8400 . ?
N1 C21 1.331(5) . ?
N1 C51 1.378(5) . ?
N1 C2 1.464(4) . ?
N2 C21 1.317(5) . ?
N2 C41 1.372(5) . ?
N2 H2N 0.8597 . ?
C1 C2 1.532(5) . ?
C2 C4 1.503(5) . ?
C2 C3 1.509(5) . ?
C3 C4 1.504(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C21 H21 0.9500 . ?
C41 C51 1.346(5) . ?
C41 H41 0.9500 . ?
C51 H51 0.9500 . ?
O1W H1W 0.8400 . ?
O1W H2W 0.8400 . ?
O2W H3W 0.8400 . ?
O2W H4W 0.8400 . ?
O3W H5W 0.8396 . ?
O3W H6W 0.8398 . ?
O4W H7W 0.8399 . ?
O4W H8W 0.8400 . ?
O5W H9W 0.8398 . ?
O5W H10W 0.8397 . ?
O6W H11W 0.8400 . ?
O6W H12W 0.8398 . ?

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 . ?
O5 Co1 O2 92.34(10) 2_756 2_756 ?
O5 Co1 O2 87.66(10) . 2_756 ?
O5 Co1 O2 87.67(10) 2_756 . ?
O5 Co1 O2 92.33(10) . . ?
O2 Co1 O2 180.0 2_756 . ?
O5 Co1 O1W 89.61(10) 2_756 2_756 ?
O5 Co1 O1W 90.39(10) . 2_756 ?
O2 Co1 O1W 87.35(10) 2_756 2_756 ?
O2 Co1 O1W 92.65(10) . 2_756 ?
O5 Co1 O1W 90.39(10) 2_756 . ?
O5 Co1 O1W 89.61(10) . . ?
O2 Co1 O1W 92.65(10) 2_756 . ?
O2 Co1 O1W 87.35(10) . . ?
O1W Co1 O1W 180.00(8) 2_756 . ?
O4 Co2 O3W 87.85(11) 2_666 . ?
O4 Co2 O3 175.97(9) 2_666 . ?
O3W Co2 O3 94.91(11) . . ?
O4 Co2 O2W 89.89(10) 2_666 . ?
O3W Co2 O2W 90.38(10) . . ?
O3 Co2 O2W 93.02(10) . . ?
O4 Co2 O6 90.99(10) 2_666 . ?
O3W Co2 O6 171.60(10) . . ?
O3 Co2 O6 85.85(10) . . ?
O2W Co2 O6 97.93(9) . . ?
O4 Co2 O7 91.03(10) 2_666 . ?
O3W Co2 O7 90.92(10) . . ?
O3 Co2 O7 86.00(10) . . ?
O2W Co2 O7 178.43(9) . . ?
O6 Co2 O7 80.78(9) . . ?
O1 P1 O2 112.69(14) . . ?
O1 P1 O3 111.96(14) . . ?
O2 P1 O3 111.72(14) . . ?
O1 P1 C1 110.42(15) . . ?
O2 P1 C1 106.32(15) . . ?
O3 P1 C1 103.15(15) . . ?
O4 P2 O5 111.30(13) . . ?
O4 P2 O6 111.39(14) . . ?
O5 P2 O6 113.33(14) . . ?
O4 P2 C1 107.90(15) . . ?
O5 P2 C1 109.30(15) . . ?
O6 P2 C1 103.16(14) . . ?
P1 O2 Co1 128.64(15) . . ?
P1 O3 Co2 113.45(13) . . ?
P2 O4 Co2 135.53(14) . 2_666 ?
P2 O5 Co1 133.54(14) . . ?
P2 O6 Co2 115.49(13) . . ?
C1 O7 Co2 101.84(18) . . ?
C1 O7 H7 109.5 . . ?
Co2 O7 H7 96.7 . . ?
C21 N1 C51 108.5(3) . . ?
C21 N1 C2 124.9(3) . . ?
C51 N1 C2 126.4(3) . . ?
C21 N2 C41 109.1(3) . . ?
C21 N2 H2N 116.5 . . ?
C41 N2 H2N 134.4 . . ?
O7 C1 C2 109.0(3) . . ?
