#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:57:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179221 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/45/4314537.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_4314537
loop_
_publ_author_name
'Qi-Bing Bo'
'Guo-Xin Sun'
'Dong-Ling Geng'
_publ_section_title
;
 Novel Three-Dimensional Pillared-Layer Ln(III)-Cu(I) Coordination
 Polymers Featuring Spindle-Shaped Heterometallic Building Units
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              561
_journal_page_last               571
_journal_paper_doi               10.1021/ic901730f
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C51 H33 Cu3 N9 O12 Pr, 5.5(H O0.50)'
_chemical_formula_sum            'C51 H43 Cu3 N9 O17 Pr'
_chemical_formula_weight         1385.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.239(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.738(2)
_cell_length_b                   10.59760(12)
_cell_length_c                   21.660(2)
_cell_measurement_reflns_used    10702
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.293
_cell_measurement_theta_min      2.741
_cell_volume                     5257.3(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25851
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  0.5231
_exptl_absorpt_correction_T_min  0.4598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         9239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0331
_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)+(0.0480P)²+5.7664P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                7369
_reflns_number_total             9239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901730f_si_002_1.cif
_cod_data_source_block           Pr-Cu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        5257.2(8)
_cod_database_code               4314537
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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 0.0000 0.77876(3) 0.7500 0.02399(9) Uani 1 2 d S . .
Pr2 Pr 0.5000 0.47456(3) 0.2500 0.02532(9) Uani 1 2 d S . .
Cu1 Cu 0.21171(2) 0.66814(6) 0.78968(2) 0.04243(15) Uani 1 1 d . . .
Cu2 Cu 0.26873(3) 0.63452(6) 0.30526(2) 0.04848(17) Uani 1 1 d . . .
Cu3 Cu 0.68646(3) 0.04926(5) 0.38387(2) 0.03968(15) Uani 1 1 d . . .
N1 N 0.04836(14) 0.9066(3) 0.67551(14) 0.0287(7) Uani 1 1 d . . .
N2 N 0.0000 0.5341(4) 0.7500 0.0238(10) Uani 1 2 d S . .
N3 N 0.48096(13) 0.3625(3) 0.35011(14) 0.0280(7) Uani 1 1 d . . .
N4 N 0.5000 0.7187(5) 0.2500 0.0356(12) Uani 1 2 d S . .
N5 N 0.22579(15) 0.6804(3) 0.70649(15) 0.0350(8) Uani 1 1 d . . .
N6 N 0.25886(16) 0.6560(3) 0.39020(15) 0.0358(8) Uani 1 1 d . . .
N7 N 0.22082(15) 0.6935(3) 0.87985(14) 0.0327(8) Uani 1 1 d . . .
N8 N 0.25695(16) 0.6583(3) 1.21508(15) 0.0340(8) Uani 1 1 d . . .
N9 N 0.69533(15) 0.0110(3) 0.47221(15) 0.0308(8) Uani 1 1 d . . .
N10 N 0.69204(15) -0.0482(3) 0.79777(14) 0.0310(8) Uani 1 1 d . . .
O1 O 0.07162(13) 0.9437(3) 0.80034(13) 0.0377(7) Uani 1 1 d . . .
O2 O 0.13583(13) 1.0963(3) 0.79765(15) 0.0461(8) Uani 1 1 d . . .
O3 O -0.02360(13) 0.7165(3) 0.63386(13) 0.0388(7) Uani 1 1 d . . .
O4 O -0.02366(17) 0.7484(4) 0.53305(15) 0.0644(10) Uani 1 1 d . . .
O5 O 0.09565(11) 0.6688(2) 0.75866(12) 0.0306(6) Uani 1 1 d . . .
O6 O 0.15206(11) 0.4983(3) 0.77449(13) 0.0335(7) Uani 1 1 d . . .
O7 O 0.40978(12) 0.5358(3) 0.28345(14) 0.0410(7) Uani 1 1 d . . .
O8 O 0.34855(14) 0.5124(4) 0.34476(15) 0.0574(10) Uani 1 1 d . . .
O9 O 0.56686(12) 0.2981(3) 0.30004(13) 0.0356(7) Uani 1 1 d . . .
O10 O 0.60329(13) 0.1631(3) 0.37977(13) 0.0410(7) Uani 1 1 d . . .
O11 O 0.44443(13) 0.5831(3) 0.15072(13) 0.0434(8) Uani 1 1 d . . .
