#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/72/7007246.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_7007246
loop_
_publ_author_name
'Natrajan, Louise S.'
'Blake, Alexander J.'
'Wilson, Claire'
'Weinstein, Julia A.'
'Arnold, Polly L.'
_publ_section_title
;
 Group I cation templated formation of luminescent mono- and
 bis-substituted thionaphthol heterobimetallic complexes of Pr, Nd, Eu
 and Tb.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4465
_journal_page_last               4473
_journal_paper_doi               10.1039/b602242a
_journal_year                    2006
_chemical_formula_moiety         'C66 H100 K O8 Pr S. 0.6(C4 H10 O)'
_chemical_formula_sum            'C68.4 H106 K O8.6 Pr S'
_chemical_formula_weight         1278.00
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom, Et2O H omitted'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.917(2)
_cell_angle_beta                 104.844(2)
_cell_angle_gamma                91.941(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0568(14)
_cell_length_b                   15.356(2)
_cell_length_c                   21.298(3)
_cell_measurement_reflns_used    7571
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.25
_cell_volume                     3470.0(8)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'SHELXL-97; enCIFer (CCDC, 2003); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_sigmaI/netI    0.069
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31401
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS version 2.01a; Sheldrick, 1996)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1358
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.74
_refine_diff_density_rms         0.10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         16042
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.050P)²+2.518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.102
_refine_ls_wR_factor_ref         0.116
_reflns_number_gt                11993
_reflns_number_total             16042
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b602242a.txt
_cod_data_source_block           PRDITH_compound_1a
_cod_original_cell_volume        3470.0(13)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C68.40 H106 K O8.60 Pr S'
_cod_database_code               7007246
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K K 0.86060(8) 0.71773(6) 0.88856(4) 0.03507(19) Uani 1 1 d . A .
S1 S 0.50493(8) 0.75454(5) 0.75993(4) 0.02341(17) Uani 1 1 d . A .
Pr Pr 0.714843(18) 0.653578(13) 0.710717(9) 0.02431(6) Uani 1 1 d . A .
O1 O 0.7769(2) 0.78751(15) 0.78133(11) 0.0262(5) Uani 1 1 d . . .
O2 O 0.6556(2) 0.60647(15) 0.79971(12) 0.0296(5) Uani 1 1 d . . .
O3 O 0.9226(2) 0.63189(16) 0.78298(11) 0.0276(5) Uani 1 1 d . . .
O4 O 0.7643(2) 0.50333(17) 0.69300(13) 0.0349(6) Uani 1 1 d . . .
O5 O 0.6157(2) 0.74078(18) 0.62853(12) 0.0347(6) Uani 1 1 d . . .
O6 O 0.8416(2) 0.67190(18) 0.63638(12) 0.0378(6) Uani 1 1 d . . .
O7 O 0.5086(2) 0.56765(19) 0.64842(14) 0.0423(7) Uani 1 1 d D . .
O8 O 0.9020(3) 0.7496(2) 1.02140(14) 0.0500(8) Uani 1 1 d D . .
C11 C 0.5872(3) 0.8581(2) 0.76553(15) 0.0227(7) Uani 1 1 d . . .
C12 C 0.7164(3) 0.8594(2) 0.77342(15) 0.0228(7) Uani 1 1 d . . .
C13 C 0.7833(3) 0.9421(2) 0.77190(16) 0.0260(7) Uani 1 1 d . . .
C14 C 0.7153(3) 1.0140(2) 0.75977(16) 0.0249(7) Uani 1 1 d . . .
H14A H 0.7591 1.0679 0.7586 0.030 Uiso 1 1 calc R . .
C15 C 0.5193(3) 1.0900(2) 0.73641(16) 0.0273(7) Uani 1 1 d . . .
H15A H 0.5661 1.1422 0.7344 0.033 Uiso 1 1 calc R . .
C16 C 0.3916(3) 1.0922(2) 0.72708(17) 0.0285(8) Uani 1 1 d . . .
C17 C 0.3259(3) 1.0116(2) 0.72815(18) 0.0310(8) Uani 1 1 d . . .
H17A H 0.2373 1.0103 0.7207 0.037 Uiso 1 1 calc R . .
C18 C 0.3849(3) 0.9359(2) 0.73945(17) 0.0277(7) Uani 1 1 d . . .
H18A H 0.3364 0.8835 0.7390 0.033 Uiso 1 1 calc R . .
C19 C 0.5168(3) 0.9338(2) 0.75176(15) 0.0226(7) Uani 1 1 d . . .
C20 C 0.5834(3) 1.0129(2) 0.74889(16) 0.0239(7) Uani 1 1 d . . .
C21 C 0.5408(3) 0.7170(2) 0.83944(16) 0.0231(7) Uani 1 1 d . . .
C22 C 0.6037(3) 0.6397(2) 0.84517(16) 0.0242(7) Uani 1 1 d . A .
