#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/52/4325280.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_4325280
loop_
_publ_author_name
'Tereza Peristeraki'
'Marianna Samios'
'Milosz Siczek'
'Tadeusz Lis'
'Constantinos J. Milios'
_publ_contact_author_email       komil@chemistry.uoc.gr
_publ_contact_author_name        'Constantinos Milios'
_publ_section_title
;
 Artificial Amino Acids in Nickel(II) and Nickel(II)/Lanthanide(III)
 Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5175
_journal_page_last               5185
_journal_paper_doi               10.1021/ic2004744
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C48 H96 N12 Ni6 O24 Pr, 3(N O3), 5.5(H2 O )'
_chemical_formula_sum            'C48 H107 N15 Ni6 O38.5 Pr'
_chemical_formula_weight         2003.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.373(7)
_cell_length_b                   17.206(8)
_cell_length_c                   13.912(4)
_cell_measurement_reflns_used    15539
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.49
_cell_volume                     3919(3)
_computing_cell_refinement       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Xcalibur PX KM4CCD'
_diffrn_measurement_method       φ
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18237
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    2.117
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5
Analytical numeric absorption correction using a 
multifaceted crystal model based on expressions
 derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             2070
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.34
_refine_diff_density_min         -1.51
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4641
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0388
_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)+(0.0285P)²+22.8690P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                3786
_reflns_number_total             4641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2004744_si_001_4.cif
_cod_data_source_block           complex_3
_cod_original_formula_sum        'C48 H107 N15 Ni6 O38.50 Pr'
_cod_database_code               4325280
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, 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
Pr Pr 0.5000 0.5000 0.5000 0.0106(4) Uani 0.972(8) 4 d SP . .
Pr1 Pr 0.4991(16) 0.536(4) 0.5000 0.0106(4) Uani 0.014(4) 2 d SP . .
Ni1 Ni 0.5000 0.5000 0.23600(5) 0.01501(16) Uani 1 2 d S . .
Ni2 Ni 0.28346(4) 0.55724(4) 0.5000 0.01356(19) Uani 0.9749(18) 2 d SP . .
Ni21 Ni 0.2776(15) 0.5018(19) 0.5000 0.01356(19) Uani 0.0251(18) 2 d SP . .
Ni3 Ni 0.56003(5) 0.70746(4) 0.5000 0.01592(19) Uani 0.9776(18) 2 d SP . .
Ni31 Ni 0.489(2) 0.7033(18) 0.5000 0.01592(19) Uani 0.0224(18) 2 d SP . .
O11 O 0.36597(16) 0.53559(16) 0.3950(2) 0.0153(6) Uani 1 1 d . . .
O21 O 0.37888(16) 0.53021(17) 0.2350(2) 0.0196(6) Uani 1 1 d . . .
N11 N 0.2066(2) 0.5784(2) 0.3868(3) 0.0274(9) Uani 1 1 d . . .
H11A H 0.1606 0.5480 0.3928 0.033 Uiso 1 1 calc R . .
H11B H 0.1905 0.6297 0.3881 0.033 Uiso 1 1 calc R . .
C11 C 0.3385(2) 0.5409(2) 0.3098(3) 0.0169(8) Uani 1 1 d . . .
C21 C 0.2470(2) 0.5615(3) 0.2933(3) 0.0204(9) Uani 1 1 d . . .
C31 C 0.2418(3) 0.6322(3) 0.2296(4) 0.0339(11) Uani 1 1 d . . .
H31A H 0.1844 0.6452 0.2181 0.051 Uiso 1 1 calc R . .
H31B H 0.2688 0.6213 0.1681 0.051 Uiso 1 1 calc R . .
H31C H 0.2690 0.6760 0.2611 0.051 Uiso 1 1 calc R . .
C41 C 0.2067(3) 0.4915(3) 0.2453(4) 0.0321(11) Uani 1 1 d . . .
H41A H 0.1491 0.5032 0.2325 0.048 Uiso 1 1 calc R . .
H41B H 0.2105 0.4463 0.2879 0.048 Uiso 1 1 calc R . .
H41C H 0.2346 0.4801 0.1846 0.048 Uiso 1 1 calc R . .
O12 O 0.52330(16) 0.58263(16) 0.3365(2) 0.0161(6) Uani 1 1 d . . .
O22 O 0.56110(19) 0.70726(16) 0.3516(2) 0.0234(7) Uani 1 1 d . . .
