#------------------------------------------------------------------------------
#$Date: 2023-10-06 03:30:40 +0300 (Fri, 06 Oct 2023) $
#$Revision: 286767 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/26/7062636.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7062636
loop_
_publ_author_name
'Moon, Josh'
'Guo, Zhifang'
'Beaumont, Owen A.'
'Hamilton, Sophie'
'Bousrez, Guillaume'
'Mottram, Eleanor'
'Wang, Jun'
'Somers, Anthony E.'
'Deacon, Glen B.'
'Junk, Peter C.'
_publ_section_title
;
 4-Hydroxybenzoato-rare earth(iii) complexes -- syntheses, a structural
 goldmine from coordination diversity and improved corrosion inhibition
 behaviour
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16843
_journal_page_last               16854
_journal_paper_doi               10.1039/D3NJ02735J
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C84 H76 O44 Pr4, 4(H2 O)'
_chemical_formula_sum            'C84 H84 O48 Pr4'
_chemical_formula_weight         2425.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-04-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-12 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                93.1860(10)
_cell_angle_beta                 102.7450(10)
_cell_angle_gamma                105.5620(10)
_cell_formula_units_Z            1
_cell_length_a                   12.0467(3)
_cell_length_b                   14.1840(4)
_cell_length_c                   14.6821(4)
_cell_measurement_reflns_used    7595
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.85
_cell_measurement_theta_min      2.30
_cell_volume                     2339.57(11)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51444
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.068
_diffrn_reflns_theta_min         1.433
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4282
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.849
_refine_diff_density_min         -1.579
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0217(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         13334
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0379P)²+0.2115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10968
_reflns_number_total             13334
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj02735j2.cif
_cod_data_source_block           p1
_cod_depositor_comments
'Adding full bibliography for 7062632--7062650.cif.'
_cod_database_code               7062636
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.674
_olex2_refinement_description
;
1. Restrained distances
 O24-H24A = O24-H24B
 0.85 with sigma of 0.02
 H24A-H24B
 1.34 with sigma of 0.04
 Pr2-H15A \\sim Pr2-H15B
 with sigma of 0.02
2.a Free rotating group:
 O23(H23A,H23B), O15(H15A,H15B)
2.b Rotating group:
 O16(H16A,H16B), O7(H7A,H7B), O8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C24(H24), C14(H14), C6(H6), C11(H11), C34(H34), C39(H39), C31(H31),
 C38(H38), C4(H4), C10(H10), C3(H3), C28(H28), C13(H13), C35(H35), C17(H17A),
 C20(H20A), C32(H32), C25(H25), C18(H18A), C21(H21A), C27(H27), C42(H42),
 C41(H41)
2.d Tetrahedral OH refined with riding coordinates:
 O17(H17), O21(H21)
2.e Idealised tetrahedral OH refined as rotating group:
 O18(H18), O20(H20), O22(H22), O19(H19)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.61657(2) 0.12578(2) 0.63590(2) 0.01731(5) Uani 1 1 d . . . . .
Pr2 Pr 0.79272(2) 0.40009(2) 0.81711(2) 0.01934(5) Uani 1 1 d D . . . .
O1 O 0.77813(15) 0.22987(13) 0.55501(11) 0.0247(4) Uani 1 1 d . . . . .
O2 O 0.59095(15) 0.18097(12) 0.47539(11) 0.0233(4) Uani 1 1 d . . . . .
O6 O 0.81609(16) 0.24261(12) 0.76540(11) 0.0266(4) Uani 1 1 d . . . . .
O16 O 0.87147(16) 0.41438(13) 0.66923(12) 0.0285(4) Uani 1 1 d . . . . .
H16A H 0.844823 0.455348 0.636967 0.043 Uiso 1 1 d R U . . .
H16B H 0.842821 0.359678 0.633366 0.043 Uiso 1 1 d R U . . .
O7 O 0.52080(16) -0.04095(13) 0.67687(12) 0.0297(4) Uani 1 1 d . . . . .
H7A H 0.449112 -0.045446 0.700208 0.045 Uiso 1 1 d R U . . .
H7B H 0.485780 -0.093787 0.623067 0.045 Uiso 1 1 d R U . . .
O10 O 0.58418(17) 0.40847(15) 0.76066(12) 0.0352(5) Uani 1 1 d . . . . .
O9 O 0.62248(16) 0.30589(13) 0.66386(12) 0.0270(4) Uani 1 1 d . . . . .
O18 O -0.11364(16) 0.13612(16) 0.43809(13) 0.0377(5) Uani 1 1 d . . . . .
H18 H -0.123562 0.164132 0.484730 0.057 Uiso 1 1 calc R U . . .
O11 O 0.67628(16) 0.28668(14) 0.90926(12) 0.0302(4) Uani 1 1 d . . . . .
