# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_crystal1
_database_code_depnum_ccdc_archive 'CCDC 1912378'
loop_
_audit_author_name
_audit_author_address
'Javier Pitarch-Jarque'
;Universitat de Valencia
Spain
;
_audit_update_record             
;
2019-04-26 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;

_audit_creation_date             2019-04-02
_audit_creation_method           
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H50 N14, 2.65(H2 O), 2(Cl O4)'
_chemical_formula_sum            'C27 H55.31 Cl2 N14 O10.65'
_chemical_formula_weight         817.54
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5140(3)
_cell_length_b                   13.1320(5)
_cell_length_c                   15.7580(6)
_cell_angle_alpha                94.242(2)
_cell_angle_beta                 103.849(2)
_cell_angle_gamma                111.844(2)
_cell_volume                     1928.43(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7859
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      0.998
_shelx_estimated_absorpt_T_max   0.960
_shelx_estimated_absorpt_T_min   0.931
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             869
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6772
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.031
_diffrn_reflns_theta_max         25.031
_diffrn_reflns_theta_min         1.699
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4619
_reflns_number_total             6772
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         6772
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0560
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0556P)²+0.9356P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1416
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.844(2)
 0.156(2)
2. Fixed Uiso
 At 1.2 times of:
  All H(H,H,H) groups, {H4A,H4B} of O4, All C(H) groups, All C(H,H) groups,
  All N(H) groups
 At 1.5 times of:
  {H1C,H1D} of O1, {H3C,H3D} of O3, {H2C,H2D} of O2
3. Restrained distances
 H4B-O24_$1
 1.6 with sigma of 0.1
 H4A-O21_$2
 2 with sigma of 0.1
 Cl2A-O21 \\sim Cl2A-O22 \\sim Cl2A-O24 \\sim Cl2A-O23
 with sigma of 0.02
 O21-O22 \\sim O21-O24 \\sim O21-O23 \\sim O22-O24 \\sim O22-O23 \\sim O24-O23
 with sigma of 0.02
 Cl2B-O28 \\sim Cl2B-O27 \\sim Cl2B-O25 \\sim Cl2B-O26
 with sigma of 0.02
 O18-O17 \\sim O18-O16 \\sim O18-O15 \\sim O17-O16 \\sim O17-O15 \\sim O16-O15
 with sigma of 0.02
 Cl1-O17 \\sim Cl1-O16 \\sim Cl1-O15 \\sim Cl1-O18
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O17) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O15) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(Cl2B)=Sof(O28)=Sof(O27)=Sof(O26)=Sof(O25)=1-FVAR(1)
 Sof(Cl2A)=Sof(O22)=Sof(O21)=Sof(O24)=Sof(O23)=FVAR(1)
 Sof(O16)=Sof(O15)=Sof(O17)=Sof(O18)=1-FVAR(2)
 Sof(O14)=Sof(O11)=Sof(O12)=Sof(O13)=FVAR(2)
 Sof(O3)=Sof(H3C)=Sof(H3D)=FVAR(3)
 Sof(O4)=Sof(H4A)=Sof(H4B)=FVAR(4)
 Fixed Sof: H11(0.5) H5A(0.5)
6.a Free rotating group:
 O1(H1C,H1D), O2(H2C,H2D), O3(H3C,H3D), O4(H4A,H4B)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C16(H16A,H16B), C19(H19A,H19B), C3(H3A,H3B),
 C10(H10C,H10D), C20(H20A,H20B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
  C21(H21A,H21B), C17(H17A,H17B), C7(H7A,H7B), C1(H1A,H1B), C8(H8A,H8B), C9(H9A,
 H9B), C12(H12A,H12B), C11(H11B,H11C)
6.c Aromatic/amide H refined with riding coordinates:
 N13(H13), N3(H3), C23(H23), C14(H14A), C5(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.8095(2) 0.78987(18) 0.14132(15) 0.0462(6) Uani 1 1 d . . . . .
O1 O 0.4360(2) 0.39592(16) 0.26875(19) 0.0675(6) Uani 1 1 d . . . . .
H1C H 0.445379 0.334356 0.263317 0.101 Uiso 1 1 d G . . . .
H1D H 0.347861 0.377223 0.264070 0.101 Uiso 1 1 d G . . . .
N5 N 0.4915(3) 0.3930(2) 0.47719(17) 0.0470(6) Uani 1 1 d . . . . .
N13 N 0.5911(3) 0.2154(2) 0.06402(16) 0.0540(6) Uani 1 1 d . . . . .
H13 H 0.551741 0.144077 0.047400 0.065 Uiso 1 1 calc R . . . .
N3 N 0.9430(3) 0.6054(2) 0.50487(16) 0.0553(7) Uani 1 1 d . . . . .
H3 H 1.021576 0.662704 0.529222 0.066 Uiso 1 1 calc R . . . .
N11 N 0.6455(2) 0.56018(19) 0.03300(17) 0.0409(5) Uani 1 1 d . . . . .
H11A H 0.658(3) 0.575(2) 0.091(2) 0.049 Uiso 1 1 d R . . . .
N9 N 0.1924(3) 0.6567(2) 0.1467(2) 0.0617(7) Uani 1 1 d . . . . .
N12 N 0.6203(3) 0.2875(2) 0.00738(16) 0.0508(6) Uani 1 1 d . . . . .
N10 N 0.5390(3) 0.7734(2) 0.17909(17) 0.0462(6) Uani 1 1 d . . . . .
H10A H 0.490(3) 0.759(3) 0.125(2) 0.055 Uiso 1 1 d R . . . .
O2 O 0.6133(2) 0.59695(18) 0.22321(16) 0.0647(6) Uani 1 1 d . . . . .
H2C H 0.565913 0.548593 0.249448 0.097 Uiso 1 1 d G . . . .
H2D H 0.699053 0.622074 0.256438 0.097 Uiso 1 1 d G . . . .
N14 N 0.4654(3) 0.1917(2) 0.23596(18) 0.0540(7) Uani 1 1 d . . . . .
H14 H 0.405(4) 0.164(3) 0.189(2) 0.065 Uiso 1 1 d R . . . .
C23 C 0.6870(3) 0.3782(2) 0.1469(2) 0.0513(7) Uani 1 1 d . . . . .
H23 H 0.723950 0.436389 0.195218 0.062 Uiso 1 1 calc R . . . .
N2 N 0.9101(3) 0.6927(2) 0.31054(17) 0.0500(6) Uani 1 1 d . . . . .
H2 H 0.921(3) 0.743(3) 0.353(2) 0.060 Uiso 1 1 d R . . . .
N8 N 0.0892(3) 0.5520(2) 0.13021(19) 0.0627(7) Uani 1 1 d . . . . .
C14 C 0.2877(3) 0.5679(2) 0.2332(2) 0.0520(7) Uani 1 1 d . . . . .
H14A H 0.350694 0.549253 0.274838 0.062 Uiso 1 1 calc R . . . .
C2 C 0.9920(3) 0.7481(3) 0.2514(2) 0.0553(8) Uani 1 1 d . . . . .
H2A H 0.980219 0.692573 0.202698 0.066 Uiso 1 1 calc R . . . .
H2B H 1.092759 0.783036 0.284075 0.066 Uiso 1 1 calc R . . . .
C24 C 0.6299(3) 0.2663(2) 0.14891(19) 0.0467(7) Uani 1 1 d . . . . .
C13 C 0.1487(3) 0.4977(3) 0.1835(2) 0.0513(7) Uani 1 1 d . . . . .
C6 C 0.7487(3) 0.4661(2) 0.48887(19) 0.0488(7) Uani 1 1 d . . . . .
C15 C 0.3127(3) 0.6694(3) 0.2085(2) 0.0506(7) Uani 1 1 d . . . . .
C4 C 0.8935(3) 0.5655(3) 0.4170(2) 0.0495(7) Uani 1 1 d . . . . .
N7 N 0.1397(3) 0.3370(2) 0.25525(18) 0.0524(7) Uani 1 1 d . . . . .
H7 H 0.131(4) 0.367(3) 0.297(2) 0.063 Uiso 1 1 d R . . . .
N6 N 0.2669(3) 0.18852(19) 0.35646(16) 0.0523(6) Uani 1 1 d . . . . .
C18 C 0.7509(3) 0.8752(2) 0.1310(2) 0.0530(8) Uani 1 1 d . . . . .
H18A H 0.688638 0.859503 0.070903 0.064 Uiso 1 1 calc R . . . .
H18B H 0.828900 0.947425 0.139256 0.064 Uiso 1 1 calc R . . . .
C22 C 0.6789(3) 0.3879(2) 0.05884(19) 0.0425(7) Uani 1 1 d . . . . .
C16 C 0.4431(3) 0.7757(2) 0.2342(2) 0.0535(8) Uani 1 1 d . . . . .
H16A H 0.415717 0.837920 0.225861 0.064 Uiso 1 1 calc R . . . .
H16B H 0.493310 0.785770 0.296534 0.064 Uiso 1 1 calc R . . . .
C19 C 0.8319(3) 0.7540(2) 0.05707(19) 0.0483(7) Uani 1 1 d . . . . .
H19A H 0.905665 0.725160 0.069296 0.058 Uiso 1 1 calc R . . . .
H19B H 0.863784 0.817531 0.027967 0.058 Uiso 1 1 calc R . . . .
C3 C 0.9718(3) 0.6199(3) 0.3540(2) 0.0551(8) Uani 1 1 d . . . . .
H3A H 1.071566 0.663506 0.386163 0.066 Uiso 1 1 calc R . . . .
H3B H 0.967486 0.562949 0.309247 0.066 Uiso 1 1 calc R . . . .
C10 C 0.1180(3) 0.1779(3) 0.3334(2) 0.0603(9) Uani 1 1 d . . . . .
H10C H 0.106661 0.220676 0.381761 0.072 Uiso 1 1 calc R . . . .
H10D H 0.055944 0.100275 0.328731 0.072 Uiso 1 1 calc R . . . .
C20 C 0.6938(3) 0.6642(2) -0.00404(19) 0.0480(7) Uani 1 1 d . . . . .
H20A H 0.619467 0.692595 -0.013978 0.058 Uiso 1 1 calc R . . . .
H20B H 0.708285 0.647159 -0.061027 0.058 Uiso 1 1 calc R . . . .
C25 C 0.6024(4) 0.2019(3) 0.2207(2) 0.0562(8) Uani 1 1 d . . . . .
H25A H 0.599421 0.128198 0.204583 0.067 Uiso 1 1 calc R . . . .
H25B H 0.679574 0.239173 0.275068 0.067 Uiso 1 1 calc R . . . .
C26 C 0.4268(4) 0.1172(3) 0.2992(2) 0.0598(9) Uani 1 1 d . . . . .
H26A H 0.495443 0.150653 0.357291 0.072 Uiso 1 1 calc R . . . .
H26B H 0.431587 0.047046 0.280272 0.072 Uiso 1 1 calc R . . . .
C27 C 0.2784(4) 0.0949(2) 0.3060(2) 0.0586(8) Uani 1 1 d . . . . .
H27A H 0.213510 0.076524 0.246521 0.070 Uiso 1 1 calc R . . . .
H27B H 0.247314 0.030293 0.334125 0.070 Uiso 1 1 calc R . . . .
C21 C 0.7243(3) 0.4898(2) 0.0184(2) 0.0488(7) Uani 1 1 d . . . . .
H21A H 0.706800 0.468081 -0.044863 0.059 Uiso 1 1 calc R . . . .
H21B H 0.826258 0.532998 0.044400 0.059 Uiso 1 1 calc R . . . .
C17 C 0.6679(3) 0.8804(2) 0.1956(2) 0.0551(8) Uani 1 1 d . . . . .
H17A H 0.728467 0.893827 0.255907 0.066 Uiso 1 1 calc R . . . .
H17B H 0.638177 0.941789 0.189230 0.066 Uiso 1 1 calc R . . . .
C7 C 0.6296(3) 0.3830(3) 0.5142(2) 0.0549(8) Uani 1 1 d . . . . .
H7A H 0.652272 0.393563 0.578470 0.066 Uiso 1 1 calc R . . . .
H7B H 0.619721 0.308522 0.492739 0.066 Uiso 1 1 calc R . . . .
C1 C 0.9456(3) 0.8353(3) 0.2141(2) 0.0557(8) Uani 1 1 d . . . . .
H1A H 0.935458 0.879932 0.261806 0.067 Uiso 1 1 calc R . . . .
H1B H 1.020511 0.884384 0.192103 0.067 Uiso 1 1 calc R . . . .
N4 N 0.8567(3) 0.5462(2) 0.55136(16) 0.0563(7) Uani 1 1 d . . . . .
C8 C 0.3716(3) 0.3114(2) 0.5024(2) 0.0553(8) Uani 1 1 d . . . . .
H8A H 0.292292 0.334293 0.490823 0.066 Uiso 1 1 calc R . . . .
H8B H 0.401837 0.311916 0.565643 0.066 Uiso 1 1 calc R . . . .
C9 C 0.3205(4) 0.1935(2) 0.4525(2) 0.0569(8) Uani 1 1 d . . . . .
H9A H 0.398871 0.169561 0.464096 0.068 Uiso 1 1 calc R . . . .
H9B H 0.244804 0.143269 0.473237 0.068 Uiso 1 1 calc R . . . .
C12 C 0.0695(3) 0.3756(3) 0.1805(2) 0.0598(8) Uani 1 1 d . . . . .
H12A H -0.027384 0.361066 0.181802 0.072 Uiso 1 1 calc R . . . .
H12B H 0.064057 0.334145 0.125188 0.072 Uiso 1 1 calc R . . . .
C5 C 0.7682(3) 0.4758(3) 0.4052(2) 0.0529(8) Uani 1 1 d . . . . .
H5 H 0.707511 0.429892 0.351560 0.063 Uiso 1 1 calc R . . . .
C11 C 0.0681(4) 0.2157(3) 0.2485(2) 0.0647(9) Uani 1 1 d . . . . .
H11B H 0.086885 0.178382 0.200495 0.078 Uiso 1 1 calc R . . . .
H11C H -0.034420 0.194397 0.234175 0.078 Uiso 1 1 calc R . . . .
O3 O 0.4022(10) 0.8688(6) 0.4082(7) 0.095(4) Uani 0.353(8) 1 d . . P A 2
H3C H 0.487604 0.916023 0.417255 0.143 Uiso 0.353(8) 1 d G . P A 2
H3D H 0.344555 0.899330 0.389953 0.143 Uiso 0.353(8) 1 d G . P A 2
Cl1 Cl 0.25003(9) 0.93679(6) 0.04697(5) 0.0588(2) Uani 1 1 d D . . . .
O14 O 0.2258(18) 1.0381(12) 0.0656(8) 0.068(5) Uani 0.410(18) 1 d . . P B 1
O11 O 0.181(2) 0.8484(18) 0.079(2) 0.216(11) Uani 0.410(18) 1 d . . P B 1
O12 O 0.4018(14) 0.9569(15) 0.0747(12) 0.106(5) Uani 0.410(18) 1 d . U P B 1
O13 O 0.216(3) 0.9006(19) -0.0492(9) 0.160(9) Uani 0.410(18) 1 d . . P B 1
Cl2A Cl 0.2256(4) 0.8877(3) 0.5361(3) 0.0804(9) Uani 0.621(7) 1 d D . P C 1
O22 O 0.2081(7) 0.7934(5) 0.5735(5) 0.108(2) Uani 0.621(7) 1 d D . P C 1
O21 O 0.2939(14) 0.9848(8) 0.6025(6) 0.173(6) Uani 0.621(7) 1 d D . P C 1
O24 O 0.0944(14) 0.8820(14) 0.4839(8) 0.141(6) Uani 0.621(7) 1 d D . P C 1
O23 O 0.3173(9) 0.8906(7) 0.4836(6) 0.170(4) Uani 0.621(7) 1 d D . P C 1
Cl2B Cl 0.2081(5) 0.9259(5) 0.5656(4) 0.0730(13) Uani 0.379(7) 1 d D . P C 2
O28 O 0.3496(14) 0.9925(11) 0.5914(13) 0.117(6) Uani 0.379(7) 1 d D . P C 2
O27 O 0.1377(11) 0.9926(8) 0.5842(7) 0.119(4) Uani 0.379(7) 1 d D . P C 2
O26 O 0.1704(11) 0.8406(12) 0.6142(10) 0.125(5) Uani 0.379(7) 1 d D . P C 2
O25 O 0.152(3) 0.891(2) 0.4709(9) 0.156(11) Uani 0.379(7) 1 d D . P C 2
H9 H 0.178(4) 0.710(4) 0.114(3) 0.105(15) Uiso 1 1 d . . . . .
O4 O 0.8860(12) 0.8981(9) 0.4054(6) 0.092(4) Uani 0.301(8) 1 d . . P D 1
H4A H 0.851680 0.944133 0.419009 0.111 Uiso 0.301(8) 1 d DG . P D 1
H4B H 0.949528 0.903738 0.452637 0.111 Uiso 0.301(8) 1 d DG . P D 1
O16 O 0.1562(9) 0.8702(8) -0.0293(6) 0.111(4) Uani 0.590(18) 1 d D . P B 2
O15 O 0.3874(10) 0.9729(8) 0.0462(10) 0.119(5) Uani 0.590(18) 1 d D U P B 2
O17 O 0.2278(12) 0.8801(8) 0.1175(4) 0.099(3) Uani 0.590(18) 1 d D U P B 2
O18 O 0.2153(15) 1.0267(10) 0.0630(8) 0.102(5) Uani 0.590(18) 1 d D . P B 2
H10B H 0.563(3) 0.713(3) 0.192(2) 0.065(10) Uiso 1 1 d . . . . .
H11 H 0.542(7) 0.520(7) 0.008(6) 0.079 Uiso 0.5 1 d R . P E -1
H5A H 0.494(10) 0.466(5) 0.494(6) 0.079 Uiso 0.5 1 d R . P F -1
H5B H 0.468(4) 0.383(3) 0.422(3) 0.079 Uiso 1 1 d R . . . .


_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 C18 1.468(4) . ?
N1 C19 1.476(4) . ?
N1 C1 1.482(4) . ?
N5 C7 1.487(4) . ?
N5 C8 1.481(4) . ?
N13 N12 1.352(3) . ?
N13 C24 1.344(4) . ?
N3 C4 1.345(4) . ?
N3 N4 1.357(3) . ?
N11 C20 1.486(3) . ?
N11 C21 1.491(4) . ?
N9 N8 1.356(4) . ?
N9 C15 1.344(4) . ?
N12 C22 1.331(3) . ?
N10 C16 1.486(4) . ?
N10 C17 1.496(4) . ?
N14 C25 1.475(4) . ?
N14 C26 1.469(4) . ?
C23 C24 1.372(4) . ?
C23 C22 1.388(4) . ?
N2 C2 1.470(4) . ?
N2 C3 1.466(4) . ?
N8 C13 1.332(4) . ?
C14 C13 1.393(4) . ?
C14 C15 1.365(4) . ?
C2 C1 1.507(4) . ?
C24 C25 1.482(4) . ?
C13 C12 1.498(4) . ?
C6 C7 1.485(4) . ?
C6 N4 1.337(4) . ?
C6 C5 1.390(4) . ?
C15 C16 1.489(4) . ?
C4 C3 1.493(4) . ?
C4 C5 1.362(4) . ?
N7 C12 1.463(4) . ?
N7 C11 1.469(4) . ?
N6 C10 1.470(4) . ?
N6 C27 1.473(4) . ?
N6 C9 1.470(4) . ?
C18 C17 1.505(4) . ?
C22 C21 1.490(4) . ?
C19 C20 1.521(4) . ?
C10 C11 1.506(4) . ?
C26 C27 1.509(5) . ?
C8 C9 1.517(4) . ?
Cl1 O14 1.467(14) . ?
Cl1 O11 1.333(12) . ?
Cl1 O12 1.464(13) . ?
Cl1 O13 1.468(15) . ?
Cl1 O16 1.348(7) . ?
Cl1 O15 1.346(7) . ?
Cl1 O17 1.400(6) . ?
Cl1 O18 1.383(10) . ?
Cl2A O22 1.380(6) . ?
Cl2A O21 1.413(8) . ?
Cl2A O24 1.398(11) . ?
Cl2A O23 1.405(8) . ?
Cl2B O28 1.355(12) . ?
Cl2B O27 1.397(11) . ?
Cl2B O26 1.393(10) . ?
Cl2B O25 1.436(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
C18 N1 C19 110.1(2) . . ?
C18 N1 C1 109.4(2) . . ?
C19 N1 C1 110.9(2) . . ?
C8 N5 C7 112.8(2) . . ?
C24 N13 N12 113.2(2) . . ?
C4 N3 N4 113.4(2) . . ?
C20 N11 C21 111.9(2) . . ?
C15 N9 N8 112.8(3) . . ?
C22 N12 N13 104.4(2) . . ?
C16 N10 C17 113.8(2) . . ?
C26 N14 C25 111.8(3) . . ?
C24 C23 C22 106.7(3) . . ?
C3 N2 C2 110.2(2) . . ?
C13 N8 N9 104.2(3) . . ?
C15 C14 C13 106.2(3) . . ?
N2 C2 C1 112.6(3) . . ?
N13 C24 C23 105.1(3) . . ?
N13 C24 C25 121.5(3) . . ?
C23 C24 C25 133.3(3) . . ?
N8 C13 C14 110.9(3) . . ?
N8 C13 C12 120.3(3) . . ?
C14 C13 C12 128.7(3) . . ?
N4 C6 C7 119.9(3) . . ?
N4 C6 C5 110.9(3) . . ?
C5 C6 C7 129.2(3) . . ?
N9 C15 C14 105.9(3) . . ?
N9 C15 C16 122.4(3) . . ?
C14 C15 C16 131.6(3) . . ?
N3 C4 C3 121.7(3) . . ?
N3 C4 C5 105.4(3) . . ?
C5 C4 C3 132.9(3) . . ?
C12 N7 C11 111.5(2) . . ?
C10 N6 C27 110.7(2) . . ?
C10 N6 C9 110.0(3) . . ?
C9 N6 C27 110.4(2) . . ?
N1 C18 C17 112.9(2) . . ?
N12 C22 C23 110.6(2) . . ?
N12 C22 C21 119.7(3) . . ?
C23 C22 C21 129.7(3) . . ?
N10 C16 C15 110.0(2) . . ?
N1 C19 C20 110.5(2) . . ?
N2 C3 C4 111.3(3) . . ?
N6 C10 C11 115.5(3) . . ?
N11 C20 C19 112.5(2) . . ?
N14 C25 C24 110.6(2) . . ?
N14 C26 C27 111.9(3) . . ?
N6 C27 C26 114.5(2) . . ?
C22 C21 N11 111.4(2) . . ?
N10 C17 C18 110.3(2) . . ?
C6 C7 N5 112.0(2) . . ?
N1 C1 C2 114.5(2) . . ?
C6 N4 N3 103.7(2) . . ?
N5 C8 C9 113.1(3) . . ?
N6 C9 C8 110.4(2) . . ?
N7 C12 C13 111.6(3) . . ?
C4 C5 C6 106.7(3) . . ?
N7 C11 C10 112.2(3) . . ?
O14 Cl1 O13 110.7(7) . . ?
O11 Cl1 O14 117.5(12) . . ?
O11 Cl1 O12 107.1(10) . . ?
O11 Cl1 O13 107.1(12) . . ?
O12 Cl1 O14 112.6(9) . . ?
O12 Cl1 O13 100.2(11) . . ?
O16 Cl1 O17 108.6(5) . . ?
O16 Cl1 O18 108.3(6) . . ?
O15 Cl1 O16 113.6(6) . . ?
O15 Cl1 O17 111.4(6) . . ?
O15 Cl1 O18 110.0(7) . . ?
O18 Cl1 O17 104.5(6) . . ?
O22 Cl2A O21 110.7(6) . . ?
O22 Cl2A O24 111.1(7) . . ?
O22 Cl2A O23 105.4(5) . . ?
O24 Cl2A O21 110.8(8) . . ?
O24 Cl2A O23 110.6(7) . . ?
O23 Cl2A O21 108.1(6) . . ?
O28 Cl2B O27 106.5(9) . . ?
O28 Cl2B O26 113.7(8) . . ?
O28 Cl2B O25 112.3(16) . . ?
O27 Cl2B O25 103.2(12) . . ?
O26 Cl2B O27 105.0(7) . . ?
O26 Cl2B O25 114.9(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1C N14 0.85 1.99 2.835(3) 173.4 . yes
O1 H1D N7 0.85 2.02 2.866(3) 178.3 . yes
N3 H3 O22 0.86 1.99 2.842(6) 173.9 1_655 yes
N10 H10A N12 0.86(3) 2.04(3) 2.894(4) 175(3) 2_665 yes
O2 H2C O1 0.85 2.06 2.866(3) 158.8 . yes
O2 H2D N2 0.85 1.99 2.825(3) 167.4 . yes
O3 H3C O28 0.85 1.73 2.565(15) 166.4 2_676 yes
N9 H9 O11 0.94(4) 1.93(5) 2.834(14) 163(4) . yes
N9 H9 O17 0.94(4) 2.09(5) 2.903(9) 145(4) . yes
O4 H4A O21 0.85 2.05 2.835(16) 154.0 2_676 yes
O4 H4B O24 0.85 1.62 2.337(15) 139.9 1_655 yes
N10 H10B O2 0.93(4) 1.86(4) 2.791(3) 177(3) . yes
N11 H11 N11 0.97(6) 1.78(6) 2.752(5) 175(8) 2_665 yes
N5 H5A N5 0.96(6) 1.82(6) 2.778(5) 177(8) 2_666 yes

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.844(2)
2 0.156(2)
####################################################################### 
# 
# 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_crystal2_nitrate
_database_code_depnum_ccdc_archive 'CCDC 1912379'
loop_
_audit_author_name
_audit_author_address
'Javier Pitarch-Jarque'
;Universitat de Valencia
Spain
;
_audit_update_record             
;
2019-04-26 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_audit_creation_date             2019-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H54 N14, 6(N O3), 5(H2 O)'
_chemical_formula_sum            'C27 H64 N20 O23'
_chemical_formula_weight         1036.98
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   19.1317(8)
_cell_length_b                   13.6910(6)
_cell_length_c                   19.6870(8)
_cell_angle_alpha                90
_cell_angle_beta                 114.465(2)
_cell_angle_gamma                90
_cell_volume                     4693.7(3)
_cell_formula_units_Z            4

_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16386
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      25.028

_shelx_estimated_absorpt_T_max   0.989
_shelx_estimated_absorpt_T_min   0.985
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28873
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.872
_diffrn_ambient_temperature      293.15

