#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:44:30 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180353 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/22/7202219.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_7202219
loop_
_publ_author_name
'Kostakis, George E.'
'Abbas, Ghulam'
'Anson, Christopher E.'
'Powell, Annie K.'
_publ_section_title
;
 A new class of 3-D porous framework: [Ln(H2O)n]3+ ions act as pillars
 between π-stacked and H-bonded sheets of (m-BDTH)− organic
 anions in [Ln(H2O)n](m-BDTH)3·9(H2O) (Ln = Pr, n = 9; Ln = Gd,
 n = 8)
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1117
_journal_paper_doi               10.1039/b807028h
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'H18 O9 Pr, 3(C8 H5 N8), 9(H2 O)'
_chemical_formula_sum            'C24 H51 N24 O18 Pr'
_chemical_formula_weight         1104.80
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.545(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8788(6)
_cell_length_b                   19.6459(12)
_cell_length_c                   22.7918(14)
_cell_measurement_reflns_used    2463
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.40
_cell_measurement_theta_min      2.26
_cell_volume                     4333.9(5)
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'SAINT+ 6.45 (Bruker AXS Inc., 2003)'
_computing_molecular_graphics    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20763
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc., 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         9675
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0416P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                7241
_reflns_number_total             9675
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807028h.txt
_cod_data_source_block           26025
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7202219
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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
Pr1 Pr 0.07301(2) 0.186701(13) 0.244519(11) 0.01395(8) Uani 1 1 d . . .
O1 O 0.2848(4) 0.2373(2) 0.30807(15) 0.0252(9) Uani 1 1 d D . .
H11 H 0.291(6) 0.234(3) 0.342(2) 0.038 Uiso 1 1 d . . .
H12 H 0.312(6) 0.270(2) 0.291(2) 0.038 Uiso 1 1 d D . .
O2 O -0.0334(4) 0.17628(17) 0.13656(14) 0.0192(8) Uani 1 1 d D . .
H21 H -0.006(5) 0.145(2) 0.119(2) 0.029 Uiso 1 1 d D . .
H22 H -0.055(6) 0.202(3) 0.115(2) 0.029 Uiso 1 1 d . . .
O3 O -0.1082(3) 0.27941(19) 0.21931(15) 0.0209(8) Uani 1 1 d . . .
H31 H -0.122(5) 0.313(3) 0.243(2) 0.031 Uiso 1 1 d . . .
H32 H -0.161(6) 0.274(3) 0.192(2) 0.031 Uiso 1 1 d . . .
O4 O 0.2804(4) 0.15039(19) 0.20653(16) 0.0244(8) Uani 1 1 d . . .
H41 H 0.324(6) 0.125(3) 0.233(2) 0.037 Uiso 1 1 d . . .
H42 H 0.273(6) 0.128(3) 0.176(2) 0.037 Uiso 1 1 d . . .
O5 O 0.0513(4) 0.0580(2) 0.20611(17) 0.0299(9) Uani 1 1 d . . .
H51 H 0.062(6) 0.046(3) 0.176(3) 0.045 Uiso 1 1 d . . .
H52 H 0.084(6) 0.028(3) 0.227(3) 0.045 Uiso 1 1 d . . .
O6 O -0.1459(4) 0.13259(19) 0.25310(16) 0.0238(8) Uani 1 1 d . . .
H61 H -0.203(6) 0.154(3) 0.259(3) 0.036 Uiso 1 1 d . . .
H62 H -0.173(5) 0.091(3) 0.241(2) 0.036 Uiso 1 1 d . . .
O7 O 0.1636(4) 0.28335(18) 0.19352(16) 0.0213(8) Uani 1 1 d . . .
H71 H 0.227(6) 0.278(3) 0.177(2) 0.032 Uiso 1 1 d . . .
H72 H 0.124(6) 0.314(3) 0.177(2) 0.032 Uiso 1 1 d . . .
