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

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2129733'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2021-12-19 deposited with the CCDC.	2022-02-20 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         ?
_chemical_formula_sum            'C66 H82 Cu3 N10 O39 P6'
_chemical_formula_weight         2015.85

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'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.5277(4)
_cell_length_b                   30.222(1)
_cell_length_c                   26.182(1)
_cell_angle_alpha                90
_cell_angle_beta                 100.361(4)
_cell_angle_gamma                90
_cell_volume                     8194.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_cell_measurement_reflns_used    11534
_cell_measurement_theta_min      4.2420
_cell_measurement_theta_max      29.3500

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'sky blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_F_000             4148
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.990
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.62289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 16.4547
_diffrn_reflns_number            64606
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         4.100
_diffrn_reflns_theta_max         30.955
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             22869
_reflns_number_gt                16194
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (Altomare 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST93 (Nardelli, 1993)'
_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)+(0.0756P)²+34.7902P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         22869
_refine_ls_number_parameters     1190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0844
_refine_ls_wR_factor_ref         0.2205
_refine_ls_wR_factor_gt          0.1999
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.004
_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 0.69501(6) 0.18511(2) 0.30261(2) 0.02585(13) Uani 1 1 d . . . . .
Cu2 Cu 0.34243(6) 0.13921(2) 0.30140(2) 0.02541(13) Uani 1 1 d . . . . .
Cu3 Cu 0.14659(6) 0.42189(2) 0.26205(2) 0.02635(14) Uani 1 1 d . . . . .
N1 N 0.8491(4) 0.20971(13) 0.26542(15) 0.0245(8) Uani 1 1 d . . . . .
C7 C 0.8769(5) 0.20441(17) 0.21807(19) 0.0300(10) Uani 1 1 d . . . . .
H7 H 0.8238 0.1863 0.1946 0.036 Uiso 1 1 calc R U . . .
C8 C 0.9820(5) 0.22474(19) 0.20207(19) 0.0344(11) Uani 1 1 d . . . . .
H8 H 1.0003 0.2193 0.1692 0.041 Uiso 1 1 calc R U . . .
C9 C 1.0580(5) 0.25299(18) 0.2356(2) 0.0322(11) Uani 1 1 d . . . . .
H9 H 1.1285 0.2668 0.2255 0.039 Uiso 1 1 calc R U . . .
C10 C 1.0294(5) 0.26100(16) 0.28475(19) 0.0269(9) Uani 1 1 d . . . . .
C11 C 1.1000(5) 0.29135(17) 0.3215(2) 0.0320(11) Uani 1 1 d . . . . .
H11 H 1.1666 0.3080 0.3123 0.038 Uiso 1 1 calc R U . . .
C12 C 1.0709(5) 0.29590(18) 0.3691(2) 0.0351(11) Uani 1 1 d . . . . .
H12 H 1.1184 0.3157 0.3922 0.042 Uiso 1 1 calc R U . . .
C13 C 0.9691(5) 0.27127(16) 0.38532(19) 0.0289(10) Uani 1 1 d . . . . .
C14 C 0.9370(5) 0.27494(19) 0.4348(2) 0.0366(12) Uani 1 1 d . . . . .
H14 H 0.9822 0.2942 0.4593 0.044 Uiso 1 1 calc R U . . .
C15 C 0.8380(5) 0.2497(2) 0.44669(19) 0.0371(12) Uani 1 1 d . . . . .
H15 H 0.8169 0.2514 0.4796 0.045 Uiso 1 1 calc R U . . .
C16 C 0.7688(5) 0.22159(19) 0.40935(18) 0.0315(11) Uani 1 1 d . . . . .
H16 H 0.7009 0.2051 0.4178 0.038 Uiso 1 1 calc R U . . .
N2 N 0.7974(4) 0.21763(13) 0.36166(15) 0.0248(8) Uani 1 1 d . . . . .
C17 C 0.8965(4) 0.24205(15) 0.34983(17) 0.0220(8) Uani 1 1 d . . . . .
C18 C 0.9251(4) 0.23758(15) 0.29862(17) 0.0236(9) Uani 1 1 d . . . . .
N4 N 0.7151(5) 0.12286(15) 0.3352(2) 0.0375(10) Uani 1 1 d . . . . .
C28 C 0.7636(7) 0.1099(2) 0.3830(3) 0.0498(16) Uani 1 1 d . . . . .
H28 H 0.7996 0.1308 0.4074 0.060 Uiso 1 1 calc R U . . .
C27 C 0.7620(8) 0.0649(3) 0.3980(4) 0.065(2) Uani 1 1 d . . . . .
H27 H 0.7948 0.0563 0.4319 0.078 Uiso 1 1 calc R U . . .
C26 C 0.7111(7) 0.0342(2) 0.3613(4) 0.067(2) Uani 1 1 d . . . . .
H26 H 0.7094 0.0046 0.3708 0.081 Uiso 1 1 calc R U . . .
C25 C 0.6626(6) 0.0459(2) 0.3109(4) 0.057(2) Uani 1 1 d . . . . .
C24 C 0.6094(7) 0.0160(2) 0.2691(4) 0.063(2) Uani 1 1 d . . . . .
H24 H 0.6055 -0.0141 0.2759 0.076 Uiso 1 1 calc R U . . .
C23 C 0.5662(7) 0.0306(2) 0.2210(4) 0.065(2) Uani 1 1 d . . . . .
H23 H 0.5368 0.0102 0.1950 0.078 Uiso 1 1 calc R U . . .
C22 C 0.5635(6) 0.0765(2) 0.2082(3) 0.0533(19) Uani 1 1 d . . . . .
C21 C 0.5169(6) 0.0944(3) 0.1600(3) 0.059(2) Uani 1 1 d . . . . .
H21 H 0.4850 0.0757 0.1324 0.071 Uiso 1 1 calc R U . . .
C20 C 0.5171(6) 0.1386(3) 0.1522(3) 0.062(2) Uani 1 1 d . . . . .
H20 H 0.4859 0.1503 0.1195 0.074 Uiso 1 1 calc R U . . .
C19 C 0.5644(5) 0.1669(2) 0.1938(2) 0.0456(15) Uani 1 1 d . . . . .
H19 H 0.5626 0.1973 0.1886 0.055 Uiso 1 1 calc R U . . .
N3 N 0.6121(4) 0.15074(16) 0.24095(18) 0.0358(10) Uani 1 1 d . . . . .
C30 C 0.6131(5) 0.1064(2) 0.2489(3) 0.0431(15) Uani 1 1 d . . . . .
C29 C 0.6648(5) 0.09176(18) 0.2998(3) 0.0440(15) Uani 1 1 d . . . . .
N5 N 0.3455(4) 0.07408(14) 0.31904(17) 0.0288(8) Uani 1 1 d . . . . .
C31 C 0.3878(5) 0.05436(18) 0.3639(2) 0.0344(11) Uani 1 1 d . . . . .
H31 H 0.4197 0.0717 0.3927 0.041 Uiso 1 1 calc R U . . .
C32 C 0.3866(6) 0.0080(2) 0.3699(3) 0.0446(14) Uani 1 1 d . . . . .
H32 H 0.4162 -0.0047 0.4022 0.054 Uiso 1 1 calc R U . . .
C33 C 0.3419(6) -0.01800(19) 0.3283(3) 0.0429(14) Uani 1 1 d . . . . .
H33 H 0.3421 -0.0486 0.3318 0.052 Uiso 1 1 calc R U . . .
C34 C 0.2950(5) 0.00176(17) 0.2794(2) 0.0356(12) Uani 1 1 d . . . . .
C35 C 0.2458(5) -0.02174(18) 0.2325(2) 0.0380(12) Uani 1 1 d . . . . .
H35 H 0.2431 -0.0525 0.2332 0.046 Uiso 1 1 calc R U . . .
C36 C 0.2037(5) -0.00083(19) 0.1878(2) 0.0390(13) Uani 1 1 d . . . . .
H36 H 0.1714 -0.0172 0.1582 0.047 Uiso 1 1 calc R U . . .
C37 C 0.2077(5) 0.04675(18) 0.1845(2) 0.0324(11) Uani 1 1 d . . . . .
C38 C 0.1672(5) 0.07122(19) 0.1388(2) 0.0362(12) Uani 1 1 d . . . . .