O4 O 0.34786(17) -0.00062(14) 0.45868(13) 0.0313(4) Uani 1 1 d . . . . .
O12 O 0.86237(16) 0.35859(14) 0.98027(12) 0.0343(5) Uani 1 1 d . . . . .
O3 O 0.41026(16) 0.10907(14) 0.58544(13) 0.0310(4) Uani 1 1 d . . . . .
O8 O 0.53600(17) 0.13662(14) 0.78066(12) 0.0333(4) Uani 1 1 d . . . . .
H8A H 0.580565 0.186672 0.818713 0.050 Uiso 1 1 d R U . . .
H8B H 0.469165 0.148391 0.765303 0.050 Uiso 1 1 d R U . . .
O13 O 0.76658(18) 0.54172(13) 0.91387(12) 0.0327(4) Uani 1 1 d . . . . .
O23 O 0.6558(2) 0.48378(16) 1.05416(14) 0.0407(5) Uani 1 1 d G . . . .
H23A H 0.692689 0.513743 1.016248 0.061 Uiso 1 1 d G U . . .
H23B H 0.619079 0.522663 1.070777 0.061 Uiso 1 1 d G U . . .
O14 O 0.80713(19) 0.57203(13) 0.77806(12) 0.0386(5) Uani 1 1 d . . . . .
O20 O 0.19403(19) 0.42241(17) 0.40001(13) 0.0443(5) Uani 1 1 d . . . . .
H20 H 0.205979 0.415158 0.347560 0.066 Uiso 1 1 calc R U . . .
O17 O 0.81099(18) 0.47488(16) 0.20771(14) 0.0450(5) Uani 1 1 d . . . . .
H17 H 0.752389 0.470947 0.165146 0.067 Uiso 1 1 calc R U . . .
O5 O 0.77795(15) 0.08220(12) 0.75476(12) 0.0277(4) Uani 1 1 d . . . . .
O15 O 1.00435(17) 0.49115(16) 0.87582(13) 0.0423(5) Uani 1 1 d G . . . .
H15A H 1.057009 0.503793 0.844490 0.064 Uiso 1 1 d DG U . . .
H15B H 1.034752 0.530811 0.926282 0.064 Uiso 1 1 d DG U . . .
O24 O 0.46591(19) 0.38750(19) 0.89683(15) 0.0475(6) Uani 1 1 d D . . . .
H24A H 0.499(3) 0.409(3) 0.8543(18) 0.071 Uiso 1 1 d D U . . .
H24B H 0.521(3) 0.394(3) 0.9449(17) 0.071 Uiso 1 1 d D U . . .
O22 O 0.6717(2) 0.96066(16) 0.88114(16) 0.0517(6) Uani 1 1 d . . . . .
H22 H 0.700354 0.997985 0.846242 0.077 Uiso 1 1 calc R U . . .
O19 O 1.33852(18) 0.19423(17) 0.84095(17) 0.0491(6) Uani 1 1 d . . . . .
H19 H 1.379875 0.251443 0.857054 0.074 Uiso 1 1 calc R U . . .
O21 O 0.70534(18) 0.06389(15) 1.27246(13) 0.0411(5) Uani 1 1 d . . . . .
H21 H 0.763602 0.080994 1.317334 0.062 Uiso 1 1 calc R U . . .
C9 C 0.2173(2) 0.08750(17) 0.49244(16) 0.0216(5) Uani 1 1 d . . . . .
C2 C 0.7259(2) 0.29546(18) 0.40946(16) 0.0237(5) Uani 1 1 d . . . . .
C22 C 0.5590(2) 0.36047(18) 0.67976(17) 0.0237(5) Uani 1 1 d . . . . .
C15 C 0.8530(2) 0.16594(18) 0.77402(16) 0.0223(5) Uani 1 1 d . . . . .
C7 C 0.6374(2) 0.29814(18) 0.33174(17) 0.0267(5) Uani 1 1 d . . . . .
H7 H 0.559689 0.260001 0.325959 0.032 Uiso 1 1 calc R U . . .
C8 C 0.3321(2) 0.06344(18) 0.51314(16) 0.0223(5) Uani 1 1 d . . . . .
C24 C 0.4518(3) 0.3449(2) 0.51149(17) 0.0351(7) Uani 1 1 d . . . . .
H24 H 0.504568 0.313571 0.495180 0.042 Uiso 1 1 calc R U . . .
C30 C 0.7527(2) 0.23312(19) 1.05527(17) 0.0283(6) Uani 1 1 d . . . . .
C29 C 0.7651(2) 0.29537(18) 0.97838(16) 0.0248(5) Uani 1 1 d . . . . .
C14 C 0.1920(2) 0.1501(2) 0.55639(18) 0.0309(6) Uani 1 1 d . . . . .
H14 H 0.249340 0.179861 0.611288 0.037 Uiso 1 1 calc R U . . .
