#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/96/7219689.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_7219689
loop_
_publ_author_name
'Zhang, Lina'
'Zhang, Chao'
'Zhang, Bin'
'Du, Chenxia'
'Hou, Hongwei'
_publ_section_title
;
 Two series of pH-dependent lanthanide complexes showing solvent-induced
 single crystal to single crystal transformation, sorption and
 luminescence properties
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2837
_journal_paper_doi               10.1039/C5CE00263J
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C73.5 H56.5 N1.5 O22 Pr2, C3 H7 N O, C3 N O'
_chemical_formula_sum            'C79.5 H71.5 N3.5 O24 Pr2'
_chemical_formula_weight         1741.66
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-17
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_audit_update_record
;
2015-01-16 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.0122(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.26463(15)
_cell_length_b                   29.8504(3)
_cell_length_c                   18.2812(2)
_cell_measurement_reflns_used    14085
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.2105
_cell_measurement_theta_min      2.8650
_cell_volume                     7443.61(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega   -3.00   25.00   0.5000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000  150.0000 56

  2 omega  -48.00   39.00   0.5000   23.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -57.0000  -30.0000 174

  3 omega  -10.00   23.00   0.5000   23.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -57.0000  150.0000 66

  4 omega    9.00   89.00   0.5000   23.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   57.0000  120.0000 160
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0408611000
_diffrn_orient_matrix_UB_12      -0.0020858000
_diffrn_orient_matrix_UB_13      0.0330671000
_diffrn_orient_matrix_UB_21      0.0018029000
_diffrn_orient_matrix_UB_22      0.0236493000
_diffrn_orient_matrix_UB_23      0.0042456000
_diffrn_orient_matrix_UB_31      -0.0320904000
_diffrn_orient_matrix_UB_32      -0.0013564000
_diffrn_orient_matrix_UB_33      0.0230978000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32578
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  0.84020
_exptl_absorpt_correction_T_min  0.80811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3500
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         15633
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0311P)²+13.3200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                12669
_reflns_number_total             15633
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00263j2.cif
_cod_data_source_block           Pr-p21c
_cod_depositor_comments
'Adding full bibliography for 7219688--7219700.cif.'
_cod_original_cell_volume        7443.61(15)
_cod_original_formula_sum        'C79.50 H71.50 N3.50 O24 Pr2'
_cod_database_code               7219689
#BEGIN Tags that were not found in dictionaries:
_chemical_oxdiff_formula         C30H3O6N2Pr2
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'
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
Pr1 Pr 0.312898(8) 0.256892(4) 0.175717(8) 0.02271(3) Uani 1 1 d . . .
Pr2 Pr 0.173654(9) 0.331119(4) 0.322843(8) 0.02381(3) Uani 1 1 d . . .
O1 O 0.34919(12) 0.32080(8) 0.37922(13) 0.0492(6) Uani 1 1 d . . .
O2 O 0.40814(13) 0.27871(8) 0.30236(12) 0.0480(6) Uani 1 1 d . . .
O3 O 0.59006(13) 0.25972(8) 0.33654(11) 0.0568(7) Uani 1 1 d . . .
H3 H 0.5320 0.2601 0.3117 0.085 Uiso 1 1 calc R . .
O4 O 1.12866(16) 0.19880(7) 0.69310(12) 0.0529(7) Uani 1 1 d . . .
O5 O 1.13644(13) 0.24942(9) 0.60885(13) 0.0555(7) Uani 1 1 d . . .
O6 O 0.98259(12) 0.27545(7) 0.50533(11) 0.0401(5) Uani 1 1 d . . .
H6 H 1.0384 0.2773 0.5344 0.060 Uiso 1 1 calc R . .
O7 O 0.17051(15) 0.25125(6) 0.33431(12) 0.0439(6) Uani 1 1 d . . .
O8 O 0.24389(13) 0.21327(6) 0.26197(11) 0.0401(5) Uani 1 1 d . . .
O9 O 0.24280(13) 0.12643(6) 0.27311(13) 0.0471(6) Uani 1 1 d . . .
H9 H 0.2617 0.1510 0.2632 0.071 Uiso 1 1 calc R . .
O10 O 0.16040(13) 0.40270(6) 0.38864(11) 0.0421(5) Uani 1 1 d . . .
O11 O 0.06160(13) 0.39855(6) 0.27131(11) 0.0400(5) Uani 1 1 d . . .
O12 O -0.05033(14) 0.46468(6) 0.21271(11) 0.0401(5) Uani 1 1 d . . .
H12 H -0.0205 0.4410 0.2148 0.060 Uiso 1 1 calc R . .
O13 O 0.31990(14) 0.33802(6) 0.17406(12) 0.0451(6) Uani 1 1 d . . .
O14 O 0.25465(13) 0.37748(7) 0.24964(12) 0.0424(5) Uani 1 1 d . . .
O15 O 0.27660(14) 0.46285(7) 0.25982(13) 0.0563(6) Uani 1 1 d . . .
H15 H 0.2594 0.4380 0.2702 0.084 Uiso 1 1 calc R . .
O16 O 0.30255(14) 0.18216(6) 0.10928(11) 0.0401(5) Uani 1 1 d . . .
O17 O 0.41456(13) 0.18559(6) 0.22112(11) 0.0371(5) Uani 1 1 d . . .
