# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003


data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Paul Clarke'
'Polly L. Arnold'
'Chuen Chan'
'Louise S. Natrajan'
'Martin A. Smith'
'Claire Wilson'

_publ_contact_author_name        'Dr Paul Clarke'
_publ_contact_author_address     
;
Chemistry
University of Nottingham
School of Chemistry
University Park
Nottingham
Notts
NG9 2QR
UNITED KINGDOM
;

_publ_contact_author_email       PAUL.CLARKE@NOTTINGHAM.AC.UK

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Mechanistic insight into the lanthanide(III) salt
catalysed monoacylation of symmetrical diols from structural models
;
#===========================================================================
#==

data_PRMHBZ
_database_code_CSD               215708

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C51 H81 O9 Pr'
_chemical_formula_sum            'C51 H81 O9 Pr'
_chemical_formula_weight         979.07

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'
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           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.576(3)
_cell_length_b                   12.662(4)
_cell_length_c                   20.988(6)
_cell_angle_alpha                79.191(7)
_cell_angle_beta                 81.482(6)
_cell_angle_gamma                81.016(5)
_cell_volume                     2706.3(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    17476
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      28.2

_exptl_crystal_description       column
_exptl_crystal_colour            'pale green'
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1036
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_T_max  0.482
_exptl_absorpt_process_details   'SHELXTL version 6.12; Bruker, 2001)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        2.1
_diffrn_reflns_number            39109
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.038
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         28.68
_reflns_number_total             12439
_reflns_number_gt                10631
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  
'SHELXL-97; enCIFer (CCDC, 2003); PLATON (Spek, 2003)'

_refine_special_details          
;
?
;

_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^)+(0.0495P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   
'placed geometrically, except H61 and H62 located from difference map'
_refine_ls_hydrogen_treatment    
'riding model, except H61 and H62 (distance restraints applied)'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12439
_refine_ls_number_parameters     556
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0828
_refine_ls_wR_factor_gt          0.0800
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_restrained_S_all      1.02
_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
Pr Pr 0.217949(12) 0.744017(11) 0.241966(6) 0.02877(5) Uani 1 1 d . . .
O31 O 0.36583(16) 0.77010(13) 0.14334(8) 0.0362(4) Uani 1 1 d . . .
C31 C 0.4410(2) 0.7091(2) 0.10895(11) 0.0316(5) Uani 1 1 d . . .
C32 C 0.4839(2) 0.5997(2) 0.13090(11) 0.0340(5) Uani 1 1 d . . .
H32A H 0.5369 0.5599 0.1004 0.041 Uiso 1 1 calc R . .
O33 O 0.37947(16) 0.58674(13) 0.23909(7) 0.0353(4) Uani 1 1 d . . .
C33 C 0.4542(2) 0.54478(19) 0.19446(11) 0.0302(5) Uani 1 1 d . . .
O41 O 0.0603(2) 0.83762(15) 0.31624(9) 0.0537(5) Uani 1 1 d . . .
C41 C -0.0157(3) 0.9251(2) 0.31637(14) 0.0443(7) Uani 1 1 d . . .
C42 C -0.0228(2) 1.0079(2) 0.26283(14) 0.0425(6) Uani 1 1 d . . .
H42A H -0.0819 1.0716 0.2674 0.051 Uiso 1 1 calc R . .
O43 O 0.13552(16) 0.92219(14) 0.19123(8) 0.0402(4) Uani 1 1 d . . .
C43 C 0.0526(2) 1.0027(2) 0.20223(13) 0.0385(6) Uani 1 1 d . . .
O51 O 0.09674(17) 0.60535(14) 0.30458(8) 0.0383(4) Uani 1 1 d . . .
C51 C 0.0521(2) 0.52549(19) 0.29214(12) 0.0310(5) Uani 1 1 d . . .
C52 C 0.0411(2) 0.51040(19) 0.22900(12) 0.0347(5) Uani 1 1 d . . .
H52A H 0.0142 0.4445 0.2242 0.042 Uiso 1 1 calc R . .
O53 O 0.10754(18) 0.67446(14) 0.17206(8) 0.0389(4) Uani 1 1 d . . .
