# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2008

data_global
_journal_name_full               'New J.Chem.'

_journal_coden_Cambridge         0440

_publ_contact_author_name        'L. MacGillivray'
_publ_contact_author_address     
;
Department of Chemistry
University of Iowa
423B Chemistry Bldg
Iowa City
Iowa
52242-1294
UNITED STATES OF AMERICA
;

_publ_contact_author_email       LEN-MACGILLIVRAY@UIOWA.EDU

_publ_section_title              
;
A lanthanide-based helicate coordination polymer
derived from a rigid monodentate organic bridge synthesized in the solid
state
;
loop_
_publ_author_name
'L. MacGillivray'
'Dejan-Kresimir Bucar'
'Tamara D. Hamilton'
'Giannis Papaefstathiou'

data_02184
_database_code_depnum_ccdc_archive 'CCDC 674103'

_audit_creation_date             2008-02-07T17:43:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_sum            'C27 H36 Cl3 N4 O5 Pr'
_chemical_formula_moiety         
;
(C24 H20 N4), (C1 H6 Cl3 O2 Pr1), 2(C1 H4 O1), (H2 O1)
;
_chemical_formula_weight         743.86

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbcn
_symmetry_space_group_name_Hall  '-P 2n 2ab'

_cell_length_a                   23.061(2)
_cell_length_b                   13.5958(14)
_cell_length_c                   20.094(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6300.3(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    190(1)
_cell_measurement_theta_min      1.03
_cell_measurement_theta_max      25.37
_cell_measurement_reflns_used    9683

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3008
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  0.836

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      190(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_number            31701
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_detector_area_resol_mean 9
_reflns_number_total             5528
_reflns_number_gt                3227
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo, Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL v6.1 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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.

The structure refinement was difficult owing to the presence of several highly
disordered solvent molecules. In particular, the structure solution suggested
the presence of a both one disordered methanol and water molecule. Despite
the extensive use of restraints, attempts to resolve the disorder were
unsuccessful since the resulting model included unreasonably short
intermolecular contacts. The electron contribution of the solvent molecules
was therefore subtracted from the diffraction data using the SQUEEZE procedure.
The solvent molecules were found to occupy 870.9 A3 (13.82% of the unit cell).
The total electron count of 211 electrons per unit cell corresponds to
approximately both one molecule of H2O and CH3OH. The use of the SQUEEZE
procedure consequently resulted in a CIF-check report that contains a series
of alerts:
1. level A: refering to the presence of a solvent accessible void
2. level B: referning to differences in the calculated and reported molecular
weight and density
3. level-C: referning to differences in the calculated and reported F000 value

The hydrogen atoms of the coordinating water and methanol molecule were located
in the Fourier difference map and included in the refinement. Their distance to
the corresponding oxygen atom [i.e. O2(methanol)-H2a, O1(water)-H1a and
O1(water)-H1b] were constraint using the SHELX DFIX command.

;

_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^)+(0.0157P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5528
_refine_ls_number_parameters     339
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.046
_refine_ls_wR_factor_gt          0.0441
_refine_ls_goodness_of_fit_ref   0.85
_refine_ls_restrained_S_all      0.852
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.069