O18 O 0.54119(14) 0.12328(6) 0.26561(11) 0.0422(6) Uani 1 1 d . . .
H18 H 0.5151 0.1478 0.2651 0.063 Uiso 1 1 calc R . .
O19 O 0.47400(14) 0.26581(8) 0.15512(14) 0.0576(7) Uani 1 1 d . . .
O20 O 0.28275(17) 0.27694(7) 0.03552(12) 0.0524(6) Uani 1 1 d . . .
O21 O 0.00601(13) 0.31492(8) 0.33834(15) 0.0597(7) Uani 1 1 d . . .
H21A H 0.0099 0.3106 0.3866 0.090 Uiso 1 1 d R . .
H21B H -0.0335 0.3376 0.3215 0.090 Uiso 1 1 d R . .
O22 O 0.19220(14) 0.30734(7) 0.46003(11) 0.0407(5) Uani 1 1 d . . .
H22A H 0.2148 0.2791 0.4685 0.061 Uiso 1 1 d R . .
H22B H 0.2347 0.3250 0.4941 0.061 Uiso 1 1 d R . .
O23 O 0.83173(18) 0.35699(11) 0.30093(18) 0.0862(10) Uani 1 1 d . . .
O24 O 0.1477(8) 0.3548(4) 0.0185(7) 0.193(3) Uiso 0.478(6) 1 d P A 1
O24A O 0.2338(8) 0.4448(4) -0.0187(6) 0.193(3) Uiso 0.522(6) 1 d P A 2
N1 N 0.63528(17) 0.27040(10) 0.16673(16) 0.0557(7) Uani 1 1 d U . .
N2 N 0.3670(4) 0.3181(2) -0.0249(3) 0.0587(14) Uani 0.50 1 d PU . .
N3 N 0.7338(2) 0.41522(11) 0.30815(19) 0.0690(8) Uani 1 1 d U . .
N4 N 0.1361(3) 0.42245(17) 0.0256(3) 0.1361(18) Uiso 1 1 d D A .
C1 C 0.41916(17) 0.30223(10) 0.36240(16) 0.0365(7) Uani 1 1 d . . .
C2 C 0.52121(17) 0.30698(10) 0.41563(15) 0.0331(7) Uani 1 1 d . . .
C3 C 0.53694(18) 0.33284(9) 0.48017(15) 0.0343(7) Uani 1 1 d . . .
H3A H 0.4836 0.3458 0.4917 0.041 Uiso 1 1 calc R . .
C4 C 0.63204(17) 0.34028(9) 0.52943(15) 0.0316(7) Uani 1 1 d . . .
C5 C 0.6480(2) 0.36856(11) 0.59342(17) 0.0442(8) Uani 1 1 d . . .
H5 H 0.5946 0.3812 0.6050 0.053 Uiso 1 1 calc R . .
C6 C 0.7409(2) 0.37785(12) 0.63908(18) 0.0520(9) Uani 1 1 d . . .
H6A H 0.7504 0.3964 0.6815 0.062 Uiso 1 1 calc R . .
C7 C 0.8213(2) 0.35898(11) 0.62076(18) 0.0468(9) Uani 1 1 d . . .
H7 H 0.8846 0.3659 0.6505 0.056 Uiso 1 1 calc R . .
C8 C 0.80854(18) 0.33073(10) 0.56038(16) 0.0356(7) Uani 1 1 d . . .
H8 H 0.8633 0.3184 0.5502 0.043 Uiso 1 1 calc R . .
C9 C 0.71363(16) 0.31952(9) 0.51227(14) 0.0275(6) Uani 1 1 d . . .
C10 C 0.69796(16) 0.29050(9) 0.44815(14) 0.0270(6) Uani 1 1 d . . .
C11 C 0.60347(17) 0.28555(10) 0.40024(15) 0.0328(7) Uani 1 1 d . . .
C12 C 0.78279(17) 0.26771(10) 0.42851(14) 0.0327(7) Uani 1 1 d . . .
H12A H 0.8290 0.2905 0.4235 0.039 Uiso 1 1 calc R . .
H12B H 0.7578 0.2532 0.3792 0.039 Uiso 1 1 calc R . .
C13 C 1.08925(19) 0.22035(10) 0.63303(16) 0.0384(8) Uani 1 1 d . . .
C14 C 0.98587(17) 0.21095(9) 0.58712(15) 0.0322(7) Uani 1 1 d . . .
C15 C 0.93953(19) 0.17355(10) 0.60195(16) 0.0391(7) Uani 1 1 d . . .
H15A H 0.9713 0.1553 0.6429 0.047 Uiso 1 1 calc R . .
C16 C 0.8444(2) 0.16207(10) 0.55637(18) 0.0426(8) Uani 1 1 d . . .
C17 C 0.8024(2) 0.12005(12) 0.5640(2) 0.0638(10) Uani 1 1 d . . .
H17 H 0.8358 0.1003 0.6021 0.077 Uiso 1 1 calc R . .
C18 C 0.7132(3) 0.10844(13) 0.5157(2) 0.0720(12) Uani 1 1 d . . .
H18A H 0.6869 0.0804 0.5199 0.086 Uiso 1 1 calc R . .
C19 C 0.6619(2) 0.13807(13) 0.4608(2) 0.0671(11) Uani 1 1 d . . .