O8 O 0.1578(4) 0.10316(19) 0.32718(16) 0.0228(8) Uani 1 1 d . . .
H81 H 0.156(6) 0.064(3) 0.321(2) 0.034 Uiso 1 1 d . . .
H82 H 0.206(6) 0.105(3) 0.357(2) 0.034 Uiso 1 1 d . . .
O9 O 0.0098(4) 0.23359(18) 0.33797(15) 0.0208(8) Uani 1 1 d D . .
H91 H -0.032(6) 0.267(3) 0.335(2) 0.031 Uiso 1 1 d . . .
H92 H 0.054(5) 0.231(3) 0.3725(16) 0.031 Uiso 1 1 d D . .
C1 C 1.1323(5) 0.4160(2) 0.4905(2) 0.0165(10) Uani 1 1 d . . .
C2 C 0.9895(5) 0.4157(2) 0.4882(2) 0.0165(10) Uani 1 1 d . . .
H2A H 0.9271 0.4167 0.4506 0.020 Uiso 1 1 calc R . .
C3 C 0.9389(5) 0.4138(2) 0.5412(2) 0.0162(10) Uani 1 1 d . . .
C4 C 1.0332(5) 0.4117(2) 0.5959(2) 0.0198(10) Uani 1 1 d . . .
H4A H 0.9999 0.4109 0.6322 0.024 Uiso 1 1 calc R . .
C5 C 1.1735(5) 0.4109(2) 0.5979(2) 0.0233(11) Uani 1 1 d . . .
H5A H 1.2363 0.4079 0.6353 0.028 Uiso 1 1 calc R . .
C6 C 1.2221(5) 0.4143(2) 0.5455(2) 0.0192(10) Uani 1 1 d . . .
H6A H 1.3189 0.4155 0.5470 0.023 Uiso 1 1 calc R . .
C7 C 1.1857(5) 0.4205(2) 0.4348(2) 0.0184(10) Uani 1 1 d . . .
N1 N 1.3197(4) 0.4267(2) 0.43174(18) 0.0218(9) Uani 1 1 d . . .
H1 H 1.408(5) 0.424(2) 0.458(2) 0.026 Uiso 1 1 d . . .
N2 N 1.3286(4) 0.4316(2) 0.37412(19) 0.0285(10) Uani 1 1 d . . .
N3 N 1.2030(5) 0.4288(2) 0.34357(19) 0.0343(12) Uani 1 1 d . . .
N4 N 1.1116(4) 0.4214(2) 0.38027(18) 0.0267(10) Uani 1 1 d . . .
C8 C 0.7900(5) 0.4151(2) 0.5403(2) 0.0152(10) Uani 1 1 d . . .
N5 N 0.7361(4) 0.40765(19) 0.58911(17) 0.0186(9) Uani 1 1 d . . .
N6 N 0.5992(4) 0.41160(19) 0.56938(17) 0.0189(9) Uani 1 1 d . . .
N7 N 0.5720(4) 0.42147(19) 0.51098(17) 0.0184(9) Uani 1 1 d . . .
N8 N 0.6909(4) 0.42323(18) 0.49074(17) 0.0162(8) Uani 1 1 d . . .
C9 C 0.7142(5) 0.0819(2) 0.46615(19) 0.0131(9) Uani 1 1 d . . .
C10 C 0.8136(5) 0.0773(2) 0.5187(2) 0.0165(10) Uani 1 1 d . . .
H10A H 0.7864 0.0717 0.5561 0.020 Uiso 1 1 calc R . .
C11 C 0.9545(5) 0.0808(2) 0.5162(2) 0.0147(9) Uani 1 1 d . . .
C12 C 0.9924(5) 0.0891(2) 0.4613(2) 0.0167(10) Uani 1 1 d . . .
H12A H 1.0875 0.0923 0.4597 0.020 Uiso 1 1 calc R . .
C13 C 0.8944(5) 0.0930(2) 0.4089(2) 0.0174(10) Uani 1 1 d . . .