_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4071
_reflns_number_total             8257
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0088(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         8257
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0594
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1039P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1939
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2E,H2F} of O2, {H3C,H3D} of O3, {H4A,H4B} of O4, {H5C,
  H5D} of O5, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  {H1C,H1D} of O1
2. Restrained distances
 O2-H2E = O2-H2F
 0.82 with sigma of 0.02
 O3-H3C = O3-H3D
 0.82 with sigma of 0.02
 O4-H4A = O4-H4B
 0.82 with sigma of 0.02
 O5-H5C = O5-H5D
 0.82 with sigma of 0.02
 O11B-N1N
 1.3 with sigma of 0.01
 H2E-H2F
 1.33 with sigma of 0.04
 H3C-H3D
 1.33 with sigma of 0.04
 H4A-H4B
 1.33 with sigma of 0.04
 H5C-H5D
 1.33 with sigma of 0.04
 O22-N2N \\sim O21-N2N \\sim O23-N2N
 with sigma of 0.02
 O0AA-O1AA \\sim O1AA-O21 \\sim O0AA-O21
 with sigma of 0.02
3. Rigid bond restraints
 N1N, O11A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O11A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
5. Others
 Sof(O13B)=Sof(O11B)=Sof(O12B)=1-FVAR(1)
 Sof(O11A)=Sof(O13A)=Sof(O12A)=FVAR(1)
 Sof(O1AA)=Sof(O0AA)=1-FVAR(2)
 Sof(O22)=Sof(O23)=FVAR(2)
6.a Free rotating group:
 O1(H1C,H1D)
6.b Rotating group with stretchable bonds:
 O2(H2E,H2F), O3(H3C,H3D), O4(H4A,H4B), O5(H5C,H5D)
6.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C16(H16A,H16B), C17(H17A,H17B),
  C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), N2(H2C,H2D), N5(H5A,H5B), N7(H7C,H7D),
 N10(H10C,H10D), N11(H11C,H11D), N14(H14A,H14B)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C14(H14), C23(H23), N4(H4), N9(H9), N13(H13)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.3374(2) 0.8185(2) 0.2403(2) 0.0506(9) Uani 1 1 d . . . . .
H1A H 0.346822 0.878183 0.218864 0.061 Uiso 1 1 calc R . . . .
H1B H 0.369253 0.819889 0.293503 0.061 Uiso 1 1 calc R . . . .
C2 C 0.2545(2) 0.8153(3) 0.2277(2) 0.0514(9) Uani 1 1 d . . . . .
H2A H 0.238501 0.880088 0.235435 0.062 Uiso 1 1 calc R . . . .
H2B H 0.223479 0.796659 0.176445 0.062 Uiso 1 1 calc R . . . .
C3 C 0.1623(2) 0.7574(3) 0.2774(2) 0.0564(10) Uani 1 1 d . . . . .
H3A H 0.157115 0.823292 0.292901 0.068 Uiso 1 1 calc R . . . .
H3B H 0.123892 0.748449 0.226796 0.068 Uiso 1 1 calc R . . . .
C4 C 0.1484(2) 0.6861(3) 0.3276(2) 0.0516(9) Uani 1 1 d . . . . .
C5 C 0.1185(2) 0.5918(3) 0.3121(2) 0.0566(10) Uani 1 1 d . . . . .
H5 H 0.100859 0.559729 0.266396 0.068 Uiso 1 1 calc R . . . .
C6 C 0.1203(2) 0.5559(3) 0.3775(2) 0.0526(10) Uani 1 1 d . . . . .
C7 C 0.0969(3) 0.4624(3) 0.3989(3) 0.0668(12) Uani 1 1 d . . . . .
H7A H 0.042497 0.464765 0.387623 0.080 Uiso 1 1 calc R . . . .
H7B H 0.124675 0.453026 0.452317 0.080 Uiso 1 1 calc R . . . .
C8 C 0.0979(2) 0.2832(3) 0.3878(2) 0.0539(10) Uani 1 1 d . . . . .
H8A H 0.054217 0.289410 0.400482 0.065 Uiso 1 1 calc R . . . .
H8B H 0.142341 0.266344 0.433005 0.065 Uiso 1 1 calc R . . . .
C9 C 0.0826(2) 0.2019(3) 0.3317(2) 0.0513(9) Uani 1 1 d . . . . .
H9A H 0.081913 0.140275 0.355770 0.062 Uiso 1 1 calc R . . . .
H9B H 0.032133 0.211401 0.291665 0.062 Uiso 1 1 calc R . . . .
C10 C 0.1105(2) 0.1294(3) 0.23397(19) 0.0516(9) Uani 1 1 d . . . . .
H10A H 0.087061 0.072664 0.245511 0.062 Uiso 1 1 calc R . . . .
H10B H 0.153183 0.106992 0.223536 0.062 Uiso 1 1 calc R . . . .
C11 C 0.0523(2) 0.1795(3) 0.1657(2) 0.0561(10) Uani 1 1 d . . . . .
H11A H 0.032156 0.132991 0.124953 0.067 Uiso 1 1 calc R . . . .
H11B H 0.009906 0.202623 0.176201 0.067 Uiso 1 1 calc R . . . .
C12 C 0.1242(2) 0.2372(3) 0.0925(2) 0.0607(11) Uani 1 1 d . . . . .
H12A H 0.088327 0.199866 0.050716 0.073 Uiso 1 1 calc R . . . .
H12B H 0.168603 0.196349 0.119182 0.073 Uiso 1 1 calc R . . . .
C13 C 0.1486(2) 0.3257(3) 0.0640(2) 0.0508(9) Uani 1 1 d . . . . .
C14 C 0.2221(2) 0.3592(3) 0.0785(2) 0.0543(10) Uani 1 1 d . . . . .
H14 H 0.268495 0.330163 0.108968 0.065 Uiso 1 1 calc R . . . .
C15 C 0.2117(2) 0.4439(3) 0.0386(2) 0.0500(9) Uani 1 1 d . . . . .
C16 C 0.2667(2) 0.5153(3) 0.0316(2) 0.0572(10) Uani 1 1 d . . . . .
H16A H 0.314836 0.482544 0.040974 0.069 Uiso 1 1 calc R . . . .
H16B H 0.246311 0.540695 -0.018933 0.069 Uiso 1 1 calc R . . . .
C17 C 0.3369(2) 0.6695(3) 0.0809(2) 0.0581(10) Uani 1 1 d . . . . .
H17A H 0.321646 0.689807 0.029484 0.070 Uiso 1 1 calc R . . . .
H17B H 0.387289 0.639600 0.097977 0.070 Uiso 1 1 calc R . . . .
C18 C 0.3410(2) 0.7578(3) 0.1285(2) 0.0534(9) Uani 1 1 d . . . . .
H18A H 0.379541 0.802330 0.126537 0.064 Uiso 1 1 calc R . . . .
H18B H 0.291925 0.791275 0.107603 0.064 Uiso 1 1 calc R . . . .
C19 C 0.4424(2) 0.7140(3) 0.2458(2) 0.0533(9) Uani 1 1 d . . . . .
H19A H 0.469911 0.774742 0.249752 0.064 Uiso 1 1 calc R . . . .
H19B H 0.456984 0.669688 0.215485 0.064 Uiso 1 1 calc R . . . .
C20 C 0.4681(2) 0.6706(3) 0.3231(2) 0.0597(10) Uani 1 1 d . . . . .
H20A H 0.523674 0.674489 0.347815 0.072 Uiso 1 1 calc R . . . .
H20B H 0.447626 0.710360 0.351362 0.072 Uiso 1 1 calc R . . . .
C21 C 0.5032(2) 0.5146(3) 0.3894(2) 0.0593(10) Uani 1 1 d . . . . .
H21A H 0.509045 0.547818 0.434911 0.071 Uiso 1 1 calc R . . . .
H21B H 0.551959 0.519011 0.385278 0.071 Uiso 1 1 calc R . . . .
C22 C 0.4863(2) 0.4098(3) 0.3959(2) 0.0501(9) Uani 1 1 d . . . . .
C23 C 0.4349(2) 0.3439(3) 0.3465(2) 0.0553(10) Uani 1 1 d . . . . .
H23 H 0.397903 0.357020 0.298813 0.066 Uiso 1 1 calc R . . . .
C24 C 0.4499(2) 0.2554(3) 0.3826(2) 0.0509(9) Uani 1 1 d . . . . .
C25 C 0.4163(2) 0.1560(3) 0.3615(2) 0.0592(10) Uani 1 1 d . . . . .
H25A H 0.455796 0.107825 0.386660 0.071 Uiso 1 1 calc R . . . .
H25B H 0.399819 0.147281 0.308175 0.071 Uiso 1 1 calc R . . . .
C26 C 0.2785(2) 0.1912(3) 0.3331(2) 0.0521(9) Uani 1 1 d . . . . .
H26A H 0.264925 0.176539 0.280977 0.062 Uiso 1 1 calc R . . . .
H26B H 0.286719 0.261098 0.340229 0.062 Uiso 1 1 calc R . . . .
C27 C 0.2137(2) 0.1599(3) 0.3543(2) 0.0518(9) Uani 1 1 d . . . . .
H27A H 0.212558 0.089207 0.356930 0.062 Uiso 1 1 calc R . . . .
H27B H 0.222909 0.185780 0.403155 0.062 Uiso 1 1 calc R . . . .
N1 N 0.35974(16) 0.73372(19) 0.20686(15) 0.0461(7) Uani 1 1 d . . . . .
N2 N 0.24067(16) 0.7451(2) 0.27878(16) 0.0498(7) Uani 1 1 d . . . . .
H2C H 0.275877 0.754173 0.325103 0.060 Uiso 1 1 calc R . . . .
H2D H 0.245629 0.684364 0.265248 0.060 Uiso 1 1 calc R . . . .
N3 N 0.1673(2) 0.7087(2) 0.39922(19) 0.0670(9) Uani 1 1 d . . . . .
N4 N 0.1498(2) 0.6276(2) 0.42769(19) 0.0663(9) Uani 1 1 d . . . . .
H4 H 0.156821 0.622276 0.473610 0.080 Uiso 1 1 calc R . . . .
N5 N 0.11196(17) 0.3790(2) 0.35936(16) 0.0523(8) Uani 1 1 d . . . . .
H5A H 0.160499 0.381508 0.364844 0.063 Uiso 1 1 calc R . . . .
H5B H 0.081828 0.383746 0.310862 0.063 Uiso 1 1 calc R . . . .
N6 N 0.13965(16) 0.1955(2) 0.29927(15) 0.0460(7) Uani 1 1 d . . . . .
N7 N 0.08740(17) 0.2637(2) 0.14284(16) 0.0523(8) Uani 1 1 d . . . . .
H7C H 0.051047 0.307899 0.120171 0.063 Uiso 1 1 calc R . . . .
H7D H 0.122400 0.291371 0.183662 0.063 Uiso 1 1 calc R . . . .
N8 N 0.09489(18) 0.3856(2) 0.01766(17) 0.0573(8) Uani 1 1 d . . . . .
N9 N 0.13508(19) 0.4572(2) 0.00343(17) 0.0562(8) Uani 1 1 d . . . . .
H9 H 0.114188 0.506293 -0.025045 0.067 Uiso 1 1 calc R . . . .
N10 N 0.28117(17) 0.5973(2) 0.08481(16) 0.0527(8) Uani 1 1 d . . . . .
H10C H 0.236938 0.627466 0.075540 0.063 Uiso 1 1 calc R . . . .
H10D H 0.298707 0.573382 0.130934 0.063 Uiso 1 1 calc R . . . .
N11 N 0.44456(16) 0.5663(2) 0.32553(16) 0.0524(8) Uani 1 1 d . . . . .
H11C H 0.399905 0.564924 0.329521 0.063 Uiso 1 1 calc R . . . .
H11D H 0.438335 0.536284 0.283305 0.063 Uiso 1 1 calc R . . . .
N12 N 0.53130(18) 0.3654(2) 0.45957(17) 0.0593(8) Uani 1 1 d . . . . .
N13 N 0.50787(18) 0.2715(2) 0.44973(19) 0.0574(8) Uani 1 1 d . . . . .
H13 H 0.527835 0.226756 0.482800 0.069 Uiso 1 1 calc R . . . .
N14 N 0.34980(16) 0.1382(2) 0.38071(16) 0.0513(8) Uani 1 1 d . . . . .
H14A H 0.339817 0.074437 0.377175 0.062 Uiso 1 1 calc R . . . .
H14B H 0.363048 0.155495 0.428009 0.062 Uiso 1 1 calc R . . . .
N3N N 0.0527(2) 0.9104(2) 0.34502(19) 0.0590(8) Uani 1 1 d . . . . .
O31 O 0.00937(18) 0.8751(2) 0.28398(17) 0.0863(9) Uani 1 1 d . . . . .
O32 O 0.11269(19) 0.9511(2) 0.35445(16) 0.0746(9) Uani 1 1 d . . . . .
O33 O 0.03670(17) 0.8990(2) 0.40114(16) 0.0801(9) Uani 1 1 d . . . . .
N4N N 0.0895(2) 0.9187(3) 0.0734(2) 0.0678(9) Uani 1 1 d . . . . .
O41 O 0.0357(2) 0.8786(3) 0.0215(2) 0.1122(12) Uani 1 1 d . . . . .
O42 O 0.08428(19) 0.9364(3) 0.13177(19) 0.1078(12) Uani 1 1 d . . . . .
O43 O 0.1504(2) 0.9366(2) 0.06659(17) 0.0865(10) Uani 1 1 d . . . . .
N5N N 0.4811(3) 0.4625(3) 0.1873(2) 0.0679(9) Uani 1 1 d . . . . .
O51 O 0.5334(2) 0.5031(2) 0.2403(2) 0.0848(9) Uani 1 1 d . . . . .
O52 O 0.4947(2) 0.4213(3) 0.13821(18) 0.0967(11) Uani 1 1 d . . . . .
O53 O 0.41425(19) 0.4644(2) 0.18431(18) 0.0854(9) Uani 1 1 d . . . . .
N6N N 0.6327(2) 0.3944(3) 0.07645(19) 0.0543(8) Uani 1 1 d . . . . .
O61 O 0.68766(16) 0.43823(19) 0.12598(16) 0.0668(7) Uani 1 1 d . . . . .
O62 O 0.58302(17) 0.4402(2) 0.02509(17) 0.0740(8) Uani 1 1 d . . . . .
O63 O 0.62962(16) 0.30314(19) 0.07928(14) 0.0654(7) Uani 1 1 d . . . . .
N2N N 0.2967(3) 0.0993(4) 0.0086(4) 0.1063(18) Uani 1 1 d D . . . .
O21 O 0.3010(3) 0.0101(4) 0.0275(3) 0.1533(17) Uani 1 1 d D . . . .
O22 O 0.3313(5) 0.1512(4) 0.0688(4) 0.092(3) Uani 0.675(17) 1 d D . P A 1
O23 O 0.2741(7) 0.1249(13) -0.0591(8) 0.169(7) Uani 0.675(17) 1 d D . P A 1
N1N N 0.2180(3) 0.4762(3) 0.2227(2) 0.0691(10) Uani 1 1 d D U . . .
O11A O 0.2470(7) 0.4129(8) 0.2631(6) 0.178(5) Uani 0.706(12) 1 d . U P B 1
O13A O 0.2474(5) 0.5499(5) 0.2173(4) 0.092(3) Uani 0.706(12) 1 d . . P B 1
O12A O 0.1460(3) 0.4649(6) 0.1881(4) 0.103(3) Uani 0.706(12) 1 d . . P B 1
O13B O 0.1875(11) 0.5506(14) 0.1900(8) 0.092(7) Uani 0.294(12) 1 d . . P B 2
O11B O 0.2918(5) 0.4765(13) 0.2322(7) 0.092(6) Uani 0.294(12) 1 d D . P B 2
O12B O 0.1972(16) 0.4037(15) 0.2399(9) 0.116(9) Uani 0.294(12) 1 d . . P B 2
O1 O 0.2632(2) 0.0640(3) 0.1747(2) 0.1014(11) Uani 1 1 d . . . . .
H1C H 0.236009 0.023710 0.141487 0.152 Uiso 1 1 d G . . . .
H1D H 0.297389 0.088182 0.162595 0.152 Uiso 1 1 d G . . . .
O2 O 0.33988(16) 0.5830(2) 0.39182(16) 0.0746(8) Uani 1 1 d D . . . .
H2E H 0.3650(4) 0.6010(3) 0.4355(7) 0.090 Uiso 1 1 d DGR . . . .
H2F H 0.3180(3) 0.5313(8) 0.39221(16) 0.090 Uiso 1 1 d DGR . . . .
O3 O 0.05671(19) 0.6328(3) 0.1021(2) 0.1087(12) Uani 1 1 d D . . . .
H3C H 0.0729(3) 0.5788(9) 0.1222(3) 0.130 Uiso 1 1 d DGR . . . .
H3D H 0.0195(6) 0.6175(4) 0.0621(6) 0.130 Uiso 1 1 d DGR . . . .
O4 O 0.15142(19) 0.6998(2) 0.0407(2) 0.1008(11) Uani 1 1 d D . . . .
H4A H 0.1118(6) 0.7037(2) -0.0003(6) 0.121 Uiso 1 1 d DGR . . . .
H4B H 0.1331(3) 0.6966(2) 0.0739(5) 0.121 Uiso 1 1 d DGR . . . .
O5 O 0.3844(2) 0.3156(3) 0.02404(17) 0.1006(11) Uani 1 1 d D . . . .
H5C H 0.3722(3) 0.2652(8) 0.0402(3) 0.121 Uiso 1 1 d DGR . . . .
H5D H 0.4181(5) 0.3395(4) 0.0622(6) 0.121 Uiso 1 1 d DGR . . . .
O1AA O 0.2617(17) 0.1459(13) 0.0249(10) 0.182(12) Uani 0.325(17) 1 d D . P A 2
O0AA O 0.2812(15) 0.0958(15) -0.0574(10) 0.106(7) Uani 0.325(17) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.501(5) . ?
C1 N1 1.482(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 N2 1.492(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.489(5) . ?
C3 N2 1.498(4) . ?
C4 C5 1.395(5) . ?
C4 N3 1.339(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.364(5) . ?
C6 C7 1.475(5) . ?
C6 N4 1.340(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 N5 1.477(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.509(5) . ?
C8 N5 1.495(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 N6 1.478(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.509(5) . ?
C10 N6 1.479(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 N7 1.494(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.489(5) . ?
C12 N7 1.479(4) . ?
C13 C14 1.391(5) . ?
C13 N8 1.336(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.368(5) . ?
C15 C16 1.485(5) . ?
C15 N9 1.349(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 N10 1.482(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.511(5) . ?
C17 N10 1.480(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 N1 1.470(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.513(5) . ?
C19 N1 1.468(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 N11 1.504(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.489(5) . ?
C21 N11 1.474(5) . ?
C22 C23 1.390(5) . ?
C22 N12 1.337(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.373(5) . ?
C24 C25 1.489(5) . ?
C24 N13 1.345(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 N14 1.491(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.524(5) . ?
C26 N14 1.486(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 N6 1.465(4) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N3 N4 1.347(4) . ?
N4 H4 0.8600 . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8900 . ?
N8 N9 1.345(4) . ?
N9 H9 0.8600 . ?
N10 H10C 0.8900 . ?
N10 H10D 0.8900 . ?
N11 H11C 0.8900 . ?
N11 H11D 0.8900 . ?
N12 N13 1.349(4) . ?
N13 H13 0.8600 . ?
N14 H14A 0.8900 . ?
N14 H14B 0.8900 . ?
N3N O31 1.240(4) . ?
N3N O32 1.219(4) . ?
N3N O33 1.272(4) . ?
N4N O41 1.239(5) . ?
N4N O42 1.218(4) . ?
N4N O43 1.252(4) . ?
N5N O51 1.238(4) . ?
N5N O52 1.237(4) . ?
N5N O53 1.255(4) . ?
N6N O61 1.252(4) . ?
N6N O62 1.234(4) . ?
N6N O63 1.254(4) . ?
N2N O21 1.268(6) . ?
N2N O22 1.303(8) . ?
N2N O23 1.269(11) . ?
N2N O1AA 1.067(15) . ?
N2N O0AA 1.208(18) . ?
N1N O11A 1.152(9) . ?
N1N O13A 1.182(7) . ?
N1N O12A 1.268(6) . ?
N1N O13B 1.218(15) . ?
N1N O11B 1.345(8) . ?
N1N O12B 1.170(15) . ?
O1 H1C 0.8495 . ?
O1 H1D 0.8505 . ?
O2 H2E 0.830(12) . ?
O2 H2F 0.825(12) . ?
O3 H3C 0.836(12) . ?
O3 H3D 0.840(12) . ?
O4 H4A 0.850(12) . ?
O4 H4B 0.859(12) . ?
O5 H5C 0.832(12) . ?
O5 H5D 0.828(12) . ?

