#------------------------------------------------------------------------------
#$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $
#$Revision: 301803 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/45/2204540.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_2204540
loop_
_publ_author_name
'Fowkes, Adrian'
'Harrison, William T. A.'
_publ_section_title
;
Bis(guanidinium) diaquapentakis(nitrato-\k^2^O,O')lanthanum
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              m1647
_journal_page_last               m1659
_journal_paper_doi               10.1107/S1600536804025255
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C H6 N3)2 [La (N O3)5 (H2 O)2]'
_chemical_formula_moiety         '2C H6 N3 +, H4 La N5 O17 2-'
_chemical_formula_sum            'C2 H16 La N11 O17'
_chemical_formula_weight         605.16
_chemical_name_systematic
;
Bis(guanidinium) diaquapentakis(nitrato-\k^2^O,O')lanthanum
;
_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   'difmap (O-H) and geom (N-H)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.5000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9918(6)
_cell_length_b                   9.0820(5)
_cell_length_c                   20.5555(11)
_cell_measurement_reflns_used    3673
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.92
_cell_volume                     2045.68(19)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and ATOMS (Shape Software, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  SHELXL97
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       \w
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9927
_diffrn_reflns_theta_full        32.51
_diffrn_reflns_theta_max         32.51
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.552
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0288
_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/[\s^2^(Fo^2^)+(0.0157P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0459
_reflns_number_gt                3094
_reflns_number_total             3682
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6290.cif
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2204540
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_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
_atom_site_type_symbol
La1 0.0000 0.642098(17) 0.2500 0.02453(5) Uani d S 1 La
O1 0.09473(12) 0.90974(15) 0.23924(8) 0.0411(4) Uani d . 1 O
O2 0.0000 1.1137(2) 0.2500 0.0877(12) Uani d S 1 O
N1 0.0000 0.9816(3) 0.2500 0.0422(7) Uani d S 1 N
O3 -0.06367(13) 0.45066(16) 0.15884(8) 0.0439(4) Uani d . 1 O
O4 0.11411(13) 0.40085(15) 0.20462(8) 0.0401(4) Uani d . 1 O
O5 0.04385(18) 0.2771(2) 0.11957(10) 0.0734(6) Uani d . 1 O
N2 0.03253(16) 0.37254(19) 0.15993(9) 0.0400(4) Uani d . 1 N