H13A H 0.9219 0.0982 0.3715 0.021 Uiso 1 1 calc R . .
C14 C 0.7559(5) 0.0892(2) 0.4114(2) 0.0182(10) Uani 1 1 d . . .
H14A H 0.6881 0.0916 0.3754 0.022 Uiso 1 1 calc R . .
C15 C 0.5655(5) 0.0814(2) 0.4675(2) 0.0160(10) Uani 1 1 d . . .
N9 N 0.4661(4) 0.0825(2) 0.41792(17) 0.0193(9) Uani 1 1 d . . .
N10 N 0.3467(4) 0.08345(19) 0.43738(18) 0.0199(9) Uani 1 1 d . . .
N11 N 0.3742(4) 0.08343(18) 0.49628(17) 0.0166(8) Uani 1 1 d . . .
N12 N 0.5121(4) 0.08208(18) 0.51656(16) 0.0158(8) Uani 1 1 d . . .
C16 C 1.0581(5) 0.0762(2) 0.5714(2) 0.0153(10) Uani 1 1 d . . .
N13 N 1.1951(4) 0.0795(2) 0.57475(17) 0.0169(9) Uani 1 1 d . . .
H13 H 1.243(5) 0.084(2) 0.551(2) 0.020 Uiso 1 1 d . . .
N14 N 1.2588(4) 0.0724(2) 0.63221(17) 0.0212(9) Uani 1 1 d . . .
N15 N 1.1620(4) 0.0660(2) 0.66275(17) 0.0221(9) Uani 1 1 d . . .
N16 N 1.0363(4) 0.06894(19) 0.62647(17) 0.0184(9) Uani 1 1 d . . .
C17 C 0.8086(4) 0.2467(2) 0.52742(19) 0.0125(9) Uani 1 1 d . . .
C18 C 0.6690(4) 0.2463(2) 0.53127(19) 0.0140(9) Uani 1 1 d . . .
H18A H 0.6431 0.2421 0.5691 0.017 Uiso 1 1 calc R . .
C19 C 0.5685(4) 0.2521(2) 0.47925(19) 0.0115(9) Uani 1 1 d . . .
C20 C 0.6077(5) 0.2569(2) 0.4242(2) 0.0168(10) Uani 1 1 d . . .
H20A H 0.5389 0.2604 0.3886 0.020 Uiso 1 1 calc R . .
C21 C 0.7459(5) 0.2568(2) 0.4205(2) 0.0174(10) Uani 1 1 d . . .
H21A H 0.7717 0.2595 0.3826 0.021 Uiso 1 1 calc R . .
C22 C 0.8459(5) 0.2526(2) 0.4720(2) 0.0156(10) Uani 1 1 d . . .
H22A H 0.9408 0.2537 0.4697 0.019 Uiso 1 1 calc R . .
C23 C 0.9143(4) 0.2389(2) 0.58214(19) 0.0121(9) Uani 1 1 d . . .
N17 N 1.0523(4) 0.23930(19) 0.58497(16) 0.0135(8) Uani 1 1 d . . .
H17 H 1.100(5) 0.242(2) 0.561(2) 0.016 Uiso 1 1 d . . .
N18 N 1.1166(4) 0.23136(18) 0.64247(16) 0.0156(8) Uani 1 1 d . . .
N19 N 1.0188(4) 0.22528(19) 0.67307(17) 0.0177(8) Uani 1 1 d . . .
N20 N 0.8931(4) 0.22982(19) 0.63722(17) 0.0187(9) Uani 1 1 d . . .
C24 C 0.4195(4) 0.2497(2) 0.48086(19) 0.0125(9) Uani 1 1 d . . .
N21 N 0.3209(4) 0.24627(19) 0.43139(16) 0.0149(8) Uani 1 1 d . . .
N22 N 0.2015(4) 0.24259(19) 0.45064(16) 0.0168(8) Uani 1 1 d . . .