H38 H 0.1342 0.0568 0.1079 0.043 Uiso 1 1 calc R U . . .
C39 C 0.1768(6) 0.1160(2) 0.1403(2) 0.0386(12) Uani 1 1 d . . . . .
H39 H 0.1497 0.1325 0.1103 0.046 Uiso 1 1 calc R U . . .
C40 C 0.2277(5) 0.13764(17) 0.18731(19) 0.0300(10) Uani 1 1 d . . . . .
H40 H 0.2337 0.1683 0.1877 0.036 Uiso 1 1 calc R U . . .
N6 N 0.2671(4) 0.11548(14) 0.23067(16) 0.0274(8) Uani 1 1 d . . . . .
C41 C 0.2555(5) 0.07052(16) 0.22925(19) 0.0272(10) Uani 1 1 d . . . . .
C42 C 0.2997(5) 0.04826(17) 0.2778(2) 0.0295(10) Uani 1 1 d . . . . .
N7 N 0.1835(4) 0.46588(15) 0.31951(17) 0.0327(9) Uani 1 1 d . . . . .
C43 C 0.2375(6) 0.4589(2) 0.3679(2) 0.0410(13) Uani 1 1 d . . . . .
H43 H 0.2672 0.4306 0.3777 0.049 Uiso 1 1 calc R U . . .
C44 C 0.2524(6) 0.4927(2) 0.4057(3) 0.0506(16) Uani 1 1 d . . . . .
H44 H 0.2898 0.4866 0.4399 0.061 Uiso 1 1 calc R U . . .
C45 C 0.2112(6) 0.5345(2) 0.3914(3) 0.0482(16) Uani 1 1 d . . . . .
H45 H 0.2200 0.5570 0.4159 0.058 Uiso 1 1 calc R U . . .
C46 C 0.1557(5) 0.54324(19) 0.3398(2) 0.0390(13) Uani 1 1 d . . . . .
C47 C 0.1116(5) 0.58625(19) 0.3193(3) 0.0447(15) Uani 1 1 d . . . . .
H47 H 0.1213 0.6106 0.3413 0.054 Uiso 1 1 calc R U . . .
C48 C 0.0577(5) 0.59169(19) 0.2698(3) 0.0444(15) Uani 1 1 d . . . . .
H48 H 0.0303 0.6198 0.2581 0.053 Uiso 1 1 calc R U . . .
C49 C 0.0406(5) 0.55551(17) 0.2337(2) 0.0361(12) Uani 1 1 d . . . . .
C50 C -0.0177(5) 0.55904(19) 0.1809(3) 0.0415(14) Uani 1 1 d . . . . .
H50 H -0.0467 0.5863 0.1671 0.050 Uiso 1 1 calc R U . . .
C51 C -0.0313(5) 0.5223(2) 0.1503(2) 0.0397(13) Uani 1 1 d . . . . .
H51 H -0.0708 0.5241 0.1157 0.048 Uiso 1 1 calc R U . . .
C52 C 0.0153(5) 0.48145(18) 0.1720(2) 0.0340(11) Uani 1 1 d . . . . .
H52 H 0.0061 0.4565 0.1508 0.041 Uiso 1 1 calc R U . . .
N8 N 0.0714(4) 0.47698(14) 0.22105(17) 0.0292(9) Uani 1 1 d . . . . .
C53 C 0.0829(5) 0.51348(17) 0.2520(2) 0.0325(11) Uani 1 1 d . . . . .
C54 C 0.1420(5) 0.50727(17) 0.3055(2) 0.0322(11) Uani 1 1 d . . . . .
N9 N 0.0960(4) 0.38222(14) 0.20045(16) 0.0290(9) Uani 1 1 d . . . . .
C55 C 0.1600(6) 0.3767(2) 0.1614(2) 0.0389(12) Uani 1 1 d . . . . .
H55 H 0.2376 0.3916 0.1622 0.047 Uiso 1 1 calc R U . . .
C56 C 0.1141(7) 0.3493(3) 0.1196(2) 0.0529(17) Uani 1 1 d . . . . .
H56 H 0.1624 0.3453 0.0935 0.063 Uiso 1 1 calc R U . . .
C57 C -0.0028(7) 0.3281(2) 0.1167(2) 0.0511(16) Uani 1 1 d . . . . .
H57 H -0.0352 0.3105 0.0882 0.061 Uiso 1 1 calc R U . . .
C58 C -0.0718(6) 0.3334(2) 0.1567(2) 0.0413(13) Uani 1 1 d . . . . .
C59 C -0.1915(6) 0.3108(2) 0.1584(3) 0.0504(17) Uani 1 1 d . . . . .
H59 H -0.2305 0.2939 0.1302 0.060 Uiso 1 1 calc R U . . .
C60 C -0.2467(6) 0.3141(2) 0.2002(3) 0.0479(16) Uani 1 1 d . . . . .
H60 H -0.3231 0.2988 0.2007 0.057 Uiso 1 1 calc R U . . .
C61 C -0.1930(5) 0.34021(18) 0.2445(2) 0.0374(12) Uani 1 1 d . . . . .
C62 C -0.2430(6) 0.34149(19) 0.2902(3) 0.0424(14) Uani 1 1 d . . . . .
H62 H -0.3162 0.3251 0.2931 0.051 Uiso 1 1 calc R U . . .
C63 C -0.1842(6) 0.3669(2) 0.3307(3) 0.0434(14) Uani 1 1 d . . . . .
H63 H -0.2170 0.3681 0.3613 0.052 Uiso 1 1 calc R U . . .
C64 C -0.0724(5) 0.39126(19) 0.3254(2) 0.0361(12) Uani 1 1 d . . . . .
H64 H -0.0335 0.4087 0.3531 0.043 Uiso 1 1 calc R U . . .
N10 N -0.0210(4) 0.39027(13) 0.28300(16) 0.0283(8) Uani 1 1 d . . . . .
C65 C -0.0801(5) 0.36470(16) 0.2429(2) 0.0288(10) Uani 1 1 d . . . . .
C66 C -0.0183(5) 0.36082(17) 0.19858(19) 0.0290(10) Uani 1 1 d . . . . .
C4 C 0.4391(5) 0.33053(15) 0.37429(16) 0.0228(9) Uani 1 1 d . . . . .
H4 H 0.3464 0.3371 0.3685 0.027 Uiso 1 1 calc R U . . .
C5 C 0.4616(4) 0.28051(15) 0.37704(16) 0.0228(9) Uani 1 1 d . . . . .
H5 H 0.5525 0.2744 0.3759 0.027 Uiso 1 1 calc R U . . .
C6 C 0.4278(5) 0.26045(16) 0.42615(17) 0.0252(9) Uani 1 1 d . . . . .
H6 H 0.3338 0.2595 0.4234 0.030 Uiso 1 1 calc R U . . .
C1 C 0.4881(5) 0.28539(17) 0.47536(17) 0.0281(10) Uani 1 1 d . . . . .
H1 H 0.5822 0.2826 0.4799 0.034 Uiso 1 1 calc R U . . .
C2 C 0.4537(5) 0.33389(17) 0.47082(18) 0.0285(10) Uani 1 1 d . . . . .
H2 H 0.4933 0.3494 0.5026 0.034 Uiso 1 1 calc R U . . .
C3 C 0.5072(5) 0.35206(16) 0.42459(18) 0.0273(10) Uani 1 1 d . . . . .
H3 H 0.5998 0.3455 0.4294 0.033 Uiso 1 1 calc R U . . .
P4 P 0.42397(12) 0.37839(4) 0.28655(5) 0.0249(2) Uani 1 1 d . . . . .
O41 O 0.4948(3) 0.34686(11) 0.33226(12) 0.0236(6) Uani 1 1 d . . . . .
O42 O 0.4383(3) 0.35227(12) 0.23679(13) 0.0291(7) Uani 1 1 d . . . . .
O43 O 0.2845(3) 0.38171(12) 0.29366(13) 0.0291(7) Uani 1 1 d . . . . .
O44 O 0.4979(4) 0.42086(11) 0.28773(14) 0.0320(8) Uani 1 1 d . . . . .
P5 P 0.42640(11) 0.23995(4) 0.28293(4) 0.0218(2) Uani 1 1 d . . . . .
O52 O 0.3773(3) 0.27308(11) 0.23962(12) 0.0251(7) Uani 1 1 d . . . . .