O6 -0.06808(13) 0.77556(17) 0.13453(8) 0.0453(4) Uani d . 1 O
O7 0.11162(14) 0.68127(17) 0.13578(8) 0.0474(4) Uani d . 1 O
O8 0.02837(17) 0.7806(2) 0.04701(9) 0.0689(6) Uani d . 1 O
N3 0.02408(17) 0.74586(19) 0.10504(10) 0.0413(4) Uani d . 1 N
O9 0.22927(11) 0.64245(15) 0.27811(8) 0.0439(4) Uani d . 1 O
H1 0.2596 0.7239 0.2810 0.053 Uiso d R 1 H
H2 0.2820 0.5820 0.2825 0.053 Uiso d R 1 H
C1 0.2587(2) 0.5006(3) -0.00306(13) 0.0488(6) Uani d . 1 C
N4 0.3114(2) 0.4031(2) -0.03940(13) 0.0725(7) Uani d . 1 N
H3 0.2902 0.3972 -0.0805 0.087 Uiso calc R 1 H
H4 0.3668 0.3455 -0.0220 0.087 Uiso calc R 1 H
N5 0.1742(2) 0.5887(3) -0.02918(11) 0.0680(7) Uani d . 1 N
H5 0.1402 0.6519 -0.0053 0.082 Uiso calc R 1 H
H6 0.1526 0.5833 -0.0702 0.082 Uiso calc R 1 H
N6 0.29067(19) 0.5099(2) 0.05970(11) 0.0626(6) Uani d . 1 N
H7 0.2562 0.5735 0.0832 0.075 Uiso calc R 1 H
H8 0.3461 0.4525 0.0773 0.075 Uiso calc R 1 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
La1 0.02193(7) 0.02200(7) 0.02968(9) 0.000 0.00206(5) 0.000
O1 0.0245(7) 0.0307(7) 0.0700(12) 0.0031(5) 0.0152(7) 0.0022(7)
O2 0.0606(16) 0.0235(12) 0.186(4) 0.000 0.058(2) 0.000
N1 0.0354(14) 0.0252(12) 0.068(2) 0.000 0.0143(13) 0.000
O3 0.0401(8) 0.0459(9) 0.0439(10) 0.0142(7) -0.0086(7) -0.0129(7)
O4 0.0379(8) 0.0342(8) 0.0461(10) 0.0061(6) -0.0091(7) -0.0047(7)
O5 0.0835(13) 0.0677(12) 0.0659(14) 0.0328(10) -0.0143(11) -0.0387(11)
N2 0.0455(10) 0.0347(9) 0.0389(11) 0.0099(8) -0.0019(8) -0.0067(9)
O6 0.0411(9) 0.0547(9) 0.0413(10) 0.0142(7) 0.0111(7) 0.0106(8)
O7 0.0430(9) 0.0529(9) 0.0474(10) 0.0163(7) 0.0105(8) 0.0101(8)
O8 0.0791(13) 0.0894(13) 0.0408(11) 0.0313(11) 0.0209(10) 0.0240(10)
N3 0.0477(11) 0.0401(10) 0.0374(11) 0.0101(8) 0.0109(9) 0.0073(9)
O9 0.0221(6) 0.0295(7) 0.0797(12) 0.0005(6) 0.0022(7) -0.0084(8)
C1 0.0469(14) 0.0483(13) 0.0512(17) 0.0087(10) 0.0032(12) -0.0092(12)
N4 0.0796(17) 0.0672(15) 0.0711(17) 0.0217(12) 0.0088(13) -0.0218(13)
N5 0.0658(14) 0.0906(17) 0.0450(13) 0.0346(13) -0.0120(12) -0.0131(12)
N6 0.0671(14) 0.0702(15) 0.0486(14) 0.0335(11) -0.0087(11) -0.0024(12)
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'
La La -0.2871 2.4523 '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
O9 La1 O9 2 . 179.86(7)
O9 La1 O3 2 . 68.43(5)
O9 La1 O3 . . 111.67(5)
O9 La1 O3 2 2 111.67(5)
O9 La1 O3 . 2 68.43(5)
O3 La1 O3 . 2 96.51(7)
O9 La1 O1 2 . 111.57(4)
O9 La1 O1 . . 68.29(4)
O3 La1 O1 . . 129.30(5)
O3 La1 O1 2 . 125.69(5)
O9 La1 O1 2 2 68.29(4)
O9 La1 O1 . 2 111.57(4)
O3 La1 O1 . 2 125.69(5)
O3 La1 O1 2 2 129.30(5)
O1 La1 O1 . 2 47.96(6)
O9 La1 O6 2 2 113.47(5)
O9 La1 O6 . 2 66.46(5)
O3 La1 O6 . 2 164.53(5)
O3 La1 O6 2 2 68.30(5)
O1 La1 O6 . 2 65.31(5)
O1 La1 O6 2 2 66.58(5)
O9 La1 O6 2 . 66.46(5)