N23 N 0.2291(4) 0.24472(18) 0.50980(16) 0.0148(8) Uani 1 1 d . . .
N24 N 0.3660(4) 0.24940(18) 0.53040(16) 0.0136(8) Uani 1 1 d . . .
O11 O -0.1277(4) 0.35443(18) 0.32017(16) 0.0275(8) Uani 1 1 d D . .
H111 H -0.203(5) 0.367(3) 0.328(2) 0.041 Uiso 1 1 d D . .
H112 H -0.061(5) 0.386(2) 0.334(2) 0.041 Uiso 1 1 d D . .
O12 O -0.3618(4) 0.1978(2) 0.28290(16) 0.0331(9) Uani 1 1 d D . .
H121 H -0.411(6) 0.161(2) 0.283(3) 0.050 Uiso 1 1 d D . .
H122 H -0.404(6) 0.222(3) 0.255(2) 0.050 Uiso 1 1 d D . .
O13 O -0.2377(4) 0.00094(19) 0.22666(16) 0.0363(10) Uani 1 1 d D . .
H131 H -0.204(6) -0.018(3) 0.192(2) 0.054 Uiso 1 1 d D . .
H132 H -0.205(6) -0.025(3) 0.260(2) 0.054 Uiso 1 1 d D . .
O14 O 0.1638(4) -0.0376(2) 0.30301(16) 0.0286(9) Uani 1 1 d D . .
H141 H 0.244(4) -0.049(3) 0.311(2) 0.043 Uiso 1 1 d D . .
H142 H 0.105(5) -0.048(3) 0.322(2) 0.043 Uiso 1 1 d D . .
O15 O 0.4487(4) 0.34912(19) 0.27850(16) 0.0274(8) Uani 1 1 d D . .
H151 H 0.507(5) 0.340(3) 0.257(2) 0.041 Uiso 1 1 d D . .
H152 H 0.392(5) 0.376(3) 0.256(2) 0.041 Uiso 1 1 d D . .
O16 O 0.0834(4) 0.40893(19) 0.14306(16) 0.0251(8) Uani 1 1 d D . .
H161 H 0.061(6) 0.409(3) 0.1077(17) 0.038 Uiso 1 1 d D . .
H162 H 0.020(5) 0.426(3) 0.156(2) 0.038 Uiso 1 1 d D . .
O17 O -0.3399(4) 0.4196(2) 0.36161(16) 0.0289(9) Uani 1 1 d D . .
H171 H -0.417(5) 0.400(3) 0.347(2) 0.043 Uiso 1 1 d D . .
H172 H -0.331(6) 0.416(3) 0.4005(17) 0.043 Uiso 1 1 d D . .
O18 O 0.4661(4) 0.0923(2) 0.29516(17) 0.0385(10) Uani 1 1 d D . .
H181 H 0.465(6) 0.049(2) 0.280(3) 0.058 Uiso 1 1 d D . .
H182 H 0.452(6) 0.092(3) 0.331(2) 0.058 Uiso 1 1 d D . .
O19 O -0.0012(4) 0.4682(2) 0.24307(18) 0.0460(11) Uani 1 1 d D . .
H191 H -0.089(5) 0.472(3) 0.263(3) 0.069 Uiso 1 1 d D . .
H192 H 0.091(5) 0.455(3) 0.274(2) 0.069 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
_geom_angle_publ_flag
O6 Pr1 O2 80.69(11) . . ?
O6 Pr1 O4 134.88(12) . . ?
O2 Pr1 O4 81.13(11) . . ?
O6 Pr1 O7 140.75(12) . . ?
O2 Pr1 O7 73.74(12) . . ?
O4 Pr1 O7 69.94(12) . . ?
O6 Pr1 O1 140.82(11) . . ?
O2 Pr1 O1 138.24(11) . . ?
O4 Pr1 O1 70.31(12) . . ?