C53 C 0.0671(2) 0.58563(19) 0.17255(11) 0.0319(5) Uani 1 1 d . . .
O61 O 0.41251(15) 0.82268(13) 0.26677(7) 0.0297(3) Uani 1 1 d D . .
H61 H 0.4707(19) 0.847(2) 0.2403(11) 0.044 Uiso 1 1 d D . .
C61 C 0.4466(2) 0.81761(18) 0.33142(10) 0.0263(5) Uani 1 1 d . . .
H61A H 0.5427 0.8116 0.3282 0.032 Uiso 1 1 calc R . .
O62 O 0.27149(16) 0.71015(14) 0.36419(8) 0.0340(4) Uani 1 1 d D . .
H62 H 0.228(2) 0.7551(19) 0.3844(13) 0.051 Uiso 1 1 d D . .
C62 C 0.4051(2) 0.71074(18) 0.37022(11) 0.0274(5) Uani 1 1 d . . .
H62A H 0.4554 0.6512 0.3481 0.033 Uiso 1 1 calc R . .
O70 O 0.63531(17) 0.89195(15) 0.20466(9) 0.0436(4) Uani 1 1 d . . .
C71 C 0.5099(4) 1.0646(2) 0.18249(17) 0.0726(11) Uani 1 1 d . . .
H71A H 0.5149 1.1409 0.1635 0.109 Uiso 1 1 calc R . .
H71B H 0.4730 1.0592 0.2285 0.109 Uiso 1 1 calc R . .
H71C H 0.4550 1.0347 0.1585 0.109 Uiso 1 1 calc R . .
C72 C 0.6426(3) 1.0019(3) 0.17784(15) 0.0594(8) Uani 1 1 d . . .
H72A H 0.6809 1.0083 0.1315 0.071 Uiso 1 1 calc R . .
H72B H 0.6984 1.0320 0.2019 0.071 Uiso 1 1 calc R . .
C73 C 0.7564(3) 0.8245(3) 0.20001(15) 0.0562(8) Uani 1 1 d . . .
H73D H 0.8168 0.8492 0.2241 0.067 Uiso 1 1 calc R . .
H73E H 0.7941 0.8291 0.1537 0.067 Uiso 1 1 calc R . .
C74 C 0.7367(3) 0.7103(3) 0.22828(17) 0.0666(9) Uani 1 1 d . . .
H74A H 0.8196 0.6635 0.2250 0.100 Uiso 1 1 calc R . .
H74B H 0.6770 0.6863 0.2041 0.100 Uiso 1 1 calc R . .
H74C H 0.7005 0.7061 0.2743 0.100 Uiso 1 1 calc R . .
C310 C 0.4878(2) 0.7645(2) 0.03948(11) 0.0392(6) Uani 1 1 d . . .
C311 C 0.5692(4) 0.6872(3) -0.00275(14) 0.0660(10) Uani 1 1 d . . .
H31A H 0.6458 0.6526 0.0181 0.099 Uiso 1 1 calc R . .
H31B H 0.5960 0.7278 -0.0459 0.099 Uiso 1 1 calc R . .
H31C H 0.5183 0.6314 -0.0076 0.099 Uiso 1 1 calc R . .
C312 C 0.5702(5) 0.8485(3) 0.04683(17) 0.0933(15) Uani 1 1 d . . .
H31D H 0.6468 0.8119 0.0670 0.140 Uiso 1 1 calc R . .
H31E H 0.5201 0.8984 0.0745 0.140 Uiso 1 1 calc R . .
H31F H 0.5969 0.8892 0.0037 0.140 Uiso 1 1 calc R . .
C313 C 0.3706(4) 0.8189(4) 0.00728(17) 0.123(2) Uani 1 1 d . . .
H31G H 0.3185 0.7638 0.0027 0.184 Uiso 1 1 calc R . .
H31H H 0.3980 0.8588 -0.0360 0.184 Uiso 1 1 calc R . .
H31I H 0.3191 0.8694 0.0342 0.184 Uiso 1 1 calc R . .
C330 C 0.5156(2) 0.4272(2) 0.21537(12) 0.0361(5) Uani 1 1 d . . .
C331 C 0.6117(3) 0.4303(2) 0.26367(14) 0.0482(7) Uani 1 1 d . . .
