# 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_do3apida
_database_code_depnum_ccdc_archive 'CCDC 1482407'
_audit_update_record             
;
2017-05-10 deposited with the CCDC.
2017-07-17 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         'C20 H36 N5 O12 P, 4(H2 O)'
_chemical_formula_sum            'C20 H44 N5 O16 P'
_chemical_formula_weight         641.57
_chemical_compound_source        'synthesized by the authors'

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                   9.5462(4)
_cell_length_b                   10.7017(7)
_cell_length_c                   16.0510(10)
_cell_angle_alpha                100.877(2)
_cell_angle_beta                 95.356(4)
_cell_angle_gamma                112.760(3)
_cell_volume                     1459.66(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5252
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      26.02

_exptl_crystal_description       prisma
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             684
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.176
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_reflns_number            10546
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.314
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5679
_reflns_number_gt                3638
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1363P)²+1.1832P] 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         5679
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.2370
_refine_ls_wR_factor_gt          0.2071
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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
N1 N 0.6761(4) 0.3667(3) 0.14988(19) 0.0419(8) Uani 1 1 d . . . . .
C2 C 0.7887(5) 0.3227(5) 0.1926(3) 0.0544(11) Uani 1 1 d . . . . .
H21 H 0.8837 0.4043 0.2190 0.065 Uiso 1 1 calc R U . . .
H22 H 0.8128 0.2610 0.1496 0.065 Uiso 1 1 calc R U . . .
C3 C 0.7249(6) 0.2486(5) 0.2604(3) 0.0594(12) Uani 1 1 d . . . . .
H31 H 0.6270 0.1701 0.2343 0.071 Uiso 1 1 calc R U . . .
H32 H 0.7955 0.2119 0.2820 0.071 Uiso 1 1 calc R U . . .
N4 N 0.7010(4) 0.3417(3) 0.3343(2) 0.0501(9) Uani 1 1 d . . . . .
H41 H 0.6395 0.3862 0.3141 0.060 Uiso 1 1 d R U . . .
C5 C 0.6026(6) 0.2614(5) 0.3907(3) 0.0625(13) Uani 1 1 d . . . . .
H51 H 0.6067 0.3263 0.4429 0.075 Uiso 1 1 calc R U . . .
H52 H 0.6445 0.1984 0.4071 0.075 Uiso 1 1 calc R U . . .
C6 C 0.4345(6) 0.1772(5) 0.3455(3) 0.0643(13) Uani 1 1 d . . . . .
H61 H 0.4275 0.0990 0.3008 0.077 Uiso 1 1 calc R U . . .
H62 H 0.3726 0.1401 0.3869 0.077 Uiso 1 1 calc R U . . .
N7 N 0.3722(4) 0.2634(4) 0.3066(2) 0.0502(9) Uani 1 1 d . . . . .
C8 C 0.2309(5) 0.1718(4) 0.2418(3) 0.0531(11) Uani 1 1 d . . . . .
H71 H 0.1602 0.2168 0.2406 0.064 Uiso 1 1 calc R U . . .
H72 H 0.1800 0.0846 0.2582 0.064 Uiso 1 1 calc R U . . .
C9 C 0.2688(5) 0.1412(4) 0.1524(3) 0.0496(10) Uani 1 1 d . . . . .
H91 H 0.3453 0.1025 0.1543 0.060 Uiso 1 1 calc R U . . .
H92 H 0.1764 0.0725 0.1127 0.060 Uiso 1 1 calc R U . . .
N10 N 0.3302(3) 0.2722(3) 0.12053(19) 0.0413(8) Uani 1 1 d . . . . .
H101 H 0.3945 0.3443 0.1650 0.050 Uiso 1 1 d R U . . .
C11 C 0.4210(4) 0.2596(5) 0.0495(2) 0.0464(10) Uani 1 1 d . . . . .
H111 H 0.4467 0.3414 0.0261 0.056 Uiso 1 1 calc R U . . .
H112 H 0.3566 0.1784 0.0033 0.056 Uiso 1 1 calc R U . . .
C12 C 0.5687(4) 0.2462(5) 0.0800(2) 0.0466(10) Uani 1 1 d . . . . .
H121 H 0.5426 0.1616 0.1003 0.056 Uiso 1 1 calc R U . . .
H122 H 0.6206 0.2373 0.0315 0.056 Uiso 1 1 calc R U . . .
C20 C 0.7570(4) 0.4855(4) 0.1131(2) 0.0448(10) Uani 1 1 d . . . . .
H201 H 0.6817 0.4930 0.0717 0.054 Uiso 1 1 calc R U . . .
H202 H 0.8300 0.4641 0.0814 0.054 Uiso 1 1 calc R U . . .
P1 P 0.86047(11) 0.65435(11) 0.18872(6) 0.0412(3) Uani 1 1 d . . . . .
O11 O 0.9303(3) 0.7598(3) 0.13781(18) 0.0504(7) Uani 1 1 d . . . . .
O12 O 0.9636(3) 0.6462(3) 0.26200(17) 0.0471(7) Uani 1 1 d . . . . .
C21 C 0.7048(4) 0.6898(4) 0.2321(2) 0.0369(8) Uani 1 1 d . . . . .
H211 H 0.6191 0.6631 0.1852 0.044 Uiso 1 1 calc R U . . .
H212 H 0.6684 0.6325 0.2724 0.044 Uiso 1 1 calc R U . . .
N22 N 0.7538(3) 0.8395(3) 0.27699(19) 0.0362(7) Uani 1 1 d . . . . .
H221 H 0.7453 0.8809 0.2313 0.043 Uiso 1 1 d R U . . .
C23 C 0.8781(5) 0.8901(4) 0.3558(3) 0.0518(11) Uani 1 1 d . . . . .
H231 H 0.9549 0.8538 0.3443 0.062 Uiso 1 1 calc R U . . .
H232 H 0.8336 0.8570 0.4036 0.062 Uiso 1 1 calc R U . . .
C24 C 0.9530(5) 1.0477(4) 0.3789(3) 0.0528(11) Uani 1 1 d . . . . .
O241 O 1.0619(4) 1.1050(3) 0.4435(2) 0.0735(10) Uani 1 1 d . . . . .
H241 H 1.0615 1.2208 0.4615 0.088 Uiso 1 1 d R U . . .
