#------------------------------------------------------------------------------
#$Date: 2016-02-17 16:02:03 +0200 (Wed, 17 Feb 2016) $
#$Revision: 176634 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/14/2241424.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241424
loop_
_publ_author_name
'Stromyer, Michael L.'
'Lilly, Cassandra P.'
'Dillner, Adam J.'
'Knaust, Jacqueline M.'
_publ_section_title
;
 Crystal structures of [Ln(NO₃)₃(μ₂-bpydo)₂], where
 Ln = Ce, Pr or Nd, and bpydo = 4,4'-bipyridine
 N,N'-dioxide: layered coordination networks containing 4⁴
 grids
;
_journal_coeditor_code           WM5242
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              25
_journal_page_last               30
_journal_paper_doi               10.1107/S205698901502318X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Pr (N O3)3 (C10 H8 N2 O2)2]'
_chemical_formula_moiety         'C20 H16 N7 O13 Pr'
_chemical_formula_sum            'C20 H16 N7 O13 Pr'
_chemical_formula_weight         703.31
_chemical_name_systematic
;Poly[[tris(nitrato-κ²O,O')praeseodymium(III)]-bis(μ-4,4'-bipyridine
N,N'-dioxide-κ²N:N')]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 105.9810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.7416(18)
_cell_length_b                   13.3127(9)
_cell_length_c                   13.7586(9)
_cell_measurement_reflns_used    11450
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.324
_cell_measurement_theta_min      2.452
_cell_volume                     4708.8(5)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
X-SEED (Barbour, 2001)
;
_computing_publication_material
;
X-SEED (Barbour, 2001)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18363
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.583
_diffrn_reflns_theta_min         1.584
_exptl_absorpt_coefficient_mu    2.158
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.891
_refine_diff_density_min         -1.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0248P)²+6.7123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0524
_reflns_number_gt                6782
_reflns_number_total             7241
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5242sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
;Adding full bibliography for 2241423--2241425.cif.

 Adding full bibliography for 2241423--2241425.cif.
;
_cod_database_code               2241424
_cod_database_fobs_code          2241424
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Pr Pr1 0.12674(2) 0.27553(2) 0.66470(2) 0.00790(3) Uani d 1
O O1 0.14910(4) 1.12982(8) 0.78780(9) 0.0121(2) Uani d 1
O O2 0.07540(5) 0.41686(8) 0.70889(10) 0.0138(2) Uani d 1
O O3 0.17985(4) 0.33321(9) 0.83058(9) 0.0115(2) Uani d 1
O O4 0.54388(4) 0.28390(8) 1.18793(9) 0.0111(2) Uani d 1