C6 C 0.6637(2) 0.35672(19) 0.26311(17) 0.0293(6) Uani 1 1 d . . . . .
H6 H 0.604048 0.358216 0.211255 0.035 Uiso 1 1 calc R U . . .
C1 C 0.6963(2) 0.23189(17) 0.48305(15) 0.0207(5) Uani 1 1 d . . . . .
C16 C 0.9809(2) 0.17644(18) 0.79735(17) 0.0251(5) Uani 1 1 d . . . . .
C11 C 0.0224(2) 0.0637(2) 0.39250(18) 0.0310(6) Uani 1 1 d . . . . .
H11 H -0.034349 0.035452 0.336868 0.037 Uiso 1 1 calc R U . . .
C12 C -0.0023(2) 0.12431(19) 0.45768(17) 0.0262(5) Uani 1 1 d . . . . .
C36 C 0.7766(2) 0.59910(18) 0.85055(17) 0.0283(6) Uani 1 1 d . . . . .
C23 C 0.4617(2) 0.37360(18) 0.60518(16) 0.0235(5) Uani 1 1 d . . . . .
C34 C 0.8343(2) 0.1854(2) 1.20404(18) 0.0354(7) Uani 1 1 d . . . . .
H34 H 0.898539 0.191751 1.254888 0.043 Uiso 1 1 calc R U . . .
C26 C 0.2841(2) 0.4056(2) 0.46567(17) 0.0303(6) Uani 1 1 d . . . . .
C39 C 0.7529(3) 0.8516(2) 0.8026(2) 0.0400(7) Uani 1 1 d . . . . .
H39 H 0.772017 0.896281 0.760496 0.048 Uiso 1 1 calc R U . . .
C31 C 0.6444(3) 0.1653(2) 1.05295(19) 0.0395(7) Uani 1 1 d . . . . .
H31 H 0.580360 0.157968 1.001688 0.047 Uiso 1 1 calc R U . . .
C37 C 0.7505(3) 0.69462(19) 0.85854(17) 0.0307(6) Uani 1 1 d . . . . .
C38 C 0.7795(3) 0.7631(2) 0.79700(19) 0.0368(7) Uani 1 1 d . . . . .
H38 H 0.817383 0.749018 0.751428 0.044 Uiso 1 1 calc R U . . .
C33 C 0.7258(3) 0.1202(2) 1.20158(18) 0.0318(6) Uani 1 1 d . . . . .
C4 C 0.8684(2) 0.4113(2) 0.34821(19) 0.0329(6) Uani 1 1 d . . . . .
H4 H 0.946015 0.449396 0.353323 0.039 Uiso 1 1 calc R U . . .
C10 C 0.1313(2) 0.0453(2) 0.41036(17) 0.0290(6) Uani 1 1 d . . . . .
H10 H 0.147305 0.004039 0.366704 0.035 Uiso 1 1 calc R U . . .
C3 C 0.8422(2) 0.35242(19) 0.41714(18) 0.0291(6) Uani 1 1 d . . . . .
H3 H 0.902218 0.350892 0.468661 0.035 Uiso 1 1 calc R U . . .
C28 C 0.3809(3) 0.4189(2) 0.62777(19) 0.0392(7) Uani 1 1 d . . . . .
H28 H 0.386854 0.439186 0.690424 0.047 Uiso 1 1 calc R U . . .
C13 C 0.0827(2) 0.1685(2) 0.53918(18) 0.0336(6) Uani 1 1 d . . . . .
H13 H 0.066559 0.210299 0.582253 0.040 Uiso 1 1 calc R U . . .
C35 C 0.8479(2) 0.2415(2) 1.13096(18) 0.0337(6) Uani 1 1 d . . . . .
H35 H 0.921566 0.285083 1.132722 0.040 Uiso 1 1 calc R U . . .
C17 C 1.0626(2) 0.2638(2) 0.78901(19) 0.0330(6) Uani 1 1 d . . . . .
H17A H 1.036759 0.318436 0.773810 0.040 Uiso 1 1 calc R U . . .
C20 C 1.1425(3) 0.1035(2) 0.8368(2) 0.0405(7) Uani 1 1 d . . . . .
H20A H 1.169676 0.050010 0.853959 0.049 Uiso 1 1 calc R U . . .
C32 C 0.6302(3) 0.1087(2) 1.1251(2) 0.0430(8) Uani 1 1 d . . . . .
H32 H 0.557349 0.063318 1.122537 0.052 Uiso 1 1 calc R U . . .
C25 C 0.3647(3) 0.3623(2) 0.44216(19) 0.0407(7) Uani 1 1 d . . . . .
H25 H 0.360384 0.344668 0.379238 0.049 Uiso 1 1 calc R U . . .
C5 C 0.7791(3) 0.4131(2) 0.27192(18) 0.0301(6) Uani 1 1 d . . . . .
