# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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 2237482'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2023-01-22 deposited with the CCDC.	2023-04-05 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            'C24 H46 Cl5 N5 O4'
_chemical_formula_weight         645.91

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'
Cl Cl 0.3639 0.7018 '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'

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

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

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

_cell_length_a                   7.688(1)
_cell_length_b                   13.744(2)
_cell_length_c                   15.732(2)
_cell_angle_alpha                80.34(1)
_cell_angle_beta                 79.66(1)
_cell_angle_gamma                79.50(1)
_cell_volume                     1592.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293
_cell_measurement_reflns_used    1578
_cell_measurement_theta_min      4.681
_cell_measurement_theta_max      49.701

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_F_000             684
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    4.455
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10612
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.681
_diffrn_reflns_theta_max         49.701
_diffrn_reflns_theta_full        49.701
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_point_group_measured_fraction_full 0.956
_reflns_number_total             3096
_reflns_number_gt                2284
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR97 (Altomare 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+(0.0960P)²+0.9912P] 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         3096
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1594
_refine_ls_wR_factor_gt          0.1428
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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
Cl1 Cl 0.9271(2) 0.17759(10) 0.80731(9) 0.0290(5) Uani 1 1 d . . . . .
Cl2 Cl 0.6169(2) 0.55495(11) 0.82331(9) 0.0342(5) Uani 1 1 d . . . . .
Cl3 Cl 1.1219(2) 0.49898(11) 0.60679(10) 0.0345(5) Uani 1 1 d . . . . .
Cl4 Cl 0.3432(2) 0.93382(11) 0.92328(10) 0.0379(5) Uani 1 1 d . . . . .
Cl5 Cl 0.7298(2) 0.01093(11) 0.63543(11) 0.0394(5) Uani 1 1 d . . . . .
N1 N 0.2583(6) 0.5020(3) 0.9940(3) 0.0243(13) Uani 1 1 d . . . . .
H1 H 0.2999 0.4942 1.0423 0.029 Uiso 1 1 calc R U . . .
N2 N 0.5774(6) 0.1840(3) 0.7359(3) 0.0258(13) Uani 1 1 d . . . . .
H2A H 0.6633 0.1878 0.7659 0.031 Uiso 1 1 calc R U . . .
H2B H 0.6079 0.1274 0.7128 0.031 Uiso 1 1 calc R U . . .
N3 N 0.7006(6) 0.5300(3) 0.6240(3) 0.0226(12) Uani 1 1 d . . . . .
H3A H 0.6879 0.5336 0.6808 0.027 Uiso 1 1 calc R U . . .
H3B H 0.8172 0.5200 0.6037 0.027 Uiso 1 1 calc R U . . .
N4 N 0.4409(6) 0.8378(3) 0.6269(3) 0.0261(13) Uani 1 1 d . . . . .
H4A H 0.3689 0.7926 0.6320 0.031 Uiso 1 1 calc R U . . .
H4B H 0.4787 0.8327 0.6780 0.031 Uiso 1 1 calc R U . . .
N5 N 0.0214(6) 0.9429(3) 0.8279(3) 0.0262(13) Uani 1 1 d . . . . .
H5A H -0.0295 1.0065 0.8177 0.031 Uiso 1 1 calc R U . . .
H5B H 0.1057 0.9402 0.8607 0.031 Uiso 1 1 calc R U . . .
C1 C 0.3605(8) 0.2659(4) 0.8503(4) 0.0215(15) Uani 1 1 d . . . . .
C2 C 0.4336(8) 0.2581(4) 0.9280(4) 0.0268(16) Uani 1 1 d . . . . .
H2 H 0.5058 0.1991 0.9464 0.032 Uiso 1 1 calc R U . . .
C3 C 0.4015(8) 0.3343(4) 0.9766(4) 0.0255(16) Uani 1 1 d . . . . .
H3 H 0.4504 0.3277 1.0276 0.031 Uiso 1 1 calc R U . . .
C4 C 0.2914(8) 0.4243(4) 0.9475(4) 0.0219(15) Uani 1 1 d . . . . .
C5 C 0.1612(8) 0.5922(4) 0.9673(4) 0.0215(15) Uani 1 1 d . . . . .
C6 C 0.1362(8) 0.6707(4) 1.0185(4) 0.0289(16) Uani 1 1 d . . . . .
H6 H 0.1811 0.6607 1.0709 0.035 Uiso 1 1 calc R U . . .
C7 C 0.0443(8) 0.7617(5) 0.9889(4) 0.0280(16) Uani 1 1 d . . . . .
H7 H 0.0279 0.8137 1.0219 0.034 Uiso 1 1 calc R U . . .
C8 C -0.0269(7) 0.7789(4) 0.9092(4) 0.0217(15) Uani 1 1 d . . . . .
C9 C -0.0085(7) 0.7011(4) 0.8624(4) 0.0239(15) Uani 1 1 d . . . . .
H9 H -0.0615 0.7105 0.8123 0.029 Uiso 1 1 calc R U . . .
C10 C 0.0899(7) 0.6062(4) 0.8892(4) 0.0200(15) Uani 1 1 d . . . . .
C11 C 0.1161(7) 0.5261(4) 0.8420(4) 0.0236(15) Uani 1 1 d . . . . .
H11 H 0.0654 0.5336 0.7914 0.028 Uiso 1 1 calc R U . . .
C12 C 0.2176(8) 0.4345(4) 0.8696(4) 0.0228(15) Uani 1 1 d . . . . .
C13 C 0.2523(8) 0.3511(4) 0.8234(4) 0.0241(15) Uani 1 1 d . . . . .
H13 H 0.2000 0.3548 0.7738 0.029 Uiso 1 1 calc R U . . .
C14 C 0.4053(8) 0.1782(4) 0.7992(4) 0.0264(16) Uani 1 1 d . . . . .
H14A H 0.4177 0.1163 0.8393 0.032 Uiso 1 1 calc R U . . .
H14B H 0.3084 0.1781 0.7673 0.032 Uiso 1 1 calc R U . . .
C15 C 0.5729(8) 0.2691(4) 0.6633(4) 0.0269(16) Uani 1 1 d . . . . .
H15A H 0.4496 0.2933 0.6551 0.032 Uiso 1 1 calc R U . . .
H15B H 0.6369 0.2454 0.6099 0.032 Uiso 1 1 calc R U . . .
C16 C 0.6553(8) 0.3544(4) 0.6802(4) 0.0289(16) Uani 1 1 d . . . . .
H16A H 0.6041 0.3723 0.7376 0.035 Uiso 1 1 calc R U . . .
H16B H 0.7833 0.3341 0.6788 0.035 Uiso 1 1 calc R U . . .
C17 C 0.6197(8) 0.4431(4) 0.6115(4) 0.0287(16) Uani 1 1 d . . . . .
H17A H 0.6688 0.4240 0.5543 0.034 Uiso 1 1 calc R U . . .
H17B H 0.4915 0.4630 0.6136 0.034 Uiso 1 1 calc R U . . .
C18 C 0.6171(8) 0.6258(4) 0.5791(4) 0.0276(16) Uani 1 1 d . . . . .
H18A H 0.4918 0.6393 0.6041 0.033 Uiso 1 1 calc R U . . .
H18B H 0.6233 0.6203 0.5179 0.033 Uiso 1 1 calc R U . . .
C19 C 0.7082(8) 0.7117(4) 0.5867(4) 0.0247(15) Uani 1 1 d . . . . .
H19A H 0.8253 0.7055 0.5508 0.030 Uiso 1 1 calc R U . . .
H19B H 0.7256 0.7081 0.6467 0.030 Uiso 1 1 calc R U . . .
C20 C 0.6013(8) 0.8129(4) 0.5585(4) 0.0308(17) Uani 1 1 d . . . . .
H20A H 0.6772 0.8640 0.5494 0.037 Uiso 1 1 calc R U . . .
H20B H 0.5612 0.8118 0.5036 0.037 Uiso 1 1 calc R U . . .
C21 C 0.3352(8) 0.9393(4) 0.6086(4) 0.0279(16) Uani 1 1 d . . . . .
H21A H 0.2494 0.9370 0.5709 0.033 Uiso 1 1 calc R U . . .
H21B H 0.4148 0.9855 0.5783 0.033 Uiso 1 1 calc R U . . .
C22 C 0.2373(8) 0.9760(4) 0.6923(4) 0.0279(16) Uani 1 1 d . . . . .
H22A H 0.1721 1.0426 0.6786 0.034 Uiso 1 1 calc R U . . .
H22B H 0.3242 0.9805 0.7287 0.034 Uiso 1 1 calc R U . . .
C23 C 0.1073(8) 0.9083(4) 0.7430(4) 0.0281(16) Uani 1 1 d . . . . .
H23A H 0.0155 0.9072 0.7084 0.034 Uiso 1 1 calc R U . . .
H23B H 0.1708 0.8407 0.7539 0.034 Uiso 1 1 calc R U . . .
C24 C -0.1175(8) 0.8824(4) 0.8779(4) 0.0302(16) Uani 1 1 d . . . . .
H24A H -0.2030 0.8781 0.8407 0.036 Uiso 1 1 calc R U . . .
H24B H -0.1818 0.9143 0.9274 0.036 Uiso 1 1 calc R U . . .
OW1 O 0.5454(6) 0.7922(3) 0.7912(3) 0.0476(13) Uani 1 1 d . . . . .
OW2 O 0.8669(6) 0.7396(3) 0.3727(3) 0.0442(12) Uani 1 1 d . . . . .
OW3 O 0.1759(5) 0.7256(3) 0.6145(3) 0.0478(13) Uani 1 1 d . . . . .
OW4 O 1.0336(7) 0.8399(4) 0.4770(3) 0.0798(18) Uani 1 1 d . . . . .