N12 N 0.5240(2) 0.5881(2) 0.1419(3) 0.0241(8) Uani 1 1 d . . .
H12A H 0.5658 0.5733 0.1015 0.029 Uiso 1 1 calc R . .
H12B H 0.4785 0.5972 0.1048 0.029 Uiso 1 1 calc R . .
C12 C 0.5437(2) 0.6487(2) 0.3027(3) 0.0177(8) Uani 1 1 d . . .
C22 C 0.5472(3) 0.6601(3) 0.1922(3) 0.0234(9) Uani 1 1 d . . .
C32 C 0.6338(4) 0.6821(4) 0.1649(4) 0.0525(18) Uani 1 1 d . . .
H32A H 0.6706 0.6388 0.1800 0.079 Uiso 1 1 calc R . .
H32B H 0.6504 0.7282 0.2013 0.079 Uiso 1 1 calc R . .
H32C H 0.6363 0.6933 0.0960 0.079 Uiso 1 1 calc R . .
C42 C 0.4859(5) 0.7241(4) 0.1673(5) 0.075(3) Uani 1 1 d . . .
H42A H 0.4978 0.7705 0.2055 0.112 Uiso 1 1 calc R . .
H42B H 0.4305 0.7060 0.1816 0.112 Uiso 1 1 calc R . .
H42C H 0.4901 0.7367 0.0988 0.112 Uiso 1 1 calc R . .
O13 O 0.6226(2) 0.6052(2) 0.5000 0.0174(8) Uani 1 2 d S . .
O23 O 0.7495(3) 0.5565(2) 0.5000 0.0225(9) Uani 1 2 d S . .
N13 N 0.6760(4) 0.7536(3) 0.5000 0.0407(16) Uani 1 2 d S . .
H13A H 0.6833 0.7831 0.4474 0.049 Uiso 1 1 d R . .
C13 C 0.7000(3) 0.6122(3) 0.5000 0.0183(12) Uani 1 2 d S . .
C23 C 0.7385(3) 0.6936(3) 0.5000 0.0199(12) Uani 1 2 d S . .
C33 C 0.7906(5) 0.7021(3) 0.4109(5) 0.073(3) Uani 1 1 d . . .
H33A H 0.7568 0.6939 0.3537 0.109 Uiso 1 1 calc R . .
H33B H 0.8346 0.6634 0.4123 0.109 Uiso 1 1 calc R . .
H33C H 0.8142 0.7544 0.4090 0.109 Uiso 1 1 calc R . .
O14 O 0.4509(2) 0.6519(2) 0.5000 0.0161(8) Uani 1 2 d S . .
O24 O 0.3146(2) 0.6732(2) 0.5000 0.0219(9) Uani 1 2 d S . .
N14 N 0.4860(3) 0.8041(3) 0.5000 0.0370(15) Uani 1 2 d S . .
H14A H 0.4919 0.8339 0.5526 0.044 Uiso 1 1 d R . .
C14 C 0.3883(3) 0.6958(3) 0.5000 0.0184(12) Uani 1 2 d S . .
C24 C 0.4003(4) 0.7857(4) 0.5000 0.0259(14) Uani 1 2 d S . .
C34 C 0.3449(13) 0.8256(10) 0.433(2) 0.027(5) Uani 0.38(5) 1 d P . 1
H34A H 0.3531 0.8051 0.3680 0.041 Uiso 0.38(5) 1 calc PR . 1
H34B H 0.3565 0.8814 0.4335 0.041 Uiso 0.38(5) 1 calc PR . 1
H34C H 0.2882 0.8168 0.4528 0.041 Uiso 0.38(5) 1 calc PR . 1
C341 C 0.3726(17) 0.8123(10) 0.3950(18) 0.060(5) Uani 0.62(5) 1 d P . 2
H34D H 0.3747 0.8691 0.3906 0.089 Uiso 0.62(5) 1 calc PR . 2
H34E H 0.3166 0.7945 0.3829 0.089 Uiso 0.62(5) 1 calc PR . 2
H34F H 0.4094 0.7896 0.3470 0.089 Uiso 0.62(5) 1 calc PR . 2
N15 N 0.6704(4) 0.4559(4) 0.0000 0.0358(15) Uani 1 2 d S . .
O15 O 0.6662(7) 0.5211(5) 0.0000 0.026(2) Uani 0.50 2 d SP . .
O25 O 0.7513(5) 0.4246(5) 0.0000 0.026(2) Uani 0.50 2 d SP . .