H33D H 0.6801 0.4728 0.2412 0.072 Uiso 1 1 calc R . .
H33E H 0.6498 0.3562 0.2798 0.072 Uiso 1 1 calc R . .
H33F H 0.5661 0.4638 0.3005 0.072 Uiso 1 1 calc R . .
C332 C 0.4087(3) 0.3605(2) 0.25049(14) 0.0462(6) Uani 1 1 d . . .
H33A H 0.3480 0.3583 0.2199 0.069 Uiso 1 1 calc R . .
H33B H 0.3629 0.3940 0.2873 0.069 Uiso 1 1 calc R . .
H33C H 0.4469 0.2865 0.2667 0.069 Uiso 1 1 calc R . .
C410 C -0.1033(3) 0.9325(2) 0.38173(16) 0.0556(8) Uani 1 1 d . . .
C411 C -0.1829(5) 1.0421(3) 0.3850(2) 0.1076(18) Uani 1 1 d . . .
H41G H -0.2358 1.0611 0.3488 0.161 Uiso 1 1 calc R . .
H41H H -0.1254 1.0971 0.3815 0.161 Uiso 1 1 calc R . .
H41I H -0.2391 1.0391 0.4266 0.161 Uiso 1 1 calc R . .
C412 C -0.0177(4) 0.9018(4) 0.43829(17) 0.0939(14) Uani 1 1 d . . .
H41D H -0.0720 0.9060 0.4801 0.141 Uiso 1 1 calc R . .
H41E H 0.0463 0.9522 0.4319 0.141 Uiso 1 1 calc R . .
H41F H 0.0266 0.8277 0.4385 0.141 Uiso 1 1 calc R . .
C413 C -0.1925(3) 0.8457(3) 0.39031(18) 0.0704(10) Uani 1 1 d . . .
H41A H -0.2488 0.8634 0.3556 0.106 Uiso 1 1 calc R . .
H41B H -0.2452 0.8431 0.4330 0.106 Uiso 1 1 calc R . .
H41C H -0.1407 0.7750 0.3878 0.106 Uiso 1 1 calc R . .
C430 C 0.0415(3) 1.0964(2) 0.14364(15) 0.0496(7) Uani 1 1 d . . .
C431 C 0.1694(3) 1.1404(3) 0.1285(2) 0.0861(13) Uani 1 1 d . . .
H43G H 0.1845 1.1716 0.1656 0.129 Uiso 1 1 calc R . .
H43H H 0.1678 1.1966 0.0895 0.129 Uiso 1 1 calc R . .
H43I H 0.2386 1.0815 0.1206 0.129 Uiso 1 1 calc R . .
C432 C 0.0160(4) 1.0479(3) 0.08544(16) 0.0695(10) Uani 1 1 d . . .
H43D H 0.0079 1.1054 0.0473 0.104 Uiso 1 1 calc R . .
H43E H -0.0640 1.0150 0.0968 0.104 Uiso 1 1 calc R . .
H43F H 0.0880 0.9924 0.0752 0.104 Uiso 1 1 calc R . .
C433 C -0.0684(3) 1.1873(2) 0.15557(19) 0.0704(10) Uani 1 1 d . . .
H43A H -0.0541 1.2196 0.1924 0.106 Uiso 1 1 calc R . .
H43B H -0.1506 1.1576 0.1656 0.106 Uiso 1 1 calc R . .
H43C H -0.0708 1.2431 0.1163 0.106 Uiso 1 1 calc R . .
C510 C 0.0034(2) 0.4460(2) 0.35284(12) 0.0368(6) Uani 1 1 d . . .
C511 C -0.0225(3) 0.3392(2) 0.33668(16) 0.0605(8) Uani 1 1 d . . .
H51G H -0.0530 0.2925 0.3770 0.091 Uiso 1 1 calc R . .
H51H H 0.0573 0.3026 0.3160 0.091 Uiso 1 1 calc R . .
H51I H -0.0884 0.3539 0.3067 0.091 Uiso 1 1 calc R . .
C512 C 0.1035(3) 0.4230(3) 0.40078(16) 0.0662(10) Uani 1 1 d . . .
H51D H 0.0740 0.3725 0.4395 0.099 Uiso 1 1 calc R . .
