#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:45:41 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195072 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/22/7042226.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_7042226
loop_
_publ_author_name
'Li, Ning'
'García-Rodríguez, Raúl'
'Matthews, Peter D.'
'Luo, He-Kuan'
'Wright, Dominic S.'
_publ_section_title
;
 Synthesis, structure and paramagnetic NMR analysis of a series of
 lanthanide-containing [LnTi6O3(O(i)Pr)9(salicylate)6] cages.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4287
_journal_page_last               4295
_journal_paper_doi               10.1039/c7dt00049a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C69 H87 O30 Pr Ti6'
_chemical_formula_sum            'C69 H87 O30 Pr Ti6'
_chemical_formula_weight         1824.69
_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_Hall           'P -6'
_space_group_name_H-M_alt        'P -6'
_symmetry_space_group_name_Hall  'P -6'
_symmetry_space_group_name_H-M   'P -6'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.9478(6)
_cell_length_b                   14.9478(6)
_cell_length_c                   23.5581(11)
_cell_measurement_reflns_used    9476
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      64.2
_cell_measurement_theta_min      3.31
_cell_volume                     4558.5(3)
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_collection       'Bruker software package, narrow-frames'
_computing_data_reduction
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39041
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        65.308
_diffrn_reflns_theta_max         65.308
_diffrn_reflns_theta_min         3.414
_exptl_absorpt_coefficient_mu    8.862
_exptl_absorpt_correction_T_max  0.370
_exptl_absorpt_correction_T_min  0.270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (SADABS) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.726
_refine_diff_density_max         8.674
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.256
_refine_ls_abs_structure_details
;
 Flack x determined using 2158 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5331
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1525P)²+10.9642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2114
_refine_ls_wR_factor_ref         0.2215
_reflns_Friedel_coverage         0.984
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4840
_reflns_number_total             5331
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00049a2.cif
_cod_data_source_block           pr_c
_cod_depositor_comments
'Adding full bibliography for 7042216--7042227.cif.'
_cod_original_cell_volume        4558.5(4)
_cod_database_code               7042226
_shelx_shelxl_version_number     2016/6
_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_min   0.270
_shelx_estimated_absorpt_t_max   0.370
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -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 0.666667 0.333333 0.500000 0.0184(8) Uani 1 6 d S T P . .
Pr2 Pr 1.000000 1.000000 1.000000 0.0177(8) Uani 1 6 d S T P . .
Ti1 Ti 0.4649(3) 0.3640(3) 0.56378(16) 0.0278(9) Uani 1 1 d . . . . .
Ti2 Ti 0.8074(3) 0.7614(3) 0.93650(15) 0.0266(9) Uani 1 1 d . . . . .
O1 O 0.4979(16) 0.3077(16) 0.500000 0.026(4) Uani 1 2 d S TU P . .
O2 O 0.4835(14) 0.4591(15) 0.500000 0.028(5) Uani 1 2 d S TU P C .
O3 O 0.3287(12) 0.2961(12) 0.5650(6) 0.040(4) Uani 1 1 d D U . . .
O4 O 0.4800(12) 0.4541(13) 0.6237(7) 0.042(4) Uani 1 1 d . U . . .
O5 O 0.4712(12) 0.2575(11) 0.6142(6) 0.033(4) Uani 1 1 d . U . . .
O6 O 0.6318(11) 0.4360(11) 0.5750(6) 0.029(3) Uani 1 1 d . U . . .
O21 O 0.8300(15) 0.8509(16) 1.000000 0.028(5) Uani 1 2 d S TU P . .
O22 O 0.8314(17) 0.6878(13) 1.000000 0.030(4) Uani 1 2 d S TU P G .
O23 O 0.6717(11) 0.6829(12) 0.9340(6) 0.033(4) Uani 1 1 d D U . . .
O24 O 0.8279(11) 0.6932(11) 0.8762(6) 0.035(4) Uani 1 1 d . U . . .
O25 O 0.9751(11) 0.8637(11) 0.9243(6) 0.027(3) Uani 1 1 d . U . . .
O26 O 0.8042(14) 0.8695(13) 0.8848(8) 0.039(4) Uani 1 1 d . U . . .
C2 C 0.479(3) 0.560(3) 0.500000 0.050(9) Uani 1 2 d S TU P . .
H2A H 0.474311 0.560898 0.542311 0.060 Uiso 0.5 1 calc R U P A -1
C2A C 0.589(4) 0.650(4) 0.500000 0.079(14) Uani 1 2 d S TU P C .