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Pr Pr -0.218 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.32470(14) 0.9734(2) 0.53206(17) 0.0263(8) Uani 1 1 d . . .
C2 C 0.29355(14) 1.0355(2) 0.57229(17) 0.0250(9) Uani 1 1 d . . .
C3 C 0.28771(13) 1.0145(2) 0.63932(17) 0.0180(8) Uani 1 1 d . . .
C4 C 0.31606(13) 0.9314(2) 0.66217(17) 0.0210(8) Uani 1 1 d . . .
C5 C 0.34656(14) 0.8729(2) 0.61821(17) 0.0218(8) Uani 1 1 d . . .
C6 C 0.25052(13) 1.0778(2) 0.68360(16) 0.0182(8) Uani 1 1 d . . .
C7 C 0.25642(13) 1.0749(2) 0.75973(15) 0.0176(8) Uani 1 1 d . . .
C8 C 0.25007(13) 1.1895(2) 0.76198(15) 0.0185(8) Uani 1 1 d . . .
C9 C 0.26187(13) 1.1914(2) 0.68513(16) 0.0188(8) Uani 1 1 d . . .
C10 C 0.32058(14) 1.2274(2) 0.66543(16) 0.0196(8) Uani 1 1 d . . .
C11 C 0.37206(13) 1.1958(2) 0.69542(17) 0.0268(9) Uani 1 1 d . . .
C12 C 0.42426(14) 1.2319(3) 0.67385(19) 0.0320(10) Uani 1 1 d . . .
C13 C 0.38092(17) 1.3299(3) 0.59743(18) 0.0378(10) Uani 1 1 d . . .
C14 C 0.32656(15) 1.2979(2) 0.61522(18) 0.0296(9) Uani 1 1 d . . .
C15 C 0.19139(13) 1.2301(2) 0.78145(16) 0.0184(8) Uani 1 1 d . . .
C16 C 0.18752(14) 1.3013(2) 0.83052(17) 0.0256(9) Uani 1 1 d . . .
C17 C 0.13443(15) 1.3438(3) 0.84429(18) 0.0343(10) Uani 1 1 d . . .
C18 C 0.08962(13) 1.2511(3) 0.76690(16) 0.0301(8) Uani 1 1 d . . .
C19 C 0.14067(14) 1.2038(2) 0.74992(17) 0.0241(8) Uani 1 1 d . . .
C20 C 0.21797(14) 1.0143(2) 0.80375(17) 0.0196(8) Uani 1 1 d . . .
C21 C 0.17963(14) 0.9436(2) 0.78092(17) 0.0244(9) Uani 1 1 d . . .
C22 C 0.14888(14) 0.8873(2) 0.82567(17) 0.0242(8) Uani 1 1 d . . .
C23 C 0.19031(14) 0.9668(2) 0.91400(18) 0.0239(8) Uani 1 1 d . . .
C24 C 0.22175(14) 1.0264(2) 0.87236(17) 0.0237(9) Uani 1 1 d . . .
C25 C 0.46736(15) 0.9808(3) 0.66584(19) 0.0402(10) Uani 1 1 d . . .
C26 C 0.52199(14) 0.8628(3) 0.49278(18) 0.0419(6) Uani 1 1 d . . .
H1 H 0.3279 0.9891 0.4872 0.032 Uiso 1 1 calc R . .
H1A H 0.4949(11) 0.679(3) 0.4086(18) 0.06 Uiso 1 1 d D . .
H1B H 0.4602(16) 0.5987(14) 0.432(2) 0.06 Uiso 1 1 d D . .
H2 H 0.2764 1.0916 0.5545 0.03 Uiso 1 1 calc R . .
H2A H 0.4654(16) 0.845(3) 0.5596(11) 0.06 Uiso 1 1 d D . .
H3a H 0.5108 0.8658 0.6624 0.056 Uiso 1 1 calc R . .
H4 H 0.3146 0.915 0.7071 0.025 Uiso 1 1 calc R . .
H5 H 0.3652 0.8174 0.6348 0.026 Uiso 1 1 calc R . .
H6 H 0.2098 1.0666 0.672 0.022 Uiso 1 1 calc R . .
H7 H 0.2968 1.0586 0.7704 0.021 Uiso 1 1 calc R . .
H8 H 0.2816 1.2205 0.7872 0.022 Uiso 1 1 calc R . .
H9 H 0.2313 1.2272 0.6615 0.023 Uiso 1 1 calc R . .
H11 H 0.3709 1.1503 0.73 0.032 Uiso 1 1 calc R . .
H12 H 0.4578 1.2088 0.6942 0.038 Uiso 1 1 calc R . .
H13 H 0.3839 1.3766 0.5638 0.045 Uiso 1 1 calc R . .
H14 H 0.2939 1.323 0.594 0.036 Uiso 1 1 calc R . .
H16 H 0.2204 1.3204 0.854 0.031 Uiso 1 1 calc R . .
H17 H 0.1329 1.3919 0.8772 0.041 Uiso 1 1 calc R . .
H18 H 0.056 1.2333 0.7443 0.036 Uiso 1 1 calc R . .
H19 H 0.1407 1.1548 0.7176 0.029 Uiso 1 1 calc R . .
H21 H 0.1746 0.9342 0.7354 0.029 Uiso 1 1 calc R . .
H22 H 0.123 0.8409 0.8092 0.029 Uiso 1 1 calc R . .
H23 H 0.194 0.9757 0.9597 0.029 Uiso 1 1 calc R . .
H24 H 0.2456 1.0749 0.89 0.028 Uiso 1 1 calc R . .
H25A H 0.4523 0.9798 0.7104 0.06 Uiso 1 1 calc R . .
H25B H 0.439 1.0088 0.6364 0.06 Uiso 1 1 calc R . .
H25C H 0.5021 1.0198 0.6646 0.06 Uiso 1 1 calc R . .
H26A H 0.5465 0.8896 0.5269 0.05 Uiso 1 1 calc R . .
H26B H 0.5128 0.9132 0.4611 0.05 Uiso 1 1 calc R . .
H26C H 0.5418 0.8099 0.4707 0.05 Uiso 1 1 calc R . .
Cl1 Cl 0.39064(4) 0.87820(6) 0.37091(4) 0.0346(2) Uani 1 1 d . . .
Cl2 Cl 0.26498(3) 0.75410(8) 0.47500(4) 0.03142(18) Uani 1 1 d . . .
Cl3 Cl 0.38336(4) 0.61244(6) 0.57418(4) 0.0390(2) Uani 1 1 d . . .
N1 N 0.35077(11) 0.89148(19) 0.55354(13) 0.0200(7) Uani 1 1 d . . .
N2 N 0.15452(11) 0.89622(19) 0.89202(14) 0.0209(7) Uani 1 1 d . . .
N3 N 0.42975(12) 1.2976(2) 0.62576(16) 0.0330(8) Uani 1 1 d . . .
N4 N 0.08551(12) 1.3203(2) 0.81352(16) 0.0329(8) Uani 1 1 d . . .
O1 O 0.46489(10) 0.65710(17) 0.42529(15) 0.0352(7) Uani 1 1 d D . .
O2 O 0.46983(11) 0.8266(2) 0.52207(13) 0.0419(6) Uani 1 1 d D . .
O3 O 0.48023(9) 0.88358(18) 0.64530(13) 0.0375(7) Uani 1 1 d . . .
Pr1 Pr 0.382937(7) 0.746776(16) 0.472358(8) 0.01902(5) Uani 1 1 d . . .