O9 La1 O6 . . 113.47(5)
O3 La1 O6 . . 68.30(5)
O3 La1 O6 2 . 164.53(5)
O1 La1 O6 . . 66.58(5)
O1 La1 O6 2 . 65.31(5)
O6 La1 O6 2 . 127.02(7)
O9 La1 O4 2 2 66.67(4)
O9 La1 O4 . 2 113.46(4)
O3 La1 O4 . 2 66.78(5)
O3 La1 O4 2 2 47.45(4)
O1 La1 O4 . 2 163.06(5)
O1 La1 O4 2 2 120.83(4)
O6 La1 O4 2 2 99.34(5)
O6 La1 O4 . 2 123.71(5)
O9 La1 O4 2 . 113.46(4)
O9 La1 O4 . . 66.67(4)
O3 La1 O4 . . 47.45(4)
O3 La1 O4 2 . 66.78(5)
O1 La1 O4 . . 120.83(4)
O1 La1 O4 2 . 163.06(5)
O6 La1 O4 2 . 123.71(5)
O6 La1 O4 . . 99.34(5)
O4 La1 O4 2 . 72.98(7)
O9 La1 O7 2 . 107.82(5)
O9 La1 O7 . . 72.16(5)
O3 La1 O7 . . 65.59(5)
O3 La1 O7 2 . 125.81(5)
O1 La1 O7 . . 66.92(5)
O1 La1 O7 2 . 98.98(5)
O6 La1 O7 2 . 125.17(5)
O6 La1 O7 . . 46.28(4)
O4 La1 O7 2 . 130.01(5)
O4 La1 O7 . . 64.19(5)
O9 La1 O7 2 2 72.16(5)
O9 La1 O7 . 2 107.82(5)
O3 La1 O7 . 2 125.81(5)
O3 La1 O7 2 2 65.59(5)
O1 La1 O7 . 2 98.98(5)
O1 La1 O7 2 2 66.92(5)
O6 La1 O7 2 2 46.28(4)
O6 La1 O7 . 2 125.17(5)
O4 La1 O7 2 2 64.19(5)
O4 La1 O7 . 2 130.01(5)
O7 La1 O7 . 2 165.17(6)
N1 O1 La1 . . 97.15(12)
O2 N1 O1 . 2 121.13(11)
O2 N1 O1 . . 121.13(11)
O1 N1 O1 2 . 117.7(2)
N2 O3 La1 . . 100.55(11)
N2 O4 La1 . . 95.36(11)
O5 N2 O4 . . 122.66(18)
O5 N2 O3 . . 121.08(18)
O4 N2 O3 . . 116.26(17)
N3 O6 La1 . . 98.58(12)
N3 O7 La1 . . 96.56(12)
O8 N3 O6 . . 120.37(19)
O8 N3 O7 . . 121.2(2)
O6 N3 O7 . . 118.39(19)
La1 O9 H1 . . 114.4
La1 O9 H2 . . 136.4
H1 O9 H2 . . 109.1
N5 C1 N6 . . 119.4(2)
N5 C1 N4 . . 120.4(3)
N6 C1 N4 . . 120.2(2)
C1 N4 H3 . . 120.0
C1 N4 H4 . . 120.0
H3 N4 H4 . . 120.0
C1 N5 H5 . . 120.0
C1 N5 H6 . . 120.0
H5 N5 H6 . . 120.0
C1 N6 H7 . . 120.0
C1 N6 H8 . . 120.0
H7 N6 H8 . . 120.0
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
La1 O9 . 2.5409(12) y
La1 O3 . 2.6112(14) y
La1 O1 . 2.6603(14) y
La1 O6 . 2.7174(15) y
La1 O4 . 2.7254(14) y
La1 O7 . 2.7562(16) y
La1 O9 2 2.5409(12) ?
La1 O3 2 2.6112(14) ?
La1 O1 2 2.6603(13) ?
La1 O6 2 2.7174(15) ?
La1 O4 2 2.7254(14) ?
La1 O7 2 2.7562(16) ?
O1 N1 . 1.2632(16) ?
O2 N1 . 1.200(3) ?
N1 O1 2 1.2632(16) ?
O3 N2 . 1.272(2) ?
O4 N2 . 1.259(2) ?
O5 N2 . 1.213(2) ?
O6 N3 . 1.250(2) ?
O7 N3 . 1.254(2) ?
O8 N3 . 1.238(2) ?
O9 H1 . 0.8114 ?
O9 H2 . 0.7982 ?
C1 N5 . 1.309(3) ?
C1 N6 . 1.313(3) ?
C1 N4 . 1.321(3) ?
N4 H3 . 0.8600 ?
N4 H4 . 0.8600 ?
N5 H5 . 0.8600 ?
N5 H6 . 0.8600 ?
N6 H7 . 0.8600 ?
N6 H8 . 0.8600 ?
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
O9 H1 O4 4 0.81 2.13 2.9157(18) 163
O9 H2 O1 4_545 0.80 2.14 2.9060(18) 161
N4 H4 O8 3_545 0.86 2.26 3.069(3) 156
N5 H5 O8 . 0.86 2.06 2.908(3) 169
N5 H6 O3 5_565 0.86 2.02 2.863(3) 166
N6 H7 O7 . 0.86 2.22 3.037(3) 159
N6 H8 O6 3_545 0.86 2.16 2.989(2) 161
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168308792