O242 O 0.9254(4) 1.1092(3) 0.3285(2) 0.0657(9) Uani 1 1 d . . . . .
C25 C 0.6134(5) 0.8610(5) 0.2961(3) 0.0510(10) Uani 1 1 d . . . . .
H251 H 0.6429 0.9405 0.3450 0.061 Uiso 1 1 calc R U . . .
H252 H 0.5421 0.7792 0.3113 0.061 Uiso 1 1 calc R U . . .
C26 C 0.5337(5) 0.8864(4) 0.2183(3) 0.0461(10) Uani 1 1 d . . . . .
O261 O 0.6088(3) 0.9157(3) 0.1607(2) 0.0547(8) Uani 1 1 d . . . . .
O262 O 0.4066(4) 0.8857(3) 0.2230(2) 0.0626(9) Uani 1 1 d . . . . .
C30 C 0.8479(5) 0.4501(5) 0.3890(3) 0.0592(12) Uani 1 1 d . . . . .
H301 H 0.9262 0.4778 0.3535 0.071 Uiso 1 1 calc R U . . .
H302 H 0.8841 0.4121 0.4324 0.071 Uiso 1 1 calc R U . . .
C31 C 0.8230(6) 0.5760(4) 0.4324(3) 0.0519(11) Uani 1 1 d . . . . .
O311 O 0.9451(3) 0.6666(3) 0.48864(18) 0.0606(9) Uani 1 1 d . . . . .
O312 O 0.7035(4) 0.5873(3) 0.41377(17) 0.0513(7) Uani 1 1 d . . . . .
C40 C 0.3430(5) 0.3604(5) 0.3709(3) 0.0524(11) Uani 1 1 d . . . . .
H401 H 0.4256 0.3978 0.4209 0.063 Uiso 1 1 calc R U . . .
H402 H 0.2472 0.3107 0.3894 0.063 Uiso 1 1 calc R U . . .
C41 C 0.3323(4) 0.4787(4) 0.3377(2) 0.0441(10) Uani 1 1 d . . . . .
O411 O 0.2955(3) 0.5615(3) 0.39386(17) 0.0523(7) Uani 1 1 d . . . . .
H411 H 0.2801 0.6185 0.3828 0.063 Uiso 1 1 d R U . . .
O412 O 0.3553(3) 0.4961(3) 0.26650(16) 0.0463(7) Uani 1 1 d . . . . .
C50 C 0.2006(4) 0.3086(4) 0.0902(3) 0.0462(10) Uani 1 1 d . . . . .
H501 H 0.1253 0.2867 0.1278 0.055 Uiso 1 1 calc R U . . .
H502 H 0.1498 0.2512 0.0325 0.055 Uiso 1 1 calc R U . . .
C51 C 0.2536(4) 0.4603(4) 0.0889(2) 0.0408(9) Uani 1 1 d . . . . .
O511 O 0.1355(3) 0.4931(3) 0.08491(18) 0.0501(7) Uani 1 1 d . . . . .
H511 H 0.1410 0.5626 0.0795 0.060 Uiso 1 1 d R U . . .
O512 O 0.3867(3) 0.5368(3) 0.08953(16) 0.0435(7) Uani 1 1 d . . . . .
O1W O 0.1858(3) 0.7449(3) 0.08075(18) 0.0515(7) Uani 1 1 d . . . . .
H11W H 0.0998 0.7615 0.1013 0.062 Uiso 1 1 d R U . . .
H12W H 0.2620 0.7984 0.1289 0.062 Uiso 1 1 d R U . . .
O2W O 0.2526(3) 0.7615(3) 0.34058(18) 0.0521(7) Uani 1 1 d . . . . .
H21W H 0.1508 0.7226 0.3155 0.062 Uiso 1 1 d R U . . .
H22W H 0.3069 0.8043 0.3048 0.062 Uiso 1 1 d R U . . .
O3W O 0.8975(4) 0.9958(4) 0.1007(3) 0.0864(12) Uani 1 1 d . . . . .
H31W H 0.8136 0.9952 0.1208 0.104 Uiso 1 1 d R U . . .
H32W H 0.9006 0.9157 0.1102 0.104 Uiso 1 1 d R U . . .
O4WA O 0.7304(6) 1.0406(6) 0.5094(3) 0.0433(12) Uani 0.5 1 d . . P A 1
H41W H 0.7510 1.1173 0.5559 0.052 Uiso 0.5 1 d R U P A 1
H42W H 0.7882 1.0007 0.5221 0.052 Uiso 0.5 1 d R U P A 1
O4WB O 0.5960(8) 1.0287(7) 0.4968(4) 0.0628(16) Uani 0.5 1 d . . P B 2
H43W H 0.5000 1.0000 0.5000 0.075 Uiso 1 2 d R U P B 2
H44W H 0.6289 1.0558 0.5568 0.075 Uiso 0.5 1 d R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C20 1.473(5) . ?
N1 C12 1.480(5) . ?
N1 C2 1.491(5) . ?
C2 C3 1.503(7) . ?
C2 H21 0.9700 . ?
C2 H22 0.9700 . ?
C3 N4 1.494(6) . ?
C3 H31 0.9700 . ?
C3 H32 0.9700 . ?
N4 C30 1.486(5) . ?
N4 C5 1.505(6) . ?
N4 H41 0.9567 . ?
C5 C6 1.527(7) . ?
C5 H51 0.9700 . ?
C5 H52 0.9700 . ?
C6 N7 1.471(6) . ?
C6 H61 0.9700 . ?
C6 H62 0.9700 . ?
N7 C40 1.447(5) . ?
N7 C8 1.481(5) . ?
C8 C9 1.520(6) . ?
C8 H71 0.9700 . ?
C8 H72 0.9700 . ?
C9 N10 1.503(5) . ?
C9 H91 0.9700 . ?
C9 H92 0.9700 . ?
N10 C50 1.500(5) . ?
N10 C11 1.512(5) . ?
N10 H101 0.9082 . ?
C11 C12 1.518(5) . ?
C11 H111 0.9700 . ?
C11 H112 0.9700 . ?
C12 H121 0.9700 . ?
C12 H122 0.9700 . ?
C20 P1 1.812(4) . ?
C20 H201 0.9700 . ?
C20 H202 0.9700 . ?
P1 O12 1.500(3) . ?
P1 O11 1.501(3) . ?