C23 C 0.6157(3) 0.5959(2) 0.90381(17) 0.0259(7) Uani 1 1 d . . .
C24 C 0.5702(3) 0.6360(2) 0.95283(17) 0.0266(7) Uani 1 1 d . . .
H24A H 0.5811 0.6092 0.9920 0.032 Uiso 1 1 calc R . .
C25 C 0.4581(3) 0.7510(2) 0.99975(16) 0.0258(7) Uani 1 1 d . . .
H25A H 0.4706 0.7229 1.0384 0.031 Uiso 1 1 calc R . .
C26 C 0.3922(3) 0.8253(2) 0.99538(16) 0.0243(7) Uani 1 1 d . . .
C27 C 0.3792(3) 0.8669(2) 0.93794(17) 0.0260(7) Uani 1 1 d . . .
H27A H 0.3362 0.9194 0.9343 0.031 Uiso 1 1 calc R . .
C28 C 0.4261(3) 0.8343(2) 0.88755(16) 0.0250(7) Uani 1 1 d . . .
H28A H 0.4151 0.8646 0.8500 0.030 Uiso 1 1 calc R C .
C29 C 0.4908(3) 0.7560(2) 0.89026(16) 0.0237(7) Uani 1 1 d . . .
C30 C 0.5083(3) 0.7148(2) 0.94848(16) 0.0239(7) Uani 1 1 d . . .
C31 C 1.0039(3) 0.5756(2) 0.78010(17) 0.0286(8) Uani 1 1 d . . .
C32 C 0.9772(3) 0.4925(2) 0.74562(19) 0.0330(8) Uani 1 1 d . . .
H32A H 1.0445 0.4549 0.7490 0.040 Uiso 1 1 calc R . .
C33 C 0.8598(3) 0.4592(2) 0.70629(18) 0.0328(8) Uani 1 1 d . . .
C41 C 0.6310(3) 0.7677(2) 0.57677(17) 0.0311(8) Uani 1 1 d . . .
C42 C 0.7350(4) 0.7512(3) 0.55247(18) 0.0368(9) Uani 1 1 d . . .
H42A H 0.7374 0.7726 0.5125 0.044 Uiso 1 1 calc R . .
C43 C 0.8356(4) 0.7053(3) 0.58347(19) 0.0361(9) Uani 1 1 d . . .
C51 C 0.4347(8) 0.5136(7) 0.6781(4) 0.074(3) Uiso 0.60 1 d PD A 1
H51A H 0.4113 0.5481 0.7146 0.088 Uiso 0.60 1 calc PR A 1
H51B H 0.4816 0.4635 0.6949 0.088 Uiso 0.60 1 calc PR A 1
C51' C 0.3991(8) 0.5538(7) 0.6718(5) 0.047(3) Uiso 0.40 1 d PD A 2
H51C H 0.3534 0.6080 0.6728 0.056 Uiso 0.40 1 calc PR A 2
H51D H 0.4225 0.5354 0.7163 0.056 Uiso 0.40 1 calc PR A 2
C52 C 0.3198(6) 0.4822(4) 0.6237(3) 0.091(2) Uiso 1 1 d D . .
H52A H 0.2458 0.5128 0.6303 0.109 Uiso 1 1 calc R A 1
H52B H 0.3023 0.4183 0.6223 0.109 Uiso 1 1 calc R A 1
C53 C 0.3488(7) 0.5033(7) 0.5606(4) 0.066(2) Uiso 0.60 1 d PD A 1
H53A H 0.3351 0.4504 0.5283 0.079 Uiso 0.60 1 calc PR A 1
H53B H 0.2957 0.5494 0.5412 0.079 Uiso 0.60 1 calc PR A 1
C53' C 0.3919(16) 0.4577(9) 0.5735(9) 0.118(7) Uiso 0.40 1 d PD A 2
H53C H 0.3353 0.4494 0.5288 0.142 Uiso 0.40 1 calc PR A 2
H53D H 0.4351 0.4030 0.5822 0.142 Uiso 0.40 1 calc PR A 2
C54 C 0.4864(5) 0.5355(4) 0.5818(3) 0.0705(15) Uiso 1 1 d D A .
