# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Patrick Gamez'
_publ_contact_author_email       P.GAMEZ@CHEM.LEIDENUNIV.NL

_publ_section_title              
;
Praseodymium(III)-based
bis-metallacalix[4]arene with host-guest behaviour
;
loop_
_publ_author_name
'Patrick Gamez'
'Jinkui Tang.'
'Simon J. Teat'
'Gong-Feng Xu.'

# Attachment 'Revised_CIF_B925297E.cif'

data_xu
_database_code_depnum_ccdc_archive 'CCDC 754928'
#TrackingRef 'Revised_CIF_B925297E.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C88 H121 N21 O70.50 Pr9'
_chemical_formula_weight         3869.25

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P4/n

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

_cell_length_a                   19.1332(4)
_cell_length_b                   19.1332(4)
_cell_length_c                   18.6926(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6843.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9049
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      25.03

_exptl_crystal_description       block
_exptl_crystal_colour            'pale green'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3782
_exptl_absorpt_coefficient_mu    3.241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_process_details   'SADABS Bruker AXS Madison WI USA'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            57844
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.09
_diffrn_reflns_theta_max         24.99
_reflns_number_total             6038
_reflns_number_gt                4251
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v7.53a'
_computing_data_reduction        'Bruker SAINT v7.53a'
_computing_structure_solution    SIR97
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
All non-hydrogens were refinement anisotropically except the partial
occupied water molecules and actonitrile. Hydrogen atoms were place
geometrically were possible, the hydroxyl hydrogen atoms were placed
to give the best hydrogen bonds. All were then constrained and refined
using a riding model. The hydrogen atoms on the acetonitrile and water
molecules could neither be found or placed and was therefore omitted
from the refinement. In the case of the acetonitrile SHELX has two
instructions for modelling the hydrogens HFIX33 and HFIX137. As HFIX33
produces the ideal stagger conformation for the hydrogen atoms it is
only applicable for methyl group attached to sp3 carbon atoms and
therefore not in this case. HFIX 137 uses a rotational fourier map to
find peaks in the electron density to position for the hydrogen atoms.
If these peak cannot be found then this is not an appropiate instruction
and the result is the methyl group hydrogen atoms continue to rotate and
stopping the shift/esd from coming down close to zero, as in this case.
Geometrical and displacement parameters restrains were use to model the
unbound nitrate. Distance constrains were used to model the disordered
acetonitrile Some displacement parameter ratios max:min are greater than
the ideal of 3:1, splitting these were considered but as no new chemical
information would result they were left as they were.

CIF CHECK Alerts:

PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ...
5.07 Ratio
****************************************
Unbound oxygen atoms in nitrate groups.
******************************************
PLAT430_ALERT_2_A Short Inter D...A Contact O2W .. O2W ..
2.53 Ang.
**************************************************************
Partial occupied water, therefore both not there at same time
**************************************************************

Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O12 - H12A ...
?
*******************
Mu-3 hydroxide.
*******************

Alert level G
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
#_chemical_formula_sum and the formula from the _atom_site* data.
#Atom count from _chemical_formula_sum:C88 H121 N21 O70.5 Pr9
Atom count from the _atom_site data: C88 H106 N21 O69.75 Pr9

Hydrogens are missing from refinement as they could not be found of placed.
The number of oxygen atoms is correct according to SHELXL, two partial
waters are on the 4-fold axis, CIF check does no seem to be correctly
calculating these.

ABSTY01_ALERT_1_G Extra text has been found in the
#_exptl_absorpt_correction_type
field, which should be only a single keyword. A lit
erature
citation should be included in the _exptl_absorpt_process_details
field.

CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G ALERT: Large difference may be due to a
symmetry error - see SYMMG tests
From the CIF: _cell_formula_units_Z 2
From the CIF: _chemical_formula_sum C88 H121 N21 O70.50 Pr9
TEST: Compare cell contents of formula and atom_site data