H51E H 0.1150 0.4910 0.4138 0.099 Uiso 1 1 calc R . .
H51F H 0.1858 0.3909 0.3798 0.099 Uiso 1 1 calc R . .
C513 C -0.1230(3) 0.5029(2) 0.38366(15) 0.0531(7) Uani 1 1 d . . .
H51A H -0.1573 0.4548 0.4225 0.080 Uiso 1 1 calc R . .
H51B H -0.1857 0.5204 0.3520 0.080 Uiso 1 1 calc R . .
H51C H -0.1069 0.5698 0.3963 0.080 Uiso 1 1 calc R . .
C530 C 0.0475(3) 0.5631(2) 0.10507(13) 0.0433(6) Uani 1 1 d . . .
C531 C 0.1664(5) 0.4966(5) 0.0810(2) 0.150(3) Uani 1 1 d . . .
H53G H 0.2407 0.5352 0.0791 0.224 Uiso 1 1 calc R . .
H53H H 0.1592 0.4833 0.0372 0.224 Uiso 1 1 calc R . .
H53I H 0.1781 0.4272 0.1107 0.224 Uiso 1 1 calc R . .
C532 C -0.0721(5) 0.5049(4) 0.10891(19) 0.0991(16) Uani 1 1 d . . .
H53D H -0.0808 0.4916 0.0653 0.149 Uiso 1 1 calc R . .
H53E H -0.1494 0.5505 0.1250 0.149 Uiso 1 1 calc R . .
H53F H -0.0619 0.4356 0.1389 0.149 Uiso 1 1 calc R . .
C533 C 0.0176(5) 0.6678(3) 0.05999(16) 0.0852(13) Uani 1 1 d . . .
H53A H 0.0899 0.7100 0.0542 0.128 Uiso 1 1 calc R . .
H53B H -0.0607 0.7091 0.0787 0.128 Uiso 1 1 calc R . .
H53C H 0.0042 0.6527 0.0175 0.128 Uiso 1 1 calc R . .
C610 C 0.3894(2) 0.92107(18) 0.35829(11) 0.0277(5) Uani 1 1 d . . .
C611 C 0.4461(3) 0.9515(2) 0.40617(13) 0.0455(7) Uani 1 1 d . . .
H61E H 0.5174 0.9060 0.4236 0.055 Uiso 1 1 calc R . .
C612 C 0.3991(3) 1.0493(2) 0.42916(15) 0.0581(8) Uani 1 1 d . . .
H61B H 0.4389 1.0700 0.4618 0.070 Uiso 1 1 calc R . .
C613 C 0.2949(3) 1.1153(2) 0.40421(14) 0.0494(7) Uani 1 1 d . . .
H61F H 0.2628 1.1815 0.4196 0.059 Uiso 1 1 calc R . .
C614 C 0.2380(3) 1.0851(2) 0.35717(16) 0.0493(7) Uani 1 1 d . . .
H61D H 0.1659 1.1302 0.3403 0.059 Uiso 1 1 calc R . .
C615 C 0.2850(2) 0.9883(2) 0.33364(13) 0.0390(6) Uani 1 1 d . . .
H61C H 0.2453 0.9686 0.3006 0.047 Uiso 1 1 calc R . .
C620 C 0.4370(2) 0.68830(18) 0.43970(11) 0.0306(5) Uani 1 1 d . . .
C621 C 0.3510(3) 0.7191(2) 0.49185(12) 0.0422(6) Uani 1 1 d . . .
H62C H 0.2656 0.7514 0.4852 0.051 Uiso 1 1 calc R . .
C622 C 0.3900(3) 0.7026(3) 0.55342(13) 0.0525(7) Uani 1 1 d . . .
H62E H 0.3306 0.7229 0.5890 0.063 Uiso 1 1 calc R . .
C623 C 0.5139(3) 0.6571(3) 0.56386(14) 0.0565(8) Uani 1 1 d . . .
H62D H 0.5405 0.6482 0.6060 0.068 Uiso 1 1 calc R . .
C624 C 0.5988(3) 0.6245(3) 0.51258(15) 0.0633(9) Uani 1 1 d . . .
H62F H 0.6837 0.5913 0.5196 0.076 Uiso 1 1 calc R . .