H54A H 0.5405 0.4868 0.5760 0.085 Uiso 1 1 calc R B 1
H54B H 0.5029 0.5825 0.5560 0.085 Uiso 1 1 calc R B 1
C61 C 0.9227(9) 0.6491(7) 1.1026(6) 0.072(3) Uani 0.60 1 d PD C 1
H61A H 0.9831 0.6199 1.1345 0.109 Uiso 0.60 1 calc PR C 1
H61B H 0.8687 0.6050 1.0701 0.109 Uiso 0.60 1 calc PR C 1
H61C H 0.8712 0.6847 1.1251 0.109 Uiso 0.60 1 calc PR C 1
C62 C 0.9920(7) 0.7072(8) 1.0690(5) 0.059(3) Uani 0.60 1 d PD C 1
H62A H 1.0466 0.7520 1.1016 0.070 Uiso 0.60 1 calc PR C 1
H62B H 1.0454 0.6718 1.0468 0.070 Uiso 0.60 1 calc PR C 1
C61' C 1.0124(13) 0.7030(9) 1.1288(5) 0.059(3) Uani 0.40 1 d PD C 2
H61D H 1.0195 0.6529 1.1543 0.089 Uiso 0.40 1 calc PR C 2
H61E H 0.9811 0.7522 1.1519 0.089 Uiso 0.40 1 calc PR C 2
H61F H 1.0950 0.7203 1.1235 0.089 Uiso 0.40 1 calc PR C 2
C62' C 0.9228(17) 0.6777(8) 1.0626(6) 0.068(4) Uani 0.40 1 d PD C 2
H62C H 0.9557 0.6284 1.0396 0.081 Uiso 0.40 1 calc PR C 2
H62D H 0.8412 0.6567 1.0686 0.081 Uiso 0.40 1 calc PR C 2
C63 C 0.8311(5) 0.8112(3) 1.0482(3) 0.0686(15) Uani 1 1 d D C .
H63A H 0.8842 0.8442 1.0889 0.082 Uiso 1 1 calc R . .
H63B H 0.7600 0.7806 1.0589 0.082 Uiso 1 1 calc R . .
C64 C 0.7839(6) 0.8719(4) 0.9995(3) 0.0790(18) Uani 1 1 d D . .
H64A H 0.7344 0.9151 1.0171 0.119 Uiso 1 1 calc R C .
H64B H 0.7312 0.8388 0.9595 0.119 Uiso 1 1 calc R . .
H64C H 0.8549 0.9022 0.9894 0.119 Uiso 1 1 calc R . .
C130 C 0.9261(3) 0.9467(2) 0.78049(19) 0.0310(8) Uani 1 1 d . . .
C131 C 0.9936(4) 0.9166(3) 0.8463(2) 0.0545(12) Uani 1 1 d . . .
H13A H 1.0843 0.9196 0.8511 0.082 Uiso 1 1 calc R . .
H13B H 0.9646 0.8560 0.8479 0.082 Uiso 1 1 calc R . .
H13C H 0.9751 0.9548 0.8820 0.082 Uiso 1 1 calc R . .
C132 C 0.9766(4) 1.0408(3) 0.7795(3) 0.0487(11) Uani 1 1 d . . .
H13D H 1.0674 1.0418 0.7849 0.073 Uiso 1 1 calc R . .
H13E H 0.9588 1.0792 0.8153 0.073 Uiso 1 1 calc R . .
H13F H 0.9358 1.0616 0.7377 0.073 Uiso 1 1 calc R . .
C133 C 0.9573(4) 0.8894(3) 0.7242(2) 0.0436(10) Uani 1 1 d . . .
H13G H 1.0483 0.8926 0.7300 0.065 Uiso 1 1 calc R . .
H13H H 0.9160 0.9104 0.6826 0.065 Uiso 1 1 calc R . .
H13I H 0.9277 0.8285 0.7240 0.065 Uiso 1 1 calc R . .
C160 C 0.3219(4) 1.1757(3) 0.7172(2) 0.0358(9) Uani 1 1 d . . .
C161 C 0.2139(4) 1.1605(3) 0.6557(2) 0.0547(12) Uani 1 1 d . . .
H16A H 0.1579 1.1115 0.6592 0.082 Uiso 1 1 calc R . .
H16B H 0.2471 1.1465 0.6176 0.082 Uiso 1 1 calc R . .
H16C H 0.1673 1.2136 0.6506 0.082 Uiso 1 1 calc R . .
C162 C 0.4072(4) 1.2526(3) 0.7102(3) 0.0523(12) Uani 1 1 d . . .
H16D H 0.4416 1.2376 0.6727 0.079 Uiso 1 1 calc R . .
H16E H 0.4759 1.2649 0.7500 0.079 Uiso 1 1 calc R . .
H16F H 0.3586 1.3046 0.7033 0.079 Uiso 1 1 calc R . .
C163 C 0.2699(4) 1.2013(3) 0.7765(2) 0.0467(11) Uani 1 1 d . . .
H16G H 0.2144 1.1529 0.7817 0.070 Uiso 1 1 calc R . .
H16H H 0.2226 1.2538 0.7696 0.070 Uiso 1 1 calc R . .
H16I H 0.3395 1.2133 0.8160 0.070 Uiso 1 1 calc R . .
C230 C 0.6733(3) 0.5063(2) 0.90785(18) 0.0293(8) Uani 1 1 d . C .
C231 C 0.5935(4) 0.4406(3) 0.8519(2) 0.0449(10) Uani 1 1 d . . .
H23A H 0.5065 0.4379 0.8549 0.067 Uiso 1 1 calc R C .
H23B H 0.6267 0.3824 0.8554 0.067 Uiso 1 1 calc R . .