H2AA H 0.588480 0.715074 0.500000 0.118 Uiso 0.5 1 calc R U P B -1
H2AB H 0.625068 0.646233 0.533966 0.118 Uiso 0.5 1 calc R U P B -1
H2AC H 0.625068 0.646233 0.466034 0.118 Uiso 0.5 1 calc R U P B -1
C2B C 0.354(5) 0.528(5) 0.491(5) 0.08(2) Uani 0.5 1 d . U P C -1
H2BA H 0.310099 0.452981 0.496091 0.124 Uiso 0.5 1 calc R U P C -1
H2BB H 0.335834 0.563963 0.519309 0.124 Uiso 0.5 1 calc R U P C -1
H2BC H 0.344701 0.547280 0.452891 0.124 Uiso 0.5 1 calc R U P C -1
C3 C 0.249(2) 0.252(3) 0.6060(15) 0.036(7) Uiso 0.55(3) 1 d D U P D 1
H3 H 0.281332 0.253960 0.643426 0.043 Uiso 0.55(3) 1 calc R U P D 1
C3A C 0.191(5) 0.303(4) 0.613(3) 0.075(10) Uiso 0.55(3) 1 d D U P D 1
H3AA H 0.236761 0.374974 0.623377 0.112 Uiso 0.55(3) 1 calc R U P D 1
H3AB H 0.155636 0.299695 0.577093 0.112 Uiso 0.55(3) 1 calc R U P D 1
H3AC H 0.138947 0.268173 0.642776 0.112 Uiso 0.55(3) 1 calc R U P D 1
C3B C 0.185(5) 0.148(3) 0.591(3) 0.075(10) Uiso 0.55(3) 1 d D U P D 1
H3BA H 0.128749 0.114898 0.618327 0.112 Uiso 0.55(3) 1 calc R U P D 1
H3BB H 0.156870 0.144425 0.552909 0.112 Uiso 0.55(3) 1 calc R U P D 1
H3BC H 0.225948 0.113410 0.590905 0.112 Uiso 0.55(3) 1 calc R U P D 1
C3' C 0.228(2) 0.213(3) 0.566(2) 0.036(7) Uiso 0.45(3) 1 d D U P D 2
H3A' H 0.240887 0.186422 0.602392 0.043 Uiso 0.45(3) 1 calc R U P D 2
C3A' C 0.167(5) 0.247(5) 0.594(3) 0.075(10) Uiso 0.45(3) 1 d D U P D 2
H3AD H 0.211663 0.317493 0.608643 0.112 Uiso 0.45(3) 1 calc R U P D 2
H3AE H 0.116502 0.247112 0.567765 0.112 Uiso 0.45(3) 1 calc R U P D 2
H3AF H 0.130654 0.201000 0.626205 0.112 Uiso 0.45(3) 1 calc R U P D 2
C3B' C 0.168(5) 0.114(4) 0.545(3) 0.075(10) Uiso 0.45(3) 1 d D U P D 2
H3BD H 0.096524 0.084753 0.559043 0.112 Uiso 0.45(3) 1 calc R U P D 2
H3BE H 0.167841 0.115456 0.503644 0.112 Uiso 0.91(6) 2 calc R U P D 2
H3BF H 0.195549 0.070187 0.558193 0.112 Uiso 0.45(3) 1 calc R U P D 2
C11 C 0.553(2) 0.5298(18) 0.6552(11) 0.039(5) Uani 1 1 d . U . . .
C12 C 0.523(2) 0.5819(19) 0.6923(10) 0.042(6) Uani 1 1 d . U . . .
H12A H 0.454243 0.568231 0.693670 0.050 Uiso 1 1 calc R U . . .
C13 C 0.598(3) 0.654(3) 0.7271(13) 0.062(8) Uani 1 1 d . U . . .
H13A H 0.577171 0.688153 0.753481 0.075 Uiso 1 1 calc R U . . .
C14 C 0.693(3) 0.681(3) 0.7274(13) 0.062(8) Uani 1 1 d . U . . .
H14A H 0.740407 0.732217 0.752747 0.074 Uiso 1 1 calc R U . . .
C15 C 0.728(2) 0.631(2) 0.6887(12) 0.054(7) Uani 1 1 d . U . . .
H15A H 0.798409 0.649235 0.686790 0.065 Uiso 1 1 calc R U . . .
C16 C 0.6530(19) 0.5540(17) 0.6532(10) 0.034(5) Uani 1 1 d . U . . .
C17 C 0.4959(17) 0.1879(19) 0.6124(10) 0.030(5) Uani 1 1 d . U . . .
C22 C 0.836(4) 0.591(4) 1.000000 0.068(12) Uani 1 2 d S TU P . .
H22' H 0.825850 0.577892 0.958221 0.082 Uiso 0.5 1 calc R U P E -1
C22A C 0.958(9) 0.647(10) 1.000000 0.20(5) Uani 1 2 d S TU P G .