O12 O 0.42143(15) 0.7522(3) 0.08846(15) 0.0563(9) Uani 1 1 d . . .
O13 O 0.92141(19) 0.4883(5) 0.9955(3) 0.1093(18) Uani 1 1 d . . .
H13C H 0.9360 0.4190 1.0121 0.131 Uiso 1 1 d R . .
H13D H 0.9286 0.4956 0.9592 0.131 Uiso 1 1 d R . .
O14 O 0.9512(3) 0.5230(6) 0.3816(3) 0.153(3) Uani 1 1 d . . .
H14C H 0.9704 0.4575 0.3770 0.184 Uiso 1 1 d R . .
H14D H 0.9754 0.5804 0.3985 0.184 Uiso 1 1 d R . .
O15 O 0.8942(2) 0.9567(6) 0.0657(2) 0.1130(19) Uani 1 1 d . . .
H15C H 0.9042 0.9847 0.1038 0.136 Uiso 1 1 d R . .
H15D H 0.9138 0.8902 0.0640 0.136 Uiso 1 1 d R . .
O16 O 0.9622(3) 0.7235(5) 0.0605(3) 0.126(2) Uani 1 1 d . . .
H16C H 0.9833 0.7456 0.0362 0.151 Uiso 1 1 d R . .
H16D H 0.9466 0.6529 0.0472 0.151 Uiso 1 1 d R . .
O17 O 0.5074(5) 0.9543(13) 0.0674(6) 0.147(5) Uani 0.50 1 d P . .
H17C H 0.4817 0.9001 0.0701 0.176 Uiso 0.50 1 d PR . .
H17D H 0.5002 0.9793 0.0288 0.176 Uiso 0.25 1 d PR . .
H17A H 0.5413 0.9222 0.0792 0.176 Uiso 0.25 1 d PR . .
O18 O 0.4024(5) 0.7896(12) 0.3552(6) 0.134(4) Uani 0.50 1 d P . .
H18A H 0.4117 0.7235 0.3378 0.161 Uiso 0.50 1 d PR . .
H18C H 0.4335 0.8260 0.3762 0.161 Uiso 0.50 1 d PR . .
C1 C 0.09969(17) 1.0162(4) 0.7719(2) 0.0319(9) Uani 1 1 d . . .
C2 C 0.08488(17) 1.0004(4) 0.6993(2) 0.0319(9) Uani 1 1 d . . .
C3 C 0.1078(2) 1.0775(5) 0.6610(2) 0.0475(12) Uani 1 1 d . . .
H3 H 0.1323 1.1440 0.6785 0.057 Uiso 1 1 calc R . .
C4 C 0.0939(2) 1.0544(5) 0.5961(2) 0.0546(13) Uani 1 1 d . . .
H4 H 0.1096 1.1042 0.5694 0.066 Uiso 1 1 calc R . .
C5 C 0.0562(2) 0.9564(5) 0.5709(2) 0.0484(12) Uani 1 1 d . . .
H5 H 0.0463 0.9394 0.5273 0.058 Uiso 1 1 calc R . .
C6 C 0.03373(18) 0.8845(4) 0.61209(19) 0.0331(9) Uani 1 1 d . . .
C7 C -0.00833(19) 0.7755(4) 0.59077(19) 0.0370(10) Uani 1 1 d . . .
C8 C 0.10348(16) 0.5509(4) 0.76396(17) 0.0244(8) Uani 1 1 d . . .
C9 C 0.05020(16) 0.4703(4) 0.75779(18) 0.0275(8) Uani 1 1 d . . .
C10 C 0.0519(2) 0.3400(4) 0.7591(2) 0.0465(12) Uani 1 1 d . . .
H10 H 0.0873 0.2974 0.7660 0.056 Uiso 1 1 calc R . .
C11 C 0.0000 0.2738(6) 0.7500 0.0553(19) Uani 1 2 d S . .
H11 H 0.0000 0.1861 0.7500 0.066 Uiso 1 2 calc SR . .
C12 C 0.39529(18) 0.4926(4) 0.33099(19) 0.0367(10) Uani 1 1 d . . .
C13 C 0.43885(18) 0.4069(4) 0.37503(19) 0.0360(10) Uani 1 1 d . . .
C14 C 0.4367(2) 0.3756(5) 0.4361(2) 0.0513(13) Uani 1 1 d . . .