atom Z*formula cif sites diff
C 176.00 176.00 0.00
H 242.00 212.00 30.00
N 42.00 42.00 0.00
O 141.00 139.50 1.50
Pr 18.00 18.00 0.00
**********************************************************************
Hydrogens are missing from refinement as they could not be found of placed.
The number of oxygen atoms is correct according to SHELXL, two partial
waters are on the 4-fold axis, CIF check does no seem to be correctly
calculating these.
**********************************************************************
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+16.7381P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6038
_refine_ls_number_parameters     435
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1247
_refine_ls_wR_factor_gt          0.1124
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.2500 0.2500 0.28043(4) 0.0229(2) Uani 1 4 d S . .
Pr2 Pr 0.15430(2) 0.35010(2) 0.12236(2) 0.02565(14) Uani 1 1 d . . .
Pr3 Pr 0.38923(2) 0.25110(2) 0.43610(2) 0.02745(14) Uani 1 1 d . . .
N1 N 0.4484(5) 0.2230(5) 0.6705(4) 0.065(3) Uani 1 1 d . . .
H1A H 0.4488 0.1922 0.7055 0.078 Uiso 1 1 calc R . .
N2 N 0.1268(5) 0.4458(4) -0.1029(5) 0.057(2) Uani 1 1 d . . .
H2A H 0.1505 0.4711 -0.1338 0.069 Uiso 1 1 calc R . .
N3 N 0.1117(4) 0.4672(4) 0.2209(4) 0.0413(19) Uani 1 1 d . . .
N4 N 0.5031(4) 0.1991(4) 0.3375(4) 0.046(2) Uani 1 1 d . . .
O1 O 0.3565(3) 0.1459(3) 0.4963(3) 0.0340(14) Uani 1 1 d . . .
O2 O 0.4479(3) 0.2423(3) 0.5526(3) 0.0412(15) Uani 1 1 d . . .
O3 O 0.3510(3) 0.0155(3) 0.4583(3) 0.0413(15) Uani 1 1 d . . .
O4 O 0.5283(5) 0.2947(6) 0.7837(5) 0.104(3) Uani 1 1 d . . .
H4B H 0.5667 0.3093 0.7993 0.156 Uiso 1 1 calc R . .
O5 O 0.2533(3) 0.4011(3) 0.0629(3) 0.0312(13) Uani 1 1 d . . .
O6 O 0.1188(3) 0.4050(3) 0.0090(3) 0.0420(15) Uani 1 1 d . . .
O7 O 0.3518(3) 0.4840(3) 0.1074(3) 0.0387(15) Uani 1 1 d . . .
O8 O 0.1211(6) 0.3282(5) -0.2009(4) 0.101(3) Uani 1 1 d . . .
H8C H 0.1567 0.3060 -0.1876 0.152 Uiso 1 1 calc R . .
O9 O 0.3266(3) 0.3257(3) 0.3531(3) 0.0269(12) Uani 1 1 d . . .
H9C H 0.3564 0.3556 0.3253 0.032 Uiso 1 1 d R . .
O10 O 0.1426(3) 0.2536(2) 0.2054(3) 0.0258(12) Uani 1 1 d . . .
H10D H 0.1000 0.2547 0.2327 0.031 Uiso 1 1 d R . .
O11 O 0.2500 0.2500 0.0972(6) 0.028(2) Uani 1 4 d S . .
H11M H 0.2500 0.2500 0.0459 0.033 Uiso 1 4 d SR . .
O12 O 0.2500 0.2500 0.4568(5) 0.030(3) Uani 1 4 d S . .
H12A H 0.2500 0.2500 0.5081 0.036 Uiso 1 4 d SR . .
O13 O 0.1038(3) 0.4035(3) 0.2388(3) 0.0370(14) Uani 1 1 d . . .
O14 O 0.1342(4) 0.4778(3) 0.1578(3) 0.0489(17) Uani 1 1 d . . .
O15 O 0.0964(4) 0.5142(4) 0.2599(4) 0.065(2) Uani 1 1 d . . .
O16 O 0.4961(4) 0.1761(4) 0.4008(4) 0.0563(19) Uani 1 1 d . . .
O17 O 0.4629(3) 0.2489(3) 0.3199(3) 0.0387(15) Uani 1 1 d . . .
O18 O 0.5445(4) 0.1740(4) 0.2956(4) 0.072(2) Uani 1 1 d . . .
C1 C 0.3966(4) 0.1026(5) 0.5331(4) 0.034(2) Uani 1 1 d . . .
C2 C 0.3947(5) 0.0314(5) 0.5161(5) 0.040(2) Uani 1 1 d . . .