O7 Pr1 O1 68.24(11) . . ?
O6 Pr1 O9 73.65(12) . . ?
O2 Pr1 O9 137.99(11) . . ?
O4 Pr1 O9 139.78(12) . . ?
O7 Pr1 O9 106.88(12) . . ?
O1 Pr1 O9 71.58(11) . . ?
O6 Pr1 O8 79.87(12) . . ?
O2 Pr1 O8 134.48(12) . . ?
O4 Pr1 O8 84.21(12) . . ?
O7 Pr1 O8 138.82(12) . . ?
O1 Pr1 O8 73.17(12) . . ?
O9 Pr1 O8 72.90(12) . . ?
O6 Pr1 O3 74.68(12) . . ?
O2 Pr1 O3 72.27(11) . . ?
O4 Pr1 O3 136.14(11) . . ?
O7 Pr1 O3 69.47(11) . . ?
O1 Pr1 O3 108.45(12) . . ?
O9 Pr1 O3 69.20(11) . . ?
O8 Pr1 O3 138.84(11) . . ?
O6 Pr1 O5 66.52(12) . . ?
O2 Pr1 O5 66.84(11) . . ?
O4 Pr1 O5 68.36(12) . . ?
O7 Pr1 O5 125.66(11) . . ?
O1 Pr1 O5 124.70(13) . . ?
O9 Pr1 O5 127.46(11) . . ?
O8 Pr1 O5 67.68(12) . . ?
O3 Pr1 O5 126.78(12) . . ?
Pr1 O1 H11 116(4) . . ?
Pr1 O1 H12 111(4) . . ?
H11 O1 H12 125(6) . . ?
Pr1 O2 H21 116(4) . . ?
Pr1 O2 H22 129(5) . . ?
H21 O2 H22 106(6) . . ?
Pr1 O3 H31 126(3) . . ?
Pr1 O3 H32 116(4) . . ?
H31 O3 H32 117(6) . . ?
Pr1 O4 H41 105(4) . . ?
Pr1 O4 H42 121(4) . . ?
H41 O4 H42 105(5) . . ?
Pr1 O5 H51 125(5) . . ?
Pr1 O5 H52 121(5) . . ?
H51 O5 H52 101(6) . . ?
Pr1 O6 H61 119(5) . . ?
Pr1 O6 H62 126(3) . . ?
H61 O6 H62 113(6) . . ?
Pr1 O7 H71 121(4) . . ?
Pr1 O7 H72 128(4) . . ?
H71 O7 H72 105(5) . . ?
Pr1 O8 H81 121(4) . . ?
Pr1 O8 H82 135(4) . . ?
H81 O8 H82 101(6) . . ?
Pr1 O9 H91 117(4) . . ?
Pr1 O9 H92 128(4) . . ?
H91 O9 H92 108(5) . . ?
C6 C1 C2 119.5(4) . . ?
C6 C1 C7 120.5(4) . . ?
C2 C1 C7 120.0(4) . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 118.7(4) . . ?
C2 C3 C8 121.2(4) . . ?
C4 C3 C8 120.0(4) . . ?
C5 C4 C3 121.1(4) . . ?
C5 C4 H4A 119.4 . . ?
C3 C4 H4A 119.4 . . ?
C6 C5 C4 119.5(5) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C1 121.1(4) . . ?
C5 C6 H6A 119.5 . . ?
C1 C6 H6A 119.5 . . ?
N4 C7 N1 108.5(4) . . ?
N4 C7 C1 126.2(4) . . ?
N1 C7 C1 125.2(4) . . ?
N2 N1 C7 108.5(4) . . ?
N2 N1 H1 113(3) . . ?
C7 N1 H1 138(3) . . ?
N3 N2 N1 106.3(4) . . ?
N2 N3 N4 110.9(4) . . ?
C7 N4 N3 105.8(4) . . ?
N5 C8 N8 111.5(4) . . ?
N5 C8 C3 123.5(4) . . ?