_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 C4 1.355(7) . ?
N1 C5 1.368(7) . ?
N2 C15 1.491(7) . ?
N2 C14 1.513(7) . ?
N3 C18 1.479(6) . ?
N3 C17 1.499(6) . ?
N4 C21 1.492(7) . ?
N4 C20 1.514(7) . ?
N5 C23 1.493(7) . ?
N5 C24 1.501(7) . ?
C1 C13 1.360(7) . ?
C1 C2 1.415(8) . ?
C1 C14 1.513(7) . ?
C2 C3 1.359(7) . ?
C3 C4 1.422(8) . ?
C4 C12 1.416(8) . ?
C5 C10 1.404(7) . ?
C5 C6 1.419(8) . ?
C6 C7 1.371(8) . ?
C7 C8 1.425(8) . ?
C8 C9 1.370(7) . ?
C8 C24 1.509(7) . ?
C9 C10 1.422(8) . ?
C10 C11 1.394(7) . ?
C11 C12 1.401(7) . ?
C12 C13 1.418(7) . ?
C15 C16 1.510(7) . ?
C16 C17 1.508(8) . ?
C18 C19 1.510(7) . ?
C19 C20 1.521(7) . ?
C21 C22 1.511(8) . ?
C22 C23 1.518(8) . ?

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
C4 N1 C5 122.7(5) . . ?
C15 N2 C14 116.0(5) . . ?
C18 N3 C17 112.4(4) . . ?
C21 N4 C20 114.8(4) . . ?
C23 N5 C24 113.5(4) . . ?
C13 C1 C2 119.6(5) . . ?
C13 C1 C14 121.7(5) . . ?
C2 C1 C14 118.7(5) . . ?
C3 C2 C1 122.0(5) . . ?
C2 C3 C4 118.4(5) . . ?
N1 C4 C12 119.3(5) . . ?
N1 C4 C3 119.9(5) . . ?
C12 C4 C3 120.8(5) . . ?
N1 C5 C10 119.7(5) . . ?
N1 C5 C6 119.3(5) . . ?
C10 C5 C6 121.0(5) . . ?
C7 C6 C5 118.4(6) . . ?
C6 C7 C8 122.0(5) . . ?
C9 C8 C7 118.8(5) . . ?
C9 C8 C24 121.9(5) . . ?
C7 C8 C24 119.2(5) . . ?
C8 C9 C10 121.1(5) . . ?
C11 C10 C5 118.7(5) . . ?
C11 C10 C9 122.8(5) . . ?
C5 C10 C9 118.5(5) . . ?
C10 C11 C12 121.0(5) . . ?
C11 C12 C4 118.5(5) . . ?
C11 C12 C13 123.6(5) . . ?
C4 C12 C13 117.8(5) . . ?
C1 C13 C12 121.2(5) . . ?
N2 C14 C1 110.8(4) . . ?
N2 C15 C16 112.7(5) . . ?
C17 C16 C15 109.4(5) . . ?
N3 C17 C16 111.9(4) . . ?
N3 C18 C19 112.0(5) . . ?
C18 C19 C20 112.5(5) . . ?
N4 C20 C19 110.7(5) . . ?
N4 C21 C22 110.8(5) . . ?
C21 C22 C23 112.8(5) . . ?
N5 C23 C22 111.5(4) . . ?
N5 C24 C8 109.2(5) . . ?

_refine_diff_density_max         0.588
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.082



# start Validation Reply Form
_vrf_THETM01_shelx               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: reflections were collected up to 2\^I? = 100 deg (1.0 A), due to a significant
lowering of intensity with increasing theta value. However, the actual reached resolution and the
reflections/refined parameters ratio (9) ensure that overall geometry of the ligand and intermolecular
distances are confidently defined
;
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.956 Why?
RESPONSE: reflections were collected up to 2\^I? = 100 deg (1.0 A), due to a significant
lowering of intensity with increasing theta value. However, the actual reached resolution and the
reflections/refined parameters ratio (9) ensure that overall geometry of the ligand and intermolecular
distances are confidently defined
;
_vrf_PLAT043_shelx               
;
PROBLEM: Calculated and Reported Mol. Weight Differ by .. 8.07 Check
RESPONSE: Water hydrogens were not localized in the DeltaF map and not introduced in the calculation
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow1 Check
RESPONSE: The isolated oxygen atoms belong to cocrystallized water molecules. The hydrogen atoms
for these water molecules have not been localized in the Fourier difference map
;
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact Ow3 ..Ow4 . 2.72 Ang.
RESPONSE: the atoms involved in these short contacts are water oxygen atoms and the contacts can be interpreted
as H-bonding contacts
;
# 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 2237483'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2023-01-22 deposited with the CCDC.	2023-04-05 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            'C24 H46 Br5 N5 O4'
_chemical_formula_weight         868.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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'

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

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

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

_cell_length_a                   7.806(1)
_cell_length_b                   13.978(1)
_cell_length_c                   16.174(2)
_cell_angle_alpha                80.313(8)
_cell_angle_beta                 78.81(1)
_cell_angle_gamma                78.280(9)
_cell_volume                     1679.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293
_cell_measurement_reflns_used    1398
_cell_measurement_theta_min      4.582
_cell_measurement_theta_max      49.635