P1 C21 1.835(4) . ?
C21 N22 1.492(5) . ?
C21 H211 0.9700 . ?
C21 H212 0.9700 . ?
N22 C25 1.494(5) . ?
N22 C23 1.506(5) . ?
N22 H221 0.9376 . ?
C23 C24 1.508(6) . ?
C23 H231 0.9700 . ?
C23 H232 0.9700 . ?
C24 O242 1.205(5) . ?
C24 O241 1.264(5) . ?
O241 H241 1.2194 . ?
C25 C26 1.523(6) . ?
C25 H251 0.9700 . ?
C25 H252 0.9700 . ?
C26 O262 1.219(5) . ?
C26 O261 1.236(5) . ?
C30 C31 1.511(7) . ?
C30 H301 0.9700 . ?
C30 H302 0.9700 . ?
C31 O312 1.209(5) . ?
C31 O311 1.309(5) . ?
C40 C41 1.498(6) . ?
C40 H401 0.9700 . ?
C40 H402 0.9700 . ?
C41 O412 1.219(4) . ?
C41 O411 1.310(5) . ?
O411 H411 0.7285 . ?
C50 C51 1.507(6) . ?
C50 H501 0.9700 . ?
C50 H502 0.9700 . ?
C51 O512 1.214(4) . ?
C51 O511 1.304(5) . ?
O511 H511 0.7472 . ?
O1W H11W 0.9780 . ?
O1W H12W 0.9280 . ?
O2W H21W 0.9119 . ?
O2W H22W 0.8822 . ?
O3W H31W 0.8891 . ?
O3W H32W 0.9089 . ?
O4WA H41W 0.9419 . ?
O4WA H42W 0.8501 . ?
O4WB H43W 0.8566 . ?
O4WB H44W 0.9375 . ?

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
C20 N1 C12 109.5(3) . . ?
C20 N1 C2 110.5(3) . . ?
C12 N1 C2 107.7(3) . . ?
N1 C2 C3 111.3(4) . . ?
N1 C2 H21 109.4 . . ?
C3 C2 H21 109.4 . . ?
N1 C2 H22 109.4 . . ?
C3 C2 H22 109.4 . . ?
H21 C2 H22 108.0 . . ?
N4 C3 C2 112.7(4) . . ?
N4 C3 H31 109.0 . . ?
C2 C3 H31 109.0 . . ?
N4 C3 H32 109.0 . . ?
C2 C3 H32 109.0 . . ?
H31 C3 H32 107.8 . . ?
C30 N4 C3 113.3(4) . . ?
C30 N4 C5 109.1(3) . . ?
C3 N4 C5 112.5(3) . . ?
C30 N4 H41 109.2 . . ?
C3 N4 H41 110.7 . . ?
C5 N4 H41 101.5 . . ?
N4 C5 C6 112.3(3) . . ?
N4 C5 H51 109.1 . . ?
C6 C5 H51 109.1 . . ?
N4 C5 H52 109.1 . . ?
C6 C5 H52 109.1 . . ?
H51 C5 H52 107.9 . . ?
N7 C6 C5 111.6(4) . . ?
N7 C6 H61 109.3 . . ?
C5 C6 H61 109.3 . . ?
N7 C6 H62 109.3 . . ?
C5 C6 H62 109.3 . . ?
H61 C6 H62 108.0 . . ?
C40 N7 C6 112.1(3) . . ?
C40 N7 C8 111.4(4) . . ?
C6 N7 C8 109.7(3) . . ?
N7 C8 C9 111.3(3) . . ?
N7 C8 H71 109.4 . . ?
C9 C8 H71 109.4 . . ?
N7 C8 H72 109.4 . . ?
C9 C8 H72 109.4 . . ?
H71 C8 H72 108.0 . . ?
N10 C9 C8 110.7(3) . . ?
N10 C9 H91 109.5 . . ?
C8 C9 H91 109.5 . . ?
N10 C9 H92 109.5 . . ?
C8 C9 H92 109.5 . . ?
H91 C9 H92 108.1 . . ?
C50 N10 C9 110.4(3) . . ?
C50 N10 C11 110.3(3) . . ?
C9 N10 C11 112.1(3) . . ?
C50 N10 H101 107.1 . . ?
C9 N10 H101 109.0 . . ?
C11 N10 H101 107.9 . . ?
N10 C11 C12 113.0(3) . . ?
N10 C11 H111 109.0 . . ?
C12 C11 H111 109.0 . . ?
N10 C11 H112 109.0 . . ?
C12 C11 H112 109.0 . . ?
H111 C11 H112 107.8 . . ?
N1 C12 C11 113.1(3) . . ?
N1 C12 H121 109.0 . . ?
C11 C12 H121 109.0 . . ?
N1 C12 H122 109.0 . . ?
C11 C12 H122 109.0 . . ?
H121 C12 H122 107.8 . . ?
N1 C20 P1 116.6(2) . . ?
N1 C20 H201 108.2 . . ?
P1 C20 H201 108.2 . . ?
N1 C20 H202 108.2 . . ?
P1 C20 H202 108.2 . . ?
H201 C20 H202 107.3 . . ?
O12 P1 O11 118.46(16) . . ?
O12 P1 C20 111.29(18) . . ?
O11 P1 C20 107.72(17) . . ?
O12 P1 C21 107.89(16) . . ?
O11 P1 C21 107.47(17) . . ?
C20 P1 C21 102.83(17) . . ?
N22 C21 P1 113.1(2) . . ?
N22 C21 H211 109.0 . . ?
P1 C21 H211 109.0 . . ?
N22 C21 H212 109.0 . . ?
P1 C21 H212 109.0 . . ?
H211 C21 H212 107.8 . . ?
C21 N22 C25 108.4(3) . . ?
C21 N22 C23 113.9(3) . . ?
C25 N22 C23 112.6(3) . . ?
C21 N22 H221 102.9 . . ?
C25 N22 H221 84.2 . . ?
C23 N22 H221 130.1 . . ?
N22 C23 C24 109.0(3) . . ?
N22 C23 H231 109.9 . . ?
C24 C23 H231 109.9 . . ?
N22 C23 H232 109.9 . . ?
C24 C23 H232 109.9 . . ?
H231 C23 H232 108.3 . . ?
O242 C24 O241 123.6(4) . . ?