H19 H 0.6010 0.1297 0.4285 0.081 Uiso 1 1 calc R . .
C20 C 0.69838(19) 0.17941(11) 0.45262(19) 0.0482(9) Uani 1 1 d . . .
H20 H 0.6612 0.1992 0.4162 0.058 Uiso 1 1 calc R . .
C21 C 0.79264(17) 0.19254(10) 0.49930(15) 0.0327(7) Uani 1 1 d . . .
C22 C 0.83764(16) 0.23304(9) 0.48659(14) 0.0279(6) Uani 1 1 d . . .
C23 C 0.93566(16) 0.23985(9) 0.52609(14) 0.0284(6) Uani 1 1 d . . .
C24 C 0.18516(19) 0.21614(9) 0.30158(15) 0.0310(7) Uani 1 1 d . . .
C25 C 0.12952(19) 0.17538(9) 0.31034(15) 0.0313(6) Uani 1 1 d . . .
C26 C 0.0447(2) 0.17977(10) 0.33100(16) 0.0394(7) Uani 1 1 d . . .
H26 H 0.0255 0.2081 0.3421 0.047 Uiso 1 1 calc R . .
C27 C -0.01344(19) 0.14268(10) 0.33574(17) 0.0401(7) Uani 1 1 d . . .
C28 C -0.1018(2) 0.14745(12) 0.3564(2) 0.0591(9) Uani 1 1 d . . .
H28 H -0.1218 0.1758 0.3668 0.071 Uiso 1 1 calc R . .
C29 C -0.1573(2) 0.11129(13) 0.3611(2) 0.0644(10) Uani 1 1 d . . .
H29 H -0.2156 0.1150 0.3734 0.077 Uiso 1 1 calc R . .
C30 C -0.1271(2) 0.06874(12) 0.34744(19) 0.0556(9) Uani 1 1 d . . .
H30 H -0.1647 0.0441 0.3520 0.067 Uiso 1 1 calc R . .
C31 C -0.0431(2) 0.06248(11) 0.32748(17) 0.0442(8) Uani 1 1 d . . .
H31 H -0.0246 0.0336 0.3186 0.053 Uiso 1 1 calc R . .
C32 C 0.01657(18) 0.09905(10) 0.31998(15) 0.0349(7) Uani 1 1 d . . .
C33 C 0.10391(18) 0.09413(9) 0.29713(16) 0.0318(6) Uani 1 1 d . . .
C34 C 0.15814(18) 0.13144(9) 0.29332(16) 0.0335(7) Uani 1 1 d . . .
C35 C 0.13558(18) 0.04817(9) 0.27605(16) 0.0338(7) Uani 1 1 d . . .
H35A H 0.1973 0.0514 0.2643 0.041 Uiso 1 1 calc R . .
H35B H 0.1468 0.0286 0.3201 0.041 Uiso 1 1 calc R . .
C36 C 0.09403(18) 0.41969(9) 0.33450(16) 0.0331(7) Uani 1 1 d . . .
C37 C 0.05179(18) 0.46436(9) 0.34381(16) 0.0327(7) Uani 1 1 d . . .
C38 C 0.08233(19) 0.48595(10) 0.41271(17) 0.0392(8) Uani 1 1 d . . .
H38 H 0.1300 0.4726 0.4527 0.047 Uiso 1 1 calc R . .
C39 C 0.0437(2) 0.52798(10) 0.42495(16) 0.0380(7) Uani 1 1 d . . .
C40 C 0.0766(2) 0.55076(12) 0.49603(19) 0.0532(9) Uani 1 1 d . . .
H40 H 0.1274 0.5386 0.5352 0.064 Uiso 1 1 calc R . .
C41 C 0.0351(3) 0.59001(11) 0.5078(2) 0.0578(10) Uani 1 1 d . . .
H41 H 0.0590 0.6051 0.5540 0.069 Uiso 1 1 calc R . .
C42 C -0.0427(2) 0.60733(11) 0.45105(19) 0.0537(9) Uani 1 1 d . . .
H42 H -0.0728 0.6334 0.4606 0.064 Uiso 1 1 calc R . .
C43 C -0.0767(2) 0.58718(10) 0.38106(18) 0.0438(8) Uani 1 1 d . . .
H43 H -0.1293 0.5997 0.3439 0.053 Uiso 1 1 calc R . .
C44 C -0.03232(18) 0.54719(9) 0.36455(16) 0.0346(7) Uani 1 1 d . . .
C45 C -0.06147(17) 0.52611(9) 0.29181(16) 0.0321(7) Uani 1 1 d . . .
C46 C -0.02113(17) 0.48538(9) 0.28236(15) 0.0306(6) Uani 1 1 d . . .
C47 C 0.30682(19) 0.37407(9) 0.20459(16) 0.0325(7) Uani 1 1 d . B .
C48 C 0.35677(18) 0.41567(9) 0.18872(15) 0.0320(7) Uani 1 1 d U . .