C3 C 0.4321(5) -0.0172(5) 0.5557(5) 0.045(2) Uani 1 1 d . . .
H3A H 0.4299 -0.0655 0.5440 0.054 Uiso 1 1 calc R . .
C4 C 0.4724(6) 0.0051(6) 0.6118(5) 0.059(3) Uani 1 1 d . . .
H4A H 0.4973 -0.0281 0.6398 0.071 Uiso 1 1 calc R . .
C5 C 0.4770(5) 0.0757(5) 0.6282(5) 0.051(3) Uani 1 1 d . . .
H5A H 0.5058 0.0909 0.6665 0.061 Uiso 1 1 calc R . .
C6 C 0.4397(5) 0.1235(5) 0.5887(5) 0.042(2) Uani 1 1 d . . .
C7 C 0.4449(5) 0.1991(6) 0.6030(5) 0.044(2) Uani 1 1 d . . .
C8 C 0.4516(7) 0.2981(6) 0.6893(7) 0.080(4) Uani 1 1 d . . .
H8A H 0.4402 0.3261 0.6463 0.095 Uiso 1 1 calc R . .
H8B H 0.4155 0.3081 0.7259 0.095 Uiso 1 1 calc R . .
C9 C 0.5178(8) 0.3200(8) 0.7161(7) 0.105(5) Uani 1 1 d . . .
H9A H 0.5553 0.3029 0.6841 0.126 Uiso 1 1 calc R . .
H9B H 0.5198 0.3717 0.7169 0.126 Uiso 1 1 calc R . .
C10 C 0.3426(6) -0.0587(5) 0.4400(6) 0.060(3) Uani 1 1 d . . .
H10A H 0.3113 -0.0632 0.3988 0.090 Uiso 1 1 calc R . .
H10B H 0.3227 -0.0838 0.4809 0.090 Uiso 1 1 calc R . .
H10C H 0.3883 -0.0787 0.4280 0.090 Uiso 1 1 calc R . .
C12 C 0.2562(4) 0.4643(4) 0.0332(4) 0.031(2) Uani 1 1 d . . .
C13 C 0.3104(4) 0.5093(4) 0.0535(5) 0.034(2) Uani 1 1 d . . .
C14 C 0.3191(5) 0.5735(5) 0.0214(6) 0.051(3) Uani 1 1 d . . .
H14A H 0.3569 0.6028 0.0347 0.061 Uiso 1 1 calc R . .
C15 C 0.2720(6) 0.5947(5) -0.0306(6) 0.059(3) Uani 1 1 d . . .
H15A H 0.2771 0.6391 -0.0529 0.070 Uiso 1 1 calc R . .
C16 C 0.2179(5) 0.5514(5) -0.0496(5) 0.052(3) Uani 1 1 d . . .
H16A H 0.1861 0.5665 -0.0854 0.062 Uiso 1 1 calc R . .
C17 C 0.2082(4) 0.4870(4) -0.0187(5) 0.034(2) Uani 1 1 d . . .
C18 C 0.1494(5) 0.4417(5) -0.0362(5) 0.043(2) Uani 1 1 d . . .
C19 C 0.0632(7) 0.4092(7) -0.1271(6) 0.076(4) Uani 1 1 d . . .
H19A H 0.0266 0.4138 -0.0899 0.091 Uiso 1 1 calc R . .
H19B H 0.0457 0.4320 -0.1711 0.091 Uiso 1 1 calc R . .
C20 C 0.0747(7) 0.3376(7) -0.1410(6) 0.081(4) Uani 1 1 d . . .
H20A H 0.0295 0.3146 -0.1514 0.098 Uiso 1 1 calc R . .
H20B H 0.0951 0.3152 -0.0981 0.098 Uiso 1 1 calc R . .
C21 C 0.4075(6) 0.5290(6) 0.1323(6) 0.069(3) Uani 1 1 d . . .
H21A H 0.4337 0.5052 0.1702 0.103 Uiso 1 1 calc R . .
H21B H 0.3875 0.5724 0.1511 0.103 Uiso 1 1 calc R . .
H21C H 0.4389 0.5397 0.0924 0.103 Uiso 1 1 calc R . .
N5 N 0.3224(15) 0.6955(19) 0.1967(19) 0.104(9) Uiso 0.50 1 d PDU A 1
C22 C 0.2750(13) 0.6668(17) 0.1919(16) 0.087(6) Uiso 0.50 1 d PDU A 1
C23 C 0.1993(13) 0.6399(18) 0.2047(19) 0.104(9) Uiso 0.50 1 d PDU A 1
N5' N 0.2066(13) 0.6183(13) 0.1755(15) 0.095(7) Uiso 0.50 1 d PDU B 2
C22' C 0.2511(16) 0.651(2) 0.175(2) 0.119(7) Uiso 0.50 1 d PDU B 2
C23' C 0.3204(17) 0.692(2) 0.176(2) 0.097(9) Uiso 0.50 1 d PDU B 2
N6 N 0.2500 0.2500 -0.0963(11) 0.144(8) Uani 1 4 d SDU . .
O19 O 0.2500 0.2500 -0.1608(9) 0.127(7) Uani 1 4 d SDU . .
O20 O 0.269(2) 0.2009(15) -0.0612(9) 0.153(8) Uani 0.50 1 d PDU . .
O1W O 0.2500 0.2500 0.606(3) 0.133(19) Uiso 0.12 1 d P C 1
O1W' O 0.2500 0.2500 0.658(3) 0.129(16) Uiso 0.14 1 d P D 2