O242 C24 C23 119.2(4) . . ?
O241 C24 C23 116.0(4) . . ?
C24 O241 H241 99.5 . . ?
N22 C25 C26 110.9(3) . . ?
N22 C25 H251 109.5 . . ?
C26 C25 H251 109.5 . . ?
N22 C25 H252 109.5 . . ?
C26 C25 H252 109.5 . . ?
H251 C25 H252 108.0 . . ?
O262 C26 O261 127.0(4) . . ?
O262 C26 C25 115.9(4) . . ?
O261 C26 C25 116.8(4) . . ?
N4 C30 C31 110.0(4) . . ?
N4 C30 H301 109.7 . . ?
C31 C30 H301 109.7 . . ?
N4 C30 H302 109.7 . . ?
C31 C30 H302 109.7 . . ?
H301 C30 H302 108.2 . . ?
O312 C31 O311 126.7(4) . . ?
O312 C31 C30 121.7(4) . . ?
O311 C31 C30 111.6(4) . . ?
N7 C40 C41 112.4(3) . . ?
N7 C40 H401 109.1 . . ?
C41 C40 H401 109.1 . . ?
N7 C40 H402 109.1 . . ?
C41 C40 H402 109.1 . . ?
H401 C40 H402 107.9 . . ?
O412 C41 O411 123.8(4) . . ?
O412 C41 C40 123.7(4) . . ?
O411 C41 C40 112.4(3) . . ?
C41 O411 H411 121.4 . . ?
N10 C50 C51 113.1(3) . . ?
N10 C50 H501 109.0 . . ?
C51 C50 H501 109.0 . . ?
N10 C50 H502 109.0 . . ?
C51 C50 H502 109.0 . . ?
H501 C50 H502 107.8 . . ?
O512 C51 O511 126.6(4) . . ?
O512 C51 C50 123.7(4) . . ?
O511 C51 C50 109.7(3) . . ?
C51 O511 H511 123.0 . . ?
H11W O1W H12W 98.4 . . ?
H21W O2W H22W 108.1 . . ?
H31W O3W H32W 102.3 . . ?
H41W O4WA H42W 107.9 . . ?
H43W O4WB H44W 93.8 . . ?

_refine_diff_density_max         1.329
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.079

####################################################################### 
# 
# 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_do3aidpcu
_database_code_depnum_ccdc_archive 'CCDC 1482406'
_audit_update_record             
;
2017-05-10 deposited with the CCDC.
2017-07-17 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         'C20 H39 Cu4 N5 O17 P, 7.5 (H2 O), Cl'
_chemical_formula_sum            'C20 H54 Cl Cu4 N5 O24.50 P'
_chemical_formula_weight         1077.26
_chemical_compound_source        'synthesized by the authors'

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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                   12.0847(5)
_cell_length_b                   12.4493(5)
_cell_length_c                   12.9847(5)
_cell_angle_alpha                85.606(2)
_cell_angle_beta                 78.603(2)
_cell_angle_gamma                86.931(2)
_cell_volume                     1907.87(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9660
_cell_measurement_theta_min      2.425
_cell_measurement_theta_max      27.49

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_F_000             1106
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.209
_exptl_absorpt_coefficient_mu    2.407
_shelx_estimated_absorpt_T_min   0.535
_shelx_estimated_absorpt_T_max   0.633
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            86722
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.216
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8790
_reflns_number_gt                7764
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0327P)²+8.9320P] 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         8790
_refine_ls_number_parameters     523
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1042
_refine_ls_wR_factor_gt          0.0977
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.125
_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
Cu1 Cu 0.53605(3) 0.74970(3) 0.73755(3) 0.01132(9) Uani 1 1 d . . . . .
N1 N 0.6684(2) 0.6982(2) 0.8107(2) 0.0125(5) Uani 1 1 d . . . . .
C2 C 0.6235(3) 0.6662(3) 0.9245(3) 0.0172(7) Uani 1 1 d . . . . .
H21 H 0.6767 0.6870 0.9679 0.021 Uiso 1 1 calc R U . . .
H22 H 0.6168 0.5870 0.9340 0.021 Uiso 1 1 calc R U . . .
C3 C 0.5097(3) 0.7207(3) 0.9600(3) 0.0169(7) Uani 1 1 d . . . . .
H31 H 0.4750 0.6905 1.0311 0.020 Uiso 1 1 calc R U . . .
H32 H 0.5183 0.7989 0.9637 0.020 Uiso 1 1 calc R U . . .
N4 N 0.4361(3) 0.7034(3) 0.8842(2) 0.0187(6) Uani 1 1 d . . . . .
C5 C 0.3340(3) 0.7760(4) 0.8993(3) 0.0272(9) Uani 1 1 d . . . . .
H51 H 0.3112 0.7908 0.9745 0.033 Uiso 1 1 calc R U . . .
H52 H 0.2710 0.7408 0.8784 0.033 Uiso 1 1 calc R U . . .
C6 C 0.3577(3) 0.8799(3) 0.8338(3) 0.0248(8) Uani 1 1 d . . . . .
H61 H 0.2868 0.9245 0.8377 0.030 Uiso 1 1 calc R U . . .
H62 H 0.4119 0.9205 0.8622 0.030 Uiso 1 1 calc R U . . .
N7 N 0.4056(3) 0.8589(3) 0.7212(2) 0.0183(6) Uani 1 1 d . . . . .
C8 C 0.4568(3) 0.9598(3) 0.6653(3) 0.0230(8) Uani 1 1 d . . . . .
H81 H 0.4101 1.0234 0.6917 0.028 Uiso 1 1 calc R U . . .
H82 H 0.4580 0.9589 0.5890 0.028 Uiso 1 1 calc R U . . .
C9 C 0.5761(3) 0.9684(3) 0.6833(3) 0.0204(7) Uani 1 1 d . . . . .
H91 H 0.6121 1.0308 0.6400 0.025 Uiso 1 1 calc R U . . .
H92 H 0.5745 0.9796 0.7583 0.025 Uiso 1 1 calc R U . . .
N10 N 0.6419(3) 0.8671(2) 0.6536(2) 0.0145(5) Uani 1 1 d . . . . .
C11 C 0.7486(3) 0.8547(3) 0.6955(3) 0.0181(7) Uani 1 1 d . . . . .