N8 C8 C3 124.9(4) . . ?
C8 N5 N6 105.0(4) . . ?
N7 N6 N5 109.6(3) . . ?
N6 N7 N8 109.5(4) . . ?
N7 N8 C8 104.3(4) . . ?
C10 C9 C14 119.5(4) . . ?
C10 C9 C15 121.1(4) . . ?
C14 C9 C15 119.4(4) . . ?
C9 C10 C11 119.7(4) . . ?
C9 C10 H10A 120.2 . . ?
C11 C10 H10A 120.2 . . ?
C12 C11 C10 119.4(4) . . ?
C12 C11 C16 121.1(4) . . ?
C10 C11 C16 119.4(4) . . ?
C13 C12 C11 121.3(4) . . ?
C13 C12 H12A 119.4 . . ?
C11 C12 H12A 119.4 . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 H13A 120.4 . . ?
C14 C13 H13A 120.4 . . ?
C13 C14 C9 120.9(4) . . ?
C13 C14 H14A 119.6 . . ?
C9 C14 H14A 119.6 . . ?
N12 C15 N9 111.2(4) . . ?
N12 C15 C9 125.6(4) . . ?
N9 C15 C9 123.2(4) . . ?
C15 N9 N10 105.4(4) . . ?
N11 N10 N9 108.8(4) . . ?
N10 N11 N12 109.7(3) . . ?
C15 N12 N11 104.8(4) . . ?
N16 C16 N13 107.8(4) . . ?
N16 C16 C11 127.3(4) . . ?
N13 C16 C11 124.9(4) . . ?
C16 N13 N14 108.7(4) . . ?
C16 N13 H13 135(4) . . ?
N14 N13 H13 116(4) . . ?
N15 N14 N13 106.4(4) . . ?
N14 N15 N16 110.7(4) . . ?
C16 N16 N15 106.3(4) . . ?
C22 C17 C18 120.1(4) . . ?
C22 C17 C23 120.6(4) . . ?
C18 C17 C23 119.3(4) . . ?
C19 C18 C17 119.4(4) . . ?
C19 C18 H18A 120.3 . . ?
C17 C18 H18A 120.3 . . ?
C20 C19 C18 119.7(4) . . ?
C20 C19 C24 118.9(4) . . ?
C18 C19 C24 121.4(4) . . ?
C21 C20 C19 120.8(4) . . ?
C21 C20 H20A 119.6 . . ?
C19 C20 H20A 119.6 . . ?
C22 C21 C20 119.7(4) . . ?
C22 C21 H21A 120.2 . . ?
C20 C21 H21A 120.2 . . ?
C21 C22 C17 120.3(4) . . ?
C21 C22 H22A 119.8 . . ?
C17 C22 H22A 119.8 . . ?
N20 C23 N17 107.8(4) . . ?
N20 C23 C17 126.8(4) . . ?
N17 C23 C17 125.5(4) . . ?
N18 N17 C23 108.7(3) . . ?
N18 N17 H17 117(3) . . ?
C23 N17 H17 134(3) . . ?
N19 N18 N17 106.0(3) . . ?
N18 N19 N20 111.2(3) . . ?
C23 N20 N19 106.4(3) . . ?
N21 C24 N24 111.6(4) . . ?
N21 C24 C19 122.8(4) . . ?
N24 C24 C19 125.7(4) . . ?
C24 N21 N22 105.5(3) . . ?
N23 N22 N21 108.5(4) . . ?
N22 N23 N24 110.3(3) . . ?
C24 N24 N23 104.2(3) . . ?
H111 O11 H112 110(5) . . ?
H121 O12 H122 107(6) . . ?
H131 O13 H132 109(5) . . ?
H141 O14 H142 125(6) . . ?
H151 O15 H152 102(5) . . ?
H161 O16 H162 108(6) . . ?
H171 O17 H172 105(5) . . ?
H181 O18 H182 111(6) . . ?