C49 C 0.4098(4) 0.4141(2) 0.1381(3) 0.0307(8) Uani 0.489(3) 1 d PU B 1
H49 H 0.4132 0.3879 0.1116 0.037 Uiso 0.489(3) 1 calc PR B 1
C49A C 0.4339(4) 0.4113(2) 0.1556(3) 0.0307(8) Uani 0.511(3) 1 d PU B 2
H49A H 0.4494 0.3827 0.1426 0.037 Uiso 0.511(3) 1 calc PR B 2
C50 C 0.4599(4) 0.4531(2) 0.1264(4) 0.0325(9) Uani 0.489(3) 1 d P B 1
C50A C 0.4888(4) 0.4474(2) 0.1411(4) 0.0325(9) Uani 0.511(3) 1 d P B 2
C51 C 0.5209(5) 0.4495(3) 0.0746(4) 0.0577(13) Uani 0.489(3) 1 d P B 1
H51 H 0.5257 0.4225 0.0506 0.069 Uiso 0.489(3) 1 calc PR B 1
C51A C 0.5634(5) 0.4456(3) 0.1086(4) 0.0577(13) Uani 0.511(3) 1 d P B 2
H51A H 0.5780 0.4180 0.0910 0.069 Uiso 0.511(3) 1 calc PR B 2
C52 C 0.5697(5) 0.4858(3) 0.0624(4) 0.0624(13) Uani 0.489(3) 1 d P B 1
H52 H 0.6095 0.4837 0.0303 0.075 Uiso 0.489(3) 1 calc PR B 1
C52A C 0.6180(5) 0.4816(3) 0.1002(4) 0.0624(13) Uani 0.511(3) 1 d P B 2
H52A H 0.6694 0.4782 0.0789 0.075 Uiso 0.511(3) 1 calc PR B 2
C53 C 0.5621(5) 0.5272(2) 0.0972(4) 0.0506(12) Uani 0.489(3) 1 d P B 1
H53 H 0.5980 0.5515 0.0880 0.061 Uiso 0.489(3) 1 calc PR B 1
C53A C 0.5958(5) 0.5238(2) 0.1240(4) 0.0506(12) Uani 0.511(3) 1 d P B 2
H53A H 0.6297 0.5492 0.1168 0.061 Uiso 0.511(3) 1 calc PR B 2
C54 C 0.5043(4) 0.5331(2) 0.1437(3) 0.0344(9) Uani 0.489(3) 1 d P B 1
H54 H 0.4931 0.5613 0.1611 0.041 Uiso 0.489(3) 1 calc PR B 1
C54A C 0.5230(5) 0.5265(2) 0.1581(4) 0.0344(9) Uani 0.511(3) 1 d P B 2
H54A H 0.5144 0.5541 0.1787 0.041 Uiso 0.511(3) 1 calc PR B 2
C55 C 0.46009(19) 0.49225(9) 0.16527(16) 0.0363(7) Uani 1 1 d . . .
C56 C 0.39402(18) 0.49547(9) 0.20988(16) 0.0315(6) Uani 1 1 d . B .
C57 C 0.34142(18) 0.45816(9) 0.21857(16) 0.0340(7) Uani 1 1 d . B .
C58 C 0.38326(18) 0.53898(9) 0.24965(17) 0.0352(7) Uani 1 1 d . . .
H58A H 0.3341 0.5347 0.2761 0.042 Uiso 1 1 calc R B .
H58B H 0.3588 0.5617 0.2109 0.042 Uiso 1 1 calc R . .
C59 C 0.37290(18) 0.16417(9) 0.16028(15) 0.0319(7) Uani 1 1 d . . .
C60 C 0.40688(17) 0.11850(9) 0.14884(15) 0.0292(6) Uani 1 1 d . . .
C61 C 0.35804(18) 0.09386(9) 0.08591(16) 0.0349(7) Uani 1 1 d . . .
H61 H 0.3035 0.1063 0.0506 0.042 Uiso 1 1 calc R . .
C62 C 0.38799(19) 0.05037(9) 0.07323(16) 0.0353(7) Uani 1 1 d . . .
C63 C 0.3361(2) 0.02556(11) 0.00829(19) 0.0471(9) Uani 1 1 d . . .
H63 H 0.2830 0.0386 -0.0275 0.056 Uiso 1 1 calc R . .
C64 C 0.3624(2) -0.01735(11) -0.0030(2) 0.0553(10) Uani 1 1 d . . .
H64 H 0.3262 -0.0338 -0.0450 0.066 Uiso 1 1 calc R . .
C65 C 0.4447(2) -0.03588(11) 0.04967(19) 0.0532(9) Uani 1 1 d . . .
H65 H 0.4632 -0.0650 0.0420 0.064 Uiso 1 1 calc R . .
C66 C 0.4986(2) -0.01278(10) 0.11179(18) 0.0432(8) Uani 1 1 d . . .
H66 H 0.5541 -0.0260 0.1447 0.052 Uiso 1 1 calc R . .
C67 C 0.47147(18) 0.03137(9) 0.12747(16) 0.0342(7) Uani 1 1 d . . .
C68 C 0.52365(17) 0.05665(9) 0.19307(15) 0.0303(6) Uani 1 1 d . . .
C69 C 0.49104(17) 0.09942(9) 0.20332(15) 0.0301(6) Uani 1 1 d . . .
C70 C 0.5567(2) 0.24902(12) 0.1683(2) 0.0542(9) Uani 1 1 d . . .
H70 H 0.5630 0.2187 0.1802 0.065 Uiso 1 1 calc R . .
