#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/11/2211128.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_2211128
loop_
_publ_author_name
'Rohde, Alexander'
'Urland, Werner'
_publ_section_title
;
 Bis(guanidinium)
 diaquapentanitrato-κ¹⁰O,O'-praseodymate(III)
;
_journal_coeditor_code           NG2104
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3026
_journal_page_last               m3028
_journal_paper_doi               10.1107/S1600536806038980
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C H6 N3)2 [Pr (N O3)5 (H2 O)2]'
_chemical_formula_moiety         '2C H6 N3 +, H4 N5 O17 Pr 2-'
_chemical_formula_sum            'C2 H16 N11 O17 Pr'
_chemical_formula_weight         607.17
_chemical_name_systematic
;
Bis(guanidinium) diaquapentanitrato-κ¹⁰O,O'-praseodymium
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.78(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.931(3)
_cell_length_b                   9.071(3)
_cell_length_c                   20.571(5)
_cell_measurement_reflns_used    8002
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      3
_cell_volume                     2032.6(10)
_computing_cell_refinement       'IPDS Software'
_computing_data_collection       'IPDS Software (Stoe & Cie, 1998)'
_computing_data_reduction        'IPDS Software'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Stoe IPDS area-detector'
_diffrn_measurement_method       φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14022
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         2.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.499
_exptl_absorpt_correction_T_max  0.2530
_exptl_absorpt_correction_T_min  0.2104
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Stoe & Cie, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.791
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.037P)²+0.3651P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0523
_reflns_number_gt                1822
_reflns_number_total             1956
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2104.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2211128
_cod_database_fobs_code          2211128
loop_
_symmetry_equiv_pos_as_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_refinement_flags
_atom_site_occupancy
Pr Pr 0.5000 0.861324(18) 0.7500 0.02072(8) Uani d S 1
O O11 0.59530(16) 0.5976(2) 0.73946(11) 0.0364(4) Uani d . 1
O O12 0.5000 0.3910(3) 0.7500 0.0838(17) Uani d S 1
N N11 0.5000 0.5229(3) 0.7500 0.0362(8) Uani d S 1
O O21 0.6132(2) 0.8233(2) 0.63757(11) 0.0430(5) Uani d . 1