O35 O 0.6198(6) 0.4026(7) 0.0000 0.033(3) Uani 0.50 2 d SP . .
O16 O 0.5909(5) 0.4910(6) 0.0000 0.029(2) Uani 0.50 2 d SP . .
O26 O 0.7220(6) 0.5071(6) 0.0000 0.033(2) Uani 0.50 2 d SP . .
O36 O 0.6674(9) 0.3916(6) 0.0000 0.039(3) Uani 0.50 2 d SP . .
O1W O 0.6263(10) 0.9346(9) 0.5000 0.043(5) Uani 0.46(3) 2 d SP . .
O2W O 0.5841(11) 0.9635(8) 0.5000 0.060(5) Uani 0.54(3) 2 d SP . .
O3W O 0.5051(5) 0.9515(6) 0.6395(7) 0.058(2) Uani 0.50 1 d P . .
O17 O 0.0461(9) 0.5452(8) 0.5000 0.160(5) Uiso 1 2 d SD . 1
O27 O 0.0000 0.5000 0.3270(10) 0.058(4) Uiso 0.50 2 d SPD A 1
N17 N 0.0000 0.5000 0.4263(14) 0.138(11) Uiso 0.50 2 d SPD . 1
O4W O 0.4952(15) 0.9226(15) 0.8347(18) 0.087(7) Uiso 0.25 1 d P . 2
O5W O 0.0254(19) 0.5279(19) 0.345(2) 0.040(7) Uiso 0.125 1 d P . 2
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'
Ni Ni 0.3393 1.1124 '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
O13 Pr O13 180.0 . 5_666
O13 Pr O11 63.22(9) . 5_666
O13 Pr O11 116.78(9) 5_666 5_666
O13 Pr O11 63.22(9) . 2_665
O13 Pr O11 116.78(9) 5_666 2_665
O11 Pr O11 65.33(12) 5_666 2_665
O13 Pr O11 116.78(9) . .
O13 Pr O11 63.22(9) 5_666 .
O11 Pr O11 180.0 5_666 .
O11 Pr O11 114.67(12) 2_665 .
O13 Pr O11 116.78(9) . 6_556
O13 Pr O11 63.22(9) 5_666 6_556
O11 Pr O11 114.67(12) 5_666 6_556
O11 Pr O11 180.0 2_665 6_556
O11 Pr O11 65.33(12) . 6_556
O13 Pr O12 62.87(6) . 6_556
O13 Pr O12 117.13(6) 5_666 6_556
O11 Pr O12 63.35(8) 5_666 6_556
O11 Pr O12 117.24(8) 2_665 6_556
O11 Pr O12 116.65(8) . 6_556
O11 Pr O12 62.76(8) 6_556 6_556
O13 Pr O12 62.87(6) . .
O13 Pr O12 117.13(6) 5_666 .
O11 Pr O12 117.24(8) 5_666 .
O11 Pr O12 63.35(8) 2_665 .
O11 Pr O12 62.76(8) . .
O11 Pr O12 116.65(8) 6_556 .
O12 Pr O12 114.19(12) 6_556 .
O13 Pr O12 117.13(6) . 2_665
O13 Pr O12 62.87(6) 5_666 2_665
O11 Pr O12 116.65(8) 5_666 2_665
O11 Pr O12 62.76(8) 2_665 2_665
O11 Pr O12 63.35(8) . 2_665
O11 Pr O12 117.24(8) 6_556 2_665
O12 Pr O12 180.0 6_556 2_665
O12 Pr O12 65.81(12) . 2_665
O13 Pr O12 117.13(6) . 5_666
O13 Pr O12 62.87(6) 5_666 5_666
O11 Pr O12 62.76(8) 5_666 5_666
O11 Pr O12 116.65(8) 2_665 5_666
O11 Pr O12 117.24(8) . 5_666
O11 Pr O12 63.35(8) 6_556 5_666
O12 Pr O12 65.81(12) 6_556 5_666
O12 Pr O12 180.00(10) . 5_666
O12 Pr O12 114.19(12) 2_665 5_666
O12 Ni1 O12 92.97(16) . 2_665
O12 Ni1 N12 83.43(13) . .
O12 Ni1 N12 176.38(14) 2_665 .
O12 Ni1 N12 176.38(14) . 2_665
O12 Ni1 N12 83.43(13) 2_665 2_665
N12 Ni1 N12 100.2(2) . 2_665
O12 Ni1 O21 90.51(11) . .