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    7.533
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11083
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.582
_diffrn_reflns_theta_max         49.635
_diffrn_reflns_theta_full        49.635
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 0.959
_reflns_number_total             3257
_reflns_number_gt                2622
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR97 (Altomare 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+(0.0998P)²+5.7958P] 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         3257
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1609
_refine_ls_wR_factor_gt          0.1471
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
Br1 Br -0.08051(14) 0.68271(7) 0.31085(7) 0.0301(4) Uani 1 1 d . . . . .
Br2 Br 1.12450(15) -0.00379(8) 0.10496(7) 0.0375(4) Uani 1 1 d . . . . .
Br3 Br 0.61790(15) 0.05264(8) 0.32476(7) 0.0354(4) Uani 1 1 d . . . . .
Br4 Br 0.34066(16) 0.43914(8) 0.42814(7) 0.0400(4) Uani 1 1 d . . . . .
Br5 Br 0.73504(16) -0.49071(8) 0.12985(8) 0.0428(4) Uani 1 1 d . . . . .
N1 N 0.2511(10) 0.0035(6) 0.4877(5) 0.028(2) Uani 1 1 d . . . . .
H1 H 0.2927 -0.0046 0.5344 0.034 Uiso 1 1 calc R U . . .
N2 N 0.5672(11) -0.3088(5) 0.2322(5) 0.028(2) Uani 1 1 d . . . . .
H2A H 0.6519 -0.3047 0.2605 0.033 Uiso 1 1 calc R U . . .
H2B H 0.5994 -0.3651 0.2100 0.033 Uiso 1 1 calc R U . . .
N3 N 0.6910(11) 0.0292(5) 0.1209(5) 0.027(2) Uani 1 1 d . . . . .
H3A H 0.6864 0.0307 0.1761 0.033 Uiso 1 1 calc R U . . .
H3B H 0.8047 0.0201 0.0969 0.033 Uiso 1 1 calc R U . . .
N4 N 0.4312(10) 0.3351(5) 0.1303(5) 0.026(2) Uani 1 1 d . . . . .
H4A H 0.3607 0.2906 0.1380 0.031 Uiso 1 1 calc R U . . .
H4B H 0.4723 0.3311 0.1786 0.031 Uiso 1 1 calc R U . . .
N5 N 0.0135(10) 0.4403(5) 0.3297(5) 0.029(2) Uani 1 1 d . . . . .
H5A H -0.0396 0.5026 0.3187 0.034 Uiso 1 1 calc R U . . .
H5B H 0.0945 0.4395 0.3618 0.034 Uiso 1 1 calc R U . . .
C1 C 0.3539(14) -0.2303(7) 0.3470(6) 0.028(3) Uani 1 1 d . . . . .
C2 C 0.4272(14) -0.2376(8) 0.4229(7) 0.033(3) Uani 1 1 d . . . . .
H2 H 0.5019 -0.2953 0.4399 0.040 Uiso 1 1 calc R U . . .
C3 C 0.3910(13) -0.1634(7) 0.4699(6) 0.027(3) Uani 1 1 d . . . . .
H3 H 0.4361 -0.1714 0.5203 0.033 Uiso 1 1 calc R U . . .
C4 C 0.2852(12) -0.0738(7) 0.4435(6) 0.022(2) Uani 1 1 d . . . . .
C5 C 0.1560(12) 0.0930(7) 0.4638(6) 0.025(3) Uani 1 1 d . . . . .
C6 C 0.1302(13) 0.1710(7) 0.5134(6) 0.029(3) Uani 1 1 d . . . . .
H6 H 0.1720 0.1602 0.5649 0.034 Uiso 1 1 calc R U . . .
C7 C 0.0440(14) 0.2616(7) 0.4850(7) 0.035(3) Uani 1 1 d . . . . .
H7 H 0.0349 0.3138 0.5154 0.042 Uiso 1 1 calc R U . . .
C8 C -0.0329(13) 0.2784(7) 0.4095(6) 0.028(3) Uani 1 1 d . . . . .
C9 C -0.0134(13) 0.2016(7) 0.3620(6) 0.027(3) Uani 1 1 d . . . . .
H9 H -0.0627 0.2119 0.3126 0.032 Uiso 1 1 calc R U . . .
C10 C 0.0814(13) 0.1081(6) 0.3888(6) 0.023(2) Uani 1 1 d . . . . .
C11 C 0.1080(12) 0.0287(7) 0.3429(6) 0.025(3) Uani 1 1 d . . . . .
H11 H 0.0588 0.0365 0.2937 0.030 Uiso 1 1 calc R U . . .
C12 C 0.2078(12) -0.0628(7) 0.3699(6) 0.022(2) Uani 1 1 d . . . . .
C13 C 0.2444(13) -0.1446(7) 0.3234(6) 0.030(3) Uani 1 1 d . . . . .
H13 H 0.1922 -0.1395 0.2754 0.036 Uiso 1 1 calc R U . . .
C14 C 0.4016(13) -0.3152(7) 0.2948(6) 0.028(3) Uani 1 1 d . . . . .
H14A H 0.4171 -0.3769 0.3325 0.034 Uiso 1 1 calc R U . . .
H14B H 0.3051 -0.3146 0.2648 0.034 Uiso 1 1 calc R U . . .
C15 C 0.5624(13) -0.2267(7) 0.1611(6) 0.028(3) Uani 1 1 d . . . . .
H15A H 0.4402 -0.2022 0.1536 0.034 Uiso 1 1 calc R U . . .
H15B H 0.6262 -0.2516 0.1092 0.034 Uiso 1 1 calc R U . . .
C16 C 0.6435(14) -0.1415(6) 0.1754(6) 0.028(3) Uani 1 1 d . . . . .
H16A H 0.5921 -0.1227 0.2312 0.034 Uiso 1 1 calc R U . . .
H16B H 0.7701 -0.1630 0.1741 0.034 Uiso 1 1 calc R U . . .
C17 C 0.6130(13) -0.0564(7) 0.1109(7) 0.030(3) Uani 1 1 d . . . . .
H17A H 0.4861 -0.0353 0.1128 0.035 Uiso 1 1 calc R U . . .
H17B H 0.6627 -0.0762 0.0553 0.035 Uiso 1 1 calc R U . . .
C18 C 0.6014(14) 0.1252(6) 0.0832(7) 0.030(3) Uani 1 1 d . . . . .
H18A H 0.4810 0.1388 0.1136 0.037 Uiso 1 1 calc R U . . .
H18B H 0.5952 0.1217 0.0245 0.037 Uiso 1 1 calc R U . . .
C19 C 0.6943(13) 0.2087(6) 0.0860(6) 0.027(3) Uani 1 1 d . . . . .
H19A H 0.8069 0.2013 0.0476 0.033 Uiso 1 1 calc R U . . .
H19B H 0.7190 0.2054 0.1430 0.033 Uiso 1 1 calc R U . . .
C20 C 0.5860(14) 0.3084(7) 0.0614(7) 0.034(3) Uani 1 1 d . . . . .
H20A H 0.6611 0.3581 0.0506 0.040 Uiso 1 1 calc R U . . .
H20B H 0.5422 0.3078 0.0093 0.040 Uiso 1 1 calc R U . . .
C21 C 0.3221(15) 0.4359(6) 0.1132(7) 0.035(3) Uani 1 1 d . . . . .
H21A H 0.2373 0.4333 0.0773 0.041 Uiso 1 1 calc R U . . .
H21B H 0.3990 0.4815 0.0830 0.041 Uiso 1 1 calc R U . . .
C22 C 0.2236(13) 0.4728(7) 0.1958(6) 0.027(3) Uani 1 1 d . . . . .
H22A H 0.3095 0.4805 0.2292 0.032 Uiso 1 1 calc R U . . .
H22B H 0.1525 0.5371 0.1827 0.032 Uiso 1 1 calc R U . . .
C23 C 0.1049(14) 0.4048(7) 0.2483(6) 0.033(3) Uani 1 1 d . . . . .
H23A H 0.0168 0.3984 0.2156 0.040 Uiso 1 1 calc R U . . .
H23B H 0.1753 0.3399 0.2603 0.040 Uiso 1 1 calc R U . . .
C24 C -0.1232(12) 0.3809(7) 0.3798(6) 0.025(3) Uani 1 1 d . . . . .
H24A H -0.1867 0.4127 0.4285 0.030 Uiso 1 1 calc R U . . .
H24B H -0.2082 0.3774 0.3445 0.030 Uiso 1 1 calc R U . . .
OW1 O 0.1630(9) 0.2264(5) 0.1249(5) 0.049(2) Uani 1 1 d . . . . .
OW2 O 0.1338(10) 0.7515(6) 0.1229(5) 0.054(2) Uani 1 1 d . . . . .
OW3 O 0.0435(14) 0.3233(8) -0.0187(6) 0.086(3) Uani 1 1 d . . . . .
OW4 O 0.5462(11) 0.2957(5) 0.2879(5) 0.053(2) Uani 1 1 d . . . . .


_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 C4 1.348(12) . ?
N1 C5 1.356(11) . ?
N2 C15 1.482(12) . ?
N2 C14 1.487(12) . ?
N3 C18 1.474(11) . ?
N3 C17 1.492(12) . ?
N4 C21 1.504(11) . ?
N4 C20 1.508(12) . ?
N5 C23 1.484(12) . ?
N5 C24 1.511(11) . ?
C1 C13 1.367(13) . ?
C1 C2 1.432(14) . ?
C1 C14 1.514(13) . ?
C2 C3 1.340(13) . ?
C3 C4 1.404(13) . ?
C4 C12 1.408(13) . ?
C5 C10 1.410(13) . ?
C5 C6 1.421(13) . ?
C6 C7 1.359(13) . ?
C7 C8 1.427(14) . ?
C8 C9 1.391(14) . ?
C8 C24 1.506(13) . ?
C9 C10 1.409(13) . ?
C10 C11 1.396(13) . ?
C11 C12 1.405(13) . ?
C12 C13 1.423(13) . ?
C15 C16 1.526(13) . ?
C16 C17 1.459(13) . ?
C18 C19 1.505(13) . ?
C19 C20 1.510(13) . ?
C21 C22 1.522(14) . ?
C22 C23 1.504(13) . ?