H14 H 0.4069 0.4066 0.4526 0.062 Uiso 1 1 calc R . .
C15 C 0.4792(2) 0.2977(6) 0.4725(2) 0.0630(16) Uani 1 1 d . . .
H15 H 0.4789 0.2770 0.5141 0.076 Uiso 1 1 calc R . .
C16 C 0.5225(2) 0.2502(5) 0.4465(2) 0.0523(13) Uani 1 1 d . . .
H16 H 0.5511 0.1961 0.4698 0.063 Uiso 1 1 calc R . .
C17 C 0.52167(18) 0.2863(4) 0.38470(19) 0.0336(9) Uani 1 1 d . . .
C18 C 0.56769(17) 0.2447(4) 0.35208(18) 0.0288(9) Uani 1 1 d . . .
C19 C 0.44404(18) 0.6992(4) 0.1401(2) 0.0371(10) Uani 1 1 d . . .
C20 C 0.47293(19) 0.7823(4) 0.1971(2) 0.0421(11) Uani 1 1 d . . .
C21 C 0.4725(3) 0.9115(5) 0.1956(3) 0.0739(18) Uani 1 1 d . . .
H21 H 0.4539 0.9542 0.1583 0.089 Uiso 1 1 calc R . .
C22 C 0.5000 0.9774(8) 0.2500 0.085(3) Uani 1 2 d S . .
H22 H 0.5000 1.0652 0.2500 0.102 Uiso 1 2 calc SR . .
C23 C 0.1833(2) 0.7190(5) 0.6560(2) 0.0434(11) Uani 1 1 d . . .
H23 H 0.1485 0.7476 0.6631 0.052 Uiso 1 1 calc R . .
C24 C 0.1886(2) 0.7184(5) 0.59410(19) 0.0421(11) Uani 1 1 d . . .
H24 H 0.1581 0.7474 0.5608 0.050 Uiso 1 1 calc R . .
C25 C 0.23978(18) 0.6741(4) 0.58162(17) 0.0312(9) Uani 1 1 d . . .
C26 C 0.28397(18) 0.6350(4) 0.63424(18) 0.0320(9) Uani 1 1 d . . .
H26 H 0.3191 0.6055 0.6285 0.038 Uiso 1 1 calc R . .
C27 C 0.27538(19) 0.6403(4) 0.69532(18) 0.0340(10) Uani 1 1 d . . .
H27 H 0.3056 0.6147 0.7298 0.041 Uiso 1 1 calc R . .
C28 C 0.30533(19) 0.6674(4) 0.44110(19) 0.0379(10) Uani 1 1 d . . .
H28 H 0.3423 0.6715 0.4341 0.045 Uiso 1 1 calc R . .
C29 C 0.30063(18) 0.6732(4) 0.50310(18) 0.0350(10) Uani 1 1 d . . .
H29 H 0.3341 0.6815 0.5368 0.042 Uiso 1 1 calc R . .
C30 C 0.24651(17) 0.6668(4) 0.51556(17) 0.0292(9) Uani 1 1 d . . .
C31 C 0.19870(19) 0.6566(5) 0.46282(18) 0.0403(11) Uani 1 1 d . . .
H31 H 0.1613 0.6536 0.4686 0.048 Uiso 1 1 calc R . .
C32 C 0.2062(2) 0.6509(5) 0.40216(19) 0.0423(11) Uani 1 1 d . . .
H32 H 0.1733 0.6432 0.3678 0.051 Uiso 1 1 calc R . .
C33 C 0.17631(18) 0.7195(4) 0.90445(18) 0.0363(10) Uani 1 1 d . . .
H33 H 0.1402 0.7376 0.8765 0.044 Uiso 1 1 calc R . .
C34 C 0.18111(18) 0.7209(4) 0.96926(18) 0.0342(10) Uani 1 1 d . . .
H34 H 0.1487 0.7397 0.9841 0.041 Uiso 1 1 calc R . .
C35 C 0.23446(17) 0.6944(4) 1.01247(17) 0.0272(9) Uani 1 1 d . . .
C36 C 0.28142(18) 0.6712(4) 0.98702(18) 0.0312(9) Uani 1 1 d . . .
H36 H 0.3183 0.6562 1.0140 0.037 Uiso 1 1 calc R . .