H23C H 0.5966 0.4597 0.8098 0.067 Uiso 1 1 calc R . .
C232 C 0.6734(4) 0.4699(3) 0.9722(2) 0.0380(9) Uani 1 1 d . . .
H23D H 0.7239 0.5101 1.0090 0.057 Uiso 1 1 calc R C .
H23E H 0.7092 0.4124 0.9726 0.057 Uiso 1 1 calc R . .
H23F H 0.5872 0.4638 0.9761 0.057 Uiso 1 1 calc R . .
C233 C 0.8094(4) 0.5103(3) 0.9031(2) 0.0410(10) Uani 1 1 d . . .
H23G H 0.8603 0.5522 0.9387 0.061 Uiso 1 1 calc R C .
H23H H 0.8125 0.5292 0.8610 0.061 Uiso 1 1 calc R . .
H23I H 0.8423 0.4521 0.9067 0.061 Uiso 1 1 calc R . .
C260 C 0.3352(3) 0.8650(2) 1.04964(17) 0.0277(7) Uani 1 1 d . . .
C261 C 0.1959(3) 0.8794(3) 1.02081(19) 0.0365(9) Uani 1 1 d . . .
H26A H 0.1877 0.9177 0.9861 0.055 Uiso 1 1 calc R . .
H26B H 0.1609 0.9069 1.0553 0.055 Uiso 1 1 calc R . .
H26C H 0.1502 0.8228 1.0027 0.055 Uiso 1 1 calc R . .
C262 C 0.4063(4) 0.9534(2) 1.08023(19) 0.0379(9) Uani 1 1 d . . .
H26D H 0.4019 0.9923 1.0462 0.057 Uiso 1 1 calc R . .
H26E H 0.4942 0.9437 1.1004 0.057 Uiso 1 1 calc R . .
H26F H 0.3681 0.9804 1.1136 0.057 Uiso 1 1 calc R . .
C263 C 0.3423(4) 0.8051(3) 1.10337(18) 0.0358(9) Uani 1 1 d . . .
H26G H 0.2972 0.7487 1.0843 0.054 Uiso 1 1 calc R . .
H26H H 0.3042 0.8326 1.1366 0.054 Uiso 1 1 calc R . .
H26I H 0.4303 0.7957 1.1236 0.054 Uiso 1 1 calc R . .
C310 C 1.1402(3) 0.6077(3) 0.81577(18) 0.0337(8) Uani 1 1 d . C .
C311 C 1.1815(4) 0.6705(3) 0.7724(2) 0.0489(11) Uani 1 1 d . . .
H31A H 1.1783 0.6386 0.7296 0.073 Uiso 1 1 calc R . .
H31B H 1.2674 0.6943 0.7933 0.073 Uiso 1 1 calc R . .
H31C H 1.1252 0.7187 0.7666 0.073 Uiso 1 1 calc R . .
C312 C 1.2311(4) 0.5347(3) 0.8261(3) 0.0578(13) Uani 1 1 d . . .
H31D H 1.2052 0.4940 0.8534 0.087 Uiso 1 1 calc R . .
H31E H 1.3158 0.5602 0.8478 0.087 Uiso 1 1 calc R . .
H31F H 1.2307 0.5030 0.7837 0.087 Uiso 1 1 calc R . .
C313 C 1.1450(4) 0.6574(3) 0.8822(2) 0.0452(10) Uani 1 1 d . . .
H31G H 1.1189 0.6174 0.9099 0.068 Uiso 1 1 calc R C .
H31H H 1.0883 0.7054 0.8763 0.068 Uiso 1 1 calc R . .
H31I H 1.2308 0.6815 0.9031 0.068 Uiso 1 1 calc R . .
C330 C 0.8400(4) 0.3638(3) 0.6735(2) 0.0484(11) Uani 1 1 d . . .
C331 C 0.7938(6) 0.3676(4) 0.5987(3) 0.0817(19) Uani 1 1 d . . .
H33A H 0.7173 0.3996 0.5891 0.123 Uiso 1 1 calc R . .
H33B H 0.7761 0.3078 0.5761 0.123 Uiso 1 1 calc R . .
H33C H 0.8589 0.3977 0.5837 0.123 Uiso 1 1 calc R . .
C332 C 0.7395(6) 0.3191(3) 0.6968(4) 0.088(2) Uani 1 1 d . . .
H33D H 0.7690 0.3163 0.7440 0.132 Uiso 1 1 calc R . .
H33E H 0.7198 0.2596 0.6740 0.132 Uiso 1 1 calc R . .
H33F H 0.6641 0.3524 0.6877 0.132 Uiso 1 1 calc R . .
C333 C 0.9585(5) 0.3134(3) 0.6858(3) 0.0657(15) Uani 1 1 d . . .
H33G H 0.9892 0.3088 0.7327 0.099 Uiso 1 1 calc R . .
H33H H 1.0228 0.3445 0.6709 0.099 Uiso 1 1 calc R . .