O51 O 0.3825(3) 0.25896(11) 0.33450(12) 0.0232(6) Uani 1 1 d . . . . .
O53 O 0.3518(3) 0.19713(11) 0.27147(13) 0.0264(7) Uani 1 1 d . . . . .
O54 O 0.5718(3) 0.23556(11) 0.29301(13) 0.0260(7) Uani 1 1 d . . . . .
P6 P 0.39810(14) 0.17244(5) 0.41725(5) 0.0321(3) Uani 1 1 d . . . . .
O61 O 0.4791(3) 0.21652(11) 0.43207(12) 0.0280(7) Uani 1 1 d . . . . .
O62 O 0.2576(4) 0.18100(13) 0.41436(14) 0.0362(8) Uani 1 1 d . . . . .
O63 O 0.4380(3) 0.15307(12) 0.36975(14) 0.0329(8) Uani 1 1 d . . . . .
O64 O 0.4548(4) 0.14220(14) 0.46460(16) 0.0457(10) Uani 1 1 d . . . . .
P1 P 0.53239(16) 0.23238(6) 0.55649(6) 0.0407(3) Uani 1 1 d . . . . .
O11 O 0.4468(4) 0.26627(13) 0.51896(13) 0.0351(8) Uani 1 1 d . . . . .
O12 O 0.4625(5) 0.18826(16) 0.54988(18) 0.0567(12) Uani 1 1 d . . . . .
O13 O 0.6680(4) 0.23249(15) 0.54630(15) 0.0442(10) Uani 1 1 d . . . . .
O14 O 0.5327(4) 0.25003(18) 0.61143(15) 0.0521(12) Uani 1 1 d . . . . .
P2 P 0.23732(14) 0.36888(5) 0.49703(6) 0.0357(3) Uani 1 1 d . . . . .
O21 O 0.3167(3) 0.33907(12) 0.46272(13) 0.0317(8) Uani 1 1 d . . . . .
O22 O 0.1880(7) 0.4066(3) 0.4550(3) 0.047(2) Uani 0.567(7) 1 d . . P . .
O23 O 0.3302(7) 0.3901(2) 0.5401(3) 0.0362(18) Uani 0.567(7) 1 d . . P . .
O24 O 0.1296(6) 0.3439(2) 0.5113(2) 0.0351(17) Uani 0.567(7) 1 d . . P . .
O23' O 0.2886(10) 0.4109(3) 0.5105(4) 0.043(3) Uani 0.433(7) 1 d . . P . .
O22' O 0.0998(9) 0.3642(4) 0.4751(4) 0.046(3) Uani 0.433(7) 1 d . . P . .
O24' O 0.2717(9) 0.3409(4) 0.5436(7) 0.084(5) Uani 0.433(7) 1 d . . P . .
P3 P 0.60981(16) 0.43235(5) 0.42502(6) 0.0379(3) Uani 1 1 d . . . . .
O31 O 0.4889(4) 0.39900(12) 0.42107(14) 0.0352(8) Uani 1 1 d . . . . .
O32 O 0.5900(5) 0.45649(15) 0.37303(17) 0.0504(11) Uani 1 1 d . . . . .
O33 O 0.5982(5) 0.46519(15) 0.46681(18) 0.0566(13) Uani 1 1 d . . . . .
O34 O 0.7322(4) 0.40569(14) 0.43582(18) 0.0468(10) Uani 1 1 d . . . . .
OW1 O 0.1418(3) 0.16093(12) 0.31820(14) 0.0297(7) Uani 1 1 d . . . . .
OW2 O 0.4793(5) 0.45227(16) 0.54111(16) 0.0591(13) Uani 1 1 d . . . . .
OW3 O 0.3204(4) 0.26160(17) 0.64369(16) 0.0533(12) Uani 1 1 d . . . . .
OW4 O 0.1141(4) 0.26760(17) 0.56397(17) 0.0536(12) Uani 1 1 d . . . . .
OW5 O 0.4756(5) 0.12751(18) 0.63184(19) 0.0616(13) Uani 1 1 d . . . . .
OW6 O 0.8698(5) 0.29155(19) 0.57839(18) 0.0614(13) Uani 1 1 d . . . . .
OW7 O -0.0317(5) 0.44284(18) 0.43776(19) 0.0603(13) Uani 1 1 d . . . . .
OW8 O -0.1217(5) 0.36944(17) 0.5260(2) 0.0601(13) Uani 1 1 d . . . . .
OW9 O 0.7327(6) 0.1525(2) 0.5108(2) 0.0725(16) Uani 1 1 d . . . . .
OW10 O 0.6891(14) -0.0617(4) 0.4136(4) 0.038(3) Uani 0.5 1 d . . P . .
OW11 O 0.1561(8) 0.1952(2) 0.5039(2) 0.100(2) Uani 1 1 d . . . . .
OW12 O 0.9660(8) 0.1300(3) 0.4896(3) 0.111(2) Uani 1 1 d . . . . .
OW13 O -0.1462(11) 0.5973(3) 0.0659(4) 0.153(4) Uani 1 1 d . . . . .
OW14 O 0.3187(13) -0.0940(4) 0.4126(6) 0.088(4) Uani 0.5 1 d . . P . .
OW15 O 0.0910(12) 0.0189(6) 0.0237(4) 0.099(5) Uani 0.5 1 d . . P . .
OW16 O 0.0517(12) 0.4426(5) 0.0486(7) 0.114(6) Uani 0.5 1 d . . P . .
OW17 O -0.342(3) 0.5420(6) 0.0121(7) 0.092(10) Uani 0.25 1 d . . P . .
OW18 O -0.176(2) 0.4618(10) 0.0530(8) 0.081(8) Uani 0.25 1 d . . P . .
OW19 O 0.415(2) -0.0369(10) 0.5002(7) 0.083(8) Uani 0.25 1 d . . P . .
OW20 O 0.682(4) -0.0558(16) 0.431(2) 0.15(2) Uani 0.25 1 d . . P . .


_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 N2 1.979(4) . ?
Cu1 N3 1.985(4) . ?
Cu1 O54 1.988(3) . ?
Cu1 N4 2.061(5) . ?
Cu1 N1 2.168(4) . ?
Cu2 O53 1.928(3) . ?
Cu2 O63 1.935(4) . ?
Cu2 N6 2.011(4) . ?
Cu2 N5 2.021(4) . ?
Cu2 OW1 2.328(3) . ?
Cu3 O43 1.958(3) . ?
Cu3 N7 1.993(4) . ?
Cu3 N9 2.003(4) . ?
Cu3 N8 2.061(4) . ?
Cu3 N10 2.162(4) . ?
N1 C7 1.334(6) . ?
N1 C18 1.362(6) . ?
C7 C8 1.394(7) . ?
C8 C9 1.374(8) . ?
C9 C10 1.394(7) . ?
C10 C18 1.407(7) . ?
C10 C11 1.437(7) . ?
C11 C12 1.342(8) . ?
C12 C13 1.431(7) . ?
C13 C14 1.401(7) . ?
C13 C17 1.404(6) . ?
C14 C15 1.371(8) . ?
C15 C16 1.398(8) . ?
C16 N2 1.341(6) . ?
N2 C17 1.358(6) . ?
C17 C18 1.433(6) . ?
N4 C28 1.325(8) . ?
N4 C29 1.359(8) . ?
C28 C27 1.415(9) . ?
C27 C26 1.374(12) . ?
C26 C25 1.371(12) . ?
C25 C29 1.419(8) . ?
C25 C24 1.453(11) . ?
C24 C23 1.333(12) . ?
C23 C22 1.427(11) . ?
C22 C21 1.379(11) . ?
C22 C30 1.423(8) . ?
C21 C20 1.353(12) . ?
C20 C19 1.403(8) . ?
C19 N3 1.337(8) . ?
N3 C30 1.356(8) . ?
C30 C29 1.416(10) . ?
N5 C31 1.320(7) . ?
N5 C42 1.350(6) . ?
C31 C32 1.410(8) . ?
C32 C33 1.357(9) . ?
C33 C34 1.417(9) . ?
C34 C42 1.407(7) . ?
C34 C35 1.433(8) . ?
C35 C36 1.335(9) . ?
C36 C37 1.441(8) . ?
C37 C41 1.389(7) . ?
C37 C38 1.406(8) . ?