C18 C 1.1806(3) 0.2702(2) 0.8029(2) 0.0375(7) Uani 1 1 d . . . . .
H18A H 1.233966 0.328902 0.796359 0.045 Uiso 1 1 calc R U . . .
C40 C 0.6982(3) 0.8741(2) 0.87029(19) 0.0366(7) Uani 1 1 d . . . . .
C21 C 1.0230(3) 0.0962(2) 0.8215(2) 0.0357(7) Uani 1 1 d . . . . .
H21A H 0.969880 0.037091 0.827280 0.043 Uiso 1 1 calc R U . . .
C27 C 0.2925(3) 0.4340(2) 0.55887(19) 0.0448(8) Uani 1 1 d . . . . .
H27 H 0.238104 0.463480 0.574966 0.054 Uiso 1 1 calc R U . . .
C19 C 1.2212(2) 0.1906(2) 0.82668(19) 0.0363(7) Uani 1 1 d . . . . .
C42 C 0.6944(3) 0.7180(2) 0.9258(2) 0.0448(8) Uani 1 1 d . . . . .
H42 H 0.673825 0.673115 0.967357 0.054 Uiso 1 1 calc R U . . .
C41 C 0.6687(3) 0.8068(2) 0.9320(2) 0.0483(8) Uani 1 1 d . . . . .
H41 H 0.631389 0.821520 0.977771 0.058 Uiso 1 1 calc R U . . .
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'
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
O1 Pr1 O6 67.43(5) . . ?
O2 Pr1 O1 50.36(5) . . ?
O2 Pr1 O6 113.67(5) . . ?
O2 Pr1 O7 126.79(5) . . ?
O2 Pr1 O9 75.56(5) . . ?
O2 Pr1 O8 139.10(6) . . ?
O2 Pr1 O5 137.28(6) . . ?
O7 Pr1 O1 146.09(6) . . ?
O7 Pr1 O6 117.06(5) . . ?
O7 Pr1 O9 141.29(6) . . ?
O7 Pr1 O8 67.73(6) . . ?
O7 Pr1 O5 74.11(6) . . ?
O9 Pr1 O1 72.44(5) . . ?
O9 Pr1 O6 65.18(5) . . ?
O9 Pr1 O5 112.54(5) . . ?
O4 Pr1 O1 77.90(6) 2_656 . ?
O4 Pr1 O2 75.72(6) 2_656 . ?
O4 Pr1 O6 114.50(6) 2_656 . ?
O4 Pr1 O7 69.82(6) 2_656 . ?
O4 Pr1 O9 147.66(6) 2_656 . ?
O4 Pr1 O8 136.76(6) 2_656 . ?
O4 Pr1 O5 79.93(6) 2_656 . ?
O3 Pr1 O1 123.59(6) . . ?
O3 Pr1 O2 75.50(6) . . ?
O3 Pr1 O6 139.52(6) . . ?
O3 Pr1 O7 76.56(6) . . ?
O3 Pr1 O9 80.77(6) . . ?
O3 Pr1 O4 105.98(6) . 2_656 ?
O3 Pr1 O8 71.78(6) . . ?
O3 Pr1 O5 145.79(6) . . ?
O8 Pr1 O1 140.70(6) . . ?
O8 Pr1 O6 78.79(6) . . ?
O8 Pr1 O9 75.58(6) . . ?
O8 Pr1 O5 81.04(6) . . ?
O5 Pr1 O1 90.62(5) . . ?
O5 Pr1 O6 48.44(5) . . ?
O6 Pr2 O16 70.67(6) . . ?
O6 Pr2 O10 112.51(6) . . ?
O6 Pr2 O9 67.94(6) . . ?
O6 Pr2 O11 78.27(6) . . ?
O6 Pr2 O12 84.89(6) . . ?
O6 Pr2 O13 163.54(6) . . ?
O6 Pr2 O14 144.45(6) . . ?
O6 Pr2 O15 98.25(7) . . ?
O16 Pr2 O9 68.84(5) . . ?
O10 Pr2 O16 103.21(6) . . ?
O10 Pr2 O9 49.63(6) . . ?
O10 Pr2 O12 120.02(6) . . ?
O10 Pr2 O13 71.27(6) . . ?
O10 Pr2 O14 73.35(7) . . ?
O11 Pr2 O16 145.73(6) . . ?
O11 Pr2 O10 75.36(6) . . ?
O11 Pr2 O9 86.51(6) . . ?
O11 Pr2 O12 51.67(6) . . ?
O11 Pr2 O13 87.62(6) . . ?
O11 Pr2 O14 134.77(6) . . ?
O12 Pr2 O16 136.03(6) . . ?
O12 Pr2 O9 134.61(6) . . ?
O12 Pr2 O13 79.68(6) . . ?
O13 Pr2 O16 124.98(6) . . ?
O13 Pr2 O9 120.09(6) . . ?