C37 C 0.27314(18) 0.6705(4) 0.92165(18) 0.0333(10) Uani 1 1 d . . .
H37 H 0.3050 0.6534 0.9055 0.040 Uiso 1 1 calc R . .
C38 C 0.30109(19) 0.6928(4) 1.19057(19) 0.0376(10) Uani 1 1 d . . .
H38 H 0.3376 0.7063 1.2186 0.045 Uiso 1 1 calc R . .
C39 C 0.29500(18) 0.7091(4) 1.12654(18) 0.0335(10) Uani 1 1 d . . .
H39 H 0.3268 0.7351 1.1122 0.040 Uiso 1 1 calc R . .
C40 C 0.24138(17) 0.6870(4) 1.08266(17) 0.0263(8) Uani 1 1 d . . .
C41 C 0.19498(18) 0.6527(4) 1.10765(18) 0.0315(9) Uani 1 1 d . . .
H41 H 0.1580 0.6386 1.0806 0.038 Uiso 1 1 calc R . .
C42 C 0.20479(19) 0.6402(4) 1.17312(18) 0.0352(10) Uani 1 1 d . . .
H42 H 0.1734 0.6180 1.1891 0.042 Uiso 1 1 calc R . .
C43 C 0.64633(18) -0.0152(4) 0.48985(18) 0.0338(10) Uani 1 1 d . . .
H43 H 0.6116 -0.0241 0.4580 0.041 Uiso 1 1 calc R . .
C44 C 0.64487(18) -0.0294(4) 0.55228(18) 0.0341(10) Uani 1 1 d . . .
H44 H 0.6097 -0.0472 0.5619 0.041 Uiso 1 1 calc R . .
C45 C 0.69628(17) -0.0171(4) 0.60172(17) 0.0273(9) Uani 1 1 d . . .
C46 C 0.74735(18) 0.0074(4) 0.58319(18) 0.0308(9) Uani 1 1 d . . .
H46 H 0.7828 0.0152 0.6139 0.037 Uiso 1 1 calc R . .
C47 C 0.74503(18) 0.0200(4) 0.51937(18) 0.0326(9) Uani 1 1 d . . .
H47 H 0.7796 0.0357 0.5082 0.039 Uiso 1 1 calc R . .
C48 C 0.65130(19) -0.1028(4) 0.75046(18) 0.0380(10) Uani 1 1 d . . .
H48 H 0.6213 -0.1471 0.7609 0.046 Uiso 1 1 calc R . .
C49 C 0.65191(19) -0.0964(4) 0.68703(18) 0.0390(11) Uani 1 1 d . . .
H49 H 0.6229 -0.1367 0.6560 0.047 Uiso 1 1 calc R . .
C50 C 0.69567(18) -0.0301(4) 0.66943(17) 0.0291(9) Uani 1 1 d . . .
C51 C 0.73823(18) 0.0251(4) 0.71840(18) 0.0340(10) Uani 1 1 d . . .
H51 H 0.7688 0.0695 0.7092 0.041 Uiso 1 1 calc R . .
C52 C 0.73489(19) 0.0137(4) 0.78075(19) 0.0362(10) Uani 1 1 d . . .
H52 H 0.7640 0.0511 0.8128 0.043 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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 O1 90.47(14) . 2_556 ?
O1 Pr1 O5 149.30(9) . 2_556 ?
O1 Pr1 O5 78.04(9) 2_556 2_556 ?
O1 Pr1 O5 78.04(9) . . ?
O1 Pr1 O5 149.30(9) 2_556 . ?
O5 Pr1 O5 124.79(12) 2_556 . ?
O1 Pr1 O3 78.38(10) . 2_556 ?
O1 Pr1 O3 124.78(9) 2_556 2_556 ?
O5 Pr1 O3 84.99(9) 2_556 2_556 ?
O5 Pr1 O3 81.06(9) . 2_556 ?
O1 Pr1 O3 124.78(9) . . ?
O1 Pr1 O3 78.38(10) 2_556 . ?
O5 Pr1 O3 81.06(9) 2_556 . ?
O5 Pr1 O3 84.99(9) . . ?
O3 Pr1 O3 149.62(14) 2_556 . ?
O1 Pr1 N2 134.77(7) . . ?
O1 Pr1 N2 134.77(7) 2_556 . ?
O5 Pr1 N2 62.40(6) 2_556 . ?
O5 Pr1 N2 62.40(6) . . ?