C625 C 0.5603(3) 0.6402(2) 0.45098(13) 0.0483(7) Uani 1 1 d . . .
H62B H 0.6193 0.6176 0.4158 0.058 Uiso 1 1 calc R . .
C730 C 0.5888(3) 0.3723(2) 0.15923(14) 0.0481(7) Uani 1 1 d . . .
H73A H 0.5293 0.3694 0.1282 0.072 Uiso 1 1 calc R . .
H73B H 0.6259 0.2985 0.1766 0.072 Uiso 1 1 calc R . .
H73C H 0.6581 0.4140 0.1369 0.072 Uiso 1 1 calc R . .

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
Pr 0.02935(7) 0.03626(8) 0.02241(7) -0.00966(5) 0.00162(4) -0.00841(5)
O31 0.0413(9) 0.0335(9) 0.0274(8) -0.0026(7) 0.0069(7) 0.0012(7)
C31 0.0320(12) 0.0378(13) 0.0235(11) -0.0044(10) 0.0001(9) -0.0041(10)
C32 0.0362(13) 0.0364(13) 0.0259(11) -0.0051(10) 0.0016(9) 0.0012(10)
O33 0.0417(9) 0.0377(9) 0.0229(8) -0.0021(7) 0.0025(7) -0.0043(8)
C33 0.0307(12) 0.0315(12) 0.0285(11) -0.0054(9) -0.0048(9) -0.0031(10)
O41 0.0645(13) 0.0383(11) 0.0501(11) -0.0126(9) 0.0293(10) -0.0099(10)
C41 0.0384(14) 0.0395(15) 0.0578(17) -0.0259(13) 0.0193(12) -0.0161(12)
C42 0.0332(13) 0.0385(15) 0.0575(17) -0.0207(13) 0.0081(12) -0.0074(11)
O43 0.0396(10) 0.0413(10) 0.0357(9) -0.0089(8) 0.0029(7) 0.0026(8)
C43 0.0292(12) 0.0385(14) 0.0504(15) -0.0150(12) -0.0005(11) -0.0079(11)
O51 0.0484(10) 0.0397(10) 0.0272(8) -0.0038(7) 0.0023(7) -0.0162(8)
C51 0.0237(11) 0.0279(12) 0.0385(13) -0.0018(10) -0.0029(9) 0.0005(9)
C52 0.0351(13) 0.0268(12) 0.0436(14) -0.0070(10) -0.0076(10) -0.0044(10)
O53 0.0563(11) 0.0356(10) 0.0284(9) -0.0037(7) -0.0110(8) -0.0136(8)
C53 0.0319(12) 0.0314(13) 0.0344(12) -0.0093(10) -0.0095(10) -0.0006(10)
O61 0.0288(8) 0.0393(9) 0.0212(8) -0.0035(7) 0.0021(6) -0.0124(7)
C61 0.0222(10) 0.0325(12) 0.0246(11) -0.0071(9) -0.0003(8) -0.0047(9)
O62 0.0316(9) 0.0437(10) 0.0292(9) -0.0087(7) -0.0005(7) -0.0128(8)
C62 0.0253(11) 0.0279(11) 0.0285(11) -0.0061(9) -0.0011(9) -0.0027(9)
O70 0.0370(10) 0.0470(11) 0.0450(10) -0.0048(8) 0.0079(8) -0.0163(8)
C71 0.105(3) 0.0347(16) 0.067(2) 0.0022(15) 0.021(2) -0.0177(18)
C72 0.069(2) 0.062(2) 0.0505(18) 0.0050(15) -0.0008(15) -0.0409(17)
C73 0.0336(14) 0.087(2) 0.0466(16) -0.0130(16) 0.0044(12) -0.0092(15)
C74 0.0469(18) 0.074(2) 0.069(2) -0.0168(18) 0.0022(15) 0.0178(17)
C310 0.0434(14) 0.0435(15) 0.0241(12) 0.0002(10) 0.0063(10) -0.0021(12)
C311 0.098(3) 0.060(2) 0.0311(15) -0.0082(14) 0.0212(16) -0.0094(18)
C312 0.154(4) 0.085(3) 0.0465(19) -0.0123(18) 0.031(2) -0.072(3)
C313 0.070(2) 0.206(5) 0.0389(19) 0.052(3) 0.0090(17) 0.044(3)
C330 0.0375(13) 0.0354(13) 0.0334(13) -0.0013(10) -0.0066(10) -0.0018(11)