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
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
N1 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
N1 C1 C2 112.6(3) . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N2 C2 C1 112.2(3) . . ?
N2 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C4 C3 N2 111.5(3) . . ?
N2 C3 H3A 109.3 . . ?
N2 C3 H3B 109.3 . . ?
C5 C4 C3 129.2(4) . . ?
N3 C4 C3 120.3(3) . . ?
N3 C4 C5 110.5(3) . . ?
C4 C5 H5 126.9 . . ?
C6 C5 C4 106.2(3) . . ?
C6 C5 H5 126.9 . . ?
C5 C6 C7 133.7(4) . . ?
N4 C6 C5 105.7(3) . . ?
N4 C6 C7 120.6(3) . . ?
C6 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
C6 C7 N5 111.8(3) . . ?
H7A C7 H7B 107.9 . . ?
N5 C7 H7A 109.3 . . ?
N5 C7 H7B 109.3 . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
N5 C8 H8A 109.1 . . ?
N5 C8 H8B 109.1 . . ?
N5 C8 C9 112.6(3) . . ?
C8 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
N6 C9 C8 114.0(3) . . ?
N6 C9 H9A 108.8 . . ?
N6 C9 H9B 108.8 . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
N6 C10 H10A 109.3 . . ?
N6 C10 H10B 109.3 . . ?
N6 C10 C11 111.7(3) . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
N7 C11 C10 111.2(3) . . ?
N7 C11 H11A 109.4 . . ?
N7 C11 H11B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C13 C12 H12A 109.4 . . ?
C13 C12 H12B 109.4 . . ?
N7 C12 H12A 109.4 . . ?
N7 C12 H12B 109.4 . . ?
N7 C12 C13 111.3(3) . . ?
C14 C13 C12 129.7(4) . . ?
N8 C13 C12 118.9(3) . . ?
N8 C13 C14 111.3(3) . . ?
C13 C14 H14 127.2 . . ?
C15 C14 C13 105.5(3) . . ?
C15 C14 H14 127.2 . . ?
C14 C15 C16 132.2(4) . . ?
N9 C15 C14 106.2(3) . . ?
N9 C15 C16 121.6(3) . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
N10 C16 C15 111.4(3) . . ?
N10 C16 H16A 109.4 . . ?
N10 C16 H16B 109.4 . . ?
H17A C17 H17B 108.1 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
N10 C17 H17A 109.5 . . ?
N10 C17 H17B 109.5 . . ?
N10 C17 C18 110.8(3) . . ?
C17 C18 H18A 108.9 . . ?
C17 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
N1 C18 C17 113.5(3) . . ?
N1 C18 H18A 108.9 . . ?
N1 C18 H18B 108.9 . . ?
H19A C19 H19B 107.5 . . ?
C20 C19 H19A 108.4 . . ?
C20 C19 H19B 108.4 . . ?
N1 C19 H19A 108.4 . . ?
N1 C19 H19B 108.4 . . ?
N1 C19 C20 115.4(3) . . ?
C19 C20 H20A 108.4 . . ?
C19 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
N11 C20 C19 115.3(3) . . ?
N11 C20 H20A 108.4 . . ?
N11 C20 H20B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C22 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
N11 C21 H21A 108.6 . . ?
N11 C21 H21B 108.6 . . ?
N11 C21 C22 114.9(3) . . ?
C23 C22 C21 133.0(4) . . ?
N12 C22 C21 116.1(3) . . ?
N12 C22 C23 110.8(3) . . ?
C22 C23 H23 127.0 . . ?
C24 C23 C22 105.9(3) . . ?
C24 C23 H23 127.0 . . ?
C23 C24 C25 133.5(4) . . ?
N13 C24 C23 105.9(3) . . ?
N13 C24 C25 120.6(3) . . ?
C24 C25 H25A 108.9 . . ?
C24 C25 H25B 108.9 . . ?
C24 C25 N14 113.2(3) . . ?
H25A C25 H25B 107.8 . . ?
N14 C25 H25A 108.9 . . ?
N14 C25 H25B 108.9 . . ?
H26A C26 H26B 108.3 . . ?
C27 C26 H26A 109.8 . . ?
C27 C26 H26B 109.8 . . ?
N14 C26 H26A 109.8 . . ?
N14 C26 H26B 109.8 . . ?
N14 C26 C27 109.2(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
N6 C27 C26 110.5(3) . . ?
N6 C27 H27A 109.5 . . ?
N6 C27 H27B 109.5 . . ?
C18 N1 C1 107.5(3) . . ?
C19 N1 C1 111.0(3) . . ?
C19 N1 C18 109.3(3) . . ?
C2 N2 C3 111.7(3) . . ?
C2 N2 H2C 109.3 . . ?
C2 N2 H2D 109.3 . . ?
C3 N2 H2C 109.3 . . ?
C3 N2 H2D 109.3 . . ?
H2C N2 H2D 107.9 . . ?
C4 N3 N4 104.1(3) . . ?
C6 N4 N3 113.4(3) . . ?
C6 N4 H4 123.3 . . ?
N3 N4 H4 123.3 . . ?
C7 N5 C8 112.1(3) . . ?
C7 N5 H5A 109.2 . . ?
C7 N5 H5B 109.2 . . ?
C8 N5 H5A 109.2 . . ?
C8 N5 H5B 109.2 . . ?
H5A N5 H5B 107.9 . . ?
C9 N6 C10 109.4(3) . . ?
C27 N6 C9 111.2(3) . . ?
C27 N6 C10 109.9(3) . . ?
C11 N7 H7C 108.7 . . ?
C11 N7 H7D 108.7 . . ?
C12 N7 C11 114.2(3) . . ?
C12 N7 H7C 108.7 . . ?
C12 N7 H7D 108.7 . . ?
H7C N7 H7D 107.6 . . ?
C13 N8 N9 104.2(3) . . ?
C15 N9 H9 123.6 . . ?
N8 N9 C15 112.8(3) . . ?
N8 N9 H9 123.6 . . ?
C16 N10 H10C 108.9 . . ?
C16 N10 H10D 108.9 . . ?
C17 N10 C16 113.4(3) . . ?
C17 N10 H10C 108.9 . . ?
C17 N10 H10D 108.9 . . ?
H10C N10 H10D 107.7 . . ?
C20 N11 H11C 109.5 . . ?
C20 N11 H11D 109.5 . . ?
C21 N11 C20 110.5(3) . . ?
C21 N11 H11C 109.5 . . ?
C21 N11 H11D 109.5 . . ?
H11C N11 H11D 108.1 . . ?
C22 N12 N13 104.6(3) . . ?
C24 N13 N12 112.8(3) . . ?
C24 N13 H13 123.6 . . ?
N12 N13 H13 123.6 . . ?
C25 N14 H14A 108.6 . . ?
C25 N14 H14B 108.6 . . ?
C26 N14 C25 114.7(3) . . ?
C26 N14 H14A 108.6 . . ?
C26 N14 H14B 108.6 . . ?
H14A N14 H14B 107.6 . . ?
O31 N3N O33 119.3(4) . . ?
O32 N3N O31 122.3(3) . . ?
O32 N3N O33 118.3(3) . . ?
O41 N4N O43 119.3(4) . . ?
O42 N4N O41 120.2(4) . . ?
O42 N4N O43 120.4(4) . . ?
O51 N5N O53 118.9(4) . . ?
O52 N5N O51 120.3(4) . . ?
O52 N5N O53 120.8(4) . . ?
O61 N6N O63 118.9(3) . . ?
O62 N6N O61 120.6(3) . . ?
O62 N6N O63 120.6(4) . . ?
O21 N2N O22 108.2(7) . . ?
O21 N2N O23 121.8(10) . . ?
O23 N2N O22 128.9(9) . . ?
O1AA N2N O21 117.4(12) . . ?
O1AA N2N O0AA 116.3(13) . . ?
O0AA N2N O21 103.6(11) . . ?
O11A N1N O13A 126.4(9) . . ?
O11A N1N O12A 112.6(8) . . ?
O13A N1N O12A 120.5(7) . . ?
O13B N1N O11B 108.5(13) . . ?
O12B N1N O13B 135.8(17) . . ?
O12B N1N O11B 115.2(16) . . ?
H1C O1 H1D 109.5 . . ?
H2E O2 H2F 108.8 . . ?
H3C O3 H3D 103.0 . . ?
H4A O4 H4B 104.0 . . ?
H5C O5 H5D 102.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2C O63 0.89 2.11 2.976(4) 164.8 2_655 yes
N2 H2D O13A 0.89 2.08 2.959(7) 171.3 . yes
N4 H4 O43 0.86 2.05 2.867(4) 158.5 4_576 yes
N5 H5A O23 0.89 2.07 2.842(13) 144.8 4_566 yes
N5 H5B O31 0.89 1.96 2.816(4) 160.5 2_545 yes
N7 H7C O33 0.89 1.99 2.849(4) 161.3 2_545 yes
N7 H7D O12A 0.89 2.41 2.968(8) 120.8 . yes
N7 H7D O12B 0.89 2.08 2.901(15) 152.9 . yes
N9 H9 O33 0.86 2.05 2.886(4) 163.7 4_575 yes
N10 H10C O4 0.89 1.79 2.665(4) 167.6 . yes
N10 H10D O13A 0.89 2.31 3.005(6) 134.9 . yes
N11 H11C O2 0.89 2.01 2.816(4) 149.5 . yes
N11 H11D O51 0.89 2.35 2.970(4) 127.0 . yes
N11 H11D O53 0.89 2.06 2.946(4) 175.0 . yes
N13 H13 O63 0.86 2.12 2.838(4) 140.4 4_566 yes
N14 H14A O61 0.89 1.93 2.819(4) 174.9 2_645 yes
N14 H14B O5 0.89 1.80 2.693(4) 175.7 4_566 yes
O1 H1C O43 0.85 2.07 2.903(5) 167.3 1_545 yes
O3 H3C O12A 0.84 2.14 2.946(10) 162.6 . yes
O3 H3C O13B 0.84 2.08 2.634(16) 123.6 . yes
O3 H3D N8 0.84 2.10 2.893(5) 157.1 3_565 yes
O4 H4B O3 0.86 1.97 2.719(5) 145.0 . yes
O5 H5C O22 0.83 1.93 2.760(6) 173.1 . yes
O5 H5D O52 0.83 1.96 2.769(5) 167.2 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 N2 C3 168.0(3) . . . . ?
C2 C1 N1 C18 85.9(3) . . . . ?
C2 C1 N1 C19 -154.6(3) . . . . ?
C3 C4 C5 C6 177.7(3) . . . . ?
C3 C4 N3 N4 -177.8(3) . . . . ?
C4 C3 N2 C2 179.2(3) . . . . ?
C4 C5 C6 C7 179.5(4) . . . . ?
C4 C5 C6 N4 0.3(4) . . . . ?
C4 N3 N4 C6 -0.6(4) . . . . ?
C5 C4 N3 N4 0.8(4) . . . . ?
C5 C6 C7 N5 36.3(6) . . . . ?
C5 C6 N4 N3 0.2(4) . . . . ?
C6 C7 N5 C8 172.6(3) . . . . ?
C7 C6 N4 N3 -179.1(3) . . . . ?
C8 C9 N6 C10 -167.5(3) . . . . ?
C8 C9 N6 C27 71.0(4) . . . . ?
C9 C8 N5 C7 157.6(3) . . . . ?
C10 C11 N7 C12 87.1(4) . . . . ?
C11 C10 N6 C9 78.9(3) . . . . ?
C11 C10 N6 C27 -158.8(3) . . . . ?
C12 C13 C14 C15 -179.6(3) . . . . ?
C12 C13 N8 N9 179.3(3) . . . . ?
C13 C12 N7 C11 172.5(3) . . . . ?
C13 C14 C15 C16 178.5(4) . . . . ?
C13 C14 C15 N9 0.3(4) . . . . ?
C13 N8 N9 C15 0.5(4) . . . . ?
C14 C13 N8 N9 -0.3(4) . . . . ?
C14 C15 C16 N10 -94.2(5) . . . . ?
C14 C15 N9 N8 -0.5(4) . . . . ?
C15 C16 N10 C17 178.9(3) . . . . ?
C16 C15 N9 N8 -179.0(3) . . . . ?
C17 C18 N1 C1 -161.9(3) . . . . ?
C17 C18 N1 C19 77.5(4) . . . . ?
C18 C17 N10 C16 172.2(3) . . . . ?
C19 C20 N11 C21 147.2(3) . . . . ?
C20 C19 N1 C1 72.1(4) . . . . ?
C20 C19 N1 C18 -169.4(3) . . . . ?
C21 C22 C23 C24 175.5(4) . . . . ?
C21 C22 N12 N13 -176.2(3) . . . . ?
C22 C21 N11 C20 -178.6(3) . . . . ?
C22 C23 C24 C25 -179.8(3) . . . . ?
C22 C23 C24 N13 -0.2(4) . . . . ?
C22 N12 N13 C24 -0.2(4) . . . . ?
C23 C22 N12 N13 0.1(4) . . . . ?
C23 C24 C25 N14 -88.9(5) . . . . ?
C23 C24 N13 N12 0.2(4) . . . . ?
C24 C25 N14 C26 72.0(4) . . . . ?
C25 C24 N13 N12 180.0(3) . . . . ?
C26 C27 N6 C9 -157.2(3) . . . . ?
C26 C27 N6 C10 81.6(3) . . . . ?
C27 C26 N14 C25 175.2(3) . . . . ?
N1 C1 C2 N2 77.4(4) . . . . ?
N1 C19 C20 N11 71.1(4) . . . . ?
N2 C3 C4 C5 -88.8(5) . . . . ?
N2 C3 C4 N3 89.4(4) . . . . ?
N3 C4 C5 C6 -0.7(4) . . . . ?
N4 C6 C7 N5 -144.7(4) . . . . ?
N5 C8 C9 N6 49.7(4) . . . . ?
N6 C10 C11 N7 62.6(4) . . . . ?
N7 C12 C13 C14 112.2(4) . . . . ?
N7 C12 C13 N8 -67.4(4) . . . . ?
N8 C13 C14 C15 0.0(4) . . . . ?
N9 C15 C16 N10 83.8(4) . . . . ?
N10 C17 C18 N1 56.0(4) . . . . ?
N11 C21 C22 C23 15.7(6) . . . . ?
N11 C21 C22 N12 -169.0(3) . . . . ?
N12 C22 C23 C24 0.0(4) . . . . ?
N13 C24 C25 N14 91.5(4) . . . . ?
N14 C26 C27 N6 -168.8(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_crystal3_phos11
_database_code_depnum_ccdc_archive 'CCDC 1912380'
loop_
_audit_author_name
_audit_author_address
'Javier Pitarch-Jarque'
;Universitat de Valencia
Spain
;
_audit_update_record             
;
2019-04-26 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_audit_creation_date             2019-03-11
_audit_creation_method           
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H58 N14, 11(H2 O4 P), 4(H2 O)'
_chemical_formula_sum            'C27 H88 N14 O48 P11'
_chemical_formula_weight         1717.78
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   14.8632(2)
_cell_length_b                   20.1186(2)
_cell_length_c                   24.7970(4)
_cell_angle_alpha                90
_cell_angle_beta                 112.3250(10)
_cell_angle_gamma                90
_cell_volume                     6859.17(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22633
_cell_measurement_temperature    288.15
_cell_measurement_theta_max      74.9314
_cell_measurement_theta_min      2.9192
_shelx_estimated_absorpt_T_max   0.778
_shelx_estimated_absorpt_T_min   0.464
_exptl_absorpt_coefficient_mu    3.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3588
_exptl_crystal_size_max          0.2503
_exptl_crystal_size_mid          0.2091
_exptl_crystal_size_min          0.0728
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            61232
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.483
_diffrn_reflns_theta_min         2.922
_diffrn_ambient_temperature      288.15
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10750
_reflns_number_total             14093
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42)'
_computing_data_collection       
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42)'
_computing_data_reduction        
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.493
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1076
_refine_ls_number_reflns         14093
_refine_ls_number_restraints     105
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0741
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1662P)²+2.3204P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2239
_refine_ls_wR_factor_ref         0.2432
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H4A,H4B} of O4, H11 of O11, H12C of O12, H93 of O93, {H2E,
  H2F} of O2, H42 of O42, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  H7AA of O74, H73 of O73, H112 of O112, H51 of O51, H76 of O76, H115 of O115,
   H72 of O72, H22 of O22, H91 of O91, H77 of O77, H31 of O31, H11E of O117,
  H111 of O111, H32 of O32, H21 of O21, H7BB of O75, H56 of O56, H5BA of O57,
  H63 of O63, H81 of O81, H52 of O52, H92 of O92, H41 of O41, {H1AA,H1AB} of
  O1A, {H3C,H3D} of O3, H61 of O61, H102 of O102, {H1BA,H1BB} of O1B, H83 of
  O83, H101 of O101
2. Restrained distances
 O31-H3C
 2.1 with sigma of 0.1
 O94-H3D
 1.9 with sigma of 0.1
 H21-H3
 2.5 with sigma of 0.2
 O1B-H1BB = O1B-H1BA
 0.85 with sigma of 0.02
 H1BB-O56
 2 with sigma of 0.1
 O84_$1-H91
 1.7 with sigma of 0.1
 H1BA-O64
 2.4 with sigma of 0.1
 O111-O114 \\sim O111-O113 \\sim O111-O112 \\sim O114-O113 \\sim O114-O112
\\sim O113-O112
 with sigma of 0.05
 O116-O118 \\sim O116-O117 \\sim O116-O115 \\sim O118-O117 \\sim O118-O115
\\sim O117-O115
 with sigma of 0.05
3. Rigid bond restraints
 O55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O116
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P7, O71, O72, O75, O76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
P3 \\sim O31 \\sim O34: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
P2 \\sim O21 \\sim O22: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O114) \\sim Ueq, Uanis(O112) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O55) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(O118) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O56) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(P11B)=Sof(O115)=Sof(H115)=Sof(O116)=Sof(O117)=Sof(H11E)=Sof(O118)=1-FVAR(1)
 Sof(P11A)=Sof(O111)=Sof(H111)=Sof(O112)=Sof(H112)=Sof(O113)=Sof(O114)=FVAR(1)
 Sof(O75)=Sof(O76)=Sof(O77)=1-FVAR(2)
 Sof(H7BB)=Sof(H76)=Sof(H77)=0.66667*(1-FVAR(3))
 Sof(H72)=Sof(H73)=Sof(H7AA)=0.66667*FVAR(3)
 Sof(O72)=Sof(O73)=Sof(O74)=FVAR(2)
 Sof(P5B)=Sof(O55)=Sof(O56)=Sof(H56)=Sof(O57)=Sof(H5BA)=Sof(O58)=1-FVAR(3)
 Sof(P5A)=Sof(O51)=Sof(H51)=Sof(O52)=Sof(H52)=Sof(O53)=Sof(O54)=FVAR(3)
 Sof(O1B)=Sof(H1BA)=Sof(H1BB)=1-FVAR(4)
 Sof(O1A)=Sof(H1AA)=Sof(H1AB)=FVAR(4)
 Fixed Sof: H91(0.66666) H92(0.66666) H93(0.66666)
6.a Free rotating group:
 O3(H3C,H3D), O1A(H1AA,H1AB), O2(H2E,H2F), O4(H4A,H4B)
6.b Rotating group with stretchable bonds:
 O42(H42), O1B(H1BA,H1BB)
6.c Ternary CH refined with riding coordinates:
 N1(H1), N6(H6)
6.d Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N5(H5A,H5B), N7(H7A,H7B), N10(H10A,H10B), N11(H11A,H11B),
 N14(H14A,H14B), C2(H2C,H2D), C3(H3A,H3B), C7(H7C,H7D), C8(H8A,H8B), C9(H9A,
 H9B), C10(H10C,H10D), C11(H11C,H11D), C12(H12A,H12B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B)
6.e Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N8(H8), N9(H9), N12(H12), N13(H13), C5(H5), C14(H14), C23(H23)
6.f Tetrahedral OH refined with riding coordinates:
 O117(H11E), O21(H21), O92(H92), O56(H56)
6.g Idealised tetrahedral OH refined as rotating group:
 O72(H72), O73(H73), O74(H7AA), O75(H7BB), O76(H76), O77(H77), O11(H11),
 O12(H12C), O115(H115), O22(H22), O31(H31), O32(H32), O91(H91), O93(H93),
 O111(H111), O112(H112), O51(H51), O52(H52), O61(H61), O63(H63), O57(H5BA),
 O41(H41), O81(H81), O83(H83), O101(H101), O102(H102)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.8894(2) 0.24153(14) 0.41309(13) 0.0472(6) Uani 1 1 d . . . . .
H1 H 0.823230 0.252226 0.409819 0.057 Uiso 1 1 calc R . . . .
N2 N 0.8081(3) 0.29334(19) 0.25598(15) 0.0637(9) Uani 1 1 d . . . . .
H2A H 0.767806 0.258862 0.244214 0.076 Uiso 1 1 calc R . . . .
H2B H 0.860744 0.284223 0.248441 0.076 Uiso 1 1 calc R . . . .
N3 N 0.6682(3) 0.41273(18) 0.27207(15) 0.0590(8) Uani 1 1 d . . . . .
H3 H 0.717449 0.434391 0.295474 0.071 Uiso 1 1 calc DR . . . .
N4 N 0.5777(2) 0.41510(16) 0.26975(14) 0.0562(7) Uani 1 1 d . . . . .
H4 H 0.559123 0.439631 0.292002 0.067 Uiso 1 1 calc R . . . .
N5 N 0.3969(2) 0.31109(16) 0.25416(15) 0.0566(7) Uani 1 1 d . . . . .
H5A H 0.397873 0.273009 0.236135 0.068 Uiso 1 1 calc R . . . .
H5B H 0.443684 0.309636 0.289576 0.068 Uiso 1 1 calc R . . . .
N6 N 0.3349(2) 0.24440(16) 0.34770(15) 0.0552(7) Uani 1 1 d . . . . .
H6 H 0.400447 0.233674 0.349722 0.066 Uiso 1 1 calc R . . . .
N7 N 0.4238(2) 0.35052(16) 0.48401(16) 0.0566(8) Uani 1 1 d . . . . .
H7A H 0.365925 0.355570 0.486326 0.068 Uiso 1 1 calc R . . . .
H7B H 0.435837 0.386909 0.467444 0.068 Uiso 1 1 calc R . . . .
N8 N 0.6288(2) 0.42757(15) 0.55562(14) 0.0510(7) Uani 1 1 d . . . . .
H8 H 0.593993 0.461012 0.557342 0.061 Uiso 1 1 calc R . . . .
N9 N 0.7205(2) 0.43063(14) 0.55939(14) 0.0492(6) Uani 1 1 d . . . . .
H9 H 0.754127 0.466385 0.563438 0.059 Uiso 1 1 calc R . . . .
N10 N 0.8596(2) 0.34759(14) 0.50226(12) 0.0465(6) Uani 1 1 d . . . . .
H10A H 0.807626 0.325245 0.479102 0.056 Uiso 1 1 calc R . . . .
H10B H 0.858912 0.387421 0.486491 0.056 Uiso 1 1 calc R . . . .
N11 N 0.8622(3) 0.06033(18) 0.44444(16) 0.0657(9) Uani 1 1 d . . . . .
H11A H 0.846229 0.069024 0.474873 0.079 Uiso 1 1 calc R . . . .
H11B H 0.925165 0.050155 0.458079 0.079 Uiso 1 1 calc R . . . .
N12 N 0.6715(3) -0.0167(2) 0.44692(17) 0.0699(9) Uani 1 1 d . . . . .
H12 H 0.710513 -0.033078 0.479416 0.084 Uiso 1 1 calc R . . . .
N13 N 0.5755(3) -0.0102(2) 0.43263(18) 0.0717(10) Uani 1 1 d . . . . .
H13 H 0.542623 -0.021543 0.453163 0.086 Uiso 1 1 calc R . . . .
N14 N 0.4170(3) 0.10235(18) 0.36516(17) 0.0621(8) Uani 1 1 d . . . . .
H14A H 0.449704 0.130470 0.351645 0.074 Uiso 1 1 calc R . . . .
H14B H 0.439230 0.106995 0.403721 0.074 Uiso 1 1 calc R . . . .
C1 C 0.8891(3) 0.2402(2) 0.35248(18) 0.0566(9) Uani 1 1 d . . . . .
H1A H 0.853(4) 0.198(3) 0.335(2) 0.068 Uiso 1 1 d R . . . .
C2 C 0.8369(3) 0.30197(19) 0.31966(17) 0.0581(9) Uani 1 1 d . . . . .
H2C H 0.779491 0.310250 0.328307 0.070 Uiso 1 1 calc R . . . .
H2D H 0.879542 0.340177 0.332597 0.070 Uiso 1 1 calc R . . . .
C3 C 0.7592(4) 0.3540(3) 0.2221(2) 0.0691(11) Uani 1 1 d . . . . .
H3A H 0.803325 0.391525 0.234337 0.083 Uiso 1 1 calc R . . . .
H3B H 0.744142 0.346512 0.180947 0.083 Uiso 1 1 calc R . . . .
C4 C 0.6676(3) 0.3702(2) 0.23099(18) 0.0586(9) Uani 1 1 d . . . . .
C5 C 0.5734(3) 0.3455(2) 0.20184(19) 0.0629(10) Uani 1 1 d . . . . .
H5 H 0.552903 0.315613 0.170908 0.076 Uiso 1 1 calc R . . . .
C6 C 0.5182(3) 0.37444(19) 0.22832(17) 0.0564(8) Uani 1 1 d . . . . .
C7 C 0.4153(3) 0.3687(2) 0.2200(2) 0.0622(9) Uani 1 1 d . . . . .
H7C H 0.376589 0.362522 0.178907 0.075 Uiso 1 1 calc R . . . .
H7D H 0.394555 0.409708 0.232332 0.075 Uiso 1 1 calc R . . . .
C8 C 0.3013(3) 0.3191(2) 0.2592(2) 0.0642(10) Uani 1 1 d . . . . .
H8A H 0.252138 0.326457 0.220628 0.077 Uiso 1 1 calc R . . . .
H8B H 0.303530 0.358336 0.282384 0.077 Uiso 1 1 calc R . . . .
C9 C 0.2714(3) 0.2610(2) 0.2862(2) 0.0671(10) Uani 1 1 d . . . . .
H9A H 0.206248 0.269320 0.284809 0.081 Uiso 1 1 calc R . . . .
H9B H 0.267923 0.222156 0.262289 0.081 Uiso 1 1 calc R . . . .
C10 C 0.3403(3) 0.3004(2) 0.3868(2) 0.0612(9) Uani 1 1 d . . . . .
H10C H 0.278426 0.304565 0.391276 0.073 Uiso 1 1 calc R . . . .
H10D H 0.351272 0.341050 0.369272 0.073 Uiso 1 1 calc R . . . .
C11 C 0.4199(3) 0.2921(2) 0.44607(19) 0.0581(9) Uani 1 1 d . . . . .
H11C H 0.408458 0.252040 0.464255 0.070 Uiso 1 1 calc R . . . .
H11D H 0.481889 0.287401 0.441887 0.070 Uiso 1 1 calc R . . . .
C12 C 0.4996(3) 0.3443(2) 0.54440(19) 0.0586(9) Uani 1 1 d . . . . .
H12A H 0.481349 0.372212 0.570496 0.070 Uiso 1 1 calc R . . . .
H12B H 0.501183 0.298684 0.557341 0.070 Uiso 1 1 calc R . . . .
C13 C 0.5994(3) 0.36362(18) 0.54866(17) 0.0532(8) Uani 1 1 d . . . . .
C14 C 0.6763(3) 0.32575(18) 0.54874(18) 0.0551(8) Uani 1 1 d . . . . .
H14 H 0.677365 0.279827 0.544763 0.066 Uiso 1 1 calc R . . . .
C15 C 0.7516(3) 0.36921(18) 0.55586(16) 0.0495(7) Uani 1 1 d . . . . .
C16 C 0.8545(3) 0.3559(2) 0.56109(16) 0.0532(8) Uani 1 1 d . . . . .
H16A H 0.895908 0.392516 0.581387 0.064 Uiso 1 1 calc R . . . .
H16B H 0.878329 0.315843 0.583878 0.064 Uiso 1 1 calc R . . . .
C17 C 0.9493(3) 0.31133(19) 0.50624(16) 0.0521(8) Uani 1 1 d . . . . .
H17A H 0.952660 0.269941 0.526987 0.063 Uiso 1 1 calc R . . . .
H17B H 1.005450 0.337781 0.529015 0.063 Uiso 1 1 calc R . . . .
C18 C 0.9551(3) 0.29591(19) 0.44810(17) 0.0521(8) Uani 1 1 d . . . . .
H18A H 0.940205 0.336180 0.424850 0.063 Uiso 1 1 calc R . . . .
H18B H 1.021683 0.283835 0.454789 0.063 Uiso 1 1 calc R . . . .
C19 C 0.9156(3) 0.17518(19) 0.44301(18) 0.0571(9) Uani 1 1 d . . . . .
H19A H 0.913219 0.178098 0.481482 0.069 Uiso 1 1 calc R . . . .
H19B H 0.981601 0.163676 0.447742 0.069 Uiso 1 1 calc R . . . .
C20 C 0.8463(3) 0.12087(19) 0.40811(19) 0.0575(9) Uani 1 1 d . . . . .
H20A H 0.779553 0.135742 0.396759 0.069 Uiso 1 1 calc R . . . .
H20B H 0.858012 0.111195 0.373012 0.069 Uiso 1 1 calc R . . . .
C21 C 0.8050(4) 0.0014(2) 0.4126(2) 0.0644(10) Uani 1 1 d . . . . .
H21A H 0.833401 -0.038716 0.434023 0.077 Uiso 1 1 calc R . . . .
H21B H 0.809224 -0.001568 0.374565 0.077 Uiso 1 1 calc R . . . .
C22 C 0.6997(3) 0.00528(19) 0.40488(19) 0.0605(9) Uani 1 1 d . . . . .
C23 C 0.6183(4) 0.0285(2) 0.36078(18) 0.0623(10) Uani 1 1 d . . . . .
H23 H 0.614449 0.047460 0.325773 0.075 Uiso 1 1 calc R . . . .
C24 C 0.5418(4) 0.0175(2) 0.3798(2) 0.0642(10) Uani 1 1 d . . . . .
C25 C 0.4360(3) 0.0339(2) 0.3512(2) 0.0642(10) Uani 1 1 d . . . . .
H25A H 0.415479 0.029129 0.309278 0.077 Uiso 1 1 calc R . . . .
H25B H 0.398506 0.003002 0.364331 0.077 Uiso 1 1 calc R . . . .
C26 C 0.3125(3) 0.1202(2) 0.34023(19) 0.0616(9) Uani 1 1 d . . . . .
H26A H 0.275110 0.085121 0.348834 0.074 Uiso 1 1 calc R . . . .
H26B H 0.291081 0.123684 0.298196 0.074 Uiso 1 1 calc R . . . .
C27 C 0.2930(3) 0.1860(2) 0.3648(2) 0.0625(10) Uani 1 1 d . . . . .
H27A H 0.223213 0.192143 0.351881 0.075 Uiso 1 1 calc R . . . .
H27B H 0.319023 0.183101 0.407010 0.075 Uiso 1 1 calc R . . . .
P7 P 0.89703(8) -0.05679(5) 0.58771(5) 0.0615(3) Uani 1 1 d . U . . .
O71 O 0.9584(3) -0.0260(2) 0.5592(2) 0.1019(13) Uani 1 1 d . U . . .
O72 O 0.9561(4) -0.1146(3) 0.6263(2) 0.0756(15) Uani 0.676(6) 1 d . U P A 1
H72 H 1.010434 -0.101338 0.647011 0.113 Uiso 0.451(4) 1 calc GR . P A 1
O73 O 0.8734(5) -0.0060(3) 0.6272(2) 0.0896(19) Uani 0.676(6) 1 d . . P A 1
H73 H 0.815146 0.002798 0.613279 0.134 Uiso 0.451(4) 1 calc GR . P A 1
O74 O 0.8017(5) -0.0798(3) 0.5453(3) 0.109(3) Uani 0.676(6) 1 d . . P A 1
H7AA H 0.804028 -0.119877 0.540057 0.164 Uiso 0.451(4) 1 calc GR . P A 1
O75 O 0.9392(15) -0.0544(8) 0.6520(6) 0.115(5) Uani 0.324(6) 1 d . U P A 2
H7BB H 0.940198 -0.015856 0.662878 0.172 Uiso 0.216(4) 1 calc GR . P A 2
O76 O 0.8875(8) -0.1360(5) 0.5736(6) 0.081(3) Uani 0.324(6) 1 d . U P A 2
H76 H 0.830053 -0.145669 0.556300 0.122 Uiso 0.216(4) 1 calc GR . P A 2
O77 O 0.7945(9) -0.0284(6) 0.5602(7) 0.091(4) Uani 0.324(6) 1 d . . P A 2
H77 H 0.797522 0.011329 0.553662 0.137 Uiso 0.216(4) 1 calc GR . P A 2
P1 P 0.62750(6) 0.24794(4) 0.38309(4) 0.0455(2) Uani 1 1 d . . . . .
O11 O 0.6414(2) 0.21253(15) 0.33094(12) 0.0586(6) Uani 1 1 d . . . . .
H11 H 0.592564 0.190936 0.312605 0.070 Uiso 1 1 calc GR . . . .
O12 O 0.5873(2) 0.19561(15) 0.41382(13) 0.0633(7) Uani 1 1 d . . . . .
H12C H 0.630173 0.184817 0.444817 0.076 Uiso 1 1 calc GR . . . .
O13 O 0.5529(2) 0.30269(14) 0.36172(13) 0.0582(6) Uani 1 1 d . . . . .
O14 O 0.72653(19) 0.27139(15) 0.42243(12) 0.0584(6) Uani 1 1 d . . . . .
P11B P 0.9898(3) 0.1695(2) 0.23122(19) 0.0891(13) Uani 0.374(3) 1 d . . P B 2
O115 O 0.9602(5) 0.2466(3) 0.2291(3) 0.0570(19) Uani 0.374(3) 1 d D . P B 2
H115 H 0.996840 0.265284 0.258633 0.085 Uiso 0.374(3) 1 calc GR . P B 2
O116 O 0.9853(17) 0.1488(11) 0.2889(7) 0.188(9) Uani 0.374(3) 1 d D U P B 2
O117 O 0.9220(15) 0.1261(10) 0.1865(8) 0.165(10) Uani 0.374(3) 1 d D . P B 2
H11E H 0.895000 0.101063 0.201688 0.248 Uiso 0.374(3) 1 calc R . P B 2
O118 O 1.0897(12) 0.1483(10) 0.2321(8) 0.149(6) Uani 0.374(3) 1 d D U P B 2
P2 P 0.83091(7) 0.50158(5) 0.41370(4) 0.0513(2) Uani 1 1 d . U . . .
O21 O 0.8196(3) 0.43939(18) 0.37449(15) 0.0863(11) Uani 1 1 d . U . . .
H21 H 0.871754 0.431042 0.371879 0.129 Uiso 1 1 calc DR . . . .
O22 O 0.9126(3) 0.5460(2) 0.4078(2) 0.0922(12) Uani 1 1 d . U . . .
H22 H 0.955508 0.522301 0.405011 0.138 Uiso 1 1 calc GR . . . .
O23 O 0.7378(2) 0.54030(15) 0.39319(13) 0.0647(7) Uani 1 1 d . . . . .
O24 O 0.8653(2) 0.47768(13) 0.47528(12) 0.0579(6) Uani 1 1 d . . . . .
P3 P 0.42768(7) 0.14325(4) 0.21262(4) 0.0510(2) Uani 1 1 d . U . . .
O31 O 0.4996(3) 0.12085(17) 0.18336(18) 0.0773(9) Uani 1 1 d D U . . .
H31 H 0.493996 0.080753 0.177007 0.116 Uiso 1 1 calc GR . . . .
O32 O 0.3581(3) 0.08400(17) 0.20796(14) 0.0738(9) Uani 1 1 d . . . . .
H32 H 0.329193 0.074198 0.173576 0.111 Uiso 1 1 calc GR . . . .
O33 O 0.4807(2) 0.15592(16) 0.27638(12) 0.0657(7) Uani 1 1 d . . . . .
O34 O 0.3748(3) 0.20258(15) 0.17963(14) 0.0726(8) Uani 1 1 d . U . . .
P9 P 0.77468(10) 0.00848(6) 0.22747(6) 0.0702(3) Uani 1 1 d . . . . .
O91 O 0.8532(4) -0.0020(2) 0.28897(18) 0.0985(13) Uani 1 1 d . . . . .
H91 H 0.844229 -0.037740 0.301970 0.148 Uiso 0.6667 1 calc DGR . P . .
O92 O 0.6776(3) 0.0080(2) 0.23597(19) 0.0900(11) Uani 1 1 d . . . . .
H92 H 0.632495 0.009021 0.204070 0.135 Uiso 0.6667 1 calc R . P . .
O93 O 0.7720(3) -0.05235(16) 0.18970(16) 0.0792(9) Uani 1 1 d . . . . .
H93 H 0.785351 -0.040975 0.161861 0.095 Uiso 0.6667 1 calc GR . P . .
O94 O 0.7911(3) 0.07068(17) 0.20073(17) 0.0775(9) Uani 1 1 d D . . . .
P11A P 0.05138(14) 0.07933(10) 0.23332(9) 0.0661(6) Uani 0.626(3) 1 d . . P B 1
O111 O 0.0735(6) 0.0128(3) 0.2649(3) 0.0881(18) Uani 0.626(3) 1 d D . P B 1
H111 H 0.114236 -0.007148 0.256272 0.132 Uiso 0.626(3) 1 calc GR . P B 1
O112 O -0.0498(5) 0.0806(5) 0.1839(3) 0.095(2) Uani 0.626(3) 1 d D U P B 1
H112 H -0.055103 0.048984 0.161993 0.142 Uiso 0.626(3) 1 calc GR . P B 1
O113 O 0.1251(5) 0.0915(4) 0.2064(4) 0.106(2) Uani 0.626(3) 1 d D . P B 1
O114 O 0.0585(5) 0.1344(3) 0.2754(3) 0.0784(15) Uani 0.626(3) 1 d D U P B 1
P5A P 0.7160(2) 0.13219(13) 0.55442(12) 0.0649(6) Uani 0.827(7) 1 d . . P C 2
O51 O 0.7874(6) 0.1769(5) 0.6012(3) 0.085(2) Uani 0.827(7) 1 d . . P C 2
H51 H 0.843131 0.164005 0.608515 0.127 Uiso 0.827(7) 1 calc GR . P C 2
O52 O 0.6166(4) 0.1647(2) 0.5485(2) 0.0839(14) Uani 0.827(7) 1 d . . P C 2
H52 H 0.588135 0.140161 0.563191 0.126 Uiso 0.827(7) 1 calc GR . P C 2
O53 O 0.7135(7) 0.0648(4) 0.5838(4) 0.0881(19) Uani 0.827(7) 1 d . . P C 2
O54 O 0.7274(3) 0.1271(2) 0.49764(18) 0.0751(13) Uani 0.827(7) 1 d . . P C 2
P6 P 0.27024(9) 0.21254(6) 0.54811(5) 0.0623(3) Uani 1 1 d . . . . .
O61 O 0.3697(2) 0.24343(18) 0.58452(15) 0.0725(8) Uani 1 1 d . . . . .
H61 H 0.369158 0.256862 0.615611 0.109 Uiso 1 1 calc GR . . . .
O62 O 0.2414(3) 0.16232(17) 0.58462(16) 0.0754(9) Uani 1 1 d . . . . .
O63 O 0.1944(3) 0.26760(19) 0.53111(19) 0.0858(10) Uani 1 1 d . . . . .
H63 H 0.211952 0.297684 0.515019 0.129 Uiso 1 1 calc GR . . . .
O64 O 0.2856(3) 0.1794(2) 0.49743(17) 0.0874(11) Uani 1 1 d D . . . .
P5B P 0.7521(11) 0.1292(8) 0.5529(7) 0.068(3) Uani 0.173(7) 1 d . . P C 1
O55 O 0.734(5) 0.061(4) 0.578(3) 0.17(3) Uani 0.173(7) 1 d . U P C 1
O56 O 0.6492(12) 0.1523(8) 0.5118(6) 0.059(5) Uani 0.173(7) 1 d D U P C 1
H56 H 0.616422 0.119850 0.496047 0.089 Uiso 0.173(7) 1 calc R . P C 1
O57 O 0.785(3) 0.1887(14) 0.5820(12) 0.070(9) Uani 0.173(7) 1 d . . P C 1
H5BA H 0.843961 0.190563 0.593278 0.105 Uiso 0.173(7) 1 calc GR . P C 1
O58 O 0.8126(17) 0.1077(9) 0.5227(9) 0.076(6) Uani 0.173(7) 1 d . U P C 1
P4 P 0.53793(7) 0.47079(5) 0.40606(5) 0.0547(2) Uani 1 1 d . . . . .
O41 O 0.6078(2) 0.52746(14) 0.44006(13) 0.0598(7) Uani 1 1 d . . . . .
H41 H 0.652488 0.530832 0.428485 0.090 Uiso 1 1 calc GR . . . .
O42 O 0.6044(2) 0.40890(17) 0.41908(15) 0.0711(8) Uani 1 1 d . . . . .
H42 H 0.585(2) 0.375(3) 0.399(2) 0.085 Uiso 1 1 d GR . . . .
O43 O 0.4607(2) 0.46457(14) 0.43115(13) 0.0607(7) Uani 1 1 d . . . . .
O44 O 0.4974(2) 0.48699(18) 0.34072(13) 0.0692(8) Uani 1 1 d . . . . .
P8 P 1.03621(9) 0.14934(7) 0.62748(6) 0.0740(3) Uani 1 1 d . . . . .
O81 O 0.9961(4) 0.1016(2) 0.57330(19) 0.1002(12) Uani 1 1 d . . . . .
H81 H 0.955590 0.076459 0.577191 0.150 Uiso 1 1 calc GR . . . .
O82 O 0.9579(3) 0.2003(2) 0.6238(2) 0.1079(14) Uani 1 1 d . . . . .
O83 O 1.1148(4) 0.1916(3) 0.6200(3) 0.125(2) Uani 1 1 d . . . . .
H83 H 1.159757 0.167719 0.620356 0.188 Uiso 1 1 calc GR . . . .
O84 O 1.0659(4) 0.1129(3) 0.6831(2) 0.1246(17) Uani 1 1 d D . . . .
P10 P 1.15643(7) 0.40043(5) 0.42910(4) 0.0516(2) Uani 1 1 d . . . . .
O101 O 1.1025(3) 0.34869(15) 0.38104(15) 0.0682(8) Uani 1 1 d . . . . .
H101 H 1.062792 0.367844 0.352839 0.102 Uiso 1 1 calc GR . . . .
O102 O 1.0755(2) 0.42819(17) 0.44823(14) 0.0672(7) Uani 1 1 d . . . . .
H102 H 1.097248 0.459190 0.470933 0.101 Uiso 1 1 calc GR . . . .
O103 O 1.2315(2) 0.36267(15) 0.47839(14) 0.0628(7) Uani 1 1 d . . . . .
O104 O 1.2015(2) 0.45428(13) 0.40507(12) 0.0610(7) Uani 1 1 d . . . . .
O3 O 0.6927(4) 0.1848(2) 0.2078(3) 0.1152(16) Uani 1 1 d . . . . .
H3C H 0.633142 0.177778 0.201684 0.173 Uiso 1 1 d DG . . . .
H3D H 0.708773 0.161685 0.184198 0.173 Uiso 1 1 d DG . . . .
O1A O 0.4486(11) 0.1091(5) 0.4899(6) 0.061(3) Uani 0.53(6) 1 d . . P D 1
H1AA H 0.494559 0.126054 0.518719 0.092 Uiso 0.53(6) 1 d G . P D 1
H1AB H 0.397195 0.120111 0.495108 0.092 Uiso 0.53(6) 1 d G . P D 1
O2 O 0.9961(3) 0.3880(2) 0.27592(19) 0.0910(11) Uani 1 1 d . . . . .
H2E H 1.020778 0.363266 0.258053 0.109 Uiso 1 1 d G . . . .
H2F H 0.987325 0.428532 0.272745 0.109 Uiso 1 1 d G . . . .
O4 O 0.1504(5) 0.1796(4) 0.1465(3) 0.1315(19) Uani 1 1 d . . . . .
H4A H 0.092357 0.174503 0.140311 0.158 Uiso 1 1 d G . . . .
H4B H 0.185899 0.181684 0.127711 0.158 Uiso 1 1 d G . . . .
O1B O 0.466(3) 0.093(3) 0.4912(10) 0.137(8) Uani 0.47(6) 1 d D . P D 2
H1BA H 0.424(3) 0.107(3) 0.5044(10) 0.205 Uiso 0.47(6) 1 d DGR . P D 2
H1BB H 0.528(3) 0.091(3) 0.5029(10) 0.205 Uiso 0.47(6) 1 d DGR . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 H1 0.9800 . ?
N1 C1 1.501(5) . ?
N1 C18 1.503(5) . ?
N1 C19 1.505(4) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.481(5) . ?
N2 C3 1.504(5) . ?
N3 H3 0.8600 . ?
N3 N4 1.326(5) . ?
N3 C4 1.328(5) . ?
N4 H4 0.8600 . ?
N4 C6 1.348(5) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 C7 1.520(5) . ?
N5 C8 1.481(5) . ?
N6 H6 0.9800 . ?
N6 C9 1.495(6) . ?
N6 C10 1.468(5) . ?
N6 C27 1.467(5) . ?
N7 H7A 0.8900 . ?
N7 H7B 0.8900 . ?
N7 C11 1.492(5) . ?
N7 C12 1.499(6) . ?
N8 H8 0.8600 . ?
N8 N9 1.331(4) . ?
N8 C13 1.349(5) . ?
N9 H9 0.8600 . ?
N9 C15 1.334(5) . ?
N10 H10A 0.8900 . ?
N10 H10B 0.8900 . ?
N10 C16 1.499(5) . ?
N10 C17 1.489(4) . ?
N11 H11A 0.8900 . ?
N11 H11B 0.8900 . ?
N11 C20 1.479(5) . ?
N11 C21 1.498(5) . ?
N12 H12 0.8600 . ?
N12 N13 1.339(6) . ?
N12 C22 1.338(6) . ?
N13 H13 0.8600 . ?
N13 C24 1.333(6) . ?
N14 H14A 0.8900 . ?
N14 H14B 0.8900 . ?
N14 C25 1.474(6) . ?
N14 C26 1.482(6) . ?
C1 H1A 1.01(5) . ?
C1 C2 1.526(5) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.495(6) . ?
C4 C5 1.400(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.361(6) . ?
C6 C7 1.468(6) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.496(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10C 0.9700 . ?
C10 H10D 0.9700 . ?
C10 C11 1.505(6) . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.497(5) . ?
C13 C14 1.374(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.378(5) . ?
C15 C16 1.508(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.509(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.526(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.506(7) . ?
C22 C23 1.368(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.405(7) . ?
C24 C25 1.496(7) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.530(6) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
P7 O71 1.486(4) . ?
P7 O72 1.550(5) . ?
P7 O73 1.546(6) . ?
P7 O74 1.481(6) . ?
P7 O75 1.475(13) . ?
P7 O76 1.626(10) . ?
P7 O77 1.524(13) . ?
O72 H72 0.8200 . ?
O73 H73 0.8200 . ?
O74 H7AA 0.8200 . ?
O75 H7BB 0.8200 . ?
O76 H76 0.8200 . ?
O77 H77 0.8200 . ?
P1 O11 1.558(3) . ?
P1 O12 1.547(3) . ?
P1 O13 1.509(3) . ?
P1 O14 1.500(3) . ?
O11 H11 0.8200 . ?
O12 H12C 0.8200 . ?
P11B O115 1.607(7) . ?
P11B O116 1.516(18) . ?
P11B O117 1.468(15) . ?
P11B O118 1.537(17) . ?
O115 H115 0.8200 . ?
O117 H11E 0.8200 . ?
P2 O21 1.554(3) . ?
P2 O22 1.558(4) . ?
P2 O23 1.499(3) . ?
P2 O24 1.494(3) . ?
O21 H21 0.8200 . ?
O22 H22 0.8200 . ?
P3 O31 1.569(3) . ?
P3 O32 1.553(3) . ?
P3 O33 1.496(3) . ?
P3 O34 1.491(3) . ?
O31 H31 0.8200 . ?
O32 H32 0.8200 . ?
P9 O91 1.543(4) . ?
P9 O92 1.536(4) . ?
P9 O93 1.532(3) . ?
P9 O94 1.479(3) . ?
O91 H91 0.8200 . ?
O92 H92 0.8200 . ?
O93 H93 0.8200 . ?
P11A O111 1.522(6) . ?
P11A O112 1.538(7) . ?
P11A O113 1.504(7) . ?
P11A O114 1.497(6) . ?
O111 H111 0.8200 . ?
O112 H112 0.8200 . ?
P5A O51 1.531(9) . ?
P5A O52 1.570(5) . ?
P5A O53 1.547(8) . ?
P5A O54 1.484(5) . ?
O51 H51 0.8200 . ?
O52 H52 0.8200 . ?
P6 O61 1.541(3) . ?
P6 O62 1.523(3) . ?
P6 O63 1.521(4) . ?
P6 O64 1.514(4) . ?
O61 H61 0.8200 . ?
O63 H63 0.8200 . ?
P5B O55 1.57(7) . ?
P5B O56 1.55(2) . ?
P5B O57 1.39(4) . ?
P5B O58 1.439(18) . ?
O56 H56 0.8200 . ?
O57 H5BA 0.8200 . ?
P4 O41 1.557(3) . ?
P4 O42 1.545(3) . ?
P4 O43 1.505(3) . ?
P4 O44 1.534(3) . ?
O41 H41 0.8200 . ?
O42 H42 0.82(6) . ?
P8 O81 1.573(5) . ?
P8 O82 1.528(5) . ?
P8 O83 1.512(5) . ?
P8 O84 1.473(5) . ?
O81 H81 0.8200 . ?
O83 H83 0.8200 . ?
P10 O101 1.556(3) . ?
P10 O102 1.555(3) . ?
P10 O103 1.510(3) . ?
P10 O104 1.510(3) . ?
O101 H101 0.8200 . ?
O102 H102 0.8200 . ?
O3 H3C 0.8510 . ?
O3 H3D 0.8505 . ?
O1A H1AA 0.8499 . ?
O1A H1AB 0.8514 . ?
O2 H2E 0.8386 . ?
O2 H2F 0.8241 . ?
O4 H4A 0.8233 . ?
O4 H4B 0.8264 . ?
O1B H1BA 0.855(15) . ?
O1B H1BB 0.850(15) . ?