O3 Pr1 N2 74.81(7) 2_556 . ?
O3 Pr1 N2 74.81(7) . . ?
O1 Pr1 N1 73.91(10) . 2_556 ?
O1 Pr1 N1 62.70(10) 2_556 2_556 ?
O5 Pr1 N1 75.53(9) 2_556 2_556 ?
O5 Pr1 N1 137.22(9) . 2_556 ?
O3 Pr1 N1 62.23(10) 2_556 2_556 ?
O3 Pr1 N1 137.71(10) . 2_556 ?
N2 Pr1 N1 121.49(7) . 2_556 ?
O1 Pr1 N1 62.70(10) . . ?
O1 Pr1 N1 73.91(10) 2_556 . ?
O5 Pr1 N1 137.22(9) 2_556 . ?
O5 Pr1 N1 75.53(9) . . ?
O3 Pr1 N1 137.71(10) 2_556 . ?
O3 Pr1 N1 62.23(10) . . ?
N2 Pr1 N1 121.49(7) . . ?
N1 Pr1 N1 117.02(14) 2_556 . ?
O11 Pr2 O11 124.97(14) 2_655 . ?
O11 Pr2 O9 148.17(9) 2_655 2_655 ?
O11 Pr2 O9 80.77(10) . 2_655 ?
O11 Pr2 O9 80.77(10) 2_655 . ?
O11 Pr2 O9 148.17(9) . . ?
O9 Pr2 O9 83.54(14) 2_655 . ?
O11 Pr2 O7 85.99(10) 2_655 . ?
O11 Pr2 O7 80.32(10) . . ?
O9 Pr2 O7 80.05(10) 2_655 . ?
O9 Pr2 O7 123.86(9) . . ?
O11 Pr2 O7 80.32(10) 2_655 2_655 ?
O11 Pr2 O7 85.99(10) . 2_655 ?
O9 Pr2 O7 123.86(9) 2_655 2_655 ?
O9 Pr2 O7 80.05(10) . 2_655 ?
O7 Pr2 O7 150.14(14) . 2_655 ?
O11 Pr2 N4 62.49(7) 2_655 . ?
O11 Pr2 N4 62.49(7) . . ?
O9 Pr2 N4 138.23(7) 2_655 . ?
O9 Pr2 N4 138.23(7) . . ?
O7 Pr2 N4 75.07(7) . . ?
O7 Pr2 N4 75.07(7) 2_655 . ?
O11 Pr2 N3 139.35(10) 2_655 2_655 ?
O11 Pr2 N3 70.19(10) . 2_655 ?
O9 Pr2 N3 61.99(9) 2_655 2_655 ?
O9 Pr2 N3 77.99(9) . 2_655 ?
O7 Pr2 N3 134.51(10) . 2_655 ?
O7 Pr2 N3 62.17(9) 2_655 2_655 ?
N4 Pr2 N3 117.02(7) . 2_655 ?
O11 Pr2 N3 70.19(10) 2_655 . ?
O11 Pr2 N3 139.35(10) . . ?
O9 Pr2 N3 77.99(9) 2_655 . ?
O9 Pr2 N3 61.99(9) . . ?
O7 Pr2 N3 62.17(9) . . ?
O7 Pr2 N3 134.51(10) 2_655 . ?
N4 Pr2 N3 117.02(7) . . ?
N3 Pr2 N3 125.96(14) 2_655 . ?
N5 Cu1 N7 160.13(15) . . ?
N5 Cu1 O6 100.02(13) . . ?
N7 Cu1 O6 99.07(12) . . ?
N8 Cu2 N6 159.31(15) 1_554 . ?
N8 Cu2 O8 110.07(13) 1_554 . ?
N6 Cu2 O8 90.38(13) . . ?
N10 Cu3 N9 163.91(14) 4 . ?
N10 Cu3 O10 104.23(12) 4 . ?
N9 Cu3 O10 91.01(12) . . ?
C2 N1 C6 119.5(3) . . ?
C2 N1 Pr1 120.0(2) . . ?
C6 N1 Pr1 120.4(3) . . ?
C9 N2 C9 119.5(5) 2_556 . ?
C9 N2 Pr1 120.2(2) 2_556 . ?
C9 N2 Pr1 120.2(2) . . ?
C17 N3 C13 119.7(3) . . ?
C17 N3 Pr2 119.0(2) . . ?