C71 C 0.6307(3) 0.31766(15) 0.1498(3) 0.0877(12) Uani 1 1 d U . .
H71A H 0.6125 0.3219 0.0954 0.132 Uiso 1 1 calc R . .
H71B H 0.6937 0.3310 0.1728 0.132 Uiso 1 1 calc R . .
H71C H 0.5827 0.3315 0.1699 0.132 Uiso 1 1 calc R . .
C72 C 0.7312(2) 0.24984(16) 0.1853(3) 0.0819(14) Uani 1 1 d U . .
H72A H 0.7738 0.2640 0.2298 0.123 Uiso 1 1 calc R . .
H72B H 0.7577 0.2534 0.1430 0.123 Uiso 1 1 calc R . .
H72C H 0.7257 0.2185 0.1953 0.123 Uiso 1 1 calc R . .
C73 C 0.3085(6) 0.3103(3) 0.0115(4) 0.074(2) Uani 0.50 1 d PU . .
H73 H 0.2780 0.3359 0.0224 0.089 Uiso 0.50 1 calc PR . .
C74 C 0.4203(6) 0.2861(3) -0.0411(4) 0.076(2) Uani 0.50 1 d PU . .
H74A H 0.4876 0.2903 -0.0121 0.114 Uiso 0.50 1 calc PR . .
H74B H 0.4146 0.2869 -0.0947 0.114 Uiso 0.50 1 calc PR . .
H74C H 0.3977 0.2577 -0.0284 0.114 Uiso 0.50 1 calc PR . .
C75 C 0.3877(6) 0.3595(3) -0.0528(4) 0.0715(17) Uani 0.50 1 d PU . .
H75A H 0.3337 0.3795 -0.0574 0.107 Uiso 0.50 1 calc PR . .
H75B H 0.3976 0.3554 -0.1021 0.107 Uiso 0.50 1 calc PR . .
H75C H 0.4459 0.3719 -0.0181 0.107 Uiso 0.50 1 calc PR . .
C76 C 0.8075(2) 0.39610(16) 0.2907(2) 0.0715(13) Uani 1 1 d . . .
H76 H 0.8447 0.4142 0.2685 0.086 Uiso 1 1 calc R . .
C77 C 0.6712(3) 0.38978(17) 0.3400(3) 0.0995(13) Uani 1 1 d U . .
H77A H 0.6724 0.4021 0.3888 0.149 Uiso 1 1 calc R . .
H77B H 0.6934 0.3593 0.3464 0.149 Uiso 1 1 calc R . .
H77C H 0.6055 0.3908 0.3063 0.149 Uiso 1 1 calc R . .
C78 C 0.7117(3) 0.46231(15) 0.2982(3) 0.0940(16) Uani 1 1 d U . .
H78A H 0.6437 0.4662 0.2706 0.141 Uiso 1 1 calc R . .
H78B H 0.7516 0.4758 0.2701 0.141 Uiso 1 1 calc R . .
H78C H 0.7251 0.4764 0.3474 0.141 Uiso 1 1 calc R . .
C79 C 0.1909(7) 0.3829(3) 0.0006(6) 0.253(5) Uiso 1 1 d D . .
C80 C 0.1828(6) 0.4668(3) 0.0083(4) 0.157(3) Uiso 1 1 d . . .
C81 C 0.0668(5) 0.4391(3) 0.0649(5) 0.213(4) Uiso 1 1 d D . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
O2 Pr1 O5 134.88(8) . 4_465
O2 Pr1 O8 75.28(7) . .
O2 Pr1 O13 74.21(7) . .
O2 Pr1 O16 129.75(7) . .
O2 Pr1 O17 78.88(7) . .
O2 Pr1 O19 80.07(8) . .
O2 Pr1 O20 141.95(7) . .
O2 Pr1 C59 104.44(7) . .
O5 Pr1 O16 77.65(7) 4_465 .
O5 Pr1 O17 119.65(7) 4_465 .
O5 Pr1 O20 70.78(8) 4_465 .
O5 Pr1 C59 99.47(8) 4_465 .
O8 Pr1 O5 74.65(7) . 4_465
O8 Pr1 O16 82.11(7) . .
O8 Pr1 O17 69.45(6) . .
O8 Pr1 O20 142.06(7) . .
O8 Pr1 C59 75.24(7) . .
O13 Pr1 O5 96.32(7) . 4_465
O13 Pr1 O8 124.20(7) . .
O13 Pr1 O16 150.91(7) . .
O13 Pr1 O17 144.01(6) . .
O13 Pr1 O19 81.12(8) . .
O13 Pr1 O20 75.39(7) . .
O13 Pr1 C59 157.91(7) . .
O16 Pr1 O17 51.10(6) . .
O16 Pr1 O20 75.77(7) . .
O16 Pr1 C59 25.54(6) . .
O17 Pr1 C59 25.59(6) . .
O19 Pr1 O5 143.19(8) . 4_465
O19 Pr1 O8 136.46(7) . .
O19 Pr1 O16 86.99(8) . .
O19 Pr1 O17 70.96(7) . .
O19 Pr1 O20 73.09(8) . .
O19 Pr1 C59 76.97(8) . .
O20 Pr1 O17 115.66(7) . .
O20 Pr1 C59 95.34(7) . .
O1 Pr2 O4 108.13(8) . 4_465
O1 Pr2 O10 96.80(7) . .