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
C1 N1 H1 107.4 . . ?
C1 N1 C18 110.2(3) . . ?
C1 N1 C19 112.3(3) . . ?
C18 N1 H1 107.4 . . ?
C18 N1 C19 111.8(3) . . ?
C19 N1 H1 107.4 . . ?
H2A N2 H2B 107.8 . . ?
C2 N2 H2A 109.1 . . ?
C2 N2 H2B 109.1 . . ?
C2 N2 C3 112.5(3) . . ?
C3 N2 H2A 109.1 . . ?
C3 N2 H2B 109.1 . . ?
N4 N3 H3 126.9 . . ?
N4 N3 C4 106.2(3) . . ?
C4 N3 H3 126.9 . . ?
N3 N4 H4 124.1 . . ?
N3 N4 C6 111.9(3) . . ?
C6 N4 H4 124.1 . . ?
H5A N5 H5B 108.1 . . ?
C7 N5 H5A 109.6 . . ?
C7 N5 H5B 109.6 . . ?
C8 N5 H5A 109.6 . . ?
C8 N5 H5B 109.6 . . ?
C8 N5 C7 110.3(3) . . ?
C9 N6 H6 109.4 . . ?
C10 N6 H6 109.4 . . ?
C10 N6 C9 111.0(3) . . ?
C27 N6 H6 109.4 . . ?
C27 N6 C9 107.5(3) . . ?
C27 N6 C10 110.2(3) . . ?
H7A N7 H7B 107.7 . . ?
C11 N7 H7A 108.9 . . ?
C11 N7 H7B 108.9 . . ?
C11 N7 C12 113.5(3) . . ?
C12 N7 H7A 108.9 . . ?
C12 N7 H7B 108.9 . . ?
N9 N8 H8 125.5 . . ?
N9 N8 C13 109.1(3) . . ?
C13 N8 H8 125.5 . . ?
N8 N9 H9 125.5 . . ?
N8 N9 C15 108.9(3) . . ?
C15 N9 H9 125.5 . . ?
H10A N10 H10B 108.0 . . ?
C16 N10 H10A 109.3 . . ?
C16 N10 H10B 109.3 . . ?
C17 N10 H10A 109.3 . . ?
C17 N10 H10B 109.3 . . ?
C17 N10 C16 111.4(3) . . ?
H11A N11 H11B 107.7 . . ?
C20 N11 H11A 108.8 . . ?
C20 N11 H11B 108.8 . . ?
C20 N11 C21 113.8(3) . . ?
C21 N11 H11A 108.8 . . ?
C21 N11 H11B 108.8 . . ?
N13 N12 H12 123.9 . . ?
C22 N12 H12 123.9 . . ?
C22 N12 N13 112.3(4) . . ?
N12 N13 H13 127.3 . . ?
C24 N13 N12 105.4(4) . . ?
C24 N13 H13 127.3 . . ?
H14A N14 H14B 107.8 . . ?
C25 N14 H14A 109.0 . . ?
C25 N14 H14B 109.0 . . ?
C25 N14 C26 113.1(3) . . ?
C26 N14 H14A 109.0 . . ?
C26 N14 H14B 109.0 . . ?
N1 C1 H1A 104(3) . . ?
N1 C1 C2 109.1(3) . . ?
C2 C1 H1A 112(3) . . ?
N2 C2 C1 110.8(3) . . ?
N2 C2 H2C 109.5 . . ?
N2 C2 H2D 109.5 . . ?
C1 C2 H2C 109.5 . . ?
C1 C2 H2D 109.5 . . ?
H2C C2 H2D 108.1 . . ?
N2 C3 H3A 109.3 . . ?
N2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 N2 111.6(3) . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
N3 C4 C3 120.8(4) . . ?
N3 C4 C5 109.8(4) . . ?
C5 C4 C3 129.4(4) . . ?
C4 C5 H5 127.3 . . ?
C6 C5 C4 105.5(4) . . ?
C6 C5 H5 127.3 . . ?
N4 C6 C5 106.6(4) . . ?
N4 C6 C7 120.1(4) . . ?
C5 C6 C7 133.3(4) . . ?
N5 C7 H7C 109.1 . . ?
N5 C7 H7D 109.1 . . ?
C6 C7 N5 112.4(3) . . ?
C6 C7 H7C 109.1 . . ?
C6 C7 H7D 109.1 . . ?
H7C C7 H7D 107.9 . . ?
N5 C8 H8A 108.7 . . ?
N5 C8 H8B 108.7 . . ?
N5 C8 C9 114.3(4) . . ?
H8A C8 H8B 107.6 . . ?
C9 C8 H8A 108.7 . . ?
C9 C8 H8B 108.7 . . ?
N6 C9 C8 116.8(4) . . ?
N6 C9 H9A 108.1 . . ?
N6 C9 H9B 108.1 . . ?
C8 C9 H9A 108.1 . . ?
C8 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
N6 C10 H10C 109.1 . . ?
N6 C10 H10D 109.1 . . ?
N6 C10 C11 112.7(3) . . ?
H10C C10 H10D 107.8 . . ?
C11 C10 H10C 109.1 . . ?
C11 C10 H10D 109.1 . . ?
N7 C11 C10 110.9(3) . . ?
N7 C11 H11C 109.5 . . ?
N7 C11 H11D 109.5 . . ?
C10 C11 H11C 109.5 . . ?
C10 C11 H11D 109.5 . . ?
H11C C11 H11D 108.1 . . ?
N7 C12 H12A 108.9 . . ?
N7 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C13 C12 N7 113.4(3) . . ?
C13 C12 H12A 108.9 . . ?
C13 C12 H12B 108.9 . . ?
N8 C13 C12 121.4(3) . . ?
N8 C13 C14 107.4(3) . . ?
C14 C13 C12 131.1(3) . . ?
C13 C14 H14 126.8 . . ?
C13 C14 C15 106.5(3) . . ?
C15 C14 H14 126.8 . . ?
N9 C15 C14 108.1(3) . . ?
N9 C15 C16 121.7(3) . . ?
C14 C15 C16 130.2(3) . . ?
N10 C16 C15 111.1(3) . . ?
N10 C16 H16A 109.4 . . ?
N10 C16 H16B 109.4 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
N10 C17 H17A 108.7 . . ?
N10 C17 H17B 108.7 . . ?
N10 C17 C18 114.3(3) . . ?
H17A C17 H17B 107.6 . . ?
C18 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
N1 C18 C17 116.2(3) . . ?
N1 C18 H18A 108.2 . . ?
N1 C18 H18B 108.2 . . ?
C17 C18 H18A 108.2 . . ?
C17 C18 H18B 108.2 . . ?
H18A C18 H18B 107.4 . . ?
N1 C19 H19A 109.4 . . ?
N1 C19 H19B 109.4 . . ?
N1 C19 C20 111.3(3) . . ?
H19A C19 H19B 108.0 . . ?
C20 C19 H19A 109.4 . . ?
C20 C19 H19B 109.4 . . ?
N11 C20 C19 109.1(3) . . ?
N11 C20 H20A 109.9 . . ?
N11 C20 H20B 109.9 . . ?
C19 C20 H20A 109.9 . . ?
C19 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
N11 C21 H21A 109.1 . . ?
N11 C21 H21B 109.1 . . ?
N11 C21 C22 112.3(4) . . ?
H21A C21 H21B 107.9 . . ?
C22 C21 H21A 109.1 . . ?
C22 C21 H21B 109.1 . . ?
N12 C22 C21 120.2(4) . . ?
N12 C22 C23 107.0(4) . . ?
C23 C22 C21 132.9(4) . . ?
C22 C23 H23 127.5 . . ?
C22 C23 C24 105.1(4) . . ?
C24 C23 H23 127.5 . . ?
N13 C24 C23 110.2(4) . . ?
N13 C24 C25 119.6(4) . . ?
C23 C24 C25 130.1(4) . . ?
N14 C25 C24 110.8(3) . . ?
N14 C25 H25A 109.5 . . ?
N14 C25 H25B 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
N14 C26 H26A 109.3 . . ?
N14 C26 H26B 109.3 . . ?
N14 C26 C27 111.7(3) . . ?
H26A C26 H26B 107.9 . . ?
C27 C26 H26A 109.3 . . ?
C27 C26 H26B 109.3 . . ?
N6 C27 C26 114.4(3) . . ?
N6 C27 H27A 108.7 . . ?
N6 C27 H27B 108.7 . . ?
C26 C27 H27A 108.7 . . ?
C26 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
O71 P7 O72 107.5(3) . . ?
O71 P7 O73 110.8(4) . . ?
O71 P7 O76 109.0(5) . . ?
O71 P7 O77 108.7(6) . . ?
O73 P7 O72 108.5(3) . . ?
O74 P7 O71 112.8(4) . . ?
O74 P7 O72 111.6(3) . . ?
O74 P7 O73 105.6(4) . . ?
O75 P7 O71 114.5(8) . . ?
O75 P7 O76 103.3(8) . . ?
O75 P7 O77 114.5(10) . . ?
O77 P7 O76 106.3(6) . . ?
P7 O72 H72 109.5 . . ?
P7 O73 H73 109.5 . . ?
P7 O74 H7AA 109.5 . . ?
P7 O75 H7BB 109.5 . . ?
P7 O76 H76 109.5 . . ?
P7 O77 H77 109.5 . . ?
O12 P1 O11 107.21(17) . . ?
O13 P1 O11 110.74(17) . . ?
O13 P1 O12 107.45(17) . . ?
O14 P1 O11 106.06(15) . . ?
O14 P1 O12 111.18(18) . . ?
O14 P1 O13 114.04(16) . . ?
P1 O11 H11 109.5 . . ?
P1 O12 H12C 109.5 . . ?
O116 P11B O115 100.8(9) . . ?
O116 P11B O118 107.4(11) . . ?
O117 P11B O115 116.6(11) . . ?
O117 P11B O116 106.6(12) . . ?
O117 P11B O118 103.1(10) . . ?
O118 P11B O115 121.2(8) . . ?
P11B O115 H115 109.5 . . ?
P11B O117 H11E 109.5 . . ?
O21 P2 O22 107.8(3) . . ?
O23 P2 O21 109.84(19) . . ?
O23 P2 O22 108.8(2) . . ?
O24 P2 O21 107.10(19) . . ?
O24 P2 O22 107.7(2) . . ?
O24 P2 O23 115.29(17) . . ?
P2 O21 H21 109.5 . . ?
P2 O22 H22 109.5 . . ?
O32 P3 O31 107.2(2) . . ?
O33 P3 O31 111.1(2) . . ?
O33 P3 O32 106.14(17) . . ?
O34 P3 O31 106.6(2) . . ?
O34 P3 O32 112.1(2) . . ?
O34 P3 O33 113.55(19) . . ?
P3 O31 H31 109.5 . . ?
P3 O32 H32 109.5 . . ?
O92 P9 O91 105.1(3) . . ?
O93 P9 O91 109.2(2) . . ?
O93 P9 O92 105.8(2) . . ?
O94 P9 O91 111.5(3) . . ?
O94 P9 O92 113.0(2) . . ?
O94 P9 O93 111.8(2) . . ?
P9 O91 H91 109.5 . . ?
P9 O92 H92 109.5 . . ?
P9 O93 H93 109.5 . . ?
O111 P11A O112 112.3(5) . . ?
O113 P11A O111 108.7(4) . . ?
O113 P11A O112 107.5(4) . . ?
O114 P11A O111 110.4(3) . . ?
O114 P11A O112 109.4(5) . . ?
O114 P11A O113 108.5(4) . . ?
P11A O111 H111 109.5 . . ?
P11A O112 H112 109.5 . . ?
O51 P5A O52 100.5(4) . . ?
O51 P5A O53 106.9(5) . . ?
O53 P5A O52 102.7(4) . . ?
O54 P5A O51 117.6(4) . . ?
O54 P5A O52 112.5(3) . . ?
O54 P5A O53 114.8(4) . . ?
P5A O51 H51 109.5 . . ?
P5A O52 H52 109.5 . . ?
O62 P6 O61 110.1(2) . . ?
O63 P6 O61 108.3(2) . . ?
O63 P6 O62 107.6(2) . . ?
O64 P6 O61 104.5(2) . . ?
O64 P6 O62 111.5(2) . . ?
O64 P6 O63 114.8(3) . . ?
P6 O61 H61 109.5 . . ?
P6 O63 H63 109.5 . . ?
O56 P5B O55 104(3) . . ?
O57 P5B O55 129(3) . . ?
O57 P5B O56 98.3(17) . . ?
O57 P5B O58 112(2) . . ?
O58 P5B O55 100(2) . . ?
O58 P5B O56 113.8(16) . . ?
P5B O56 H56 109.5 . . ?
P5B O57 H5BA 109.5 . . ?
O42 P4 O41 103.57(18) . . ?
O43 P4 O41 107.09(16) . . ?
O43 P4 O42 111.98(19) . . ?
O43 P4 O44 113.53(18) . . ?
O44 P4 O41 109.27(19) . . ?
O44 P4 O42 110.82(19) . . ?
P4 O41 H41 109.5 . . ?
P4 O42 H42 119.3 . . ?
O82 P8 O81 109.0(3) . . ?
O83 P8 O81 107.4(3) . . ?
O83 P8 O82 102.8(3) . . ?
O84 P8 O81 112.2(3) . . ?
O84 P8 O82 109.9(3) . . ?
O84 P8 O83 115.1(4) . . ?
P8 O81 H81 109.5 . . ?
P8 O83 H83 109.5 . . ?
O102 P10 O101 103.94(18) . . ?
O103 P10 O101 106.90(19) . . ?
O103 P10 O102 110.70(18) . . ?
O103 P10 O104 112.20(18) . . ?
O104 P10 O101 110.75(17) . . ?
O104 P10 O102 111.93(19) . . ?
P10 O101 H101 109.5 . . ?
P10 O102 H102 109.5 . . ?
H3C O3 H3D 109.3 . . ?
H1AA O1A H1AB 104.4 . . ?
H2E O2 H2F 128.4 . . ?
H4A O4 H4B 138.6 . . ?
H1BA O1B H1BB 136.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O14 0.98 1.63 2.589(4) 165.3 . yes
N2 H2A O3 0.89 1.87 2.753(6) 168.7 . yes
N2 H2B O115 0.89 1.88 2.755(7) 167.7 . yes
N3 H3 O21 0.86 1.97 2.731(5) 146.3 . yes
N4 H4 O44 0.86 2.01 2.865(4) 170.8 . yes
N5 H5A O34 0.89 1.93 2.798(5) 164.7 . yes
N5 H5B O13 0.89 1.91 2.797(4) 173.9 . yes
N7 H7A O103 0.89 1.94 2.819(4) 170.9 1_455 yes
N7 H7B O43 0.89 1.91 2.798(5) 179.4 . yes
N8 H8 O43 0.86 1.78 2.630(4) 171.0 3_666 yes
N9 H9 O104 0.86 1.79 2.590(4) 154.0 3_766 yes
N10 H10A O14 0.89 1.82 2.685(4) 163.1 . yes
N10 H10B O24 0.89 1.84 2.711(4) 163.7 . yes
N11 H11A O58 0.89 1.65 2.511(15) 162.8 . yes
N11 H11B O71 0.89 1.99 2.789(6) 148.0 3_756 yes
N12 H12 O74 0.86 1.93 2.780(7) 171.6 . yes
N12 H12 O77 0.86 1.92 2.718(15) 154.1 . yes
N13 H13 O1A 0.86 2.23 2.880(14) 132.4 3_656 yes
N13 H13 O1B 0.86 2.02 2.75(3) 142.1 3_656 yes
N14 H14A O12 0.89 2.42 3.010(4) 123.6 . yes
N14 H14A O33 0.89 2.15 2.914(5) 143.8 . yes
N14 H14B O1A 0.89 2.09 2.951(14) 162.7 . yes
N14 H14B O1B 0.89 2.07 2.93(2) 162.8 . yes
C16 H16A O117 0.97 2.51 2.90(2) 104.0 4_566 yes
O76 H76 O64 0.82 1.86 2.653(11) 163.3 3_656 yes
O77 H77 O53 0.82 2.00 2.417(14) 111.3 . yes
O11 H11 O33 0.82 1.71 2.526(4) 171.1 . yes
O12 H12C O54 0.82 1.93 2.696(5) 155.8 . yes
O12 H12C O56 0.82 1.71 2.411(13) 142.8 . yes
O117 H11E O94 0.82 1.65 2.382(16) 147.0 . yes
O31 H31 O44 0.82 1.95 2.762(5) 169.5 2_645 yes
O32 H32 O23 0.82 1.72 2.526(4) 169.0 2_645 yes
O91 H91 O84 0.82 1.96 2.506(7) 123.5 3_756 yes
O92 H92 O44 0.82 1.88 2.608(5) 147.6 2_645 yes
O93 H93 O104 0.82 1.75 2.529(4) 159.3 2_745 yes
O51 H51 O82 0.82 1.76 2.425(10) 137.1 . yes
O52 H52 O1B 0.82 2.22 2.59(2) 107.7 . yes
O61 H61 O34 0.82 1.76 2.572(5) 171.0 4_566 yes
O63 H63 O103 0.82 1.68 2.494(4) 172.0 1_455 yes
O56 H56 O1A 0.82 2.45 2.95(2) 120.4 . yes
O41 H41 O23 0.82 1.80 2.618(4) 172.0 . yes
O42 H42 O13 0.82 1.70 2.519(4) 175.8 . yes
O83 H83 O62 0.82 1.76 2.432(6) 138.3 1_655 yes
O101 H101 O2 0.82 1.83 2.606(6) 157.3 . yes
O102 H102 O24 0.82 1.77 2.587(4) 172.6 3_766 yes
O3 H3C O31 0.85 2.18 2.989(6) 157.7 . yes
O3 H3D O94 0.85 2.15 2.764(6) 128.5 . yes
O1A H1AA O56 0.85 2.43 2.95(2) 120.6 . yes
O1A H1AB O64 0.85 2.06 2.873(11) 159.0 . yes
O2 H2E O84 0.84 2.25 2.862(7) 129.5 4_565 yes
O2 H2F O111 0.82 1.98 2.757(8) 156.7 2_655 yes
O4 H4A O118 0.82 2.35 2.68(2) 104.5 1_455 yes
O4 H4A O113 0.82 2.26 2.432(10) 92.1 . yes
O1B H1BB O52 0.85 2.03 2.59(2) 123.2 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 -162.6(3) . . . . ?
N1 C19 C20 N11 -168.6(3) . . . . ?
N2 C3 C4 N3 93.2(5) . . . . ?
N2 C3 C4 C5 -85.5(6) . . . . ?
N3 N4 C6 C5 -1.3(5) . . . . ?
N3 N4 C6 C7 178.3(4) . . . . ?
N3 C4 C5 C6 -1.2(5) . . . . ?
N4 N3 C4 C3 -178.6(4) . . . . ?
N4 N3 C4 C5 0.4(5) . . . . ?
N4 C6 C7 N5 -93.7(4) . . . . ?
N5 C8 C9 N6 62.4(5) . . . . ?
N6 C10 C11 N7 179.0(3) . . . . ?
N7 C12 C13 N8 84.5(4) . . . . ?
N7 C12 C13 C14 -97.9(5) . . . . ?
N8 N9 C15 C14 0.9(4) . . . . ?
N8 N9 C15 C16 -177.6(3) . . . . ?
N8 C13 C14 C15 -0.1(5) . . . . ?
N9 N8 C13 C12 178.6(3) . . . . ?
N9 N8 C13 C14 0.6(4) . . . . ?
N9 C15 C16 N10 -99.0(4) . . . . ?
N10 C17 C18 N1 -73.5(4) . . . . ?
N11 C21 C22 N12 -85.9(5) . . . . ?
N11 C21 C22 C23 93.8(6) . . . . ?
N12 N13 C24 C23 0.0(5) . . . . ?
N12 N13 C24 C25 -178.0(4) . . . . ?
N12 C22 C23 C24 -0.9(5) . . . . ?
N13 N12 C22 C21 -179.2(4) . . . . ?
N13 N12 C22 C23 1.0(5) . . . . ?
N13 C24 C25 N14 91.3(5) . . . . ?
N14 C26 C27 N6 66.9(5) . . . . ?
C1 N1 C18 C17 169.5(3) . . . . ?
C1 N1 C19 C20 -57.5(4) . . . . ?
C2 N2 C3 C4 -61.2(5) . . . . ?
C3 N2 C2 C1 -178.2(4) . . . . ?
C3 C4 C5 C6 177.7(4) . . . . ?
C4 N3 N4 C6 0.6(4) . . . . ?
C4 C5 C6 N4 1.4(5) . . . . ?
C4 C5 C6 C7 -178.1(4) . . . . ?
C5 C6 C7 N5 85.8(6) . . . . ?
C7 N5 C8 C9 173.4(4) . . . . ?
C8 N5 C7 C6 162.9(4) . . . . ?
C9 N6 C10 C11 -167.2(4) . . . . ?
C9 N6 C27 C26 77.0(5) . . . . ?
C10 N6 C9 C8 60.2(5) . . . . ?
C10 N6 C27 C26 -162.0(4) . . . . ?
C11 N7 C12 C13 82.5(4) . . . . ?
C12 N7 C11 C10 178.1(3) . . . . ?
C12 C13 C14 C15 -177.8(4) . . . . ?
C13 N8 N9 C15 -0.9(4) . . . . ?
C13 C14 C15 N9 -0.5(5) . . . . ?
C13 C14 C15 C16 177.8(4) . . . . ?
C14 C15 C16 N10 82.9(5) . . . . ?
C16 N10 C17 C18 174.9(3) . . . . ?
C17 N10 C16 C15 -159.5(3) . . . . ?
C18 N1 C1 C2 -69.5(4) . . . . ?
C18 N1 C19 C20 178.0(3) . . . . ?
C19 N1 C1 C2 165.2(3) . . . . ?
C19 N1 C18 C17 -64.8(4) . . . . ?
C20 N11 C21 C22 -76.9(5) . . . . ?
C21 N11 C20 C19 -174.1(4) . . . . ?
C21 C22 C23 C24 179.4(4) . . . . ?
C22 N12 N13 C24 -0.6(5) . . . . ?
C22 C23 C24 N13 0.6(5) . . . . ?
C22 C23 C24 C25 178.4(4) . . . . ?
C23 C24 C25 N14 -86.3(6) . . . . ?
C25 N14 C26 C27 169.1(4) . . . . ?
C26 N14 C25 C24 -177.2(4) . . . . ?
C27 N6 C9 C8 -179.3(4) . . . . ?
C27 N6 C10 C11 73.9(4) . . . . ?