O7 C1 P1 104.0(2) . . ?
C2 C1 P1 111.5(2) . . ?
O7 C1 P2 104.3(2) . . ?
C2 C1 P2 116.7(2) . . ?
P1 C1 P2 110.31(18) . . ?
N1 C2 C4 114.3(3) . . ?
N1 C2 C3 112.3(3) . . ?
C4 C2 C3 59.9(2) . . ?
N1 C2 C1 113.8(3) . . ?
C4 C2 C1 122.0(3) . . ?
C3 C2 C1 124.2(3) . . ?
C4 C3 C2 59.8(2) . . ?
C4 C3 H3A 117.8 . . ?
C2 C3 H3A 117.8 . . ?
C4 C3 H3B 117.8 . . ?
C2 C3 H3B 117.8 . . ?
H3A C3 H3B 114.9 . . ?
C2 C4 C3 60.3(2) . . ?
C2 C4 H4A 117.7 . . ?
C3 C4 H4A 117.7 . . ?
C2 C4 H4B 117.7 . . ?
C3 C4 H4B 117.7 . . ?
H4A C4 H4B 114.9 . . ?
N2 C21 N1 108.5(3) . . ?
N2 C21 H21 125.8 . . ?
N1 C21 H21 125.8 . . ?
C51 C41 N2 107.1(3) . . ?
C51 C41 H41 126.4 . . ?
N2 C41 H41 126.4 . . ?
C41 C51 N1 106.8(4) . . ?
C41 C51 H51 126.6 . . ?
N1 C51 H51 126.6 . . ?
Co1 O1W H1W 102.4 . . ?
Co1 O1W H2W 115.8 . . ?
H1W O1W H2W 110.4 . . ?
Co2 O2W H3W 115.8 . . ?
Co2 O2W H4W 111.4 . . ?
H3W O2W H4W 110.4 . . ?
Co2 O3W H5W 113.9 . . ?
Co2 O3W H6W 126.3 . . ?
H5W O3W H6W 110.5 . . ?
H7W O4W H8W 110.5 . . ?
H9W O5W H10W 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 -179.98(16) . . . . ?
O3 P1 O2 Co1 -52.9(2) . . . . ?
C1 P1 O2 Co1 58.9(2) . . . . ?
O1 P1 O3 Co2 -95.07(16) . . . . ?
O2 P1 O3 Co2 137.46(14) . . . . ?
C1 P1 O3 Co2 23.65(17) . . . . ?
O5 P2 O4 Co2 -144.10(19) . . . 2_666 ?
O6 P2 O4 Co2 -16.6(3) . . . 2_666 ?
C1 P2 O4 Co2 96.0(2) . . . 2_666 ?
O4 P2 O5 Co1 -160.87(18) . . . . ?
O6 P2 O5 Co1 72.7(2) . . . . ?
C1 P2 O5 Co1 -41.8(2) . . . . ?
O4 P2 O6 Co2 111.96(15) . . . . ?
O5 P2 O6 Co2 -121.61(15) . . . . ?
C1 P2 O6 Co2 -3.54(18) . . . . ?
Co2 O7 C1 C2 174.5(2) . . . . ?
Co2 O7 C1 P1 55.5(2) . . . . ?
Co2 O7 C1 P2 -60.14(19) . . . . ?
O1 P1 C1 O7 64.6(2) . . . . ?
O2 P1 C1 O7 -172.9(2) . . . . ?
O3 P1 C1 O7 -55.2(2) . . . . ?
O1 P1 C1 C2 -52.8(3) . . . . ?
O2 P1 C1 C2 69.8(3) . . . . ?
O3 P1 C1 C2 -172.6(2) . . . . ?
O1 P1 C1 P2 175.89(15) . . . . ?
O2 P1 C1 P2 -61.6(2) . . . . ?
O3 P1 C1 P2 56.10(19) . . . . ?
O4 P2 C1 O7 -74.2(2) . . . . ?
O5 P2 C1 O7 164.67(19) . . . . ?
O6 P2 C1 O7 43.8(2) . . . . ?
O4 P2 C1 C2 46.1(3) . . . . ?
O5 P2 C1 C2 -75.1(3) . . . . ?