H191 O19 H192 113(5) . . ?
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 O6 2.453(3) . ?
Pr1 O2 2.483(3) . ?
Pr1 O4 2.483(3) . ?
Pr1 O7 2.485(3) . ?
Pr1 O1 2.500(4) . ?
Pr1 O9 2.511(3) . ?
Pr1 O8 2.513(3) . ?
Pr1 O3 2.538(3) . ?
Pr1 O5 2.670(4) . ?
O1 H11 0.77(5) . ?
O1 H12 0.81(3) . ?
O2 H21 0.81(3) . ?
O2 H22 0.72(5) . ?
O3 H31 0.87(5) . ?
O3 H32 0.73(5) . ?
O4 H41 0.83(6) . ?
O4 H42 0.80(5) . ?
O5 H51 0.75(6) . ?
O5 H52 0.79(6) . ?
O6 H61 0.74(6) . ?
O6 H62 0.89(5) . ?
O7 H71 0.80(5) . ?
O7 H72 0.76(5) . ?
O8 H81 0.79(5) . ?
O8 H82 0.75(5) . ?
O9 H91 0.77(5) . ?
O9 H92 0.82(3) . ?
C1 C6 1.382(6) . ?
C1 C2 1.401(6) . ?
C1 C7 1.471(6) . ?
C2 C3 1.397(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.399(6) . ?
C3 C8 1.467(6) . ?
C4 C5 1.378(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.377(6) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 N4 1.311(6) . ?
C7 N1 1.345(6) . ?
N1 N2 1.337(5) . ?
N1 H1 0.96(5) . ?
N2 N3 1.297(5) . ?
N3 N4 1.356(5) . ?
C8 N5 1.334(5) . ?
C8 N8 1.348(6) . ?
N5 N6 1.339(5) . ?
N6 N7 1.318(5) . ?
N7 N8 1.345(5) . ?
C9 C10 1.392(6) . ?
C9 C14 1.398(6) . ?
C9 C15 1.476(6) . ?
C10 C11 1.406(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.386(6) . ?
C11 C16 1.458(6) . ?
C12 C13 1.381(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.383(6) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 N12 1.329(5) . ?
C15 N9 1.340(6) . ?
N9 N10 1.341(5) . ?
N10 N11 1.315(5) . ?
N11 N12 1.349(5) . ?
C16 N16 1.322(5) . ?
C16 N13 1.342(5) . ?
N13 N14 1.342(5) . ?
N13 H13 0.78(5) . ?
N14 N15 1.297(5) . ?
N15 N16 1.348(5) . ?
C17 C22 1.389(6) . ?
C17 C18 1.399(6) . ?
C17 C23 1.466(6) . ?
C18 C19 1.390(6) . ?
C18 H18A 0.9500 . ?
C19 C20 1.390(6) . ?
C19 C24 1.480(6) . ?
C20 C21 1.384(6) . ?
C20 H20A 0.9500 . ?
C21 C22 1.378(6) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 N20 1.326(5) . ?
C23 N17 1.352(5) . ?
N17 N18 1.346(5) . ?
N17 H17 0.80(4) . ?
N18 N19 1.305(5) . ?
N19 N20 1.346(5) . ?
C24 N21 1.336(5) . ?
C24 N24 1.339(5) . ?
N21 N22 1.340(5) . ?
N22 N23 1.322(5) . ?
N23 N24 1.344(5) . ?
O11 H111 0.83(4) . ?
O11 H112 0.91(4) . ?
O12 H121 0.87(4) . ?
O12 H122 0.85(4) . ?
O13 H131 0.99(4) . ?
O13 H132 0.91(4) . ?
O14 H141 0.81(4) . ?
O14 H142 0.81(4) . ?
O15 H151 0.85(4) . ?
O15 H152 0.86(4) . ?
O16 H161 0.79(4) . ?
O16 H162 0.82(4) . ?
O17 H171 0.85(4) . ?