C13 N3 Pr2 119.0(3) . . ?
C20 N4 C20 119.6(6) 2_655 . ?
C20 N4 Pr2 120.2(3) 2_655 . ?
C20 N4 Pr2 120.2(3) . . ?
C27 N5 C23 117.4(3) . . ?
C27 N5 Cu1 121.9(3) . . ?
C23 N5 Cu1 120.4(3) . . ?
C32 N6 C28 116.8(3) . . ?
C32 N6 Cu2 122.1(3) . . ?
C28 N6 Cu2 120.9(3) . . ?
C33 N7 C37 117.1(3) . . ?
C33 N7 Cu1 123.0(3) . . ?
C37 N7 Cu1 119.5(3) . . ?
C42 N8 C38 116.6(3) . . ?
C42 N8 Cu2 122.2(3) . 1_556 ?
C38 N8 Cu2 121.2(3) . 1_556 ?
C43 N9 C47 116.8(3) . . ?
C43 N9 Cu3 116.9(3) . . ?
C47 N9 Cu3 126.0(3) . . ?
C52 N10 C48 116.6(3) . . ?
C52 N10 Cu3 121.7(3) . 4_556 ?
C48 N10 Cu3 121.6(3) . 4_556 ?
C1 O1 Pr1 126.6(3) . . ?
C7 O3 Pr1 125.5(3) . . ?
C8 O5 Pr1 125.0(2) . . ?
C8 O6 Cu1 100.6(2) . . ?
C12 O7 Pr2 125.4(3) . . ?
C12 O8 Cu2 135.8(3) . . ?
C18 O9 Pr2 125.7(2) . . ?
C18 O10 Cu3 148.2(3) . . ?
C19 O11 Pr2 126.1(3) . . ?
H13C O13 H13D 108.1 . . ?
H14C O14 H14D 108.4 . . ?
H15C O15 H15D 108.4 . . ?
H16C O16 H16D 108.0 . . ?
H17C O17 H17D 108.6 . . ?
H17C O17 H17A 110.3 . . ?
H17D O17 H17A 110.3 . . ?
H18A O18 H18C 108.8 . . ?
O2 C1 O1 125.9(4) . . ?
O2 C1 C2 119.1(4) . . ?
O1 C1 C2 115.0(4) . . ?
N1 C2 C3 122.1(4) . . ?
N1 C2 C1 115.5(3) . . ?
C3 C2 C1 122.4(4) . . ?
C2 C3 C4 118.9(5) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C3 C4 C5 119.4(4) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 118.6(4) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
N1 C6 C5 121.5(4) . . ?
N1 C6 C7 114.6(3) . . ?
C5 C6 C7 123.9(4) . . ?
O4 C7 O3 124.7(4) . . ?
O4 C7 C6 118.6(4) . . ?
O3 C7 C6 116.7(3) . . ?
O6 C8 O5 124.4(4) . . ?
O6 C8 C9 118.6(3) . . ?
O5 C8 C9 117.0(3) . . ?
N2 C9 C10 121.8(4) . . ?
N2 C9 C8 115.1(3) . . ?
C10 C9 C8 123.1(4) . . ?
C9 C10 C11 118.9(4) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C10 C11 C10 119.2(6) 2_556 . ?
C10 C11 H11 120.4 2_556 . ?
C10 C11 H11 120.4 . . ?
O8 C12 O7 126.2(4) . . ?
O8 C12 C13 117.2(4) . . ?
O7 C12 C13 116.6(4) . . ?
N3 C13 C14 121.5(4) . . ?
N3 C13 C12 114.6(3) . . ?
C14 C13 C12 123.9(4) . . ?
C13 C14 C15 119.0(4) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C14 C15 C16 119.6(4) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 117.8(4) . . ?
C17 C16 H16 121.1 . . ?
C15 C16 H16 121.1 . . ?
N3 C17 C16 122.3(4) . . ?
N3 C17 C18 114.9(3) . . ?
C16 C17 C18 122.8(4) . . ?
O10 C18 O9 126.4(4) . . ?
O10 C18 C17 117.3(3) . . ?
O9 C18 C17 116.3(3) . . ?
O12 C19 O11 126.3(4) . . ?
O12 C19 C20 117.7(4) . . ?
O11 C19 C20 116.1(4) . . ?
N4 C20 C21 121.5(5) . . ?
