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#$Date: 2017-03-04 03:43:09 +0200 (Sat, 04 Mar 2017) $
#$Revision: 192917 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/53/4345353.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_4345353
loop_
_publ_author_name
'Marinho, Maria Vanda'
'Reis, Daniella O.'
'Oliveira, Willian X. C.'
'Marques, Lippy F.'
'Stumpf, Humberto O.'
'Déniz, Mariadel'
'Pasán, Jorge'
'Ruiz-Pérez, Catalina'
'Cano, Joan'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 Photoluminescent and Slow Magnetic Relaxation Studies on
 Lanthanide(III)-2,5-pyrazinedicarboxylate Frameworks.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2108
_journal_page_last               2123
_journal_paper_doi               10.1021/acs.inorgchem.6b02774
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C9 H13 N3 O11 Pr'
_chemical_formula_weight         480.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                72.398(7)
_cell_angle_beta                 88.980(6)
_cell_angle_gamma                89.043(6)
_cell_formula_units_Z            2
_cell_length_a                   6.0820(5)
_cell_length_b                   10.5091(8)
_cell_length_c                   13.6280(10)
_cell_measurement_reflns_used    5500
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.46
_cell_measurement_theta_min      3.40
_cell_volume                     830.08(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31f (release 05-03-2014 CrysAlis171 .NET)
(compiled Mar  5 2014,18:34:03)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31f (release 05-03-2014 CrysAlis171 .NET)
(compiled Mar  5 2014,18:34:03)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31f (release 05-03-2014 CrysAlis171 .NET)
(compiled Mar  5 2014,18:34:03)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5500
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         73.464
_diffrn_reflns_theta_min         3.403
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    23.100
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.024
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_description       Needle
_exptl_crystal_F_000             450
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.419
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0727P)²+0.7415P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3124
_reflns_number_total             3227
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02774_si_001.cif
_cod_data_source_block           compound2
_cod_database_code               4345353
_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.
;
_shelx_estimated_absorpt_t_min   0.028
_shelx_estimated_absorpt_t_max   0.458
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pr1 Pr 0.25128(3) 0.66056(2) 0.70878(2) 0.02001(12) Uani 1 1 d . . .
N1 N 0.0782(7) 0.8870(4) 0.5755(3) 0.0270(8) Uani 1 1 d . . .
N2 N 0.4340(7) 0.5569(4) 0.8984(3) 0.0275(8) Uani 1 1 d . . .
N3 N 0.0896(7) 0.5722(4) 0.5582(3) 0.0253(8) Uani 1 1 d . . .
O1 O 0.4534(6) 0.7712(4) 0.5472(3) 0.0333(8) Uani 1 1 d . . .
O3 O 0.0633(7) 0.6982(4) 0.8568(3) 0.0373(9) Uani 1 1 d . . .
O5 O -0.1542(6) 0.6414(4) 0.6992(3) 0.0291(7) Uani 1 1 d . . .
O2 O 0.5028(7) 0.9113(4) 0.3898(3) 0.0425(10) Uani 1 1 d . . .
O4 O -0.0019(8) 0.6792(5) 1.0208(3) 0.0493(12) Uani 1 1 d . . .
O6 O -0.4399(5) 0.5239(4) 0.6754(3) 0.0268(7) Uani 1 1 d . . .
O1W O 0.1538(7) 0.4181(4) 0.7818(3) 0.0353(8) Uani 1 1 d . . .
O2W O 0.4379(8) 0.8465(4) 0.7471(3) 0.0417(9) Uani 1 1 d . . .
C1 C 0.4000(8) 0.8682(5) 0.4730(4) 0.0268(10) Uani 1 1 d . . .
C2 C 0.1867(8) 0.9400(5) 0.4861(4) 0.0260(9) Uani 1 1 d . . .
C3 C -0.1090(9) 0.9474(5) 0.5890(4) 0.0306(10) Uani 1 1 d . . .
H3 H -0.1895 0.9137 0.6497 0.037 Uiso 1 1 calc R U .
C4 C 0.1096(9) 0.6578(5) 0.9506(4) 0.0297(10) Uani 1 1 d . . .
C5 C 0.3183(8) 0.5732(5) 0.9773(4) 0.0264(10) Uani 1 1 d . . .
C6 C 0.6176(9) 0.4827(5) 0.9213(4) 0.0305(11) Uani 1 1 d . . .
H6 H 0.7037 0.4684 0.8685 0.037 Uiso 1 1 calc R U .
C7 C -0.2469(8) 0.5677(5) 0.6562(3) 0.0220(9) Uani 1 1 d . . .
C8 C -0.1172(7) 0.5289(5) 0.5746(3) 0.0230(9) Uani 1 1 d . . .
C9 C -0.2049(8) 0.4565(5) 0.5148(4) 0.0263(10) Uani 1 1 d . . .
H9 H -0.3494 0.4277 0.5268 0.032 Uiso 1 1 calc R U .
O6W O 0.6250(15) 0.8401(8) 0.9285(7) 0.101(3) Uani 1 1 d . . .