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
C4 N1 C5 124.6(8) . . ?
C15 N2 C14 117.7(8) . . ?
C18 N3 C17 114.1(7) . . ?
C21 N4 C20 115.1(7) . . ?
C23 N5 C24 114.5(7) . . ?
C13 C1 C2 117.8(9) . . ?
C13 C1 C14 122.2(9) . . ?
C2 C1 C14 120.0(9) . . ?
C3 C2 C1 121.8(9) . . ?
C2 C3 C4 120.3(9) . . ?
N1 C4 C3 121.8(9) . . ?
N1 C4 C12 117.8(8) . . ?
C3 C4 C12 120.3(9) . . ?
N1 C5 C10 119.3(9) . . ?
N1 C5 C6 120.7(9) . . ?
C10 C5 C6 120.0(8) . . ?
C7 C6 C5 119.3(9) . . ?
C6 C7 C8 121.5(10) . . ?
C9 C8 C7 119.5(9) . . ?
C9 C8 C24 121.2(9) . . ?
C7 C8 C24 119.2(9) . . ?
C8 C9 C10 119.8(9) . . ?
C11 C10 C9 122.4(9) . . ?
C11 C10 C5 117.8(8) . . ?
C9 C10 C5 119.8(9) . . ?
C10 C11 C12 121.0(9) . . ?
C11 C12 C4 119.3(9) . . ?
C11 C12 C13 123.0(9) . . ?
C4 C12 C13 117.6(8) . . ?
C1 C13 C12 122.1(9) . . ?
N2 C14 C1 111.6(8) . . ?
N2 C15 C16 113.1(8) . . ?
C17 C16 C15 111.6(8) . . ?
C16 C17 N3 114.2(8) . . ?
N3 C18 C19 112.9(8) . . ?
C18 C19 C20 112.5(8) . . ?
N4 C20 C19 111.6(8) . . ?
N4 C21 C22 110.8(8) . . ?
C23 C22 C21 113.2(8) . . ?
N5 C23 C22 112.6(8) . . ?
C8 C24 N5 109.7(7) . . ?

_refine_diff_density_max         0.828
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.158



# start Validation Reply Form
_vrf_THETM01_shelx               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: reflections were collected up to 2\^I? = 100 deg (1.0 A), due to a significant
lowering of intensity with increasing theta value. However, the actual reached resolution and the
reflections/refined parameters ratio (9.5) ensure that overall geometry of the ligand and intermolecular
distances are confidently defined. 
;
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.959 Why?
RESPONSE: reflections were collected up to 2\^I? = 100 deg (1.0 A), due to a significant
lowering of intensity with increasing theta value. However, the actual reached resolution and the
reflections/refined parameters ratio (9.5) ensure that overall geometry of the ligand and intermolecular
distances are confidently defined.
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow1 Check
RESPONSE: The isolated oxygen atoms belong to cocrystallized water molecules. The hydrogen atoms
for these water molecules have not been localized in the Fourier difference map 
;
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact Ow1 ..Ow3 . 2.71 Ang.
RESPONSE: the atoms involved in these short contacts are water oxygen atoms and the contacts can be interpreted
as H-bonding contacts
;
# 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_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2237484'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2023-01-22 deposited with the CCDC.	2023-04-05 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            'C24 H44 N10 O18'
_chemical_formula_weight         760.69

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'

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

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

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

_cell_length_a                   7.664(1)
_cell_length_b                   11.930(1)
_cell_length_c                   19.291(2)
_cell_angle_alpha                78.898(9)
_cell_angle_beta                 82.80(1)
_cell_angle_gamma                87.09(1)
_cell_volume                     1716.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293
_cell_measurement_reflns_used    1328
_cell_measurement_theta_min      4.7
_cell_measurement_theta_max      49.7

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_F_000             804
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    1.094
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11316
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.705
_diffrn_reflns_theta_max         49.700
_diffrn_reflns_theta_full        49.700
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             3329
_reflns_number_gt                1615
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR97 (Altomare 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+(0.1925P)²] 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         3329
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1530
_refine_ls_R_factor_gt           0.0944
_refine_ls_wR_factor_ref         0.2906
_refine_ls_wR_factor_gt          0.2592
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_restrained_S_all      0.989
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002

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 0.5016(9) 0.0539(5) 0.1040(3) 0.0567(17) Uani 1 1 d . . . . .
H1 H 0.5791 0.1060 0.0953 0.068 Uiso 1 1 calc R U . . .
N2 N -0.1084(10) 0.0788(6) 0.3425(4) 0.093(2) Uani 1 1 d . . . . .
H2A H -0.0114 0.1097 0.3507 0.111 Uiso 1 1 calc R U . . .
H2B H -0.1975 0.0998 0.3720 0.111 Uiso 1 1 calc R U . . .
N3 N 0.1580(10) -0.2528(6) 0.4127(3) 0.088(2) Uani 1 1 d . . . . .
H3A H 0.2306 -0.1952 0.4079 0.106 Uiso 1 1 calc R U . . .
H3B H 0.1423 -0.2621 0.3693 0.106 Uiso 1 1 calc R U . . .
N4 N 0.5426(11) -0.4819(6) 0.3096(4) 0.101(3) Uani 1 1 d . . . . .
H4A H 0.6415 -0.4875 0.3299 0.121 Uiso 1 1 calc R U . . .
H4B H 0.5422 -0.4151 0.2796 0.121 Uiso 1 1 calc R U . . .
N5 N 0.7590(8) -0.4459(5) 0.0843(3) 0.0632(19) Uani 1 1 d . . . . .
H5A H 0.7998 -0.5113 0.0718 0.076 Uiso 1 1 calc R U . . .
H5B H 0.8486 -0.4113 0.0957 0.076 Uiso 1 1 calc R U . . .
C1 C 0.0216(12) 0.1111(8) 0.2181(4) 0.065(2) Uani 1 1 d . . . . .
C2 C 0.1513(14) 0.1944(7) 0.2032(5) 0.070(2) Uani 1 1 d . . . . .
H2 H 0.1309 0.2616 0.2211 0.085 Uiso 1 1 calc R U . . .
C3 C 0.3005(13) 0.1788(6) 0.1645(4) 0.068(2) Uani 1 1 d . . . . .
H3 H 0.3821 0.2366 0.1535 0.082 Uiso 1 1 calc R U . . .
C4 C 0.3396(13) 0.0750(6) 0.1391(4) 0.061(2) Uani 1 1 d . . . . .
C5 C 0.5419(12) -0.0468(7) 0.0829(4) 0.058(2) Uani 1 1 d . . . . .
C6 C 0.7182(12) -0.0689(6) 0.0538(4) 0.067(2) Uani 1 1 d . . . . .
H6 H 0.8030 -0.0138 0.0484 0.080 Uiso 1 1 calc R U . . .
C7 C 0.7609(10) -0.1710(7) 0.0339(4) 0.064(2) Uani 1 1 d . . . . .
H7 H 0.8761 -0.1855 0.0155 0.077 Uiso 1 1 calc R U . . .
C8 C 0.6323(12) -0.2567(6) 0.0408(4) 0.057(2) Uani 1 1 d . . . . .
C9 C 0.4677(12) -0.2344(6) 0.0675(4) 0.063(2) Uani 1 1 d . . . . .
H9 H 0.3847 -0.2903 0.0717 0.075 Uiso 1 1 calc R U . . .
C10 C 0.4105(12) -0.1276(6) 0.0905(4) 0.056(2) Uani 1 1 d . . . . .
C11 C 0.2480(12) -0.1069(7) 0.1241(4) 0.063(2) Uani 1 1 d . . . . .
H11 H 0.1617 -0.1611 0.1299 0.076 Uiso 1 1 calc R U . . .
C12 C 0.2092(12) -0.0069(7) 0.1496(4) 0.058(2) Uani 1 1 d . . . . .
C13 C 0.0474(12) 0.0146(7) 0.1904(4) 0.065(2) Uani 1 1 d . . . . .
H13 H -0.0417 -0.0381 0.1981 0.078 Uiso 1 1 calc R U . . .
C14 C -0.1428(12) 0.1247(7) 0.2672(5) 0.085(3) Uani 1 1 d . . . . .
H14A H -0.2373 0.0835 0.2553 0.102 Uiso 1 1 calc R U . . .
H14B H -0.1781 0.2049 0.2620 0.102 Uiso 1 1 calc R U . . .
C15 C -0.0863(14) -0.0484(8) 0.3584(5) 0.103(3) Uani 1 1 d . . . . .
H15A H -0.1913 -0.0825 0.3491 0.124 Uiso 1 1 calc R U . . .
H15B H 0.0121 -0.0716 0.3270 0.124 Uiso 1 1 calc R U . . .
C16 C -0.0545(13) -0.0918(9) 0.4341(5) 0.101(3) Uani 1 1 d . . . . .
H16A H -0.1569 -0.0734 0.4653 0.121 Uiso 1 1 calc R U . . .
H16B H 0.0448 -0.0529 0.4443 0.121 Uiso 1 1 calc R U . . .
C17 C -0.0179(14) -0.2196(8) 0.4499(6) 0.111(3) Uani 1 1 d . . . . .
H17A H -0.0190 -0.2450 0.5008 0.133 Uiso 1 1 calc R U . . .
H17B H -0.1107 -0.2581 0.4347 0.133 Uiso 1 1 calc R U . . .
C18 C 0.2466(16) -0.3608(9) 0.4501(6) 0.133(4) Uani 1 1 d . . . . .
H18A H 0.2719 -0.3491 0.4961 0.160 Uiso 1 1 calc R U . . .
H18B H 0.1652 -0.4230 0.4582 0.160 Uiso 1 1 calc R U . . .
C19 C 0.4060(14) -0.3934(9) 0.4112(5) 0.108(4) Uani 1 1 d . . . . .
H19A H 0.4880 -0.4230 0.4452 0.130 Uiso 1 1 calc R U . . .
H19B H 0.4559 -0.3248 0.3815 0.130 Uiso 1 1 calc R U . . .
C20 C 0.3969(14) -0.4823(9) 0.3633(6) 0.121(4) Uani 1 1 d . . . . .
H20A H 0.3898 -0.5578 0.3930 0.145 Uiso 1 1 calc R U . . .
H20B H 0.2898 -0.4679 0.3407 0.145 Uiso 1 1 calc R U . . .
C21 C 0.5429(13) -0.5763(7) 0.2681(5) 0.090(3) Uani 1 1 d . . . . .
H21A H 0.4302 -0.5766 0.2503 0.108 Uiso 1 1 calc R U . . .
H21B H 0.5606 -0.6493 0.2990 0.108 Uiso 1 1 calc R U . . .
C22 C 0.6898(13) -0.5595(7) 0.2057(5) 0.091(3) Uani 1 1 d . . . . .
H22A H 0.7952 -0.5337 0.2203 0.109 Uiso 1 1 calc R U . . .
H22B H 0.7178 -0.6308 0.1892 0.109 Uiso 1 1 calc R U . . .
C23 C 0.6237(12) -0.4708(7) 0.1473(5) 0.079(3) Uani 1 1 d . . . . .
H23A H 0.5189 -0.4979 0.1331 0.094 Uiso 1 1 calc R U . . .
H23B H 0.5918 -0.4010 0.1652 0.094 Uiso 1 1 calc R U . . .
C24 C 0.6846(10) -0.3714(6) 0.0228(4) 0.064(2) Uani 1 1 d . . . . .
H24A H 0.5828 -0.4068 0.0118 0.076 Uiso 1 1 calc R U . . .
H24B H 0.7718 -0.3624 -0.0188 0.076 Uiso 1 1 calc R U . . .
N6 N 0.6087(17) -0.1920(11) 0.2439(5) 0.112(3) Uani 1 1 d . . . . .
O61 O 0.4668(14) -0.2355(7) 0.2523(4) 0.140(3) Uani 1 1 d . . . . .
O62 O 0.6225(9) -0.0902(7) 0.2410(3) 0.113(2) Uani 1 1 d . . . . .
O63 O 0.7291(14) -0.2626(9) 0.2379(6) 0.187(5) Uani 1 1 d . . . . .
N7 N -0.4503(14) 0.1693(9) 0.4494(7) 0.118(3) Uani 1 1 d . . . . .
O71 O -0.4722(10) 0.1418(7) 0.3943(4) 0.118(3) Uani 1 1 d . . . . .
O72 O -0.3054(13) 0.1375(7) 0.4770(4) 0.140(3) Uani 1 1 d . . . . .
O73 O -0.5503(12) 0.2266(9) 0.4810(5) 0.159(3) Uani 1 1 d . . . . .
N8 N 0.9189(19) -0.5715(11) 0.3799(7) 0.136(4) Uani 1 1 d . . . . .
O81 O 0.8302(12) -0.4838(9) 0.3844(6) 0.169(4) Uani 1 1 d . . . . .
O82 O 1.0517(13) -0.5971(9) 0.4109(7) 0.187(5) Uani 1 1 d . . . . .
O83 O 0.8646(14) -0.6442(9) 0.3495(4) 0.162(4) Uani 1 1 d . . . . .
N9 N 1.1390(13) -0.4280(8) 0.1606(6) 0.098(3) Uani 1 1 d . . . . .
O91 O 1.2332(10) -0.4107(7) 0.2043(4) 0.121(3) Uani 1 1 d . . . . .
O92 O 1.0315(9) -0.3533(5) 0.1373(4) 0.102(2) Uani 1 1 d . . . . .
O93 O 1.1517(10) -0.5181(7) 0.1364(5) 0.139(3) Uani 1 1 d . . . . .
N10 N 0.7930(13) -0.7210(8) 0.0575(4) 0.071(2) Uani 1 1 d . . . . .
O101 O 0.8234(8) -0.8205(5) 0.0565(3) 0.098(2) Uani 1 1 d . . . . .
O102 O 0.6442(10) -0.6876(6) 0.0734(4) 0.107(2) Uani 1 1 d . . . . .
O103 O 0.9072(9) -0.6506(5) 0.0421(4) 0.101(2) Uani 1 1 d . . . . .
OW1 O 0.1730(10) 0.1956(6) 0.3704(4) 0.135(3) Uani 1 1 d . . . . .
OW2 O 0.0630(9) -0.2647(6) 0.2803(3) 0.128(3) Uani 1 1 d . . . . .
OW3 O 0.3569(10) -0.0528(6) 0.3493(4) 0.156(3) Uani 1 1 d . . . . .