O O22 0.43183(19) 0.7291(2) 0.63608(10) 0.0404(5) Uani d . 1
O O23 0.5299(3) 0.7213(3) 0.54893(11) 0.0648(8) Uani d . 1
N N21 0.5256(2) 0.7578(3) 0.60669(12) 0.0375(6) Uani d . 1
O O31 0.43540(18) 1.0491(2) 0.65959(10) 0.0390(5) Uani d . 1
O O32 0.61354(18) 1.1021(2) 0.70610(10) 0.0363(4) Uani d . 1
O O33 0.5420(3) 1.2247(3) 0.62082(13) 0.0657(8) Uani d . 1
N N31 0.5318(2) 1.1291(2) 0.66136(13) 0.0353(6) Uani d . 1
C C1 0.2403(3) 0.9993(4) 0.50270(16) 0.0457(7) Uani d . 1
N N1A 0.2079(3) 1.0080(3) 0.43994(14) 0.0602(8) Uani d . 1
H H1A1 0.2421 1.0718 0.4164 0.072 Uiso calc R 1
H H1A2 0.1524 0.9498 0.4224 0.072 Uiso calc R 1
N N1B 0.3246(3) 1.0880(4) 0.52926(15) 0.0633(9) Uani d . 1
H H1B1 0.3587 1.1517 0.5056 0.076 Uiso calc R 1
H H1B2 0.3460 1.0826 0.5704 0.076 Uiso calc R 1
N N1C 0.1876(3) 0.9011(4) 0.53889(19) 0.0674(9) Uani d . 1
H H1C1 0.2087 0.8955 0.5800 0.081 Uiso calc R 1
H H1C2 0.1322 0.8430 0.5213 0.081 Uiso calc R 1
O O1W 0.27266(18) 0.86096(18) 0.72199(12) 0.0380(5) Uani d . 1
H H1W 0.2160 0.7830 0.7186 0.046 Uiso d R 1
H H2W 0.2190 0.9323 0.7284 0.046 Uiso d R 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pr Pr -0.2180 2.8214 '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'
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'
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
_geom_angle_publ_flag
O1W Pr O1W 2_656 . 179.85(8) no
O1W Pr O31 2_656 2_656 68.14(7) no
O1W Pr O31 . 2_656 111.96(7) no
O1W Pr O31 2_656 . 111.96(7) no
O1W Pr O31 . . 68.14(7) no
O31 Pr O31 2_656 . 97.24(10) no
O1W Pr O11 2_656 2_656 111.90(6) no
O1W Pr O11 . 2_656 67.96(6) no
O31 Pr O11 2_656 2_656 129.01(7) no
O31 Pr O11 . 2_656 125.11(7) no
O1W Pr O11 2_656 . 67.96(6) no
O1W Pr O11 . . 111.90(6) no
O31 Pr O11 2_656 . 125.11(7) no
O31 Pr O11 . . 129.01(7) no
O11 Pr O11 2_656 . 48.67(8) no
O1W Pr O22 2_656 . 113.49(7) no
O1W Pr O22 . . 66.43(7) no
O31 Pr O22 2_656 . 164.93(7) no
O31 Pr O22 . . 68.00(7) no
O11 Pr O22 2_656 . 65.26(7) no
O11 Pr O22 . . 66.66(7) no
O1W Pr O22 2_656 2_656 66.43(7) no
O1W Pr O22 . 2_656 113.49(7) no
O31 Pr O22 2_656 2_656 68.00(7) no
O31 Pr O22 . 2_656 164.93(7) no
O11 Pr O22 2_656 2_656 66.66(7) no
O11 Pr O22 . 2_656 65.26(7) no
O22 Pr O22 . 2_656 126.89(10) no
O1W Pr O32 2_656 . 66.64(6) no
O1W Pr O32 . . 113.49(6) no
O31 Pr O32 2_656 . 66.51(7) no
O31 Pr O32 . . 48.00(6) no
O11 Pr O32 2_656 . 163.70(7) no
O11 Pr O32 . . 120.79(6) no
O22 Pr O32 . . 99.85(6) no
O22 Pr O32 2_656 . 123.44(7) no
O1W Pr O32 2_656 2_656 113.49(6) no
O1W Pr O32 . 2_656 66.64(6) no