O6 P2 C1 C2 164.1(2) . . . . ?
O4 P2 C1 P1 174.66(15) . . . . ?
O5 P2 C1 P1 53.5(2) . . . . ?
O6 P2 C1 P1 -67.36(19) . . . . ?
C21 N1 C2 C4 51.2(5) . . . . ?
C51 N1 C2 C4 -133.1(4) . . . . ?
C21 N1 C2 C3 117.1(4) . . . . ?
C51 N1 C2 C3 -67.3(4) . . . . ?
C21 N1 C2 C1 -95.3(4) . . . . ?
C51 N1 C2 C1 80.4(4) . . . . ?
O7 C1 C2 N1 -52.9(4) . . . . ?
P1 C1 C2 N1 61.4(3) . . . . ?
P2 C1 C2 N1 -170.6(2) . . . . ?
O7 C1 C2 C4 163.5(3) . . . . ?
P1 C1 C2 C4 -82.2(4) . . . . ?
P2 C1 C2 C4 45.7(4) . . . . ?
O7 C1 C2 C3 90.3(4) . . . . ?
P1 C1 C2 C3 -155.4(3) . . . . ?
P2 C1 C2 C3 -27.4(4) . . . . ?
N1 C2 C3 C4 -106.0(3) . . . . ?
C1 C2 C3 C4 110.3(4) . . . . ?
N1 C2 C4 C3 102.7(3) . . . . ?
C1 C2 C4 C3 -113.8(4) . . . . ?
C41 N2 C21 N1 -0.4(4) . . . . ?
C51 N1 C21 N2 0.6(4) . . . . ?
C2 N1 C21 N2 176.9(3) . . . . ?
C21 N2 C41 C51 0.0(4) . . . . ?
N2 C41 C51 N1 0.3(4) . . . . ?
C21 N1 C51 C41 -0.5(4) . . . . ?
C2 N1 C51 C41 -176.8(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 H7 O6 0.84 1.95 2.771(4) 166.6 2_666
N2 H2N O2 0.86 1.94 2.781(4) 164.3 2_755
O1W H1W O3 0.84 1.97 2.794(3) 167.3 .
O1W H2W O5W 0.84 2.22 2.960(5) 147.1 .
O2W H3W O3 0.84 1.94 2.778(3) 171.9 2_656
O2W H4W O5W 0.84 2.33 3.100(4) 152.9 .
O3W H5W O6W 0.84 1.98 2.734(4) 149.1 .
O3W H6W O4W 0.84 1.89 2.712(4) 164.7 .
O4W H7W O5W 0.84 1.93 2.764(5) 175.5 1_554
O4W H8W O1 0.84 1.77 2.610(4) 176.6 .
O5W H9W O6 0.84 1.97 2.801(4) 171.1 .
O5W H10W O4W 0.84 2.14 2.852(5) 143.1 2_656
O6W H11W O5 0.84 1.92 2.744(3) 166.7 1_455
O6W H12W O2W 0.84 2.18 2.903(4) 144.8 .
C3 H3B O4 0.99 2.18 2.954(5) 134.3 .
C4 H4B O1W 0.99 2.46 3.320(5) 144.5 2_756
C21 H21 O1 0.95 2.29 3.061(5) 137.4 2_755

_refine_diff_density_max         0.542
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.120

####################################################################### 
# 
# 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_tr101
_database_code_depnum_ccdc_archive 'CCDC 1526911'
_audit_update_record             
;
2017-01-11 deposited with the CCDC.
2017-04-24 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         'C7 H12 N2 O7 P2, H2 O'
_chemical_formula_sum            'C7 H14 N2 O8 P2'
_chemical_formula_weight         316.14

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                   7.836(3)
_cell_length_b                   8.142(3)
_cell_length_c                   10.067(3)
_cell_angle_alpha                68.41(3)
_cell_angle_beta                 84.66(3)
_cell_angle_gamma                79.50(3)
_cell_volume                     587.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8415
_cell_measurement_theta_min      3.37
_cell_measurement_theta_max      36.83

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_F_000             328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.412
_shelx_estimated_absorpt_T_min   0.856
_shelx_estimated_absorpt_T_max   0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.894
_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 KM4-CCD, Sapphire2, large Be window'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            10066
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.378
_diffrn_reflns_theta_max         36.914
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.788
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.788
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4685
_reflns_number_gt                4181
_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)+(0.0858P)²+0.1860P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4685
_refine_ls_number_parameters     182
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1267
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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 0.72399(4) 0.19838(3) 0.50309(3) 0.00908(8) Uani 1 1 d . . . . .