_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 C5 1.351(8) . ?
N1 C4 1.373(9) . ?
N2 C15 1.495(9) . ?
N2 C14 1.502(9) . ?
N3 C17 1.517(10) . ?
N3 C18 1.522(11) . ?
N4 C20 1.424(11) . ?
N4 C21 1.502(10) . ?
N5 C23 1.489(9) . ?
N5 C24 1.495(8) . ?
C1 C13 1.356(10) . ?
C1 C2 1.407(11) . ?
C1 C14 1.500(11) . ?
C2 C3 1.310(10) . ?
C3 C4 1.423(10) . ?
C4 C12 1.402(10) . ?
C5 C10 1.404(10) . ?
C5 C6 1.429(10) . ?
C6 C7 1.358(9) . ?
C7 C8 1.433(10) . ?
C8 C9 1.336(9) . ?
C8 C24 1.498(9) . ?
C9 C10 1.458(10) . ?
C10 C11 1.364(10) . ?
C11 C12 1.381(10) . ?
C12 C13 1.422(10) . ?
C15 C16 1.499(11) . ?
C16 C17 1.515(11) . ?
C18 C19 1.428(12) . ?
C19 C20 1.545(12) . ?
C21 C22 1.532(11) . ?
C22 C23 1.508(10) . ?
N6 O61 1.208(10) . ?
N6 O62 1.215(10) . ?
N6 O63 1.227(11) . ?
N7 O73 1.189(10) . ?
N7 O71 1.206(11) . ?
N7 O72 1.299(11) . ?
N8 O81 1.230(12) . ?
N8 O83 1.250(12) . ?
N8 O82 1.241(13) . ?
N9 O91 1.227(10) . ?
N9 O92 1.241(9) . ?
N9 O93 1.246(9) . ?
N10 O101 1.201(8) . ?
N10 O102 1.211(8) . ?
N10 O103 1.213(8) . ?

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
C5 N1 C4 121.5(7) . . ?
C15 N2 C14 113.0(6) . . ?
C17 N3 C18 115.4(7) . . ?
C20 N4 C21 114.1(8) . . ?
C23 N5 C24 111.3(6) . . ?
C13 C1 C2 120.1(8) . . ?
C13 C1 C14 119.0(9) . . ?
C2 C1 C14 120.8(8) . . ?
C3 C2 C1 120.9(8) . . ?
C2 C3 C4 121.1(9) . . ?
N1 C4 C12 119.5(7) . . ?
N1 C4 C3 121.4(9) . . ?
C12 C4 C3 119.1(9) . . ?
N1 C5 C10 119.4(8) . . ?
N1 C5 C6 119.0(8) . . ?
C10 C5 C6 121.6(7) . . ?
C7 C6 C5 119.4(8) . . ?
C6 C7 C8 121.4(8) . . ?
C9 C8 C7 118.5(7) . . ?
C9 C8 C24 120.9(8) . . ?
C7 C8 C24 120.5(8) . . ?
C8 C9 C10 123.8(8) . . ?
C11 C10 C5 119.5(7) . . ?
C11 C10 C9 124.9(8) . . ?
C5 C10 C9 115.3(8) . . ?
C10 C11 C12 121.2(8) . . ?
C11 C12 C4 118.6(8) . . ?
C11 C12 C13 123.4(9) . . ?
C4 C12 C13 117.8(8) . . ?
C1 C13 C12 120.7(8) . . ?
C1 C14 N2 109.2(6) . . ?
C16 C15 N2 111.8(7) . . ?
C15 C16 C17 112.7(8) . . ?
N3 C17 C16 112.2(8) . . ?
C19 C18 N3 113.8(9) . . ?
C18 C19 C20 118.2(10) . . ?
N4 C20 C19 114.2(9) . . ?
N4 C21 C22 110.2(8) . . ?
C23 C22 C21 107.1(7) . . ?
N5 C23 C22 111.5(7) . . ?
N5 C24 C8 109.8(6) . . ?
O61 N6 O62 121.7(12) . . ?
O61 N6 O63 111.5(12) . . ?
O62 N6 O63 126.7(13) . . ?
O73 N7 O71 125.1(12) . . ?
O73 N7 O72 115.9(12) . . ?
O71 N7 O72 119.0(10) . . ?
O81 N8 O83 119.5(15) . . ?
O81 N8 O82 122.5(15) . . ?
O83 N8 O82 117.6(14) . . ?
O91 N9 O92 120.2(9) . . ?
O91 N9 O93 121.9(11) . . ?
O92 N9 O93 117.8(11) . . ?
O101 N10 O102 120.1(9) . . ?
O101 N10 O103 122.1(9) . . ?
O102 N10 O103 117.7(8) . . ?