H111 H 0.7804 0.9263 0.6954 0.022 Uiso 1 1 calc R U . . .
H112 H 0.8046 0.8097 0.6495 0.022 Uiso 1 1 calc R U . . .
C12 C 0.7264(3) 0.8027(3) 0.8060(3) 0.0166(7) Uani 1 1 d . . . . .
H121 H 0.7989 0.7891 0.8303 0.020 Uiso 1 1 calc R U . . .
H122 H 0.6785 0.8523 0.8538 0.020 Uiso 1 1 calc R U . . .
C20 C 0.7532(3) 0.6149(3) 0.7640(3) 0.0151(6) Uani 1 1 d . . . . .
H201 H 0.8139 0.6099 0.8056 0.018 Uiso 1 1 calc R U . . .
H202 H 0.7873 0.6440 0.6924 0.018 Uiso 1 1 calc R U . . .
P1 P 0.71466(7) 0.47588(7) 0.75192(6) 0.01260(16) Uani 1 1 d . . . . .
O11 O 0.6766(2) 0.46314(19) 0.6497(2) 0.0178(5) Uani 1 1 d . . . . .
O12 O 0.6394(3) 0.4278(2) 0.8478(2) 0.0362(8) Uani 1 1 d . . . . .
C21 C 0.8602(3) 0.4229(3) 0.7309(3) 0.0249(8) Uani 1 1 d . . . . .
H211 H 0.9068 0.4738 0.6802 0.030 Uiso 1 1 calc R U . . .
H212 H 0.8865 0.4227 0.7984 0.030 Uiso 1 1 calc R U . . .
N22 N 0.8837(2) 0.3133(2) 0.6917(2) 0.0152(6) Uani 1 1 d . . . . .
C23 C 0.8511(3) 0.2272(3) 0.7759(3) 0.0216(7) Uani 1 1 d . . . . .
H231 H 0.8468 0.2566 0.8454 0.026 Uiso 1 1 calc R U . . .
H232 H 0.9099 0.1682 0.7685 0.026 Uiso 1 1 calc R U . . .
C24 C 0.7383(3) 0.1823(3) 0.7713(3) 0.0218(7) Uani 1 1 d . . . . .
O241 O 0.6953(2) 0.2099(2) 0.6900(2) 0.0186(5) Uani 1 1 d . . . . .
O242 O 0.6951(3) 0.1189(3) 0.8446(3) 0.0412(8) Uani 1 1 d . . . . .
C25 C 1.0039(3) 0.3051(3) 0.6378(3) 0.0200(7) Uani 1 1 d . . . . .
H251 H 1.0302 0.2284 0.6362 0.024 Uiso 1 1 calc R U . . .
H252 H 1.0512 0.3428 0.6766 0.024 Uiso 1 1 calc R U . . .
C26 C 1.0154(3) 0.3558(3) 0.5257(3) 0.0210(7) Uani 1 1 d . . . . .
O261 O 0.9266(2) 0.3540(2) 0.4848(2) 0.0215(5) Uani 1 1 d . . . . .
O262 O 1.1059(2) 0.3912(2) 0.4797(3) 0.0303(6) Uani 1 1 d . . . . .
C30 C 0.6700(3) 0.8639(3) 0.5375(3) 0.0188(7) Uani 1 1 d . . . . .
H301 H 0.7466 0.8911 0.5115 0.023 Uiso 1 1 calc R U . . .
H302 H 0.6161 0.9125 0.5063 0.023 Uiso 1 1 calc R U . . .
C31 C 0.6660(3) 0.7525(3) 0.5014(3) 0.0134(6) Uani 1 1 d . . . . .
O311 O 0.64138(19) 0.67644(18) 0.57140(18) 0.0126(4) Uani 1 1 d . . . . .
O312 O 0.6855(2) 0.7461(2) 0.40338(18) 0.0178(5) Uani 1 1 d . . . . .
C40 C 0.3121(3) 0.8251(3) 0.6728(3) 0.0220(8) Uani 1 1 d . . . . .
H401 H 0.2601 0.8884 0.6666 0.026 Uiso 1 1 calc R U . . .
H402 H 0.2694 0.7704 0.7220 0.026 Uiso 1 1 calc R U . . .
C41 C 0.3450(3) 0.7789(3) 0.5651(3) 0.0169(7) Uani 1 1 d . . . . .
O411 O 0.4361(2) 0.7944(2) 0.5060(2) 0.0211(5) Uani 1 1 d . . . . .
O412 O 0.2649(2) 0.7244(2) 0.5460(2) 0.0218(5) Uani 1 1 d . . . . .
C50 C 0.4060(4) 0.5893(3) 0.8887(3) 0.0258(9) Uani 1 1 d . . . . .
H501 H 0.3301 0.5804 0.9334 0.031 Uiso 1 1 calc R U . . .
H502 H 0.4607 0.5436 0.9217 0.031 Uiso 1 1 calc R U . . .
C51 C 0.4058(3) 0.5522(3) 0.7806(3) 0.0170(7) Uani 1 1 d . . . . .
O511 O 0.4508(2) 0.6083(2) 0.70055(18) 0.0162(5) Uani 1 1 d . . . . .
O512 O 0.3624(2) 0.4634(2) 0.7825(2) 0.0271(6) Uani 1 1 d . . . . .
Cu2 Cu 0.79830(3) 0.28692(3) 0.57790(3) 0.01504(10) Uani 1 1 d . . . . .
O1C O 0.8852(3) 0.1027(3) 0.5479(3) 0.0521(10) Uani 1 1 d . . . . .
H11C H 0.9254 0.0595 0.5847 0.063 Uiso 1 1 d R U . . .
H12C H 0.8999 0.0703 0.4899 0.063 Uiso 1 1 d R U . . .
Cu3 Cu 0.58189(3) 0.53435(3) 0.55994(3) 0.01034(9) Uani 1 1 d . . . . .
O2C O 0.48404(19) 0.41145(19) 0.56273(17) 0.0120(4) Uani 1 1 d . . . . .
H21C H 0.5169 0.3425 0.5505 0.014 Uiso 1 1 d R U . . .
O3C O 0.7497(2) 0.5072(2) 0.4171(2) 0.0212(5) Uani 1 1 d . . . . .
H31C H 0.8022 0.5305 0.4462 0.025 Uiso 1 1 d R U . . .