C331 0.0463(16) 0.0498(17) 0.0471(16) 0.0037(13) -0.0176(13) -0.0051(13)
C332 0.0458(15) 0.0361(15) 0.0529(17) 0.0008(12) -0.0028(13) -0.0073(12)
C410 0.0534(17) 0.0521(17) 0.0613(19) -0.0290(15) 0.0293(15) -0.0182(14)
C411 0.127(4) 0.061(2) 0.114(3) -0.038(2) 0.077(3) -0.007(2)
C412 0.077(3) 0.154(4) 0.058(2) -0.048(3) 0.028(2) -0.034(3)
C413 0.061(2) 0.073(2) 0.078(2) -0.0302(19) 0.0342(18) -0.0328(18)
C430 0.0400(15) 0.0395(15) 0.0644(19) -0.0036(14) 0.0007(13) -0.0029(12)
C431 0.0488(19) 0.078(3) 0.117(3) 0.024(2) 0.001(2) -0.0247(18)
C432 0.084(3) 0.061(2) 0.055(2) 0.0035(16) -0.0114(18) 0.0039(19)
C433 0.058(2) 0.0403(17) 0.100(3) 0.0015(17) 0.0055(19) 0.0019(15)
C510 0.0292(12) 0.0331(13) 0.0424(14) 0.0063(11) -0.0025(10) -0.0038(10)
C511 0.072(2) 0.0335(15) 0.068(2) 0.0045(14) 0.0027(17) -0.0106(15)
C512 0.0521(18) 0.080(2) 0.058(2) 0.0304(17) -0.0188(15) -0.0207(17)
C513 0.0470(16) 0.0459(16) 0.0541(17) 0.0050(14) 0.0118(13) -0.0023(13)
C530 0.0532(16) 0.0439(15) 0.0381(14) -0.0177(12) -0.0116(12) -0.0039(13)
C531 0.107(4) 0.254(7) 0.104(4) -0.134(4) -0.050(3) 0.088(4)
C532 0.146(4) 0.115(4) 0.063(2) -0.019(2) -0.033(3) -0.073(3)
C533 0.147(4) 0.079(3) 0.0406(18) -0.0073(17) -0.041(2) -0.023(3)
C610 0.0268(11) 0.0274(11) 0.0273(11) -0.0039(9) 0.0043(9) -0.0062(9)
C611 0.0572(17) 0.0390(15) 0.0430(15) -0.0138(12) -0.0189(13) 0.0056(13)
C612 0.088(2) 0.0450(17) 0.0475(17) -0.0219(14) -0.0183(16) -0.0010(16)
C613 0.0626(18) 0.0302(14) 0.0499(16) -0.0112(12) 0.0084(14) 0.0011(13)
C614 0.0400(15) 0.0322(14) 0.072(2) -0.0083(13) -0.0035(14) 0.0030(12)
C615 0.0346(13) 0.0330(13) 0.0512(15) -0.0090(11) -0.0087(11) -0.0043(11)
C620 0.0339(12) 0.0286(12) 0.0278(11) -0.0002(9) -0.0019(9) -0.0067(10)
C621 0.0403(14) 0.0526(16) 0.0318(13) -0.0062(12) -0.0020(11) -0.0034(12)
C622 0.0614(19) 0.068(2) 0.0284(13) -0.0070(13) 0.0014(12) -0.0165(16)
C623 0.0623(19) 0.076(2) 0.0323(14) 0.0055(14) -0.0154(13) -0.0210(17)
C624 0.0457(17) 0.094(3) 0.0455(17) 0.0025(17) -0.0168(14) -0.0010(17)
C625 0.0389(14) 0.0632(19) 0.0369(14) -0.0017(13) -0.0058(11) 0.0042(13)
C730 0.0535(17) 0.0381(15) 0.0482(16) -0.0086(12) -0.0024(13) 0.0055(13)

_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
Pr O53 2.3676(17) . y
Pr O43 2.3966(18) . y
Pr O31 2.4054(16) . y
Pr O51 2.4066(17) . y
Pr O33 2.4165(17) . y
Pr O41 2.4333(17) . y
Pr O61 2.5785(16) . y
Pr O62 2.6507(18) . y
O31 C31 1.264(3) . ?