_olex2_submission_original_sample_id phos11
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_crystal7_arsen
_database_code_depnum_ccdc_archive 'CCDC 1912384'
loop_
_audit_author_name
_audit_author_address
'Javier Pitarch-Jarque'
;Universitat de Valencia
Spain
;
_audit_update_record             
;
2019-04-26 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_audit_creation_date             2019-03-12
_audit_creation_method           
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(As H2 O4), As H3 O4, 4(C F3 O3 S), 3(H2 O), C27 H55 N14'
_chemical_formula_sum            'C31 H68 As3 F12 N14 O27 S4'
_chemical_formula_weight         1649.99
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   12.6927(4)
_cell_length_b                   15.1722(5)
_cell_length_c                   17.0426(5)
_cell_angle_alpha                96.081(3)
_cell_angle_beta                 90.171(3)
_cell_angle_gamma                109.012(3)
_cell_volume                     3083.06(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    120.00(10)
_cell_measurement_reflns_used    9451
_cell_measurement_theta_min      3.5520
_cell_measurement_theta_max      27.2210
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_min  0.92932
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1678
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.825
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22380
_diffrn_reflns_point_group_measured_fraction_full 0.641
_diffrn_reflns_point_group_measured_fraction_max 0.524
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.935
_diffrn_reflns_theta_min         3.348
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.825
_diffrn_ambient_temperature      120.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.0267
_reflns_Friedel_coverage         0.270
_reflns_Friedel_fraction_full    0.290
_reflns_Friedel_fraction_max     0.223
_reflns_number_gt                13989
_reflns_number_total             15491
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla et al.,  2007)'
_refine_diff_density_max         2.605
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 
;
 Flack x determined using 2869 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.063(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1735
_refine_ls_number_reflns         15491
_refine_ls_number_restraints     104
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0553
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0715P)²+12.3248P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1420
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C60-F61 = C60-F63 = C60-F62
 1.322 with sigma of 0.015
 S6-C60
 1.814 with sigma of 0.017
 O85_$1-H2E
 3.1 with sigma of 0.1
 O47_$2-H1D
 2.11 with sigma of 0.1
 O25_$1-H1C
 1.76 with sigma of 0.1
 H2F-O1_$3
 1.9 with sigma of 0.1
 H4A-N17_$4
 2.24 with sigma of 0.1
 O6-H5D
 2.4 with sigma of 0.1
 O15-H5C
 2.1 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(O54) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C62) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O87) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O75A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F72B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F71B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C61B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(S7B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O76B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O77B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(F73B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O75B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O76A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(S7B)=Sof(O75B)=Sof(O76B)=Sof(O77B)=Sof(C61B)=Sof(F72B)=Sof(F71B)=
 Sof(F73B)=1-FVAR(1)
 Sof(S7A)=Sof(F72A)=Sof(F73A)=Sof(F71A)=Sof(O77A)=Sof(O75A)=Sof(O76A)=
 Sof(C61A)=FVAR(1)
 Sof(O67B)=Sof(O65B)=Sof(O66B)=1-FVAR(2)
 Sof(O66A)=Sof(O67A)=Sof(O65A)=FVAR(2)
5.a Free rotating group:
 S8(O87,O85,O86,C62,F83,F82,F81), O4(H4A,H4B), O2(H2E,H2F), O5(H5C,H5D),
 O3(H3C,H3D), O1(H1C,H1D), O6(H6A,H6B), S7B(O75B,O76B,O77B,C61B,F72B,F71B,F73B)
5.b Ternary CH refined with riding coordinates:
 N1(H1), N20(H20)
5.c Secondary CH2 refined with riding coordinates:
 N14(H14A,H14B), N11(H11A,H11B), N5(H5A,H5B), N10(H10A,H10B), N2(H2A,H2B),
 N7(H7A,H7B), C20(H20A,H20B), C18(H18A,H18B), C17(H17A,H17B), C12(H12A,H12B),
 C27(H27A,H27B), C3(H3A,H3B), C9(H9A,H9B), C7(H7C,H7D), C8(H8A,H8B), C16(H16A,
 H16B), C19(H19A,H19B), C2(H2C,H2D), C21(H21A,H21B), C26(H26A,H26B), C25(H25A,
 H25B), C1(H1A,H1B), C11(H11C,H11D), C10(H10C,H10D), N19(H19C,H19D), N21(H21C,
 H21D), N25(H25C,H25D), N28(H28A,H28B), N24(H24A,H24B), N16(H16C,H16D),
 C35(H35A,H35B), C48(H48A,H48B), C45(H45A,H45B), C39(H39A,H39B), C47(H47A,H47B),
  C28(H28C,H28D), C36(H36A,H36B), C54(H54A,H54B), C38(H38A,H38B), C43(H43A,
 H43B), C44(H44A,H44B), C46(H46A,H46B), C53(H53A,H53B), C37(H37A,H37B),
 C52(H52A,H52B), C29(H29A,H29B), C34(H34A,H34B), C30(H30A,H30B)
5.d Aromatic/amide H refined with riding coordinates:
 N4(H4), N13(H13), N9(H9), C14(H14), C23(H23), C5(H5), N23(H23A), N18(H18),
 N27(H27), C32(H32), C41(H41), C50(H50)
5.e Tetrahedral OH refined with riding coordinates:
 O21(H21)
5.f Idealised tetrahedral OH refined as rotating group:
 O22(H22), O31(H31), O32(H32A), O33(H33), O11(H11), O12(H12), O41(H41A),
 O42(H42), O52(H52), O51(H51), O61(H61), O62(H62), O63(H63)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
As2 As 0.98432(7) 0.57724(6) 0.44888(6) 0.0144(2) Uani 1 1 d . . . . .
O21 O 0.8388(6) 0.5361(5) 0.4372(4) 0.0206(16) Uani 1 1 d . . . . .
H21 H 0.814569 0.482936 0.450376 0.031 Uiso 1 1 calc R . . . .
O22 O 1.0312(6) 0.5607(5) 0.3560(5) 0.0232(17) Uani 1 1 d . . . . .
H22 H 1.078184 0.534459 0.357827 0.035 Uiso 1 1 calc GR . . . .
O24 O 1.0241(6) 0.6905(5) 0.4778(4) 0.0194(15) Uani 1 1 d . . . . .
O23 O 1.0128(6) 0.5008(5) 0.5002(5) 0.0229(17) Uani 1 1 d . . . . .
As3 As 0.62115(8) 0.66019(7) 0.43009(6) 0.0180(2) Uani 1 1 d . . . . .
O31 O 0.5615(6) 0.6414(6) 0.5188(4) 0.0225(17) Uani 1 1 d . . . . .
H31 H 0.606128 0.633459 0.549965 0.034 Uiso 1 1 calc GR . . . .
O34 O 0.7580(6) 0.6913(5) 0.4348(4) 0.0210(16) Uani 1 1 d . . . . .
O32 O 0.5732(7) 0.7394(6) 0.3906(5) 0.0272(18) Uani 1 1 d . . . . .
H32A H 0.526866 0.712218 0.354859 0.041 Uiso 1 1 calc GR . . . .
O33 O 0.5665(6) 0.5601(5) 0.3676(5) 0.0277(18) Uani 1 1 d . . . . .
H33 H 0.500827 0.535102 0.377092 0.042 Uiso 1 1 calc GR . . . .
As1 As 0.35473(8) 0.58695(7) 0.92409(6) 0.0185(2) Uani 1 1 d . . . . .
O11 O 0.4997(6) 0.6320(5) 0.9325(5) 0.0233(17) Uani 1 1 d . . . . .
H11 H 0.524772 0.589322 0.937151 0.035 Uiso 1 1 calc GR . . . .
O12 O 0.3161(7) 0.6125(6) 1.0193(5) 0.0271(18) Uani 1 1 d . . . . .
H12 H 0.318342 0.571423 1.046227 0.041 Uiso 1 1 calc GR . . . .
O14 O 0.3188(6) 0.6560(5) 0.8685(4) 0.0196(16) Uani 1 1 d . . . . .
O13 O 0.3154(6) 0.4740(5) 0.9007(5) 0.0286(19) Uani 1 1 d . . . . .
As4 As 0.16431(8) 0.75103(7) 0.21048(6) 0.0178(2) Uani 1 1 d . . . . .
O41 O 0.2368(6) 0.8701(5) 0.2175(5) 0.0264(17) Uani 1 1 d . . . . .
H41A H 0.290309 0.879473 0.188955 0.040 Uiso 1 1 calc GR . . . .
O43 O 0.2596(6) 0.7007(5) 0.1914(4) 0.0229(16) Uani 1 1 d . . . . .
O44 O 0.1015(6) 0.7294(5) 0.2951(4) 0.0191(15) Uani 1 1 d . . . . .
O42 O 0.0662(6) 0.7310(6) 0.1366(5) 0.0344(19) Uani 1 1 d . . . . .
H42 H 0.013013 0.684632 0.143366 0.052 Uiso 1 1 calc GR . . . .
As5 As 0.20004(8) 0.45837(7) 0.18032(6) 0.0192(2) Uani 1 1 d . . . . .
O54 O 0.2708(6) 0.4554(5) 0.0982(5) 0.0245(17) Uani 1 1 d . U . . .
O52 O 0.1928(6) 0.3648(5) 0.2313(5) 0.0311(19) Uani 1 1 d . . . . .
H52 H 0.252113 0.375145 0.255794 0.047 Uiso 1 1 calc GR . . . .
O51 O 0.2712(6) 0.5521(5) 0.2465(5) 0.0279(17) Uani 1 1 d . . . . .
H51 H 0.265297 0.600260 0.232198 0.042 Uiso 1 1 calc GR . . . .
O53 O 0.0702(6) 0.4549(5) 0.1622(5) 0.0250(17) Uani 1 1 d . . . . .
As6 As 0.72384(8) 0.50690(8) 0.93324(7) 0.0243(3) Uani 1 1 d . . . . .
O64 O 0.5850(6) 0.4758(6) 0.9349(4) 0.0264(18) Uani 1 1 d . . . . .
O61 O 0.7706(6) 0.5007(7) 0.8408(5) 0.034(2) Uani 1 1 d . . . . .
H61 H 0.722536 0.501747 0.809029 0.050 Uiso 1 1 calc GR . . . .
O62 O 0.7764(7) 0.4395(8) 0.9853(5) 0.045(2) Uani 1 1 d . . . . .
H62 H 0.839399 0.443932 0.971095 0.067 Uiso 1 1 calc GR . . . .
O63 O 0.7879(7) 0.6163(7) 0.9765(7) 0.055(3) Uani 1 1 d . . . . .
H63 H 0.757156 0.625018 1.017429 0.082 Uiso 1 1 calc GR . . . .
S1 S 0.4925(2) 0.3143(2) 0.49729(17) 0.0249(6) Uani 1 1 d . . . . .
F13 F 0.5120(7) 0.2177(5) 0.6113(5) 0.0466(19) Uani 1 1 d . . . . .
F12 F 0.3443(7) 0.2084(5) 0.5842(5) 0.054(2) Uani 1 1 d . . . . .
F11 F 0.4273(7) 0.1328(5) 0.5072(5) 0.049(2) Uani 1 1 d . . . . .
O15 O 0.4076(7) 0.2979(7) 0.4368(6) 0.048(3) Uani 1 1 d D . . . .
O17 O 0.5015(7) 0.3919(6) 0.5568(5) 0.033(2) Uani 1 1 d . . . . .
O16 O 0.5977(6) 0.3091(6) 0.4688(5) 0.033(2) Uani 1 1 d . . . . .
C55 C 0.4409(10) 0.2136(8) 0.5519(8) 0.032(3) Uani 1 1 d . . . . .
S2 S 0.8418(2) 0.8471(2) 0.88552(18) 0.0288(7) Uani 1 1 d . . . . .
F22 F 1.0005(7) 0.9668(6) 0.8172(7) 0.074(3) Uani 1 1 d . . . . .
F23 F 0.9086(7) 1.0302(6) 0.8953(6) 0.063(3) Uani 1 1 d . . . . .
F21 F 0.8348(9) 0.9603(7) 0.7834(6) 0.075(3) Uani 1 1 d . . . . .
O27 O 0.8400(7) 0.7773(6) 0.8209(5) 0.0320(19) Uani 1 1 d . . . . .
O26 O 0.7333(7) 0.8467(7) 0.9088(5) 0.042(2) Uani 1 1 d . . . . .
O25 O 0.9197(7) 0.8553(7) 0.9505(5) 0.039(2) Uani 1 1 d D . . . .
C56 C 0.8969(13) 0.9580(10) 0.8436(10) 0.051(4) Uani 1 1 d . . . . .
S3 S 0.2208(2) 0.8694(2) 0.69576(16) 0.0237(6) Uani 1 1 d . . . . .
F33 F 0.3577(8) 1.0269(6) 0.7649(6) 0.067(3) Uani 1 1 d . . . . .
F32 F 0.2291(8) 1.0412(6) 0.6892(6) 0.072(3) Uani 1 1 d . . . . .
F31 F 0.3652(7) 1.0077(6) 0.6345(6) 0.061(2) Uani 1 1 d . . . . .
O37 O 0.1642(7) 0.8466(6) 0.6182(5) 0.036(2) Uani 1 1 d . . . . .
O35 O 0.3054(7) 0.8273(6) 0.7065(5) 0.0288(18) Uani 1 1 d . . . . .
O36 O 0.1473(7) 0.8645(6) 0.7604(5) 0.036(2) Uani 1 1 d . . . . .
C57 C 0.2988(12) 0.9942(10) 0.6944(9) 0.045(3) Uani 1 1 d . . . . .
S6 S 0.1022(2) 0.3125(2) 0.70954(18) 0.0283(6) Uani 1 1 d D . . . .
F62 F 0.0941(9) 0.1431(7) 0.7308(7) 0.085(4) Uani 1 1 d D . . . .
F61 F -0.0538(9) 0.1536(8) 0.6787(14) 0.166(9) Uani 1 1 d D . . . .
F63 F 0.077(2) 0.1552(9) 0.6190(9) 0.198(11) Uani 1 1 d D . . . .
C60 C 0.0496(12) 0.1871(8) 0.6896(10) 0.075(7) Uani 1 1 d D . . . .
O66A O 0.0430(12) 0.3428(11) 0.6487(10) 0.034(4) Uani 0.65(3) 1 d . . P A 1
O67A O 0.2196(13) 0.3331(12) 0.6960(16) 0.062(7) Uani 0.65(3) 1 d . . P A 1
O65A O 0.080(2) 0.3237(10) 0.7882(8) 0.052(7) Uani 0.65(3) 1 d . . P A 1
O67B O 0.165(3) 0.338(2) 0.7882(15) 0.042(9) Uani 0.35(3) 1 d . . P A 2
O65B O 0.012(3) 0.352(2) 0.706(3) 0.072(18) Uani 0.35(3) 1 d . . P A 2
O66B O 0.170(3) 0.328(2) 0.649(2) 0.061(12) Uani 0.35(3) 1 d . . P A 2
S4 S 0.1307(4) 0.0412(2) 0.1500(2) 0.0475(10) Uani 1 1 d . . . . .
F41 F 0.2854(8) 0.1919(7) 0.2175(6) 0.070(3) Uani 1 1 d . . . . .
F43 F 0.2400(7) 0.0752(6) 0.2871(4) 0.049(2) Uani 1 1 d . . . . .
F42 F 0.1308(7) 0.1549(6) 0.2761(5) 0.054(2) Uani 1 1 d . . . . .
O46 O 0.2089(15) 0.0017(13) 0.1192(7) 0.122(7) Uani 1 1 d . . . . .
O45 O 0.0999(7) 0.0994(6) 0.1024(5) 0.037(2) Uani 1 1 d . . . . .
O47 O 0.0388(14) -0.0256(8) 0.1832(7) 0.104(6) Uani 1 1 d D . . . .
C58 C 0.2013(12) 0.1206(8) 0.2361(9) 0.040(3) Uani 1 1 d . . . . .
S5 S 0.6444(3) 0.0606(3) 0.2687(2) 0.0522(10) Uani 1 1 d . . . . .
F51 F 0.4910(6) -0.0519(5) 0.3416(5) 0.053(2) Uani 1 1 d . . . . .
F53 F 0.5946(8) 0.0714(6) 0.4155(6) 0.066(3) Uani 1 1 d . . . . .
F52 F 0.4700(9) 0.0810(7) 0.3377(6) 0.079(3) Uani 1 1 d . . . . .
O57 O 0.5742(8) 0.0171(6) 0.1938(6) 0.045(2) Uani 1 1 d . . . . .
O55 O 0.6910(9) 0.1626(7) 0.2680(7) 0.064(3) Uani 1 1 d . . . . .
O56 O 0.7219(9) 0.0126(7) 0.2897(7) 0.066(3) Uani 1 1 d . . . . .
C59 C 0.5487(12) 0.0385(9) 0.3450(8) 0.042(3) Uani 1 1 d . . . . .
S8 S 0.6949(4) 0.1926(3) 0.9195(4) 0.139(4) Uani 1 1 d . U . . .
O87 O 0.7270(6) 0.1092(4) 0.9104(6) 0.29(2) Uani 1 1 d G U . . .
O85 O 0.5887(5) 0.1823(6) 0.9546(5) 0.160(9) Uani 1 1 d DG . . . .
O86 O 0.7833(6) 0.2790(4) 0.9452(5) 0.181(11) Uani 1 1 d G . . . .
C62 C 0.6662(5) 0.2075(4) 0.8160(4) 0.085(6) Uani 1 1 d G U . . .
F83 F 0.6344(6) 0.2828(5) 0.8113(5) 0.125(6) Uani 1 1 d G . . . .
F82 F 0.7561(7) 0.2185(7) 0.7723(5) 0.199(11) Uani 1 1 d G . . . .
F81 F 0.5848(7) 0.1333(5) 0.7806(5) 0.208(12) Uani 1 1 d G . . . .
O4 O 0.1608(8) 0.6062(7) 0.7349(6) 0.045(2) Uani 1 1 d . . . . .
H4A H 0.215370 0.635478 0.708437 0.068 Uiso 1 1 d DG . . . .
H4B H 0.146168 0.547413 0.723122 0.068 Uiso 1 1 d G . . . .
O2 O 0.7491(9) 0.0317(9) 0.0541(10) 0.088(5) Uani 1 1 d . . . . .
H2E H 0.723249 0.036801 0.009324 0.132 Uiso 1 1 d DG . . . .
H2F H 0.755694 -0.022493 0.049093 0.132 Uiso 1 1 d DG . . . .
O5 O 0.3979(9) 0.4022(6) 0.2850(8) 0.061(3) Uani 1 1 d . . . . .
H5C H 0.381567 0.371316 0.324603 0.091 Uiso 1 1 d DG . . . .
H5D H 0.409661 0.367429 0.245952 0.091 Uiso 1 1 d DG . . . .
O3 O 0.9207(8) 0.1799(6) 0.1231(7) 0.048(2) Uani 1 1 d . . . . .
H3C H 0.978341 0.163401 0.124987 0.072 Uiso 1 1 d G . . . .
H3D H 0.866817 0.130548 0.128844 0.072 Uiso 1 1 d G . . . .
O1 O 0.8223(9) 0.8839(8) 0.0935(7) 0.066(3) Uani 1 1 d D . . . .
H1C H 0.867886 0.895764 0.056469 0.099 Uiso 1 1 d DG . . . .
H1D H 0.853358 0.925332 0.131582 0.099 Uiso 1 1 d DG . . . .
O6 O 0.5416(8) 0.2950(8) 0.2894(7) 0.053(3) Uani 1 1 d D . . . .
H6A H 0.563838 0.283331 0.333017 0.080 Uiso 1 1 d G . . . .
H6B H 0.601069 0.320496 0.266051 0.080 Uiso 1 1 d G . . . .
N4 N 0.6339(8) 0.6454(7) 0.7704(5) 0.024(2) Uani 1 1 d . . . . .
H4 H 0.696015 0.689011 0.784114 0.029 Uiso 1 1 calc R . . . .
N8 N 0.0578(7) 0.6118(6) 1.0089(5) 0.0204(18) Uani 1 1 d . . . . .
N1 N 0.3128(7) 0.2618(6) 0.9484(5) 0.0203(19) Uani 1 1 d . . . . .
H1 H 0.321979 0.328250 0.946439 0.024 Uiso 1 1 calc R . . . .
N14 N 0.4611(7) 0.8273(6) 1.1618(5) 0.0208(19) Uani 1 1 d . . . . .
H14A H 0.455217 0.880916 1.184616 0.025 Uiso 1 1 calc R . . . .
H14B H 0.396169 0.782471 1.166044 0.025 Uiso 1 1 calc R . . . .
N6 N 0.3939(7) 0.8740(6) 0.9581(5) 0.0196(19) Uani 1 1 d . . . . .
N3 N 0.6200(7) 0.5540(7) 0.7684(5) 0.023(2) Uani 1 1 d . . . . .
N11 N 0.4633(7) 0.4158(6) 1.0665(5) 0.0197(19) Uani 1 1 d . . . . .
H11A H 0.400097 0.424442 1.081941 0.024 Uiso 1 1 calc R . . . .
H11B H 0.476065 0.433726 1.018375 0.024 Uiso 1 1 calc R . . . .
N13 N 0.6485(7) 0.7220(6) 1.1175(5) 0.0202(19) Uani 1 1 d . . . . .
H13 H 0.692727 0.772841 1.102160 0.024 Uiso 1 1 calc R . . . .
N5 N 0.5149(7) 0.7949(6) 0.8351(5) 0.0194(19) Uani 1 1 d . . . . .
H5A H 0.449493 0.757925 0.849619 0.023 Uiso 1 1 calc R . . . .
H5B H 0.567394 0.791642 0.868341 0.023 Uiso 1 1 calc R . . . .
N10 N 0.1287(7) 0.3420(6) 0.9537(6) 0.026(2) Uani 1 1 d . . . . .
H10A H 0.182767 0.380237 0.986624 0.032 Uiso 1 1 calc R . . . .
H10B H 0.149869 0.350550 0.904548 0.032 Uiso 1 1 calc R . . . .
N2 N 0.4305(7) 0.3730(6) 0.8159(5) 0.0204(19) Uani 1 1 d . . . . .
H2A H 0.488523 0.393632 0.850255 0.025 Uiso 1 1 calc R . . . .
H2B H 0.378963 0.397298 0.833851 0.025 Uiso 1 1 calc R . . . .
N12 N 0.6518(7) 0.6363(6) 1.0927(5) 0.0218(19) Uani 1 1 d . . . . .
N7 N 0.1649(7) 0.7557(6) 0.8833(5) 0.0203(19) Uani 1 1 d . . . . .
H7A H 0.214629 0.726916 0.890011 0.024 Uiso 1 1 calc R . . . .
H7B H 0.173192 0.775012 0.835516 0.024 Uiso 1 1 calc R . . . .
N9 N 0.0526(7) 0.5265(6) 1.0260(5) 0.0228(19) Uani 1 1 d . . . . .
H9 H 0.057816 0.512822 1.073179 0.027 Uiso 1 1 calc R . . . .
C4 C 0.5125(9) 0.5101(8) 0.7437(7) 0.024(2) Uani 1 1 d . . . . .
C13 C 0.0489(7) 0.6049(7) 0.9309(6) 0.016(2) Uani 1 1 d . . . . .
C22 C 0.5729(8) 0.5783(7) 1.1300(6) 0.019(2) Uani 1 1 d . . . . .
C20 C 0.4509(9) 0.3154(7) 1.0635(7) 0.024(2) Uani 1 1 d . . . . .
H20A H 0.459850 0.301192 1.116831 0.028 Uiso 1 1 calc R . . . .
H20B H 0.510616 0.303891 1.033208 0.028 Uiso 1 1 calc R . . . .
C18 C 0.1961(10) 0.2056(8) 0.9267(7) 0.028(3) Uani 1 1 d . . . . .
H18A H 0.183329 0.142100 0.939036 0.033 Uiso 1 1 calc R . . . .
H18B H 0.184628 0.202770 0.870026 0.033 Uiso 1 1 calc R . . . .
C24 C 0.5681(8) 0.7195(7) 1.1691(6) 0.017(2) Uani 1 1 d . . . . .
C6 C 0.5398(8) 0.6626(8) 0.7486(6) 0.021(2) Uani 1 1 d . . . . .
C17 C 0.1116(9) 0.2423(7) 0.9671(7) 0.026(3) Uani 1 1 d . . . . .
H17A H 0.037438 0.203284 0.947584 0.032 Uiso 1 1 calc R . . . .
H17B H 0.116624 0.238363 1.023385 0.032 Uiso 1 1 calc R . . . .
C12 C 0.0493(8) 0.6854(8) 0.8863(6) 0.021(2) Uani 1 1 d . . . . .
H12A H 0.000589 0.716745 0.911392 0.026 Uiso 1 1 calc R . . . .
H12B H 0.019952 0.661244 0.832840 0.026 Uiso 1 1 calc R . . . .
C27 C 0.4042(9) 0.8819(7) 1.0444(6) 0.022(2) Uani 1 1 d . . . . .
H27A H 0.330763 0.854146 1.064547 0.026 Uiso 1 1 calc R . . . .
H27B H 0.430378 0.947902 1.064623 0.026 Uiso 1 1 calc R . . . .
C3 C 0.4674(11) 0.4076(8) 0.7374(6) 0.030(3) Uani 1 1 d . . . . .
H3A H 0.523894 0.381605 0.717641 0.036 Uiso 1 1 calc R . . . .
H3B H 0.404318 0.385580 0.699729 0.036 Uiso 1 1 calc R . . . .
C9 C 0.5020(8) 0.9296(7) 0.9254(7) 0.022(2) Uani 1 1 d . . . . .
H9A H 0.563536 0.927251 0.958153 0.026 Uiso 1 1 calc R . . . .
H9B H 0.505718 0.994631 0.927269 0.026 Uiso 1 1 calc R . . . .
C14 C 0.0371(9) 0.5128(8) 0.8973(7) 0.023(2) Uani 1 1 d . . . . .
H14 H 0.029962 0.490041 0.843985 0.027 Uiso 1 1 calc R . . . .
C15 C 0.0384(7) 0.4644(8) 0.9607(6) 0.021(2) Uani 1 1 d . . . . .
C7 C 0.5363(9) 0.7584(8) 0.7525(6) 0.024(2) Uani 1 1 d . . . . .
H7C H 0.477875 0.759739 0.716289 0.029 Uiso 1 1 calc R . . . .
H7D H 0.606724 0.799281 0.735874 0.029 Uiso 1 1 calc R . . . .
C23 C 0.5187(9) 0.6266(8) 1.1789(6) 0.022(2) Uani 1 1 d . . . . .
H23 H 0.460725 0.601297 1.211675 0.027 Uiso 1 1 calc R . . . .
C5 C 0.4608(9) 0.5748(8) 0.7297(6) 0.027(3) Uani 1 1 d . . . . .
H5 H 0.387669 0.561861 0.711200 0.032 Uiso 1 1 calc R . . . .
C8 C 0.5140(9) 0.8925(8) 0.8417(6) 0.023(2) Uani 1 1 d . . . . .
H8A H 0.452727 0.895270 0.809018 0.028 Uiso 1 1 calc R . . . .
H8B H 0.582853 0.932225 0.821999 0.028 Uiso 1 1 calc R . . . .
C16 C 0.0256(8) 0.3653(7) 0.9663(7) 0.024(2) Uani 1 1 d . . . . .
H16A H -0.031027 0.326415 0.927485 0.029 Uiso 1 1 calc R . . . .
H16B H -0.000652 0.349834 1.018110 0.029 Uiso 1 1 calc R . . . .
C19 C 0.3409(10) 0.2488(8) 1.0279(7) 0.030(3) Uani 1 1 d . . . . .
H19A H 0.342054 0.185192 1.027688 0.036 Uiso 1 1 calc R . . . .
H19B H 0.282127 0.255172 1.061984 0.036 Uiso 1 1 calc R . . . .
C2 C 0.3842(10) 0.2693(8) 0.8118(7) 0.028(3) Uani 1 1 d . . . . .
H2C H 0.426611 0.241686 0.775594 0.034 Uiso 1 1 calc R . . . .
H2D H 0.307618 0.248401 0.791320 0.034 Uiso 1 1 calc R . . . .
C21 C 0.5561(8) 0.4743(8) 1.1216(6) 0.022(2) Uani 1 1 d . . . . .
H21A H 0.624550 0.464936 1.103675 0.026 Uiso 1 1 calc R . . . .
H21B H 0.542694 0.452386 1.173255 0.026 Uiso 1 1 calc R . . . .
C26 C 0.4814(8) 0.8360(8) 1.0756(6) 0.018(2) Uani 1 1 d . . . . .
H26A H 0.558232 0.873542 1.068879 0.022 Uiso 1 1 calc R . . . .
H26B H 0.467719 0.774442 1.046777 0.022 Uiso 1 1 calc R . . . .
C25 C 0.5498(8) 0.8049(7) 1.2062(6) 0.019(2) Uani 1 1 d . . . . .
H25A H 0.618979 0.857089 1.207859 0.022 Uiso 1 1 calc R . . . .
H25B H 0.527918 0.796451 1.260120 0.022 Uiso 1 1 calc R . . . .
C1 C 0.3875(10) 0.2349(8) 0.8926(7) 0.031(3) Uani 1 1 d . . . . .
H1A H 0.367180 0.167084 0.885783 0.037 Uiso 1 1 calc R . . . .
H1B H 0.463238 0.260255 0.914823 0.037 Uiso 1 1 calc R . . . .
C11 C 0.1894(8) 0.8376(8) 0.9421(6) 0.023(2) Uani 1 1 d . . . . .
H11C H 0.183731 0.817475 0.994508 0.028 Uiso 1 1 calc R . . . .
H11D H 0.134504 0.868662 0.936085 0.028 Uiso 1 1 calc R . . . .
C10 C 0.3057(8) 0.9070(8) 0.9339(7) 0.022(2) Uani 1 1 d . . . . .
H10C H 0.314858 0.919428 0.879252 0.027 Uiso 1 1 calc R . . . .
H10D H 0.312334 0.965690 0.965590 0.027 Uiso 1 1 calc R . . . .
N19 N 1.2199(7) 0.8279(6) 0.4600(5) 0.025(2) Uani 1 1 d . . . . .
H19C H 1.213080 0.836156 0.512022 0.031 Uiso 1 1 calc R . . . .
H19D H 1.157016 0.785137 0.439589 0.031 Uiso 1 1 calc R . . . .
N23 N 0.7136(7) 0.5227(6) 0.6021(5) 0.0194(19) Uani 1 1 d . . . . .
H23A H 0.652191 0.479690 0.585790 0.023 Uiso 1 1 calc R . . . .
N15 N 0.9441(7) 0.2786(6) 0.4252(5) 0.0207(19) Uani 1 1 d . . . . .
N22 N 0.7301(7) 0.6167(6) 0.6058(5) 0.0164(18) Uani 1 1 d . . . . .
N21 N 0.9103(7) 0.7968(6) 0.5636(5) 0.0185(18) Uani 1 1 d . . . . .
H21C H 0.962661 0.775362 0.542671 0.022 Uiso 1 1 calc R . . . .
H21D H 0.849702 0.774434 0.531581 0.022 Uiso 1 1 calc R . . . .
N25 N 0.8993(6) 0.3282(6) 0.2186(5) 0.0181(18) Uani 1 1 d . . . . .
H25C H 0.898479 0.270721 0.200642 0.022 Uiso 1 1 calc R . . . .
H25D H 0.965168 0.368146 0.208031 0.022 Uiso 1 1 calc R . . . .
N20 N 1.0321(7) 0.9066(6) 0.4362(5) 0.0183(18) Uani 1 1 d . . . . .
H20 H 1.021474 0.840147 0.439456 0.022 Uiso 1 1 calc R . . . .
N28 N 0.8988(7) 0.7492(6) 0.3113(5) 0.0153(17) Uani 1 1 d . . . . .
H28A H 0.873891 0.726923 0.356354 0.018 Uiso 1 1 calc R . . . .
H28B H 0.967006 0.745708 0.305127 0.018 Uiso 1 1 calc R . . . .
N18 N 1.3024(7) 0.7024(7) 0.5626(6) 0.031(2) Uani 1 1 d . . . . .
H18 H 1.307682 0.750465 0.595991 0.038 Uiso 1 1 calc R . . . .
N24 N 0.8233(7) 0.3697(6) 0.5422(5) 0.0193(19) Uani 1 1 d . . . . .
H24A H 0.888187 0.404074 0.524834 0.023 Uiso 1 1 calc R . . . .
H24B H 0.769202 0.373728 0.510801 0.023 Uiso 1 1 calc R . . . .
N16 N 1.1581(8) 0.4019(7) 0.5070(7) 0.032(2) Uani 1 1 d . . . . .
H16C H 1.116590 0.431209 0.485708 0.039 Uiso 1 1 calc R . . . .
H16D H 1.134190 0.390638 0.555197 0.039 Uiso 1 1 calc R . . . .
N27 N 0.7199(7) 0.5339(6) 0.2768(5) 0.0195(19) Uani 1 1 d . . . . .
H27 H 0.674803 0.551892 0.306911 0.023 Uiso 1 1 calc R . . . .
N26 N 0.7192(7) 0.4455(6) 0.2592(5) 0.0212(19) Uani 1 1 d . . . . .
N17 N 1.2943(7) 0.6164(7) 0.5826(6) 0.029(2) Uani 1 1 d D . . . .
C35 C 1.2328(9) 0.9185(8) 0.4274(6) 0.024(2) Uani 1 1 d . . . . .
H35A H 1.223386 0.907106 0.370286 0.029 Uiso 1 1 calc R . . . .
H35B H 1.307544 0.961615 0.440437 0.029 Uiso 1 1 calc R . . . .
C40 C 0.8341(9) 0.6584(8) 0.6331(6) 0.020(2) Uani 1 1 d . . . . .
C48 C 0.8090(8) 0.3500(7) 0.1742(6) 0.018(2) Uani 1 1 d . . . . .
H48A H 0.826252 0.351561 0.118899 0.022 Uiso 1 1 calc R . . . .
H48B H 0.738319 0.300709 0.177932 0.022 Uiso 1 1 calc R . . . .
C45 C 0.8349(9) 0.2323(8) 0.4529(7) 0.025(2) Uani 1 1 d . . . . .
H45A H 0.822937 0.165578 0.450194 0.030 Uiso 1 1 calc R . . . .
H45B H 0.779186 0.240942 0.418239 0.030 Uiso 1 1 calc R . . . .
C32 C 1.2900(8) 0.6164(9) 0.4503(7) 0.031(3) Uani 1 1 d . . . . .
H32 H 1.285602 0.595547 0.396697 0.037 Uiso 1 1 calc R . . . .
C39 C 0.8833(9) 0.7631(7) 0.6431(6) 0.021(2) Uani 1 1 d . . . . .
H39A H 0.950501 0.782492 0.676718 0.025 Uiso 1 1 calc R . . . .
H39B H 0.830602 0.790305 0.667959 0.025 Uiso 1 1 calc R . . . .
C47 C 0.8890(8) 0.3336(7) 0.3057(6) 0.019(2) Uani 1 1 d . . . . .
H47A H 0.810888 0.313438 0.318384 0.023 Uiso 1 1 calc R . . . .
H47B H 0.923416 0.397863 0.329259 0.023 Uiso 1 1 calc R . . . .
C49 C 0.7988(8) 0.4418(8) 0.2068(6) 0.019(2) Uani 1 1 d . . . . .
C28 C 1.0262(10) 0.2418(7) 0.4569(7) 0.025(2) Uani 1 1 d . . . . .
H28C H 1.022440 0.183644 0.425476 0.030 Uiso 1 1 calc R . . . .
H28D H 1.007913 0.227878 0.510471 0.030 Uiso 1 1 calc R . . . .
C51 C 0.8034(8) 0.5886(7) 0.2391(6) 0.017(2) Uani 1 1 d . . . . .
C36 C 1.1487(8) 0.9627(7) 0.4599(6) 0.023(2) Uani 1 1 d . . . . .
H36A H 1.156447 0.971431 0.517114 0.027 Uiso 1 1 calc R . . . .
H36B H 1.165280 1.024162 0.441926 0.027 Uiso 1 1 calc R . . . .
C54 C 1.0112(9) 0.9202(8) 0.3524(6) 0.024(2) Uani 1 1 d . . . . .
H54A H 1.073107 0.914410 0.321455 0.029 Uiso 1 1 calc R . . . .
H54B H 1.009002 0.983283 0.351044 0.029 Uiso 1 1 calc R . . . .
C38 C 0.9503(9) 0.9009(7) 0.5705(6) 0.021(2) Uani 1 1 d . . . . .
H38A H 1.023926 0.925012 0.596324 0.025 Uiso 1 1 calc R . . . .
H38B H 0.900381 0.924743 0.602637 0.025 Uiso 1 1 calc R . . . .
C42 C 0.8047(9) 0.5057(8) 0.6272(6) 0.023(2) Uani 1 1 d . . . . .
C43 C 0.8100(9) 0.4086(8) 0.6249(6) 0.022(2) Uani 1 1 d . . . . .
H43A H 0.742291 0.368336 0.645492 0.026 Uiso 1 1 calc R . . . .
H43B H 0.872466 0.409453 0.658254 0.026 Uiso 1 1 calc R . . . .
C41 C 0.8855(9) 0.5903(7) 0.6479(6) 0.018(2) Uani 1 1 d . U . . .
H41 H 0.957693 0.601139 0.667347 0.021 Uiso 1 1 calc R . . . .
C44 C 0.8191(9) 0.2691(8) 0.5375(7) 0.024(2) Uani 1 1 d . . . . .
H44A H 0.747756 0.231140 0.555200 0.029 Uiso 1 1 calc R . . . .
H44B H 0.877260 0.264274 0.572157 0.029 Uiso 1 1 calc R . . . .
C50 C 0.8538(9) 0.5357(7) 0.1924(7) 0.020(2) Uani 1 1 d . . . . .
H50 H 0.911751 0.556975 0.158548 0.024 Uiso 1 1 calc R . . . .
C31 C 1.2862(8) 0.5634(8) 0.5120(7) 0.027(2) Uani 1 1 d . . . . .
C46 C 0.9463(9) 0.2706(7) 0.3390(6) 0.024(2) Uani 1 1 d . . . . .
H46A H 0.908872 0.205949 0.317596 0.028 Uiso 1 1 calc R . . . .
H46B H 1.023043 0.288299 0.323094 0.028 Uiso 1 1 calc R . . . .
C53 C 0.9030(9) 0.8504(7) 0.3143(7) 0.023(2) Uani 1 1 d . . . . .
H53A H 0.840710 0.858209 0.343661 0.028 Uiso 1 1 calc R . . . .
H53B H 0.894473 0.864652 0.260919 0.028 Uiso 1 1 calc R . . . .
C33 C 1.3011(9) 0.7030(9) 0.4822(7) 0.034(3) Uani 1 1 d . . . . .
C37 C 0.9552(9) 0.9351(8) 0.4874(6) 0.024(2) Uani 1 1 d . . . . .
H37A H 0.881150 0.910717 0.462308 0.028 Uiso 1 1 calc R . . . .
H37B H 0.977043 1.003028 0.493532 0.028 Uiso 1 1 calc R . . . .
C52 C 0.8219(9) 0.6910(8) 0.2427(6) 0.022(2) Uani 1 1 d . . . . .
H52A H 0.750462 0.701147 0.247018 0.026 Uiso 1 1 calc R . . . .
H52B H 0.853382 0.712814 0.193737 0.026 Uiso 1 1 calc R . . . .
C29 C 1.1441(10) 0.3103(9) 0.4574(8) 0.035(3) Uani 1 1 d . . . . .
H29A H 1.195456 0.281848 0.477474 0.043 Uiso 1 1 calc R . . . .
H29B H 1.163227 0.322453 0.403588 0.043 Uiso 1 1 calc R . . . .
C34 C 1.3132(8) 0.7909(9) 0.4443(8) 0.033(3) Uani 1 1 d . . . . .
H34A H 1.382481 0.838729 0.463693 0.040 Uiso 1 1 calc R . . . .
H34B H 1.317657 0.777730 0.387666 0.040 Uiso 1 1 calc R . . . .
C30 C 1.2764(10) 0.4633(10) 0.5130(9) 0.042(3) Uani 1 1 d . . . . .
H30A H 1.315788 0.444416 0.469174 0.051 Uiso 1 1 calc R . . . .
H30B H 1.311010 0.455887 0.561564 0.051 Uiso 1 1 calc R . . . .
S7A S 0.6151(3) 0.8880(2) 0.5677(2) 0.0199(9) Uani 0.775(8) 1 d . . P B 1
F72A F 0.6189(7) 1.0636(6) 0.5880(6) 0.031(2) Uani 0.775(8) 1 d . . P B 1
F73A F 0.7784(9) 1.0449(9) 0.5657(11) 0.059(4) Uani 0.775(8) 1 d . . P B 1
F71A F 0.7038(13) 1.0198(10) 0.6802(7) 0.065(4) Uani 0.775(8) 1 d . . P B 1
O77A O 0.6876(8) 0.8426(7) 0.5927(8) 0.034(3) Uani 0.775(8) 1 d . . P B 1
O75A O 0.5119(10) 0.8624(9) 0.5980(11) 0.056(5) Uani 0.775(8) 1 d . U P B 1
O76A O 0.6011(15) 0.8885(10) 0.4858(9) 0.058(5) Uani 0.775(8) 1 d . U P B 1
C61A C 0.6805(13) 1.0117(10) 0.6012(9) 0.031(3) Uani 0.775(8) 1 d . . P B 1
S7B S 0.6842(9) 0.9374(8) 0.5309(7) 0.026(4) Uani 0.225(8) 1 d . U P B 2
O75B O 0.7706(16) 1.0267(12) 0.5284(17) 0.052(19) Uani 0.225(8) 1 d G U P B 2
O76B O 0.6125(19) 0.903(2) 0.4606(9) 0.052(18) Uani 0.225(8) 1 d G U P B 2
O77B O 0.717(2) 0.8679(16) 0.5671(14) 0.035(12) Uani 0.225(8) 1 d G U P B 2
C61B C 0.5893(19) 0.9669(17) 0.6036(12) 0.060(18) Uani 0.225(8) 1 d G U P B 2
F72B F 0.502(2) 0.892(2) 0.615(2) 0.057(16) Uani 0.225(8) 1 d G U P B 2
F71B F 0.641(3) 1.001(3) 0.6743(10) 0.12(3) Uani 0.225(8) 1 d G U P B 2
F73B F 0.549(3) 1.032(2) 0.581(2) 0.095(17) Uani 0.225(8) 1 d G U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As2 O21 1.750(7) . ?
As2 O22 1.715(7) . ?
As2 O24 1.644(7) . ?
As2 O23 1.651(7) . ?
As3 O31 1.703(7) . ?
As3 O34 1.644(7) . ?
As3 O32 1.707(7) . ?
As3 O33 1.700(8) . ?
As1 O11 1.741(7) . ?
As1 O12 1.737(7) . ?
As1 O14 1.650(7) . ?
As1 O13 1.626(8) . ?
As4 O41 1.731(7) . ?
As4 O43 1.644(7) . ?
As4 O44 1.662(7) . ?
As4 O42 1.700(8) . ?
As5 O54 1.669(7) . ?
As5 O52 1.719(7) . ?
As5 O51 1.710(8) . ?
As5 O53 1.658(7) . ?
As6 O64 1.670(7) . ?
As6 O61 1.690(8) . ?
As6 O62 1.707(9) . ?
As6 O63 1.678(9) . ?
S1 O15 1.433(9) . ?
S1 O17 1.445(9) . ?
S1 O16 1.445(8) . ?
S1 C55 1.811(12) . ?
F13 C55 1.338(15) . ?
F12 C55 1.328(13) . ?
F11 C55 1.332(14) . ?
S2 O27 1.439(9) . ?
S2 O26 1.433(8) . ?
S2 O25 1.450(9) . ?
S2 C56 1.822(16) . ?
F22 C56 1.361(17) . ?
F23 C56 1.298(17) . ?
F21 C56 1.301(18) . ?
S3 O37 1.455(8) . ?
S3 O35 1.437(8) . ?
S3 O36 1.438(8) . ?
S3 C57 1.832(15) . ?
F33 C57 1.369(16) . ?
F32 C57 1.313(16) . ?
F31 C57 1.316(16) . ?
S6 C60 1.793(12) . ?
S6 O66A 1.474(15) . ?
S6 O67A 1.443(14) . ?
S6 O65A 1.376(14) . ?
S6 O67B 1.50(3) . ?
S6 O65B 1.46(3) . ?
S6 O66B 1.34(3) . ?
F62 C60 1.265(12) . ?
F61 C60 1.250(13) . ?
F63 C60 1.337(15) . ?
S4 O46 1.392(12) . ?
S4 O45 1.403(8) . ?
S4 O47 1.436(13) . ?
S4 C58 1.823(14) . ?
F41 C58 1.315(15) . ?
F43 C58 1.347(15) . ?
F42 C58 1.330(15) . ?
S5 O57 1.512(10) . ?
S5 O55 1.467(10) . ?
S5 O56 1.464(10) . ?
S5 C59 1.765(15) . ?
F51 C59 1.323(14) . ?
F53 C59 1.308(16) . ?
F52 C59 1.365(15) . ?
S8 O87 1.4450 . ?
S8 O85 1.4448 . ?
S8 O86 1.4448 . ?
S8 C62 1.8511 . ?
C62 F83 1.3387 . ?
C62 F82 1.3386 . ?
C62 F81 1.3388 . ?
N4 N3 1.337(13) . ?
N4 C6 1.361(14) . ?
N8 N9 1.337(12) . ?
N8 C13 1.324(13) . ?
N1 C18 1.471(14) . ?
N1 C19 1.450(14) . ?
N1 C1 1.466(14) . ?
N14 C26 1.505(12) . ?
N14 C25 1.502(12) . ?
N6 C27 1.465(13) . ?
N6 C9 1.501(13) . ?
N6 C10 1.442(12) . ?
N3 C4 1.351(14) . ?
N11 C20 1.476(13) . ?
N11 C21 1.481(12) . ?
N13 N12 1.337(12) . ?
N13 C24 1.343(13) . ?
N5 C7 1.515(13) . ?
N5 C8 1.478(13) . ?
N10 C17 1.499(13) . ?
N10 C16 1.473(12) . ?
N2 C3 1.509(13) . ?
N2 C2 1.484(14) . ?
N12 C22 1.315(14) . ?
N7 C12 1.512(13) . ?
N7 C11 1.459(13) . ?
N9 C15 1.350(14) . ?
C4 C3 1.464(16) . ?
C4 C5 1.385(15) . ?
C13 C12 1.505(13) . ?
C13 C14 1.413(14) . ?
C22 C23 1.380(14) . ?
C22 C21 1.513(14) . ?
C20 C19 1.511(15) . ?
C18 C17 1.499(14) . ?
C24 C23 1.372(15) . ?
C24 C25 1.468(14) . ?
C6 C7 1.463(16) . ?
C6 C5 1.386(16) . ?
C27 C26 1.499(13) . ?
C9 C8 1.504(15) . ?
C14 C15 1.373(15) . ?
C15 C16 1.472(14) . ?
C2 C1 1.528(16) . ?
C11 C10 1.526(14) . ?
N19 C35 1.497(13) . ?
N19 C34 1.481(14) . ?
N23 N22 1.366(12) . ?
N23 C42 1.342(13) . ?
N15 C45 1.441(13) . ?
N15 C28 1.459(13) . ?
N15 C46 1.461(13) . ?
N22 C40 1.321(14) . ?
N21 C39 1.500(13) . ?
N21 C38 1.485(13) . ?
N25 C48 1.514(12) . ?
N25 C47 1.487(13) . ?
N20 C36 1.476(13) . ?
N20 C54 1.499(13) . ?
N20 C37 1.450(13) . ?
N28 C53 1.515(13) . ?
N28 C52 1.520(12) . ?
N18 N17 1.356(13) . ?
N18 C33 1.370(15) . ?
N24 C43 1.501(13) . ?
N24 C44 1.503(13) . ?
N16 C29 1.507(15) . ?
N16 C30 1.484(16) . ?
N27 N26 1.339(12) . ?
N27 C51 1.330(13) . ?
N26 C49 1.362(12) . ?
N17 C31 1.358(14) . ?
C35 C36 1.513(15) . ?
C40 C39 1.497(15) . ?
C40 C41 1.433(14) . ?
C48 C49 1.490(14) . ?
C45 C44 1.528(15) . ?
C32 C31 1.382(17) . ?
C32 C33 1.331(17) . ?
C47 C46 1.526(14) . ?
C49 C50 1.415(15) . ?
C28 C29 1.518(16) . ?
C51 C50 1.375(14) . ?
C51 C52 1.487(14) . ?
C54 C53 1.527(15) . ?
C38 C37 1.554(14) . ?
C42 C43 1.494(14) . ?
C42 C41 1.366(15) . ?
C31 C30 1.485(17) . ?
C33 C34 1.506(17) . ?
S7A O77A 1.405(10) . ?
S7A O75A 1.360(12) . ?
S7A O76A 1.408(15) . ?
S7A C61A 1.815(15) . ?
F72A C61A 1.310(17) . ?
F73A C61A 1.35(2) . ?
F71A C61A 1.362(19) . ?
S7B O75B 1.4449 . ?
S7B O76B 1.4463 . ?
S7B O77B 1.4450 . ?
S7B C61B 1.8513 . ?
C61B F72B 1.3390 . ?
C61B F71B 1.3380 . ?
C61B F73B 1.3380 . ?

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
O22 As2 O21 105.0(4) . . ?
O24 As2 O21 108.1(3) . . ?
O24 As2 O22 108.6(3) . . ?
O24 As2 O23 123.3(4) . . ?
O23 As2 O21 104.1(3) . . ?
O23 As2 O22 106.3(4) . . ?
O31 As3 O32 107.5(4) . . ?
O34 As3 O31 113.8(4) . . ?
O34 As3 O32 113.1(4) . . ?
O34 As3 O33 110.3(3) . . ?
O33 As3 O31 107.7(4) . . ?
O33 As3 O32 103.8(4) . . ?
O12 As1 O11 102.6(4) . . ?
O14 As1 O11 104.7(4) . . ?
O14 As1 O12 106.7(4) . . ?
O13 As1 O11 109.6(4) . . ?
O13 As1 O12 110.0(4) . . ?
O13 As1 O14 121.6(4) . . ?
O43 As4 O41 104.6(4) . . ?
O43 As4 O44 115.0(3) . . ?
O43 As4 O42 114.6(4) . . ?
O44 As4 O41 107.4(4) . . ?
O44 As4 O42 109.2(4) . . ?
O42 As4 O41 105.2(4) . . ?
O54 As5 O52 111.0(4) . . ?
O54 As5 O51 110.9(4) . . ?
O51 As5 O52 102.3(4) . . ?
O53 As5 O54 112.7(4) . . ?
O53 As5 O52 107.2(4) . . ?
O53 As5 O51 112.2(4) . . ?
O64 As6 O61 112.9(4) . . ?
O64 As6 O62 112.7(4) . . ?
O64 As6 O63 112.7(4) . . ?
O61 As6 O62 107.1(4) . . ?
O63 As6 O61 107.3(5) . . ?
O63 As6 O62 103.5(6) . . ?
O15 S1 O17 115.2(6) . . ?
O15 S1 O16 114.5(6) . . ?
O15 S1 C55 103.5(6) . . ?
O17 S1 C55 102.6(5) . . ?
O16 S1 O17 114.8(5) . . ?
O16 S1 C55 104.1(5) . . ?
F13 C55 S1 111.2(8) . . ?
F12 C55 S1 112.3(9) . . ?
F12 C55 F13 106.3(10) . . ?
F12 C55 F11 107.8(10) . . ?
F11 C55 S1 112.6(8) . . ?
F11 C55 F13 106.2(10) . . ?
O27 S2 O25 115.2(5) . . ?
O27 S2 C56 104.2(6) . . ?
O26 S2 O27 113.8(5) . . ?
O26 S2 O25 114.7(5) . . ?
O26 S2 C56 102.7(6) . . ?
O25 S2 C56 104.2(7) . . ?
F22 C56 S2 109.0(9) . . ?
F23 C56 S2 112.7(12) . . ?
F23 C56 F22 106.2(13) . . ?
F23 C56 F21 110.3(12) . . ?
F21 C56 S2 111.0(11) . . ?
F21 C56 F22 107.5(14) . . ?
O37 S3 C57 101.1(6) . . ?
O35 S3 O37 115.5(5) . . ?
O35 S3 O36 114.3(5) . . ?
O35 S3 C57 104.2(6) . . ?
O36 S3 O37 114.1(5) . . ?
O36 S3 C57 105.7(6) . . ?
F33 C57 S3 108.3(10) . . ?
F32 C57 S3 109.7(10) . . ?
F32 C57 F33 107.1(12) . . ?
F32 C57 F31 109.2(12) . . ?
F31 C57 S3 111.1(10) . . ?
F31 C57 F33 111.3(12) . . ?
O66A S6 C60 102.7(7) . . ?
O67A S6 C60 102.4(9) . . ?
O67A S6 O66A 113.1(10) . . ?
O65A S6 C60 100.4(9) . . ?
O65A S6 O66A 121.4(10) . . ?
O65A S6 O67A 113.1(13) . . ?
O67B S6 C60 108.6(13) . . ?
O65B S6 C60 110.6(13) . . ?
O65B S6 O67B 113(2) . . ?
O66B S6 C60 96.7(16) . . ?
O66B S6 O67B 113(2) . . ?
O66B S6 O65B 115(2) . . ?
F62 C60 S6 115.6(9) . . ?
F62 C60 F63 97.2(13) . . ?
F61 C60 S6 114.4(10) . . ?
F61 C60 F62 116.2(14) . . ?
F61 C60 F63 97.2(16) . . ?
F63 C60 S6 113.2(11) . . ?
O46 S4 O45 116.0(7) . . ?
O46 S4 O47 112.7(11) . . ?
O46 S4 C58 105.1(8) . . ?
O45 S4 O47 114.4(8) . . ?
O45 S4 C58 103.8(6) . . ?
O47 S4 C58 103.1(7) . . ?
F41 C58 S4 112.8(10) . . ?
F41 C58 F43 108.2(12) . . ?
F41 C58 F42 108.0(10) . . ?
F43 C58 S4 111.1(8) . . ?
F42 C58 S4 110.8(10) . . ?
F42 C58 F43 105.7(11) . . ?
O57 S5 C59 104.5(6) . . ?
O55 S5 O57 109.6(6) . . ?
O55 S5 C59 107.8(7) . . ?
O56 S5 O57 114.6(6) . . ?
O56 S5 O55 116.6(7) . . ?
O56 S5 C59 102.4(7) . . ?
F51 C59 S5 111.1(10) . . ?
F51 C59 F52 104.5(11) . . ?
F53 C59 S5 113.7(10) . . ?
F53 C59 F51 111.0(11) . . ?
F53 C59 F52 104.3(12) . . ?
F52 C59 S5 111.7(9) . . ?
O87 S8 C62 102.4 . . ?
O85 S8 O87 115.6 . . ?
O85 S8 C62 102.3 . . ?
O86 S8 O87 115.6 . . ?
O86 S8 O85 115.5 . . ?
O86 S8 C62 102.4 . . ?
F83 C62 S8 111.9 . . ?
F83 C62 F81 106.9 . . ?
F82 C62 S8 111.9 . . ?
F82 C62 F83 107.0 . . ?
F82 C62 F81 106.9 . . ?
F81 C62 S8 111.9 . . ?
N3 N4 C6 113.2(10) . . ?
C13 N8 N9 105.5(9) . . ?
C19 N1 C18 110.3(9) . . ?
C19 N1 C1 109.9(9) . . ?
C1 N1 C18 110.1(9) . . ?
C25 N14 C26 114.8(8) . . ?
C27 N6 C9 110.2(8) . . ?
C10 N6 C27 110.4(8) . . ?
C10 N6 C9 109.9(8) . . ?
N4 N3 C4 104.7(9) . . ?
C20 N11 C21 111.4(8) . . ?
N12 N13 C24 112.2(9) . . ?
C8 N5 C7 113.3(8) . . ?
C16 N10 C17 111.1(8) . . ?
C2 N2 C3 113.4(8) . . ?
C22 N12 N13 105.5(8) . . ?
C11 N7 C12 114.6(8) . . ?
N8 N9 C15 112.4(9) . . ?
N3 C4 C3 119.3(10) . . ?
N3 C4 C5 110.7(10) . . ?
C5 C4 C3 130.0(11) . . ?
N8 C13 C12 123.2(9) . . ?
N8 C13 C14 110.8(9) . . ?
C14 C13 C12 126.0(9) . . ?
N12 C22 C23 110.9(9) . . ?
N12 C22 C21 121.1(9) . . ?
C23 C22 C21 127.8(10) . . ?
N11 C20 C19 114.9(9) . . ?
N1 C18 C17 114.5(9) . . ?
N13 C24 C23 105.7(9) . . ?
N13 C24 C25 122.4(9) . . ?
C23 C24 C25 131.9(9) . . ?
N4 C6 C7 121.2(10) . . ?
N4 C6 C5 105.1(10) . . ?
C5 C6 C7 133.6(10) . . ?
N10 C17 C18 112.0(9) . . ?
C13 C12 N7 112.2(8) . . ?
N6 C27 C26 114.6(8) . . ?
C4 C3 N2 111.8(9) . . ?
N6 C9 C8 111.8(9) . . ?
C15 C14 C13 104.7(9) . . ?
N9 C15 C14 106.6(9) . . ?
N9 C15 C16 121.4(10) . . ?
C14 C15 C16 132.0(11) . . ?
C6 C7 N5 111.8(8) . . ?
C24 C23 C22 105.8(9) . . ?
C4 C5 C6 106.2(10) . . ?
N5 C8 C9 112.2(8) . . ?
C15 C16 N10 114.3(8) . . ?
N1 C19 C20 115.9(10) . . ?
N2 C2 C1 112.0(9) . . ?
N11 C21 C22 115.0(9) . . ?
C27 C26 N14 108.5(8) . . ?
C24 C25 N14 111.5(8) . . ?
N1 C1 C2 113.3(9) . . ?
N7 C11 C10 111.8(9) . . ?
N6 C10 C11 113.4(9) . . ?
C34 N19 C35 114.5(8) . . ?
C42 N23 N22 111.8(9) . . ?
C45 N15 C28 110.6(9) . . ?
C45 N15 C46 112.5(9) . . ?
C28 N15 C46 110.0(8) . . ?
C40 N22 N23 105.3(8) . . ?
C38 N21 C39 110.5(8) . . ?
C47 N25 C48 114.7(7) . . ?
C36 N20 C54 108.2(8) . . ?
C37 N20 C36 110.8(8) . . ?
C37 N20 C54 110.2(8) . . ?
C53 N28 C52 109.5(8) . . ?
N17 N18 C33 111.3(10) . . ?
C43 N24 C44 111.9(8) . . ?
C30 N16 C29 111.3(9) . . ?
C51 N27 N26 107.3(8) . . ?
N27 N26 C49 110.8(9) . . ?
N18 N17 C31 103.8(9) . . ?
N19 C35 C36 111.7(8) . . ?
N22 C40 C39 120.6(10) . . ?
N22 C40 C41 110.6(9) . . ?
C41 C40 C39 128.8(10) . . ?
C49 C48 N25 111.3(8) . . ?
N15 C45 C44 113.0(9) . . ?
C33 C32 C31 106.9(11) . . ?
C40 C39 N21 109.1(8) . . ?
N25 C47 C46 109.3(8) . . ?
N26 C49 C48 120.6(9) . . ?
N26 C49 C50 105.8(9) . . ?
C50 C49 C48 133.5(9) . . ?
N15 C28 C29 112.4(9) . . ?
N27 C51 C50 110.7(9) . . ?
N27 C51 C52 120.4(9) . . ?
C50 C51 C52 128.5(9) . . ?
N20 C36 C35 113.5(9) . . ?
N20 C54 C53 113.8(9) . . ?
N21 C38 C37 110.2(8) . . ?
N23 C42 C43 122.2(10) . . ?
N23 C42 C41 107.7(9) . . ?
C41 C42 C43 129.9(10) . . ?
C42 C43 N24 111.1(8) . . ?
C42 C41 C40 104.5(9) . . ?
N24 C44 C45 110.6(8) . . ?
C51 C50 C49 105.3(9) . . ?
N17 C31 C32 110.8(10) . . ?
N17 C31 C30 117.7(11) . . ?
C32 C31 C30 131.5(12) . . ?
N15 C46 C47 111.0(8) . . ?
N28 C53 C54 113.3(9) . . ?
N18 C33 C34 122.1(12) . . ?
C32 C33 N18 107.2(12) . . ?
C32 C33 C34 130.7(12) . . ?
N20 C37 C38 113.6(8) . . ?
C51 C52 N28 113.9(8) . . ?
N16 C29 C28 112.6(9) . . ?
N19 C34 C33 113.1(9) . . ?
N16 C30 C31 111.4(10) . . ?
O77A S7A O76A 117.2(9) . . ?
O77A S7A C61A 106.1(7) . . ?
O75A S7A O77A 116.1(8) . . ?
O75A S7A O76A 107.4(11) . . ?
O75A S7A C61A 106.3(9) . . ?
O76A S7A C61A 102.2(8) . . ?
F72A C61A S7A 113.9(11) . . ?
F72A C61A F73A 108.8(13) . . ?
F72A C61A F71A 109.2(13) . . ?
F73A C61A S7A 109.6(12) . . ?
F73A C61A F71A 107.4(15) . . ?
F71A C61A S7A 107.7(11) . . ?
O75B S7B O76B 115.5 . . ?
O75B S7B O77B 115.6 . . ?
O75B S7B C61B 102.4 . . ?
O76B S7B C61B 102.4 . . ?
O77B S7B O76B 115.5 . . ?
O77B S7B C61B 102.4 . . ?
F72B C61B S7B 111.9 . . ?
F71B C61B S7B 111.9 . . ?
F71B C61B F72B 107.0 . . ?
F71B C61B F73B 106.9 . . ?
F73B C61B S7B 111.9 . . ?
F73B C61B F72B 107.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O31 H31 N22 0.82 1.94 2.745(11) 168.7 . yes
O12 H12 O54 0.82 1.97 2.760(10) 160.7 1_556 yes
O52 H52 O5 0.82 1.82 2.617(13) 165.2 . yes
O51 H51 O43 0.82 1.76 2.579(10) 173.4 . yes
O61 H61 N3 0.82 1.89 2.653(13) 153.6 . yes
O63 H63 N12 0.82 1.89 2.690(12) 164.3 . yes
O2 H2F O1 0.85 2.08 2.83(2) 147.9 1_545 yes
O3 H3D O2 0.85 2.06 2.724(15) 135.0 . yes
O1 H1C O25 0.85 2.03 2.793(15) 149.4 1_554 yes
O6 H6B N26 0.85 2.01 2.732(13) 141.7 . yes
N4 H4 O27 0.86 1.94 2.792(13) 173.8 . yes
N14 H14A O57 0.89 2.11 2.761(13) 128.8 1_566 yes
N14 H14B O43 0.89 1.86 2.738(11) 170.2 1_556 yes
N11 H11A O54 0.89 1.86 2.742(10) 169.3 1_556 yes
N11 H11B O64 0.89 1.99 2.789(11) 148.3 . yes
N13 H13 O1 0.86 1.95 2.785(14) 162.3 1_556 yes
N5 H5A O14 0.89 1.92 2.793(11) 166.9 . yes
N10 H10B O65A 0.89 2.11 2.851(17) 139.6 . yes
N10 H10B O67B 0.89 1.99 2.86(3) 165.0 . yes
N2 H2A O64 0.89 1.94 2.776(12) 156.7 . yes
N2 H2B O13 0.89 1.91 2.752(11) 157.7 . yes
N7 H7A O14 0.89 1.97 2.832(11) 162.0 . yes
N7 H7B O36 0.89 2.06 2.853(12) 147.6 . yes
N9 H9 O53 0.86 1.86 2.704(12) 165.6 1_556 yes
N19 H19C O37 0.89 1.92 2.798(12) 167.4 1_655 yes
N19 H19D O24 0.89 1.99 2.716(11) 137.8 . yes
N23 H23A O17 0.86 1.97 2.822(12) 172.2 . yes
N21 H21C O24 0.89 1.96 2.803(11) 157.1 . yes
N25 H25C O3 0.89 1.90 2.722(12) 153.7 . yes
N25 H25D O53 0.89 1.79 2.648(11) 161.4 1_655 yes
N28 H28A O34 0.89 1.97 2.791(10) 152.3 . yes
N28 H28B O44 0.89 1.81 2.697(10) 175.5 1_655 yes
N24 H24A O23 0.89 1.86 2.730(11) 165.5 . yes
N16 H16C O23 0.89 1.94 2.739(11) 148.5 . yes
N16 H16D O66B 0.89 2.06 2.79(4) 138.5 1_655 yes
N27 H27 O33 0.86 1.75 2.595(11) 166.5 . yes