P2 P 0.46451(4) 0.37725(4) 0.25311(3) 0.00924(8) Uani 1 1 d . . . . .
O1 O 0.61509(12) 0.06194(11) 0.59650(10) 0.01438(16) Uani 1 1 d . . . . .
O2 O 0.92014(11) 0.13535(12) 0.52078(9) 0.01365(16) Uani 1 1 d . . . . .
H2 H 0.9508 0.0494 0.4921 0.020 Uiso 0.5 1 calc R U P . .
O3 O 0.68010(13) 0.38088(11) 0.52123(10) 0.01495(17) Uani 1 1 d . . . . .
H3 H 0.6345 0.3676 0.6027 0.022 Uiso 1 1 calc R U . . .
O4 O 0.44345(11) 0.56139(11) 0.25980(9) 0.01184(15) Uani 1 1 d . . . . .
O5 O 0.44824(12) 0.37889(12) 0.10253(10) 0.01454(16) Uani 1 1 d . . . . .
H5 H 0.4916 0.4649 0.0428 0.022 Uiso 0.5 1 calc R U P . .
O6 O 0.32961(11) 0.27051(12) 0.35636(10) 0.01399(16) Uani 1 1 d . . . . .
H6 H 0.3530 0.1628 0.3636 0.021 Uiso 1 1 calc R U . . .
O7 O 0.69496(11) 0.07513(10) 0.29901(9) 0.01187(15) Uani 1 1 d . . . . .
H7 H 0.6121 0.0240 0.3441 0.018 Uiso 1 1 calc R U . . .
N1 N 0.84720(13) 0.50817(12) 0.21583(11) 0.01150(17) Uani 1 1 d . . . . .
N2 N 0.81685(18) 0.79458(15) 0.16345(16) 0.0256(3) Uani 1 1 d D . . . .
H2N H 0.7870 0.9111 0.1220 0.031 Uiso 1 1 d DR U . . .
C1 C 0.68135(13) 0.24603(13) 0.31373(11) 0.00897(17) Uani 1 1 d . . . . .
C2 C 0.82488(13) 0.33619(13) 0.21246(11) 0.00930(17) Uani 1 1 d . . . . .
C3 C 0.98988(14) 0.22436(14) 0.18392(12) 0.01125(18) Uani 1 1 d . . . . .
H3A H 1.0996 0.2729 0.1724 0.014 Uiso 1 1 calc R U . . .
H3B H 1.0011 0.0928 0.2309 0.014 Uiso 1 1 calc R U . . .
C4 C 0.85831(15) 0.31623(15) 0.06855(12) 0.01214(18) Uani 1 1 d . . . . .
H4A H 0.7891 0.2408 0.0450 0.015 Uiso 1 1 calc R U . . .
H4B H 0.8875 0.4210 -0.0136 0.015 Uiso 1 1 calc R U . . .
C21 C 0.76832(16) 0.66912(15) 0.12845(13) 0.0163(2) Uani 1 1 d . . . . .
H21 H 0.6913 0.6885 0.0547 0.020 Uiso 1 1 calc R U . . .
C41 C 0.93088(18) 0.71261(18) 0.27691(18) 0.0223(3) Uani 1 1 d . . . . .
H41 H 0.9849 0.7712 0.3235 0.027 Uiso 1 1 calc R U . . .
C51 C 0.94954(16) 0.53505(16) 0.30743(14) 0.0153(2) Uani 1 1 d . . . . .
H51 H 1.0203 0.4449 0.3790 0.018 Uiso 1 1 calc R U . . .
O1W O 0.3554(5) 0.9288(2) 0.0824(4) 0.0444(6) Uani 0.801(15) 1 d D . P A 1
O10W O 0.3106(12) 0.9179(3) 0.1060(5) 0.0172(19) Uiso 0.199(15) 1 d D . P A 2
H1W H 0.3721 0.8168 0.1221 0.026 Uiso 1 1 d DR U . . .