C38 C39 1.357(8) . ?
C39 C40 1.413(7) . ?
C40 N6 1.319(6) . ?
N6 C41 1.364(6) . ?
C41 C42 1.439(7) . ?
N7 C43 1.310(7) . ?
N7 C54 1.354(7) . ?
C43 C44 1.412(8) . ?
C44 C45 1.366(10) . ?
C45 C46 1.397(9) . ?
C46 C54 1.401(7) . ?
C46 C47 1.451(9) . ?
C47 C48 1.328(10) . ?
C48 C49 1.435(8) . ?
C49 C53 1.402(7) . ?
C49 C50 1.410(9) . ?
C50 C51 1.363(9) . ?
C51 C52 1.408(7) . ?
C52 N8 1.321(7) . ?
N8 C53 1.361(7) . ?
C53 C54 1.438(8) . ?
N9 C55 1.332(7) . ?
N9 C66 1.359(7) . ?
C55 C56 1.388(8) . ?
C56 C57 1.378(10) . ?
C57 C58 1.388(9) . ?
C58 C66 1.409(7) . ?
C58 C59 1.441(9) . ?
C59 C60 1.333(10) . ?
C60 C61 1.431(9) . ?
C61 C62 1.392(8) . ?
C61 C65 1.407(7) . ?
C62 C63 1.363(9) . ?
C63 C64 1.416(8) . ?
C64 N10 1.320(6) . ?
N10 C65 1.361(6) . ?
C65 C66 1.434(7) . ?
C4 O41 1.425(5) . ?
C4 C3 1.527(6) . ?
C4 C5 1.530(6) . ?
C5 O51 1.423(5) . ?
C5 C6 1.521(6) . ?
C6 O61 1.431(6) . ?
C6 C1 1.529(6) . ?
C1 O11 1.416(5) . ?
C1 C2 1.509(7) . ?
C2 O21 1.427(6) . ?
C2 C3 1.526(6) . ?
C3 O31 1.432(6) . ?
P4 O44 1.499(4) . ?
P4 O43 1.516(4) . ?
P4 O42 1.553(3) . ?
P4 O41 1.605(3) . ?
P5 O54 1.512(3) . ?
P5 O53 1.515(3) . ?
P5 O52 1.531(3) . ?
P5 O51 1.610(3) . ?
P6 O62 1.490(4) . ?
P6 O63 1.501(4) . ?
P6 O64 1.569(4) . ?
P6 O61 1.592(4) . ?
P1 O13 1.498(4) . ?
P1 O12 1.518(5) . ?
P1 O14 1.534(4) . ?
P1 O11 1.584(4) . ?
P2 O23' 1.400(10) . ?
P2 O22' 1.466(10) . ?
P2 O24 1.467(6) . ?
P2 O24' 1.476(16) . ?
P2 O23 1.499(7) . ?
P2 O22 1.605(7) . ?
P2 O21 1.609(4) . ?
O22 O23' 1.641(13) . ?
O22 O22' 1.718(13) . ?
O23 O23' 1.033(11) . ?
O23 O24' 1.620(14) . ?
O24 O22' 1.127(12) . ?
O24 O24' 1.584(12) . ?
P3 O33 1.498(4) . ?
P3 O34 1.503(5) . ?
P3 O32 1.525(5) . ?
P3 O31 1.612(4) . ?

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
N2 Cu1 N3 173.25(17) . . ?
N2 Cu1 O54 88.22(15) . . ?
N3 Cu1 O54 96.72(17) . . ?
N2 Cu1 N4 97.42(19) . . ?
N3 Cu1 N4 81.7(2) . . ?
O54 Cu1 N4 140.21(16) . . ?
N2 Cu1 N1 80.46(15) . . ?
N3 Cu1 N1 93.98(17) . . ?
O54 Cu1 N1 101.78(14) . . ?
N4 Cu1 N1 118.01(16) . . ?
O53 Cu2 O63 97.08(15) . . ?
O53 Cu2 N6 89.44(15) . . ?
O63 Cu2 N6 169.22(16) . . ?
O53 Cu2 N5 167.85(16) . . ?
O63 Cu2 N5 90.86(17) . . ?
N6 Cu2 N5 81.40(17) . . ?
O53 Cu2 OW1 86.29(14) . . ?
O63 Cu2 OW1 95.91(14) . . ?
N6 Cu2 OW1 93.06(14) . . ?
N5 Cu2 OW1 102.08(14) . . ?
O43 Cu3 N7 93.77(17) . . ?
O43 Cu3 N9 92.21(16) . . ?
N7 Cu3 N9 173.99(18) . . ?
O43 Cu3 N8 155.14(16) . . ?
N7 Cu3 N8 81.87(18) . . ?
N9 Cu3 N8 92.44(17) . . ?
O43 Cu3 N10 101.29(15) . . ?
N7 Cu3 N10 99.23(17) . . ?
N9 Cu3 N10 80.16(17) . . ?
N8 Cu3 N10 103.57(16) . . ?
C7 N1 C18 117.7(4) . . ?
C7 N1 Cu1 133.1(3) . . ?
C18 N1 Cu1 109.1(3) . . ?
N1 C7 C8 123.0(5) . . ?
C9 C8 C7 119.0(5) . . ?
C8 C9 C10 120.0(5) . . ?
C9 C10 C18 117.3(5) . . ?
C9 C10 C11 123.9(5) . . ?
C18 C10 C11 118.8(4) . . ?
C12 C11 C10 120.7(5) . . ?
C11 C12 C13 122.0(5) . . ?
C14 C13 C17 117.9(5) . . ?
C14 C13 C12 123.5(5) . . ?
C17 C13 C12 118.6(4) . . ?
C15 C14 C13 119.0(5) . . ?
C14 C15 C16 120.1(5) . . ?
N2 C16 C15 122.0(5) . . ?
C16 N2 C17 118.3(4) . . ?
C16 N2 Cu1 126.1(3) . . ?
C17 N2 Cu1 115.1(3) . . ?
N2 C17 C13 122.7(4) . . ?
N2 C17 C18 117.5(4) . . ?
C13 C17 C18 119.8(4) . . ?
N1 C18 C10 122.8(4) . . ?
N1 C18 C17 117.2(4) . . ?
C10 C18 C17 120.0(4) . . ?
C28 N4 C29 118.5(6) . . ?
C28 N4 Cu1 131.0(5) . . ?
C29 N4 Cu1 110.5(4) . . ?
N4 C28 C27 121.6(7) . . ?
C26 C27 C28 118.6(8) . . ?
C25 C26 C27 122.0(7) . . ?
C26 C25 C29 115.6(7) . . ?
C26 C25 C24 126.3(7) . . ?
C29 C25 C24 118.1(8) . . ?
C23 C24 C25 121.7(7) . . ?
C24 C23 C22 122.3(7) . . ?
C21 C22 C30 117.4(7) . . ?
C21 C22 C23 125.8(7) . . ?
C30 C22 C23 116.8(8) . . ?
C20 C21 C22 121.0(6) . . ?
C21 C20 C19 119.6(8) . . ?
N3 C19 C20 121.2(7) . . ?
C19 N3 C30 119.5(5) . . ?
C19 N3 Cu1 126.7(4) . . ?
C30 N3 Cu1 113.7(4) . . ?
N3 C30 C29 116.4(5) . . ?
N3 C30 C22 121.3(7) . . ?
C29 C30 C22 122.3(6) . . ?
N4 C29 C30 117.5(5) . . ?
N4 C29 C25 123.7(7) . . ?
C30 C29 C25 118.8(6) . . ?
C31 N5 C42 117.8(5) . . ?
C31 N5 Cu2 129.2(4) . . ?
C42 N5 Cu2 113.0(3) . . ?
N5 C31 C32 122.6(6) . . ?
C33 C32 C31 119.7(6) . . ?
C32 C33 C34 119.6(5) . . ?
C42 C34 C33 116.1(5) . . ?
C42 C34 C35 118.5(5) . . ?
C33 C34 C35 125.3(5) . . ?
C36 C35 C34 122.0(5) . . ?
C35 C36 C37 121.0(5) . . ?
C41 C37 C38 117.0(5) . . ?
C41 C37 C36 118.4(5) . . ?
C38 C37 C36 124.6(5) . . ?
C39 C38 C37 119.4(5) . . ?
C38 C39 C40 120.0(5) . . ?