O1 Pr2 O11 134.97(7) . .
O1 Pr2 O14 73.15(7) . .
O1 Pr2 O21 144.70(8) . .
O1 Pr2 O22 75.51(7) . .
O1 Pr2 C36 117.35(7) . .
O4 Pr2 O10 138.58(7) 4_465 .
O4 Pr2 O11 88.39(7) 4_465 .
O4 Pr2 O14 72.91(7) 4_465 .
O4 Pr2 O21 92.89(8) 4_465 .
O4 Pr2 O22 141.12(7) 4_465 .
O4 Pr2 C36 114.01(7) 4_465 .
O7 Pr2 O1 83.12(7) . .
O7 Pr2 O4 73.39(7) . 4_465
O7 Pr2 O10 143.82(7) . .
O7 Pr2 O11 141.79(6) . .
O7 Pr2 O14 129.57(7) . .
O7 Pr2 O21 75.99(8) . .
O7 Pr2 O22 68.61(7) . .
O7 Pr2 C36 151.69(8) . .
O10 Pr2 O11 51.50(6) . .
O10 Pr2 O21 84.39(7) . .
O10 Pr2 O22 76.33(7) . .
O10 Pr2 C36 25.46(6) . .
O11 Pr2 C36 26.04(6) . .
O14 Pr2 O10 83.86(7) . .
O14 Pr2 O11 72.44(7) . .
O14 Pr2 O21 141.57(7) . .
O14 Pr2 O22 140.35(6) . .
O14 Pr2 C36 77.43(7) . .
O21 Pr2 O11 71.62(7) . .
O21 Pr2 O22 70.50(7) . .
O21 Pr2 C36 76.35(8) . .
O22 Pr2 O11 116.98(7) . .
O22 Pr2 C36 96.40(7) . .
C1 O1 Pr2 138.19(18) . .
C1 O2 Pr1 150.60(17) . .
C13 O4 Pr2 164.2(2) . 4_666
C13 O5 Pr1 110.35(17) . 4_666
C24 O7 Pr2 141.27(19) . .
C24 O8 Pr1 142.16(17) . .
C36 O10 Pr2 96.43(16) . .
C36 O11 Pr2 91.93(15) . .
C47 O13 Pr1 147.3(2) . .
C47 O14 Pr2 140.81(18) . .
C59 O16 Pr1 95.62(16) . .
C59 O17 Pr1 93.37(15) . .
C70 O19 Pr1 144.0(2) . .
C73 O20 Pr1 126.2(4) . .
C70 N1 C71 120.0(3) . .
C70 N1 C72 123.4(3) . .
C71 N1 C72 116.5(3) . .
C73 N2 C74 121.0(8) . .
C73 N2 C75 127.7(8) . .
C74 N2 C75 111.4(7) . .
C76 N3 C77 120.7(4) . .
C76 N3 C78 123.7(4) . .
C77 N3 C78 115.6(4) . .
C80 N4 C79 107.7(6) . .
C81 N4 C79 150.3(7) . .
C81 N4 C80 101.6(6) . .
O1 C1 O2 123.2(2) . .
O1 C1 C2 119.2(3) . .
O2 C1 C2 117.5(2) . .
C3 C2 C1 119.6(2) . .
C3 C2 C11 118.8(2) . .
C11 C2 C1 121.6(2) . .
C2 C3 C4 121.5(2) . .
C3 C4 C9 118.9(2) . .
C5 C4 C3 121.2(3) . .
C5 C4 C9 119.8(2) . .
C6 C5 C4 121.4(3) . .
C5 C6 C7 119.0(3) . .
C8 C7 C6 121.2(3) . .
C7 C8 C9 121.7(3) . .
C8 C9 C4 116.8(2) . .
C10 C9 C4 120.2(2) . .
C10 C9 C8 123.0(2) . .
C9 C10 C12 121.6(2) . .
C11 C10 C9 118.4(2) . .
C11 C10 C12 119.9(2) . .
O3 C11 C2 120.1(2) . .
O3 C11 C10 117.9(2) . .
C10 C11 C2 122.0(2) . .
C10 C12 C22 114.9(2) . .
O4 C13 O5 120.9(2) . .
O4 C13 C14 120.7(3) . .
O5 C13 C14 118.3(2) . .
C15 C14 C13 119.9(2) . .
C15 C14 C23 119.2(2) . .
C23 C14 C13 120.9(2) . .
C14 C15 C16 121.3(3) . .
C15 C16 C17 121.2(3) . .
C15 C16 C21 118.8(3) . .
C17 C16 C21 119.9(3) . .
C18 C17 C16 120.2(3) . .
C17 C18 C19 120.3(3) . .
C20 C19 C18 121.5(3) . .
C19 C20 C21 120.5(3) . .
C16 C21 C20 117.5(3) . .
C16 C21 C22 120.3(2) . .
C22 C21 C20 122.0(3) . .
C21 C22 C12 121.9(2) . .
C23 C22 C12 119.8(2) . .
C23 C22 C21 118.3(2) . .
O6 C23 C14 120.8(2) . .
O6 C23 C22 118.0(2) . .
C22 C23 C14 121.1(2) . .
O7 C24 O8 124.2(3) . .
O7 C24 C25 117.6(3) . .
O8 C24 C25 118.2(2) . .