_refine_diff_density_max         0.464
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.077



# start Validation Reply Form
_vrf_THETM01_shelx               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: reflections were collected up to 2\^I? = 100 deg (1.0 A), due to a significant
lowering of intensity with increasing theta value.
;
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.954 Why?
RESPONSE: reflections were collected up to 2\^I? = 100 deg (1.0 A), due to a significant
lowering of intensity with increasing theta value.
;
_vrf_PLAT088_shelx               
;
PROBLEM: Poor Data / Parameter Ratio .................... 7.10 Note
RESPONSE: Crystallization attempts only afforded low quality crystals. Reflections were collected up 
to 2\^I? = 100 deg (1.0 A), due to a significant lowering of intensity with increasing theta value.
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow1 Check
RESPONSE: The isolated oxygen atoms belong to cocrystallized water molecules. The hydrogen atoms
for these water molecules have not been localized in the Fourier difference map
;
_vrf_PLAT340_shelx               
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01273 Ang.
RESPONSE: the overall low quality of the crystals and the low number of observed
data explain the high e.s.d. on C-C bonds
;
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact Ow1 ..O82 . 2.81 Ang.
RESPONSE: the atoms involved in these short contacts are water oxygen atoms and the contacts can be interpreted
as H-bonding contacts
;
# 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_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2237485'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2023-01-22 deposited with the CCDC.	2023-04-05 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            'C24 H62 N5 O32 P7'
_chemical_formula_weight         1149.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.961(2)
_cell_length_b                   13.583(2)
_cell_length_c                   15.357(2)
_cell_angle_alpha                85.66(1)
_cell_angle_beta                 75.95(1)
_cell_angle_gamma                69.72(1)
_cell_volume                     2270.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293
_cell_measurement_reflns_used    1480
_cell_measurement_theta_min      4.3
_cell_measurement_theta_max      58.0