O2W O 0.693(4) 0.250(4) 0.602(5) 0.11(3) Uiso 0.13 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pr1 0.0249(3) 0.0249(3) 0.0189(4) 0.000 0.000 0.000
Pr2 0.0269(3) 0.0275(3) 0.0226(2) 0.00184(19) -0.00081(19) 0.00112(19)
Pr3 0.0290(3) 0.0308(3) 0.0225(2) -0.00126(19) -0.00329(19) 0.0006(2)
N1 0.102(8) 0.064(6) 0.028(5) -0.003(4) -0.009(5) -0.013(5)
N2 0.070(6) 0.057(6) 0.046(5) 0.015(4) -0.014(5) -0.012(5)
N3 0.039(5) 0.037(5) 0.048(5) -0.006(4) 0.006(4) 0.008(4)
N4 0.044(5) 0.054(5) 0.041(5) -0.001(4) 0.004(4) 0.003(4)
O1 0.035(3) 0.042(3) 0.026(3) 0.007(3) -0.007(3) -0.002(3)
O2 0.046(4) 0.048(4) 0.030(4) -0.001(3) -0.013(3) -0.005(3)
O3 0.050(4) 0.035(4) 0.038(4) -0.004(3) -0.009(3) 0.007(3)
O4 0.092(7) 0.159(10) 0.061(6) -0.015(6) -0.004(5) -0.021(6)
O5 0.036(3) 0.028(3) 0.029(3) 0.007(2) 0.003(3) -0.001(2)
O6 0.039(4) 0.051(4) 0.035(4) 0.017(3) -0.005(3) -0.001(3)
O7 0.040(4) 0.027(3) 0.049(4) 0.001(3) -0.008(3) -0.004(3)
O8 0.151(9) 0.109(8) 0.044(5) -0.012(5) -0.002(5) -0.020(7)
O9 0.030(3) 0.028(3) 0.022(3) 0.001(2) 0.000(2) -0.002(2)
O10 0.021(3) 0.028(3) 0.028(3) 0.001(2) 0.002(2) 0.001(2)
O11 0.027(4) 0.027(4) 0.029(6) 0.000 0.000 0.000
O12 0.036(4) 0.036(4) 0.017(6) 0.000 0.000 0.000
O13 0.040(4) 0.035(4) 0.036(4) -0.001(3) 0.001(3) 0.004(3)
O14 0.073(5) 0.035(4) 0.038(4) 0.003(3) 0.020(3) 0.002(3)
O15 0.086(6) 0.050(4) 0.060(5) -0.015(4) 0.035(4) 0.013(4)
O16 0.056(5) 0.063(5) 0.050(4) 0.011(4) 0.007(4) 0.020(4)
O17 0.033(3) 0.039(4) 0.044(4) 0.003(3) 0.000(3) 0.000(3)
O18 0.067(5) 0.071(5) 0.079(6) -0.005(4) 0.034(4) 0.024(4)
C1 0.037(5) 0.041(5) 0.025(4) 0.004(4) -0.003(4) 0.004(4)
C2 0.040(5) 0.051(6) 0.030(5) 0.007(4) -0.006(4) 0.007(4)
C3 0.046(6) 0.040(5) 0.049(6) 0.000(5) -0.006(5) 0.012(4)
C4 0.062(7) 0.063(7) 0.053(7) 0.020(6) -0.024(6) 0.011(6)
C5 0.056(7) 0.056(7) 0.041(6) 0.008(5) -0.016(5) 0.003(5)
C6 0.046(6) 0.057(6) 0.024(5) 0.002(4) -0.012(4) 0.005(5)
C7 0.037(5) 0.069(7) 0.025(5) 0.003(5) -0.004(4) -0.006(5)
C8 0.106(11) 0.057(8) 0.076(9) -0.015(7) -0.021(8) -0.013(7)
C9 0.127(14) 0.130(14) 0.058(9) 0.018(9) -0.020(9) -0.038(11)
C10 0.061(7) 0.045(6) 0.073(8) 0.000(6) -0.018(6) 0.009(5)
C12 0.040(5) 0.032(5) 0.022(4) 0.005(4) 0.014(4) 0.004(4)
C13 0.035(5) 0.026(5) 0.041(5) 0.004(4) 0.008(4) -0.002(4)
C14 0.049(6) 0.037(6) 0.068(7) 0.009(5) 0.003(5) -0.009(5)
C15 0.065(7) 0.038(6) 0.073(8) 0.021(5) 0.000(6) -0.007(5)
C16 0.052(6) 0.056(7) 0.048(6) 0.023(5) 0.001(5) 0.022(5)
C17 0.030(5) 0.035(5) 0.037(5) 0.011(4) 0.001(4) 0.012(4)
C18 0.040(6) 0.059(7) 0.031(5) 0.006(5) -0.008(4) 0.020(5)
C19 0.093(10) 0.079(9) 0.055(8) 0.011(7) -0.008(7) 0.010(8)
C20 0.111(11) 0.089(10) 0.045(7) -0.004(7) 0.004(7) -0.029(8)
C21 0.063(8) 0.059(7) 0.084(9) 0.011(6) -0.025(6) -0.021(6)
N6 0.191(12) 0.191(12) 0.049(10) 0.000 0.000 0.000
O19 0.175(11) 0.175(11) 0.030(8) 0.000 0.000 0.000
O20 0.200(14) 0.200(15) 0.060(10) 0.016(8) -0.008(9) 0.003(9)