H32C H 0.7654 0.4440 0.4132 0.025 Uiso 1 1 d R U . . .
Cu4 Cu 0.65388(3) 0.62871(3) 0.32499(3) 0.01290(9) Uani 1 1 d . . . . .
O4C O 0.5241(3) 0.7343(3) 0.2351(2) 0.0371(8) Uani 1 1 d . . . . .
H41C H 0.4628 0.7652 0.2707 0.044 Uiso 1 1 d R U . . .
H42C H 0.5015 0.6773 0.2057 0.044 Uiso 1 1 d R U . . .
O5C O 0.7921(2) 0.6705(2) 0.2194(2) 0.0266(6) Uani 1 1 d . . . . .
H51C H 0.8015 0.6444 0.1623 0.032 Uiso 1 1 d R U . . .
H52C H 0.8200 0.7356 0.2001 0.032 Uiso 1 1 d R U . . .
Cl1A Cl 1.0504(4) -0.0099(3) 0.6715(4) 0.0463(11) Uani 0.5 1 d . . P . .
Cl1B Cl 1.0299(5) -0.0328(5) 0.7177(5) 0.0447(13) Uani 0.35 1 d . . P . .
Cl1C Cl 1.1027(12) 0.0238(11) 0.6371(9) 0.051(3) Uani 0.15 1 d . . P . .
O1W O 0.8370(6) -0.0034(5) 0.9442(6) 0.101(2) Uani 1 1 d . . . . .
H11W H 0.8829 -0.0306 0.8900 0.122 Uiso 1 1 d R U . . .
H12W H 0.7872 0.0313 0.9125 0.122 Uiso 1 1 d R U . . .
O2W O 0.3540(4) 0.1252(3) 0.9160(4) 0.0645(13) Uani 1 1 d . . . . .
H21W H 0.2832 0.1496 0.9082 0.077 Uiso 1 1 d R U . . .
H22W H 0.3847 0.1682 0.8734 0.077 Uiso 1 1 d R U . . .
O3W O 0.8570(4) 0.8742(3) 0.1630(4) 0.0649(12) Uani 1 1 d . . . . .
H31W H 0.8745 0.9107 0.2105 0.078 Uiso 1 1 d R U . . .
H32W H 0.9152 0.8792 0.1054 0.078 Uiso 1 1 d R U . . .
O4W O 1.0351(5) 0.8603(5) -0.0185(5) 0.0939(18) Uani 1 1 d . . . . .
H41W H 1.0335 0.8867 -0.0849 0.113 Uiso 1 1 d R U . . .
H42W H 1.0783 0.9123 0.0076 0.113 Uiso 1 1 d R U . . .
O5W O 0.9814(3) 0.2792(4) 0.2784(3) 0.0648(13) Uani 1 1 d . . . . .
H51W H 0.9647 0.3021 0.3398 0.078 Uiso 1 1 d R U . . .
H52W H 0.9497 0.2117 0.2978 0.078 Uiso 1 1 d R U . . .
O6W O 0.8583(3) 0.5646(4) 0.0338(3) 0.0545(10) Uani 1 1 d . . . . .
H61W H 0.9176 0.5968 -0.0013 0.065 Uiso 1 1 d R U . . .
H62W H 0.8778 0.5007 0.0636 0.065 Uiso 1 1 d R U . . .
O7W O 0.9373(4) 0.3470(4) 0.0838(4) 0.0648(12) Uani 1 1 d . . . . .
H71W H 0.9248 0.3502 0.1536 0.078 Uiso 1 1 d R U . . .
H72W H 0.9373 0.2874 0.0489 0.078 Uiso 1 1 d R U . . .
O8W O 0.5302(5) 0.0157(6) 0.9635(5) 0.0380(15) Uani 0.5 1 d . . P . .
H81W H 0.5404 -0.0177 1.0182 0.046 Uiso 1 1 d 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
Cu1 N7 2.059(3) . ?
Cu1 N1 2.066(3) . ?
Cu1 N10 2.089(3) . ?
Cu1 N4 2.101(3) . ?
Cu1 O511 2.216(2) . ?
N1 C20 1.493(4) . ?
N1 C2 1.501(4) . ?
N1 C12 1.502(4) . ?
C2 C3 1.504(5) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.485(4) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.478(5) . ?
N4 C5 1.480(5) . ?
C5 C6 1.501(6) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.500(4) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C40 1.490(4) . ?
N7 C8 1.500(5) . ?
C8 C9 1.516(5) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.490(4) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C30 1.481(4) . ?
N10 C11 1.491(5) . ?
C11 C12 1.508(5) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.842(3) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.494(3) . ?
P1 O11 1.509(2) . ?
P1 C21 1.821(4) . ?
O11 Cu3 1.928(2) . ?
C21 N22 1.486(4) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C23 1.482(5) . ?
N22 C25 1.484(4) . ?
N22 Cu2 2.018(3) . ?
C23 C24 1.514(5) . ?
C23 H231 0.9900 . ?
C23 H232 0.9900 . ?
C24 O242 1.239(5) . ?
C24 O241 1.282(5) . ?
O241 Cu2 1.946(2) . ?
C25 C26 1.525(5) . ?
C25 H251 0.9900 . ?
C25 H252 0.9900 . ?
C26 O262 1.224(5) . ?
C26 O261 1.290(4) . ?
O261 Cu2 1.951(3) . ?
C30 C31 1.503(5) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 O312 1.256(4) . ?
C31 O311 1.266(4) . ?
O311 Cu3 1.972(2) . ?
O312 Cu4 1.939(2) . ?
C40 C41 1.525(5) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C41 O411 1.226(4) . ?
C41 O412 1.284(4) . ?
O412 Cu2 1.930(2) 2_666 ?
C50 C51 1.512(5) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O512 1.245(4) . ?
C51 O511 1.253(4) . ?
O511 Cu3 2.376(2) . ?
O512 Cu4 1.919(3) 2_666 ?
Cu2 O412 1.930(2) 2_666 ?
O1C H11C 0.8818 . ?
O1C H12C 0.8647 . ?
Cu3 O2C 1.976(2) 2_666 ?
Cu3 O2C 1.977(2) . ?
Cu3 Cu3 2.9454(7) 2_666 ?
O2C Cu3 1.977(2) 2_666 ?
O2C Cu4 2.042(2) 2_666 ?