C26 C25 C24 119.5(2) . .
C26 C25 C34 118.4(2) . .
C34 C25 C24 122.0(2) . .
C25 C26 C27 121.8(3) . .
C26 C27 C28 121.6(3) . .
C26 C27 C32 119.4(3) . .
C28 C27 C32 119.1(3) . .
C29 C28 C27 121.0(3) . .
C28 C29 C30 119.9(3) . .
C31 C30 C29 121.2(3) . .
C30 C31 C32 121.3(3) . .
C27 C32 C33 119.4(2) . .
C31 C32 C27 117.4(3) . .
C31 C32 C33 123.2(3) . .
C32 C33 C35 120.8(2) . .
C34 C33 C32 118.9(2) . .
C34 C33 C35 120.3(2) . .
O9 C34 C25 119.2(2) . .
C33 C34 O9 118.7(2) . .
C33 C34 C25 122.1(2) . .
C45 C35 C33 114.0(2) 2_545 .
O10 C36 Pr2 58.10(14) . .
O10 C36 O11 120.1(2) . .
O10 C36 C37 120.4(2) . .
O11 C36 Pr2 62.03(13) . .
O11 C36 C37 119.5(2) . .
C37 C36 Pr2 177.2(2) . .
C38 C37 C36 119.7(2) . .
C38 C37 C46 118.6(2) . .
C46 C37 C36 121.7(2) . .
C37 C38 C39 122.0(3) . .
C38 C39 C40 122.0(3) . .
C38 C39 C44 118.6(3) . .
C40 C39 C44 119.4(3) . .
C41 C40 C39 121.0(3) . .
C40 C41 C42 119.8(3) . .
C43 C42 C41 121.7(3) . .
C42 C43 C44 120.6(3) . .
C39 C44 C43 117.3(3) . .
C45 C44 C39 119.8(2) . .
C45 C44 C43 122.9(2) . .
C44 C45 C35 121.0(2) . 2
C46 C45 C35 119.7(2) . 2
C46 C45 C44 119.4(2) . .
O12 C46 C37 119.1(2) . .
O12 C46 C45 119.4(2) . .
C45 C46 C37 121.5(2) . .
O13 C47 O14 123.5(3) . .
O13 C47 C48 118.9(3) . .
O14 C47 C48 117.5(2) . .
C49 C48 C47 119.7(3) . .
C49 C48 C57 118.1(3) . .
C49A C48 C47 118.8(3) . .
C49A C48 C57 118.3(3) . .
C57 C48 C47 121.9(3) . .
C48 C49 C50 118.9(5) . .
C50A C49A C48 124.1(5) . .
C49 C50 C51 117.4(6) . .
C55 C50 C49 123.3(5) . .
C55 C50 C51 119.1(5) . .
C49A C50A C55 114.4(5) . .
C51A C50A C49A 127.1(6) . .
C51A C50A C55 118.5(5) . .
C52 C51 C50 118.8(7) . .
C52A C51A C50A 124.4(7) . .
C51 C52 C53 121.4(7) . .
C51A C52A C53A 119.0(7) . .
C54 C53 C52 122.5(7) . .
C54A C53A C52A 118.0(6) . .
C53 C54 C55 116.4(5) . .
C53A C54A C55 126.8(6) . .
C50 C55 C54 120.2(4) . .
C50 C55 C54A 118.8(4) . .
C50 C55 C56 117.1(3) . .
C54 C55 C50A 118.8(4) . .
C54A C55 C50A 112.8(4) . .
C54A C55 C56 124.0(4) . .
C56 C55 C50A 120.9(3) . .
C56 C55 C54 120.3(3) . .
C55 C56 C58 120.7(2) . .
C57 C56 C55 119.2(2) . .
C57 C56 C58 120.1(2) . .
O15 C57 C48 120.7(2) . .
O15 C57 C56 117.5(2) . .
C56 C57 C48 121.7(3) . .
C56 C58 C68 115.8(2) . 2_655
O16 C59 Pr1 58.84(14) . .
O16 C59 C60 120.4(2) . .
O17 C59 Pr1 61.04(13) . .
O17 C59 O16 119.8(2) . .
O17 C59 C60 119.9(2) . .
C60 C59 Pr1 176.0(2) . .
C61 C60 C59 120.3(2) . .
C61 C60 C69 119.1(2) . .
C69 C60 C59 120.6(2) . .
C60 C61 C62 121.9(2) . .
C61 C62 C63 120.9(2) . .
C61 C62 C67 119.0(2) . .
C63 C62 C67 120.2(3) . .
C64 C63 C62 121.3(3) . .
C63 C64 C65 118.6(3) . .
C66 C65 C64 122.1(3) . .
C65 C66 C67 121.1(3) . .
C62 C67 C66 116.6(2) . .
C62 C67 C68 119.9(2) . .
C66 C67 C68 123.5(2) . .
C67 C68 C58 122.0(2) . 2_645
C69 C68 C58 118.9(2) . 2_645
C69 C68 C67 119.1(2) . .
O18 C69 C60 120.2(2) . .
O18 C69 C68 118.7(2) . .
C68 C69 C60 121.1(2) . .
O19 C70 N1 125.2(3) . .
O20 C73 N2 133.6(9) . .
O23 C76 N3 126.2(4) . .