_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
Pr1 O9 2.469(5) 2 ?
Pr1 O9 2.469(5) 4 ?
Pr1 O9 2.469(5) 3 ?
Pr1 O9 2.469(5) . ?
Pr1 O10 2.489(5) . ?
Pr1 O10 2.489(5) 3 ?
Pr1 O10 2.489(5) 4 ?
Pr1 O10 2.489(5) 2 ?
Pr1 Pr3 3.9451(7) . ?
Pr1 Pr3 3.9451(7) 3 ?
Pr1 Pr3 3.9451(7) 2 ?
Pr1 Pr3 3.9451(7) 4 ?
Pr2 O5 2.403(5) . ?
Pr2 O5 2.405(5) 3 ?
Pr2 O10 2.423(5) . ?
Pr2 O10 2.457(5) 4 ?
Pr2 O6 2.461(6) . ?
Pr2 O14 2.560(6) . ?
Pr2 O13 2.591(6) . ?
Pr2 O7 2.660(5) 3 ?
Pr2 O11 2.6909(19) . ?
Pr2 N3 3.012(8) . ?
Pr2 Pr2 3.7471(6) 3 ?
Pr2 Pr2 3.7472(6) 4 ?
Pr3 O1 2.390(5) . ?
Pr3 O1 2.406(5) 3 ?
Pr3 O9 2.424(5) . ?
Pr3 O2 2.455(5) . ?
Pr3 O9 2.469(5) 4 ?
Pr3 O16 2.585(6) . ?
Pr3 O17 2.590(6) . ?
Pr3 O3 2.673(6) 3 ?
Pr3 O12 2.6918(15) . ?
Pr3 Pr3 3.7674(6) 3 ?
Pr3 Pr3 3.7675(6) 4 ?
N1 C7 1.344(11) . ?
N1 C8 1.481(13) . ?
N1 H1A 0.8800 . ?
N2 C18 1.321(11) . ?
N2 C19 1.475(14) . ?
N2 H2A 0.8800 . ?
N3 O15 1.195(9) . ?
N3 O14 1.271(9) . ?
N3 O13 1.273(9) . ?
N4 O18 1.214(10) . ?
N4 O17 1.267(9) . ?
N4 O16 1.269(10) . ?
O1 C1 1.322(10) . ?
O1 Pr3 2.406(5) 4 ?
O2 C7 1.255(10) . ?
O3 C2 1.399(10) . ?
O3 C10 1.471(11) . ?
O3 Pr3 2.673(6) 4 ?
O4 C9 1.368(14) . ?
O4 H4B 0.8400 . ?
O5 C12 1.333(9) . ?
O5 Pr2 2.405(5) 4 ?
O6 C18 1.245(11) . ?
O7 C13 1.371(10) . ?
O7 C21 1.446(11) . ?
O7 Pr2 2.660(5) 4 ?
O8 C20 1.440(14) . ?
O8 H8C 0.8400 . ?
O9 Pr3 2.469(5) 3 ?
O9 H9C 0.9600 . ?
O10 Pr2 2.457(5) 3 ?
O10 H10D 0.9601 . ?
O11 Pr2 2.6909(19) 4 ?
O11 Pr2 2.6909(19) 3 ?
O11 Pr2 2.6909(19) 2 ?
O11 H11M 0.9601 . ?
O12 Pr3 2.6918(15) 2 ?
O12 Pr3 2.6918(15) 4 ?
O12 Pr3 2.6918(15) 3 ?
O12 H12A 0.9601 . ?
C1 C6 1.387(12) . ?
C1 C2 1.399(12) . ?
C2 C3 1.388(12) . ?
C3 C4 1.370(13) . ?
C3 H3A 0.9500 . ?
C4 C5 1.388(14) . ?
C4 H4A 0.9500 . ?
C5 C6 1.375(12) . ?
C5 H5A 0.9500 . ?
C6 C7 1.474(13) . ?
C8 C9 1.424(17) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C12 C13 1.399(12) . ?
C12 C17 1.405(11) . ?
C13 C14 1.376(12) . ?
C14 C15 1.386(14) . ?
C14 H14A 0.9500 . ?
C15 C16 1.373(14) . ?
C15 H15A 0.9500 . ?
C16 C17 1.374(12) . ?
C16 H16A 0.9500 . ?
C17 C18 1.458(13) . ?
C19 C20 1.411(16) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N5 C22 1.064(9) . ?
C22 C23 1.555(9) . ?
N5' C22' 1.056(9) . ?
C22' C23' 1.540(9) . ?
N6 O20 1.205(15) 3 ?
N6 O20 1.205(15) 2 ?
N6 O20 1.205(15) 4 ?
N6 O20 1.205(15) . ?
N6 O19 1.206(16) . ?
O20 O20 1.43(3) 3 ?
O20 O20 1.43(3) 4 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 Pr1 O9 72.37(12) 2 4 ?
O9 Pr1 O9 72.37(12) 2 3 ?
O9 Pr1 O9 113.2(2) 4 3 ?
O9 Pr1 O9 113.2(2) 2 . ?
O9 Pr1 O9 72.37(12) 4 . ?
O9 Pr1 O9 72.37(12) 3 . ?
O9 Pr1 O10 80.53(17) 2 . ?
O9 Pr1 O10 144.18(16) 4 . ?
O9 Pr1 O10 79.00(16) 3 . ?
O9 Pr1 O10 141.67(16) . . ?
O9 Pr1 O10 78.99(16) 2 3 ?
O9 Pr1 O10 80.53(17) 4 3 ?
O9 Pr1 O10 141.67(16) 3 3 ?
O9 Pr1 O10 144.18(16) . 3 ?
O10 Pr1 O10 71.50(12) . 3 ?
O9 Pr1 O10 144.18(16) 2 4 ?
O9 Pr1 O10 141.67(16) 4 4 ?
O9 Pr1 O10 80.53(17) 3 4 ?
O9 Pr1 O10 78.99(16) . 4 ?
O10 Pr1 O10 71.51(12) . 4 ?
O10 Pr1 O10 111.4(2) 3 4 ?
O9 Pr1 O10 141.67(16) 2 2 ?
O9 Pr1 O10 78.99(16) 4 2 ?
O9 Pr1 O10 144.18(16) 3 2 ?
O9 Pr1 O10 80.53(17) . 2 ?