O14 Pr2 O16 73.86(6) . . ?
O14 Pr2 O9 97.09(6) . . ?
O14 Pr2 O12 123.89(6) . . ?
O14 Pr2 O13 51.71(5) . . ?
O15 Pr2 O16 75.91(6) . . ?
O15 Pr2 O10 147.26(7) . . ?
O15 Pr2 O9 144.65(6) . . ?
O15 Pr2 O11 123.73(6) . . ?
O15 Pr2 O12 72.06(6) . . ?
O15 Pr2 O13 82.47(7) . . ?
O15 Pr2 O14 75.11(8) . . ?
C1 O1 Pr1 90.65(13) . . ?
C1 O2 Pr1 98.37(14) . . ?
Pr2 O6 Pr1 112.47(6) . . ?
C15 O6 Pr1 87.75(14) . . ?
C15 O6 Pr2 155.95(15) . . ?
Pr2 O16 H16A 109.6 . . ?
Pr2 O16 H16B 109.6 . . ?
H16A O16 H16B 104.3 . . ?
Pr1 O7 H7A 114.8 . . ?
Pr1 O7 H7B 115.3 . . ?
H7A O7 H7B 98.6 . . ?
C22 O10 Pr2 98.68(15) . . ?
Pr1 O9 Pr2 111.29(6) . . ?
C22 O9 Pr1 141.87(17) . . ?
C22 O9 Pr2 90.01(14) . . ?
C12 O18 H18 109.5 . . ?
C29 O11 Pr2 94.64(14) . . ?
C8 O4 Pr1 176.40(18) . 2_656 ?
C29 O12 Pr2 94.29(14) . . ?
C8 O3 Pr1 132.29(16) . . ?
Pr1 O8 H8A 109.4 . . ?
Pr1 O8 H8B 109.4 . . ?
H8A O8 H8B 104.5 . . ?
C36 O13 Pr2 93.87(14) . . ?
H23A O23 H23B 104.4 . . ?
C36 O14 Pr2 94.79(15) . . ?
C26 O20 H20 109.5 . . ?
C5 O17 H17 109.5 . . ?
C15 O5 Pr1 98.49(14) . . ?
Pr2 O15 H15A 127.5 . . ?
Pr2 O15 H15B 125.7 . . ?
H15A O15 H15B 104.5 . . ?
H24A O24 H24B 106(3) . . ?
C40 O22 H22 109.5 . . ?
C19 O19 H19 109.5 . . ?
C33 O21 H21 109.5 . . ?
C14 C9 C8 120.8(2) . . ?
C10 C9 C8 120.5(2) . . ?
C10 C9 C14 118.6(2) . . ?
C7 C2 C1 120.1(2) . . ?
C7 C2 C3 119.2(2) . . ?
C3 C2 C1 120.7(2) . . ?
O10 C22 O9 118.7(2) . . ?
O10 C22 C23 119.5(2) . . ?
O9 C22 C23 121.7(2) . . ?
O6 C15 C16 120.0(2) . . ?
O5 C15 O6 118.7(2) . . ?
O5 C15 C16 121.0(2) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.7(2) . . ?
C6 C7 H7 119.7 . . ?
O4 C8 O3 122.8(2) . . ?
O4 C8 C9 119.4(2) . . ?
O3 C8 C9 117.8(2) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C25 C24 C23 120.6(2) . . ?
C31 C30 C29 120.4(2) . . ?
C35 C30 C29 120.9(2) . . ?
C35 C30 C31 118.6(2) . . ?
O11 C29 C30 120.0(2) . . ?
O12 C29 O11 118.8(2) . . ?
O12 C29 C30 121.2(2) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 C9 120.7(2) . . ?
C13 C14 H14 119.6 . . ?
C7 C6 H6 120.3 . . ?
C7 C6 C5 119.5(2) . . ?
C5 C6 H6 120.3 . . ?
O1 C1 C2 120.0(2) . . ?
O2 C1 O1 119.9(2) . . ?
O2 C1 C2 120.1(2) . . ?
C17 C16 C15 121.1(2) . . ?
C17 C16 C21 118.1(3) . . ?
C21 C16 C15 120.6(2) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.7(2) . . ?
O18 C12 C11 117.0(2) . . ?
O18 C12 C13 122.6(2) . . ?
C13 C12 C11 120.3(2) . . ?
O13 C36 C37 121.4(2) . . ?
O14 C36 O13 119.0(2) . . ?
O14 C36 C37 119.6(2) . . ?
C24 C23 C22 121.0(2) . . ?
C24 C23 C28 118.6(2) . . ?
C28 C23 C22 120.3(2) . . ?
C33 C34 H34 120.0 . . ?
C33 C34 C35 120.1(3) . . ?
C35 C34 H34 120.0 . . ?
O20 C26 C25 122.7(2) . . ?
O20 C26 C27 117.5(2) . . ?