O24 C79 N4 96.5(10) . .
O24A C80 N4 88.0(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr1 O2 2.4062(19) .
Pr1 O5 2.4628(18) 4_465
Pr1 O8 2.461(2) .
Pr1 O13 2.4243(19) .
Pr1 O16 2.5236(19) .
Pr1 O17 2.5725(18) .
Pr1 O19 2.449(2) .
Pr1 O20 2.543(2) .
Pr1 C59 2.935(3) .
Pr2 O1 2.4325(17) .
Pr2 O4 2.438(2) 4_465
Pr2 O7 2.3950(19) .
Pr2 O10 2.4863(19) .
Pr2 O11 2.5714(18) .
Pr2 O14 2.438(2) .
Pr2 O21 2.536(2) .
Pr2 O22 2.5447(19) .
Pr2 C36 2.910(3) .
O1 C1 1.256(3) .
O2 C1 1.273(4) .
O3 C11 1.363(3) .
O4 Pr2 2.438(2) 4_666
O4 C13 1.255(3) .
O5 Pr1 2.4628(17) 4_666
O5 C13 1.255(4) .
O6 C23 1.368(3) .
O7 C24 1.254(3) .
O8 C24 1.260(3) .
O9 C34 1.370(3) .
O10 C36 1.259(3) .
O11 C36 1.278(3) .
O12 C46 1.366(3) .
O13 C47 1.251(3) .
O14 C47 1.265(4) .
O15 C57 1.361(4) .
O16 C59 1.272(3) .
O17 C59 1.270(3) .
O18 C69 1.356(3) .
O19 C70 1.239(4) .
O20 C73 1.189(9) .
O23 C76 1.216(5) .
O24 C79 1.145(16) .
O24A C80 1.189(13) .
N1 C70 1.297(4) .
N1 C71 1.442(5) .
N1 C72 1.447(4) .
N2 C73 1.233(10) .
N2 C74 1.307(10) .
N2 C75 1.400(10) .
N3 C76 1.315(5) .
N3 C77 1.420(5) .
N3 C78 1.440(5) .
N4 C79 1.557(8) .
N4 C80 1.556(9) .
N4 C81 1.467(7) .
C1 C2 1.502(3) .
C2 C3 1.372(4) .
C2 C11 1.435(4) .
C3 C4 1.409(3) .
C4 C5 1.406(4) .
C4 C9 1.432(4) .
C5 C6 1.372(4) .
C6 C7 1.404(5) .
C7 C8 1.358(4) .
C8 C9 1.422(3) .
C9 C10 1.422(4) .
C10 C11 1.384(3) .
C10 C12 1.520(4) .
C12 C22 1.525(4) .
C13 C14 1.495(3) .
C14 C15 1.364(4) .
C14 C23 1.426(4) .
C15 C16 1.412(4) .
C16 C17 1.414(5) .
C16 C21 1.418(4) .
C17 C18 1.365(5) .
C18 C19 1.377(5) .
C19 C20 1.364(5) .
C20 C21 1.421(3) .
C21 C22 1.419(4) .
C22 C23 1.388(3) .
C24 C25 1.487(4) .
C25 C26 1.375(4) .
C25 C34 1.435(4) .
C26 C27 1.401(4) .
C27 C28 1.425(4) .
C27 C32 1.426(4) .
C28 C29 1.356(5) .
C29 C30 1.387(5) .
C30 C31 1.364(4) .
C31 C32 1.415(4) .
C32 C33 1.433(4) .
C33 C34 1.369(4) .
C33 C35 1.529(4) .
C35 C45 1.524(4) 2_545
C36 C37 1.493(4) .
C37 C38 1.368(4) .
C37 C46 1.433(3) .
C38 C39 1.414(4) .
C39 C40 1.419(4) .
C39 C44 1.422(4) .
C40 C41 1.358(5) .
C41 C42 1.379(5) .
C42 C43 1.368(4) .
C43 C44 1.424(4) .
C44 C45 1.419(4) .
C45 C35 1.524(4) 2
C45 C46 1.377(4) .
C47 C48 1.501(4) .
C48 C49 1.357(7) .
C48 C49A 1.408(7) .
C48 C57 1.423(4) .
C49 C50 1.413(8) .
C49A C50A 1.403(9) .
C50 C51 1.465(10) .
C50 C55 1.368(7) .
C50A C51A 1.363(10) .
C50A C55 1.504(7) .
C51 C52 1.344(10) .
C51A C52A 1.361(10) .
C52 C53 1.408(10) .
C52A C53A 1.399(11) .
C53 C54 1.357(10) .
C53A C54A 1.361(10) .
C54 C55 1.477(7) .
C54A C55 1.392(7) .
C55 C56 1.418(4) .
C56 C57 1.378(4) .
C56 C58 1.518(4) .
C58 C68 1.525(3) 2_655
C59 C60 1.482(4) .
C60 C61 1.371(4) .
C60 C69 1.434(3) .
C61 C62 1.407(4) .
C62 C63 1.411(4) .
C62 C67 1.425(4) .
C63 C64 1.367(4) .
C64 C65 1.397(4) .
C65 C66 1.358(4) .
C66 C67 1.426(4) .
C67 C68 1.428(4) .
C68 C58 1.525(3) 2_645
C68 C69 1.390(4) .