O10 Pr1 O10 111.4(2) . 2 ?
O10 Pr1 O10 71.51(12) 3 2 ?
O10 Pr1 O10 71.51(12) 4 2 ?
O9 Pr1 Pr3 89.90(12) 2 . ?
O9 Pr1 Pr3 36.97(12) 4 . ?
O9 Pr1 Pr3 89.26(12) 3 . ?
O9 Pr1 Pr3 35.89(12) . . ?
O10 Pr1 Pr3 166.64(12) . . ?
O10 Pr1 Pr3 116.00(11) 3 . ?
O10 Pr1 Pr3 113.11(11) 4 . ?
O10 Pr1 Pr3 81.83(12) 2 . ?
O9 Pr1 Pr3 89.26(12) 2 3 ?
O9 Pr1 Pr3 89.90(12) 4 3 ?
O9 Pr1 Pr3 35.89(12) 3 3 ?
O9 Pr1 Pr3 36.97(12) . 3 ?
O10 Pr1 Pr3 113.11(11) . 3 ?
O10 Pr1 Pr3 166.64(12) 3 3 ?
O10 Pr1 Pr3 81.83(12) 4 3 ?
O10 Pr1 Pr3 116.00(11) 2 3 ?
Pr3 Pr1 Pr3 57.042(12) . 3 ?
O9 Pr1 Pr3 35.89(12) 2 2 ?
O9 Pr1 Pr3 89.26(12) 4 2 ?
O9 Pr1 Pr3 36.97(12) 3 2 ?
O9 Pr1 Pr3 89.90(12) . 2 ?
O10 Pr1 Pr3 81.83(12) . 2 ?
O10 Pr1 Pr3 113.11(11) 3 2 ?
O10 Pr1 Pr3 116.00(11) 4 2 ?
O10 Pr1 Pr3 166.64(12) 2 2 ?
Pr3 Pr1 Pr3 84.95(2) . 2 ?
Pr3 Pr1 Pr3 57.042(12) 3 2 ?
O9 Pr1 Pr3 36.97(12) 2 4 ?
O9 Pr1 Pr3 35.89(12) 4 4 ?
O9 Pr1 Pr3 89.90(12) 3 4 ?
O9 Pr1 Pr3 89.26(12) . 4 ?
O10 Pr1 Pr3 116.00(11) . 4 ?
O10 Pr1 Pr3 81.83(12) 3 4 ?
O10 Pr1 Pr3 166.64(12) 4 4 ?
O10 Pr1 Pr3 113.11(11) 2 4 ?
Pr3 Pr1 Pr3 57.043(12) . 4 ?
Pr3 Pr1 Pr3 84.95(2) 3 4 ?
Pr3 Pr1 Pr3 57.042(12) 2 4 ?
O5 Pr2 O5 116.5(3) . 3 ?
O5 Pr2 O10 132.74(17) . . ?
O5 Pr2 O10 70.62(17) 3 . ?
O5 Pr2 O10 70.09(17) . 4 ?
O5 Pr2 O10 132.56(17) 3 4 ?
O10 Pr2 O10 73.2(2) . 4 ?
O5 Pr2 O6 69.30(19) . . ?
O5 Pr2 O6 79.00(19) 3 . ?
O10 Pr2 O6 148.35(19) . . ?
O10 Pr2 O6 137.16(18) 4 . ?
O5 Pr2 O14 81.41(19) . . ?
O5 Pr2 O14 142.0(2) 3 . ?
O10 Pr2 O14 123.19(18) . . ?
O10 Pr2 O14 84.12(19) 4 . ?
O6 Pr2 O14 77.0(2) . . ?
O5 Pr2 O13 121.48(19) . . ?
O5 Pr2 O13 121.81(18) 3 . ?
O10 Pr2 O13 74.20(17) . . ?
O10 Pr2 O13 74.63(17) 4 . ?
O6 Pr2 O13 116.89(19) . . ?
O14 Pr2 O13 49.48(18) . . ?
O5 Pr2 O7 136.92(18) . 3 ?
O5 Pr2 O7 61.50(17) 3 3 ?
O10 Pr2 O7 89.10(18) . 3 ?
O10 Pr2 O7 146.54(18) 4 3 ?
O6 Pr2 O7 68.26(19) . 3 ?
O14 Pr2 O7 82.3(2) . 3 ?
O13 Pr2 O7 73.30(18) . 3 ?
O5 Pr2 O11 70.84(16) . . ?
O5 Pr2 O11 70.80(16) 3 . ?
O10 Pr2 O11 68.4(2) . . ?
O10 Pr2 O11 68.0(2) 4 . ?
O6 Pr2 O11 110.0(3) . . ?
O14 Pr2 O11 145.73(16) . . ?
O13 Pr2 O11 132.9(3) . . ?
O7 Pr2 O11 131.83(14) 3 . ?
O5 Pr2 N3 101.2(2) . . ?
O5 Pr2 N3 137.36(19) 3 . ?
O10 Pr2 N3 98.63(19) . . ?
O10 Pr2 N3 77.31(18) 4 . ?
O6 Pr2 N3 97.7(2) . . ?
O14 Pr2 N3 24.70(19) . . ?
O13 Pr2 N3 24.83(18) . . ?
O7 Pr2 N3 77.64(19) 3 . ?
O11 Pr2 N3 145.1(2) . . ?
O5 Pr2 Pr2 115.06(13) . 3 ?
O5 Pr2 Pr2 38.77(12) 3 3 ?
O10 Pr2 Pr2 40.18(12) . 3 ?
O10 Pr2 Pr2 94.28(12) 4 3 ?
O6 Pr2 Pr2 114.85(15) . 3 ?
O14 Pr2 Pr2 161.91(14) . 3 ?
O13 Pr2 Pr2 112.69(13) . 3 ?
O7 Pr2 Pr2 89.42(13) 3 3 ?
O11 Pr2 Pr2 45.87(4) . 3 ?
N3 Pr2 Pr2 137.51(15) . 3 ?
O5 Pr2 Pr2 38.83(13) . 4 ?
O5 Pr2 Pr2 115.03(13) 3 4 ?
O10 Pr2 Pr2 94.34(12) . 4 ?
O10 Pr2 Pr2 39.51(12) 4 4 ?
O6 Pr2 Pr2 106.60(14) . 4 ?
O14 Pr2 Pr2 99.87(16) . 4 ?
O13 Pr2 Pr2 112.43(13) . 4 ?
O7 Pr2 Pr2 173.94(13) 3 4 ?
O11 Pr2 Pr2 45.87(4) . 4 ?
N3 Pr2 Pr2 106.70(14) . 4 ?
Pr2 Pr2 Pr2 90.0 3 4 ?
O1 Pr3 O1 114.4(3) . 3 ?
O1 Pr3 O9 131.92(18) . . ?
O1 Pr3 O9 70.59(17) 3 . ?
O1 Pr3 O2 69.18(19) . . ?
O1 Pr3 O2 76.70(19) 3 . ?
O9 Pr3 O2 146.44(19) . . ?
O1 Pr3 O9 70.10(17) . 4 ?