N4 C20 C19 114.5(4) . . ?
C21 C20 C19 124.0(4) . . ?
C20 C21 C22 119.2(6) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C21 C22 C21 119.0(8) . 2_655 ?
C21 C22 H22 120.5 . . ?
C21 C22 H22 120.5 2_655 . ?
N5 C23 C24 123.4(4) . . ?
N5 C23 H23 118.3 . . ?
C24 C23 H23 118.3 . . ?
C23 C24 C25 119.8(4) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 116.7(4) . . ?
C26 C25 C30 121.7(4) . . ?
C24 C25 C30 121.7(4) . . ?
C27 C26 C25 119.9(4) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
N5 C27 C26 122.9(4) . . ?
N5 C27 H27 118.6 . . ?
C26 C27 H27 118.6 . . ?
N6 C28 C29 122.9(4) . . ?
N6 C28 H28 118.5 . . ?
C29 C28 H28 118.5 . . ?
C28 C29 C30 120.4(4) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C31 116.4(3) . . ?
C29 C30 C25 121.8(4) . . ?
C31 C30 C25 121.8(4) . . ?
C32 C31 C30 120.5(4) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
N6 C32 C31 123.0(4) . . ?
N6 C32 H32 118.5 . . ?
C31 C32 H32 118.5 . . ?
N7 C33 C34 123.2(4) . . ?
N7 C33 H33 118.4 . . ?
C34 C33 H33 118.4 . . ?
C33 C34 C35 120.0(4) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 116.9(3) . . ?
C36 C35 C40 120.8(3) . . ?
C34 C35 C40 122.3(3) . . ?
C37 C36 C35 119.8(4) . . ?
C37 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
N7 C37 C36 123.0(4) . . ?
N7 C37 H37 118.5 . . ?
C36 C37 H37 118.5 . . ?
N8 C38 C39 123.3(4) . . ?
N8 C38 H38 118.3 . . ?
C39 C38 H38 118.3 . . ?
C38 C39 C40 120.3(4) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
C39 C40 C41 116.8(3) . . ?
C39 C40 C35 121.6(3) . . ?
C41 C40 C35 121.5(3) . . ?
C42 C41 C40 119.0(4) . . ?
C42 C41 H41 120.5 . . ?
C40 C41 H41 120.5 . . ?
N8 C42 C41 123.9(4) . . ?
N8 C42 H42 118.1 . . ?
C41 C42 H42 118.1 . . ?
N9 C43 C44 123.4(4) . . ?
N9 C43 H43 118.3 . . ?
C44 C43 H43 118.3 . . ?
C43 C44 C45 120.1(4) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C46 C45 C44 116.4(3) . . ?
C46 C45 C50 122.6(4) . . ?
C44 C45 C50 121.1(4) . . ?
C47 C46 C45 119.9(4) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
N9 C47 C46 123.5(4) . . ?
N9 C47 H47 118.3 . . ?
C46 C47 H47 118.3 . . ?
N10 C48 C49 123.1(4) . . ?
N10 C48 H48 118.5 . . ?
C49 C48 H48 118.5 . . ?
C48 C49 C50 120.2(4) . . ?
C48 C49 H49 119.9 . . ?
C50 C49 H49 119.9 . . ?
C51 C50 C49 116.8(3) . . ?
C51 C50 C45 121.6(4) . . ?
C49 C50 C45 121.6(4) . . ?
C52 C51 C50 119.6(4) . . ?
C52 C51 H51 120.2 . . ?
C50 C51 H51 120.2 . . ?
N10 C52 C51 123.7(4) . . ?
N10 C52 H52 118.1 . . ?
C51 C52 H52 118.1 . . ?
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 2.482(3) . ?
Pr1 O1 2.482(3) 2_556 ?
Pr1 O5 2.515(3) 2_556 ?
Pr1 O5 2.515(3) . ?
Pr1 O3 2.517(3) 2_556 ?
Pr1 O3 2.517(3) . ?
Pr1 N2 2.593(4) . ?
Pr1 N1 2.595(3) 2_556 ?
Pr1 N1 2.595(3) . ?
Pr2 O11 2.489(3) 2_655 ?
Pr2 O11 2.489(3) . ?
Pr2 O9 2.507(3) 2_655 ?
Pr2 O9 2.507(3) . ?
Pr2 O7 2.520(3) . ?