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
C1 0.036(2) 0.026(2) 0.017(2) -0.0026(18) 0.0042(19) 0.0022(17)
C2 0.033(2) 0.020(2) 0.022(2) 0.0012(17) 0.0006(18) 0.0040(16)
C3 0.0163(19) 0.0164(19) 0.021(2) -0.0005(16) -0.0025(16) -0.0032(15)
C4 0.024(2) 0.020(2) 0.018(2) 0.0033(16) -0.0013(17) -0.0009(16)
C5 0.022(2) 0.0177(19) 0.026(2) 0.0001(17) -0.0017(17) 0.0001(16)
C6 0.0156(18) 0.0192(18) 0.020(2) 0.0013(16) -0.0001(16) 0.0020(15)
C7 0.0200(19) 0.0114(17) 0.021(2) -0.0007(15) 0.0004(17) 0.0036(15)
C8 0.0185(18) 0.0169(19) 0.020(2) -0.0014(15) 0.0017(17) -0.0021(16)
C9 0.0201(19) 0.0165(19) 0.020(2) 0.0002(16) 0.0005(16) 0.0028(15)
C10 0.0251(19) 0.015(2) 0.019(2) -0.0064(15) 0.0054(16) 0.0012(15)
C11 0.026(2) 0.0179(19) 0.036(2) 0.0033(17) 0.0040(18) 0.0002(16)
C12 0.022(2) 0.032(3) 0.042(2) -0.007(2) -0.0008(18) -0.0004(18)
C13 0.041(2) 0.035(2) 0.038(2) 0.0058(18) 0.011(2) -0.003(2)
C14 0.030(2) 0.029(2) 0.030(2) 0.0052(18) 0.0024(19) 0.0010(17)
C15 0.0216(19) 0.015(2) 0.0185(19) 0.0039(15) 0.0067(15) 0.0014(15)
C16 0.026(2) 0.024(2) 0.027(2) 0.0040(18) 0.0018(18) 0.0018(17)
C17 0.048(3) 0.026(2) 0.028(2) -0.0053(18) 0.015(2) 0.0043(19)
C18 0.0211(17) 0.038(2) 0.031(2) 0.010(2) 0.0013(16) -0.004(2)
C19 0.024(2) 0.0229(19) 0.025(2) -0.0025(17) 0.0046(18) 0.0028(16)
C20 0.022(2) 0.0153(19) 0.021(2) 0.0019(16) -0.0002(17) 0.0058(15)
C21 0.033(2) 0.022(2) 0.018(2) 0.0006(16) -0.0037(18) 0.0037(18)
C22 0.0223(19) 0.023(2) 0.027(2) -0.0008(17) -0.0049(18) -0.0030(17)
C23 0.032(2) 0.022(2) 0.018(2) 0.0032(17) -0.0054(18) -0.0054(17)
C24 0.024(2) 0.021(2) 0.027(2) -0.0019(17) -0.0006(18) -0.0036(16)
C25 0.036(2) 0.035(2) 0.050(3) 0.003(2) -0.009(2) -0.004(2)
C26 0.0317(13) 0.0549(15) 0.0392(15) -0.0093(13) 0.0039(12) -0.0073(11)
Cl1 0.0424(6) 0.0339(5) 0.0275(5) 0.0073(4) -0.0018(5) -0.0070(5)
Cl2 0.0217(4) 0.0317(4) 0.0408(5) -0.0070(5) 0.0014(4) -0.0015(5)
Cl3 0.0577(6) 0.0316(5) 0.0277(5) 0.0061(4) 0.0036(6) 0.0022(5)
N1 0.0186(16) 0.0202(16) 0.0213(18) -0.0035(13) -0.0034(14) -0.0014(13)
N2 0.0190(16) 0.0200(16) 0.0237(19) 0.0052(13) -0.0018(14) -0.0015(13)
N3 0.0273(19) 0.0299(18) 0.042(2) 0.0002(17) 0.0117(17) -0.0050(15)
N4 0.0289(19) 0.035(2) 0.035(2) 0.0001(16) 0.0119(17) 0.0060(16)
O1 0.0248(15) 0.0233(14) 0.057(2) -0.0064(15) 0.0196(14) -0.0017(13)
O2 0.0317(13) 0.0549(15) 0.0392(15) -0.0093(13) 0.0039(12) -0.0073(11)
O3 0.0276(15) 0.0456(17) 0.0395(18) -0.0083(14) -0.0129(13) 0.0089(13)
Pr1 0.01943(8) 0.01827(9) 0.01937(9) -0.00216(10) 0.00150(9) 0.00031(13)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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 H1 0.93 . ?
C2 C1 1.372(4) . ?
C2 H2 0.93 . ?
C3 C2 1.384(4) . ?
C4 C3 1.383(4) . ?
C4 H4 0.93 . ?
C5 C4 1.381(4) . ?
C5 H5 0.93 . ?
C6 C3 1.506(4) . ?
C6 C7 1.536(4) . ?
C6 H6 0.98 . ?
C7 C8 1.566(4) . ?
C7 H7 0.98 . ?
C8 H8 0.98 . ?
C9 C6 1.567(4) . ?
C9 C8 1.568(4) . ?
C9 H9 0.98 . ?
C10 C9 1.493(4) . ?
C10 C11 1.399(4) . ?
C10 C14 1.399(4) . ?
C11 H11 0.93 . ?
C12 C11 1.371(4) . ?
C12 H12 0.93 . ?
C12 N3 1.322(4) . ?
C13 H13 0.93 . ?
C14 C13 1.374(4) . ?
C14 H14 0.93 . ?
C15 C8 1.513(4) . ?
C15 C16 1.385(4) . ?
C15 C19 1.377(4) . ?
C16 C17 1.382(4) . ?
C16 H16 0.93 . ?
C17 H17 0.93 . ?
C18 C19 1.384(4) . ?
C18 H18 0.93 . ?
C18 N4 1.331(4) . ?
C19 H19 0.93 . ?
C20 C7 1.499(4) . ?
C20 C21 1.384(4) . ?
C20 C24 1.391(4) . ?
C21 C22 1.377(4) . ?
C21 H21 0.93 . ?
C22 H22 0.93 . ?
C23 H23 0.93 . ?
C24 C23 1.372(4) . ?
C24 H24 0.93 . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C26 H26A 0.96 . ?
C26 H26B 0.96 . ?
C26 H26C 0.96 . ?
N1 C1 1.337(4) . ?
N1 C5 1.328(4) . ?
N2 C22 1.345(4) . ?
N2 C23 1.340(4) . ?
N2 Pr1 2.671(3) 2_565 ?
N3 C13 1.336(4) . ?
N4 C17 1.326(4) . ?
O1 H1A 0.825(18) . ?
O1 H1B 0.813(18) . ?
O2 C26 1.426(4) . ?
O2 H2A 0.800(18) . ?
O3 C25 1.417(4) . ?
O3 H3a 0.82 . ?
Pr1 Cl1 2.7166(9) . ?
Pr1 Cl2 2.7226(7) . ?
Pr1 Cl3 2.7427(9) . ?
Pr1 N1 2.661(3) . ?
Pr1 N2 2.671(3) 2_564 ?
Pr1 O1 2.440(2) . ?
Pr1 O2 2.488(3) . ?