H22A H 0.986521 0.712809 0.979511 0.296 Uiso 0.5 1 calc R U P F -1
H22B H 0.983591 0.660313 1.039207 0.296 Uiso 0.5 1 calc R U P F -1
H22C H 0.980383 0.602847 0.981282 0.296 Uiso 0.5 1 calc R U P F -1
C22B C 0.745(7) 0.507(5) 1.016(3) 0.09(2) Uani 0.5 1 d . U P G -1
H22D H 0.752323 0.445715 1.015659 0.130 Uiso 0.5 1 calc R U P G -1
H22E H 0.728061 0.518219 1.055068 0.130 Uiso 0.5 1 calc R U P G -1
H22F H 0.689843 0.497891 0.990469 0.130 Uiso 0.5 1 calc R U P G -1
C23 C 0.602(3) 0.640(4) 0.887(2) 0.064(11) Uiso 0.46(3) 1 d D U P H 1
H23A H 0.639889 0.675180 0.851549 0.077 Uiso 0.46(3) 1 calc R U P H 1
C23A C 0.518(5) 0.659(5) 0.894(3) 0.068(8) Uiso 0.46(3) 1 d D U P H 1
H23B H 0.544337 0.733006 0.898374 0.102 Uiso 0.46(3) 1 calc R U P H 1
H23C H 0.473037 0.633633 0.860362 0.102 Uiso 0.46(3) 1 calc R U P H 1
H23D H 0.477798 0.622220 0.927676 0.102 Uiso 0.46(3) 1 calc R U P H 1
C23B C 0.561(5) 0.532(4) 0.881(3) 0.068(8) Uiso 0.46(3) 1 d D U P H 1
H23E H 0.617086 0.517169 0.876012 0.102 Uiso 0.46(3) 1 calc R U P H 1
H23F H 0.520380 0.496158 0.914610 0.102 Uiso 0.46(3) 1 calc R U P H 1
H23G H 0.515619 0.507572 0.847296 0.102 Uiso 0.46(3) 1 calc R U P H 1
C23' C 0.564(2) 0.632(3) 0.938(2) 0.064(11) Uiso 0.54(3) 1 d D U P H 2
H23H H 0.539334 0.592753 0.974484 0.077 Uiso 0.54(3) 1 calc R U P H 2
C23C C 0.566(5) 0.725(4) 0.940(2) 0.068(8) Uiso 0.54(3) 1 d D U P H 2
H23I H 0.495275 0.712162 0.943691 0.102 Uiso 0.54(3) 1 calc R U P H 2
H23J H 0.606255 0.764143 0.973535 0.102 Uiso 0.54(3) 1 calc R U P H 2
H23K H 0.597898 0.764439 0.905819 0.102 Uiso 0.54(3) 1 calc R U P H 2
C23D C 0.503(5) 0.574(4) 0.891(2) 0.068(8) Uiso 0.54(3) 1 d D U P H 2
H23L H 0.501290 0.507644 0.889455 0.102 Uiso 0.54(3) 1 calc R U P H 2
H23M H 0.432303 0.561370 0.896114 0.102 Uiso 0.54(3) 1 calc R U P H 2
H23N H 0.532231 0.612474 0.856127 0.102 Uiso 0.54(3) 1 calc R U P H 2
C31 C 0.9039(19) 0.6976(17) 0.8427(10) 0.037(5) Uani 1 1 d . U . . .
C32 C 0.879(2) 0.621(2) 0.8036(12) 0.047(6) Uani 1 1 d . U . . .
H32A H 0.810273 0.564276 0.802303 0.057 Uiso 1 1 calc R U . . .
C33 C 0.953(3) 0.624(2) 0.7654(12) 0.059(7) Uani 1 1 d . U . . .
H33A H 0.934376 0.571329 0.737654 0.070 Uiso 1 1 calc R U . . .
C34 C 1.056(3) 0.708(3) 0.7699(14) 0.069(9) Uani 1 1 d . U . . .
H34A H 1.108269 0.712875 0.744857 0.083 Uiso 1 1 calc R U . . .
C35 C 1.080(2) 0.782(2) 0.8099(10) 0.044(6) Uani 1 1 d . U . . .
H35A H 1.149177 0.838143 0.811926 0.053 Uiso 1 1 calc R U . . .
C36 C 1.0062(18) 0.7790(18) 0.8488(11) 0.035(5) Uani 1 1 d . U . . .