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_F_000             1204
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.520
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16499
_diffrn_reflns_av_unetI/netI     0.1790
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.349
_diffrn_reflns_theta_max         58.098
_diffrn_reflns_theta_full        58.098
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measured_fraction_theta_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_point_group_measured_fraction_full 0.909
_reflns_number_total             5765
_reflns_number_gt                2711
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR97 (Altomare 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+(0.0937P)²] 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         5765
_refine_ls_number_parameters     640
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.0739
_refine_ls_wR_factor_ref         0.1945
_refine_ls_wR_factor_gt          0.1748
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.9306(2) 0.00889(18) 0.14384(15) 0.0214(6) Uani 1 1 d . . . . .
O11 O 0.8470(5) 0.0642(4) 0.0768(4) 0.0228(15) Uani 1 1 d . . . . .
O12 O 1.0574(5) -0.0520(4) 0.0918(3) 0.0197(14) Uani 1 1 d . . . . .
O13 O 0.9234(5) 0.0904(4) 0.2090(3) 0.0215(15) Uani 1 1 d . . . . .
O14 O 0.8721(5) -0.0739(4) 0.1963(4) 0.0274(16) Uani 1 1 d . . . . .
P2 P 0.9215(2) 0.18261(19) -0.57753(16) 0.0245(7) Uani 1 1 d . . . . .
O21 O 0.9112(5) 0.2821(4) -0.6303(4) 0.0420(19) Uani 1 1 d . . . . .
O24 O 0.9965(5) 0.1683(5) -0.5089(4) 0.0417(19) Uani 1 1 d . . . . .
O23 O 0.9830(5) 0.0864(4) -0.6447(4) 0.0293(16) Uani 1 1 d . . . . .
O22 O 0.7918(5) 0.1833(4) -0.5272(4) 0.0295(16) Uani 1 1 d . . . . .
P3 P 0.5717(2) 0.47805(19) -0.13964(17) 0.0272(7) Uani 1 1 d . . . . .
O34 O 0.6677(5) 0.5121(4) -0.2130(4) 0.0328(17) Uani 1 1 d . . . . .
O33 O 0.6313(5) 0.4050(4) -0.0718(4) 0.0268(16) Uani 1 1 d . . . . .
O32 O 0.4764(5) 0.5829(4) -0.0927(4) 0.0292(16) Uani 1 1 d . . . . .
O31 O 0.5097(5) 0.4313(4) -0.1934(4) 0.0333(17) Uani 1 1 d . . . . .
P4 P 0.7161(2) -0.0374(2) 0.45004(17) 0.0304(7) Uani 1 1 d . . . . .
O41 O 0.6016(5) -0.0685(4) 0.4806(4) 0.0342(17) Uani 1 1 d . . . . .
O42 O 0.6790(5) 0.0813(4) 0.4291(4) 0.0319(17) Uani 1 1 d . . . . .
O43 O 0.8004(5) -0.1038(4) 0.3681(3) 0.0326(17) Uani 1 1 d . . . . .
O44 O 0.7842(5) -0.0592(4) 0.5281(4) 0.0342(17) Uani 1 1 d . . . . .
P5 P 1.0697(3) 0.4128(2) 0.22012(19) 0.0375(8) Uani 1 1 d . . . . .
O51 O 1.0986(6) 0.2987(4) 0.2548(4) 0.0428(18) Uani 1 1 d . . . . .
O54 O 1.0306(7) 0.4855(5) 0.3024(5) 0.085(3) Uani 1 1 d . . . . .
O52 O 0.9644(6) 0.4381(6) 0.1744(6) 0.095(3) Uani 1 1 d . . . . .
O53 O 1.1842(5) 0.4250(5) 0.1610(4) 0.0395(18) Uani 1 1 d . . . . .
P6 P 0.7477(3) -0.3516(2) 0.07344(19) 0.0360(8) Uani 1 1 d . . . . .
O63 O 0.7522(8) -0.2495(5) 0.0710(7) 0.119(4) Uani 1 1 d . . . . .
O64 O 0.8736(8) -0.4322(6) 0.0627(6) 0.114(3) Uani 1 1 d . . . . .
O61 O 0.6480(11) -0.3594(13) 0.1481(8) 0.221(7) Uani 1 1 d . . . . .
O62 O 0.7069(11) -0.3697(13) -0.0066(9) 0.271(10) Uani 1 1 d . . . . .
P7 P 0.3029(4) 0.3262(3) 0.6344(3) 0.0879(13) Uani 1 1 d . . . . .
O71 O 0.2483(10) 0.4344(7) 0.6830(7) 0.144(4) Uani 1 1 d . U . . .
O76 O 0.2515(17) 0.2499(13) 0.6874(11) 0.063(6) Uani 0.5 1 d . U P . .
O73 O 0.3807(16) 0.3515(12) 0.5543(10) 0.063(5) Uani 0.5 1 d . U P . .
O77 O 0.3836(17) 0.2587(15) 0.7122(14) 0.117(7) Uani 0.5 1 d . U P . .
O72 O 0.2684(16) 0.3473(13) 0.5346(11) 0.093(6) Uani 0.5 1 d . U P . .
O74 O 0.4449(18) 0.2796(17) 0.6013(14) 0.114(7) Uani 0.5 1 d . U P . .
O75 O 0.2041(17) 0.2819(16) 0.6522(14) 0.090(7) Uani 0.5 1 d . U P . .
N1 N 0.6545(6) -0.0447(5) 0.0466(5) 0.0219(19) Uani 1 1 d . . . . .
H1 H 0.6883 -0.1106 0.0550 0.026 Uiso 1 1 calc R U . . .
C10 C 0.5312(7) 0.1275(7) 0.1069(6) 0.019(2) Uani 1 1 d . . . . .
N2 N 0.8184(6) 0.1022(5) -0.3531(5) 0.029(2) Uani 1 1 d . . . . .
H2A H 0.8162 0.1383 -0.4039 0.035 Uiso 1 1 calc R U . . .
H2B H 0.8612 0.0352 -0.3678 0.035 Uiso 1 1 calc R U . . .
C5 C 0.5913(8) 0.0178(7) 0.1205(6) 0.020(2) Uani 1 1 d . . . . .
N5 N 0.4732(6) 0.2475(5) 0.3935(4) 0.031(2) Uani 1 1 d . . . . .
H5A H 0.5311 0.1870 0.4001 0.038 Uiso 1 1 calc R U . . .
H5B H 0.4313 0.2723 0.4482 0.038 Uiso 1 1 calc R U . . .
N3 N 0.8773(6) 0.2692(5) -0.1293(4) 0.0262(19) Uani 1 1 d . . . . .
H3A H 0.7975 0.2986 -0.1057 0.031 Uiso 1 1 calc R U . . .
H3B H 0.8972 0.2001 -0.1221 0.031 Uiso 1 1 calc R U . . .
C11 C 0.5412(7) 0.1658(6) 0.0200(6) 0.018(2) Uani 1 1 d . . . . .
H11 H 0.5024 0.2366 0.0106 0.022 Uiso 1 1 calc R U . . .
C4 C 0.6675(8) -0.0101(7) -0.0385(6) 0.022(2) Uani 1 1 d . . . . .
C6 C 0.5834(8) -0.0215(7) 0.2080(6) 0.029(2) Uani 1 1 d . . . . .
H6 H 0.6228 -0.0922 0.2177 0.035 Uiso 1 1 calc R U . . .
N4 N 0.8303(6) 0.3049(5) 0.1729(4) 0.0214(19) Uani 1 1 d . . . . .
H4A H 0.8632 0.2369 0.1838 0.026 Uiso 1 1 calc R U . . .
H4B H 0.8831 0.3357 0.1782 0.026 Uiso 1 1 calc R U . . .
C8 C 0.4569(7) 0.1527(7) 0.2670(6) 0.023(2) Uani 1 1 d . . . . .
C19 C 0.9428(8) 0.2749(7) 0.0132(6) 0.029(2) Uani 1 1 d . . . . .
H19A H 0.9999 0.2972 0.0351 0.035 Uiso 1 1 calc R U . . .
H19B H 0.9711 0.1988 0.0142 0.035 Uiso 1 1 calc R U . . .
C12 C 0.6094(7) 0.0988(7) -0.0538(6) 0.019(2) Uani 1 1 d . . . . .
C20 C 0.8178(8) 0.3158(6) 0.0780(5) 0.020(2) Uani 1 1 d . . . . .
H20A H 0.7778 0.3891 0.0657 0.025 Uiso 1 1 calc R U . . .
H20B H 0.7671 0.2768 0.0692 0.025 Uiso 1 1 calc R U . . .
C18 C 0.9472(8) 0.3091(7) -0.0813(6) 0.026(2) Uani 1 1 d . . . . .
H18A H 0.9160 0.3852 -0.0821 0.031 Uiso 1 1 calc R U . . .
H18B H 1.0322 0.2865 -0.1142 0.031 Uiso 1 1 calc R U . . .
C1 C 0.6839(8) 0.0690(7) -0.2134(6) 0.023(2) Uani 1 1 d . . . . .
C9 C 0.4615(7) 0.1919(7) 0.1832(6) 0.023(2) Uani 1 1 d . . . . .
H9 H 0.4182 0.2622 0.1754 0.028 Uiso 1 1 calc R U . . .
C17 C 0.9040(8) 0.2936(7) -0.2286(5) 0.023(2) Uani 1 1 d . . . . .
H17A H 0.8857 0.3688 -0.2356 0.027 Uiso 1 1 calc R U . . .
H17B H 0.9908 0.2597 -0.2541 0.027 Uiso 1 1 calc R U . . .
C24 C 0.3875(8) 0.2249(7) 0.3473(6) 0.037(3) Uani 1 1 d . . . . .
H24A H 0.3347 0.2902 0.3278 0.044 Uiso 1 1 calc R U . . .
H24B H 0.3361 0.1924 0.3894 0.044 Uiso 1 1 calc R U . . .
C13 C 0.6205(8) 0.1354(7) -0.1415(6) 0.028(2) Uani 1 1 d . . . . .
H13 H 0.5841 0.2065 -0.1515 0.033 Uiso 1 1 calc R U . . .
C14 C 0.6927(7) 0.1099(7) -0.3074(6) 0.025(2) Uani 1 1 d . . . . .
H14A H 0.6635 0.0705 -0.3414 0.030 Uiso 1 1 calc R U . . .
H14B H 0.6400 0.1828 -0.3058 0.030 Uiso 1 1 calc R U . . .
C23 C 0.5352(8) 0.3234(7) 0.3484(6) 0.030(3) Uani 1 1 d . . . . .
H23A H 0.5615 0.3516 0.3930 0.036 Uiso 1 1 calc R U . . .
H23B H 0.4761 0.3815 0.3254 0.036 Uiso 1 1 calc R U . . .
C21 C 0.7161(8) 0.3491(6) 0.2436(6) 0.026(2) Uani 1 1 d . . . . .
H21A H 0.6641 0.4130 0.2214 0.031 Uiso 1 1 calc R U . . .
H21B H 0.7373 0.3677 0.2957 0.031 Uiso 1 1 calc R U . . .
C15 C 0.8859(7) 0.1417(6) -0.2993(5) 0.023(2) Uani 1 1 d . . . . .
H15A H 0.8852 0.1048 -0.2427 0.027 Uiso 1 1 calc R U . . .
H15B H 0.9706 0.1246 -0.3320 0.027 Uiso 1 1 calc R U . . .
C22 C 0.6453(8) 0.2756(7) 0.2720(6) 0.030(3) Uani 1 1 d . . . . .
H22A H 0.6979 0.2098 0.2912 0.037 Uiso 1 1 calc R U . . .
H22B H 0.6180 0.2609 0.2214 0.037 Uiso 1 1 calc R U . . .
C3 C 0.7323(8) -0.0775(7) -0.1107(6) 0.027(2) Uani 1 1 d . . . . .
H3 H 0.7710 -0.1484 -0.1011 0.033 Uiso 1 1 calc R U . . .
C7 C 0.5174(8) 0.0451(7) 0.2789(6) 0.023(2) Uani 1 1 d . . . . .
H7 H 0.5122 0.0186 0.3369 0.028 Uiso 1 1 calc R U . . .
C16 C 0.8323(8) 0.2587(7) -0.2802(5) 0.026(2) Uani 1 1 d . . . . .
H16A H 0.8318 0.2961 -0.3365 0.031 Uiso 1 1 calc R U . . .
H16B H 0.7482 0.2761 -0.2461 0.031 Uiso 1 1 calc R U . . .
C2 C 0.7394(8) -0.0392(7) -0.1969(6) 0.026(2) Uani 1 1 d . . . . .
H2 H 0.7813 -0.0852 -0.2452 0.032 Uiso 1 1 calc R U . . .
OW1 O 0.5759(7) 0.3803(6) -0.3790(5) 0.090(3) Uani 1 1 d . . . . .
OW2 O 0.7433(10) 0.4491(8) 0.4994(8) 0.164(5) Uani 1 1 d . . . . .
OW3 O 1.0412(10) 0.3439(9) 0.5294(10) 0.192(6) Uani 1 1 d . . . . .
OW4 O 1.1411(18) 0.4464(16) 0.4224(12) 0.312(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O12 1.505(5) . ?
P1 O13 1.515(5) . ?
P1 O11 1.578(5) . ?
P1 O14 1.593(5) . ?
P2 O24 1.504(6) . ?
P2 O21 1.505(6) . ?
P2 O22 1.553(6) . ?
P2 O23 1.575(5) . ?
P3 O33 1.514(6) . ?
P3 O31 1.530(6) . ?
P3 O34 1.570(6) . ?
P3 O32 1.574(6) . ?
P4 O41 1.527(6) . ?
P4 O43 1.530(5) . ?
P4 O42 1.547(6) . ?
P4 O44 1.563(6) . ?
P5 O53 1.503(6) . ?
P5 O52 1.512(7) . ?
P5 O54 1.540(7) . ?
P5 O51 1.548(6) . ?
P6 O63 1.404(7) . ?
P6 O61 1.468(10) . ?
P6 O62 1.493(10) . ?
P6 O64 1.503(8) . ?
P7 O73 1.449(13) . ?
P7 O75 1.465(18) . ?
P7 O76 1.478(16) . ?
P7 O74 1.558(19) . ?
P7 O71 1.552(9) . ?
P7 O72 1.662(16) . ?
P7 O77 1.726(19) . ?
O76 O75 0.86(2) . ?
O76 O77 1.76(2) . ?
O73 O74 1.31(2) . ?
O73 O72 1.47(2) . ?
O77 O74 1.73(3) . ?
N1 C4 1.346(9) . ?
N1 C5 1.365(10) . ?
C10 C11 1.387(10) . ?
C10 C9 1.417(10) . ?
C10 C5 1.437(11) . ?
N2 C14 1.467(9) . ?
N2 C15 1.521(9) . ?
C5 C6 1.403(11) . ?
N5 C24 1.501(9) . ?
N5 C23 1.506(9) . ?
N3 C18 1.486(9) . ?
N3 C17 1.516(9) . ?
C11 C12 1.405(10) . ?
C4 C3 1.383(11) . ?
C4 C12 1.428(11) . ?
C6 C7 1.365(11) . ?
N4 C21 1.488(9) . ?
N4 C20 1.493(9) . ?
C8 C9 1.351(11) . ?
C8 C7 1.409(11) . ?
C8 C24 1.515(11) . ?
C19 C18 1.484(10) . ?
C19 C20 1.522(10) . ?
C12 C13 1.391(11) . ?
C1 C13 1.370(11) . ?
C1 C2 1.419(11) . ?
C1 C14 1.500(11) . ?
C17 C16 1.504(10) . ?
C23 C22 1.519(10) . ?
C21 C22 1.499(10) . ?
C15 C16 1.514(10) . ?
C3 C2 1.379(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
O12 P1 O13 115.6(3) . . ?
O12 P1 O11 109.7(3) . . ?
O13 P1 O11 108.8(3) . . ?
O12 P1 O14 107.4(3) . . ?
O13 P1 O14 109.8(3) . . ?
O11 P1 O14 105.1(3) . . ?
O24 P2 O21 113.1(4) . . ?
O24 P2 O22 107.7(3) . . ?
O21 P2 O22 109.7(3) . . ?
O24 P2 O23 108.6(3) . . ?
O21 P2 O23 108.6(3) . . ?
O22 P2 O23 109.0(3) . . ?
O33 P3 O31 115.0(3) . . ?
O33 P3 O34 111.7(3) . . ?
O31 P3 O34 104.2(3) . . ?
O33 P3 O32 110.6(3) . . ?
O31 P3 O32 109.3(3) . . ?
O34 P3 O32 105.5(3) . . ?
O41 P4 O43 109.2(3) . . ?
O41 P4 O42 109.8(3) . . ?
O43 P4 O42 111.5(3) . . ?
O41 P4 O44 108.6(4) . . ?
O43 P4 O44 109.2(3) . . ?
O42 P4 O44 108.4(3) . . ?
O53 P5 O52 114.1(4) . . ?
O53 P5 O54 107.8(4) . . ?
O52 P5 O54 109.3(5) . . ?
O53 P5 O51 109.3(4) . . ?
O52 P5 O51 108.7(4) . . ?
O54 P5 O51 107.4(4) . . ?
O63 P6 O61 109.4(8) . . ?
O63 P6 O62 109.6(9) . . ?
O61 P6 O62 102.5(8) . . ?
O63 P6 O64 111.0(5) . . ?
O61 P6 O64 119.8(7) . . ?
O62 P6 O64 103.7(6) . . ?
O73 P7 O75 135.0(11) . . ?
O73 P7 O76 149.9(9) . . ?
O75 P7 O76 34.1(9) . . ?
O73 P7 O74 51.4(9) . . ?
O75 P7 O74 134.3(11) . . ?
O76 P7 O74 112.1(12) . . ?
O73 P7 O71 99.7(8) . . ?
O75 P7 O71 106.2(9) . . ?
O76 P7 O71 110.4(8) . . ?
O74 P7 O71 117.4(9) . . ?
O73 P7 O72 55.8(8) . . ?
O75 P7 O72 81.7(11) . . ?
O76 P7 O72 112.0(10) . . ?
O74 P7 O72 98.1(10) . . ?
O71 P7 O72 106.1(8) . . ?
O73 P7 O77 112.8(10) . . ?
O75 P7 O77 100.0(11) . . ?
O76 P7 O77 65.9(9) . . ?
O74 P7 O77 63.2(9) . . ?
O71 P7 O77 96.8(8) . . ?
O72 P7 O77 155.6(9) . . ?
O75 O76 P7 72.1(19) . . ?
O75 O76 O77 136(2) . . ?
P7 O76 O77 63.8(9) . . ?
O74 O73 P7 68.7(12) . . ?
O74 O73 O72 122.5(16) . . ?
P7 O73 O72 69.5(9) . . ?
P7 O77 O74 53.6(9) . . ?
P7 O77 O76 50.2(8) . . ?
O74 O77 O76 92.6(13) . . ?
O73 O72 P7 54.7(8) . . ?
O73 O74 P7 60.0(10) . . ?
O73 O74 O77 121.0(17) . . ?
P7 O74 O77 63.1(10) . . ?
O76 O75 P7 73.8(19) . . ?
C4 N1 C5 124.5(8) . . ?
C11 C10 C9 122.6(8) . . ?
C11 C10 C5 119.0(8) . . ?
C9 C10 C5 118.3(8) . . ?
C14 N2 C15 115.4(6) . . ?
N1 C5 C6 122.3(8) . . ?
N1 C5 C10 118.1(8) . . ?
C6 C5 C10 119.6(8) . . ?
C24 N5 C23 117.0(7) . . ?
C18 N3 C17 111.3(6) . . ?
C10 C11 C12 120.8(8) . . ?
N1 C4 C3 121.8(8) . . ?
N1 C4 C12 118.5(8) . . ?
C3 C4 C12 119.7(8) . . ?
C7 C6 C5 119.3(9) . . ?
C21 N4 C20 116.8(6) . . ?
C9 C8 C7 119.7(8) . . ?
C9 C8 C24 119.8(8) . . ?
C7 C8 C24 120.5(8) . . ?
C18 C19 C20 115.7(7) . . ?
C13 C12 C11 121.8(8) . . ?
C13 C12 C4 119.2(8) . . ?
C11 C12 C4 119.0(8) . . ?
N4 C20 C19 110.8(6) . . ?
N3 C18 C19 115.5(7) . . ?
C13 C1 C2 118.5(8) . . ?
C13 C1 C14 120.6(8) . . ?
C2 C1 C14 120.9(8) . . ?
C8 C9 C10 121.1(8) . . ?
C16 C17 N3 113.7(7) . . ?
N5 C24 C8 111.4(7) . . ?
C1 C13 C12 121.5(9) . . ?
N2 C14 C1 112.3(7) . . ?
N5 C23 C22 114.1(7) . . ?
N4 C21 C22 113.7(7) . . ?
C16 C15 N2 114.2(7) . . ?
C21 C22 C23 110.4(7) . . ?
C2 C3 C4 119.7(9) . . ?
C6 C7 C8 122.0(8) . . ?
C17 C16 C15 111.9(7) . . ?
C3 C2 C1 121.4(8) . . ?