H2W H 0.3541 0.9771 0.1434 0.026 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 1.5079(11) . ?
P1 O2 1.5342(11) . ?
P1 O3 1.5367(11) . ?
P1 C1 1.8502(13) . ?
P2 O4 1.5039(10) . ?
P2 O5 1.5280(11) . ?
P2 O6 1.5552(11) . ?
P2 C1 1.8581(13) . ?
O2 H2 0.8400 . ?
O3 H3 0.8400 . ?
O5 H5 0.8400 . ?
O6 H6 0.8400 . ?
O7 C1 1.4367(14) . ?
O7 H7 0.8400 . ?
N1 C21 1.3530(16) . ?
N1 C51 1.3752(17) . ?
N1 C2 1.4553(15) . ?
N2 C21 1.3205(19) . ?
N2 C41 1.400(2) . ?
N2 H2N 0.8803 . ?
C1 C2 1.5427(15) . ?
C2 C3 1.5091(16) . ?
C2 C4 1.5103(16) . ?
C3 C4 1.5079(17) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C21 H21 0.9500 . ?
C41 C51 1.3454(18) . ?
C41 H41 0.9500 . ?
C51 H51 0.9500 . ?
O1W H1W 0.8401 . ?
O1W H2W 0.8407 . ?
O10W H1W 0.8412 . ?
O10W H2W 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
O1 P1 O2 113.85(6) . . ?
O1 P1 O3 114.26(6) . . ?
O2 P1 O3 107.96(6) . . ?
O1 P1 C1 108.72(6) . . ?
O2 P1 C1 106.48(6) . . ?
O3 P1 C1 104.93(6) . . ?
O4 P2 O5 113.32(6) . . ?
O4 P2 O6 109.79(6) . . ?
O5 P2 O6 109.88(6) . . ?
O4 P2 C1 111.70(6) . . ?
O5 P2 C1 105.85(6) . . ?
O6 P2 C1 105.99(6) . . ?
P1 O2 H2 109.5 . . ?
P1 O3 H3 109.5 . . ?
P2 O5 H5 109.5 . . ?
P2 O6 H6 109.5 . . ?
C1 O7 H7 109.5 . . ?
C21 N1 C51 108.75(11) . . ?
C21 N1 C2 124.94(11) . . ?
C51 N1 C2 126.31(10) . . ?
C21 N2 C41 108.71(11) . . ?
C21 N2 H2N 127.0 . . ?
C41 N2 H2N 124.3 . . ?
O7 C1 C2 104.77(8) . . ?
O7 C1 P1 106.16(7) . . ?
C2 C1 P1 111.78(8) . . ?
O7 C1 P2 108.66(8) . . ?
C2 C1 P2 110.02(8) . . ?
P1 C1 P2 114.84(6) . . ?
N1 C2 C3 114.69(9) . . ?
N1 C2 C4 115.33(9) . . ?
C3 C2 C4 59.92(8) . . ?
N1 C2 C1 115.63(9) . . ?
C3 C2 C1 120.35(9) . . ?
C4 C2 C1 119.50(9) . . ?
C4 C3 C2 60.08(8) . . ?
C4 C3 H3A 117.8 . . ?
C2 C3 H3A 117.8 . . ?
C4 C3 H3B 117.8 . . ?
C2 C3 H3B 117.8 . . ?
H3A C3 H3B 114.9 . . ?
C3 C4 C2 60.00(8) . . ?
C3 C4 H4A 117.8 . . ?
C2 C4 H4A 117.8 . . ?
C3 C4 H4B 117.8 . . ?
C2 C4 H4B 117.8 . . ?
H4A C4 H4B 114.9 . . ?
N2 C21 N1 108.17(13) . . ?
N2 C21 H21 125.9 . . ?
N1 C21 H21 125.9 . . ?
C51 C41 N2 107.02(12) . . ?
C51 C41 H41 126.5 . . ?
N2 C41 H41 126.5 . . ?
C41 C51 N1 107.34(12) . . ?