C37 C 0.8257(17) 0.9606(18) 0.8894(10) 0.026(5) Uani 1 1 d . U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -2.4164 10.2820 '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
O1 Pr1 O1 120.000(8) . 2_655
O1 Pr1 O1 120.000(1) . 3_665
O1 Pr1 O1 120.000(3) 2_655 3_665
O1 Pr1 O6 136.0(3) . 3_665
O1 Pr1 O6 72.9(5) 2_655 3_665
O1 Pr1 O6 64.8(5) 3_665 3_665
O1 Pr1 O6 72.9(5) . 5_656
O1 Pr1 O6 64.8(5) 2_655 5_656
O1 Pr1 O6 136.0(3) 3_665 5_656
O6 Pr1 O6 137.6(2) 3_665 5_656
O1 Pr1 O6 136.0(3) . 6_666
O1 Pr1 O6 72.9(5) 2_655 6_666
O1 Pr1 O6 64.8(5) 3_665 6_666
O6 Pr1 O6 87.3(6) 3_665 6_666
O6 Pr1 O6 77.6(5) 5_656 6_666
O1 Pr1 O6 72.9(5) . 2_655
O1 Pr1 O6 64.8(5) 2_655 2_655
O1 Pr1 O6 136.0(3) 3_665 2_655
O6 Pr1 O6 77.6(5) 3_665 2_655
O6 Pr1 O6 87.3(6) 5_656 2_655
O6 Pr1 O6 137.6(2) 6_666 2_655
O1 Pr1 O6 64.8(5) . 4_556
O1 Pr1 O6 136.0(3) 2_655 4_556
O1 Pr1 O6 72.9(5) 3_665 4_556
O6 Pr1 O6 137.6(2) 3_665 4_556
O6 Pr1 O6 77.6(5) 5_656 4_556
O6 Pr1 O6 77.6(5) 6_666 4_556
O6 Pr1 O6 137.6(2) 2_655 4_556
O1 Pr1 O6 64.8(5) . .
O1 Pr1 O6 136.0(3) 2_655 .
O1 Pr1 O6 72.9(5) 3_665 .
O6 Pr1 O6 77.6(5) 3_665 .
O6 Pr1 O6 137.6(2) 5_656 .
O6 Pr1 O6 137.6(2) 6_666 .
O6 Pr1 O6 77.6(5) 2_655 .
O6 Pr1 O6 87.3(6) 4_556 .
O1 Pr1 Ti1 103.5(5) . 5_656
O1 Pr1 Ti1 28.7(3) 2_655 5_656
O1 Pr1 Ti1 130.1(4) 3_665 5_656
O6 Pr1 Ti1 100.7(3) 3_665 5_656
O6 Pr1 Ti1 36.9(3) 5_656 5_656
O6 Pr1 Ti1 67.0(3) 6_666 5_656
O6 Pr1 Ti1 77.1(3) 2_655 5_656
O6 Pr1 Ti1 109.0(3) 4_556 5_656
O6 Pr1 Ti1 154.4(3) . 5_656
O1 Pr1 Ti1 103.5(5) . 2_655
O1 Pr1 Ti1 28.7(3) 2_655 2_655
O1 Pr1 Ti1 130.1(4) 3_665 2_655
O6 Pr1 Ti1 67.0(3) 3_665 2_655
O6 Pr1 Ti1 77.1(3) 5_656 2_655
O6 Pr1 Ti1 100.7(3) 6_666 2_655
O6 Pr1 Ti1 36.9(3) 2_655 2_655
O6 Pr1 Ti1 154.4(3) 4_556 2_655
O6 Pr1 Ti1 109.0(3) . 2_655
Ti1 Pr1 Ti1 49.36(12) 5_656 2_655
O1 Pr1 Ti1 130.1(4) . 3_665
O1 Pr1 Ti1 103.5(5) 2_655 3_665
O1 Pr1 Ti1 28.7(3) 3_665 3_665
O6 Pr1 Ti1 36.9(3) 3_665 3_665
O6 Pr1 Ti1 154.4(3) 5_656 3_665
O6 Pr1 Ti1 77.1(3) 6_666 3_665
O6 Pr1 Ti1 109.0(3) 2_655 3_665
O6 Pr1 Ti1 100.7(3) 4_556 3_665
O6 Pr1 Ti1 67.0(3) . 3_665
Ti1 Pr1 Ti1 125.96(3) 5_656 3_665
Ti1 Pr1 Ti1 103.79(7) 2_655 3_665
O21 Pr2 O21 120.00(2) 3_675 2_765
O21 Pr2 O21 119.999(7) 3_675 .
O21 Pr2 O21 120.001(7) 2_765 .
O21 Pr2 O25 136.4(3) 3_675 .
O21 Pr2 O25 71.1(5) 2_765 .
O21 Pr2 O25 66.5(5) . .