_refine_diff_density_max         1.023
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.107



# start Validation Reply Form
_vrf_THETM01_shelx               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: reflections were collected up to 2theta = 116 deg (0.9 A), due to a significant
lowering of intensity with increasing theta value.
;
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.909 Why? 
RESPONSE: data collection completeness falls below 0.97 at sin(theta)/Lambda higher than 0.5
;
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact Ow1 ..O74 . 2.49 Ang.
RESPONSE: the OW1 involved in the short contact is a water oxygen atom and the contact can be interpreted
as H-bonding contact
;
_vrf_PLAT043_shelx               
;
PROBLEM: Calculated and Reported Mol. Weight Differ by .. 24.19 Check
RESPONSE: Water hydrogens were not localized in the DeltaF map and not introduced in the calculation
;
_vrf_PLAT214_shelx               
;
PROBLEM: Atom O63 (Anion/Solvent) ADP max/min Ratio 5.4 prolat
RESPONSE: O63 oxygen belongs to a disordered PO4 group
;
_vrf_PLAT260_shelx               
;
PROBLEM: Large Average Ueq of Residue Including Ow4 0.314 Check
RESPONSE: The PO4 groups and the cocrystallized water molecules are affected by
a significant degree of disorder
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow1 Check
RESPONSE: The isolated oxygen atoms belong to cocrystallized water molecules. The hydrogen atoms
for these water molecules have not been localized in the Fourier difference map
;
_vrf_PLAT340_shelx               
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01291 Ang.
RESPONSE: the overall low quality of the crystals and the low number of observed
data explain the high e.s.d. on C-C bonds
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.551 572 Report
RESPONSE: Missing reflections are high theta reflections. Actually, data collection completeness
falls below 0.97 at sin(th)/Lambda higher than 0.5
;
# end Validation Reply Form

#===END