O O5 0.19376(6) 0.41071(11) 0.65327(11) 0.0253(3) Uani d 1
O O6 0.12068(6) 0.42773(10) 0.53849(11) 0.0236(3) Uani d 1
O O7 0.18928(7) 0.50822(10) 0.52428(13) 0.0324(4) Uani d 1
O O8 0.21197(5) 0.18554(11) 0.66227(10) 0.0196(3) Uani d 1
O O9 0.16890(5) 0.24298(10) 0.51644(10) 0.0144(2) Uani d 1
O O10 0.23564(5) 0.14508(10) 0.52791(10) 0.0181(2) Uani d 1
O O11 0.05832(5) 0.25265(10) 0.49034(9) 0.0144(2) Uani d 1
O O12 0.09581(4) 0.11451(9) 0.55595(9) 0.0135(2) Uani d 1
O O13 0.03605(5) 0.11082(10) 0.41182(10) 0.0198(3) Uani d 1
N N1 0.14024(5) 1.03189(10) 0.77697(10) 0.0100(2) Uani d 1
N N2 0.08667(5) 0.51456(10) 0.71901(11) 0.0117(2) Uani d 1
N N3 0.23089(5) 0.32704(10) 0.87050(10) 0.0096(2) Uani d 1
N N4 0.49530(5) 0.28712(10) 1.12884(11) 0.0097(2) Uani d 1
N N5 0.16820(7) 0.45013(11) 0.57063(13) 0.0219(3) Uani d 1
N N6 0.20645(5) 0.19037(11) 0.56710(11) 0.0129(3) Uani d 1
N N7 0.06291(5) 0.15870(11) 0.48410(10) 0.0124(3) Uani d 1
C C1 0.18032(6) 0.96583(12) 0.79944(13) 0.0127(3) Uani d 1
H H1 0.2151 0.9899 0.8217 0.015 Uiso calc 1
C C2 0.17102(6) 0.86383(12) 0.79021(13) 0.0130(3) Uani d 1
H H2 0.1994 0.8182 0.8072 0.016 Uiso calc 1
C C3 0.12013(6) 0.82702(12) 0.75610(12) 0.0106(3) Uani d 1
C C4 0.07981(6) 0.89758(12) 0.73481(13) 0.0126(3) Uani d 1
H H4 0.0447 0.8756 0.7120 0.015 Uiso calc 1
C C5 0.09060(6) 0.99871(12) 0.74667(12) 0.0120(3) Uani d 1
H H5 0.0628 1.0457 0.7334 0.014 Uiso calc 1
C C6 0.05349(6) 0.58208(12) 0.66223(13) 0.0152(3) Uani d 1
H H6 0.0230 0.5593 0.6138 0.018 Uiso calc 1
C C7 0.06337(6) 0.68346(12) 0.67370(13) 0.0145(3) Uani d 1
H H7 0.0394 0.7301 0.6340 0.017 Uiso calc 1
C C8 0.10860(6) 0.71840(11) 0.74358(13) 0.0109(3) Uani d 1
C C9 0.14177(6) 0.64669(12) 0.80127(13) 0.0149(3) Uani d 1
H H9 0.1727 0.6674 0.8499 0.018 Uiso calc 1
C C10 0.12999(6) 0.54590(12) 0.78830(14) 0.0154(3) Uani d 1
H H10 0.1527 0.4979 0.8288 0.019 Uiso calc 1
C C11 0.25850(6) 0.41103(12) 0.90557(12) 0.0116(3) Uani d 1
H H11 0.2417 0.4746 0.8969 0.014 Uiso calc 1
C C12 0.31102(6) 0.40482(12) 0.95382(13) 0.0120(3) Uani d 1
H H12 0.3300 0.4640 0.9790 0.014 Uiso calc 1
C C13 0.33636(6) 0.31196(12) 0.96590(12) 0.0100(3) Uani d 1
C C14 0.30678(6) 0.22808(11) 0.92570(13) 0.0122(3) Uani d 1
H H14 0.3231 0.1642 0.9302 0.015 Uiso calc 1
C C15 0.25433(6) 0.23623(12) 0.87957(13) 0.0116(3) Uani d 1
H H15 0.2346 0.1780 0.8540 0.014 Uiso calc 1
C C16 0.47654(6) 0.37537(12) 1.08487(12) 0.0117(3) Uani d 1
H H16 0.4990 0.4318 1.0914 0.014 Uiso calc 1
C C17 0.42522(6) 0.38374(12) 1.03083(13) 0.0120(3) Uani d 1
H H17 0.4124 0.4461 1.0005 0.014 Uiso calc 1
C C18 0.39185(6) 0.30165(12) 1.02012(12) 0.0102(3) Uani d 1
C C19 0.41298(6) 0.21084(12) 1.06397(13) 0.0113(3) Uani d 1
H H19 0.3916 0.1528 1.0566 0.014 Uiso calc 1
C C20 0.46461(6) 0.20508(12) 1.11778(13) 0.0116(3) Uani d 1