O21 Pr2 O25 71.1(5) 3_675 5_767
O21 Pr2 O25 66.5(5) 2_765 5_767
O21 Pr2 O25 136.4(3) . 5_767
O25 Pr2 O25 137.5(2) . 5_767
O21 Pr2 O25 66.5(5) 3_675 3_675
O21 Pr2 O25 136.4(3) 2_765 3_675
O21 Pr2 O25 71.1(5) . 3_675
O25 Pr2 O25 77.8(5) . 3_675
O25 Pr2 O25 137.5(2) 5_767 3_675
O21 Pr2 O25 66.5(5) 3_675 6_677
O21 Pr2 O25 136.4(3) 2_765 6_677
O21 Pr2 O25 71.1(5) . 6_677
O25 Pr2 O25 137.5(2) . 6_677
O25 Pr2 O25 77.8(5) 5_767 6_677
O25 Pr2 O25 87.0(6) 3_675 6_677
O21 Pr2 O25 71.1(5) 3_675 2_765
O21 Pr2 O25 66.5(5) 2_765 2_765
O21 Pr2 O25 136.4(3) . 2_765
O25 Pr2 O25 77.8(5) . 2_765
O25 Pr2 O25 87.0(7) 5_767 2_765
O25 Pr2 O25 77.8(5) 3_675 2_765
O25 Pr2 O25 137.5(2) 6_677 2_765
O21 Pr2 O25 136.4(3) 3_675 4_557
O21 Pr2 O25 71.1(5) 2_765 4_557
O21 Pr2 O25 66.5(5) . 4_557
O25 Pr2 O25 87.0(6) . 4_557
O25 Pr2 O25 77.8(5) 5_767 4_557
O25 Pr2 O25 137.5(2) 3_675 4_557
O25 Pr2 O25 77.8(5) 6_677 4_557
O25 Pr2 O25 137.5(2) 2_765 4_557
O21 Pr2 Ti2 131.6(5) 3_675 .
O21 Pr2 Ti2 101.9(5) 2_765 .
O21 Pr2 Ti2 29.5(3) . .
O25 Pr2 Ti2 37.5(3) . .
O25 Pr2 Ti2 154.8(3) 5_767 .
O25 Pr2 Ti2 66.6(3) 3_675 .
O25 Pr2 Ti2 100.1(3) 6_677 .
O25 Pr2 Ti2 109.4(3) 2_765 .
O25 Pr2 Ti2 77.2(3) 4_557 .
O21 Pr2 Ti2 101.9(5) 3_675 5_767
O21 Pr2 Ti2 29.5(3) 2_765 5_767
O21 Pr2 Ti2 131.6(5) . 5_767
O25 Pr2 Ti2 100.1(3) . 5_767
O25 Pr2 Ti2 37.5(3) 5_767 5_767
O25 Pr2 Ti2 154.8(3) 3_675 5_767
O25 Pr2 Ti2 109.4(3) 6_677 5_767
O25 Pr2 Ti2 77.2(3) 2_765 5_767
O25 Pr2 Ti2 66.6(3) 4_557 5_767
Ti2 Pr2 Ti2 125.89(3) . 5_767
O21 Pr2 Ti2 131.6(5) 3_675 4_557
O21 Pr2 Ti2 101.9(5) 2_765 4_557
O21 Pr2 Ti2 29.5(3) . 4_557
O25 Pr2 Ti2 77.2(3) . 4_557
O25 Pr2 Ti2 109.4(3) 5_767 4_557
O25 Pr2 Ti2 100.1(3) 3_675 4_557
O25 Pr2 Ti2 66.6(3) 6_677 4_557
O25 Pr2 Ti2 154.8(3) 2_765 4_557
O25 Pr2 Ti2 37.5(3) 4_557 4_557
Ti2 Pr2 Ti2 49.07(12) . 4_557
Ti2 Pr2 Ti2 103.96(7) 5_767 4_557
O3 Ti1 O4 95.2(7) . .
O3 Ti1 O1 103.8(8) . .
O4 Ti1 O1 160.4(8) . .
O3 Ti1 O2 97.6(8) . .
O4 Ti1 O2 97.5(7) . .
O1 Ti1 O2 75.3(7) . .
O3 Ti1 O5 91.8(7) . .
O4 Ti1 O5 95.0(7) . .
O1 Ti1 O5 89.5(6) . .
O2 Ti1 O5 163.6(6) . .
O3 Ti1 O6 171.0(7) . .
O4 Ti1 O6 81.9(6) . .
O1 Ti1 O6 80.1(7) . .
O2 Ti1 O6 91.3(7) . .
O5 Ti1 O6 80.0(6) . .
O3 Ti1 Ti1 90.9(5) . 4_556
O4 Ti1 Ti1 138.5(5) . 4_556
O1 Ti1 Ti1 37.9(5) . 4_556
O2 Ti1 Ti1 41.0(4) . 4_556
O5 Ti1 Ti1 125.9(4) . 4_556
O6 Ti1 Ti1 96.9(4) . 4_556
O3 Ti1 Pr1 137.2(6) . .
O4 Ti1 Pr1 126.5(5) . .
O1 Ti1 Pr1 36.4(6) . .
O2 Ti1 Pr1 87.1(5) . .
O5 Ti1 Pr1 76.9(4) . .
O6 Ti1 Pr1 44.7(4) . .
Ti1 Ti1 Pr1 65.32(6) 4_556 .
O23 Ti2 O24 93.4(7) . .