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_crystal6_percl
_database_code_depnum_ccdc_archive 'CCDC 1912383'
loop_
_audit_author_name
_audit_author_address
'Javier Pitarch-Jarque'
;Universitat de Valencia
Spain
;
_audit_update_record             
;
2019-04-26 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_audit_creation_date             2019-03-11
_audit_creation_method           
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '7(Cl O4), C27 H55 N14, 4(H2 O)'
_chemical_formula_sum            'C27 H63 Cl7 N14 O32'
_chemical_formula_weight         1344.06
_chemical_absolute_configuration .
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   13.8160(10)
_cell_length_b                   13.9700(10)
_cell_length_c                   28.6830(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5536.1(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22979
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            43512
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         1.420
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6890
_reflns_number_total             12640
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla et al.,  2007)'
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.58(14)
_refine_ls_extinction_coef       0.0088(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         12640
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.0923
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1840P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2567
_refine_ls_wR_factor_ref         0.2928
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.42(14)
 0.58(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 H1C-O24_$1
 2.2 with sigma of 0.1
 N3_$3-H3C
 1.8 with sigma of 0.1
 O3-H3C = O3-H3D
 0.85 with sigma of 0.02
 O43_$4-H3D
 2.2 with sigma of 0.1
 H3C-H3D
 1.33 with sigma of 0.02
4.a Free rotating group:
 O2(H2E,H2F), O1(H1C,H1D), O4(H4A,H4B)
4.b Ternary CH refined with riding coordinates:
 N1(H1)
4.c Secondary CH2 refined with riding coordinates:
 N14(H14A,H14B), N5(H5A,H5B), N11(H11A,H11B), N2(H2A,H2B), N10(H10A,H10B),
 N7(H7A,H7B), C26(H26A,H26B), C3(H3A,H3B), C8(H8A,H8B), C20(H20A,H20B), C2(H2C,
 H2D), C7(H7C,H7D), C25(H25A,H25B), C21(H21A,H21B), C17(H17A,H17B), C9(H9A,H9B),
  C27(H27A,H27B), C10(H10C,H10D), C12(H12A,H12B), C11(H11C,H11D), C16(H16A,
 H16B), C19(H19A,H19B), C1(H1A,H1B), C18(H18A,H18B)
4.d Aromatic/amide H refined with riding coordinates:
 N12(H12), N4(H4), C23(H23), C5(H5), N9(H9), C14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.87720(16) 0.51369(17) 0.38227(7) 0.0485(5) Uani 1 1 d . . . . .
Cl2 Cl 0.36963(19) 0.28200(18) 0.51975(9) 0.0581(7) Uani 1 1 d . . . . .
Cl5 Cl 0.6274(2) 0.4834(2) 0.70204(9) 0.0629(7) Uani 1 1 d . . . . .
Cl3 Cl 0.3746(2) 0.6876(2) 0.51198(12) 0.0733(9) Uani 1 1 d . . . . .
Cl4 Cl 0.2093(2) 0.5168(2) 0.30501(10) 0.0729(8) Uani 1 1 d . . . . .
Cl6 Cl 0.5296(3) 0.8741(3) 0.36039(11) 0.0924(12) Uani 1 1 d . . . . .
Cl7 Cl 0.4708(5) 0.2327(4) 0.37164(14) 0.133(2) Uani 1 1 d . . . . .
O12 O 0.9724(4) 0.5206(5) 0.3597(2) 0.0578(17) Uani 1 1 d . . . . .
O13 O 0.8027(5) 0.5124(6) 0.3483(2) 0.0644(19) Uani 1 1 d . . . . .
O14 O 0.8671(5) 0.5954(5) 0.4115(2) 0.0567(17) Uani 1 1 d . . . . .
O11 O 0.8744(6) 0.4261(5) 0.4092(2) 0.0651(19) Uani 1 1 d . . . . .
N14 N 1.0888(6) 0.3569(6) 0.4026(3) 0.0481(18) Uani 1 1 d . . . . .
H14A H 1.099249 0.406514 0.383857 0.058 Uiso 1 1 calc R . . . .
H14B H 1.030060 0.363741 0.414967 0.058 Uiso 1 1 calc R . . . .
N6 N 1.0896(5) 0.5127(6) 0.4712(2) 0.0470(17) Uani 1 1 d . . . . .
N12 N 0.8596(7) 0.1806(6) 0.3299(3) 0.057(2) Uani 1 1 d . . . . .
H12 H 0.813113 0.139638 0.329841 0.069 Uiso 1 1 calc R . . . .
N3 N 0.8657(7) 0.8535(6) 0.3306(3) 0.064(2) Uani 1 1 d D . . . .
N5 N 1.0687(6) 0.6841(6) 0.4089(3) 0.0528(19) Uani 1 1 d . . . . .
H5A H 1.016101 0.701546 0.424678 0.063 Uiso 1 1 calc R . . . .
H5B H 1.056013 0.627731 0.395814 0.063 Uiso 1 1 calc R . . . .
N1 N 0.5896(5) 0.5292(6) 0.2854(3) 0.0455(17) Uani 1 1 d . . . . .
H1 H 0.649901 0.526568 0.303305 0.055 Uiso 1 1 calc R . . . .
N11 N 0.7201(6) 0.3559(6) 0.2856(3) 0.055(2) Uani 1 1 d . . . . .
H11A H 0.699894 0.340109 0.314012 0.066 Uiso 1 1 calc R . . . .
H11B H 0.751418 0.411450 0.287579 0.066 Uiso 1 1 calc R . . . .
N2 N 0.7336(6) 0.6844(6) 0.2760(3) 0.054(2) Uani 1 1 d . . . . .
H2A H 0.768584 0.631343 0.272530 0.065 Uiso 1 1 calc R . . . .
H2B H 0.713643 0.687089 0.305431 0.065 Uiso 1 1 calc R . . . .
N10 N 0.5720(6) 0.5249(7) 0.3919(3) 0.061(2) Uani 1 1 d . . . . .
H10A H 0.617480 0.569076 0.387591 0.073 Uiso 1 1 calc R . . . .
H10B H 0.597945 0.467651 0.386442 0.073 Uiso 1 1 calc R . . . .
O22 O 0.4617(6) 0.2533(6) 0.5374(3) 0.072(2) Uani 1 1 d . . . . .
C22 C 0.8661(8) 0.2600(7) 0.3023(3) 0.055(2) Uani 1 1 d . . . . .
C4 C 0.8708(7) 0.7840(7) 0.2998(3) 0.052(2) Uani 1 1 d . . . . .
N7 N 0.8876(6) 0.4617(6) 0.5570(3) 0.055(2) Uani 1 1 d . . . . .
H7A H 0.926902 0.463648 0.581563 0.066 Uiso 1 1 calc R . . . .
H7B H 0.878375 0.400420 0.549770 0.066 Uiso 1 1 calc R . . . .
N4 N 0.9484(7) 0.8524(6) 0.3582(3) 0.063(2) Uani 1 1 d . . . . .
H4 H 0.963761 0.893542 0.379245 0.076 Uiso 1 1 calc R . . . .
C26 C 1.1600(8) 0.3582(7) 0.4398(3) 0.053(2) Uani 1 1 d . . . . .
H26A H 1.138489 0.316392 0.464764 0.063 Uiso 1 1 calc R . . . .
H26B H 1.220783 0.333271 0.428057 0.063 Uiso 1 1 calc R . . . .
N13 N 0.9395(6) 0.1777(6) 0.3573(3) 0.053(2) Uani 1 1 d . . . . .
O52 O 0.6566(7) 0.4879(6) 0.7501(3) 0.079(2) Uani 1 1 d . . . . .
O2 O 0.6947(7) 0.6909(6) 0.3772(3) 0.074(2) Uani 1 1 d . . . . .
H2E H 0.751363 0.696317 0.388444 0.110 Uiso 1 1 d G . . . .
H2F H 0.669914 0.746273 0.380322 0.110 Uiso 1 1 d G . . . .
O21 O 0.3800(7) 0.3721(6) 0.4985(4) 0.091(3) Uani 1 1 d . . . . .
O53 O 0.6628(8) 0.3976(6) 0.6823(3) 0.092(3) Uani 1 1 d . . . . .
O1 O 0.6855(7) 0.3423(7) 0.3846(3) 0.075(2) Uani 1 1 d . . . . .
H1C H 0.706659 0.341452 0.412437 0.113 Uiso 1 1 d DG . . . .
H1D H 0.626874 0.324610 0.386967 0.113 Uiso 1 1 d G . . . .
O4 O 0.4515(10) 0.4774(7) 0.5901(3) 0.100(3) Uani 1 1 d . . . . .
H4A H 0.512600 0.480788 0.593029 0.149 Uiso 1 1 d G . . . .
H4B H 0.435191 0.429799 0.606794 0.149 Uiso 1 1 d G . . . .
C3 C 0.7941(9) 0.7679(8) 0.2658(3) 0.061(3) Uani 1 1 d . . . . .
H3A H 0.823091 0.759806 0.235270 0.073 Uiso 1 1 calc R . . . .
H3B H 0.753206 0.824315 0.264613 0.073 Uiso 1 1 calc R . . . .
C6 C 0.9987(8) 0.7765(8) 0.3459(3) 0.056(3) Uani 1 1 d . . . . .
O24 O 0.3066(7) 0.2924(8) 0.5568(4) 0.094(3) Uani 1 1 d D . . . .
C8 C 1.1463(8) 0.6706(7) 0.4420(4) 0.059(3) Uani 1 1 d . . . . .
H8A H 1.167118 0.732564 0.453517 0.070 Uiso 1 1 calc R . . . .
H8B H 1.200864 0.641092 0.426303 0.070 Uiso 1 1 calc R . . . .
O51 O 0.6653(8) 0.5635(6) 0.6796(3) 0.089(3) Uani 1 1 d . . . . .
C23 C 0.9531(7) 0.3064(7) 0.3121(3) 0.048(2) Uani 1 1 d . . . . .
H23 H 0.977479 0.361187 0.297959 0.058 Uiso 1 1 calc R . . . .
C20 C 0.6363(8) 0.3667(8) 0.2546(4) 0.060(3) Uani 1 1 d . . . . .
H20A H 0.610542 0.303899 0.247189 0.071 Uiso 1 1 calc R . . . .
H20B H 0.657031 0.396282 0.225648 0.071 Uiso 1 1 calc R . . . .
C2 C 0.6494(8) 0.6801(7) 0.2450(4) 0.057(3) Uani 1 1 d . . . . .
H2C H 0.667721 0.702800 0.214318 0.068 Uiso 1 1 calc R . . . .
H2D H 0.599282 0.722186 0.256927 0.068 Uiso 1 1 calc R . . . .
C7 C 1.0840(9) 0.7543(8) 0.3712(4) 0.063(3) Uani 1 1 d . . . . .
H7C H 1.109729 0.812798 0.384589 0.076 Uiso 1 1 calc R . . . .
H7D H 1.131997 0.729270 0.349770 0.076 Uiso 1 1 calc R . . . .
C25 C 1.0910(7) 0.2655(7) 0.3740(4) 0.051(2) Uani 1 1 d . . . . .
H25A H 1.101292 0.211000 0.394386 0.061 Uiso 1 1 calc R . . . .
H25B H 1.144249 0.268073 0.351969 0.061 Uiso 1 1 calc R . . . .
C5 C 0.9566(8) 0.7299(8) 0.3077(4) 0.061(3) Uani 1 1 d . . . . .
H5 H 0.979198 0.676693 0.291549 0.074 Uiso 1 1 calc R . . . .
N8 N 0.6558(8) 0.4144(8) 0.5385(4) 0.081(3) Uani 1 1 d . . . . .
C21 C 0.7875(9) 0.2806(8) 0.2678(4) 0.061(3) Uani 1 1 d . . . . .
H21A H 0.816111 0.301826 0.238733 0.073 Uiso 1 1 calc R . . . .
H21B H 0.751405 0.222410 0.261683 0.073 Uiso 1 1 calc R . . . .
C24 C 0.9957(7) 0.2532(6) 0.3477(3) 0.048(2) Uani 1 1 d . . . . .
C15 C 0.6100(7) 0.5049(8) 0.4772(3) 0.060(3) Uani 1 1 d . . . . .
C17 C 0.4919(7) 0.5415(9) 0.3601(4) 0.061(3) Uani 1 1 d . . . . .
H17A H 0.446815 0.584935 0.375020 0.073 Uiso 1 1 calc R . . . .
H17B H 0.458384 0.481198 0.355435 0.073 Uiso 1 1 calc R . . . .
C9 C 1.1161(7) 0.6086(7) 0.4828(3) 0.054(2) Uani 1 1 d . . . . .
H9A H 1.169040 0.606393 0.504921 0.065 Uiso 1 1 calc R . . . .
H9B H 1.061591 0.638862 0.498169 0.065 Uiso 1 1 calc R . . . .
C27 C 1.1761(7) 0.4534(8) 0.4586(4) 0.059(3) Uani 1 1 d . . . . .
H27A H 1.213826 0.489078 0.435986 0.070 Uiso 1 1 calc R . . . .
H27B H 1.215743 0.446881 0.486358 0.070 Uiso 1 1 calc R . . . .
O34 O 0.3635(7) 0.5952(9) 0.5006(6) 0.147(6) Uani 1 1 d . . . . .
N9 N 0.6014(8) 0.4235(8) 0.5038(4) 0.080(3) Uani 1 1 d . . . . .
H9 H 0.559890 0.379941 0.496807 0.096 Uiso 1 1 calc R . . . .
C10 C 1.0365(6) 0.4678(7) 0.5102(3) 0.048(2) Uani 1 1 d . . . . .
H10C H 1.073772 0.475960 0.538609 0.058 Uiso 1 1 calc R . . . .
H10D H 1.031023 0.399641 0.504316 0.058 Uiso 1 1 calc R . . . .
C13 C 0.7176(7) 0.4935(8) 0.5352(3) 0.055(2) Uani 1 1 d . . . . .
C12 C 0.7944(9) 0.5034(9) 0.5703(4) 0.071(3) Uani 1 1 d . . . . .
H12A H 0.803850 0.570979 0.576700 0.085 Uiso 1 1 calc R . . . .
H12B H 0.772878 0.473405 0.598974 0.085 Uiso 1 1 calc R . . . .
O23 O 0.3300(7) 0.2152(7) 0.4886(4) 0.103(3) Uani 1 1 d . . . . .
C11 C 0.9357(7) 0.5086(8) 0.5178(3) 0.055(2) Uani 1 1 d . . . . .
H11C H 0.940399 0.576770 0.523895 0.066 Uiso 1 1 calc R . . . .
H11D H 0.897452 0.499821 0.489793 0.066 Uiso 1 1 calc R . . . .
C14 C 0.6903(8) 0.5511(9) 0.4981(4) 0.067(3) Uani 1 1 d . . . . .
H14 H 0.718917 0.608259 0.488800 0.080 Uiso 1 1 calc R . . . .
O54 O 0.5264(6) 0.4863(8) 0.7013(4) 0.107(3) Uani 1 1 d . . . . .
O41 O 0.1482(10) 0.4319(10) 0.3067(7) 0.172(7) Uani 1 1 d . . . . .
O62 O 0.5607(16) 0.8393(15) 0.4010(4) 0.209(11) Uani 1 1 d . . . . .
O33 O 0.4688(7) 0.6985(8) 0.5280(5) 0.116(4) Uani 1 1 d . . . . .
O61 O 0.5803(10) 0.8463(10) 0.3212(4) 0.129(5) Uani 1 1 d . . . . .
C16 C 0.5356(10) 0.5294(13) 0.4405(4) 0.094(5) Uani 1 1 d . . . . .
H16A H 0.481387 0.485687 0.443561 0.113 Uiso 1 1 calc R . . . .
H16B H 0.511599 0.593522 0.446423 0.113 Uiso 1 1 calc R . . . .
C19 C 0.5542(9) 0.4293(10) 0.2772(5) 0.078(4) Uani 1 1 d . . . . .
H19A H 0.498359 0.430811 0.256675 0.094 Uiso 1 1 calc R . . . .
H19B H 0.534365 0.401070 0.306555 0.094 Uiso 1 1 calc R . . . .
O43 O 0.2875(9) 0.4973(14) 0.2760(5) 0.156(6) Uani 1 1 d D . . . .
C1 C 0.6083(12) 0.5763(10) 0.2409(4) 0.083(4) Uani 1 1 d . . . . .
H1A H 0.548475 0.578513 0.223317 0.100 Uiso 1 1 calc R . . . .
H1B H 0.653976 0.537707 0.223408 0.100 Uiso 1 1 calc R . . . .
O71 O 0.5295(12) 0.1983(10) 0.4067(4) 0.139(5) Uani 1 1 d . . . . .
O32 O 0.3053(10) 0.7213(14) 0.5443(7) 0.193(9) Uani 1 1 d . . . . .
C18 C 0.5172(9) 0.5823(11) 0.3122(5) 0.078(3) Uani 1 1 d . . . . .
H18A H 0.458266 0.585716 0.293868 0.094 Uiso 1 1 calc R . . . .
H18B H 0.540374 0.647284 0.316394 0.094 Uiso 1 1 calc R . . . .
O72 O 0.5201(18) 0.2288(12) 0.3274(4) 0.206(11) Uani 1 1 d . . . . .
O31 O 0.3698(11) 0.7464(18) 0.4748(7) 0.213(11) Uani 1 1 d . . . . .
O44 O 0.1564(11) 0.5899(9) 0.2836(6) 0.152(5) Uani 1 1 d . . . . .
O74 O 0.3898(13) 0.1751(11) 0.3688(4) 0.161(7) Uani 1 1 d . . . . .
O64 O 0.513(2) 0.9697(12) 0.3619(5) 0.233(13) Uani 1 1 d . . . . .
O73 O 0.4450(18) 0.3236(11) 0.3794(7) 0.196(9) Uani 1 1 d . . . . .
O42 O 0.2181(18) 0.5357(17) 0.3478(6) 0.244(13) Uani 1 1 d . . . . .
O63 O 0.4483(14) 0.832(3) 0.3562(9) 0.35(2) Uani 1 1 d . . . . .
O3 O 0.2480(13) 0.4755(9) 0.6706(8) 0.173(7) Uani 1 1 d D . . . .
H3C H 0.297(12) 0.512(14) 0.676(9) 0.260 Uiso 1 1 d DR . . . .
H3D H 0.23(2) 0.456(14) 0.698(3) 0.260 Uiso 1 1 d DR . . . .


_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
Cl1 O12 1.470(7) . ?
Cl1 O13 1.417(7) . ?
Cl1 O14 1.423(7) . ?
Cl1 O11 1.447(8) . ?
Cl2 O22 1.427(8) . ?
Cl2 O21 1.407(9) . ?
Cl2 O24 1.381(10) . ?
Cl2 O23 1.403(9) . ?
Cl5 O52 1.437(8) . ?
Cl5 O53 1.413(9) . ?
Cl5 O51 1.393(9) . ?
Cl5 O54 1.395(9) . ?
Cl3 O34 1.340(11) . ?
Cl3 O33 1.387(10) . ?
Cl3 O32 1.414(14) . ?
Cl3 O31 1.349(16) . ?
Cl4 O41 1.455(13) . ?
Cl4 O43 1.390(12) . ?
Cl4 O44 1.398(13) . ?
Cl4 O42 1.262(15) . ?
Cl6 O62 1.333(13) . ?
Cl6 O61 1.381(10) . ?
Cl6 O64 1.355(15) . ?
Cl6 O63 1.272(17) . ?
Cl7 O71 1.377(13) . ?
Cl7 O72 1.442(17) . ?
Cl7 O74 1.382(13) . ?
Cl7 O73 1.337(18) . ?
N14 C26 1.452(13) . ?
N14 C25 1.519(12) . ?
N6 C9 1.428(12) . ?
N6 C27 1.499(13) . ?
N6 C10 1.479(11) . ?
N12 C22 1.365(13) . ?
N12 N13 1.356(12) . ?
N3 C4 1.314(13) . ?
N3 N4 1.391(13) . ?
N5 C8 1.444(14) . ?
N5 C7 1.475(13) . ?
N1 C19 1.497(15) . ?
N1 C1 1.457(14) . ?
N1 C18 1.464(15) . ?
N11 C20 1.468(13) . ?
N11 C21 1.494(14) . ?
N2 C3 1.465(13) . ?
N2 C2 1.464(13) . ?
N10 C17 1.453(13) . ?
N10 C16 1.484(14) . ?
C22 C23 1.394(15) . ?
C22 C21 1.497(15) . ?
C4 C3 1.457(15) . ?
C4 C5 1.425(15) . ?
N7 C12 1.464(15) . ?
N7 C11 1.461(12) . ?
N4 C6 1.316(14) . ?
C26 C27 1.451(15) . ?
N13 C24 1.339(13) . ?
C6 C7 1.417(16) . ?
C6 C5 1.401(15) . ?
C8 C9 1.515(15) . ?
C23 C24 1.392(13) . ?
C20 C19 1.573(18) . ?
C2 C1 1.562(17) . ?
C25 C24 1.527(14) . ?
N8 N9 1.254(14) . ?
N8 C13 1.399(14) . ?
C15 N9 1.374(16) . ?
C15 C14 1.416(15) . ?
C15 C16 1.512(17) . ?
C17 C18 1.527(17) . ?
C10 C11 1.520(13) . ?
C13 C12 1.471(16) . ?
C13 C14 1.386(15) . ?

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
O13 Cl1 O12 110.4(4) . . ?
O13 Cl1 O14 110.1(4) . . ?
O13 Cl1 O11 109.6(5) . . ?
O14 Cl1 O12 107.2(4) . . ?
O14 Cl1 O11 111.2(4) . . ?
O11 Cl1 O12 108.3(5) . . ?
O21 Cl2 O22 108.3(6) . . ?
O24 Cl2 O22 108.6(6) . . ?
O24 Cl2 O21 107.7(6) . . ?
O24 Cl2 O23 108.3(6) . . ?
O23 Cl2 O22 112.8(5) . . ?
O23 Cl2 O21 111.1(7) . . ?
O53 Cl5 O52 108.9(5) . . ?
O51 Cl5 O52 107.6(6) . . ?
O51 Cl5 O53 111.5(6) . . ?
O51 Cl5 O54 110.2(7) . . ?
O54 Cl5 O52 107.0(7) . . ?
O54 Cl5 O53 111.4(7) . . ?
O34 Cl3 O33 107.1(7) . . ?
O34 Cl3 O32 113.7(10) . . ?
O34 Cl3 O31 112.9(14) . . ?
O33 Cl3 O32 112.4(8) . . ?
O31 Cl3 O33 103.9(9) . . ?
O31 Cl3 O32 106.4(14) . . ?
O43 Cl4 O41 108.2(9) . . ?
O43 Cl4 O44 106.7(10) . . ?
O44 Cl4 O41 107.9(10) . . ?
O42 Cl4 O41 101.2(16) . . ?
O42 Cl4 O43 123.2(13) . . ?
O42 Cl4 O44 109.0(12) . . ?
O62 Cl6 O61 116.5(9) . . ?
O62 Cl6 O64 112.7(11) . . ?
O64 Cl6 O61 112.8(10) . . ?
O63 Cl6 O62 101.4(16) . . ?
O63 Cl6 O61 104.0(18) . . ?
O63 Cl6 O64 108(2) . . ?
O71 Cl7 O72 110.5(13) . . ?
O71 Cl7 O74 108.5(8) . . ?
O74 Cl7 O72 108.0(9) . . ?
O73 Cl7 O71 111.6(12) . . ?
O73 Cl7 O72 107.9(11) . . ?
O73 Cl7 O74 110.3(14) . . ?
C26 N14 C25 113.2(8) . . ?
C9 N6 C27 111.7(8) . . ?
C9 N6 C10 110.4(7) . . ?
C10 N6 C27 110.1(7) . . ?
N13 N12 C22 107.8(9) . . ?
C4 N3 N4 109.3(9) . . ?
C8 N5 C7 117.5(8) . . ?
C1 N1 C19 109.9(9) . . ?
C1 N1 C18 110.7(10) . . ?
C18 N1 C19 109.4(9) . . ?
C20 N11 C21 110.9(7) . . ?
C2 N2 C3 111.4(8) . . ?
C17 N10 C16 109.0(9) . . ?
N12 C22 C23 108.5(9) . . ?
N12 C22 C21 119.4(10) . . ?
C23 C22 C21 132.0(10) . . ?
N3 C4 C3 121.6(10) . . ?
N3 C4 C5 109.2(9) . . ?
C5 C4 C3 129.1(10) . . ?
C11 N7 C12 115.0(9) . . ?
C6 N4 N3 106.9(9) . . ?
C27 C26 N14 112.9(8) . . ?
C24 N13 N12 109.3(8) . . ?
C4 C3 N2 113.9(8) . . ?
N4 C6 C7 118.6(10) . . ?
N4 C6 C5 111.4(10) . . ?
C5 C6 C7 130.0(11) . . ?
N5 C8 C9 112.2(9) . . ?
C24 C23 C22 105.3(9) . . ?
N11 C20 C19 112.1(8) . . ?
N2 C2 C1 111.8(8) . . ?
C6 C7 N5 113.7(9) . . ?
N14 C25 C24 110.1(8) . . ?
C6 C5 C4 102.9(10) . . ?
N9 N8 C13 103.3(9) . . ?
N11 C21 C22 111.3(8) . . ?
N13 C24 C23 109.0(9) . . ?
N13 C24 C25 119.1(9) . . ?
C23 C24 C25 131.8(9) . . ?
N9 C15 C14 102.2(10) . . ?
N9 C15 C16 121.0(11) . . ?
C14 C15 C16 136.4(12) . . ?
N10 C17 C18 116.8(8) . . ?
N6 C9 C8 115.3(8) . . ?
C26 C27 N6 118.2(8) . . ?
N8 N9 C15 118.2(10) . . ?
N6 C10 C11 113.8(7) . . ?
N8 C13 C12 117.9(9) . . ?
C14 C13 N8 110.2(10) . . ?
C14 C13 C12 131.8(10) . . ?
N7 C12 C13 114.7(8) . . ?
N7 C11 C10 111.0(8) . . ?
C13 C14 C15 105.8(10) . . ?
N10 C16 C15 114.5(10) . . ?
N1 C19 C20 110.3(9) . . ?
N1 C1 C2 114.7(9) . . ?
N1 C18 C17 116.1(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N14 H14B N6 0.89 2.76 2.933(11) 92.4 . yes
N14 H14B O22 0.89 2.33 2.900(11) 121.8 3_556 yes
N12 H12 O3 0.86 1.84 2.671(18) 160.9 3_556 yes
N5 H5A O33 0.89 2.05 2.806(14) 141.4 3_566 yes
N5 H5B O12 0.89 2.16 2.997(11) 157.3 . yes
N5 H5B N6 0.89 2.73 3.001(11) 98.8 . yes
N11 H11A O1 0.89 2.03 2.886(12) 159.9 . yes
N11 H11B N1 0.89 2.78 3.019(11) 97.1 . yes
N11 H11B O52 0.89 2.18 2.949(13) 144.5 2_664 yes
N2 H2A O52 0.89 2.06 2.940(12) 168.1 2_664 yes
N2 H2B O2 0.89 2.07 2.954(12) 169.1 . yes
N10 H10A O2 0.89 2.03 2.905(13) 166.7 . yes
N10 H10B O1 0.89 2.13 3.002(14) 166.5 . yes
N7 H7A O74 0.89 2.46 2.861(13) 107.9 3_556 yes
N7 H7B O23 0.89 2.07 2.907(13) 157.3 3_556 yes
N4 H4 O4 0.86 2.01 2.803(14) 152.2 3_566 yes
O2 H2E O14 0.85 2.23 2.902(11) 135.7 . yes
O2 H2E O32 0.85 2.37 2.985(16) 130.0 3_566 yes
O2 H2F O62 0.85 2.08 2.863(18) 153.1 . yes
O1 H1C O11 0.85 2.60 2.946(12) 105.4 . yes
O1 H1D O71 0.85 2.29 3.015(17) 143.5 . yes
O4 H4A N8 0.85 2.69 3.306(17) 130.8 . yes
O4 H4B N13 0.85 1.82 2.646(12) 162.7 3_456 yes
C25 H25B O53 0.97 2.53 2.963(13) 107.2 3_556 yes
O3 H3C N3 0.86(3) 2.12(11) 2.890(17) 150(20) 3_466 yes