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 C2 C3 119.8(3) . . ?
C1 C2 H2 120.1 . . ?
C1 N1 Pr1 122.9(2) . . ?
C2 C1 H1 118 . . ?
C2 C3 C4 116.5(3) . . ?
C2 C3 C6 120.8(3) . . ?
C3 C2 H2 120.1 . . ?
C3 C4 H4 120 . . ?
C3 C6 C7 121.6(3) . . ?
C3 C6 C9 118.7(3) . . ?
C3 C6 H6 108.5 . . ?
C4 C3 C6 122.6(3) . . ?
C4 C5 H5 118.2 . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120 . . ?
C5 N1 C1 116.2(3) . . ?
C5 N1 Pr1 118.7(2) . . ?
C6 C9 C8 88.5(2) . . ?
C6 C9 H9 111.1 . . ?
C6 C7 C8 89.7(2) . . ?
C6 C7 H7 107.9 . . ?
C7 C6 C9 89.5(2) . . ?
C7 C6 H6 108.5 . . ?
C7 C8 C9 88.4(2) . . ?
C7 C8 H8 111.9 . . ?
C8 C7 H7 107.9 . . ?
C8 C7 H7 107.9 . . ?
C8 C7 H7 107.9 . . ?
C8 C9 H9 111.1 . . ?
C9 C6 H6 108.5 . . ?
C10 C9 C6 118.0(3) . . ?
C10 C9 C8 115.1(3) . . ?
C10 C9 H9 111.1 . . ?
C10 C11 H11 120 . . ?
C10 C14 H14 120.2 . . ?
C11 C10 C9 123.7(3) . . ?
C11 C10 C14 116.0(3) . . ?
C11 C12 H12 118.1 . . ?
C12 C11 C10 119.9(3) . . ?
C12 C11 H11 120 . . ?
C12 N3 C13 116.9(3) . . ?
C13 C14 C10 119.6(3) . . ?
C13 C14 H14 120.2 . . ?
C14 C10 C9 120.4(3) . . ?
C14 C13 H13 118.2 . . ?
C15 C8 C7 117.0(3) . . ?
C15 C8 C9 113.8(3) . . ?
C15 C8 H8 111.9 . . ?
C15 C16 H16 120.3 . . ?
C15 C19 C18 119.2(3) . . ?
C15 C19 H19 120.4 . . ?
C16 C15 C8 119.8(3) . . ?
C16 C17 H17 118 . . ?
C17 C16 C15 119.5(3) . . ?
C17 C16 H16 120.3 . . ?
C17 N4 C18 116.0(3) . . ?
C18 C19 H19 120.4 . . ?
C19 C15 C8 123.1(3) . . ?
C19 C15 C16 117.0(3) . . ?
C19 C18 H18 117.9 . . ?
C20 C7 C6 123.3(3) . . ?
C20 C7 C8 118.3(3) . . ?
C20 C7 H7 107.9 . . ?
C20 C21 H21 120.1 . . ?
C20 C24 H24 120 . . ?
C21 C20 C7 124.3(3) . . ?
C21 C20 C24 116.8(3) . . ?
C21 C22 H22 118.4 . . ?
C22 C21 C20 119.9(3) . . ?
C22 C21 H21 120.1 . . ?
C22 N2 Pr1 120.2(2) . 2_565 ?
C23 C24 C20 120.1(3) . . ?
C23 C24 H24 120 . . ?
C23 N2 C22 116.8(3) . . ?
C23 N2 Pr1 121.4(2) . 2_565 ?
C24 C20 C7 118.9(3) . . ?
C24 C23 H23 118.4 . . ?
C25 O3 H3a 109.5 . . ?
C26 O2 H2A 113(3) . . ?
C26 O2 Pr1 131.6(2) . . ?
H1A O1 H1B 122(4) . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Cl1 Pr1 Cl2 93.21(3) . . ?
Cl1 Pr1 Cl3 176.01(3) . . ?
Cl2 Pr1 Cl3 90.76(3) . . ?
N1 C1 C2 123.9(3) . . ?
N1 C1 H1 118 . . ?
N1 C5 C4 123.6(3) . . ?
N1 C5 H5 118.2 . . ?
N1 Pr1 Cl1 89.54(6) . . ?
N1 Pr1 Cl2 71.49(6) . . ?
N1 Pr1 Cl3 92.06(6) . . ?
N1 Pr1 N2 144.94(7) . 2_564 ?
N2 Pr1 Cl1 92.66(6) 2_564 . ?
N2 Pr1 Cl2 73.45(6) 2_564 . ?
N2 Pr1 Cl3 88.13(6) 2_564 . ?
N2 C22 C21 123.2(3) . . ?
N2 C22 H22 118.4 . . ?
N2 C23 C24 123.2(3) . . ?
N2 C23 H23 118.4 . . ?
N3 C12 C11 123.9(3) . . ?
N3 C12 H12 118.1 . . ?
N3 C13 C14 123.7(3) . . ?
N3 C13 H13 118.2 . . ?
N4 C17 C16 124.0(3) . . ?
N4 C17 H17 118 . . ?
N4 C18 C19 124.2(3) . . ?
N4 C18 H18 117.9 . . ?
O1 Pr1 Cl1 89.26(7) . . ?
O1 Pr1 Cl2 143.11(7) . . ?
O1 Pr1 Cl3 87.35(7) . . ?
O1 Pr1 N1 145.39(8) . . ?
O1 Pr1 N2 69.66(8) . 2_564 ?
O1 Pr1 O2 75.52(8) . . ?
O2 C26 H26A 109.5 . . ?
O2 C26 H26B 109.5 . . ?
O2 C26 H26C 109.5 . . ?
O2 Pr1 Cl1 87.80(7) . . ?
O2 Pr1 Cl2 141.33(6) . . ?
O2 Pr1 Cl3 89.33(7) . . ?
O2 Pr1 N1 69.87(8) . . ?
O2 Pr1 N2 145.17(8) . 2_564 ?
O3 C25 H25A 109.5 . . ?
O3 C25 H25B 109.5 . . ?
O3 C25 H25C 109.5 . . ?
Pr1 O1 H1A 129(3) . . ?
Pr1 O1 H1B 109(3) . . ?
Pr1 O2 H2A 114(3) . . ?

# Attachment 'CCDC-674104.cif'

data_mcg7115b
_database_code_depnum_ccdc_archive 'CCDC 674104'

_audit_creation_date             2008-01-10T17:48:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_sum            'C49.59 H52.85 N11 O13.84 Pr'
_chemical_formula_moiety         
;
2(C24 H20 N4), (C1.59 H11.17 N3 O13 Pr1), 4(O0.21 H0.42)
;
_chemical_formula_weight         1165.31

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

_cell_length_a                   23.020(3)
_cell_length_b                   16.8687(18)
_cell_length_c                   13.8344(15)
_cell_angle_alpha                90
_cell_angle_beta                 96.593(5)
_cell_angle_gamma                90
_cell_volume                     5336.6(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(1)
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.88
_cell_measurement_reflns_used    12442

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.45
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2388
_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_T_max  0.944

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      200(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_number            17468
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         5.85
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_detector_area_resol_mean 9
_reflns_number_total             4637
_reflns_number_gt                4081
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo, Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL v6.1 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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.

The coordination sphere of Pr(III) reveals a coorination site that is
partially occupied by methanol and water molecules (occupancies 0.79:021).
Since the oxygen atoms of the methanol (O7) and water (O8) molecules are
occupying the same position, the structure refinement required the use of
the SHELX EXYZ and EADP constraints. Oxygen atoms O9 and O10 were refined
with an isotropic thermal parameter owing to the thermal parameters refining
to non-positive definite or unreasonably large values. In addition, the
results of the structure refinement have indicated that atoms O9 and O10
are not fully occupied. Since these atoms participate in a trimeric water
chain that propagates starting from the Pr(III)-coordinating water molecule
(O8, occupancy 0.21), the occupancies of O9 and O10 were set to be equal
to the one of O8.