O2C H21C 0.9378 . ?
O3C Cu4 2.268(3) . ?
O3C H31C 0.8723 . ?
O3C H32C 0.8023 . ?
Cu4 O512 1.918(3) 2_666 ?
Cu4 O5C 2.005(3) . ?
Cu4 O2C 2.042(2) 2_666 ?
Cu4 O4C 2.412(3) . ?
O4C H41C 0.8786 . ?
O4C H42C 0.9098 . ?
O5C H51C 0.8174 . ?
O5C H52C 0.8926 . ?
O1W H11W 0.8828 . ?
O1W H12W 0.8719 . ?
O2W H21W 0.9146 . ?
O2W H22W 0.7904 . ?
O3W H31W 0.8566 . ?
O3W H32W 0.9212 . ?
O4W H41W 0.9018 . ?
O4W H42W 0.9730 . ?
O5W H51W 0.8507 . ?
O5W H52W 0.9382 . ?
O6W H61W 0.8685 . ?
O6W H62W 0.8985 . ?
O7W H71W 0.8924 . ?
O7W H72W 0.8985 . ?
O8W O8W 1.134(13) 2_657 ?
O8W H81W 0.8223 . ?

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
N7 Cu1 N1 149.84(11) . . ?
N7 Cu1 N10 85.74(12) . . ?
N1 Cu1 N10 87.19(11) . . ?
N7 Cu1 N4 85.48(13) . . ?
N1 Cu1 N4 83.67(12) . . ?
N10 Cu1 N4 144.98(11) . . ?
N7 Cu1 O511 95.33(11) . . ?
N1 Cu1 O511 109.67(10) . . ?
N10 Cu1 O511 136.77(10) . . ?
N4 Cu1 O511 77.83(10) . . ?
C20 N1 C2 109.9(3) . . ?
C20 N1 C12 108.5(3) . . ?
C2 N1 C12 107.6(2) . . ?
C20 N1 Cu1 120.3(2) . . ?
C2 N1 Cu1 109.6(2) . . ?
C12 N1 Cu1 99.80(19) . . ?
N1 C2 C3 110.2(3) . . ?
N1 C2 H21 109.6 . . ?
C3 C2 H21 109.6 . . ?
N1 C2 H22 109.6 . . ?
C3 C2 H22 109.6 . . ?
H21 C2 H22 108.1 . . ?
N4 C3 C2 109.1(3) . . ?
N4 C3 H31 109.9 . . ?
C2 C3 H31 109.9 . . ?
N4 C3 H32 109.9 . . ?
C2 C3 H32 109.9 . . ?
H31 C3 H32 108.3 . . ?
C50 N4 C5 111.2(3) . . ?
C50 N4 C3 111.7(3) . . ?
C5 N4 C3 111.8(3) . . ?
C50 N4 Cu1 111.0(2) . . ?
C5 N4 Cu1 107.5(2) . . ?
C3 N4 Cu1 103.4(2) . . ?
N4 C5 C6 109.9(3) . . ?
N4 C5 H51 109.7 . . ?
C6 C5 H51 109.7 . . ?
N4 C5 H52 109.7 . . ?
C6 C5 H52 109.7 . . ?
H51 C5 H52 108.2 . . ?
N7 C6 C5 110.8(3) . . ?
N7 C6 H61 109.5 . . ?
C5 C6 H61 109.5 . . ?
N7 C6 H62 109.5 . . ?
C5 C6 H62 109.5 . . ?
H61 C6 H62 108.1 . . ?
C40 N7 C6 108.0(3) . . ?
C40 N7 C8 111.3(3) . . ?
C6 N7 C8 109.0(3) . . ?
C40 N7 Cu1 118.8(2) . . ?
C6 N7 Cu1 101.4(2) . . ?
C8 N7 Cu1 107.5(2) . . ?
N7 C8 C9 110.5(3) . . ?
N7 C8 H81 109.5 . . ?
C9 C8 H81 109.5 . . ?
N7 C8 H82 109.5 . . ?
C9 C8 H82 109.5 . . ?
H81 C8 H82 108.1 . . ?
N10 C9 C8 108.8(3) . . ?
N10 C9 H91 109.9 . . ?
C8 C9 H91 109.9 . . ?
N10 C9 H92 109.9 . . ?
C8 C9 H92 109.9 . . ?
H91 C9 H92 108.3 . . ?
C30 N10 C9 110.2(3) . . ?
C30 N10 C11 108.9(3) . . ?
C9 N10 C11 112.6(3) . . ?
C30 N10 Cu1 117.4(2) . . ?
C9 N10 Cu1 101.8(2) . . ?
C11 N10 Cu1 105.9(2) . . ?
N10 C11 C12 110.4(3) . . ?
N10 C11 H111 109.6 . . ?
C12 C11 H111 109.6 . . ?
N10 C11 H112 109.6 . . ?
C12 C11 H112 109.6 . . ?
H111 C11 H112 108.1 . . ?
N1 C12 C11 111.0(3) . . ?
N1 C12 H121 109.4 . . ?
C11 C12 H121 109.4 . . ?
N1 C12 H122 109.4 . . ?
C11 C12 H122 109.4 . . ?
H121 C12 H122 108.0 . . ?
N1 C20 P1 122.1(2) . . ?
N1 C20 H201 106.8 . . ?
P1 C20 H201 106.8 . . ?
N1 C20 H202 106.8 . . ?
P1 C20 H202 106.8 . . ?
H201 C20 H202 106.7 . . ?
O12 P1 O11 114.76(18) . . ?
O12 P1 C21 114.7(2) . . ?
O11 P1 C21 104.89(17) . . ?
O12 P1 C20 114.00(16) . . ?
O11 P1 C20 112.36(15) . . ?
C21 P1 C20 94.01(16) . . ?
P1 O11 Cu3 140.68(16) . . ?
N22 C21 P1 117.8(2) . . ?
N22 C21 H211 107.9 . . ?
P1 C21 H211 107.9 . . ?
N22 C21 H212 107.9 . . ?
P1 C21 H212 107.9 . . ?
H211 C21 H212 107.2 . . ?
C23 N22 C25 113.9(3) . . ?
C23 N22 C21 112.3(3) . . ?
C25 N22 C21 108.3(3) . . ?
C23 N22 Cu2 105.6(2) . . ?
C25 N22 Cu2 103.6(2) . . ?