H33I H 0.9397 0.2545 0.6619 0.099 Uiso 1 1 calc R . .
C410 C 0.5276(4) 0.8248(3) 0.54293(18) 0.0392(9) Uani 1 1 d . . .
C411 C 0.4016(5) 0.7909(5) 0.5517(3) 0.088(2) Uani 1 1 d . . .
H41A H 0.3352 0.8269 0.5304 0.131 Uiso 1 1 calc R . .
H41B H 0.4060 0.7942 0.5985 0.131 Uiso 1 1 calc R . .
H41C H 0.3831 0.7298 0.5319 0.131 Uiso 1 1 calc R . .
C412 C 0.5581(6) 0.9168(3) 0.5779(3) 0.0795(19) Uani 1 1 d . . .
H41D H 0.6384 0.9396 0.5727 0.119 Uiso 1 1 calc R . .
H41E H 0.5637 0.9157 0.6245 0.119 Uiso 1 1 calc R . .
H41F H 0.4918 0.9546 0.5592 0.119 Uiso 1 1 calc R . .
C413 C 0.5174(5) 0.8261(4) 0.4706(2) 0.0615(14) Uani 1 1 d . . .
H41G H 0.5976 0.8482 0.4649 0.092 Uiso 1 1 calc R . .
H41H H 0.4515 0.8643 0.4522 0.092 Uiso 1 1 calc R . .
H41I H 0.4965 0.7665 0.4480 0.092 Uiso 1 1 calc R . .
C430 C 0.9511(4) 0.6940(3) 0.5558(2) 0.0453(10) Uani 1 1 d . . .
C431 C 0.9873(5) 0.5994(3) 0.5595(3) 0.0661(15) Uani 1 1 d . . .
H43A H 1.0605 0.5906 0.5422 0.099 Uiso 1 1 calc R . .
H43B H 0.9170 0.5596 0.5336 0.099 Uiso 1 1 calc R . .
H43C H 1.0076 0.5871 0.6052 0.099 Uiso 1 1 calc R . .
C432 C 1.0577(4) 0.7558(4) 0.5991(2) 0.0582(13) Uani 1 1 d . . .
H43D H 1.0346 0.8166 0.5964 0.087 Uiso 1 1 calc R . .
H43E H 1.1339 0.7476 0.5843 0.087 Uiso 1 1 calc R . .
H43F H 1.0729 0.7429 0.6445 0.087 Uiso 1 1 calc R . .
C433 C 0.9285(5) 0.7160(4) 0.4855(2) 0.0659(15) Uani 1 1 d . . .
H43G H 0.9068 0.7772 0.4836 0.099 Uiso 1 1 calc R . .
H43H H 0.8596 0.6773 0.4570 0.099 Uiso 1 1 calc R . .
H43I H 1.0048 0.7076 0.4707 0.099 Uiso 1 1 calc R . .
C1S C 0.8602(15) 0.0747(11) 0.5729(7) 0.125(5) Uiso 0.60 1 d PD . .
C2S C 0.8757(12) 0.0404(11) 0.5073(7) 0.135(5) Uiso 0.60 1 d PD . .
O1S O 1.0012(11) 0.0214(7) 0.5117(5) 0.121(3) Uiso 0.60 1 d PD . .
C3S C 1.0368(16) 0.0038(12) 0.4525(7) 0.151(6) Uiso 0.60 1 d PD . .
C4S C 1.1605(18) -0.0274(16) 0.4495(13) 0.199(10) Uiso 0.60 1 d PD . .
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'
S S 0.1246 0.1234 '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'
K K 0.2009 0.2494 '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 K O8 142.46(9) . . y
O1 K O3 66.50(7) . . ?
O8 K O3 148.90(8) . . ?
O1 K O2 69.48(7) . . y
O8 K O2 126.12(9) . . ?
O3 K O2 65.88(7) . . y
O1 K C22 78.90(9) . . y
O8 K C22 103.54(10) . . ?
O3 K C22 91.89(9) . . ?
O2 K C22 26.01(8) . . ?
O1 K C233 123.78(10) . . ?
O8 K C233 87.42(10) . . ?
O3 K C233 76.56(9) . . ?
O2 K C233 57.04(9) . . ?
C22 K C233 61.06(10) . . ?
O1 K C313 104.26(9) . . ?
O8 K C313 98.93(10) . . ?
O3 K C313 53.48(8) . . ?
O2 K C313 113.83(9) . . ?
C22 K C313 136.77(10) . . ?
C233 K C313 83.89(10) . . ?
O1 K C23 104.62(8) . . ?
O8 K C23 81.90(9) . . ?
O3 K C23 103.94(8) . . ?
O2 K C23 44.23(8) . . ?
C22 K C23 25.80(9) . . ?
C233 K C23 45.38(9) . . ?
C313 K C23 129.27(10) . . ?
O1 K C21 66.21(7) . . ?
O8 K C21 101.00(9) . . ?
O3 K C21 103.66(8) . . ?