C31 C32 1.402(3) . ?
C31 C310 1.541(3) . ?
C32 C33 1.399(3) . ?
O33 C33 1.273(3) . ?
C33 C330 1.539(3) . ?
O41 C41 1.263(3) . ?
C41 C42 1.389(4) . ?
C41 C410 1.547(4) . ?
C42 C43 1.405(3) . ?
O43 C43 1.270(3) . ?
C43 C430 1.544(4) . ?
O51 C51 1.264(3) . ?
C51 C52 1.398(3) . ?
C51 C510 1.546(3) . ?
C52 C53 1.396(3) . ?
O53 C53 1.262(3) . ?
C53 C530 1.545(3) . ?
O61 C61 1.442(3) . y
C61 C610 1.526(3) . ?
C61 C62 1.534(3) . ?
O62 C62 1.438(3) . y
C62 C620 1.510(3) . ?
O70 C72 1.410(3) . ?
O70 C73 1.425(3) . ?
C71 C72 1.500(5) . ?
C73 C74 1.490(5) . ?
C310 C313 1.508(4) . ?
C310 C312 1.518(5) . ?
C310 C311 1.524(4) . ?
C330 C730 1.529(3) . ?
C330 C332 1.534(4) . ?
C330 C331 1.548(4) . ?
C410 C411 1.515(4) . ?
C410 C413 1.525(4) . ?
C410 C412 1.554(5) . ?
C430 C431 1.510(4) . ?
C430 C433 1.531(4) . ?
C430 C432 1.540(5) . ?
C510 C512 1.526(4) . ?
C510 C511 1.528(4) . ?
C510 C513 1.530(4) . ?
C530 C531 1.479(5) . ?
C530 C533 1.496(4) . ?
C530 C532 1.545(5) . ?
C610 C611 1.384(3) . ?
C610 C615 1.386(3) . ?
C611 C612 1.405(4) . ?
C612 C613 1.381(4) . ?
C613 C614 1.369(4) . ?
C614 C615 1.398(4) . ?
C620 C625 1.385(3) . ?
C620 C621 1.390(3) . ?
C621 C622 1.383(4) . ?
C622 C623 1.378(4) . ?
C623 C624 1.378(4) . ?
C624 C625 1.383(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
O53 Pr O43 87.67(6) . . y
O53 Pr O31 80.77(6) . . y
O43 Pr O31 78.28(6) . . y
O53 Pr O51 70.21(6) . . y
O43 Pr O51 127.57(6) . . y
O31 Pr O51 138.56(6) . . y
O53 Pr O33 88.27(6) . . y
O43 Pr O33 148.43(6) . . y
O31 Pr O33 70.17(5) . . ?
O51 Pr O33 79.79(6) . . ?
O53 Pr O41 108.85(7) . . ?
O43 Pr O41 67.80(6) . . ?
O31 Pr O41 143.93(6) . . ?
O51 Pr O41 75.32(6) . . ?
O33 Pr O41 142.33(6) . . ?
O53 Pr O61 152.31(6) . . ?
O43 Pr O61 88.91(6) . . ?
O31 Pr O61 71.63(6) . . ?
O51 Pr O61 131.24(6) . . ?
O33 Pr O61 80.45(6) . . ?
O41 Pr O61 95.16(7) . . ?
O53 Pr O62 141.61(6) . . ?
O43 Pr O62 120.08(6) . . ?
O31 Pr O62 127.66(6) . . ?
O51 Pr O62 71.71(5) . . ?
O33 Pr O62 80.41(5) . . ?
O41 Pr O62 65.21(7) . . ?
O61 Pr O62 61.26(5) . . y
C31 O31 Pr 135.79(15) . . ?
O31 C31 C32 124.3(2) . . ?
O31 C31 C310 115.0(2) . . ?
C32 C31 C310 120.7(2) . . ?
C33 C32 C31 124.6(2) . . ?
C33 O33 Pr 135.36(14) . . ?
O33 C33 C32 124.1(2) . . ?
O33 C33 C330 115.2(2) . . ?