N6 C40 C39 121.8(5) . . ?
C40 N6 C41 118.0(4) . . ?
C40 N6 Cu2 128.5(3) . . ?
C41 N6 Cu2 113.5(3) . . ?
N6 C41 C37 123.7(5) . . ?
N6 C41 C42 115.4(4) . . ?
C37 C41 C42 120.9(5) . . ?
N5 C42 C34 124.2(5) . . ?
N5 C42 C41 116.7(4) . . ?
C34 C42 C41 119.1(5) . . ?
C43 N7 C54 118.4(5) . . ?
C43 N7 Cu3 127.9(4) . . ?
C54 N7 Cu3 113.7(4) . . ?
N7 C43 C44 122.4(6) . . ?
C45 C44 C43 119.1(6) . . ?
C44 C45 C46 119.9(6) . . ?
C45 C46 C54 116.7(6) . . ?
C45 C46 C47 125.3(5) . . ?
C54 C46 C47 118.0(6) . . ?
C48 C47 C46 121.6(5) . . ?
C47 C48 C49 121.9(6) . . ?
C53 C49 C50 117.3(5) . . ?
C53 C49 C48 118.1(6) . . ?
C50 C49 C48 124.6(5) . . ?
C51 C50 C49 119.7(5) . . ?
C50 C51 C52 119.0(6) . . ?
N8 C52 C51 122.9(5) . . ?
C52 N8 C53 118.2(5) . . ?
C52 N8 Cu3 130.7(4) . . ?
C53 N8 Cu3 111.1(4) . . ?
N8 C53 C49 122.8(5) . . ?
N8 C53 C54 116.8(5) . . ?
C49 C53 C54 120.4(5) . . ?
N7 C54 C46 123.5(5) . . ?
N7 C54 C53 116.5(5) . . ?
C46 C54 C53 120.0(5) . . ?
C55 N9 C66 118.6(5) . . ?
C55 N9 Cu3 126.5(4) . . ?
C66 N9 Cu3 114.8(3) . . ?
N9 C55 C56 121.9(6) . . ?
C57 C56 C55 120.1(6) . . ?
C56 C57 C58 119.3(6) . . ?
C57 C58 C66 117.7(6) . . ?
C57 C58 C59 123.2(6) . . ?
C66 C58 C59 119.0(6) . . ?
C60 C59 C58 120.1(6) . . ?
C59 C60 C61 122.7(6) . . ?
C62 C61 C65 117.6(5) . . ?
C62 C61 C60 123.8(6) . . ?
C65 C61 C60 118.6(6) . . ?
C63 C62 C61 119.6(5) . . ?
C62 C63 C64 119.1(5) . . ?
N10 C64 C63 122.9(6) . . ?
C64 N10 C65 117.5(5) . . ?
C64 N10 Cu3 132.9(4) . . ?
C65 N10 Cu3 109.6(3) . . ?
N10 C65 C61 123.2(5) . . ?
N10 C65 C66 117.4(4) . . ?
C61 C65 C66 119.3(5) . . ?
N9 C66 C58 122.4(5) . . ?
N9 C66 C65 117.4(4) . . ?
C58 C66 C65 120.1(5) . . ?
O41 C4 C3 108.9(4) . . ?
O41 C4 C5 107.2(3) . . ?
C3 C4 C5 109.6(4) . . ?
O51 C5 C6 106.6(4) . . ?
O51 C5 C4 110.6(4) . . ?
C6 C5 C4 112.1(4) . . ?
O61 C6 C5 108.7(4) . . ?
O61 C6 C1 105.9(4) . . ?
C5 C6 C1 113.0(4) . . ?
O11 C1 C2 110.8(4) . . ?
O11 C1 C6 109.7(4) . . ?
C2 C1 C6 110.8(4) . . ?
O21 C2 C1 109.9(4) . . ?
O21 C2 C3 110.5(4) . . ?
C1 C2 C3 107.1(4) . . ?
O31 C3 C2 110.1(4) . . ?
O31 C3 C4 109.2(4) . . ?
C2 C3 C4 110.3(4) . . ?
O44 P4 O43 116.8(2) . . ?
O44 P4 O42 108.9(2) . . ?
O43 P4 O42 112.2(2) . . ?
O44 P4 O41 108.85(19) . . ?
O43 P4 O41 106.17(18) . . ?
O42 P4 O41 102.80(18) . . ?
C4 O41 P4 125.5(3) . . ?
P4 O43 Cu3 130.5(2) . . ?
O54 P5 O53 115.62(19) . . ?
O54 P5 O52 112.53(19) . . ?
O53 P5 O52 108.53(19) . . ?
O54 P5 O51 108.60(18) . . ?
O53 P5 O51 104.73(18) . . ?
O52 P5 O51 106.14(18) . . ?
C5 O51 P5 127.2(3) . . ?
P5 O53 Cu2 139.2(2) . . ?
P5 O54 Cu1 134.9(2) . . ?
O62 P6 O63 116.7(2) . . ?
O62 P6 O64 112.0(2) . . ?
O63 P6 O64 107.7(2) . . ?
O62 P6 O61 110.5(2) . . ?
O63 P6 O61 108.1(2) . . ?
O64 P6 O61 100.6(2) . . ?
C6 O61 P6 125.1(3) . . ?
P6 O63 Cu2 132.4(2) . . ?
O13 P1 O12 116.1(3) . . ?
O13 P1 O14 109.0(3) . . ?
O12 P1 O14 109.4(3) . . ?
O13 P1 O11 110.0(2) . . ?
O12 P1 O11 106.7(3) . . ?
O14 P1 O11 105.2(2) . . ?
C1 O11 P1 122.8(3) . . ?
O23' P2 O22' 119.6(6) . . ?
O23' P2 O24 133.2(5) . . ?
O22' P2 O24 45.2(5) . . ?
O23' P2 O24' 106.7(6) . . ?
O22' P2 O24' 110.4(6) . . ?
O24 P2 O24' 65.1(5) . . ?
O23' P2 O23 41.6(5) . . ?
O22' P2 O23 143.3(5) . . ?
O24 P2 O23 117.3(4) . . ?
O24' P2 O23 66.0(5) . . ?
O23' P2 O22 65.8(5) . . ?
O22' P2 O22 67.9(5) . . ?
O24 P2 O22 111.8(4) . . ?
O24' P2 O22 167.4(6) . . ?
O23 P2 O22 107.4(4) . . ?
O23' P2 O21 115.6(4) . . ?
O22' P2 O21 107.7(4) . . ?
O24 P2 O21 111.0(3) . . ?
O24' P2 O21 93.7(5) . . ?
O23 P2 O21 109.0(3) . . ?
O22 P2 O21 98.7(3) . . ?
C2 O21 P2 126.2(3) . . ?
P2 O22 O23' 51.1(4) . . ?
P2 O22 O22' 52.2(4) . . ?
O23' O22 O22' 95.0(6) . . ?
O23' O23 P2 64.1(7) . . ?
O23' O23 O24' 119.1(9) . . ?
P2 O23 O24' 56.3(6) . . ?
O22' O24 P2 67.3(6) . . ?
O22' O24 O24' 125.0(9) . . ?
P2 O24 O24' 57.7(7) . . ?
O23 O23' P2 74.3(7) . . ?
O23 O23' O22 137.4(10) . . ?
P2 O23' O22 63.1(5) . . ?
O24 O22' P2 67.4(6) . . ?
O24 O22' O22 125.5(8) . . ?
P2 O22' O22 59.9(4) . . ?
P2 O24' O24 57.2(5) . . ?
P2 O24' O23 57.7(6) . . ?
O24 O24' O23 104.4(8) . . ?
O33 P3 O34 113.4(3) . . ?
O33 P3 O32 108.6(3) . . ?
O34 P3 O32 113.5(3) . . ?
O33 P3 O31 107.1(2) . . ?
O34 P3 O31 108.5(2) . . ?
O32 P3 O31 105.2(2) . . ?
C3 O31 P3 121.3(3) . . ?

_refine_diff_density_max         2.078
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.123


# start Validation Reply Form
_vrf_PLAT214_shelx               
;
PROBLEM: Atom Ow17 (Anion/Solvent) ADP max/min Ratio 10.1 prolat
RESPONSE: this oxygen belong to a disordered water molecule
;
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact Ow2 ..O23' . 2.38 Ang.