H H20 0.4787 0.1431 1.1472 0.014 Uiso calc 1
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O4 Pr1 O3 8_455 . 106.95(4)
O4 Pr1 O2 8_455 . 68.60(4)
O3 Pr1 O2 . . 75.79(4)
O4 Pr1 O1 8_455 1_545 73.85(4)
O3 Pr1 O1 . 1_545 69.44(4)
O2 Pr1 O1 . 1_545 117.22(4)
O4 Pr1 O5 8_455 . 154.35(4)
O3 Pr1 O5 . . 66.68(4)
O2 Pr1 O5 . . 85.82(5)
O1 Pr1 O5 1_545 . 122.36(4)
O4 Pr1 O8 8_455 . 133.11(4)
O3 Pr1 O8 . . 82.56(4)
O2 Pr1 O8 . . 153.82(4)
O1 Pr1 O8 1_545 . 66.88(4)
O5 Pr1 O8 . . 72.05(5)
O4 Pr1 O11 8_455 . 69.62(4)
O3 Pr1 O11 . . 166.61(4)
O2 Pr1 O11 . . 91.05(4)
O1 Pr1 O11 1_545 . 120.17(4)
O5 Pr1 O11 . . 110.48(4)
O8 Pr1 O11 . . 109.43(4)
O4 Pr1 O12 8_455 . 69.86(4)
O3 Pr1 O12 . . 143.04(4)
O2 Pr1 O12 . . 130.35(4)
O1 Pr1 O12 1_545 . 74.59(4)
O5 Pr1 O12 . . 130.84(4)
O8 Pr1 O12 . . 75.74(4)
O11 Pr1 O12 . . 49.12(4)
O4 Pr1 O9 8_455 . 130.11(4)
O3 Pr1 O9 . . 120.78(4)
O2 Pr1 O9 . . 134.05(4)
O1 Pr1 O9 1_545 . 108.67(4)
O5 Pr1 O9 . . 67.21(4)
O8 Pr1 O9 . . 49.00(4)
O11 Pr1 O9 . . 66.91(4)
O12 Pr1 O9 . . 63.63(4)
O4 Pr1 O6 8_455 . 115.98(4)
O3 Pr1 O6 . . 106.61(4)
O2 Pr1 O6 . . 69.19(4)
O1 Pr1 O6 1_545 . 170.15(4)
O5 Pr1 O6 . . 48.87(5)
O8 Pr1 O6 . . 103.98(4)
O11 Pr1 O6 . . 65.42(4)
O12 Pr1 O6 . . 107.45(4)
O9 Pr1 O6 . . 65.03(4)
O4 Pr1 N5 8_455 . 139.09(4)
O3 Pr1 N5 . . 88.34(4)
O2 Pr1 N5 . . 79.39(4)
O1 Pr1 N5 1_545 . 146.01(4)
O5 Pr1 N5 . . 24.63(5)
O8 Pr1 N5 . . 85.53(5)
O11 Pr1 N5 . . 86.73(5)
O12 Pr1 N5 . . 118.82(4)
O9 Pr1 N5 . . 60.42(4)
O6 Pr1 N5 . . 24.63(5)
N1 O1 Pr1 . 1_565 132.45(9)
N2 O2 Pr1 . . 129.47(9)
N3 O3 Pr1 . . 129.16(9)
N4 O4 Pr1 . 8_556 134.06(10)
N5 O5 Pr1 . . 97.56(10)
N5 O6 Pr1 . . 94.43(10)
N6 O8 Pr1 . . 97.84(9)
N6 O9 Pr1 . . 96.25(9)
N7 O11 Pr1 . . 97.00(9)
N7 O12 Pr1 . . 96.18(9)
O1 N1 C5 . . 119.07(13)
O1 N1 C1 . . 120.46(13)
C5 N1 C1 . . 120.42(14)
O2 N2 C10 . . 120.08(13)
O2 N2 C6 . . 119.67(13)
C10 N2 C6 . . 120.20(14)
O3 N3 C15 . . 119.46(13)
O3 N3 C11 . . 119.65(13)
C15 N3 C11 . . 120.82(13)
O4 N4 C20 . . 120.28(13)
O4 N4 C16 . . 118.73(13)
C20 N4 C16 . . 120.89(14)
O7 N5 O6 . . 121.81(18)
O7 N5 O5 . . 120.86(18)
O6 N5 O5 . . 117.33(15)
O7 N5 Pr1 . . 168.42(12)
O6 N5 Pr1 . . 60.94(9)
O5 N5 Pr1 . . 57.81(8)
O10 N6 O9 . . 122.44(15)
O10 N6 O8 . . 121.27(14)
O9 N6 O8 . . 116.28(14)
O13 N7 O11 . . 121.44(14)
O13 N7 O12 . . 120.85(14)
O11 N7 O12 . . 117.70(13)
N1 C1 C2 . . 120.45(14)
N1 C1 H1 . . 119.8
C2 C1 H1 . . 119.8
C1 C2 C3 . . 120.60(15)
C1 C2 H2 . . 119.7
C3 C2 H2 . . 119.7
C4 C3 C2 . . 117.20(14)
C4 C3 C8 . . 120.55(14)
C2 C3 C8 . . 122.25(14)
C5 C4 C3 . . 120.50(14)
C5 C4 H4 . . 119.8
C3 C4 H4 . . 119.8
N1 C5 C4 . . 120.79(15)
N1 C5 H5 . . 119.6
C4 C5 H5 . . 119.6
N2 C6 C7 . . 120.78(15)
N2 C6 H6 . . 119.6
C7 C6 H6 . . 119.6
C6 C7 C8 . . 120.43(15)
C6 C7 H7 . . 119.8
C8 C7 H7 . . 119.8