C32 C33 C330 120.6(2) . . ?
C41 O41 Pr 140.12(18) . . ?
O41 C41 C42 123.8(2) . . ?
O41 C41 C410 114.2(3) . . ?
C42 C41 C410 122.0(2) . . ?
C41 C42 C43 123.5(2) . . ?
C43 O43 Pr 141.30(17) . . ?
O43 C43 C42 123.3(3) . . ?
O43 C43 C430 114.7(2) . . ?
C42 C43 C430 122.0(2) . . ?
C51 O51 Pr 135.33(15) . . ?
O51 C51 C52 123.9(2) . . ?
O51 C51 C510 114.9(2) . . ?
C52 C51 C510 121.2(2) . . ?
C53 C52 C51 124.4(2) . . ?
C53 O53 Pr 135.68(15) . . ?
O53 C53 C52 124.0(2) . . ?
O53 C53 C530 115.4(2) . . ?
C52 C53 C530 120.5(2) . . ?
C61 O61 Pr 124.53(12) . . y
O61 C61 C610 110.70(18) . . ?
O61 C61 C62 104.74(17) . . ?
C610 C61 C62 117.00(17) . . ?
C62 O62 Pr 114.29(12) . . y
O62 C62 C620 114.58(18) . . ?
O62 C62 C61 108.36(17) . . ?
C620 C62 C61 112.97(18) . . ?
C72 O70 C73 113.8(2) . . ?
O70 C72 C71 109.5(2) . . ?
O70 C73 C74 109.1(2) . . ?
C313 C310 C312 110.3(3) . . ?
C313 C310 C311 109.7(3) . . ?
C312 C310 C311 108.0(3) . . ?
C313 C310 C31 107.9(2) . . ?
C312 C310 C31 107.0(2) . . ?
C311 C310 C31 113.9(2) . . ?
C730 C330 C332 109.0(2) . . ?
C730 C330 C33 114.6(2) . . ?
C332 C330 C33 108.4(2) . . ?
C730 C330 C331 108.3(2) . . ?
C332 C330 C331 109.4(2) . . ?
C33 C330 C331 107.0(2) . . ?
C411 C410 C413 109.7(3) . . ?
C411 C410 C41 114.4(3) . . ?
C413 C410 C41 106.4(2) . . ?
C411 C410 C412 110.1(3) . . ?
C413 C410 C412 107.4(3) . . ?
C41 C410 C412 108.5(3) . . ?
C431 C430 C433 110.4(3) . . ?
C431 C430 C432 110.0(3) . . ?
C433 C430 C432 108.0(3) . . ?
C431 C430 C43 107.3(3) . . ?
C433 C430 C43 113.8(2) . . ?
C432 C430 C43 107.3(2) . . ?
C512 C510 C511 109.5(2) . . ?
C512 C510 C513 109.8(3) . . ?
C511 C510 C513 108.6(2) . . ?
C512 C510 C51 108.5(2) . . ?
C511 C510 C51 113.4(2) . . ?
C513 C510 C51 106.9(2) . . ?
C531 C530 C533 112.9(4) . . ?
C531 C530 C53 107.0(2) . . ?
C533 C530 C53 110.1(2) . . ?
C531 C530 C532 111.1(4) . . ?
C533 C530 C532 103.9(3) . . ?
C53 C530 C532 112.0(2) . . ?
C611 C610 C615 118.9(2) . . ?
C611 C610 C61 119.6(2) . . ?
C615 C610 C61 121.4(2) . . ?
C610 C611 C612 120.5(3) . . ?
C613 C612 C611 119.9(3) . . ?
C614 C613 C612 119.7(2) . . ?
C613 C614 C615 120.7(3) . . ?
C610 C615 C614 120.3(2) . . ?
C625 C620 C621 118.8(2) . . ?
C625 C620 C62 118.0(2) . . ?
C621 C620 C62 123.1(2) . . ?
C622 C621 C620 119.8(3) . . ?
C623 C622 C621 121.0(3) . . ?
C622 C623 C624 119.4(3) . . ?
C623 C624 C625 119.9(3) . . ?
C624 C625 C620 121.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.891
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.08
_refine_diff_density_min         -0.55
_refine_diff_density_rms         0.07

#===END of CIF