RESPONSE: the short O...O contacts are H-bonds. Several of them involve disordered groups
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 68 Note
RESPONSE: these reflections were covered by the used beamstop's mask
;
# end Validation Reply Form
#===END
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2129734'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2022-01-31 deposited with the CCDC.	2022-02-20 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         ?
_chemical_formula_sum            'C36 H56 Cu2 N6 O26.50 P3'
_chemical_formula_weight         1216.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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                   14.6359(5)
_cell_length_b                   14.6677(5)
_cell_length_c                   15.1995(8)
_cell_angle_alpha                63.897(4)
_cell_angle_beta                 64.765(4)
_cell_angle_gamma                65.067(4)
_cell_volume                     2538.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    7321
_cell_measurement_theta_min      5.5300
_cell_measurement_theta_max      72.0370

_exptl_crystal_description       prismatic
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_F_000             1258
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    2.754
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.71213
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.1241
_diffrn_reflns_number            17570
_diffrn_reflns_av_unetI/netI     0.1225
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.030
_diffrn_reflns_theta_max         72.515
_diffrn_reflns_theta_full        65.000
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measured_fraction_theta_full 0.910
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_Laue_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_point_group_measured_fraction_full 0.910
_reflns_number_total             8712
_reflns_number_gt                6177
_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 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_structure_solution    'SIR97 (Altomare 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST93 (Nardelli, 1993)'
_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)+(0.1431P)²+2.8535P] 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         8712
_refine_ls_number_parameters     680
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0799
_refine_ls_wR_factor_ref         0.2659
_refine_ls_wR_factor_gt          0.2054
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_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
C1 C 1.1169(4) 0.3265(4) 0.9840(4) 0.0165(11) Uani 1 1 d . . . . .
H1 H 1.0893 0.3791 1.0193 0.020 Uiso 1 1 calc R U . . .
C2 C 1.0402(5) 0.3504(4) 0.9270(5) 0.0197(12) Uani 1 1 d . . . . .
H2 H 0.9699 0.3496 0.9759 0.024 Uiso 1 1 calc R U . . .
C3 C 1.0348(5) 0.4583(5) 0.8474(5) 0.0193(11) Uani 1 1 d . . . . .
H3 H 1.0082 0.5115 0.8816 0.023 Uiso 1 1 calc R U . . .
C4 C 1.1416(4) 0.4658(5) 0.7690(4) 0.0184(11) Uani 1 1 d . . . . .
H4 H 1.1656 0.4146 0.7330 0.022 Uiso 1 1 calc R U . . .
C5 C 1.2223(5) 0.4371(5) 0.8222(5) 0.0214(12) Uani 1 1 d . . . . .
H5 H 1.2039 0.4937 0.8498 0.026 Uiso 1 1 calc R U . . .
C6 C 1.2276(5) 0.3307(4) 0.9113(5) 0.0185(11) Uani 1 1 d . . . . .
H6 H 1.2589 0.2723 0.8827 0.022 Uiso 1 1 calc R U . . .
P1 P 1.04991(12) 0.20080(11) 1.17242(11) 0.0206(3) Uani 1 1 d . . . . .
O11 O 1.1287(3) 0.2236(3) 1.0579(3) 0.0204(8) Uani 1 1 d . . . . .
O12 O 1.0254(4) 0.2868(3) 1.2137(3) 0.0243(9) Uani 1 1 d . . . . .
O13 O 0.9456(4) 0.2050(3) 1.1632(3) 0.0243(9) Uani 1 1 d . . . . .
O14 O 1.1059(4) 0.0916(3) 1.2286(3) 0.0251(9) Uani 1 1 d . . . . .
P2 P 1.00259(12) 0.19941(12) 0.91133(12) 0.0211(3) Uani 1 1 d . . . . .
O21 O 1.0779(3) 0.2700(3) 0.8790(3) 0.0194(8) Uani 1 1 d . . . . .
O22 O 1.0628(4) 0.1338(3) 0.8402(3) 0.0244(9) Uani 1 1 d . . . . .
O23 O 0.9887(4) 0.1335(3) 1.0246(3) 0.0287(10) Uani 1 1 d . . . . .
O24 O 0.8966(3) 0.2738(3) 0.8991(3) 0.0242(9) Uani 1 1 d . . . . .
P3 P 0.84136(12) 0.54277(11) 0.83074(12) 0.0203(3) Uani 1 1 d . . . . .
O31 O 0.9638(3) 0.4814(3) 0.7927(3) 0.0188(8) Uani 1 1 d . . . . .
O32 O 0.8089(3) 0.5244(3) 0.9440(3) 0.0241(9) Uani 1 1 d . . . . .
O33 O 0.8324(3) 0.6626(3) 0.7674(3) 0.0227(9) Uani 1 1 d . . . . .
O34 O 0.7851(3) 0.5092(3) 0.7933(3) 0.0245(9) Uani 1 1 d . . . . .
O41 O 1.1359(3) 0.5678(3) 0.6956(3) 0.0226(9) Uani 1 1 d . . . . .
H41 H 1.0854 0.6115 0.7201 0.034 Uiso 1 1 calc R U . . .
O51 O 1.3258(3) 0.4291(4) 0.7504(3) 0.0262(9) Uani 1 1 d . . . . .
H51 H 1.3231 0.4389 0.6941 0.039 Uiso 1 1 calc R U . . .
O61 O 1.2911(3) 0.3179(3) 0.9682(3) 0.0229(9) Uani 1 1 d . . . . .
H61 H 1.2640 0.3652 0.9943 0.034 Uiso 1 1 calc R U . . .
Cu1 Cu 0.82300(7) 0.34698(7) 0.79693(7) 0.0211(3) Uani 1 1 d . . . . .
N1 N 0.6774(4) 0.3393(4) 0.8984(4) 0.0214(10) Uani 1 1 d . . . . .
C7 C 0.6505(5) 0.3226(5) 1.0011(5) 0.0279(14) Uani 1 1 d . . . . .
H7 H 0.7028 0.3028 1.0307 0.033 Uiso 1 1 calc R U . . .
C8 C 0.5475(6) 0.3348(6) 1.0607(6) 0.0362(16) Uani 1 1 d . . . . .
H8 H 0.5296 0.3213 1.1309 0.043 Uiso 1 1 calc R U . . .
C9 C 0.4711(6) 0.3675(7) 1.0145(6) 0.0409(18) Uani 1 1 d . . . . .
H9 H 0.4007 0.3784 1.0539 0.049 Uiso 1 1 calc R U . . .
C10 C 0.4965(5) 0.3845(6) 0.9114(6) 0.0340(15) Uani 1 1 d . . . . .
H10 H 0.4449 0.4055 0.8805 0.041 Uiso 1 1 calc R U . . .
C11 C 0.6012(5) 0.3691(5) 0.8563(5) 0.0272(14) Uani 1 1 d . . . . .
N2 N 0.7456(4) 0.3768(4) 0.7043(4) 0.0222(11) Uani 1 1 d . . . . .
C12 C 0.6427(5) 0.3859(5) 0.7433(6) 0.0292(15) Uani 1 1 d . . . . .
C13 C 0.5844(6) 0.4052(5) 0.6827(6) 0.0334(16) Uani 1 1 d . . . . .
H13 H 0.5130 0.4096 0.7097 0.040 Uiso 1 1 calc R U . . .
C14 C 0.6379(6) 0.4181(6) 0.5777(6) 0.0328(15) Uani 1 1 d . . . . .
H14 H 0.6004 0.4343 0.5338 0.039 Uiso 1 1 calc R U . . .
C15 C 0.7440(6) 0.4072(5) 0.5391(6) 0.0309(15) Uani 1 1 d . . . . .
H15 H 0.7793 0.4126 0.4704 0.037 Uiso 1 1 calc R U . . .
C16 C 0.7975(5) 0.3879(5) 0.6052(5) 0.0236(13) Uani 1 1 d . . . . .
N3 N 0.9424(4) 0.3517(4) 0.6614(4) 0.0222(11) Uani 1 1 d . . . . .
C17 C 0.9119(5) 0.3725(5) 0.5804(5) 0.0228(13) Uani 1 1 d . . . . .
C18 C 0.9808(6) 0.3809(5) 0.4823(5) 0.0281(14) Uani 1 1 d . . . . .