C21 N22 Cu2 112.9(2) . . ?
N22 C23 C24 111.7(3) . . ?
N22 C23 H231 109.3 . . ?
C24 C23 H231 109.3 . . ?
N22 C23 H232 109.3 . . ?
C24 C23 H232 109.3 . . ?
H231 C23 H232 107.9 . . ?
O242 C24 O241 124.2(4) . . ?
O242 C24 C23 118.0(4) . . ?
O241 C24 C23 117.8(3) . . ?
C24 O241 Cu2 113.3(2) . . ?
N22 C25 C26 109.2(3) . . ?
N22 C25 H251 109.8 . . ?
C26 C25 H251 109.8 . . ?
N22 C25 H252 109.8 . . ?
C26 C25 H252 109.8 . . ?
H251 C25 H252 108.3 . . ?
O262 C26 O261 124.7(4) . . ?
O262 C26 C25 119.9(3) . . ?
O261 C26 C25 115.4(3) . . ?
C26 O261 Cu2 114.1(2) . . ?
N10 C30 C31 112.9(3) . . ?
N10 C30 H301 109.0 . . ?
C31 C30 H301 109.0 . . ?
N10 C30 H302 109.0 . . ?
C31 C30 H302 109.0 . . ?
H301 C30 H302 107.8 . . ?
O312 C31 O311 127.1(3) . . ?
O312 C31 C30 115.3(3) . . ?
O311 C31 C30 117.6(3) . . ?
C31 O311 Cu3 129.4(2) . . ?
C31 O312 Cu4 128.1(2) . . ?
N7 C40 C41 117.1(3) . . ?
N7 C40 H401 108.0 . . ?
C41 C40 H401 108.0 . . ?
N7 C40 H402 108.0 . . ?
C41 C40 H402 108.0 . . ?
H401 C40 H402 107.3 . . ?
O411 C41 O412 126.2(3) . . ?
O411 C41 C40 122.9(3) . . ?
O412 C41 C40 110.9(3) . . ?
C41 O412 Cu2 133.3(2) . 2_666 ?
N4 C50 C51 112.0(3) . . ?
N4 C50 H501 109.2 . . ?
C51 C50 H501 109.2 . . ?
N4 C50 H502 109.2 . . ?
C51 C50 H502 109.2 . . ?
H501 C50 H502 107.9 . . ?
O512 C51 O511 126.8(3) . . ?
O512 C51 C50 113.6(3) . . ?
O511 C51 C50 119.5(3) . . ?
C51 O511 Cu1 113.5(2) . . ?
C51 O511 Cu3 122.6(2) . . ?
Cu1 O511 Cu3 103.95(10) . . ?
C51 O512 Cu4 133.4(2) . 2_666 ?
O412 Cu2 O241 104.34(11) 2_666 . ?
O412 Cu2 O261 86.98(11) 2_666 . ?
O241 Cu2 O261 167.14(11) . . ?
O412 Cu2 N22 170.59(12) 2_666 . ?
O241 Cu2 N22 85.07(11) . . ?
O261 Cu2 N22 83.70(12) . . ?
H11C O1C H12C 98.4 . . ?
O11 Cu3 O311 92.27(10) . . ?
O11 Cu3 O2C 164.06(10) . 2_666 ?
O311 Cu3 O2C 91.81(9) . 2_666 ?
O11 Cu3 O2C 95.97(10) . . ?
O311 Cu3 O2C 164.95(10) . . ?
O2C Cu3 O2C 83.69(10) 2_666 . ?
O11 Cu3 O511 94.53(10) . . ?
O311 Cu3 O511 76.20(9) . . ?
O2C Cu3 O511 101.40(9) 2_666 . ?
O2C Cu3 O511 90.58(9) . . ?
O11 Cu3 Cu3 135.65(8) . 2_666 ?
O311 Cu3 Cu3 132.03(7) . 2_666 ?
O2C Cu3 Cu3 41.85(7) 2_666 2_666 ?
O2C Cu3 Cu3 41.83(6) . 2_666 ?
O511 Cu3 Cu3 98.01(6) . 2_666 ?
Cu3 O2C Cu3 96.31(10) 2_666 . ?
Cu3 O2C Cu4 103.45(10) 2_666 2_666 ?
Cu3 O2C Cu4 127.03(12) . 2_666 ?
Cu3 O2C H21C 108.8 2_666 . ?
Cu3 O2C H21C 119.6 . . ?
Cu4 O2C H21C 99.7 2_666 . ?
Cu4 O3C H31C 118.2 . . ?
Cu4 O3C H32C 133.5 . . ?
H31C O3C H32C 103.8 . . ?
O512 Cu4 O312 165.53(11) 2_666 . ?
O512 Cu4 O5C 81.96(11) 2_666 . ?
O312 Cu4 O5C 86.10(11) . . ?
O512 Cu4 O2C 100.26(10) 2_666 2_666 ?
O312 Cu4 O2C 91.81(10) . 2_666 ?
O5C Cu4 O2C 177.63(10) . 2_666 ?
O512 Cu4 O3C 96.93(12) 2_666 . ?
O312 Cu4 O3C 91.99(10) . . ?
O5C Cu4 O3C 93.87(11) . . ?
O2C Cu4 O3C 85.07(9) 2_666 . ?
O512 Cu4 O4C 78.13(13) 2_666 . ?
O312 Cu4 O4C 94.83(12) . . ?
O5C Cu4 O4C 94.84(11) . . ?
O2C Cu4 O4C 86.45(10) 2_666 . ?
O3C Cu4 O4C 169.27(11) . . ?
Cu4 O4C H41C 120.8 . . ?
Cu4 O4C H42C 94.9 . . ?
H41C O4C H42C 106.8 . . ?
Cu4 O5C H51C 116.8 . . ?
Cu4 O5C H52C 129.6 . . ?
H51C O5C H52C 100.7 . . ?
H11W O1W H12W 100.6 . . ?
H21W O2W H22W 93.8 . . ?
H31W O3W H32W 107.4 . . ?
H41W O4W H42W 103.5 . . ?
H51W O5W H52W 95.3 . . ?
H61W O6W H62W 110.9 . . ?
H71W O7W H72W 126.2 . . ?
O8W O8W H81W 47.6 2_657 . ?

_refine_diff_density_max         1.675
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.121