O23 Ti2 O21 103.5(8) . .
O24 Ti2 O21 163.0(8) . .
O23 Ti2 O22 97.0(8) . .
O24 Ti2 O22 98.4(7) . .
O21 Ti2 O22 77.4(7) . .
O23 Ti2 O26 91.9(7) . .
O24 Ti2 O26 93.1(7) . .
O21 Ti2 O26 88.8(8) . .
O22 Ti2 O26 165.0(7) . .
O23 Ti2 O25 170.4(6) . .
O24 Ti2 O25 80.7(6) . .
O21 Ti2 O25 82.9(7) . .
O22 Ti2 O25 91.4(7) . .
O26 Ti2 O25 80.9(7) . .
O23 Ti2 Ti2 91.9(5) . 4_557
O24 Ti2 Ti2 139.7(5) . 4_557
O21 Ti2 Ti2 38.8(5) . 4_557
O22 Ti2 Ti2 41.4(4) . 4_557
O26 Ti2 Ti2 126.6(5) . 4_557
O25 Ti2 Ti2 97.5(4) . 4_557
O23 Ti2 Pr2 139.1(5) . .
O24 Ti2 Pr2 126.2(5) . .
O21 Ti2 Pr2 38.0(6) . .
O22 Ti2 Pr2 87.7(5) . .
O26 Ti2 Pr2 77.8(5) . .
O25 Ti2 Pr2 45.6(3) . .
Ti2 Ti2 Pr2 65.46(6) 4_557 .
Ti1 O1 Ti1 104.2(9) 4_556 .
Ti1 O1 Pr1 114.9(7) 4_556 .
Ti1 O1 Pr1 114.9(7) . .
C2 O2 Ti1 129.8(5) . 4_556
C2 O2 Ti1 129.8(5) . .
Ti1 O2 Ti1 98.1(8) 4_556 .
C3' O3 Ti1 159(2) . .
C3 O3 Ti1 137.8(19) . .
C11 O4 Ti1 140.9(15) . .
C17 O5 Ti1 140.6(17) . .
C17 O6 Ti1 129.6(15) 3_665 .
C17 O6 Pr1 131.7(15) 3_665 .
Ti1 O6 Pr1 98.4(5) . .
Ti2 O21 Ti2 102.3(11) . 4_557
Ti2 O21 Pr2 112.5(7) . .
Ti2 O21 Pr2 112.5(7) 4_557 .
C22 O22 Ti2 130.3(6) . .
C22 O22 Ti2 130.3(6) . 4_557
Ti2 O22 Ti2 97.3(8) . 4_557
C23' O23 Ti2 171(2) . .
C23 O23 Ti2 131(2) . .
C31 O24 Ti2 141.3(14) . .
C37 O25 Ti2 133.7(15) 2_765 .
C37 O25 Pr2 129.0(15) 2_765 .
Ti2 O25 Pr2 97.0(5) . .
C37 O26 Ti2 136.2(19) . .
C2A C2 O2 108(3) . .
C2A C2 C2B 144(4) . .
O2 C2 C2B 107(3) . .
C2A C2 H2A 92.7 . .
O2 C2 H2A 92.7 . .
C2B C2 H2A 92.7 . .
C2 C2A H2AA 109.5 . .
C2 C2A H2AB 109.5 . .
H2AA C2A H2AB 109.5 . .
C2 C2A H2AC 109.5 . .
H2AA C2A H2AC 109.5 . .
H2AB C2A H2AC 109.5 . .
C2 C2B H2BA 109.5 . .
C2 C2B H2BB 109.5 . .
H2BA C2B H2BB 109.5 . .
C2 C2B H2BC 109.5 . .
H2BA C2B H2BC 109.5 . .
H2BB C2B H2BC 109.5 . .
C3B C3 O3 107(3) . .
C3B C3 C3A 111(3) . .
O3 C3 C3A 115(4) . .
C3B C3 H3 107.7 . .
O3 C3 H3 107.7 . .
C3A C3 H3 107.7 . .
C3 C3A H3AA 109.5 . .
C3 C3A H3AB 109.5 . .
H3AA C3A H3AB 109.5 . .
C3 C3A H3AC 109.5 . .
H3AA C3A H3AC 109.5 . .
H3AB C3A H3AC 109.5 . .
C3 C3B H3BA 109.5 . .
C3 C3B H3BB 109.5 . .
H3BA C3B H3BB 109.5 . .
C3 C3B H3BC 109.5 . .
H3BA C3B H3BC 109.5 . .
H3BB C3B H3BC 109.5 . .
C3B' C3' O3 141(4) . .
C3B' C3' C3A' 111(3) . .
O3 C3' C3A' 107(4) . .
C3B' C3' H3A' 91.8 . .
O3 C3' H3A' 91.8 . .
C3A' C3' H3A' 91.8 . .