O31 Pr O32 2_656 2_656 48.00(6) no
O31 Pr O32 . 2_656 66.51(7) no
O11 Pr O32 2_656 2_656 120.79(6) no
O11 Pr O32 . 2_656 163.70(7) no
O22 Pr O32 . 2_656 123.44(7) no
O22 Pr O32 2_656 2_656 99.85(6) no
O32 Pr O32 . 2_656 72.27(9) no
O1W Pr O21 2_656 . 71.58(8) no
O1W Pr O21 . . 108.40(8) no
O31 Pr O21 2_656 . 125.29(7) no
O31 Pr O21 . . 65.73(7) no
O11 Pr O21 2_656 . 99.54(6) no
O11 Pr O21 . . 66.71(7) no
O22 Pr O21 . . 46.92(6) no
O22 Pr O21 2_656 . 124.77(7) no
O32 Pr O21 . . 64.32(6) no
O32 Pr O21 2_656 . 129.57(7) no
O1W Pr O21 2_656 2_656 108.40(8) no
O1W Pr O21 . 2_656 71.58(8) no
O31 Pr O21 2_656 2_656 65.73(7) no
O31 Pr O21 . 2_656 125.29(6) no
O11 Pr O21 2_656 2_656 66.71(7) no
O11 Pr O21 . 2_656 99.54(6) no
O22 Pr O21 . 2_656 124.77(7) no
O22 Pr O21 2_656 2_656 46.92(6) no
O32 Pr O21 . 2_656 129.57(7) no
O32 Pr O21 2_656 2_656 64.32(6) no
O21 Pr O21 . 2_656 165.51(9) no
N11 O11 Pr . . 97.75(15) no
O12 N11 O11 . . 122.09(15) no
O12 N11 O11 . 2_656 122.09(15) no
O11 N11 O11 . 2_656 115.8(3) no
N21 O21 Pr . . 96.21(15) no
N21 O22 Pr . . 98.57(15) no
O23 N21 O21 . . 121.7(3) no
O23 N21 O22 . . 120.2(3) no
O21 N21 O22 . . 118.2(2) no
N31 O31 Pr . . 100.33(16) no
N31 O32 Pr . . 94.84(14) no
O33 N31 O32 . . 122.9(3) no
O33 N31 O31 . . 120.6(3) no
O32 N31 O31 . . 116.5(2) no
N1B C1 N1A . . 119.8(3) no
N1B C1 N1C . . 120.2(3) no
N1A C1 N1C . . 119.9(3) no
C1 N1A H1A1 . . 120.0 no
C1 N1A H1A2 . . 120.0 no
H1A1 N1A H1A2 . . 120.0 no
C1 N1B H1B1 . . 120.0 no
C1 N1B H1B2 . . 120.0 no
H1B1 N1B H1B2 . . 120.0 no
C1 N1C H1C1 . . 120.0 no
C1 N1C H1C2 . . 120.0 no
H1C1 N1C H1C2 . . 120.0 no
Pr O1W H1W . . 130.8 no
Pr O1W H2W . . 128.2 no
H1W O1W H2W . . 96.9 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pr O1W 2_656 2.504(2) yes
Pr O1W . 2.504(2) yes
Pr O31 2_656 2.577(2) yes
Pr O31 . 2.577(2) yes
Pr O11 2_656 2.625(2) yes
Pr O11 . 2.625(2) yes
Pr O22 . 2.682(2) yes
Pr O22 2_656 2.682(2) yes
Pr O32 . 2.704(2) yes
Pr O32 2_656 2.704(2) yes
Pr O21 . 2.734(2) yes
Pr O21 2_656 2.734(2) yes
O11 N11 . 1.277(2) no
O12 N11 . 1.196(5) no
N11 O11 2_656 1.277(2) no
O21 N21 . 1.254(3) no
O22 N21 . 1.260(3) no
O23 N21 . 1.238(3) no
O31 N31 . 1.277(3) no
O32 N31 . 1.253(3) no
O33 N31 . 1.214(3) no
C1 N1B . 1.309(4) no
C1 N1A . 1.312(4) no
C1 N1C . 1.323(4) no
N1A H1A1 . 0.8600 no
N1A H1A2 . 0.8600 no
N1B H1B1 . 0.8600 no
N1B H1B2 . 0.8600 no
N1C H1C1 . 0.8600 no
N1C H1C2 . 0.8600 no
O1W H1W . 0.9390 no
O1W H2W . 0.8899 no
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
N1A H1A1 O21 5_676 0.86 2.22 3.038(4) 158.6