O2 K C21 42.98(7) . . ?
C22 K C21 23.84(9) . . ?
C233 K C21 84.28(9) . . ?
C313 K C21 156.28(9) . . ?
C23 K C21 42.71(8) . . ?
O1 K C64 100.36(11) . . ?
O8 K C64 42.55(11) . . ?
O3 K C64 165.17(12) . . ?
O2 K C64 117.33(12) . . ?
C22 K C64 92.19(13) . . ?
C233 K C64 117.76(13) . . ?
C313 K C64 128.21(12) . . ?
C23 K C64 85.61(12) . . ?
C21 K C64 75.51(12) . . ?
O1 K Pr 39.45(5) . . ?
O8 K Pr 163.85(7) . . ?
O3 K Pr 41.47(5) . . ?
O2 K Pr 38.67(5) . . ?
C22 K Pr 60.33(7) . . ?
C233 K Pr 85.07(8) . . ?
C313 K Pr 94.46(7) . . ?
C23 K Pr 82.66(6) . . ?
C21 K Pr 64.06(6) . . ?
C64 K Pr 131.30(9) . . ?
C11 S1 C21 108.85(15) . . ?
C11 S1 Pr 91.97(11) . . ?
C21 S1 Pr 95.91(11) . . ?
O2 Pr O5 132.15(8) . . y
O2 Pr O1 83.76(8) . . y
O5 Pr O1 86.89(9) . . y
O2 Pr O6 158.51(8) . . y
O5 Pr O6 69.34(8) . . y
O1 Pr O6 99.19(9) . . y
O2 Pr O4 83.32(9) . . ?
O5 Pr O4 126.04(9) . . ?
O1 Pr O4 143.76(8) . . y
O6 Pr O4 81.91(9) . . ?
O2 Pr O3 79.74(8) . . y
O5 Pr O3 141.28(8) . . ?
O1 Pr O3 74.02(8) . . ?
O6 Pr O3 80.65(8) . . ?
O4 Pr O3 70.42(8) . . y
O2 Pr O7 81.43(9) . . y
O5 Pr O7 74.23(9) . . ?
O1 Pr O7 137.07(8) . . y
O6 Pr O7 109.04(9) . . ?
O4 Pr O7 73.60(9) . . ?
O3 Pr O7 140.91(9) . . ?
O2 Pr S1 62.24(6) . . ?
O5 Pr S1 71.95(6) . . ?
O1 Pr S1 62.07(6) . . y
O6 Pr S1 137.71(6) . . ?
O4 Pr S1 136.38(6) . . ?
O3 Pr S1 123.25(6) . . ?
O7 Pr S1 75.40(6) . . ?
O2 Pr K 51.46(7) . . ?
O5 Pr K 129.75(7) . . ?
O1 Pr K 43.58(6) . . ?
O6 Pr K 117.85(7) . . ?
O4 Pr K 103.87(6) . . ?
O3 Pr K 47.25(6) . . ?
O7 Pr K 132.30(6) . . ?
S1 Pr K 76.01(2) . . ?
C12 O1 Pr 123.5(2) . . ?
C12 O1 K 128.0(2) . . ?
Pr O1 K 96.97(8) . . ?
C22 O2 Pr 137.3(2) . . ?
C22 O2 K 77.30(18) . . ?
Pr O2 K 89.87(8) . . ?
C31 O3 Pr 133.1(2) . . ?
C31 O3 K 130.6(2) . . ?
Pr O3 K 91.29(7) . . ?
C33 O4 Pr 137.5(2) . . ?
C41 O5 Pr 139.8(2) . . ?
C43 O6 Pr 139.0(2) . . ?
C54 O7 C51' 111.4(5) . . ?
C54 O7 C51 108.7(5) . . ?
C54 O7 Pr 121.2(3) . . ?
C51' O7 Pr 127.1(4) . . ?
C51 O7 Pr 124.2(3) . . ?
C63 O8 C62 115.0(5) . . ?
C63 O8 C62' 107.9(8) . . ?
C63 O8 K 119.6(3) . . ?
C62 O8 K 125.4(5) . . ?
C62' O8 K 121.0(6) . . ?
C12 C11 C19 122.4(3) . . ?
C12 C11 S1 117.9(3) . . ?
C19 C11 S1 118.9(2) . . ?
O1 C12 C11 121.0(3) . . ?
O1 C12 C13 120.4(3) . . ?
C11 C12 C13 118.6(3) . . ?
C14 C13 C12 118.2(3) . . ?
C14 C13 C130 121.2(3) . . ?
C12 C13 C130 120.5(3) . . ?
C13 C14 C20 123.7(3) . . ?
C16 C15 C20 122.4(3) . . ?
C15 C16 C17 116.4(3) . . ?
C15 C16 C160 123.1(3) . . ?
C17 C16 C160 120.5(3) . . ?
C18 C17 C16 122.6(3) . . ?
C17 C18 C19 121.5(3) . . ?