The hydrogen atoms of the coordinating water and methanol molecules were
located in the Fourier difference map and included in the refinement. All bond
distances within the water molecule [O6-H6a, O6-H6b, H6a...H6b), as well as
the O7(methanol)-H7a bond distance, were constraint using the SHELX DFIX
command.

;
_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^)+(0.0237P)^2^+14.8669P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4637
_refine_ls_number_parameters     350
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.072
_refine_ls_wR_factor_gt          0.0696
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.071

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.218 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.56552(14) 0.5914(2) -0.0040(2) 0.0303(8) Uani 1 1 d . . .
C2 C 0.58032(13) 0.53290(19) 0.0645(2) 0.0247(7) Uani 1 1 d . . .
C3 C 0.62001(12) 0.54947(17) 0.1457(2) 0.0208(6) Uani 1 1 d . . .
C4 C 0.64194(13) 0.62622(18) 0.1544(2) 0.0265(7) Uani 1 1 d . . .
C5 C 0.62444(14) 0.68105(19) 0.0825(2) 0.0308(7) Uani 1 1 d . . .
C6 C 0.63960(12) 0.48425(17) 0.2153(2) 0.0213(6) Uani 1 1 d . . .
C7 C 0.65182(12) 0.50222(17) 0.3269(2) 0.0208(6) Uani 1 1 d . . .
C8 C 0.71837(12) 0.50163(18) 0.3209(2) 0.0211(6) Uani 1 1 d . . .
C9 C 0.70601(13) 0.46290(17) 0.2166(2) 0.0221(6) Uani 1 1 d . . .
C10 C 0.72090(13) 0.37653(18) 0.2107(2) 0.0244(7) Uani 1 1 d . . .
C11 C 0.68603(14) 0.31553(18) 0.2390(2) 0.0288(7) Uani 1 1 d . . .
C12 C 0.70313(15) 0.2379(2) 0.2300(2) 0.0326(8) Uani 1 1 d . . .
C13 C 0.78661(17) 0.2751(2) 0.1729(3) 0.0483(10) Uani 1 1 d . . .
C14 C 0.77284(15) 0.3544(2) 0.1773(3) 0.0378(8) Uani 1 1 d . . .
C15 C 0.75937(13) 0.45949(18) 0.3963(2) 0.0243(7) Uani 1 1 d . . .
C16 C 0.74092(16) 0.4121(2) 0.4673(3) 0.0453(10) Uani 1 1 d . . .
C17 C 0.78093(17) 0.3725(3) 0.5312(3) 0.0512(11) Uani 1 1 d . . .
C18 C 0.85631(16) 0.4231(2) 0.4619(3) 0.0473(10) Uani 1 1 d . . .
C19 C 0.81895(15) 0.4650(2) 0.3948(3) 0.0426(9) Uani 1 1 d . . .
C20 C 0.62470(13) 0.57164(17) 0.3728(2) 0.0213(6) Uani 1 1 d . . .
C21 C 0.65583(15) 0.61398(19) 0.4486(2) 0.0297(7) Uani 1 1 d . . .
C22 C 0.62778(16) 0.6745(2) 0.4926(2) 0.0362(8) Uani 1 1 d . . .
C23 C 0.54367(15) 0.65649(19) 0.3931(2) 0.0324(8) Uani 1 1 d . . .
C24 C 0.56744(14) 0.59447(19) 0.3458(2) 0.0283(7) Uani 1 1 d . . .
C25 C 0.5587(2) 0.8816(3) 0.5262(3) 0.0395(5) Uani 0.793(4) 1 d P A 1
H1 H 0.5391 0.579 -0.0578 0.036 Uiso 1 1 calc R . .
H2 H 0.5638 0.4827 0.0563 0.03 Uiso 1 1 calc R . .
H4 H 0.6681 0.6406 0.2078 0.032 Uiso 1 1 calc R . .
H5 H 0.6394 0.7322 0.0897 0.037 Uiso 1 1 calc R . .
H6 H 0.6149 0.4371 0.2031 0.026 Uiso 1 1 calc R . .
H6A H 0.6086(15) 0.809(2) 0.890(3) 0.058 Uiso 1 1 d D . .
H6B H 0.5770(17) 0.7449(19) 0.899(3) 0.058 Uiso 1 1 d D . .
H7 H 0.6422 0.4544 0.362 0.025 Uiso 1 1 calc R . .
H7A H 0.544(2) 0.781(2) 0.558(3) 0.058 Uiso 0.793(4) 1 d PD . .
H8 H 0.7319 0.5562 0.3142 0.025 Uiso 1 1 calc R . .
H9 H 0.7241 0.4937 0.168 0.027 Uiso 1 1 calc R . .
H11 H 0.6512 0.3271 0.264 0.035 Uiso 1 1 calc R . .
H12 H 0.6784 0.1983 0.2479 0.039 Uiso 1 1 calc R . .
H13 H 0.8222 0.262 0.1514 0.058 Uiso 1 1 calc R . .
H14 H 0.7982 0.3927 0.158 0.045 Uiso 1 1 calc R . .
H16 H 0.7012 0.4068 0.4723 0.054 Uiso 1 1 calc R . .
H17 H 0.7669 0.3407 0.5783 0.061 Uiso 1 1 calc R . .
H18 H 0.8963 0.4278 0.4592 0.057 Uiso 1 1 calc R . .
H19 H 0.8341 0.4969 0.3488 0.051 Uiso 1 1 calc R . .
H21 H 0.6947 0.6018 0.4691 0.036 Uiso 1 1 calc R . .
H22 H 0.6489 0.7017 0.5436 0.043 Uiso 1 1 calc R . .
H23 H 0.5053 0.6714 0.3724 0.039 Uiso 1 1 calc R . .
H24 H 0.5449 0.568 0.2958 0.034 Uiso 1 1 calc R . .
H25A H 0.5729 0.8586 0.4699 0.059 Uiso 0.3966(19) 1 calc PR A 1
H25B H 0.589 0.913 0.5609 0.059 Uiso 0.3966(19) 1 calc PR A 1
H25C H 0.5255 0.9146 0.506 0.059 Uiso 0.3966(19) 1 calc PR A 1
H25D H 0.552 0.9322 0.5546 0.059 Uiso 0.3966(19) 1 calc PR A 1
H25E H 0.5359 0.8778 0.4637 0.059 Uiso 0.3966(19) 1 calc PR A 1
H25F H 0.5994 0.8762 0.5186 0.059 Uiso 0.3966(19) 1 calc PR A 1
N1 N 0.57806(13) 0.96773(17) 0.8067(2) 0.0366(7) Uani 1 1 d . . .
N2 N 0.5 0.6440(2) 0.75 0.0247(8) Uani 1 2 d S . .
N3 N 0.58731(11) 0.66503(17) 0.00329(18) 0.0309(6) Uani 1 1 d . . .
N4 N 0.75302(13) 0.21610(17) 0.1970(2) 0.0418(7) Uani 1 1 d . . .
N5 N 0.83839(13) 0.37667(18) 0.5298(2) 0.0388(7) Uani 1 1 d . . .
N6 N 0.57265(13) 0.69627(16) 0.4667(2) 0.0348(7) Uani 1 1 d . . .
O1 O 0.59023(10) 0.91876(14) 0.74326(16) 0.0350(5) Uani 1 1 d . A .
O2 O 0.53336(10) 0.95299(13) 0.84918(16) 0.0352(6) Uani 1 1 d . A .
O3 O 0.60807(13) 1.02674(17) 0.8267(2) 0.0641(8) Uani 1 1 d . A .
O4 O 0.52620(9) 0.68299(13) 0.69039(15) 0.0299(5) Uani 1 1 d . A .
O5 O 0.5 0.57089(18) 0.75 0.0369(8) Uani 1 2 d S A .
O6 O 0.58333(10) 0.77926(14) 0.86089(15) 0.0290(5) Uani 1 1 d D A .
O7 O 0.54157(12) 0.81924(14) 0.58884(17) 0.0395(5) Uani 0.793(4) 1 d PD A 1
O8 O 0.54157(12) 0.81924(14) 0.58884(17) 0.0395(5) Uani 0.207(4) 1 d P A 2
O9 O 0.4980(6) 0.9102(8) 0.4311(10) 0.06 Uiso 0.207(4) 1 d P A 2
O10 O 0.5253(6) 0.8310(9) 0.2369(10) 0.06 Uiso 0.207(4) 1 d P . 2
Pr1 Pr 0.5 0.827339(14) 0.75 0.02059(9) Uani 1 2 d S . .