O17 H172 0.88(4) . ?
O18 H181 0.92(4) . ?
O18 H182 0.86(4) . ?
O19 H191 1.05(4) . ?
O19 H192 1.07(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H11 N21 0.77(5) 2.01(5) 2.767(5) 168(6) .
O1 H12 O15 0.81(3) 2.12(4) 2.888(5) 157(5) .
O2 H21 N6 0.81(3) 2.01(3) 2.801(5) 164(5) 4_565
O2 H22 N24 0.72(5) 2.14(5) 2.830(5) 160(6) 4_565
O3 H31 O11 0.87(5) 1.96(5) 2.770(5) 154(5) .
O3 H32 N18 0.73(5) 2.27(5) 2.932(5) 151(6) 4_465
O4 H41 O18 0.83(6) 1.90(6) 2.695(5) 161(5) .
O4 H42 N5 0.80(5) 2.07(5) 2.861(5) 167(5) 4_565
O5 H51 N6 0.75(6) 2.66(6) 3.299(5) 144(6) 4_565
O5 H52 O14 0.79(6) 2.18(6) 2.943(5) 165(6) .
O6 H61 O12 0.74(6) 1.96(6) 2.689(5) 170(6) .
O6 H62 O13 0.89(5) 1.89(6) 2.767(5) 171(5) .
O7 H71 N20 0.80(5) 2.04(5) 2.832(5) 177(5) 4_565
O7 H72 O16 0.76(5) 2.04(5) 2.770(5) 160(6) .
O8 H81 O14 0.79(5) 2.04(5) 2.823(5) 176(6) .
O8 H82 N10 0.75(5) 2.11(5) 2.840(5) 166(6) .
O9 H91 O11 0.77(5) 1.96(5) 2.725(5) 174(6) .
O9 H92 N22 0.82(3) 2.07(4) 2.875(5) 165(5) .
N1 H1 N7 0.96(5) 1.81(5) 2.772(6) 177(4) 1_655
N13 H13 N11 0.78(5) 1.98(5) 2.757(5) 173(5) 1_655
N17 H17 N23 0.80(4) 1.89(4) 2.682(5) 174(5) 1_655
O11 H111 O17 0.83(4) 1.98(4) 2.778(5) 161(6) .
O11 H112 N4 0.91(4) 1.95(4) 2.811(5) 158(5) 1_455
O12 H121 O18 0.87(4) 1.87(4) 2.731(6) 168(6) 1_455
O12 H122 N19 0.85(4) 2.13(4) 2.960(5) 168(6) 4_465
O13 H131 O17 0.99(4) 1.84(4) 2.794(5) 161(5) 2_445
O13 H132 N15 0.91(4) 1.91(4) 2.808(5) 167(5) 3_656
O14 H141 O16 0.81(4) 1.99(4) 2.761(5) 159(6) 2_545
O14 H142 N16 0.81(4) 2.04(4) 2.853(5) 175(6) 3_656
O15 H151 N19 0.85(4) 2.32(5) 3.010(5) 138(5) 4_565
O15 H152 O14 0.86(4) 2.17(4) 2.968(6) 154(5) 2
O16 H161 N12 0.79(4) 2.04(4) 2.833(5) 174(6) 4_565
O16 H162 O19 0.82(4) 2.19(5) 2.831(5) 135(5) .
O17 H171 O15 0.85(4) 2.09(4) 2.878(5) 153(5) 1_455
O17 H172 N8 0.88(4) 2.03(4) 2.898(5) 171(5) 1_455
O18 H181 O19 0.92(4) 1.73(4) 2.634(6) 167(6) 2_545
O18 H182 N9 0.86(4) 1.96(4) 2.804(5) 166(6) .
O19 H191 O13 1.05(4) 1.87(5) 2.873(6) 158(5) 2_455
O19 H192 N3 1.07(4) 1.81(4) 2.840(6) 160(5) 1_455