C25 C26 C27 119.8(2) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C40 C39 C38 120.2(3) . . ?
C30 C31 H31 119.4 . . ?
C32 C31 C30 121.3(3) . . ?
C32 C31 H31 119.4 . . ?
C38 C37 C36 120.6(2) . . ?
C42 C37 C36 121.3(2) . . ?
C42 C37 C38 118.1(2) . . ?
C39 C38 C37 121.0(3) . . ?
C39 C38 H38 119.5 . . ?
C37 C38 H38 119.5 . . ?
O21 C33 C34 123.2(3) . . ?
O21 C33 C32 116.5(2) . . ?
C34 C33 C32 120.3(2) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C5 C4 C3 119.7(2) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 121.0(2) . . ?
C11 C10 H10 119.5 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.1(2) . . ?
C4 C3 H3 120.0 . . ?
C23 C28 H28 119.6 . . ?
C27 C28 C23 120.8(2) . . ?
C27 C28 H28 119.6 . . ?
C14 C13 H13 120.2 . . ?
C12 C13 C14 119.6(2) . . ?
C12 C13 H13 120.2 . . ?
C30 C35 H35 119.8 . . ?
C34 C35 C30 120.5(2) . . ?
C34 C35 H35 119.8 . . ?
C16 C17 H17A 119.7 . . ?
C18 C17 C16 120.7(3) . . ?
C18 C17 H17A 119.7 . . ?
C21 C20 H20A 120.2 . . ?
C19 C20 H20A 120.2 . . ?
C19 C20 C21 119.6(3) . . ?
C31 C32 C33 119.1(3) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.1(2) . . ?
C26 C25 H25 119.9 . . ?
O17 C5 C6 122.6(2) . . ?
O17 C5 C4 116.5(2) . . ?
C4 C5 C6 120.9(2) . . ?
C17 C18 H18A 119.7 . . ?
C17 C18 C19 120.7(3) . . ?
C19 C18 H18A 119.7 . . ?
O22 C40 C39 123.3(3) . . ?
O22 C40 C41 117.0(3) . . ?
C39 C40 C41 119.6(3) . . ?
C16 C21 H21A 119.5 . . ?
C20 C21 C16 121.0(3) . . ?
C20 C21 H21A 119.5 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.1(3) . . ?
C28 C27 H27 120.0 . . ?
O19 C19 C20 117.8(3) . . ?
O19 C19 C18 122.3(3) . . ?
C20 C19 C18 119.9(3) . . ?
C37 C42 H42 119.5 . . ?
C41 C42 C37 121.0(3) . . ?
C41 C42 H42 119.5 . . ?
C40 C41 H41 119.9 . . ?
C42 C41 C40 120.1(3) . . ?
C42 C41 H41 119.9 . . ?
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 O1 2.6555(16) . ?
Pr1 O2 2.5052(16) . ?
Pr1 O6 2.7630(17) . ?
Pr1 O7 2.5071(17) . ?
Pr1 O9 2.5443(17) . ?
Pr1 O4 2.3791(18) 2_656 ?
Pr1 O3 2.3736(18) . ?
Pr1 O8 2.5372(17) . ?
Pr1 O5 2.5446(17) . ?
Pr2 O6 2.4267(16) . ?
Pr2 O16 2.5515(16) . ?
Pr2 O10 2.5030(19) . ?
Pr2 O9 2.6858(17) . ?
Pr2 O11 2.5008(17) . ?
Pr2 O12 2.5147(17) . ?
Pr2 O13 2.5243(17) . ?
Pr2 O14 2.5056(18) . ?
Pr2 O15 2.4598(19) . ?
O1 C1 1.283(3) . ?
O2 C1 1.258(3) . ?
O6 C15 1.283(3) . ?
O16 H16A 0.8536 . ?
O16 H16B 0.8538 . ?
O7 H7A 0.9853 . ?
O7 H7B 0.9905 . ?
O10 C22 1.267(3) . ?
O9 C22 1.271(3) . ?
O18 H18 0.8200 . ?
O18 C12 1.366(3) . ?
O11 C29 1.275(3) . ?
O4 C8 1.257(3) . ?
O12 C29 1.264(3) . ?
O3 C8 1.260(3) . ?
O8 H8A 0.8505 . ?
O8 H8B 0.8503 . ?
O13 C36 1.274(3) . ?
O23 H23A 0.8496 . ?
O23 H23B 0.8504 . ?
O14 C36 1.272(3) . ?
O20 H20 0.8200 . ?
O20 C26 1.366(3) . ?
O17 H17 0.8200 . ?
O17 C5 1.369(3) . ?
O5 C15 1.258(3) . ?
O15 H15A 0.8503 . ?
O15 H15B 0.8502 . ?
O24 H24A 0.842(17) . ?
O24 H24B 0.834(18) . ?