O12 Ni1 O21 90.02(11) 2_665 .
N12 Ni1 O21 89.66(14) . .
N12 Ni1 O21 89.85(14) 2_665 .
O12 Ni1 O21 90.02(11) . 2_665
O12 Ni1 O21 90.50(11) 2_665 2_665
N12 Ni1 O21 89.85(14) . 2_665
N12 Ni1 O21 89.66(14) 2_665 2_665
O21 Ni1 O21 179.24(17) . 2_665
O11 Ni2 O11 92.38(15) . 6_556
O11 Ni2 O23 89.99(11) . 5_666
O11 Ni2 O23 89.99(11) 6_556 5_666
O11 Ni2 N11 83.59(13) . .
O11 Ni2 N11 175.94(13) 6_556 .
O23 Ni2 N11 90.48(14) 5_666 .
O11 Ni2 N11 175.94(13) . 6_556
O11 Ni2 N11 83.59(13) 6_556 6_556
O23 Ni2 N11 90.48(14) 5_666 6_556
N11 Ni2 N11 100.4(2) . 6_556
O11 Ni2 O24 90.74(11) . .
O11 Ni2 O24 90.74(11) 6_556 .
O23 Ni2 O24 178.95(16) 5_666 .
N11 Ni2 O24 88.85(14) . .
N11 Ni2 O24 88.85(14) 6_556 .
O14 Ni3 O13 92.04(15) . .
O14 Ni3 N14 82.09(19) . .
O13 Ni3 N14 174.13(19) . .
O14 Ni3 N13 174.5(2) . .
O13 Ni3 N13 82.5(2) . .
N14 Ni3 N13 103.4(2) . .
O14 Ni3 O22 90.39(9) . .
O13 Ni3 O22 89.67(9) . .
N14 Ni3 O22 90.37(9) . .
N13 Ni3 O22 89.59(9) . .
O14 Ni3 O22 90.39(9) . 6_556
O13 Ni3 O22 89.67(9) . 6_556
N14 Ni3 O22 90.37(9) . 6_556
N13 Ni3 O22 89.58(9) . 6_556
O22 Ni3 O22 179.00(18) . 6_556
C11 O11 Ni2 115.1(2) . .
C11 O11 Pr 143.8(2) . .
Ni2 O11 Pr 101.15(11) . .
Ni21 O11 Pr 96.8(5) . .
C11 O21 Ni1 123.0(3) . .
C21 N11 Ni2 111.3(2) . .
C21 N11 H11A 109.4 . .
Ni2 N11 H11A 109.4 . .
Ni21 N11 H11A 91.4 . .
C21 N11 H11B 109.4 . .
Ni2 N11 H11B 109.4 . .
Ni21 N11 H11B 131.6 . .
H11A N11 H11B 108.0 . .
O21 C11 O11 125.5(3) . .
O21 C11 C21 114.8(3) . .
O11 C11 C21 119.7(4) . .
N11 C21 C31 109.3(4) . .
N11 C21 C41 110.2(4) . .
C31 C21 C41 110.8(4) . .
N11 C21 C11 110.0(3) . .
C31 C21 C11 108.9(3) . .
C41 C21 C11 107.5(3) . .
C21 C31 H31A 109.5 . .
C21 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C21 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C21 C41 H41A 109.5 . .
C21 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
C21 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C12 O12 Ni1 114.8(3) . .
C12 O12 Pr 144.5(3) . .
Ni1 O12 Pr 100.61(11) . .
C12 O22 Ni3 122.9(3) . .
C22 N12 Ni1 111.7(3) . .
C22 N12 H12A 109.3 . .
Ni1 N12 H12A 109.3 . .
C22 N12 H12B 109.3 . .
Ni1 N12 H12B 109.3 . .
H12A N12 H12B 107.9 . .
O22 C12 O12 125.4(4) . .
O22 C12 C22 115.4(4) . .
O12 C12 C22 119.2(4) . .
N12 C22 C32 109.4(4) . .
N12 C22 C42 109.2(4) . .
C32 C22 C42 112.2(5) . .
N12 C22 C12 110.8(3) . .
C32 C22 C12 108.3(4) . .
C42 C22 C12 107.0(4) . .
C22 C32 H32A 109.5 . .
C22 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C22 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C22 C42 H42A 109.5 . .