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.42(14)
2 0.58(14)
####################################################################### 
# 
# 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_crystal5_sulphate
_database_code_depnum_ccdc_archive 'CCDC 1912382'
loop_
_audit_author_name
_audit_author_address
'Javier Pitarch-Jarque'
;Universitat de Valencia
Spain
;
_audit_update_record             
;
2019-04-26 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_audit_creation_date             2019-03-11
_audit_creation_method           
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H57 N14, 3(O4 S), 3(H O4 S), 6(H2 O)'
_chemical_formula_sum            'C27 H72 N14 O30 S6'
_chemical_formula_weight         1265.34
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   11.4324(2)
_cell_length_b                   17.2812(3)
_cell_length_c                   26.4489(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.7130(10)
_cell_angle_gamma                90
_cell_volume                     5189.57(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20583
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      0.998
_shelx_estimated_absorpt_T_max   0.993
_shelx_estimated_absorpt_T_min   0.910
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            42829
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         1.948
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6370
_reflns_number_total             11838
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         11838
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.0553
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0793P)²+0.8105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1604
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H3D-O51
 1.9 with sigma of 0.1
 O20_$6-H3C
 1.4 with sigma of 0.1
 O43-H2E
 2 with sigma of 0.1
 H4A-O3
 2 with sigma of 0.1
 O21-O24 \\sim O21-O25 \\sim O21-O20 \\sim O24-O25 \\sim O24-O20 \\sim O24-O21
 with sigma of 0.02
 S2A-O21 \\sim S2A-O24 \\sim S2A-O25 \\sim S2A-O20
 with sigma of 0.02
 O23-O22 \\sim O23-O27 \\sim O23-O26 \\sim O22-O27 \\sim O22-O26 \\sim O27-O26
 with sigma of 0.02
 S2B-O27 \\sim S2B-O22 \\sim S2B-O23 \\sim S2B-O26
 with sigma of 0.02
3. Rigid bond restraints
 S2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5. Others
 Sof(S2B)=Sof(O26)=Sof(O23)=Sof(O27)=Sof(O22)=1-FVAR(1)
 Sof(S2A)=Sof(O25)=Sof(O20)=Sof(O24)=Sof(O21)=FVAR(1)
 Fixed X: H1C(0.431409) H1D(0.432329) H3C(0.04363) H3D(0.08855)
 Fixed Y: H1C(0.29216) H1D(0.317361) H3C(0.06403) H3D(0.08434)
 Fixed Z: H1C(0.34235) H1D(0.287459) H3C(0.03868) H3D(0.086519)
6.a Free rotating group:
 O2(H2E,H2F), O4(H4A,H4B), O5(H5C,H5D), O6(H6A,H6B)
6.b Secondary CH2 refined with riding coordinates:
 N10(H10A,H10B), N2(H2A,H2B), N5(H5A,H5B), N14(H14A,H14B), N11(H11A,H11B),
 N7(H7A,H7B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C1(H1A,H1B),
 C2(H2C,H2D), C3(H3A,H3B), C7(H7C,H7D), C8(H8A,H8B), C9(H9A,H9B), C27(H27A,
 H27B), C26(H26A,H26B), C25(H25A,H25B), C21(H21A,H21B), C20(H20A,H20B),
 C19(H19A,H19B), C10(H10C,H10D), C11(H11C,H11D), C12(H12A,H12B)
6.c Aromatic/amide H refined with riding coordinates:
 N8(H8), N9(H9), N3(H3), N4(H4), N13(H13), N12(H12), C23(H23), C14(H14), C5(H5)
6.d Idealised tetrahedral OH refined as rotating group:
 O13(H13A), O54(H54), O63(H63)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
N8 N 0.6433(2) 0.53401(16) 0.26557(9) 0.0352(6) Uani 1 1 d . . . . .
H8 H 0.639255 0.577688 0.280847 0.042 Uiso 1 1 calc R . . . .
N9 N 0.6360(2) 0.52456(16) 0.21530(9) 0.0358(6) Uani 1 1 d . . . . .
H9 H 0.626684 0.561018 0.193060 0.043 Uiso 1 1 calc R . . . .
N10 N 0.5174(2) 0.40184(16) 0.12964(9) 0.0331(6) Uani 1 1 d . . . . .
H10A H 0.494478 0.359095 0.144452 0.040 Uiso 1 1 calc R . . . .
H10B H 0.469201 0.440060 0.136140 0.040 Uiso 1 1 calc R . . . .
N1 N 0.2990(2) 0.43156(15) 0.05783(9) 0.0344(6) Uani 1 1 d . . . . .
N2 N 0.2863(2) 0.59027(16) 0.09829(10) 0.0394(7) Uani 1 1 d . . . . .
H2A H 0.363936 0.596177 0.104782 0.047 Uiso 1 1 calc R . . . .
H2B H 0.265646 0.550463 0.116669 0.047 Uiso 1 1 calc R . . . .
N3 N 0.3580(3) 0.70285(18) 0.18855(11) 0.0488(8) Uani 1 1 d . . . . .
H3 H 0.414588 0.716241 0.171614 0.059 Uiso 1 1 calc R . . . .
N4 N 0.3563(3) 0.70639(17) 0.23899(10) 0.0454(7) Uani 1 1 d . . . . .
H4 H 0.414304 0.722894 0.259849 0.054 Uiso 1 1 calc R . . . .
N5 N 0.2913(2) 0.62125(15) 0.33975(9) 0.0356(6) Uani 1 1 d . . . . .
H5A H 0.269241 0.575159 0.326976 0.043 Uiso 1 1 calc R . . . .
H5B H 0.368444 0.625981 0.338588 0.043 Uiso 1 1 calc R . . . .
N6 N 0.3332(2) 0.48803(16) 0.40511(10) 0.0363(6) Uani 1 1 d . . . . .
N14 N 0.0688(2) 0.36278(16) 0.36802(10) 0.0398(7) Uani 1 1 d . . . . .
H14A H 0.048551 0.360896 0.399485 0.048 Uiso 1 1 calc R . . . .
H14B H 0.024901 0.399131 0.351185 0.048 Uiso 1 1 calc R . . . .
N13 N 0.1745(2) 0.24574(16) 0.28184(9) 0.0356(6) Uani 1 1 d . . . . .
H13 H 0.224228 0.224638 0.304629 0.043 Uiso 1 1 calc R . . . .
N12 N 0.1837(2) 0.24737(16) 0.23211(10) 0.0356(6) Uani 1 1 d . . . . .
H12 H 0.240270 0.227180 0.217816 0.043 Uiso 1 1 calc R . . . .
N11 N 0.1495(2) 0.34742(15) 0.12761(9) 0.0336(6) Uani 1 1 d . . . . .
H11A H 0.224457 0.340649 0.140173 0.040 Uiso 1 1 calc R . . . .
H11B H 0.128506 0.395307 0.135048 0.040 Uiso 1 1 calc R . . . .
N7 N 0.5464(2) 0.45171(17) 0.36141(9) 0.0361(6) Uani 1 1 d . . . . .
H7A H 0.501702 0.490177 0.347649 0.043 Uiso 1 1 calc R . . . .
H7B H 0.514332 0.407445 0.349496 0.043 Uiso 1 1 calc R . . . .
C15 C 0.6456(3) 0.4490(2) 0.20500(12) 0.0346(7) Uani 1 1 d . . . . .
C16 C 0.6404(3) 0.4216(2) 0.15134(12) 0.0373(8) Uani 1 1 d . . . . .
H16A H 0.689963 0.376212 0.150120 0.045 Uiso 1 1 calc R . . . .
H16B H 0.670819 0.461598 0.130748 0.045 Uiso 1 1 calc R . . . .
C17 C 0.5097(3) 0.3894(2) 0.07346(11) 0.0383(8) Uani 1 1 d . . . . .
H17A H 0.561444 0.347132 0.066713 0.046 Uiso 1 1 calc R . . . .
H17B H 0.537366 0.435624 0.057717 0.046 Uiso 1 1 calc R . . . .
C18 C 0.3867(3) 0.3713(2) 0.04942(12) 0.0379(8) Uani 1 1 d . . . . .
H18A H 0.387989 0.364631 0.013077 0.045 Uiso 1 1 calc R . . . .
H18B H 0.361986 0.322663 0.063041 0.045 Uiso 1 1 calc R . . . .
C1 C 0.3214(3) 0.5014(2) 0.02821(12) 0.0419(8) Uani 1 1 d . . . . .
H1A H 0.298575 0.491016 -0.007623 0.050 Uiso 1 1 calc R . . . .
H1B H 0.405178 0.512297 0.032697 0.050 Uiso 1 1 calc R . . . .
C2 C 0.2560(3) 0.5722(2) 0.04327(12) 0.0442(9) Uani 1 1 d . . . . .
H2C H 0.275894 0.616110 0.023062 0.053 Uiso 1 1 calc R . . . .
H2D H 0.171838 0.563407 0.036266 0.053 Uiso 1 1 calc R . . . .
C3 C 0.2271(4) 0.6617(2) 0.11433(13) 0.0473(9) Uani 1 1 d . . . . .
H3A H 0.142570 0.656762 0.105753 0.057 Uiso 1 1 calc R . . . .
H3B H 0.253320 0.705926 0.096113 0.057 Uiso 1 1 calc R . . . .
C4 C 0.2547(3) 0.67450(19) 0.17034(12) 0.0386(8) Uani 1 1 d . . . . .
C6 C 0.2530(3) 0.68106(19) 0.25365(13) 0.0380(8) Uani 1 1 d . . . . .
C7 C 0.2285(3) 0.68289(19) 0.30780(12) 0.0397(8) Uani 1 1 d . . . . .
H7C H 0.251606 0.732970 0.322228 0.048 Uiso 1 1 calc R . . . .
H7D H 0.144442 0.677167 0.308858 0.048 Uiso 1 1 calc R . . . .
C8 C 0.2667(3) 0.6252(2) 0.39368(12) 0.0419(8) Uani 1 1 d . . . . .
H8A H 0.183610 0.615523 0.395313 0.050 Uiso 1 1 calc R . . . .
H8B H 0.284469 0.676813 0.406825 0.050 Uiso 1 1 calc R . . . .
C9 C 0.3393(3) 0.5664(2) 0.42669(12) 0.0415(8) Uani 1 1 d . . . . .
H9A H 0.420799 0.583177 0.431237 0.050 Uiso 1 1 calc R . . . .
H9B H 0.311660 0.565052 0.459992 0.050 Uiso 1 1 calc R . . . .
C27 C 0.2158(3) 0.4537(2) 0.40705(13) 0.0404(8) Uani 1 1 d . . . . .
H27A H 0.155965 0.492801 0.398280 0.049 Uiso 1 1 calc R . . . .
H27B H 0.208962 0.436280 0.441440 0.049 Uiso 1 1 calc R . . . .
C26 C 0.1949(3) 0.3864(2) 0.37090(12) 0.0396(8) Uani 1 1 d . . . . .
H26A H 0.213652 0.401202 0.337396 0.048 Uiso 1 1 calc R . . . .
H26B H 0.245298 0.343403 0.382864 0.048 Uiso 1 1 calc R . . . .
C25 C 0.0402(3) 0.2868(2) 0.34288(13) 0.0427(9) Uani 1 1 d . . . . .
H25A H 0.079705 0.246027 0.363541 0.051 Uiso 1 1 calc R . . . .
H25B H -0.043967 0.277867 0.341191 0.051 Uiso 1 1 calc R . . . .
C24 C 0.0755(3) 0.28213(19) 0.29078(12) 0.0346(8) Uani 1 1 d . . . . .
C22 C 0.0921(3) 0.28502(18) 0.20790(12) 0.0333(7) Uani 1 1 d . . . . .
C21 C 0.0735(3) 0.2902(2) 0.15115(12) 0.0396(8) Uani 1 1 d . . . . .
H21A H -0.008279 0.303404 0.140882 0.048 Uiso 1 1 calc R . . . .
H21B H 0.087087 0.239392 0.137329 0.048 Uiso 1 1 calc R . . . .
C20 C 0.1362(3) 0.3367(2) 0.07088(11) 0.0374(8) Uani 1 1 d . . . . .
H20A H 0.053628 0.327849 0.059212 0.045 Uiso 1 1 calc R . . . .
H20B H 0.179134 0.290594 0.063110 0.045 Uiso 1 1 calc R . . . .
C19 C 0.1790(3) 0.4037(2) 0.04147(12) 0.0388(8) Uani 1 1 d . . . . .
H19A H 0.174716 0.388743 0.005957 0.047 Uiso 1 1 calc R . . . .
H19B H 0.124979 0.446622 0.043508 0.047 Uiso 1 1 calc R . . . .
C23 C 0.0211(3) 0.3079(2) 0.24407(12) 0.0378(8) Uani 1 1 d . . . . .
H23 H -0.049246 0.335243 0.238273 0.045 Uiso 1 1 calc R . . . .
C10 C 0.4245(3) 0.4371(2) 0.43159(12) 0.0413(8) Uani 1 1 d . . . . .
H10C H 0.404406 0.383673 0.423387 0.050 Uiso 1 1 calc R . . . .
H10D H 0.425074 0.443545 0.468050 0.050 Uiso 1 1 calc R . . . .
C11 C 0.5458(3) 0.4536(2) 0.41747(12) 0.0420(8) Uani 1 1 d . . . . .
H11C H 0.571496 0.504120 0.430321 0.050 Uiso 1 1 calc R . . . .
H11D H 0.600638 0.415331 0.433122 0.050 Uiso 1 1 calc R . . . .
C12 C 0.6661(3) 0.4588(2) 0.34502(12) 0.0408(8) Uani 1 1 d . . . . .
H12A H 0.712576 0.413631 0.356024 0.049 Uiso 1 1 calc R . . . .
H12B H 0.705281 0.504075 0.360735 0.049 Uiso 1 1 calc R . . . .
C13 C 0.6576(3) 0.46593(19) 0.28842(12) 0.0327(7) Uani 1 1 d . . . . .
C14 C 0.6601(3) 0.4102(2) 0.25089(12) 0.0354(8) Uani 1 1 d . . . . .
H14 H 0.669600 0.357147 0.255684 0.043 Uiso 1 1 calc R . . . .
C5 C 0.1863(3) 0.65976(19) 0.20937(13) 0.0400(8) Uani 1 1 d . . . . .
H5 H 0.110428 0.639491 0.206120 0.048 Uiso 1 1 calc R . . . .
S2A S 0.1062(7) 0.8215(4) 0.0233(3) 0.0542(14) Uani 0.483(11) 1 d D . P A 1
O25 O 0.0316(8) 0.7517(7) 0.0239(5) 0.144(5) Uani 0.483(11) 1 d D . P A 1
O20 O 0.0599(19) 0.8761(14) -0.0091(7) 0.320(16) Uani 0.483(11) 1 d D . P A 1
O24 O 0.1230(10) 0.8411(6) 0.0748(3) 0.104(4) Uani 0.483(11) 1 d D . P A 1
O21 O 0.2092(8) 0.7889(6) 0.0090(3) 0.090(4) Uani 0.483(11) 1 d D . P A 1
S1 S 0.33260(7) 0.45404(5) 0.22568(3) 0.0337(2) Uani 1 1 d . . . . .
O12 O 0.3703(2) 0.48974(14) 0.27364(8) 0.0448(6) Uani 1 1 d . . . . .
O11 O 0.3588(2) 0.49841(15) 0.18237(9) 0.0517(7) Uani 1 1 d . . . . .
O14 O 0.3702(2) 0.37481(14) 0.22095(9) 0.0520(7) Uani 1 1 d . . . . .
O13 O 0.1958(2) 0.44674(18) 0.22175(10) 0.0600(8) Uani 1 1 d . . . . .
H13A H 0.170395 0.477049 0.241672 0.090 Uiso 1 1 calc GR . . . .
S3 S 0.41898(7) 0.19731(5) 0.16060(3) 0.0363(2) Uani 1 1 d . . . . .
O33 O 0.3828(2) 0.18440(13) 0.21248(8) 0.0421(6) Uani 1 1 d . . . . .
O34 O 0.5207(2) 0.25052(14) 0.16533(9) 0.0468(6) Uani 1 1 d . . . . .
O32 O 0.4552(2) 0.12250(14) 0.14216(9) 0.0478(6) Uani 1 1 d . . . . .
O31 O 0.3203(2) 0.22927(15) 0.12826(9) 0.0520(7) Uani 1 1 d . . . . .
S4 S 0.38437(8) 0.14992(5) 0.39094(3) 0.0399(2) Uani 1 1 d . . . . .
O41 O 0.3383(2) 0.15683(14) 0.33632(8) 0.0446(6) Uani 1 1 d . . . . .
O43 O 0.2838(2) 0.1397(2) 0.41992(9) 0.0702(9) Uani 1 1 d D . . . .
O42 O 0.4598(3) 0.08275(18) 0.39683(11) 0.0748(9) Uani 1 1 d . . . . .
O44 O 0.4472(3) 0.21866(19) 0.40851(11) 0.0836(10) Uani 1 1 d . . . . .
S5 S 0.02434(8) 0.03923(5) 0.20242(3) 0.0427(2) Uani 1 1 d . . . . .
O51 O 0.0367(3) 0.10078(16) 0.16732(10) 0.0647(8) Uani 1 1 d D . . . .
O52 O 0.0760(2) -0.03277(16) 0.18916(11) 0.0599(7) Uani 1 1 d . . . . .
O53 O -0.0984(2) 0.02773(15) 0.21055(9) 0.0506(6) Uani 1 1 d . . . . .
O54 O 0.0909(3) 0.06831(17) 0.25272(10) 0.0628(8) Uani 1 1 d . . . . .
H54 H 0.080654 0.038061 0.275680 0.094 Uiso 1 1 calc GR . . . .
S6 S 0.05753(8) 0.00882(6) 0.37845(3) 0.0443(2) Uani 1 1 d . . . . .
O62 O -0.0684(2) 0.00399(16) 0.37649(11) 0.0602(7) Uani 1 1 d . . . . .
O61 O 0.0989(3) -0.01975(18) 0.33195(10) 0.0673(8) Uani 1 1 d . . . . .
O63 O 0.0832(3) 0.09507(16) 0.38279(13) 0.0721(9) Uani 1 1 d . . . . .
H63 H 0.151048 0.101681 0.395967 0.108 Uiso 1 1 calc GR . . . .
O64 O 0.1177(3) -0.03028(17) 0.42194(11) 0.0748(9) Uani 1 1 d . . . . .
O1 O 0.4469(3) 0.32237(15) 0.31920(10) 0.0589(7) Uani 1 1 d . . . . .
H1C H 0.431409 0.292160 0.342350 0.088 Uiso 1 1 d R . . . .
H1D H 0.432329 0.317361 0.287459 0.088 Uiso 1 1 d R . . . .
O2 O 0.1962(5) 0.2738(2) 0.4661(2) 0.1309(17) Uani 1 1 d . . . . .
H2E H 0.224468 0.229883 0.461005 0.196 Uiso 1 1 d DG . . . .
H2F H 0.128455 0.268551 0.475453 0.196 Uiso 1 1 d G . . . .
O3 O 0.1005(9) 0.0539(6) 0.0621(3) 0.293(5) Uani 1 1 d D . . . .
H3C H 0.043630 0.064030 0.038680 0.440 Uiso 1 1 d DR . . . .
H3D H 0.088550 0.084340 0.086519 0.440 Uiso 1 1 d DR . . . .
O4 O 0.3035(6) 0.1304(5) 0.0356(2) 0.213(4) Uani 1 1 d . . . . .
H4A H 0.227694 0.124357 0.020867 0.319 Uiso 1 1 d DG . . . .
H4B H 0.328522 0.148702 0.064088 0.319 Uiso 1 1 d G . . . .
O5 O 0.5589(5) 0.2281(3) 0.00140(16) 0.1275(16) Uani 1 1 d . . . . .
H5C H 0.513667 0.244502 -0.024151 0.191 Uiso 1 1 d G . . . .
H5D H 0.626525 0.248711 0.001641 0.191 Uiso 1 1 d G . . . .
O6 O 0.8050(3) 0.31459(18) 0.08444(11) 0.0673(8) Uani 1 1 d . . . . .
H6A H 0.826821 0.363591 0.081085 0.101 Uiso 1 1 d G . . . .
H6B H 0.810043 0.283847 0.059791 0.101 Uiso 1 1 d G . . . .
S2B S 0.1215(8) 0.8362(6) 0.0255(4) 0.105(3) Uani 0.517(11) 1 d D U P A 2
O26 O 0.0114(12) 0.8306(12) 0.0412(5) 0.239(9) Uani 0.517(11) 1 d D U P A 2
O23 O 0.2060(14) 0.8336(8) 0.0636(8) 0.322(17) Uani 0.517(11) 1 d D . P A 2
O27 O 0.1258(14) 0.9043(9) -0.0004(6) 0.276(13) Uani 0.517(11) 1 d D U P A 2
O22 O 0.131(2) 0.7796(11) -0.0082(7) 0.39(2) Uani 0.517(11) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N8 H8 0.8600 . ?
N8 N9 1.332(3) . ?
N8 C13 1.324(4) . ?
N9 H9 0.8600 . ?
N9 C15 1.341(4) . ?
N10 H10A 0.8900 . ?
N10 H10B 0.8900 . ?
N10 C16 1.494(4) . ?
N10 C17 1.494(4) . ?
N1 C18 1.480(4) . ?
N1 C1 1.478(4) . ?
N1 C19 1.471(4) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.489(4) . ?
N2 C3 1.493(4) . ?
N3 H3 0.8600 . ?
N3 N4 1.338(4) . ?
N3 C4 1.318(4) . ?
N4 H4 0.8600 . ?
N4 C6 1.358(4) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 C7 1.491(4) . ?
N5 C8 1.488(4) . ?
N6 C9 1.469(4) . ?
N6 C27 1.474(4) . ?
N6 C10 1.477(4) . ?
N14 H14A 0.8900 . ?
N14 H14B 0.8900 . ?
N14 C26 1.492(4) . ?
N14 C25 1.491(4) . ?
N13 H13 0.8600 . ?
N13 N12 1.332(3) . ?
N13 C24 1.340(4) . ?
N12 H12 0.8600 . ?
N12 C22 1.332(4) . ?
N11 H11A 0.8900 . ?
N11 H11B 0.8900 . ?
N11 C21 1.499(4) . ?
N11 C20 1.502(4) . ?
N7 H7A 0.8900 . ?
N7 H7B 0.8900 . ?
N7 C11 1.484(4) . ?
N7 C12 1.488(4) . ?
C15 C16 1.491(4) . ?
C15 C14 1.380(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.507(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.512(5) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.495(5) . ?
C4 C5 1.389(5) . ?
C6 C7 1.491(5) . ?
C6 C5 1.371(5) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.521(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C26 1.507(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C24 1.483(4) . ?
C24 C23 1.390(5) . ?
C22 C21 1.494(4) . ?
C22 C23 1.383(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C19 1.509(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C23 H23 0.9300 . ?
C10 H10C 0.9700 . ?
C10 H10D 0.9700 . ?
C10 C11 1.505(5) . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.494(4) . ?
C13 C14 1.386(4) . ?
C14 H14 0.9300 . ?
C5 H5 0.9300 . ?
S2A O25 1.478(11) . ?
S2A O20 1.342(11) . ?
S2A O24 1.393(10) . ?
S2A O21 1.397(9) . ?
S1 O12 1.431(2) . ?
S1 O11 1.439(2) . ?
S1 O14 1.445(3) . ?
S1 O13 1.560(3) . ?
O13 H13A 0.8200 . ?
S3 O33 1.495(2) . ?
S3 O34 1.476(3) . ?
S3 O32 1.459(2) . ?
S3 O31 1.444(2) . ?
S4 O41 1.484(2) . ?
S4 O43 1.465(3) . ?
S4 O42 1.444(3) . ?
S4 O44 1.437(3) . ?
S5 O51 1.430(3) . ?
S5 O52 1.438(3) . ?
S5 O53 1.458(2) . ?
S5 O54 1.538(3) . ?
O54 H54 0.8200 . ?
S6 O62 1.436(3) . ?
S6 O61 1.455(3) . ?
S6 O63 1.521(3) . ?
S6 O64 1.438(3) . ?
O63 H63 0.8200 . ?
O1 H1C 0.839(2) . ?
O1 H1D 0.841(3) . ?
O2 H2E 0.8427 . ?
O2 H2F 0.8443 . ?
O3 H3C 0.861(9) . ?
O3 H3D 0.857(11) . ?
O4 H4A 0.9132 . ?
O4 H4B 0.8368 . ?
O5 H5C 0.8500 . ?
O5 H5D 0.8510 . ?
O6 H6A 0.8901 . ?
O6 H6B 0.8482 . ?
S2B O26 1.374(11) . ?
S2B O23 1.311(12) . ?
S2B O27 1.366(11) . ?
S2B O22 1.338(12) . ?

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
N9 N8 H8 125.2 . . ?
C13 N8 H8 125.2 . . ?
C13 N8 N9 109.7(3) . . ?
N8 N9 H9 125.5 . . ?
N8 N9 C15 109.0(3) . . ?
C15 N9 H9 125.5 . . ?
H10A N10 H10B 108.0 . . ?
C16 N10 H10A 109.4 . . ?
C16 N10 H10B 109.4 . . ?
C17 N10 H10A 109.4 . . ?
C17 N10 H10B 109.4 . . ?
C17 N10 C16 111.0(2) . . ?
C1 N1 C18 109.4(2) . . ?
C19 N1 C18 110.6(3) . . ?
C19 N1 C1 108.9(3) . . ?
H2A N2 H2B 107.8 . . ?
C2 N2 H2A 109.0 . . ?
C2 N2 H2B 109.0 . . ?
C2 N2 C3 112.9(3) . . ?
C3 N2 H2A 109.0 . . ?
C3 N2 H2B 109.0 . . ?
N4 N3 H3 127.3 . . ?
C4 N3 H3 127.3 . . ?
C4 N3 N4 105.3(3) . . ?
N3 N4 H4 123.7 . . ?
N3 N4 C6 112.6(3) . . ?
C6 N4 H4 123.7 . . ?
H5A N5 H5B 107.9 . . ?
C7 N5 H5A 109.2 . . ?
C7 N5 H5B 109.2 . . ?
C8 N5 H5A 109.2 . . ?
C8 N5 H5B 109.2 . . ?
C8 N5 C7 112.2(3) . . ?
C9 N6 C27 111.1(3) . . ?
C9 N6 C10 111.5(3) . . ?
C27 N6 C10 109.9(3) . . ?
H14A N14 H14B 107.5 . . ?
C26 N14 H14A 108.5 . . ?
C26 N14 H14B 108.5 . . ?
C25 N14 H14A 108.5 . . ?
C25 N14 H14B 108.5 . . ?
C25 N14 C26 115.1(3) . . ?
N12 N13 H13 125.3 . . ?
N12 N13 C24 109.3(3) . . ?
C24 N13 H13 125.3 . . ?
N13 N12 H12 125.2 . . ?
C22 N12 N13 109.6(3) . . ?
C22 N12 H12 125.2 . . ?
H11A N11 H11B 108.2 . . ?
C21 N11 H11A 109.7 . . ?
C21 N11 H11B 109.7 . . ?
C21 N11 C20 109.7(2) . . ?
C20 N11 H11A 109.7 . . ?
C20 N11 H11B 109.7 . . ?
H7A N7 H7B 107.7 . . ?
C11 N7 H7A 108.8 . . ?
C11 N7 H7B 108.8 . . ?
C11 N7 C12 113.7(2) . . ?
C12 N7 H7A 108.8 . . ?
C12 N7 H7B 108.8 . . ?
N9 C15 C16 120.5(3) . . ?
N9 C15 C14 107.4(3) . . ?
C14 C15 C16 132.0(3) . . ?
N10 C16 H16A 109.3 . . ?
N10 C16 H16B 109.3 . . ?
C15 C16 N10 111.7(2) . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?
N10 C17 H17A 108.9 . . ?
N10 C17 H17B 108.9 . . ?
N10 C17 C18 113.2(3) . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
N1 C18 C17 113.9(3) . . ?
N1 C18 H18A 108.8 . . ?
N1 C18 H18B 108.8 . . ?
C17 C18 H18A 108.8 . . ?
C17 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
N1 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
N1 C1 C2 113.6(3) . . ?
H1A C1 H1B 107.7 . . ?
C2 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
N2 C2 C1 111.2(3) . . ?
N2 C2 H2C 109.4 . . ?
N2 C2 H2D 109.4 . . ?
C1 C2 H2C 109.4 . . ?
C1 C2 H2D 109.4 . . ?
H2C C2 H2D 108.0 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
N2 C3 C4 110.7(3) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
N3 C4 C3 119.6(3) . . ?
N3 C4 C5 110.8(3) . . ?
C5 C4 C3 129.6(3) . . ?
N4 C6 C7 122.3(3) . . ?
N4 C6 C5 105.0(3) . . ?
C5 C6 C7 132.7(3) . . ?
N5 C7 C6 113.4(3) . . ?
N5 C7 H7C 108.9 . . ?
N5 C7 H7D 108.9 . . ?
C6 C7 H7C 108.9 . . ?
C6 C7 H7D 108.9 . . ?
H7C C7 H7D 107.7 . . ?
N5 C8 H8A 109.3 . . ?
N5 C8 H8B 109.3 . . ?
N5 C8 C9 111.6(3) . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
N6 C9 C8 113.3(3) . . ?
N6 C9 H9A 108.9 . . ?
N6 C9 H9B 108.9 . . ?
C8 C9 H9A 108.9 . . ?
C8 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
N6 C27 H27A 109.3 . . ?
N6 C27 H27B 109.3 . . ?
N6 C27 C26 111.5(3) . . ?
H27A C27 H27B 108.0 . . ?
C26 C27 H27A 109.3 . . ?
C26 C27 H27B 109.3 . . ?
N14 C26 C27 108.9(3) . . ?
N14 C26 H26A 109.9 . . ?
N14 C26 H26B 109.9 . . ?
C27 C26 H26A 109.9 . . ?
C27 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
N14 C25 H25A 109.0 . . ?
N14 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C24 C25 N14 113.1(3) . . ?
C24 C25 H25A 109.0 . . ?
C24 C25 H25B 109.0 . . ?
N13 C24 C25 121.1(3) . . ?
N13 C24 C23 107.0(3) . . ?
C23 C24 C25 131.8(3) . . ?
N12 C22 C21 121.6(3) . . ?
N12 C22 C23 107.4(3) . . ?
C23 C22 C21 130.7(3) . . ?
N11 C21 H21A 108.3 . . ?
N11 C21 H21B 108.3 . . ?
C22 C21 N11 115.8(3) . . ?
C22 C21 H21A 108.3 . . ?
C22 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
N11 C20 H20A 108.6 . . ?
N11 C20 H20B 108.6 . . ?
N11 C20 C19 114.8(3) . . ?
H20A C20 H20B 107.6 . . ?
C19 C20 H20A 108.6 . . ?
C19 C20 H20B 108.6 . . ?
N1 C19 C20 116.5(3) . . ?
N1 C19 H19A 108.2 . . ?
N1 C19 H19B 108.2 . . ?
C20 C19 H19A 108.2 . . ?
C20 C19 H19B 108.2 . . ?
H19A C19 H19B 107.3 . . ?
C24 C23 H23 126.7 . . ?
C22 C23 C24 106.6(3) . . ?
C22 C23 H23 126.7 . . ?
N6 C10 H10C 109.0 . . ?
N6 C10 H10D 109.0 . . ?
N6 C10 C11 113.0(3) . . ?
H10C C10 H10D 107.8 . . ?
C11 C10 H10C 109.0 . . ?
C11 C10 H10D 109.0 . . ?
N7 C11 C10 110.8(3) . . ?
N7 C11 H11C 109.5 . . ?
N7 C11 H11D 109.5 . . ?
C10 C11 H11C 109.5 . . ?
C10 C11 H11D 109.5 . . ?
H11C C11 H11D 108.1 . . ?
N7 C12 H12A 109.6 . . ?
N7 C12 H12B 109.6 . . ?
N7 C12 C13 110.2(3) . . ?
H12A C12 H12B 108.1 . . ?
C13 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
N8 C13 C12 121.4(3) . . ?
N8 C13 C14 107.6(3) . . ?
C14 C13 C12 131.0(3) . . ?
C15 C14 C13 106.4(3) . . ?
C15 C14 H14 126.8 . . ?
C13 C14 H14 126.8 . . ?
C4 C5 H5 126.9 . . ?
C6 C5 C4 106.3(3) . . ?
C6 C5 H5 126.9 . . ?
O20 S2A O25 113.3(14) . . ?
O20 S2A O24 116.9(10) . . ?
O20 S2A O21 113.1(9) . . ?
O24 S2A O25 101.7(7) . . ?
O24 S2A O21 109.8(7) . . ?
O21 S2A O25 100.4(6) . . ?
O12 S1 O11 114.02(16) . . ?
O12 S1 O14 115.07(15) . . ?
O12 S1 O13 106.82(14) . . ?
O11 S1 O14 110.15(15) . . ?
O11 S1 O13 106.88(16) . . ?
O14 S1 O13 102.90(16) . . ?
S1 O13 H13A 109.5 . . ?
O34 S3 O33 108.34(14) . . ?
O32 S3 O33 107.12(14) . . ?
O32 S3 O34 109.19(14) . . ?
O31 S3 O33 108.67(14) . . ?
O31 S3 O34 111.41(15) . . ?
O31 S3 O32 111.95(15) . . ?
O43 S4 O41 107.92(15) . . ?
O42 S4 O41 108.03(16) . . ?
O42 S4 O43 110.04(19) . . ?
O44 S4 O41 110.83(17) . . ?
O44 S4 O43 108.88(19) . . ?
O44 S4 O42 111.1(2) . . ?
O51 S5 O52 114.24(17) . . ?
O51 S5 O53 111.55(16) . . ?
O51 S5 O54 104.00(17) . . ?
O52 S5 O53 110.37(16) . . ?
O52 S5 O54 108.53(17) . . ?
O53 S5 O54 107.72(16) . . ?
S5 O54 H54 109.5 . . ?
O62 S6 O61 111.91(17) . . ?
O62 S6 O63 104.10(17) . . ?
O62 S6 O64 112.66(19) . . ?
O61 S6 O63 108.51(19) . . ?
O64 S6 O61 110.14(18) . . ?
O64 S6 O63 109.26(18) . . ?
S6 O63 H63 109.5 . . ?
H1C O1 H1D 129.1(3) . . ?
H2E O2 H2F 109.4 . . ?
H3C O3 H3D 104.2(9) . . ?
H4A O4 H4B 129.4 . . ?
H5C O5 H5D 109.5 . . ?
H6A O6 H6B 118.3 . . ?
O23 S2B O26 112.6(10) . . ?
O23 S2B O27 110.4(10) . . ?
O23 S2B O22 112.0(11) . . ?
O27 S2B O26 107.5(9) . . ?
O22 S2B O26 107.5(10) . . ?
O22 S2B O27 106.5(10) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N8 H8 O33 0.86 1.87 2.687(3) 157.5 2_655 yes
N9 H9 O41 0.86 1.89 2.696(4) 155.1 2_655 yes
N10 H10A O34 0.89 1.97 2.779(4) 150.6 . yes
N2 H2B O11 0.89 2.13 2.779(3) 129.3 . yes
N4 H4 O34 0.86 2.09 2.851(4) 147.9 2_655 yes
N14 H14A O24 0.89 2.18 2.831(9) 129.8 2_545 yes
N14 H14A O26 0.89 1.86 2.726(10) 164.0 2_545 yes
N14 H14B O52 0.89 1.89 2.775(4) 173.6 2 yes
N13 H13 O41 0.86 1.88 2.704(4) 161.1 . yes
N12 H12 O33 0.86 1.81 2.629(4) 158.4 . yes
N11 H11A O31 0.89 2.25 2.824(4) 121.5 . yes
N11 H11B O62 0.89 2.01 2.858(4) 158.6 2 yes
N7 H7B O1 0.89 1.80 2.691(4) 174.3 . yes
O13 H13A O53 0.82 1.81 2.621(3) 168.8 2 yes
O54 H54 O61 0.82 1.78 2.583(4) 164.1 . yes
O63 H63 O43 0.82 1.71 2.508(4) 165.3 . yes
O1 H1D O14 0.841(3) 2.072(2) 2.795(4) 143.74(19) . yes
O2 H2E O43 0.84 2.06 2.855(6) 157.4 . yes
O2 H2F O25 0.84 1.85 2.675(12) 163.5 2_545 yes
O2 H2F O26 0.84 1.93 2.554(16) 129.5 2_545 yes
O3 H3C O20 0.861(9) 1.693(11) 2.486(14) 152.1(12) 3_565 yes
O5 H5C O44 0.85 1.96 2.789(5) 165.1 4_565 yes
O5 H5D O21 0.85 2.04 2.713(10) 135.8 3_665 yes
O6 H6A O64 0.89 1.95 2.834(4) 176.0 2_655 yes
O6 H6B O22 0.85 1.93 2.754(13) 163.6 3_665 yes