O22 H22 0.8200 . ?
O22 C40 1.360(3) . ?
O19 H19 0.8200 . ?
O19 C19 1.368(3) . ?
O21 H21 0.8200 . ?
O21 C33 1.372(3) . ?
C9 C8 1.483(3) . ?
C9 C14 1.393(3) . ?
C9 C10 1.386(3) . ?
C2 C7 1.389(3) . ?
C2 C1 1.488(3) . ?
C2 C3 1.393(4) . ?
C22 C23 1.477(3) . ?
C15 C16 1.467(4) . ?
C7 H7 0.9300 . ?
C7 C6 1.378(3) . ?
C24 H24 0.9300 . ?
C24 C23 1.383(3) . ?
C24 C25 1.377(4) . ?
C30 C29 1.480(3) . ?
C30 C31 1.390(4) . ?
C30 C35 1.384(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.382(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.379(4) . ?
C16 C17 1.391(4) . ?
C16 C21 1.398(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.384(3) . ?
C11 C10 1.377(4) . ?
C12 C13 1.380(3) . ?
C36 C37 1.475(4) . ?
C23 C28 1.387(4) . ?
C34 H34 0.9300 . ?
C34 C33 1.375(4) . ?
C34 C35 1.383(3) . ?
C26 C25 1.372(4) . ?
C26 C27 1.379(4) . ?
C39 H39 0.9300 . ?
C39 C38 1.379(4) . ?
C39 C40 1.374(4) . ?
C31 H31 0.9300 . ?
C31 C32 1.377(4) . ?
C37 C38 1.392(3) . ?
C37 C42 1.385(4) . ?
C38 H38 0.9300 . ?
C33 C32 1.387(4) . ?
C4 H4 0.9300 . ?
C4 C3 1.384(3) . ?
C4 C5 1.378(4) . ?
C10 H10 0.9300 . ?
C3 H3 0.9300 . ?
C28 H28 0.9300 . ?
C28 C27 1.369(4) . ?
C13 H13 0.9300 . ?
C35 H35 0.9300 . ?
C17 H17A 0.9300 . ?
C17 C18 1.367(4) . ?
C20 H20A 0.9300 . ?
C20 C21 1.381(4) . ?
C20 C19 1.379(4) . ?
C32 H32 0.9300 . ?
C25 H25 0.9300 . ?
C18 H18A 0.9300 . ?
C18 C19 1.379(4) . ?
C40 C41 1.383(4) . ?
C21 H21A 0.9300 . ?
C27 H27 0.9300 . ?
C42 H42 0.9300 . ?
C42 C41 1.378(4) . ?
C41 H41 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pr1 O1 C1 O2 -8.1(2) . . . . ?
Pr1 O1 C1 C2 171.04(19) . . . . ?
Pr1 O2 C1 O1 8.7(2) . . . . ?
Pr1 O2 C1 C2 -170.45(18) . . . . ?
Pr1 O6 C15 O5 -24.8(2) . . . . ?
Pr1 O6 C15 C16 149.6(2) . . . . ?
Pr1 O9 C22 O10 109.3(3) . . . . ?
Pr1 O9 C22 C23 -74.2(3) . . . . ?
Pr1 O3 C8 O4 14.1(4) . . . . ?
Pr1 O3 C8 C9 -165.71(15) . . . . ?
Pr1 O5 C15 O6 27.4(2) . . . . ?
Pr1 O5 C15 C16 -146.95(19) . . . . ?
Pr2 O6 C15 O5 123.5(4) . . . . ?
Pr2 O6 C15 C16 -62.1(5) . . . . ?
Pr2 O10 C22 O9 18.2(3) . . . . ?
Pr2 O10 C22 C23 -158.37(19) . . . . ?
Pr2 O9 C22 O10 -16.7(2) . . . . ?
Pr2 O9 C22 C23 159.8(2) . . . . ?
Pr2 O11 C29 O12 7.8(2) . . . . ?
Pr2 O11 C29 C30 -173.2(2) . . . . ?
Pr2 O12 C29 O11 -7.7(2) . . . . ?
Pr2 O12 C29 C30 173.3(2) . . . . ?
Pr2 O13 C36 O14 -8.0(3) . . . . ?
Pr2 O13 C36 C37 170.3(2) . . . . ?
Pr2 O14 C36 O13 8.1(3) . . . . ?
Pr2 O14 C36 C37 -170.3(2) . . . . ?
O6 C15 C16 C17 -15.2(4) . . . . ?
O6 C15 C16 C21 169.9(2) . . . . ?
O10 C22 C23 C24 162.3(3) . . . . ?
O10 C22 C23 C28 -15.0(4) . . . . ?
O9 C22 C23 C24 -14.1(4) . . . . ?
O9 C22 C23 C28 168.5(3) . . . . ?
O18 C12 C13 C14 177.3(3) . . . . ?