O1 Pr3 O9 131.42(18) 3 4 ?
O9 Pr3 O9 73.1(2) . 4 ?
O2 Pr3 O9 137.82(18) . 4 ?
O1 Pr3 O16 81.9(2) . . ?
O1 Pr3 O16 143.7(2) 3 . ?
O9 Pr3 O16 123.7(2) . . ?
O2 Pr3 O16 80.0(2) . . ?
O9 Pr3 O16 83.9(2) 4 . ?
O1 Pr3 O17 121.57(19) . . ?
O1 Pr3 O17 123.93(19) 3 . ?
O9 Pr3 O17 75.06(18) . . ?
O2 Pr3 O17 119.58(19) . . ?
O9 Pr3 O17 74.41(17) 4 . ?
O16 Pr3 O17 49.1(2) . . ?
O1 Pr3 O3 135.03(18) . 3 ?
O1 Pr3 O3 61.19(19) 3 3 ?
O9 Pr3 O3 90.87(18) . 3 ?
O2 Pr3 O3 66.38(19) . 3 ?
O9 Pr3 O3 149.76(17) 4 3 ?
O16 Pr3 O3 84.1(2) . 3 ?
O17 Pr3 O3 76.76(18) . 3 ?
O1 Pr3 O12 70.54(16) . . ?
O1 Pr3 O12 70.31(16) 3 . ?
O9 Pr3 O12 66.9(2) . . ?
O2 Pr3 O12 108.9(3) . . ?
O9 Pr3 O12 66.3(2) 4 . ?
O16 Pr3 O12 144.63(17) . . ?
O17 Pr3 O12 131.2(2) . . ?
O3 Pr3 O12 131.14(15) 3 . ?
O1 Pr3 Pr3 113.86(13) . 3 ?
O1 Pr3 Pr3 38.07(13) 3 3 ?
O9 Pr3 Pr3 40.09(12) . 3 ?
O2 Pr3 Pr3 111.94(14) . 3 ?
O9 Pr3 Pr3 94.12(12) 4 3 ?
O16 Pr3 Pr3 162.48(15) . 3 ?
O17 Pr3 Pr3 113.56(13) . 3 ?
O3 Pr3 Pr3 89.10(13) 3 3 ?
O12 Pr3 Pr3 45.59(3) . 3 ?
O1 Pr3 Pr3 38.37(13) . 4 ?
O1 Pr3 Pr3 113.69(14) 3 4 ?
O9 Pr3 Pr3 94.19(12) . 4 ?
O2 Pr3 Pr3 105.78(14) . 4 ?
O9 Pr3 Pr3 39.23(12) 4 4 ?
O16 Pr3 Pr3 99.16(17) . 4 ?
O17 Pr3 Pr3 111.73(13) . 4 ?
O3 Pr3 Pr3 171.01(13) 3 4 ?
O12 Pr3 Pr3 45.59(3) . 4 ?
Pr3 Pr3 Pr3 90.0 3 4 ?
O1 Pr3 Pr1 99.56(13) . . ?
O1 Pr3 Pr1 99.26(13) 3 . ?
O9 Pr3 Pr1 36.65(12) . . ?
O2 Pr3 Pr1 164.23(14) . . ?
O9 Pr3 Pr1 36.96(12) 4 . ?
O16 Pr3 Pr1 110.05(16) . . ?
O17 Pr3 Pr1 75.47(13) . . ?
O3 Pr3 Pr1 125.37(13) 3 . ?
O12 Pr3 Pr1 55.8(2) . . ?
Pr3 Pr3 Pr1 61.479(6) 3 . ?
Pr3 Pr3 Pr1 61.479(6) 4 . ?
C7 N1 C8 123.7(9) . . ?
C7 N1 H1A 118.1 . . ?
C8 N1 H1A 118.1 . . ?
C18 N2 C19 122.1(9) . . ?
C18 N2 H2A 119.0 . . ?
C19 N2 H2A 119.0 . . ?
O15 N3 O14 122.0(8) . . ?
O15 N3 O13 122.1(8) . . ?
O14 N3 O13 115.9(7) . . ?
O15 N3 Pr2 178.5(6) . . ?
O14 N3 Pr2 57.3(4) . . ?
O13 N3 Pr2 58.7(4) . . ?
O18 N4 O17 121.8(8) . . ?
O18 N4 O16 122.2(8) . . ?
O17 N4 O16 116.0(8) . . ?
C1 O1 Pr3 128.4(5) . . ?
C1 O1 Pr3 123.7(5) . 4 ?
Pr3 O1 Pr3 103.6(2) . 4 ?
C7 O2 Pr3 133.6(6) . . ?
C2 O3 C10 117.0(7) . . ?
C2 O3 Pr3 113.5(5) . 4 ?
C10 O3 Pr3 123.0(5) . 4 ?
C9 O4 H4B 109.5 . . ?
C12 O5 Pr2 126.5(5) . . ?
C12 O5 Pr2 124.1(5) . 4 ?
Pr2 O5 Pr2 102.40(19) . 4 ?
C18 O6 Pr2 134.0(6) . . ?
C13 O7 C21 116.8(7) . . ?
C13 O7 Pr2 115.0(5) . 4 ?
C21 O7 Pr2 124.6(6) . 4 ?
C20 O8 H8C 109.5 . . ?
Pr3 O9 Pr1 107.46(19) . . ?
Pr3 O9 Pr3 100.69(18) . 3 ?
Pr1 O9 Pr3 106.07(19) . 3 ?
Pr3 O9 H9C 113.9 . . ?
Pr1 O9 H9C 113.8 . . ?
Pr3 O9 H9C 113.8 3 . ?
Pr2 O10 Pr2 100.31(18) . 3 ?
Pr2 O10 Pr1 107.77(19) . . ?
Pr2 O10 Pr1 106.70(18) 3 . ?
Pr2 O10 H10D 113.7 . . ?
Pr2 O10 H10D 113.7 3 . ?
Pr1 O10 H10D 113.7 . . ?
Pr2 O11 Pr2 159.9(5) 4 3 ?
Pr2 O11 Pr2 88.26(8) 4 2 ?
Pr2 O11 Pr2 88.26(8) 3 2 ?
Pr2 O11 Pr2 88.26(8) 4 . ?
Pr2 O11 Pr2 88.26(8) 3 . ?
Pr2 O11 Pr2 159.9(5) 2 . ?
Pr2 O11 H11M 100.0 4 . ?
Pr2 O11 H11M 100.0 3 . ?
Pr2 O11 H11M 100.0 2 . ?
Pr2 O11 H11M 100.0 . . ?
Pr3 O12 Pr3 163.5(4) . 2 ?
Pr3 O12 Pr3 88.82(6) . 4 ?
Pr3 O12 Pr3 88.82(6) 2 4 ?
Pr3 O12 Pr3 88.82(6) . 3 ?
Pr3 O12 Pr3 88.82(6) 2 3 ?
Pr3 O12 Pr3 163.5(4) 4 3 ?
Pr3 O12 H12A 98.2 . . ?