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

C1 0.0276(18) 0.038(2) 0.0241(17) 0.0002(14) -0.0022(14) 0.0044(15)
C2 0.0237(16) 0.0270(17) 0.0228(16) -0.0018(13) 0.0001(13) 0.0011(13)
C3 0.0212(16) 0.0225(16) 0.0189(15) 0.0013(12) 0.0032(12) 0.0055(13)
C4 0.0273(17) 0.0269(18) 0.0242(16) 0.0009(13) -0.0022(13) -0.0010(14)
C5 0.0348(18) 0.0225(18) 0.0348(18) 0.0049(14) 0.0029(15) -0.0010(15)
C6 0.0222(16) 0.0194(16) 0.0216(15) 0.0004(12) -0.0001(12) 0.0014(13)
C7 0.0230(16) 0.0185(16) 0.0206(15) 0.0019(12) 0.0013(12) 0.0009(12)
C8 0.0215(16) 0.0204(16) 0.0211(15) 0.0004(12) 0.0003(12) -0.0013(12)
C9 0.0244(16) 0.0212(16) 0.0208(15) 0.0037(12) 0.0025(12) 0.0031(13)
C10 0.0273(17) 0.0267(18) 0.0179(15) 0.0002(13) -0.0032(13) 0.0054(14)
C11 0.0318(18) 0.0269(19) 0.0281(17) 0.0029(14) 0.0045(14) 0.0062(14)
C12 0.039(2) 0.0271(18) 0.0301(18) 0.0056(14) -0.0031(15) 0.0007(16)
C13 0.036(2) 0.037(2) 0.074(3) -0.008(2) 0.017(2) 0.0113(18)
C14 0.0311(19) 0.0314(19) 0.053(2) -0.0019(16) 0.0129(17) 0.0007(15)
C15 0.0271(17) 0.0229(17) 0.0219(15) -0.0020(13) -0.0017(13) 0.0018(13)
C16 0.0254(19) 0.067(3) 0.043(2) 0.0262(19) 0.0000(16) 0.0048(18)
C17 0.045(2) 0.065(3) 0.042(2) 0.029(2) -0.0027(18) 0.006(2)
C18 0.0222(19) 0.063(3) 0.054(2) 0.010(2) -0.0059(17) 0.0024(18)
C19 0.0271(19) 0.055(2) 0.044(2) 0.0191(18) -0.0028(16) -0.0035(17)
C20 0.0255(16) 0.0194(16) 0.0199(15) 0.0050(12) 0.0059(12) -0.0003(13)
C21 0.0336(19) 0.0291(18) 0.0250(17) 0.0008(14) -0.0027(14) 0.0015(15)
C22 0.054(2) 0.0308(18) 0.0228(16) -0.0072(15) 0.0004(15) -0.0017(18)
C23 0.0334(19) 0.031(2) 0.0335(18) 0.0034(15) 0.0078(15) 0.0058(15)
C24 0.0270(18) 0.0301(18) 0.0274(17) -0.0029(14) 0.0010(14) 0.0025(14)
C25 0.0632(15) 0.0254(12) 0.0338(12) -0.0002(9) 0.0227(10) -0.0019(11)
N1 0.0433(18) 0.0274(16) 0.0383(17) -0.0001(14) 0.0015(14) -0.0100(14)
N2 0.024(2) 0.025(2) 0.0236(19) 0 -0.0055(16) 0
N3 0.0286(14) 0.0365(17) 0.0269(14) 0.0106(13) 0.0003(11) 0.0051(13)
N4 0.0428(19) 0.0276(17) 0.054(2) -0.0030(14) 0.0031(15) 0.0098(14)
N5 0.0357(18) 0.0418(18) 0.0357(16) 0.0040(14) -0.0094(13) 0.0086(14)
N6 0.0482(19) 0.0279(16) 0.0304(15) 0.0009(12) 0.0137(14) 0.0071(13)
O1 0.0386(14) 0.0324(13) 0.0351(13) -0.0032(11) 0.0081(11) -0.0067(11)
O2 0.0382(14) 0.0340(14) 0.0342(13) -0.0055(10) 0.0078(11) -0.0107(11)
O3 0.071(2) 0.0451(17) 0.079(2) -0.0186(15) 0.0199(16) -0.0354(16)
O4 0.0349(13) 0.0276(13) 0.0276(11) 0.0027(10) 0.0058(10) -0.0013(10)
O5 0.050(2) 0.0144(17) 0.046(2) 0 0.0038(16) 0
O6 0.0295(13) 0.0281(13) 0.0265(12) 0.0056(10) -0.0096(10) -0.0073(10)
O7 0.0632(15) 0.0254(12) 0.0338(12) -0.0002(9) 0.0227(10) -0.0019(11)
O8 0.0632(15) 0.0254(12) 0.0338(12) -0.0002(9) 0.0227(10) -0.0019(11)
Pr1 0.02290(14) 0.01863(13) 0.01978(13) 0 0.00048(9) 0