C20 C19 C18 116.7(3) . . ?
C20 C19 C11 117.8(3) . . ?
C18 C19 C11 125.5(3) . . ?
C19 C20 C15 120.4(3) . . ?
C19 C20 C14 119.0(3) . . ?
C15 C20 C14 120.6(3) . . ?
C22 C21 C29 121.8(3) . . ?
C22 C21 S1 115.9(2) . . ?
C29 C21 S1 121.5(2) . . ?
C22 C21 K 57.78(18) . . ?
C29 C21 K 111.5(2) . . ?
S1 C21 K 105.64(13) . . ?
O2 C22 C21 121.6(3) . . ?
O2 C22 C23 119.0(3) . . ?
C21 C22 C23 119.3(3) . . ?
O2 C22 K 76.68(18) . . ?
C21 C22 K 98.4(2) . . ?
C23 C22 K 93.3(2) . . ?
C24 C23 C22 117.7(3) . . ?
C24 C23 C230 122.5(3) . . ?
C22 C23 C230 119.8(3) . . ?
C24 C23 K 109.4(2) . . ?
C22 C23 K 60.87(17) . . ?
C230 C23 K 99.6(2) . . ?
C23 C24 C30 123.8(3) . . ?
C26 C25 C30 122.2(3) . . ?
C25 C26 C27 117.1(3) . . ?
C25 C26 C260 123.3(3) . . ?
C27 C26 C260 119.6(3) . . ?
C28 C27 C26 122.5(3) . . ?
C27 C28 C29 121.2(3) . . ?
C28 C29 C30 117.2(3) . . ?
C28 C29 C21 124.7(3) . . ?
C30 C29 C21 118.1(3) . . ?
C24 C30 C25 121.1(3) . . ?
C24 C30 C29 119.1(3) . . ?
C25 C30 C29 119.7(3) . . ?
O3 C31 C32 124.5(3) . . ?
O3 C31 C310 115.0(3) . . ?
C32 C31 C310 120.4(3) . . ?
C31 C32 C33 125.8(3) . . ?
O4 C33 C32 124.3(4) . . ?
O4 C33 C330 114.7(3) . . ?
C32 C33 C330 121.0(3) . . ?
O5 C41 C42 123.9(3) . . ?
O5 C41 C410 114.7(3) . . ?
C42 C41 C410 121.3(3) . . ?
C43 C42 C41 123.8(3) . . ?
O6 C43 C42 123.7(3) . . ?
O6 C43 C430 115.2(3) . . ?
C42 C43 C430 121.1(3) . . ?
O7 C51 C52 104.7(5) . . ?
O7 C51' C52 105.1(6) . . ?
C51' C52 C53' 106.2(7) . . ?
C51 C52 C53' 94.9(9) . . ?
C51' C52 C53 100.7(6) . . ?
C51 C52 C53 106.2(6) . . ?
C54 C53 C52 104.0(5) . . ?
C52 C53' C54 104.1(7) . . ?
O7 C54 C53 104.9(5) . . ?
O7 C54 C53' 103.3(7) . . ?
O8 C62 C61 109.2(7) . . ?
O8 C62' C61' 113.7(9) . . ?
O8 C63 C64 108.2(5) . . ?
C63 C64 K 85.7(3) . . ?
C133 C130 C132 107.4(3) . . ?
C133 C130 C131 110.2(3) . . ?
C132 C130 C131 107.7(3) . . ?
C133 C130 C13 109.9(3) . . ?
C132 C130 C13 111.2(3) . . ?
C131 C130 C13 110.3(3) . . ?
C161 C160 C16 109.8(3) . . ?
C161 C160 C162 108.1(4) . . ?
C16 C160 C162 112.1(3) . . ?
C161 C160 C163 109.3(3) . . ?
C16 C160 C163 109.3(3) . . ?
C162 C160 C163 108.1(4) . . ?
C232 C230 C233 106.9(3) . . ?
C232 C230 C23 111.9(3) . . ?
C233 C230 C23 112.5(3) . . ?
C232 C230 C231 107.3(3) . . ?
C233 C230 C231 109.3(3) . . ?
C23 C230 C231 108.7(3) . . ?
C230 C233 K 102.4(2) . . ?
C263 C260 C26 112.3(3) . . ?
C263 C260 C261 107.2(3) . . ?
C26 C260 C261 109.9(3) . . ?
C263 C260 C262 108.9(3) . . ?
C26 C260 C262 108.9(3) . . ?
C261 C260 C262 109.6(3) . . ?
C313 C310 C312 108.5(3) . . ?
C313 C310 C311 109.4(4) . . ?
C312 C310 C311 108.8(4) . . ?
C313 C310 C31 110.0(3) . . ?
C312 C310 C31 114.3(3) . . ?
C311 C310 C31 105.8(3) . . ?
C310 C313 K 110.8(2) . . ?
C332 C330 C333 111.2(4) . . ?