O13 C36 C37 C38 169.8(3) . . . . ?
O13 C36 C37 C42 -11.6(4) . . . . ?
O14 C36 C37 C38 -11.9(4) . . . . ?
O14 C36 C37 C42 166.8(3) . . . . ?
O20 C26 C25 C24 -178.3(3) . . . . ?
O20 C26 C27 C28 179.9(3) . . . . ?
O5 C15 C16 C17 159.1(2) . . . . ?
O5 C15 C16 C21 -15.9(4) . . . . ?
O22 C40 C41 C42 -179.2(3) . . . . ?
O21 C33 C32 C31 178.2(3) . . . . ?
C9 C14 C13 C12 0.0(4) . . . . ?
C2 C7 C6 C5 0.0(4) . . . . ?
C22 C23 C28 C27 178.0(3) . . . . ?
C15 C16 C17 C18 -174.3(2) . . . . ?
C15 C16 C21 C20 175.2(3) . . . . ?
C7 C2 C1 O1 -179.7(2) . . . . ?
C7 C2 C1 O2 -0.5(4) . . . . ?
C7 C2 C3 C4 0.4(4) . . . . ?
C7 C6 C5 O17 -178.3(2) . . . . ?
C7 C6 C5 C4 0.3(4) . . . . ?
C8 C9 C14 C13 -176.7(2) . . . . ?
C8 C9 C10 C11 177.0(2) . . . . ?
C24 C23 C28 C27 0.6(4) . . . . ?
C30 C31 C32 C33 0.3(5) . . . . ?
C29 C30 C31 C32 -178.1(3) . . . . ?
C29 C30 C35 C34 177.8(3) . . . . ?
C14 C9 C8 O4 173.0(2) . . . . ?
C14 C9 C8 O3 -7.1(3) . . . . ?
C14 C9 C10 C11 -0.8(4) . . . . ?
C1 C2 C7 C6 180.0(2) . . . . ?
C1 C2 C3 C4 -180.0(2) . . . . ?
C16 C17 C18 C19 -0.8(4) . . . . ?
C11 C12 C13 C14 -1.4(4) . . . . ?
C12 C11 C10 C9 -0.6(4) . . . . ?
C36 C37 C38 C39 178.5(3) . . . . ?
C36 C37 C42 C41 -179.0(3) . . . . ?
C23 C24 C25 C26 -2.1(5) . . . . ?
C23 C28 C27 C26 -1.1(5) . . . . ?
C34 C33 C32 C31 -1.8(5) . . . . ?
C39 C40 C41 C42 0.2(5) . . . . ?
C31 C30 C29 O11 -0.3(4) . . . . ?
C31 C30 C29 O12 178.7(3) . . . . ?
C31 C30 C35 C34 -1.9(4) . . . . ?
C37 C42 C41 C40 0.3(5) . . . . ?
C38 C39 C40 O22 178.6(3) . . . . ?
C38 C39 C40 C41 -0.8(5) . . . . ?
C38 C37 C42 C41 -0.4(5) . . . . ?
C33 C34 C35 C30 0.5(5) . . . . ?
C10 C9 C8 O4 -4.7(3) . . . . ?
C10 C9 C8 O3 175.1(2) . . . . ?
C10 C9 C14 C13 1.1(4) . . . . ?
C10 C11 C12 O18 -177.1(2) . . . . ?
C10 C11 C12 C13 1.7(4) . . . . ?
C3 C2 C7 C6 -0.4(4) . . . . ?
C3 C2 C1 O1 0.7(4) . . . . ?
C3 C2 C1 O2 179.9(2) . . . . ?
C3 C4 C5 O17 178.4(2) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C35 C30 C29 O11 -179.9(3) . . . . ?
C35 C30 C29 O12 -0.9(4) . . . . ?
C35 C30 C31 C32 1.5(5) . . . . ?
C35 C34 C33 O21 -178.5(3) . . . . ?
C35 C34 C33 C32 1.4(5) . . . . ?
C17 C16 C21 C20 0.1(4) . . . . ?
C17 C18 C19 O19 179.8(3) . . . . ?
C17 C18 C19 C20 -0.2(4) . . . . ?
C25 C24 C23 C22 -176.5(3) . . . . ?
C25 C24 C23 C28 0.9(4) . . . . ?
C25 C26 C27 C28 -0.1(5) . . . . ?
C5 C4 C3 C2 -0.1(4) . . . . ?
C40 C39 C38 C37 0.8(5) . . . . ?
C21 C16 C17 C18 0.8(4) . . . . ?
C21 C20 C19 O19 -178.9(3) . . . . ?
C21 C20 C19 C18 1.2(4) . . . . ?
C27 C26 C25 C24 1.7(5) . . . . ?
C19 C20 C21 C16 -1.1(5) . . . . ?
C42 C37 C38 C39 -0.2(5) . . . . ?
