#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$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-κ²O,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-κ²O,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       ω
_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/[σ²(Fo²)+(0.0157P)²] where P = (Fo²+2Fc²)/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>2σ(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_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