N1A H1A2 O22 7_566 0.86 2.18 3.001(4) 160.0
N1A H1A2 O23 7_566 0.86 2.63 3.351(4) 142.0
N1B H1B1 O23 5_676 0.86 2.07 2.921(4) 168.9
N1B H1B2 O31 . 0.86 2.03 2.870(4) 165.8
N1C H1C2 O23 7_566 0.86 2.27 3.071(5) 155.8
O1W H1W O32 3_445 0.94 1.99 2.925(3) 172.3
O1W H2W O11 3_455 0.89 2.05 2.935(3) 177.9
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1W Pr O11 N11 2_656 . 153.12(14) no
O1W Pr O11 N11 . . -26.85(14) no
O31 Pr O11 N11 2_656 . 113.98(12) no
O31 Pr O11 N11 . . -105.86(12) no
O11 Pr O11 N11 2_656 . 0.0 no
O22 Pr O11 N11 . . -76.86(12) no
O22 Pr O11 N11 2_656 . 79.88(12) no
O32 Pr O11 N11 . . -164.55(10) no
O32 Pr O11 N11 2_656 . 54.6(3) no
O21 Pr O11 N11 . . -128.24(14) no
O21 Pr O11 N11 2_656 . 47.02(13) no
Pr O11 N11 O12 . . 180.0 no
Pr O11 N11 O11 . 2_656 0.0 no
O1W Pr O21 N21 2_656 . 154.52(18) no
O1W Pr O21 N21 . . -25.33(18) no
O31 Pr O21 N21 2_656 . -161.25(15) no
O31 Pr O21 N21 . . -79.85(18) no
O11 Pr O21 N21 2_656 . 44.48(18) no
O11 Pr O21 N21 . . 81.21(17) no
O22 Pr O21 N21 . . 2.05(15) no
O22 Pr O21 N21 2_656 . 112.61(18) no
O32 Pr O21 N21 . . -133.16(19) no
O32 Pr O21 N21 2_656 . -99.83(17) no
O21 Pr O21 N21 2_656 . 62.17(17) no
O1W Pr O22 N21 2_656 . -30.62(18) no
O1W Pr O22 N21 . . 149.53(18) no
O31 Pr O22 N21 2_656 . 62.4(3) no
O31 Pr O22 N21 . . 74.71(17) no
O11 Pr O22 N21 2_656 . -134.94(18) no
O11 Pr O22 N21 . . -81.32(16) no
O22 Pr O22 N21 2_656 . -107.98(17) no
O32 Pr O22 N21 . . 38.08(17) no
O32 Pr O22 N21 2_656 . 113.27(16) no
O21 Pr O22 N21 . . -2.05(15) no
O21 Pr O22 N21 2_656 . -166.74(15) no
Pr O21 N21 O23 . . 176.5(3) no
Pr O21 N21 O22 . . -3.6(3) no
Pr O22 N21 O23 . . -176.4(3) no
Pr O22 N21 O21 . . 3.7(3) no
O1W Pr O31 N31 2_656 . -16.84(18) no
O1W Pr O31 N31 . . 163.27(18) no
O31 Pr O31 N31 2_656 . 52.46(15) no
O11 Pr O31 N31 2_656 . -157.65(15) no
O11 Pr O31 N31 . . -95.65(17) no
O22 Pr O31 N31 . . -124.34(17) no
O22 Pr O31 N31 2_656 . 63.9(3) no
O32 Pr O31 N31 . . 3.39(15) no
O32 Pr O31 N31 2_656 . 90.22(17) no
O21 Pr O31 N31 . . -73.09(16) no
O21 Pr O31 N31 2_656 . 117.78(17) no
O1W Pr O32 N31 2_656 . 156.13(18) no
O1W Pr O32 N31 . . -23.79(18) no
O31 Pr O32 N31 2_656 . -128.61(17) no
O31 Pr O32 N31 . . -3.42(15) no
O11 Pr O32 N31 2_656 . 67.8(3) no
O11 Pr O32 N31 . . 113.29(16) no
O22 Pr O32 N31 . . 44.68(16) no
O22 Pr O32 N31 2_656 . -167.67(15) no
O32 Pr O32 N31 2_656 . -77.44(16) no
O21 Pr O32 N31 . . 76.17(16) no
O21 Pr O32 N31 2_656 . -108.75(16) no
Pr O32 N31 O33 . . -173.5(3) no
Pr O32 N31 O31 . . 5.7(2) no
Pr O31 N31 O33 . . 173.1(3) no
Pr O31 N31 O32 . . -6.1(3) no