H18 H 0.9576 0.3959 0.4279 0.034 Uiso 1 1 calc R U . . .
C19 C 1.0852(6) 0.3664(6) 0.4679(5) 0.0309(15) Uani 1 1 d . . . . .
H19 H 1.1340 0.3691 0.4034 0.037 Uiso 1 1 calc R U . . .
C20 C 1.1173(5) 0.3477(5) 0.5492(5) 0.0266(13) Uani 1 1 d . . . . .
H20 H 1.1869 0.3399 0.5401 0.032 Uiso 1 1 calc R U . . .
C21 C 1.0425(5) 0.3412(4) 0.6449(5) 0.0207(12) Uani 1 1 d . . . . .
H21 H 1.0634 0.3288 0.6999 0.025 Uiso 1 1 calc R U . . .
Cu2 Cu 1.11967(7) -0.06892(7) 1.25415(7) 0.0237(3) Uani 1 1 d . . . . .
N4 N 0.9855(5) -0.0847(4) 1.3720(4) 0.0256(11) Uani 1 1 d . . . . .
C22 C 0.8902(6) -0.0644(6) 1.3674(5) 0.0350(16) Uani 1 1 d . . . . .
H22 H 0.8811 -0.0430 1.3035 0.042 Uiso 1 1 calc R U . . .
C23 C 0.8040(7) -0.0736(7) 1.4530(6) 0.0415(18) Uani 1 1 d . . . . .
H23 H 0.7385 -0.0597 1.4468 0.050 Uiso 1 1 calc R U . . .
C24 C 0.8160(7) -0.1039(7) 1.5491(6) 0.0424(18) Uani 1 1 d . . . . .
H24 H 0.7590 -0.1116 1.6080 0.051 Uiso 1 1 calc R U . . .
C25 C 0.9145(7) -0.1224(6) 1.5552(5) 0.0366(17) Uani 1 1 d . . . . .
H25 H 0.9244 -0.1406 1.6180 0.044 Uiso 1 1 calc R U . . .
C26 C 0.9979(6) -0.1132(5) 1.4658(5) 0.0294(14) Uani 1 1 d . . . . .
N5 N 1.1762(5) -0.1236(4) 1.3679(4) 0.0243(11) Uani 1 1 d . . . . .
C27 C 1.1072(6) -0.1332(5) 1.4634(5) 0.0299(15) Uani 1 1 d . . . . .
C28 C 1.1424(7) -0.1649(6) 1.5456(6) 0.0417(18) Uani 1 1 d . . . . .
H28 H 1.0964 -0.1745 1.6119 0.050 Uiso 1 1 calc R U . . .
C29 C 1.2500(7) -0.1824(6) 1.5263(6) 0.044(2) Uani 1 1 d . . . . .
H29 H 1.2757 -0.2029 1.5806 0.053 Uiso 1 1 calc R U . . .
C30 C 1.3178(7) -0.1699(6) 1.4290(7) 0.043(2) Uani 1 1 d . . . . .
H30 H 1.3889 -0.1800 1.4164 0.052 Uiso 1 1 calc R U . . .
C31 C 1.2779(6) -0.1416(5) 1.3494(6) 0.0354(16) Uani 1 1 d . . . . .
N6 N 1.2766(5) -0.1015(4) 1.1802(5) 0.0320(13) Uani 1 1 d . . . . .
C32 C 1.3374(6) -0.1278(5) 1.2392(6) 0.0325(16) Uani 1 1 d . . . . .
C33 C 1.4462(6) -0.1435(5) 1.1971(7) 0.0384(17) Uani 1 1 d . . . . .
H33 H 1.4879 -0.1629 1.2382 0.046 Uiso 1 1 calc R U . . .
C34 C 1.4907(7) -0.1295(6) 1.0931(8) 0.048(2) Uani 1 1 d . . . . .
H34 H 1.5630 -0.1393 1.0639 0.057 Uiso 1 1 calc R U . . .
C35 C 1.4309(6) -0.1021(6) 1.0345(7) 0.0430(19) Uani 1 1 d . . . . .
H35 H 1.4611 -0.0922 0.9646 0.052 Uiso 1 1 calc R U . . .
C36 C 1.3224(6) -0.0883(5) 1.0788(5) 0.0319(15) Uani 1 1 d . . . . .
H36 H 1.2809 -0.0698 1.0378 0.038 Uiso 1 1 calc R U . . .
OW1 O 1.0740(4) -0.0514(4) 1.1434(4) 0.0304(11) Uani 1 1 d D . . . .
OW2 O 0.6425(5) 0.6695(5) 0.6923(6) 0.0577(17) Uani 1 1 d . . . . .
OW3 O 0.6217(7) 0.0541(8) 1.2602(9) 0.101(3) Uani 1 1 d . . . . .
OW4 O 0.5664(14) 0.0957(14) 1.4392(14) 0.081(5) Uani 0.5 1 d . U P . .
OW5 O 0.7985(4) 0.0667(4) 1.1044(6) 0.0567(18) Uani 1 1 d . . . . .
OW6 O 1.3939(6) 0.2965(6) 0.6313(5) 0.0619(17) Uani 1 1 d . . . . .
OW7 O 1.3690(5) 0.6112(5) 0.6882(5) 0.0584(17) Uani 1 1 d . . . . .
OW8 O 0.7558(4) 0.3622(4) 1.1239(4) 0.0350(11) Uani 1 1 d . . . . .
OW9 O 1.3221(4) 0.1281(4) 1.1406(4) 0.0317(10) Uani 1 1 d . . . . .
OW10 O 1.4074(5) 0.1451(6) 1.2638(5) 0.0507(15) Uani 1 1 d . . . . .
OW11 O 1.2742(6) 0.1595(6) 0.7112(6) 0.070(2) Uani 1 1 d . . . . .
OW12 O 0.5367(6) 0.6942(7) 0.5719(6) 0.070(2) Uani 1 1 d . . . . .
HW1 H 1.062(8) 0.002(8) 1.100(8) 0.050 Uiso 1 1 d D U . . .
HW2 H 1.033(9) -0.115(10) 1.144(9) 0.08(4) Uiso 1 1 d . . . . .
H330 H 0.866(8) 0.694(8) 0.779(7) 0.050 Uiso 1 1 d . 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
C1 O11 1.423(7) . ?
C1 C6 1.532(8) . ?
C1 C2 1.538(7) . ?
C2 O21 1.447(8) . ?
C2 C3 1.505(8) . ?
C3 O31 1.441(6) . ?
C3 C4 1.522(8) . ?
C4 O41 1.413(7) . ?
C4 C5 1.524(8) . ?
C5 O51 1.433(7) . ?
C5 C6 1.550(8) . ?
C6 O61 1.428(6) . ?
P1 O12 1.495(5) . ?
P1 O14 1.501(4) . ?
P1 O13 1.565(4) . ?
P1 O11 1.604(4) . ?
O14 Cu2 2.145(4) . ?
P2 O22 1.503(5) . ?
P2 O24 1.507(5) . ?
P2 O23 1.531(5) . ?
P2 O21 1.606(4) . ?
O24 Cu1 1.926(4) . ?
P3 O34 1.495(4) . ?
P3 O32 1.505(5) . ?
P3 O33 1.567(4) . ?
P3 O31 1.604(4) . ?
O34 Cu1 2.184(4) . ?
Cu1 N2 1.964(5) . ?
Cu1 N1 2.044(5) . ?
Cu1 N3 2.052(5) . ?
N1 C11 1.340(8) . ?
N1 C7 1.369(9) . ?
C7 C8 1.370(10) . ?
C8 C9 1.376(11) . ?
C9 C10 1.377(11) . ?
C10 C11 1.372(10) . ?
C11 C12 1.497(10) . ?
N2 C12 1.333(9) . ?
N2 C16 1.336(8) . ?
C12 C13 1.376(9) . ?
C13 C14 1.410(11) . ?
C14 C15 1.370(10) . ?
C15 C16 1.392(9) . ?
C16 C17 1.488(9) . ?
N3 C21 1.327(8) . ?
N3 C17 1.353(8) . ?
C17 C18 1.384(9) . ?
C18 C19 1.382(10) . ?
C19 C20 1.383(9) . ?
C20 C21 1.390(9) . ?
Cu2 N5 1.938(5) . ?
Cu2 OW1 1.944(5) . ?
Cu2 N6 2.028(6) . ?