C22 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C22 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C13 O13 Ni3 114.7(4) . .
C13 O13 Pr 143.4(4) . .
Ni3 O13 Pr 101.85(15) . .
C13 O23 Ni2 124.4(4) . 5_666
C23 N13 Ni3 112.1(4) . .
C23 N13 H13A 107.9 . .
Ni3 N13 H13A 109.9 . .
O23 C13 O13 124.7(5) . .
O23 C13 C23 115.6(5) . .
O13 C13 C23 119.7(5) . .
N13 C23 C33 109.2(4) . 6_556
N13 C23 C33 109.2(4) . .
C33 C23 C33 110.1(8) 6_556 .
N13 C23 C13 111.0(5) . .
C33 C23 C13 108.7(4) 6_556 .
C33 C23 C13 108.7(4) . .
C23 C33 H33A 109.5 . .
C23 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C23 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C14 O14 Ni3 115.4(4) . .
C14 O14 Pr1 148.1(11) . .
Ni3 O14 Pr1 96.5(10) . .
C14 O14 Pr 143.6(4) . .
Ni3 O14 Pr 101.05(15) . .
C14 O24 Ni2 122.2(4) . .
C24 N14 Ni3 113.3(4) . .
C24 N14 H14A 103.2 . .
Ni3 N14 H14A 113.5 . .
O24 C14 O14 125.7(5) . .
O24 C14 C24 115.1(5) . .
O14 C14 C24 119.2(5) . .
N14 C24 C34 119.9(10) . 6_556
N14 C24 C34 119.9(10) . .
C34 C24 C34 79(2) 6_556 .
N14 C24 C14 110.0(5) . .
C34 C24 C14 112.7(8) 6_556 .
C34 C24 C14 112.7(8) . .
N14 C24 C341 102.4(10) . 6_556
C14 C24 C341 104.4(7) . 6_556
N14 C24 C341 102.4(10) . .
C14 C24 C341 104.4(7) . .
C341 C24 C341 132(2) 6_556 .
C24 C34 C34 50.7(12) . 6_556
C24 C34 H34A 109.5 . .
C34 C34 H34A 157.4 6_556 .
C24 C34 H34B 109.5 . .
C34 C34 H34B 89.6 6_556 .
H34A C34 H34B 109.5 . .
C24 C34 H34C 109.5 . .
C34 C34 H34C 73.7 6_556 .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C24 C341 H34D 109.5 . .
C24 C341 H34E 109.5 . .
H34D C341 H34E 109.5 . .
C24 C341 H34F 109.5 . .
H34D C341 H34F 109.5 . .
H34E C341 H34F 109.5 . .
O36 N15 O15 174.0(12) . .
O36 N15 O26 138.7(12) . .
O15 N15 O26 47.2(7) . .
O15 N15 O35 134.4(11) . .
O26 N15 O35 178.3(11) . .
O36 N15 O25 70.4(10) . .
O15 N15 O25 115.6(8) . .
O26 N15 O25 68.3(7) . .
O35 N15 O25 110.0(9) . .
O36 N15 O16 112.4(10) . .
O15 N15 O16 61.7(8) . .
O26 N15 O16 108.9(9) . .
O35 N15 O16 72.8(8) . .
O25 N15 O16 177.2(7) . .
O26 O15 N15 71.7(9) . .
O26 O15 O16 142.4(12) . .
N15 O15 O16 70.7(8) . .
O36 O25 O26 93.8(7) . .
O36 O35 N15 61.6(11) . .
O36 O35 O16 121.0(15) . .
N15 O35 O16 59.4(7) . .
O15 O16 N15 47.7(5) . .
O15 O16 O35 95.5(7) . .
N15 O16 O35 47.8(5) . .
O15 O26 N15 61.0(8) . .
O15 O26 O25 123.5(11) . .
N15 O26 O25 62.5(7) . .
O35 O36 N15 78.8(14) . .
O35 O36 O25 143.9(16) . .
N15 O36 O25 65.1(8) . .
N17 O17 N17 86.8(15) . 5_566
O27 N17 O17 133.4(8) . 5_566
O27 N17 O17 133.4(8) . .
O17 N17 O17 93.2(15) 5_566 .
O4W O5W O5W 109(4) 7_575 2_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr Pr1 0.62(8) .
Pr Pr1 0.62(8) 5_666
Pr O13 2.703(4) .
Pr O13 2.703(4) 5_666
Pr O11 2.706(3) 5_666
Pr O11 2.706(3) 2_665
Pr O11 2.706(3) .