O5W O 0.009(5) 1.019(3) 0.836(2) 0.183(13) Uani 0.5 1 d . . P
O3W O 0.173(3) 0.2282(11) 0.6839(12) 0.201(8) Uani 1 1 d . . .
O4W O -0.380(6) 1.171(4) 0.868(4) 0.28(3) Uani 0.5 1 d . . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -2.4164 10.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O3 Pr1 O6 137.90(12) . 1_655
O3 Pr1 O2W 72.72(15) . .
O6 Pr1 O2W 102.97(14) 1_655 .
O3 Pr1 O1 144.01(14) . .
O6 Pr1 O1 67.19(12) 1_655 .
O2W Pr1 O1 76.49(14) . .
O3 Pr1 O5 68.27(13) . .
O6 Pr1 O5 132.37(12) 1_655 .
O2W Pr1 O5 124.55(14) . .
O1 Pr1 O5 117.58(12) . .
O3 Pr1 O1W 87.70(14) . .
O6 Pr1 O1W 71.34(13) 1_655 .
O2W Pr1 O1W 143.61(14) . .
O1 Pr1 O1W 128.27(13) . .
O5 Pr1 O1W 71.83(13) . .
O3 Pr1 N3 129.47(13) . .
O6 Pr1 N3 78.09(12) 1_655 .
O2W Pr1 N3 145.03(14) . .
O1 Pr1 N3 71.81(13) . .
O5 Pr1 N3 61.78(12) . .
O1W Pr1 N3 70.54(13) . .
O3 Pr1 N1 92.91(13) . .
O6 Pr1 N1 127.15(12) 1_655 .
O2W Pr1 N1 74.74(14) . .
O1 Pr1 N1 60.92(12) . .
O5 Pr1 N1 69.66(13) . .
O1W Pr1 N1 138.12(14) . .
N3 Pr1 N1 77.20(13) . .
O3 Pr1 N2 61.49(13) . .
O6 Pr1 N2 76.95(12) 1_655 .
O2W Pr1 N2 73.48(14) . .
O1 Pr1 N2 125.75(13) . .
O5 Pr1 N2 116.66(12) . .
O1W Pr1 N2 70.21(13) . .
N3 Pr1 N2 138.43(13) . .
N1 Pr1 N2 143.90(13) . .
C3 N1 C2 116.6(4) . .
C3 N1 Pr1 126.0(3) . .
C2 N1 Pr1 117.3(3) . .
C5 N2 C6 116.5(4) . .
C5 N2 Pr1 116.1(3) . .
C6 N2 Pr1 127.2(3) . .
C9 N3 C8 118.1(4) 2_566 .
C9 N3 Pr1 126.0(3) 2_566 .
C8 N3 Pr1 114.4(3) . .
C1 O1 Pr1 130.2(3) . .
C4 O3 Pr1 130.4(3) . .
C7 O5 Pr1 124.3(3) . .
C7 O6 Pr1 122.7(3) . 1_455
O1 C1 O2 126.4(5) . .
O1 C1 C2 116.0(4) . .
O2 C1 C2 117.6(4) . .
N1 C2 C3 122.1(5) . 2_576
N1 C2 C1 115.3(4) . .
C3 C2 C1 122.6(4) 2_576 .
N1 C3 C2 121.3(5) . 2_576
O4 C4 O3 125.3(5) . .
O4 C4 C5 119.0(5) . .
O3 C4 C5 115.7(4) . .
N2 C5 C6 122.5(5) . 2_667
N2 C5 C4 116.1(4) . .
C6 C5 C4 121.4(5) 2_667 .
N2 C6 C5 121.1(5) . 2_667
O5 C7 O6 125.5(4) . .
O5 C7 C8 117.0(4) . .
O6 C7 C8 117.5(4) . .
N3 C8 C9 120.1(4) . .
N3 C8 C7 116.6(4) . .
C9 C8 C7 123.2(4) . .
N3 C9 C8 121.8(5) 2_566 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr1 O3 2.432(4) .
Pr1 O6 2.464(3) 1_655
Pr1 O2W 2.468(4) .
Pr1 O1 2.473(4) .
Pr1 O5 2.486(3) .
Pr1 O1W 2.516(4) .
Pr1 N3 2.702(4) .
Pr1 N1 2.728(4) .
Pr1 N2 2.731(4) .
N1 C3 1.331(7) .
N1 C2 1.343(6) .
N2 C5 1.327(7) .
N2 C6 1.337(7) .
N3 C9 1.312(7) 2_566
N3 C8 1.336(6) .
O1 C1 1.243(6) .
O3 C4 1.255(7) .
O5 C7 1.249(6) .
O2 C1 1.247(6) .
O4 C4 1.237(7) .
O6 C7 1.262(6) .
O6 Pr1 2.464(3) 1_455
C1 C2 1.525(7) .
C2 C3 1.392(7) 2_576
C3 C2 1.392(7) 2_576
C4 C5 1.522(7) .
C5 C6 1.388(7) 2_667
C6 C5 1.388(7) 2_667
C7 C8 1.503(6) .
C8 C9 1.389(7) .
C9 N3 1.312(7) 2_566