C3' C3A' H3AD 109.5 . .
C3' C3A' H3AE 109.5 . .
H3AD C3A' H3AE 109.5 . .
C3' C3A' H3AF 109.5 . .
H3AD C3A' H3AF 109.5 . .
H3AE C3A' H3AF 109.5 . .
C3' C3B' H3BD 109.5 . .
C3' C3B' H3BE 109.5 . .
H3BD C3B' H3BE 109.5 . .
C3' C3B' H3BF 109.5 . .
H3BD C3B' H3BF 109.5 . .
H3BE C3B' H3BF 109.5 . .
O4 C11 C16 122(2) . .
O4 C11 C12 118(2) . .
C16 C11 C12 120(3) . .
C13 C12 C11 117(3) . .
C13 C12 H12A 121.3 . .
C11 C12 H12A 121.3 . .
C14 C13 C12 126(3) . .
C14 C13 H13A 116.9 . .
C12 C13 H13A 116.9 . .
C13 C14 C15 118(3) . .
C13 C14 H14A 120.8 . .
C15 C14 H14A 120.8 . .
C16 C15 C14 117(3) . .
C16 C15 H15A 121.3 . .
C14 C15 H15A 121.3 . .
C11 C16 C15 121(2) . .
C11 C16 C17 123(2) . 3_665
C15 C16 C17 116(2) . 3_665
O5 C17 O6 119(2) . 2_655
O5 C17 C16 119(2) . 2_655
O6 C17 C16 122(2) 2_655 2_655
C22B C22 O22 113(5) . .
C22B C22 C22A 147(7) . .
O22 C22 C22A 95(6) . .
C22B C22 H22' 96.9 . .
O22 C22 H22' 96.9 . .
C22A C22 H22' 96.9 . .
C22 C22A H22A 109.5 . .
C22 C22A H22B 109.5 . .
H22A C22A H22B 109.5 . .
C22 C22A H22C 109.5 . .
H22A C22A H22C 109.5 . .
H22B C22A H22C 109.5 . .
C22 C22B H22D 109.5 . .
C22 C22B H22E 109.5 . .
H22D C22B H22E 109.5 . .
C22 C22B H22F 109.5 . .
H22D C22B H22F 109.5 . .
H22E C22B H22F 109.5 . .
C23B C23 C23A 108(3) . .
C23B C23 O23 113(5) . .
C23A C23 O23 110(4) . .
C23B C23 H23A 108.5 . .
C23A C23 H23A 108.5 . .
O23 C23 H23A 108.5 . .
C23 C23A H23B 109.5 . .
C23 C23A H23C 109.5 . .
H23B C23A H23C 109.5 . .
C23 C23A H23D 109.5 . .
H23B C23A H23D 109.5 . .
H23C C23A H23D 109.5 . .
C23 C23B H23E 109.5 . .
C23 C23B H23F 109.5 . .
H23E C23B H23F 109.5 . .
C23 C23B H23G 109.5 . .
H23E C23B H23G 109.5 . .
H23F C23B H23G 109.5 . .
C23C C23' O23 91(4) . .
C23C C23' C23D 109(3) . .
O23 C23' C23D 120(4) . .
C23C C23' H23H 111.7 . .
O23 C23' H23H 111.7 . .
C23D C23' H23H 111.7 . .
C23' C23C H23I 109.5 . .
C23' C23C H23J 109.5 . .
H23I C23C H23J 109.5 . .
C23' C23C H23K 109.5 . .
H23I C23C H23K 109.5 . .
H23J C23C H23K 109.5 . .
C23' C23D H23L 109.5 . .
C23' C23D H23M 109.5 . .
H23L C23D H23M 109.5 . .
C23' C23D H23N 109.5 . .
H23L C23D H23N 109.5 . .
H23M C23D H23N 109.5 . .
O24 C31 C32 119(2) . .
O24 C31 C36 120(2) . .
C32 C31 C36 121(2) . .
C31 C32 C33 122(3) . .
C31 C32 H32A 119.2 . .
C33 C32 H32A 119.2 . .
C32 C33 C34 118(3) . .
C32 C33 H33A 121.1 . .
C34 C33 H33A 121.1 . .
C35 C34 C33 120(3) . .
C35 C34 H34A 120.1 . .
C33 C34 H34A 120.1 . .
C34 C35 C36 123(3) . .
C34 C35 H35A 118.7 . .
C36 C35 H35A 118.7 . .
C31 C36 C35 117(2) . .
C31 C36 C37 125(2) . 2_765
C35 C36 C37 118(2) . 2_765
O26 C37 O25 126(2) . 3_675
O26 C37 C36 115(2) . 3_675
O25 C37 C36 119(2) 3_675 3_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr1 O1 2.35(2) .