Cu2 N4 2.035(6) . ?
N4 C22 1.325(9) . ?
N4 C26 1.368(9) . ?
C22 C23 1.375(11) . ?
C23 C24 1.394(11) . ?
C24 C25 1.386(12) . ?
C25 C26 1.384(10) . ?
C26 C27 1.487(10) . ?
N5 C31 1.320(9) . ?
N5 C27 1.356(9) . ?
C27 C28 1.370(10) . ?
C28 C29 1.402(13) . ?
C29 C30 1.367(13) . ?
C30 C31 1.391(11) . ?
C31 C32 1.487(11) . ?
N6 C36 1.352(9) . ?
N6 C32 1.353(9) . ?
C32 C33 1.397(11) . ?
C33 C34 1.384(13) . ?
C34 C35 1.332(13) . ?
C35 C36 1.397(11) . ?

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
O11 C1 C6 106.6(4) . . ?
O11 C1 C2 111.7(4) . . ?
C6 C1 C2 112.2(5) . . ?
O21 C2 C3 110.4(5) . . ?
O21 C2 C1 109.0(5) . . ?
C3 C2 C1 108.9(4) . . ?
O31 C3 C2 109.5(5) . . ?
O31 C3 C4 107.6(5) . . ?
C2 C3 C4 112.5(5) . . ?
O41 C4 C3 112.1(5) . . ?
O41 C4 C5 109.5(4) . . ?
C3 C4 C5 110.5(5) . . ?
O51 C5 C4 110.5(5) . . ?
O51 C5 C6 107.3(5) . . ?
C4 C5 C6 113.9(4) . . ?
O61 C6 C1 108.9(5) . . ?
O61 C6 C5 110.6(4) . . ?
C1 C6 C5 110.6(5) . . ?
O12 P1 O14 115.9(2) . . ?
O12 P1 O13 108.2(3) . . ?
O14 P1 O13 112.6(2) . . ?
O12 P1 O11 110.0(2) . . ?
O14 P1 O11 103.8(2) . . ?
O13 P1 O11 105.8(2) . . ?
C1 O11 P1 122.4(4) . . ?
P1 O14 Cu2 137.4(3) . . ?
O22 P2 O24 115.6(3) . . ?
O22 P2 O23 113.4(3) . . ?
O24 P2 O23 108.6(3) . . ?
O22 P2 O21 102.7(2) . . ?
O24 P2 O21 107.8(2) . . ?
O23 P2 O21 108.1(2) . . ?
C2 O21 P2 118.2(4) . . ?
P2 O24 Cu1 139.7(3) . . ?
O34 P3 O32 118.1(3) . . ?
O34 P3 O33 106.2(2) . . ?
O32 P3 O33 111.4(2) . . ?
O34 P3 O31 105.6(2) . . ?
O32 P3 O31 109.6(2) . . ?
O33 P3 O31 105.0(2) . . ?
C3 O31 P3 120.5(4) . . ?
P3 O34 Cu1 124.0(2) . . ?
O24 Cu1 N2 162.0(2) . . ?
O24 Cu1 N1 95.5(2) . . ?
N2 Cu1 N1 79.2(2) . . ?
O24 Cu1 N3 103.4(2) . . ?
N2 Cu1 N3 79.3(2) . . ?
N1 Cu1 N3 157.8(2) . . ?
O24 Cu1 O34 98.86(17) . . ?
N2 Cu1 O34 98.24(18) . . ?
N1 Cu1 O34 89.73(19) . . ?
N3 Cu1 O34 98.57(19) . . ?
C11 N1 C7 119.1(6) . . ?
C11 N1 Cu1 115.5(4) . . ?
C7 N1 Cu1 124.7(4) . . ?
C8 C7 N1 120.8(6) . . ?
C7 C8 C9 118.6(7) . . ?
C8 C9 C10 121.5(7) . . ?
C11 C10 C9 117.1(7) . . ?
N1 C11 C10 123.0(7) . . ?
N1 C11 C12 112.8(6) . . ?
C10 C11 C12 124.2(6) . . ?
C12 N2 C16 122.7(6) . . ?
C12 N2 Cu1 118.2(5) . . ?
C16 N2 Cu1 119.1(4) . . ?
N2 C12 C13 121.0(7) . . ?
N2 C12 C11 113.7(6) . . ?
C13 C12 C11 125.3(6) . . ?
C12 C13 C14 116.9(7) . . ?
C15 C14 C13 121.3(6) . . ?
C14 C15 C16 118.3(7) . . ?
N2 C16 C15 119.7(6) . . ?
N2 C16 C17 112.8(5) . . ?
C15 C16 C17 127.5(6) . . ?
C21 N3 C17 118.1(6) . . ?
C21 N3 Cu1 127.4(4) . . ?
C17 N3 Cu1 114.4(4) . . ?
N3 C17 C18 122.8(6) . . ?
N3 C17 C16 114.3(6) . . ?
C18 C17 C16 122.8(6) . . ?
C19 C18 C17 117.8(6) . . ?
C18 C19 C20 120.1(6) . . ?
C19 C20 C21 118.0(6) . . ?
N3 C21 C20 123.0(6) . . ?
N5 Cu2 OW1 165.6(2) . . ?
N5 Cu2 N6 79.3(2) . . ?
OW1 Cu2 N6 97.0(2) . . ?
N5 Cu2 N4 81.0(2) . . ?
OW1 Cu2 N4 99.3(2) . . ?
N6 Cu2 N4 157.4(2) . . ?
N5 Cu2 O14 92.68(18) . . ?
OW1 Cu2 O14 101.41(18) . . ?
N6 Cu2 O14 92.6(2) . . ?
N4 Cu2 O14 99.4(2) . . ?
C22 N4 C26 118.4(6) . . ?
C22 N4 Cu2 128.2(5) . . ?
C26 N4 Cu2 113.1(5) . . ?
N4 C22 C23 122.8(7) . . ?
C22 C23 C24 119.3(8) . . ?
C25 C24 C23 118.8(7) . . ?
C24 C25 C26 118.6(7) . . ?
N4 C26 C25 122.1(7) . . ?
N4 C26 C27 114.6(6) . . ?
C25 C26 C27 123.3(7) . . ?
C31 N5 C27 122.5(6) . . ?
C31 N5 Cu2 119.5(5) . . ?
C27 N5 Cu2 117.8(5) . . ?
N5 C27 C28 120.1(7) . . ?
N5 C27 C26 112.7(6) . . ?
C28 C27 C26 127.1(7) . . ?
C27 C28 C29 117.8(8) . . ?
C30 C29 C28 121.1(7) . . ?
C29 C30 C31 118.4(8) . . ?
N5 C31 C30 120.1(7) . . ?
N5 C31 C32 112.3(6) . . ?
C30 C31 C32 127.6(7) . . ?
C36 N6 C32 119.0(7) . . ?
C36 N6 Cu2 126.5(5) . . ?
C32 N6 Cu2 114.1(5) . . ?
N6 C32 C33 120.9(7) . . ?
N6 C32 C31 113.7(6) . . ?
C33 C32 C31 125.3(7) . . ?
C34 C33 C32 118.6(8) . . ?
C35 C34 C33 120.6(8) . . ?
C34 C35 C36 119.6(8) . . ?
N6 C36 C35 121.3(7) . . ?

_refine_diff_density_max         1.735
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.184


# start Validation Reply Form
_vrf_PLAT027_shelx               
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 65.00 Degree
RESPONSE: when theta was above 50 deg, I/sigma(I) ratio was below 3. theta_full = 65 deg was choosen balancing 
resolution limit and reflections' intensity
;
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.910 Why?
RESPONSE: Reflections' intensity at high theta value was not so good. Average completness was about 96% up to
50 deg (limit for I/sigma(I) > 3) 
;
_vrf_PLAT305_shelx               
;
PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??) Hw2 Check
RESPONSE: Hw2 is not isolated. It is shared between the water oxygen OW1 and the symmetry related O22 phosphate oxygen, 
it is equidistant from both oxygens and defines a three-centre four-electrons bond
;
_vrf_PLAT415_shelx               
;
PROBLEM: Short Inter D-H..H-X Hw1 ..Hw2 . 1.69 Ang.
RESPONSE: Hw2 and Hw1 belong to the same water molecule
;
# end Validation Reply Form
#===END