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_crystal4__phos6
_database_code_depnum_ccdc_archive 'CCDC 1912381'
loop_
_audit_author_name
_audit_author_address
'Javier Pitarch-Jarque'
;Universitat de Valencia
Spain
;
_audit_update_record             
;
2019-04-26 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_audit_creation_date             2019-03-11
_audit_creation_method           
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H54 N14, 6(H2 O4 P), 8(H2 O)'
_chemical_formula_sum            'C27 H82 N14 O32 P6'
_chemical_formula_weight         1300.88
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   50.9218(10)
_cell_length_b                   11.2705(4)
_cell_length_c                   18.5910(5)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     10669.6(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8432
_cell_measurement_temperature    120.05(10)
_cell_measurement_theta_max      28.5650
_cell_measurement_theta_min      2.9200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5504
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -69
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40015
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.112
_diffrn_reflns_theta_min         2.910
_diffrn_ambient_temperature      120.05(10)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9956
_reflns_number_total             12642
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         12642
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1644
_refine_ls_R_factor_gt           0.1396
_refine_ls_restrained_S_all      1.197
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0101P)²+148.2749P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2466
_refine_ls_wR_factor_ref         0.2588
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O14-H3F
 2.2 with sigma of 0.02
3.a Free rotating group:
 O2(H2G,H2H), O6(H6C,H6D), O5(H5E,H5F), O3(H3E,H3F), O7(H7E,H7F), O4(H4C,H4D),
 O1(H1E,H1F), O8(H8C,H8D)
3.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N5(H5A,H5B), N7(H7A,H7B), N10(H10A,H10B), N11(H11A,H11B),
 N14(H14A,H14B), C1(H1A,H1B), C2(H2C,H2D), C3(H3A,H3B), C7(H7C,H7D), C8(H8A,
 H8B), C9(H9A,H9B), C10(H10C,H10D), C11(H11C,H11D), C12(H12A,H12B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N9(H9), N12(H12), C5(H5), C14(H14), C23(H23)
3.d Idealised tetrahedral OH refined as rotating group:
 O12(H1C), O13(H1D), O41(H4A), O44(H4B), O52(H5C), O54(H5D), O22(H2E),
 O24(H2F), O31(H3C), O34(H3D), O62(H6A), O64(H6B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.70974(10) 0.5335(5) 0.7467(3) 0.0202(12) Uani 1 1 d . . . . .
N2 N 0.68916(11) 0.4039(7) 0.6193(3) 0.0268(15) Uani 1 1 d . . . . .
H2A H 0.679890 0.469832 0.631659 0.032 Uiso 1 1 calc R . . . .
H2B H 0.684317 0.344493 0.649646 0.032 Uiso 1 1 calc R . . . .
N3 N 0.64318(12) 0.2437(6) 0.5772(3) 0.0304(15) Uani 1 1 d . . . . .
H3 H 0.652509 0.196490 0.604895 0.036 Uiso 1 1 calc R . . . .
N4 N 0.61689(12) 0.2322(6) 0.5677(4) 0.0316(15) Uani 1 1 d . . . . .
N5 N 0.57028(11) 0.4334(5) 0.5372(3) 0.0204(12) Uani 1 1 d . . . . .
H5A H 0.570791 0.417026 0.585107 0.025 Uiso 1 1 calc R . . . .
H5B H 0.579318 0.501918 0.529712 0.025 Uiso 1 1 calc R . . . .
N6 N 0.53295(11) 0.5702(5) 0.6263(3) 0.0183(12) Uani 1 1 d . . . . .
N7 N 0.54869(10) 0.4557(5) 0.7640(3) 0.0199(12) Uani 1 1 d . . . . .
H7A H 0.558400 0.413641 0.731720 0.024 Uiso 1 1 calc R . . . .
H7B H 0.555328 0.530531 0.766182 0.024 Uiso 1 1 calc R . . . .
N8 N 0.58276(11) 0.4800(5) 0.9209(3) 0.0202(12) Uani 1 1 d . . . . .
N9 N 0.60867(11) 0.4680(5) 0.9340(3) 0.0213(12) Uani 1 1 d . . . . .
H9 H 0.617077 0.506280 0.968247 0.026 Uiso 1 1 calc R . . . .
N10 N 0.66502(10) 0.4435(6) 0.8482(3) 0.0222(13) Uani 1 1 d . . . . .
H10A H 0.662829 0.519490 0.863615 0.027 Uiso 1 1 calc R . . . .
H10B H 0.659459 0.439418 0.801735 0.027 Uiso 1 1 calc R . . . .
N11 N 0.68255(10) 0.7644(5) 0.7085(3) 0.0223(13) Uani 1 1 d . . . . .
H11A H 0.685578 0.739360 0.662655 0.027 Uiso 1 1 calc R . . . .
H11B H 0.670283 0.715579 0.728246 0.027 Uiso 1 1 calc R . . . .
N12 N 0.64680(11) 0.9140(6) 0.5936(3) 0.0252(13) Uani 1 1 d . . . . .
H12 H 0.661059 0.923563 0.567494 0.030 Uiso 1 1 calc R . . . .
N13 N 0.62217(11) 0.9185(6) 0.5668(3) 0.0221(13) Uani 1 1 d . . . . .
N14 N 0.56512(10) 0.7896(5) 0.6357(3) 0.0178(11) Uani 1 1 d . . . . .
H14A H 0.572405 0.728814 0.610339 0.021 Uiso 1 1 calc R . . . .
H14B H 0.568222 0.776525 0.683224 0.021 Uiso 1 1 calc R . . . .
C1 C 0.72452(13) 0.4374(8) 0.7085(4) 0.0276(17) Uani 1 1 d . . . . .
H1A H 0.720625 0.360457 0.731900 0.033 Uiso 1 1 calc R . . . .
H1B H 0.743588 0.452388 0.713533 0.033 Uiso 1 1 calc R . . . .
C2 C 0.71783(13) 0.4286(8) 0.6295(4) 0.0291(17) Uani 1 1 d . . . . .
H2C H 0.722463 0.503875 0.605219 0.035 Uiso 1 1 calc R . . . .
H2D H 0.728257 0.364167 0.607263 0.035 Uiso 1 1 calc R . . . .
C3 C 0.68188(14) 0.3692(8) 0.5439(4) 0.0303(18) Uani 1 1 d . . . . .
H3A H 0.685352 0.436470 0.510953 0.036 Uiso 1 1 calc R . . . .
H3B H 0.692874 0.301419 0.528343 0.036 Uiso 1 1 calc R . . . .
C4 C 0.65362(14) 0.3356(7) 0.5395(4) 0.0258(16) Uani 1 1 d . . . . .
C5 C 0.63301(14) 0.3851(7) 0.5016(4) 0.0232(15) Uani 1 1 d . . . . .
H5 H 0.633674 0.450431 0.469351 0.028 Uiso 1 1 calc R . . . .
C6 C 0.61121(14) 0.3190(6) 0.5206(3) 0.0208(14) Uani 1 1 d . . . . .
C7 C 0.58357(13) 0.3332(6) 0.4961(3) 0.0206(14) Uani 1 1 d . . . . .
H7C H 0.573842 0.258328 0.504104 0.025 Uiso 1 1 calc R . . . .
H7D H 0.583285 0.350959 0.443995 0.025 Uiso 1 1 calc R . . . .
C8 C 0.54235(13) 0.4506(7) 0.5146(4) 0.0227(15) Uani 1 1 d . . . . .
H8A H 0.531828 0.381212 0.530020 0.027 Uiso 1 1 calc R . . . .
H8B H 0.541451 0.455636 0.461517 0.027 Uiso 1 1 calc R . . . .
C9 C 0.53069(13) 0.5638(7) 0.5475(4) 0.0229(15) Uani 1 1 d . . . . .
H9A H 0.539671 0.633406 0.526344 0.027 Uiso 1 1 calc R . . . .
H9B H 0.511891 0.568717 0.534258 0.027 Uiso 1 1 calc R . . . .
C10 C 0.51811(14) 0.4711(7) 0.6583(4) 0.0260(16) Uani 1 1 d . . . . .
H10C H 0.524224 0.396094 0.636259 0.031 Uiso 1 1 calc R . . . .
H10D H 0.499322 0.480759 0.645927 0.031 Uiso 1 1 calc R . . . .
C11 C 0.52051(12) 0.4604(7) 0.7392(4) 0.0211(14) Uani 1 1 d . . . . .
H11C H 0.511717 0.529078 0.762061 0.025 Uiso 1 1 calc R . . . .
H11D H 0.511350 0.387549 0.755246 0.025 Uiso 1 1 calc R . . . .
C12 C 0.55058(13) 0.3984(7) 0.8366(4) 0.0222(14) Uani 1 1 d . . . . .
H12A H 0.538143 0.437427 0.869961 0.027 Uiso 1 1 calc R . . . .
H12B H 0.545603 0.313771 0.832681 0.027 Uiso 1 1 calc R . . . .
C13 C 0.57788(13) 0.4079(6) 0.8660(4) 0.0203(14) Uani 1 1 d . . . . .
C14 C 0.60065(13) 0.3486(6) 0.8436(4) 0.0183(13) Uani 1 1 d . . . . .
H14 H 0.602304 0.292279 0.805821 0.022 Uiso 1 1 calc R . . . .
C15 C 0.62021(13) 0.3907(6) 0.8888(4) 0.0197(14) Uani 1 1 d . . . . .
C16 C 0.64857(13) 0.3613(6) 0.8940(4) 0.0221(15) Uani 1 1 d . . . . .
H16A H 0.651372 0.278392 0.878177 0.027 Uiso 1 1 calc R . . . .
H16B H 0.654261 0.367586 0.944777 0.027 Uiso 1 1 calc R . . . .
C17 C 0.69384(13) 0.4113(7) 0.8517(4) 0.0230(15) Uani 1 1 d . . . . .
H17A H 0.696999 0.339753 0.822069 0.028 Uiso 1 1 calc R . . . .
H17B H 0.698545 0.391920 0.902040 0.028 Uiso 1 1 calc R . . . .
C18 C 0.71129(13) 0.5111(8) 0.8253(4) 0.0269(16) Uani 1 1 d . . . . .
H18A H 0.706448 0.584756 0.851039 0.032 Uiso 1 1 calc R . . . .
H18B H 0.729714 0.492176 0.837861 0.032 Uiso 1 1 calc R . . . .
C19 C 0.72324(13) 0.6469(7) 0.7302(4) 0.0251(16) Uani 1 1 d . . . . .
H19A H 0.727103 0.649778 0.678036 0.030 Uiso 1 1 calc R . . . .
H19B H 0.740196 0.649011 0.756218 0.030 Uiso 1 1 calc R . . . .
C20 C 0.70731(12) 0.7557(7) 0.7506(4) 0.0230(15) Uani 1 1 d . . . . .
H20A H 0.703021 0.752181 0.802505 0.028 Uiso 1 1 calc R . . . .
H20B H 0.718002 0.827722 0.742218 0.028 Uiso 1 1 calc R . . . .
C21 C 0.67219(13) 0.8874(6) 0.7067(4) 0.0220(15) Uani 1 1 d . . . . .
H21A H 0.685310 0.940406 0.684117 0.026 Uiso 1 1 calc R . . . .
H21B H 0.669144 0.915389 0.756492 0.026 Uiso 1 1 calc R . . . .
C22 C 0.64696(13) 0.8932(6) 0.6652(4) 0.0209(14) Uani 1 1 d . . . . .
C23 C 0.62126(12) 0.8847(6) 0.6863(4) 0.0187(13) Uani 1 1 d . . . . .
H23 H 0.614767 0.871484 0.733550 0.022 Uiso 1 1 calc R . . . .
C24 C 0.60668(13) 0.8997(6) 0.6235(3) 0.0166(13) Uani 1 1 d . . . . .
C25 C 0.57756(12) 0.9045(6) 0.6134(4) 0.0179(13) Uani 1 1 d . . . . .
H25A H 0.573505 0.920492 0.562194 0.022 Uiso 1 1 calc R . . . .
H25B H 0.570204 0.970156 0.642467 0.022 Uiso 1 1 calc R . . . .
C26 C 0.53613(12) 0.7926(6) 0.6225(4) 0.0204(14) Uani 1 1 d . . . . .
H26A H 0.532865 0.798213 0.570068 0.024 Uiso 1 1 calc R . . . .
H26B H 0.528628 0.864268 0.645400 0.024 Uiso 1 1 calc R . . . .
C27 C 0.52240(14) 0.6837(6) 0.6518(4) 0.0237(15) Uani 1 1 d . . . . .
H27A H 0.523523 0.685276 0.704927 0.028 Uiso 1 1 calc R . . . .
H27B H 0.503587 0.687999 0.638633 0.028 Uiso 1 1 calc R . . . .
P1 P 0.62829(3) 0.53829(15) 0.68946(8) 0.0127(3) Uani 1 1 d . . . . .
O11 O 0.63800(10) 0.4210(5) 0.7051(3) 0.0271(12) Uani 1 1 d . . . . .
O12 O 0.60135(9) 0.5335(5) 0.6687(3) 0.0303(12) Uani 1 1 d . . . . .
H1C H 0.594873 0.468389 0.681729 0.046 Uiso 1 1 calc GR . . . .
O13 O 0.63116(10) 0.6089(5) 0.7531(3) 0.0252(11) Uani 1 1 d . . . . .
H1D H 0.624537 0.676163 0.746146 0.038 Uiso 1 1 calc GR . . . .
O14 O 0.64362(10) 0.5879(5) 0.6323(3) 0.0301(12) Uani 1 1 d D . . . .
P4 P 0.56209(3) 0.48174(16) 0.30594(9) 0.0176(3) Uani 1 1 d . . . . .
O41 O 0.57721(13) 0.5373(6) 0.3613(3) 0.0432(15) Uani 1 1 d . . . . .
H4A H 0.569945 0.525968 0.401271 0.065 Uiso 1 1 calc GR . . . .
O42 O 0.57972(11) 0.4237(5) 0.2562(3) 0.0367(14) Uani 1 1 d . . . . .
O43 O 0.54512(11) 0.3951(5) 0.3373(3) 0.0319(13) Uani 1 1 d . . . . .
O44 O 0.54703(12) 0.5689(5) 0.2686(3) 0.0358(14) Uani 1 1 d . . . . .
H4B H 0.545483 0.629622 0.294483 0.054 Uiso 1 1 calc GR . . . .
P5 P 0.28248(4) 0.9590(2) 0.44097(11) 0.0267(4) Uani 1 1 d . . . . .
O51 O 0.27955(12) 1.0616(7) 0.3984(4) 0.0519(19) Uani 1 1 d . . . . .
O52 O 0.30912(11) 0.9459(7) 0.4631(4) 0.0482(17) Uani 1 1 d . . . . .
H5C H 0.313616 1.005191 0.487596 0.072 Uiso 1 1 calc GR . . . .
O53 O 0.27568(16) 0.8632(8) 0.3998(4) 0.068(2) Uani 1 1 d . . . . .
O54 O 0.26600(13) 0.9686(7) 0.5021(4) 0.0528(19) Uani 1 1 d . . . . .
H5D H 0.262407 0.900448 0.517582 0.079 Uiso 1 1 calc GR . . . .
P2 P 0.35650(3) 0.26097(19) 0.58970(10) 0.0231(4) Uani 1 1 d . . . . .
O21 O 0.3458(2) 0.3226(11) 0.6451(4) 0.113(5) Uani 1 1 d . . . . .
O22 O 0.35532(11) 0.3252(5) 0.5247(3) 0.0341(13) Uani 1 1 d . . . . .
H2E H 0.356230 0.277969 0.489802 0.051 Uiso 1 1 calc GR . . . .
O23 O 0.38247(10) 0.2242(5) 0.6047(3) 0.0317(13) Uani 1 1 d . . . . .
O24 O 0.34110(15) 0.1550(8) 0.5785(6) 0.092(4) Uani 1 1 d . . . . .
H2F H 0.329476 0.168409 0.547470 0.139 Uiso 1 1 calc GR . . . .
P3 P 0.71101(3) 0.42272(18) 0.35858(10) 0.0209(4) Uani 1 1 d . . . . .
O31 O 0.72618(16) 0.3376(7) 0.3910(5) 0.072(3) Uani 1 1 d . . . . .
H3C H 0.730610 0.286509 0.360486 0.109 Uiso 1 1 calc GR . . . .
O32 O 0.71845(16) 0.5350(7) 0.3826(5) 0.075(3) Uani 1 1 d . . . . .
O33 O 0.71402(12) 0.4217(8) 0.2834(3) 0.057(2) Uani 1 1 d . . . . .
O34 O 0.68403(11) 0.3978(7) 0.3740(4) 0.0520(19) Uani 1 1 d . . . . .
H3D H 0.677037 0.457617 0.392927 0.078 Uiso 1 1 calc GR . . . .
P6 P 0.51298(4) 0.13785(19) 0.59072(13) 0.0306(5) Uani 1 1 d . . . . .
O61 O 0.50042(13) 0.0265(5) 0.5893(4) 0.0431(15) Uani 1 1 d . . . . .
O62 O 0.5180(2) 0.1713(9) 0.6613(5) 0.091(3) Uani 1 1 d . . . . .
H6A H 0.503783 0.186869 0.682160 0.137 Uiso 1 1 calc GR . . . .
O63 O 0.49765(11) 0.2249(5) 0.5540(4) 0.0408(15) Uani 1 1 d . . . . .
O64 O 0.53748(15) 0.1303(9) 0.5552(8) 0.124(5) Uani 1 1 d . . . . .
H6B H 0.543687 0.061814 0.560450 0.186 Uiso 1 1 calc GR . . . .
O2 O 0.59007(9) 0.6597(5) 0.5215(3) 0.0223(11) Uani 1 1 d . . . . .
H2G H 0.606377 0.675563 0.518316 0.033 Uiso 1 1 d G . . . .
H2H H 0.585199 0.691867 0.480316 0.033 Uiso 1 1 d G . . . .
O6 O 0.44146(10) 0.2058(5) 0.5718(3) 0.0310(12) Uani 1 1 d . . . . .
H6C H 0.435581 0.135376 0.570203 0.047 Uiso 1 1 d G . . . .
H6D H 0.458151 0.204306 0.569975 0.047 Uiso 1 1 d G . . . .
O5 O 0.67444(12) 0.2016(7) 0.7053(3) 0.0452(16) Uani 1 1 d . . . . .
H5E H 0.660405 0.201280 0.729916 0.068 Uiso 1 1 d G . . . .
H5F H 0.686965 0.174291 0.730625 0.068 Uiso 1 1 d G . . . .
O3 O 0.69077(10) 0.6814(6) 0.5687(3) 0.0326(13) Uani 1 1 d . . . . .
H3E H 0.696583 0.713590 0.530543 0.049 Uiso 1 1 d G . . . .
H3F H 0.674146 0.675553 0.565967 0.049 Uiso 1 1 d DG . . . .
O7 O 0.36426(13) 0.6132(6) 0.7015(4) 0.0499(18) Uani 1 1 d . . . . .
H7E H 0.367746 0.558117 0.671977 0.075 Uiso 1 1 d G . . . .
H7F H 0.375353 0.612243 0.735615 0.075 Uiso 1 1 d G . . . .
O4 O 0.57128(12) 0.2932(5) 0.6664(3) 0.0370(14) Uani 1 1 d . . . . .
H4C H 0.564080 0.227322 0.677127 0.056 Uiso 1 1 d G . . . .
H4D H 0.587159 0.281574 0.654262 0.056 Uiso 1 1 d G . . . .
O1 O 0.42579(9) 0.1862(5) 0.7216(3) 0.0229(11) Uani 1 1 d . . . . .
H1E H 0.431039 0.227866 0.686360 0.034 Uiso 1 1 d G . . . .
H1F H 0.409198 0.177373 0.719009 0.034 Uiso 1 1 d G . . . .
O8 O 0.72454(15) 0.7539(8) 0.4636(5) 0.068(2) Uani 1 1 d . . . . .
H8C H 0.734146 0.766412 0.500200 0.102 Uiso 1 1 d G . . . .
H8D H 0.731938 0.703096 0.436485 0.102 Uiso 1 1 d G . . . .


_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 C1 1.499(9) . ?
N1 C18 1.484(9) . ?
N1 C19 1.483(9) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 C2 1.498(8) . ?
N2 C3 1.502(9) . ?
N3 H3 0.8800 . ?
N3 N4 1.357(8) . ?
N3 C4 1.358(10) . ?
N4 C6 1.343(10) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 C7 1.521(8) . ?
N5 C8 1.495(8) . ?
N6 C9 1.470(8) . ?
N6 C10 1.474(9) . ?
N6 C27 1.466(9) . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?
N7 C11 1.508(8) . ?
N7 C12 1.499(9) . ?
N8 N9 1.348(7) . ?
N8 C13 1.328(9) . ?
N9 H9 0.8800 . ?
N9 C15 1.346(9) . ?
N10 H10A 0.9100 . ?
N10 H10B 0.9100 . ?
N10 C16 1.512(9) . ?
N10 C17 1.513(8) . ?
N11 H11A 0.9100 . ?
N11 H11B 0.9100 . ?
N11 C20 1.488(8) . ?
N11 C21 1.484(9) . ?
N12 H12 0.8800 . ?
N12 N13 1.350(8) . ?
N12 C22 1.352(9) . ?
N13 C24 1.333(8) . ?
N14 H14A 0.9100 . ?
N14 H14B 0.9100 . ?
N14 C25 1.501(9) . ?
N14 C26 1.497(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.511(10) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.491(10) . ?
C4 C5 1.382(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(10) . ?
C6 C7 1.488(9) . ?
C7 H7C 0.9900 . ?
C7 H7D 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.535(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10C 0.9900 . ?
C10 H10D 0.9900 . ?
C10 C11 1.514(9) . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.498(9) . ?
C13 C14 1.402(9) . ?
C14 H14 0.9500 . ?
C14 C15 1.387(9) . ?
C15 C16 1.485(9) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.515(10) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.519(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.500(9) . ?
C22 C23 1.370(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.394(9) . ?
C24 C25 1.496(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.514(10) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
P1 O11 1.441(6) . ?
P1 O12 1.426(5) . ?
P1 O13 1.433(5) . ?
P1 O14 1.432(5) . ?
O12 H1C 0.8400 . ?
O13 H1D 0.8400 . ?
P4 O41 1.429(6) . ?
P4 O42 1.446(6) . ?
P4 O43 1.428(5) . ?
P4 O44 1.426(6) . ?
O41 H4A 0.8400 . ?
O44 H4B 0.8400 . ?
P5 O51 1.409(7) . ?
P5 O52 1.426(6) . ?
P5 O53 1.369(9) . ?
P5 O54 1.418(6) . ?
O52 H5C 0.8400 . ?
O54 H5D 0.8400 . ?
P2 O21 1.357(8) . ?
P2 O22 1.411(6) . ?
P2 O23 1.413(5) . ?
P2 O24 1.444(9) . ?
O22 H2E 0.8400 . ?
O24 H2F 0.8400 . ?
P3 O31 1.372(7) . ?
P3 O32 1.394(8) . ?
P3 O33 1.406(6) . ?
P3 O34 1.431(6) . ?
O31 H3C 0.8400 . ?
O34 H3D 0.8400 . ?
P6 O61 1.409(6) . ?
P6 O62 1.390(9) . ?
P6 O63 1.428(6) . ?
P6 O64 1.414(8) . ?
O62 H6A 0.8400 . ?
O64 H6B 0.8400 . ?
O2 H2G 0.8516 . ?
O2 H2H 0.8831 . ?
O6 H6C 0.8487 . ?
O6 H6D 0.8507 . ?
O5 H5E 0.8482 . ?
O5 H5F 0.8502 . ?
O3 H3E 0.8498 . ?
O3 H3F 0.8504 . ?
O7 H7E 0.8477 . ?
O7 H7F 0.8489 . ?
O4 H4C 0.8516 . ?
O4 H4D 0.8499 . ?
O1 H1E 0.8498 . ?
O1 H1F 0.8520 . ?
O8 H8C 0.8494 . ?
O8 H8D 0.8509 . ?

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
C18 N1 C1 108.5(6) . . ?
C19 N1 C1 107.0(5) . . ?
C19 N1 C18 109.1(6) . . ?
H2A N2 H2B 107.6 . . ?
C2 N2 H2A 108.7 . . ?
C2 N2 H2B 108.7 . . ?
C2 N2 C3 114.0(5) . . ?
C3 N2 H2A 108.7 . . ?
C3 N2 H2B 108.7 . . ?
N4 N3 H3 123.5 . . ?
N4 N3 C4 113.1(6) . . ?
C4 N3 H3 123.5 . . ?
C6 N4 N3 103.2(6) . . ?
H5A N5 H5B 107.9 . . ?
C7 N5 H5A 109.2 . . ?
C7 N5 H5B 109.2 . . ?
C8 N5 H5A 109.2 . . ?
C8 N5 H5B 109.2 . . ?
C8 N5 C7 112.2(5) . . ?
C9 N6 C10 109.0(6) . . ?
C27 N6 C9 109.6(6) . . ?
C27 N6 C10 110.0(5) . . ?
H7A N7 H7B 108.1 . . ?
C11 N7 H7A 109.5 . . ?
C11 N7 H7B 109.5 . . ?
C12 N7 H7A 109.5 . . ?
C12 N7 H7B 109.5 . . ?
C12 N7 C11 110.6(5) . . ?
C13 N8 N9 105.1(6) . . ?
N8 N9 H9 123.8 . . ?
C15 N9 N8 112.3(6) . . ?
C15 N9 H9 123.8 . . ?
H10A N10 H10B 108.0 . . ?
C16 N10 H10A 109.3 . . ?
C16 N10 H10B 109.3 . . ?
C16 N10 C17 111.5(5) . . ?
C17 N10 H10A 109.3 . . ?
C17 N10 H10B 109.3 . . ?
H11A N11 H11B 107.9 . . ?
C20 N11 H11A 109.2 . . ?
C20 N11 H11B 109.2 . . ?
C21 N11 H11A 109.2 . . ?
C21 N11 H11B 109.2 . . ?
C21 N11 C20 112.0(6) . . ?
N13 N12 H12 124.0 . . ?
N13 N12 C22 112.0(6) . . ?
C22 N12 H12 124.0 . . ?
C24 N13 N12 104.6(5) . . ?
H14A N14 H14B 108.1 . . ?
C25 N14 H14A 109.5 . . ?
C25 N14 H14B 109.5 . . ?
C26 N14 H14A 109.5 . . ?
C26 N14 H14B 109.5 . . ?
C26 N14 C25 110.6(5) . . ?
N1 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
N1 C1 C2 113.3(6) . . ?
H1A C1 H1B 107.7 . . ?
C2 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
N2 C2 C1 110.8(6) . . ?
N2 C2 H2C 109.5 . . ?
N2 C2 H2D 109.5 . . ?
C1 C2 H2C 109.5 . . ?
C1 C2 H2D 109.5 . . ?
H2C C2 H2D 108.1 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 N2 110.8(6) . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
N3 C4 C3 123.0(7) . . ?
N3 C4 C5 105.9(6) . . ?
C5 C4 C3 131.2(8) . . ?
C4 C5 H5 127.4 . . ?
C4 C5 C6 105.1(6) . . ?
C6 C5 H5 127.4 . . ?
N4 C6 C5 112.7(6) . . ?
N4 C6 C7 118.8(7) . . ?
C5 C6 C7 128.5(7) . . ?
N5 C7 H7C 109.6 . . ?
N5 C7 H7D 109.6 . . ?
C6 C7 N5 110.3(5) . . ?
C6 C7 H7C 109.6 . . ?
C6 C7 H7D 109.6 . . ?
H7C C7 H7D 108.1 . . ?
N5 C8 H8A 109.4 . . ?
N5 C8 H8B 109.4 . . ?
N5 C8 C9 111.3(5) . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
N6 C9 C8 114.0(6) . . ?
N6 C9 H9A 108.7 . . ?
N6 C9 H9B 108.7 . . ?
C8 C9 H9A 108.7 . . ?
C8 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
N6 C10 H10C 108.5 . . ?
N6 C10 H10D 108.5 . . ?
N6 C10 C11 114.9(6) . . ?
H10C C10 H10D 107.5 . . ?
C11 C10 H10C 108.5 . . ?
C11 C10 H10D 108.5 . . ?
N7 C11 C10 112.5(5) . . ?
N7 C11 H11C 109.1 . . ?
N7 C11 H11D 109.1 . . ?
C10 C11 H11C 109.1 . . ?
C10 C11 H11D 109.1 . . ?
H11C C11 H11D 107.8 . . ?
N7 C12 H12A 109.4 . . ?
N7 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C13 C12 N7 111.0(5) . . ?
C13 C12 H12A 109.4 . . ?
C13 C12 H12B 109.4 . . ?
N8 C13 C12 119.9(6) . . ?
N8 C13 C14 111.5(6) . . ?
C14 C13 C12 128.6(6) . . ?
C13 C14 H14 127.7 . . ?
C15 C14 C13 104.5(6) . . ?
C15 C14 H14 127.7 . . ?
N9 C15 C14 106.6(6) . . ?
N9 C15 C16 121.9(6) . . ?
C14 C15 C16 131.5(6) . . ?
N10 C16 H16A 109.3 . . ?
N10 C16 H16B 109.3 . . ?
C15 C16 N10 111.4(5) . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
N10 C17 H17A 109.2 . . ?
N10 C17 H17B 109.2 . . ?
N10 C17 C18 112.1(6) . . ?
H17A C17 H17B 107.9 . . ?
C18 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
N1 C18 C17 114.5(6) . . ?
N1 C18 H18A 108.6 . . ?
N1 C18 H18B 108.6 . . ?
C17 C18 H18A 108.6 . . ?
C17 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
N1 C19 H19A 108.9 . . ?
N1 C19 H19B 108.9 . . ?
N1 C19 C20 113.3(5) . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
N11 C20 C19 112.0(6) . . ?
N11 C20 H20A 109.2 . . ?
N11 C20 H20B 109.2 . . ?
C19 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
N11 C21 H21A 109.5 . . ?
N11 C21 H21B 109.5 . . ?
N11 C21 C22 110.9(6) . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
N12 C22 C21 121.3(6) . . ?
N12 C22 C23 106.8(6) . . ?
C23 C22 C21 131.9(6) . . ?
C22 C23 H23 127.5 . . ?
C22 C23 C24 105.1(6) . . ?
C24 C23 H23 127.5 . . ?
N13 C24 C23 111.5(6) . . ?
N13 C24 C25 118.8(6) . . ?
C23 C24 C25 129.6(6) . . ?
N14 C25 H25A 109.5 . . ?
N14 C25 H25B 109.5 . . ?
C24 C25 N14 110.6(5) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
N14 C26 H26A 109.2 . . ?
N14 C26 H26B 109.2 . . ?
N14 C26 C27 112.2(6) . . ?
H26A C26 H26B 107.9 . . ?
C27 C26 H26A 109.2 . . ?
C27 C26 H26B 109.2 . . ?
N6 C27 C26 115.0(6) . . ?
N6 C27 H27A 108.5 . . ?
N6 C27 H27B 108.5 . . ?
C26 C27 H27A 108.5 . . ?
C26 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?
O12 P1 O11 110.5(3) . . ?
O12 P1 O13 110.0(3) . . ?
O12 P1 O14 109.8(3) . . ?
O13 P1 O11 107.9(3) . . ?
O14 P1 O11 108.7(3) . . ?
O14 P1 O13 109.9(3) . . ?
P1 O12 H1C 109.5 . . ?
P1 O13 H1D 109.5 . . ?
O41 P4 O42 108.9(4) . . ?
O43 P4 O41 109.4(4) . . ?
O43 P4 O42 109.1(4) . . ?
O44 P4 O41 109.8(4) . . ?
O44 P4 O42 109.5(3) . . ?
O44 P4 O43 110.1(3) . . ?
P4 O41 H4A 109.5 . . ?
P4 O44 H4B 109.5 . . ?
O51 P5 O52 110.4(4) . . ?
O51 P5 O54 109.0(4) . . ?
O53 P5 O51 107.9(5) . . ?
O53 P5 O52 108.7(5) . . ?
O53 P5 O54 111.0(5) . . ?
O54 P5 O52 109.8(4) . . ?
P5 O52 H5C 109.5 . . ?
P5 O54 H5D 109.5 . . ?
O21 P2 O22 111.8(5) . . ?
O21 P2 O23 112.1(5) . . ?
O21 P2 O24 108.4(7) . . ?
O22 P2 O23 111.0(3) . . ?
O22 P2 O24 106.1(4) . . ?
O23 P2 O24 107.1(4) . . ?
P2 O22 H2E 109.5 . . ?
P2 O24 H2F 109.5 . . ?
O31 P3 O32 109.9(5) . . ?
O31 P3 O33 111.7(6) . . ?
O31 P3 O34 108.4(5) . . ?
O32 P3 O33 107.2(6) . . ?
O32 P3 O34 112.0(5) . . ?
O33 P3 O34 107.6(4) . . ?
P3 O31 H3C 109.5 . . ?
P3 O34 H3D 109.5 . . ?
O61 P6 O63 110.8(4) . . ?
O61 P6 O64 109.8(6) . . ?
O62 P6 O61 110.1(5) . . ?
O62 P6 O63 111.4(6) . . ?
O62 P6 O64 107.1(8) . . ?
O64 P6 O63 107.5(5) . . ?
P6 O62 H6A 109.5 . . ?
P6 O64 H6B 109.5 . . ?
H2G O2 H2H 97.3 . . ?
H6C O6 H6D 109.4 . . ?
H5E O5 H5F 109.4 . . ?
H3E O3 H3F 109.3 . . ?
H7E O7 H7F 109.6 . . ?
H4C O4 H4D 109.7 . . ?
H1E O1 H1F 109.4 . . ?
H8C O8 H8D 109.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N5 H5B O2 0.91 1.87 2.758(8) 165.8 . yes
N7 H7A O4 0.91 1.94 2.822(8) 164.2 . yes
N10 H10A O24 0.91 1.88 2.764(10) 163.4 3_656 yes
N11 H11A O3 0.91 1.88 2.793(8) 177.3 . yes
O2 H2H O6 0.88 2.03 2.808(7) 146.7 5_666 yes
O6 H6C N8 0.85 1.99 2.831(8) 170.0 3_646 yes
O5 H5E O7 0.85 2.05 2.806(10) 148.7 3_646 yes
O3 H3E O8 0.85 1.94 2.727(10) 152.7 . yes

_olex2_submission_special_instructions 'No special instructions were received'