C9 C8 C7 . . 117.22(14)
C9 C8 C3 . . 121.62(14)
C7 C8 C3 . . 121.16(14)
C10 C9 C8 . . 120.43(15)
C10 C9 H9 . . 119.8
C8 C9 H9 . . 119.8
N2 C10 C9 . . 120.93(15)
N2 C10 H10 . . 119.5
C9 C10 H10 . . 119.5
N3 C11 C12 . . 120.32(14)
N3 C11 H11 . . 119.8
C12 C11 H11 . . 119.8
C11 C12 C13 . . 120.37(14)
C11 C12 H12 . . 119.8
C13 C12 H12 . . 119.8
C14 C13 C12 . . 117.30(14)
C14 C13 C18 . . 120.64(14)
C12 C13 C18 . . 122.05(14)
C15 C14 C13 . . 121.05(15)
C15 C14 H14 . . 119.5
C13 C14 H14 . . 119.5
N3 C15 C14 . . 120.09(14)
N3 C15 H15 . . 120.0
C14 C15 H15 . . 120.0
N4 C16 C17 . . 120.31(14)
N4 C16 H16 . . 119.8
C17 C16 H16 . . 119.8
C16 C17 C18 . . 120.61(15)
C16 C17 H17 . . 119.7
C18 C17 H17 . . 119.7
C17 C18 C19 . . 117.47(14)
C17 C18 C13 . . 120.49(14)
C19 C18 C13 . . 122.02(14)
C20 C19 C18 . . 120.40(15)
C20 C19 H19 . . 119.8
C18 C19 H19 . . 119.8
N4 C20 C19 . . 120.27(15)
N4 C20 H20 . . 119.9
C19 C20 H20 . . 119.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pr1 O4 8_455 2.4554(12)
Pr1 O3 . 2.4558(11)
Pr1 O2 . 2.5009(12)
Pr1 O1 1_545 2.5360(12)
Pr1 O5 . 2.5750(13)
Pr1 O8 . 2.5832(13)
Pr1 O11 . 2.6036(12)
Pr1 O12 . 2.6147(12)
Pr1 O9 . 2.6242(13)
Pr1 O6 . 2.6443(14)
O1 N1 . 1.3261(17)
O1 Pr1 1_565 2.5360(12)
O2 N2 . 1.3337(17)
O3 N3 . 1.3261(16)
O4 N4 . 1.3300(17)
O4 Pr1 8_556 2.4554(12)
O5 N5 . 1.268(2)
O6 N5 . 1.261(2)
O7 N5 . 1.233(2)
O8 N6 . 1.2782(19)
O9 N6 . 1.2646(18)
O10 N6 . 1.2229(18)
O11 N7 . 1.2620(18)
O12 N7 . 1.2722(18)
O13 N7 . 1.2319(18)
N1 C5 . 1.352(2)
N1 C1 . 1.355(2)
N2 C10 . 1.348(2)
N2 C6 . 1.351(2)
N3 C15 . 1.352(2)
N3 C11 . 1.353(2)
N4 C20 . 1.349(2)
N4 C16 . 1.353(2)
C1 C2 . 1.380(2)
C1 H1 . 0.9500
C2 C3 . 1.400(2)
C2 H2 . 0.9500
C3 C4 . 1.399(2)
C3 C8 . 1.479(2)
C4 C5 . 1.377(2)
C4 H4 . 0.9500
C5 H5 . 0.9500
C6 C7 . 1.376(2)
C6 H6 . 0.9500
C7 C8 . 1.401(2)
C7 H7 . 0.9500
C8 C9 . 1.393(2)
C9 C10 . 1.379(2)
C9 H9 . 0.9500
C10 H10 . 0.9500
C11 C12 . 1.381(2)
C11 H11 . 0.9500
C12 C13 . 1.397(2)
C12 H12 . 0.9500
C13 C14 . 1.392(2)
C13 C18 . 1.472(2)
C14 C15 . 1.375(2)
C14 H14 . 0.9500
C15 H15 . 0.9500
C16 C17 . 1.373(2)
C16 H16 . 0.9500
C17 C18 . 1.393(2)
C17 H17 . 0.9500
C18 C19 . 1.399(2)
C19 C20 . 1.377(2)
C19 H19 . 0.9500
C20 H20 . 0.9500
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C1 H1 O5 4_556 0.95 2.59 3.331(2) 135.0
C4 H4 O13 5_566 0.95 2.36 3.200(2) 147.0
C5 H5 O4 8_465 0.95 2.37 3.168(2) 141.3
C9 H9 O9 6_566 0.95 2.61 3.204(2) 120.9
C9 H9 O10 4_556 0.95 2.58 3.468(2) 155.8
C10 H10 O3 . 0.95 2.31 3.115(2) 142.6
C10 H10 O7 6_566 0.95 2.60 3.277(3) 128.7
C11 H11 O10 4_556 0.95 2.50 3.239(2) 134.8
C14 H14 O7 4_546 0.95 2.22 3.002(2) 139.0
C15 H15 O1 1_545 0.95 2.31 3.0924(19) 139.8
C16 H16 O13 4_556 0.95 2.56 3.154(2) 121.1
C17 H17 O12 4_556 0.95 2.36 3.288(2) 164.4
C20 H20 O2 8_556 0.95 2.62 3.307(2) 130.0