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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 H1 0.93 . ?
C2 C1 1.383(4) . ?
C2 C3 1.393(4) . ?
C2 H2 0.93 . ?
C3 C4 1.390(4) . ?
C4 H4 0.93 . ?
C5 C4 1.383(4) . ?
C5 H5 0.93 . ?
C6 C3 1.497(4) . ?
C6 C9 1.569(4) . ?
C6 H6 0.98 . ?
C7 C6 1.568(4) . ?
C7 C20 1.501(4) . ?
C7 H7 0.98 . ?
C8 C7 1.544(4) . ?
C8 C9 1.580(4) . ?
C8 C15 1.503(4) . ?
C8 H8 0.98 . ?
C9 C10 1.501(4) . ?
C9 H9 0.98 . ?
C11 C10 1.388(4) . ?
C11 C12 1.377(4) . ?
C11 H11 0.93 . ?
C12 H12 0.93 . ?
C13 H13 0.93 . ?
C14 C10 1.382(4) . ?
C14 C13 1.378(5) . ?
C14 H14 0.93 . ?
C15 C16 1.371(4) . ?
C15 C19 1.377(4) . ?
C16 C17 1.375(5) . ?
C16 H16 0.93 . ?
C17 H17 0.93 . ?
C17 N5 1.327(5) . ?
C18 N5 1.324(5) . ?
C18 H18 0.93 . ?
C19 C18 1.386(5) . ?
C19 H19 0.93 . ?
C20 C21 1.397(4) . ?
C20 C24 1.383(4) . ?
C21 H21 0.93 . ?
C22 C21 1.386(5) . ?
C22 H22 0.93 . ?
C24 C23 1.380(4) . ?
C24 H24 0.93 . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C25 H25D 0.96 . ?
C25 H25E 0.96 . ?
C25 H25F 0.96 . ?
N1 O3 1.225(4) . ?
N2 O4 1.262(3) 2_656 ?
N2 O5 1.233(4) . ?
N3 C1 1.339(4) . ?
N3 C5 1.338(4) . ?
N4 C12 1.335(4) . ?
N4 C13 1.326(5) . ?
N6 C22 1.330(4) . ?
N6 C23 1.333(4) . ?
O1 N1 1.260(3) . ?
O2 N1 1.267(3) . ?
O4 N2 1.262(3) . ?
O6 H6A 0.83(2) . ?
O6 H6B 0.80(2) . ?
O7 C25 1.446(5) . ?
O7 H7A 0.78(3) . ?
O7 Pr1 2.529(2) . ?
O10 O10 1.26(2) 2_655 ?
Pr1 O1 2.597(2) . ?
Pr1 O1 2.597(2) 2_656 ?
Pr1 O2 2.593(2) . ?
Pr1 O2 2.593(2) 2_656 ?
Pr1 O4 2.662(2) 2_656 ?
Pr1 O4 2.662(2) . ?
Pr1 O6 2.453(2) 2_656 ?
Pr1 O6 2.453(2) . ?
Pr1 O7 2.529(2) 2_656 ?
Pr1 O8 2.529(2) 2_656 ?