C332 C330 C33 107.5(4) . . ?
C333 C330 C33 114.1(4) . . ?
C332 C330 C331 109.5(5) . . ?
C333 C330 C331 107.5(4) . . ?
C33 C330 C331 107.0(4) . . ?
C412 C410 C413 109.7(4) . . ?
C412 C410 C411 108.3(5) . . ?
C413 C410 C411 109.3(4) . . ?
C412 C410 C41 107.0(4) . . ?
C413 C410 C41 113.5(3) . . ?
C411 C410 C41 108.9(3) . . ?
C431 C430 C432 109.6(4) . . ?
C431 C430 C433 110.0(4) . . ?
C432 C430 C433 108.4(4) . . ?
C431 C430 C43 108.0(4) . . ?
C432 C430 C43 107.5(3) . . ?
C433 C430 C43 113.3(4) . . ?
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
K O1 2.590(2) . y
K O8 2.737(3) . y
K O3 2.739(2) . y
K O2 2.917(3) . y
K C22 2.925(3) . y
K C233 3.276(4) . y
K C313 3.340(4) . y
K C23 3.342(3) . y
K C21 3.420(3) . y
K C64 3.452(6) . y
K Pr 3.7296(10) . y
S1 C11 1.783(3) . y
S1 C21 1.797(3) . y
S1 Pr 3.1693(9) . y
Pr O2 2.331(2) . y
Pr O5 2.379(2) . y
Pr O1 2.388(2) . y
Pr O6 2.398(2) . y
Pr O4 2.404(3) . y
Pr O3 2.470(2) . y
Pr O7 2.567(3) . ?
O1 C12 1.314(4) . y
O2 C22 1.315(4) . y
O3 C31 1.276(4) . y
O4 C33 1.261(4) . y
O5 C41 1.264(4) . ?
O6 C43 1.273(4) . ?
O7 C54 1.410(5) . ?
O7 C51' 1.439(8) . ?
O7 C51 1.442(7) . ?
O8 C63 1.416(5) . ?
O8 C62 1.450(8) . ?
O8 C62' 1.469(9) . ?
C11 C12 1.395(5) . ?
C11 C19 1.433(5) . ?
C12 C13 1.454(5) . ?
C13 C14 1.366(5) . ?
C13 C130 1.541(5) . ?
C14 C20 1.416(5) . ?
C15 C16 1.377(5) . ?
C15 C20 1.415(5) . ?
C16 C17 1.419(5) . ?
C16 C160 1.524(5) . ?
C17 C18 1.365(5) . ?
C18 C19 1.416(5) . ?
C19 C20 1.414(5) . ?
C21 C22 1.397(5) . ?
C21 C29 1.425(4) . ?
C22 C23 1.457(5) . ?
C23 C24 1.371(5) . ?
C23 C230 1.537(5) . ?
C24 C30 1.410(5) . ?
C25 C26 1.374(5) . ?
C25 C30 1.420(4) . ?
C26 C27 1.415(5) . ?
C26 C260 1.536(4) . ?
C27 C28 1.365(4) . ?
C28 C29 1.418(5) . ?
C29 C30 1.422(5) . ?
C31 C32 1.388(5) . ?
C31 C310 1.542(5) . ?
C32 C33 1.399(5) . ?
C33 C330 1.540(5) . ?
C41 C42 1.398(5) . ?
C41 C410 1.539(5) . ?
C42 C43 1.393(5) . ?
C43 C430 1.546(5) . ?
C51 C52 1.509(7) . ?
C51' C52 1.506(8) . ?
C52 C53' 1.514(8) . ?
C52 C53 1.522(7) . ?
C53 C54 1.521(7) . ?
C53' C54 1.526(8) . ?
C61 C62 1.503(10) . ?
C61' C62' 1.506(11) . ?
C63 C64 1.474(7) . ?
C130 C133 1.532(5) . ?
C130 C132 1.535(5) . ?
C130 C131 1.536(6) . ?
C160 C161 1.521(6) . ?
C160 C162 1.530(6) . ?
C160 C163 1.538(6) . ?
C230 C232 1.532(5) . ?
C230 C233 1.534(5) . ?
C230 C231 1.539(6) . ?
C260 C263 1.529(5) . ?
C260 C261 1.538(5) . ?
C260 C262 1.538(5) . ?
C310 C313 1.525(5) . ?
C310 C312 1.525(6) . ?
C310 C311 1.537(6) . ?
C330 C332 1.501(7) . ?
C330 C333 1.522(6) . ?
C330 C331 1.551(7) . ?
C410 C412 1.512(6) . ?
C410 C413 1.518(5) . ?
C410 C411 1.534(7) . ?
C430 C431 1.524(7) . ?
C430 C432 1.526(7) . ?
C430 C433 1.529(6) . ?
C1S C2S 1.496(8) . ?
C2S O1S 1.408(8) . ?
O1S C3S 1.419(8) . ?
C3S C4S 1.479(8) . ?