Pr3 O12 H12A 98.2 2 . ?
Pr3 O12 H12A 98.2 4 . ?
Pr3 O12 H12A 98.2 3 . ?
N3 O13 Pr2 96.4(5) . . ?
N3 O14 Pr2 98.0(5) . . ?
N4 O16 Pr3 97.4(5) . . ?
N4 O17 Pr3 97.2(5) . . ?
O1 C1 C6 123.6(8) . . ?
O1 C1 C2 118.5(7) . . ?
C6 C1 C2 117.8(8) . . ?
C3 C2 C1 121.2(8) . . ?
C3 C2 O3 125.1(9) . . ?
C1 C2 O3 113.7(7) . . ?
C4 C3 C2 119.4(9) . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 H3A 120.3 . . ?
C3 C4 C5 120.5(9) . . ?
C3 C4 H4A 119.8 . . ?
C5 C4 H4A 119.8 . . ?
C6 C5 C4 119.8(9) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
C5 C6 C1 121.2(9) . . ?
C5 C6 C7 121.4(8) . . ?
C1 C6 C7 117.3(8) . . ?
O2 C7 N1 118.6(9) . . ?
O2 C7 C6 120.9(8) . . ?
N1 C7 C6 120.4(9) . . ?
C9 C8 N1 114.0(12) . . ?
C9 C8 H8A 108.8 . . ?
N1 C8 H8A 108.8 . . ?
C9 C8 H8B 108.8 . . ?
N1 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
O4 C9 C8 110.5(12) . . ?
O4 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
O4 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
O3 C10 H10A 109.5 . . ?
O3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C12 C13 118.5(8) . . ?
O5 C12 C17 122.7(8) . . ?
C13 C12 C17 118.8(8) . . ?
O7 C13 C14 124.5(8) . . ?
O7 C13 C12 114.2(7) . . ?
C14 C13 C12 121.3(9) . . ?
C13 C14 C15 119.3(9) . . ?
C13 C14 H14A 120.3 . . ?
C15 C14 H14A 120.3 . . ?
C16 C15 C14 119.6(9) . . ?
C16 C15 H15A 120.2 . . ?
C14 C15 H15A 120.2 . . ?
C15 C16 C17 122.3(9) . . ?
C15 C16 H16A 118.8 . . ?
C17 C16 H16A 118.8 . . ?
C16 C17 C12 118.6(8) . . ?
C16 C17 C18 122.9(8) . . ?
C12 C17 C18 118.5(7) . . ?
O6 C18 N2 121.3(9) . . ?
O6 C18 C17 123.1(8) . . ?
N2 C18 C17 115.4(9) . . ?
C20 C19 N2 112.9(11) . . ?
C20 C19 H19A 109.0 . . ?
N2 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
N2 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 O8 111.2(11) . . ?
C19 C20 H20A 109.4 . . ?
O8 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
O8 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
O7 C21 H21A 109.5 . . ?
O7 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O7 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 162(3) . . ?
N5' C22' C23' 174(5) . . ?
O20 N6 O20 72.8(13) 3 2 ?
O20 N6 O20 114(3) 3 4 ?
O20 N6 O20 72.8(13) 2 4 ?
O20 N6 O20 72.8(13) 3 . ?
O20 N6 O20 114(3) 2 . ?
O20 N6 O20 72.8(13) 4 . ?
O20 N6 O19 123.0(14) 3 . ?
O20 N6 O19 123.0(14) 2 . ?
O20 N6 O19 123.0(14) 4 . ?
O20 N6 O19 123.0(14) . . ?
N6 O20 O20 53.6(7) . 3 ?
N6 O20 O20 53.6(7) . 4 ?
O20 O20 O20 90.000(4) 3 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
N1 H1A O8 0.88 2.24 2.917(12) 133.9 2_556
N2 H2A O4 0.88 2.16 3.041(13) 175.5 3_554
O4 H4B N5 0.84 2.12 2.89(3) 150.7 5_666
O8 H8C O19 0.84 2.14 2.980(11) 176.2 .
O8 H8C N6 0.84 2.69 3.485(15) 157.9 .
O9 H9C O13 0.96 2.01 2.924(8) 158.9 4
O10 H10D O17 0.96 2.03 2.942(8) 158.3 2
O11 H11M O20 0.96 2.24 3.13(2) 153.2 .
O11 H11M O20 0.96 2.24 3.13(2) 153.2 2
O11 H11M O20 0.96 2.24 3.13(2) 153.2 4
O11 H11M O20 0.96 2.24 3.13(2) 153.2 3
O11 H11M N6 0.96 2.66 3.62(2) 180.0 .
O12 H12A O1W 0.96 1.83 2.79(6) 180.0 .

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.408
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.170