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 C2 C3 119.8(3) . . ?
C1 C2 H2 120.1 . . ?
C2 C1 H1 118.3 . . ?
C2 C3 C6 119.5(3) . . ?
C3 C2 H2 120.1 . . ?
C3 C4 H4 120.4 . . ?
C3 C6 C7 119.9(2) . . ?
C3 C6 C9 113.4(2) . . ?
C3 C6 H6 111.1 . . ?
C4 C3 C2 117.0(3) . . ?
C4 C3 C6 123.4(3) . . ?
C4 C5 H5 118 . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C5 N3 C1 116.6(3) . . ?
C6 C7 H7 107.7 . . ?
C6 C9 C8 89.3(2) . . ?
C6 C9 H9 111.1 . . ?
C7 C6 C9 88.2(2) . . ?
C7 C6 H6 111.1 . . ?
C7 C8 C9 88.7(2) . . ?
C7 C8 H8 109.2 . . ?
C8 C7 C6 90.7(2) . . ?
C8 C7 H7 107.7 . . ?
C8 C9 H9 111.1 . . ?
C9 C6 H6 111.1 . . ?
C9 C8 H8 109.2 . . ?
C10 C9 C6 116.8(2) . . ?
C10 C9 C8 115.6(2) . . ?
C10 C9 H9 111.1 . . ?
C10 C11 H11 120 . . ?
C10 C14 H14 120.4 . . ?
C11 C10 C9 124.1(3) . . ?
C11 C12 H12 118 . . ?
C12 C11 C10 119.9(3) . . ?
C12 C11 H11 120 . . ?
C13 C14 C10 119.3(3) . . ?
C13 C14 H14 120.4 . . ?
C13 N4 C12 115.3(3) . . ?
C14 C10 C9 119.4(3) . . ?
C14 C10 C11 116.4(3) . . ?
C14 C13 H13 117.5 . . ?
C15 C8 C7 120.9(2) . . ?
C15 C8 C9 118.1(2) . . ?
C15 C8 H8 109.2 . . ?
C15 C16 C17 120.3(3) . . ?
C15 C16 H16 119.8 . . ?
C15 C19 C18 119.8(3) . . ?
C15 C19 H19 120.1 . . ?
C16 C15 C8 123.5(3) . . ?
C16 C15 C19 116.2(3) . . ?
C16 C17 H17 118 . . ?
C17 C16 H16 119.8 . . ?
C18 C19 H19 120.1 . . ?
C18 N5 C17 115.8(3) . . ?
C19 C15 C8 120.3(3) . . ?
C19 C18 H18 118.1 . . ?
C20 C7 C6 122.1(2) . . ?
C20 C7 C8 119.4(2) . . ?
C20 C7 H7 107.7 . . ?
C20 C21 H21 120.6 . . ?
C20 C24 H24 120 . . ?
C21 C20 C7 120.9(3) . . ?
C21 C22 H22 117.9 . . ?
C22 C21 C20 118.8(3) . . ?
C22 C21 H21 120.6 . . ?
C22 N6 C23 116.4(3) . . ?
C23 C24 C20 120.1(3) . . ?
C23 C24 H24 120 . . ?
C24 C20 C7 122.2(3) . . ?
C24 C20 C21 116.8(3) . . ?
C24 C23 H23 118.2 . . ?
C25 O7 H7A 103(4) . . ?
C25 O7 Pr1 130.2(2) . . ?
H6A O6 H6B 107(3) . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25A C25 H25D 141.1 . . ?
H25A C25 H25E 56.3 . . ?
H25A C25 H25F 56.3 . . ?
H25B C25 H25C 109.5 . . ?
H25B C25 H25D 56.3 . . ?
H25B C25 H25E 141.1 . . ?
H25B C25 H25F 56.3 . . ?
H25C C25 H25D 56.3 . . ?
H25C C25 H25E 56.3 . . ?
H25C C25 H25F 141.1 . . ?
H25D C25 H25E 109.5 . . ?
H25D C25 H25F 109.5 . . ?
H25E C25 H25F 109.5 . . ?
N1 O1 Pr1 96.99(17) . . ?
N1 O2 Pr1 97.01(17) . . ?
N2 O4 Pr1 97.62(18) . . ?
N3 C1 C2 123.3(3) . . ?
N3 C1 H1 118.3 . . ?
N3 C5 C4 124.0(3) . . ?
N3 C5 H5 118 . . ?
N4 C12 C11 124.0(3) . . ?
N4 C12 H12 118 . . ?
N4 C13 C14 125.0(3) . . ?
N4 C13 H13 117.5 . . ?
N5 C17 C16 124.0(3) . . ?
N5 C17 H17 118 . . ?
N5 C18 C19 123.9(3) . . ?
N5 C18 H18 118.1 . . ?
N6 C22 C21 124.3(3) . . ?
N6 C22 H22 117.9 . . ?
N6 C23 C24 123.6(3) . . ?
N6 C23 H23 118.2 . . ?
O1 N1 O2 116.9(3) . . ?
O1 Pr1 O1 107.15(10) . 2_656 ?
O1 Pr1 O4 108.75(7) 2_656 2_656 ?
O1 Pr1 O4 108.75(7) . . ?
O1 Pr1 O4 139.89(7) 2_656 . ?
O1 Pr1 O4 139.89(7) . 2_656 ?
O2 Pr1 O1 49.01(7) 2_656 2_656 ?
O2 Pr1 O1 49.01(7) . . ?
O2 Pr1 O1 71.65(7) 2_656 . ?
O2 Pr1 O1 71.65(7) . 2_656 ?
O2 Pr1 O2 70.33(10) . 2_656 ?
O2 Pr1 O4 130.37(7) 2_656 . ?
O2 Pr1 O4 130.37(7) . 2_656 ?
O2 Pr1 O4 147.97(7) 2_656 2_656 ?
O2 Pr1 O4 147.97(7) . . ?
O3 N1 O1 121.7(3) . . ?
O3 N1 O2 121.4(3) . . ?
O4 N2 O4 117.1(3) 2_656 . ?
O4 Pr1 O4 47.68(9) 2_656 . ?
O5 N2 O4 121.46(17) . 2_656 ?
O5 N2 O4 121.46(17) . . ?
O6 Pr1 O1 69.36(7) . . ?
O6 Pr1 O1 69.36(7) 2_656 2_656 ?
O6 Pr1 O1 138.17(7) . 2_656 ?
O6 Pr1 O1 138.17(7) 2_656 . ?
O6 Pr1 O2 77.08(8) . . ?
O6 Pr1 O2 77.08(8) 2_656 2_656 ?
O6 Pr1 O2 139.83(8) 2_656 . ?
O6 Pr1 O2 139.83(8) . 2_656 ?
O6 Pr1 O4 72.09(7) 2_656 . ?
O6 Pr1 O4 72.70(7) . . ?
O6 Pr1 O4 72.70(7) 2_656 2_656 ?
O6 Pr1 O4 72.09(7) . 2_656 ?
O6 Pr1 O6 141.38(11) 2_656 . ?
O6 Pr1 O7 100.70(8) 2_656 2_656 ?
O6 Pr1 O7 77.21(8) . 2_656 ?
O6 Pr1 O7 77.21(8) 2_656 . ?
O6 Pr1 O7 100.70(8) . . ?
O6 Pr1 O8 100.70(8) 2_656 2_656 ?
O6 Pr1 O8 77.21(8) . 2_656 ?
O7 C25 H25A 109.5 . . ?
O7 C25 H25B 109.5 . . ?
O7 C25 H25C 109.5 . . ?
O7 C25 H25D 109.5 . . ?
O7 C25 H25E 109.5 . . ?
O7 C25 H25F 109.5 . . ?
O7 Pr1 O1 116.67(8) 2_656 . ?
O7 Pr1 O1 67.37(8) . . ?
O7 Pr1 O1 67.37(8) 2_656 2_656 ?
O7 Pr1 O1 116.67(8) . 2_656 ?
O7 Pr1 O2 72.35(7) 2_656 . ?
O7 Pr1 O2 113.05(7) . . ?
O7 Pr1 O2 113.05(7) 2_656 2_656 ?
O7 Pr1 O2 72.35(7) . 2_656 ?
O7 Pr1 O4 110.23(7) 2_656 . ?
O7 Pr1 O4 63.60(7) . . ?
O7 Pr1 O4 63.60(7) 2_656 2_656 ?
O7 Pr1 O4 110.23(7) . 2_656 ?
O7 Pr1 O7 173.81(11) 2_656 . ?
O8 Pr1 O1 116.67(8) 2_656 . ?
O8 Pr1 O1 67.37(8) 2_656 2_656 ?
O8 Pr1 O2 72.35(7) 2_656 . ?
O8 Pr1 O2 113.05(7) 2_656 2_656 ?
O8 Pr1 O4 63.60(7) 2_656 2_656 ?
O8 Pr1 O4 110.23(7) 2_656 . ?
O8 Pr1 O7 0.00(15) 2_656 2_656 ?
O8 Pr1 O7 173.81(11) 2_656 . ?
Pr1 O6 H6A 124(3) . . ?
Pr1 O6 H6B 117(3) . . ?
Pr1 O7 H7A 126(4) . . ?