Pr2 O7 2.520(3) 2_655 ?
Pr2 N4 2.588(5) . ?
Pr2 N3 2.614(3) 2_655 ?
Pr2 N3 2.614(3) . ?
Cu1 N5 1.922(3) . ?
Cu1 N7 1.926(3) . ?
Cu1 O6 2.260(3) . ?
Cu2 N8 1.916(3) 1_554 ?
Cu2 N6 1.928(3) . ?
Cu2 O8 2.268(3) . ?
Cu3 N10 1.904(3) 4 ?
Cu3 N9 1.913(3) . ?
Cu3 O10 2.295(3) . ?
N1 C2 1.330(5) . ?
N1 C6 1.346(5) . ?
N2 C9 1.341(4) 2_556 ?
N2 C9 1.341(4) . ?
N3 C17 1.329(5) . ?
N3 C13 1.340(5) . ?
N4 C20 1.338(5) 2_655 ?
N4 C20 1.338(5) . ?
N5 C27 1.332(5) . ?
N5 C23 1.343(5) . ?
N6 C32 1.343(5) . ?
N6 C28 1.344(5) . ?
N7 C33 1.331(5) . ?
N7 C37 1.353(5) . ?
N8 C42 1.343(5) . ?
N8 C38 1.344(5) . ?
N8 Cu2 1.916(3) 1_556 ?
N9 C43 1.345(5) . ?
N9 C47 1.346(5) . ?
N10 C52 1.341(5) . ?
N10 C48 1.341(5) . ?
N10 Cu3 1.904(3) 4_556 ?
O1 C1 1.276(5) . ?
O2 C1 1.232(5) . ?
O3 C7 1.254(5) . ?
O4 C7 1.241(5) . ?
O5 C8 1.264(4) . ?
O6 C8 1.247(4) . ?
O7 C12 1.255(5) . ?
O8 C12 1.240(5) . ?
O9 C18 1.257(5) . ?
O10 C18 1.247(5) . ?
O11 C19 1.251(5) . ?
O12 C19 1.242(5) . ?
O13 H13C 0.8500 . ?
O13 H13D 0.8500 . ?
O14 H14C 0.8501 . ?
O14 H14D 0.8500 . ?
O15 H15C 0.8500 . ?
O15 H15D 0.8500 . ?
O16 H16C 0.8502 . ?
O16 H16D 0.8500 . ?
O17 H17C 0.8499 . ?
O17 H17D 0.8500 . ?
O17 H17A 0.8501 . ?
O18 H18A 0.8501 . ?
O18 H18C 0.8500 . ?
C1 C2 1.528(6) . ?
C2 C3 1.375(6) . ?
C3 C4 1.378(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.517(6) . ?
C8 C9 1.502(5) . ?
C9 C10 1.381(6) . ?
C10 C11 1.386(6) . ?
C10 H10 0.9300 . ?
C11 C10 1.386(6) 2_556 ?
C11 H11 0.9300 . ?
C12 C13 1.512(6) . ?
C13 C14 1.379(6) . ?
C14 C15 1.380(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.389(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.388(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.514(5) . ?
C19 C20 1.525(6) . ?
C20 C21 1.370(7) . ?
C21 C22 1.377(7) . ?
C21 H21 0.9300 . ?
C22 C21 1.377(7) 2_655 ?
C22 H22 0.9300 . ?
C23 C24 1.378(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.394(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.394(6) . ?
C25 C30 1.483(5) . ?
C26 C27 1.392(5) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.378(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.382(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.387(5) . ?
C31 C32 1.373(5) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.378(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.391(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.389(5) . ?
C35 C40 1.488(5) . ?
C36 C37 1.377(5) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 C39 1.367(5) . ?
C38 H38 0.9300 . ?
C39 C40 1.394(5) . ?
C39 H39 0.9300 . ?
C40 C41 1.397(5) . ?
C41 C42 1.382(5) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 C44 1.370(5) . ?
C43 H43 0.9300 . ?
C44 C45 1.402(5) . ?
C44 H44 0.9300 . ?
C45 C46 1.398(6) . ?
C45 C50 1.477(5) . ?
C46 C47 1.375(5) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 C49 1.379(5) . ?
C48 H48 0.9300 . ?
C49 C50 1.388(6) . ?
C49 H49 0.9300 . ?
C50 C51 1.387(5) . ?
C51 C52 1.379(5) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