Pr O11 2.706(3) 6_556
Pr O12 2.710(3) 6_556
Pr O12 2.710(3) .
Pr O12 2.710(3) 2_665
Pr O12 2.710(3) 5_666
Pr1 Pr1 1.24(15) 5_666
Pr1 O14 2.14(7) .
Pr1 O13 2.35(4) .
Pr1 O12 2.44(3) .
Pr1 O12 2.44(3) 6_556
Pr1 O11 2.62(2) 6_556
Pr1 O11 2.62(2) .
Pr1 Ni31 2.88(8) .
Pr1 O11 2.92(4) 5_666
Pr1 O11 2.92(4) 2_665
Pr1 Ni3 3.11(7) .
Ni1 O12 2.030(3) .
Ni1 O12 2.030(3) 2_665
Ni1 N12 2.041(4) .
Ni1 N12 2.041(4) 2_665
Ni1 O21 2.050(3) .
Ni1 O21 2.050(3) 2_665
Ni2 Ni21 0.96(3) .
Ni2 O11 2.024(3) .
Ni2 O11 2.024(3) 6_556
Ni2 O23 2.030(4) 5_666
Ni2 N11 2.049(4) .
Ni2 N11 2.049(4) 6_556
Ni2 O24 2.060(4) .
Ni21 O23 1.10(3) 5_666
Ni21 C13 2.00(3) 5_666
Ni21 O11 2.14(2) .
Ni21 O11 2.14(2) 6_556
Ni21 N11 2.36(2) 6_556
Ni21 N11 2.36(2) .
Ni3 Ni31 1.16(3) .
Ni3 O14 2.027(4) .
Ni3 O13 2.036(4) .
Ni3 N14 2.057(6) .
Ni3 N13 2.058(6) .
Ni3 O22 2.065(3) .
Ni3 O22 2.065(3) 6_556
Ni31 O14 1.09(3) .
Ni31 C14 1.66(3) .
Ni31 N14 1.73(3) .
Ni31 C24 2.03(3) .
Ni31 O22 2.376(16) .
Ni31 O22 2.376(16) 6_556
O11 C11 1.271(5) .
O11 Pr1 2.92(4) 5_666
O21 C11 1.247(5) .
N11 C21 1.489(6) .
N11 H11A 0.9200 .
N11 H11B 0.9200 .
C11 C21 1.557(5) .
C21 C31 1.507(6) .
C21 C41 1.526(6) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
O12 C12 1.274(5) .
O22 C12 1.249(5) .
N12 C22 1.473(6) .
N12 H12A 0.9200 .
N12 H12B 0.9200 .
C12 C22 1.552(6) .
C22 C32 1.516(7) .
C22 C42 1.529(7) .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
O13 C13 1.274(7) .
O23 Ni21 1.10(3) 5_666
O23 C13 1.255(7) .
O23 Ni2 2.030(4) 5_666
N13 C23 1.453(8) .
N13 H13A 0.8988 .
C13 C23 1.535(8) .
C13 Ni21 2.00(3) 5_666
C23 C33 1.512(7) 6_556
C23 C33 1.512(7) .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
O14 C14 1.273(7) .
O24 C14 1.267(7) .
N14 C24 1.439(8) .
N14 H14A 0.8986 .
C14 C24 1.558(8) .
C24 C34 1.471(17) 6_556
C24 C34 1.471(17) .
C24 C341 1.597(16) 6_556
C24 C341 1.597(16) .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
C341 H34D 0.9800 .
C341 H34E 0.9800 .
C341 H34F 0.9800 .
N15 O36 1.107(12) .
N15 O15 1.125(11) .
N15 O26 1.221(11) .
N15 O35 1.236(12) .
N15 O25 1.431(11) .
N15 O16 1.435(11) .
O15 O26 0.944(12) .
O15 O16 1.339(14) .
O25 O36 1.487(17) .
O25 O26 1.500(14) .
O35 O36 0.803(13) .
O35 O16 1.593(16) .
O1W O2W 0.851(13) .
O3W O3W 1.677(19) 2_675
O17 N17 1.492(13) .
O17 N17 1.492(13) 5_566
O27 N17 1.381(17) .
N17 O17 1.492(13) 5_566
O4W O5W 0.99(3) 7_676
O5W O4W 0.99(3) 7_575
O5W O5W 1.27(7) 2_565