C41 C51 H51 126.3 . . ?
N1 C51 H51 126.3 . . ?
H1W O1W H2W 110.3 . . ?
H1W O10W H2W 110.2 . . ?

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 -48.57(8) . . . . ?
O2 P1 C1 O7 74.48(8) . . . . ?
O3 P1 C1 O7 -171.21(7) . . . . ?
O1 P1 C1 C2 -162.25(7) . . . . ?
O2 P1 C1 C2 -39.20(8) . . . . ?
O3 P1 C1 C2 75.11(8) . . . . ?
O1 P1 C1 P2 71.51(7) . . . . ?
O2 P1 C1 P2 -165.44(6) . . . . ?
O3 P1 C1 P2 -51.13(7) . . . . ?
O4 P2 C1 O7 -177.67(6) . . . . ?
O5 P2 C1 O7 -53.90(8) . . . . ?
O6 P2 C1 O7 62.79(8) . . . . ?
O4 P2 C1 C2 -63.50(9) . . . . ?
O5 P2 C1 C2 60.26(9) . . . . ?
O6 P2 C1 C2 176.95(7) . . . . ?
O4 P2 C1 P1 63.64(7) . . . . ?
O5 P2 C1 P1 -172.59(6) . . . . ?
O6 P2 C1 P1 -55.90(7) . . . . ?
C21 N1 C2 C3 120.54(12) . . . . ?
C51 N1 C2 C3 -59.90(15) . . . . ?
C21 N1 C2 C4 53.66(14) . . . . ?
C51 N1 C2 C4 -126.79(12) . . . . ?
C21 N1 C2 C1 -92.58(13) . . . . ?
C51 N1 C2 C1 86.97(14) . . . . ?
O7 C1 C2 N1 -175.49(9) . . . . ?
P1 C1 C2 N1 -60.96(11) . . . . ?
P2 C1 C2 N1 67.88(11) . . . . ?
O7 C1 C2 C3 -30.61(13) . . . . ?
P1 C1 C2 C3 83.92(11) . . . . ?
P2 C1 C2 C3 -147.24(9) . . . . ?
O7 C1 C2 C4 39.75(12) . . . . ?
P1 C1 C2 C4 154.28(8) . . . . ?
P2 C1 C2 C4 -76.88(11) . . . . ?
N1 C2 C3 C4 -106.14(11) . . . . ?
C1 C2 C3 C4 108.68(12) . . . . ?
N1 C2 C4 C3 105.07(11) . . . . ?
C1 C2 C4 C3 -110.07(11) . . . . ?
C41 N2 C21 N1 0.06(14) . . . . ?
C51 N1 C21 N2 -0.55(13) . . . . ?
C2 N1 C21 N2 179.07(10) . . . . ?
C21 N2 C41 C51 0.45(15) . . . . ?
N2 C41 C51 N1 -0.78(14) . . . . ?
C21 N1 C51 C41 0.84(14) . . . . ?
C2 N1 C51 C41 -178.78(10) . . . . ?

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 O2 0.84 1.69 2.485(2) 156.2 2_756
O3 H3 O4 0.84 1.71 2.4934(15) 154.0 2_666
O5 H5 O5 0.84 1.64 2.467(2) 165.7 2_665
O6 H6 O1 0.84 1.70 2.5309(16) 171.1 2_656
O7 H7 O1 0.84 1.99 2.8113(16) 165.1 2_656
N2 H2N O1W 0.88 2.26 2.904(3) 130.0 2_675
N2 H2N O10W 0.88 2.32 2.969(3) 130.7 2_675
C3 H3B O2 0.99 2.56 3.338(2) 135.9 2_756
C21 H21 O5 0.95 2.28 3.176(2) 157.6 2_665
C41 H41 O2 0.95 2.21 3.1413(19) 165.9 2_766
O1W H1W O4 0.84 2.04 2.856(2) 164.1 .
O10W H1W O4 0.84 2.04 2.792(3) 148.7 .
O1W H2W O1 0.84 2.55 3.291(3) 148.0 2_666
O10W H2W O1 0.84 2.55 3.171(3) 131.7 2_666

_refine_diff_density_max         0.780
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.117