Pr1 O1 2.35(2) 2_655
Pr1 O1 2.35(2) 3_665
Pr1 O6 2.558(14) 3_665
Pr1 O6 2.558(14) 5_656
Pr1 O6 2.558(14) 6_666
Pr1 O6 2.558(14) 2_655
Pr1 O6 2.558(14) 4_556
Pr1 O6 2.558(14) .
Pr1 Ti1 3.598(4) 5_656
Pr1 Ti1 3.598(4) 2_655
Pr1 Ti1 3.598(4) 3_665
Pr2 O21 2.400(19) 3_675
Pr2 O21 2.400(19) 2_765
Pr2 O21 2.400(19) .
Pr2 O25 2.591(13) .
Pr2 O25 2.591(13) 5_767
Pr2 O25 2.591(13) 3_675
Pr2 O25 2.591(13) 6_677
Pr2 O25 2.591(13) 2_765
Pr2 O25 2.591(13) 4_557
Pr2 Ti2 3.602(4) .
Pr2 Ti2 3.602(4) 5_767
Pr2 Ti2 3.602(4) 4_557
Ti1 O3 1.764(16) .
Ti1 O4 1.886(17) .
Ti1 O1 1.904(12) .
Ti1 O2 1.990(13) .
Ti1 O5 2.026(15) .
Ti1 O6 2.183(15) .
Ti1 Ti1 3.005(7) 4_556
Ti2 O23 1.765(15) .
Ti2 O24 1.861(14) .
Ti2 O21 1.920(15) .
Ti2 O22 1.993(13) .
Ti2 O26 2.043(18) .
Ti2 O25 2.208(16) .
Ti2 Ti2 2.992(7) 4_557
O2 C2 1.55(4) .
O3 C3' 1.40(3) .
O3 C3 1.42(3) .
O4 C11 1.34(3) .
O5 C17 1.27(3) .
O6 C17 1.31(3) 3_665
O22 C22 1.48(6) .
O23 C23' 1.39(3) .
O23 C23 1.43(3) .
O24 C31 1.36(3) .
O25 C37 1.26(3) 2_765
O26 C37 1.24(3) .
C2 C2A 1.51(6) .
C2 C2B 1.69(8) .
C2 H2A 1.0000 .
C2A H2AA 0.9800 .
C2A H2AB 0.9800 .
C2A H2AC 0.9800 .
C2B H2BA 0.9800 .
C2B H2BB 0.9800 .
C2B H2BC 0.9800 .
C3 C3B 1.40(3) .
C3 C3A 1.42(3) .
C3 H3 1.0000 .
C3A H3AA 0.9800 .
C3A H3AB 0.9800 .
C3A H3AC 0.9800 .
C3B H3BA 0.9800 .
C3B H3BB 0.9800 .
C3B H3BC 0.9800 .
C3' C3B' 1.39(3) .
C3' C3A' 1.41(3) .
C3' H3A' 1.0000 .
C3A' H3AD 0.9800 .
C3A' H3AE 0.9800 .
C3A' H3AF 0.9800 .
C3B' H3BD 0.9800 .
C3B' H3BE 0.9800 .
C3B' H3BF 0.9800 .
C11 C16 1.35(4) .
C11 C12 1.38(3) .
C12 C13 1.37(4) .
C12 H12A 0.9500 .
C13 C14 1.27(4) .
C13 H13A 0.9500 .
C14 C15 1.42(4) .
C14 H14A 0.9500 .
C15 C16 1.41(4) .
C15 H15A 0.9500 .
C16 C17 1.50(3) 3_665
C22 C22B 1.36(9) .
C22 C22A 1.59(12) .
C22 H22' 1.0000 .
C22A H22A 0.9800 .
C22A H22B 0.9800 .
C22A H22C 0.9800 .
C22B H22D 0.9800 .
C22B H22E 0.9800 .
C22B H22F 0.9800 .
C23 C23B 1.42(3) .
C23 C23A 1.43(3) .
C23 H23A 1.0000 .
C23A H23B 0.9800 .
C23A H23C 0.9800 .
C23A H23D 0.9800 .
C23B H23E 0.9800 .
C23B H23F 0.9800 .
C23B H23G 0.9800 .
C23' C23C 1.38(3) .
C23' C23D 1.42(3) .
C23' H23H 1.0000 .
C23C H23I 0.9800 .
C23C H23J 0.9800 .
C23C H23K 0.9800 .
C23D H23L 0.9800 .
C23D H23M 0.9800 .
C23D H23N 0.9800 .
C31 C32 1.37(3) .
C31 C36 1.41(3) .
C32 C33 1.41(4) .
C32 H32A 0.9500 .
C33 C34 1.43(5) .
C33 H33A 0.9500 .
C34 C35 1.35(4) .
C34 H34A 0.9500 .
C35 C36 1.42(3) .
C35 H35A 0.9500 .
C36 C37 1.48(3) 2_765
