##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
                                             
data_global
_audit_creation_method     'from SHELXTL CIF and IUCr SHELXL97-template'
_journal_date_recd_electronic     2003-10-30
_journal_date_accepted     2003-11-04
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2003
_journal_volume     59
_journal_issue     12
_journal_page_first     m1124
_journal_page_last     m1126
_journal_paper_category     EM
_publ_contact_author_name     'Professor Richard Dronskowski'
_publ_contact_author_address
;
      Institut für Anorganische Chemie
      RWTH Aachen
      Prof.-Pirlet-Str.1
      52056 Aachen
      Germany
;
_publ_contact_author_email     drons@HAL9000.ac.rwth-aachen.de
_publ_contact_author_fax     '+49 241 80 92288'
_publ_contact_author_phone     '+49 241 80 93642'
_publ_section_title
;
Hexaaquabis(dicyanoguanidine)terbium(III) trichloride
;
loop_
    _publ_author_name
    _publ_author_address
    'Liao, Wuping'
;
Institut für Anorganische Chemie
RWTH Aachen
Prof.-Pirlet-Straße 1
52056 Aachen
Germany
;
    'Hu, Chunhua'
;
Institut für Anorganische Chemie
RWTH Aachen
Prof.-Pirlet-Straße 1
52056 Aachen
Germany
;
    'Dronskowski, Richard'
;
Institut für Anorganische Chemie
RWTH Aachen
Prof.-Pirlet-Straße 1
52056 Aachen
Germany
;
data_I
_chemical_name_systematic
;
Hexaaquabis(dicyanoguanidine)terbium(III) trichloride
;
_chemical_name_common     ?
_chemical_formula_moiety     'C4 H20 N8 O6 Tb 3+, 3Cl 1-'
_chemical_formula_sum     'C4 H20 Cl3 N8 O6 Tb'
_chemical_formula_iupac     '[Tb (C2 H4 N4)2 (H2 O)6], Cl3'
_chemical_formula_weight     541.55
_chemical_melting_point     ?
_symmetry_cell_setting     'orthorhombic'
_symmetry_space_group_name_H-M     'F d d 2'
_symmetry_space_group_name_Hall     'F 2 -2d'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, z'
    'x+1/4, -y+1/4, z+1/4'
    '-x+1/4, y+1/4, z+1/4'
    'x, y+1/2, z+1/2'
    '-x, -y+1/2, z+1/2'
    'x+1/4, -y+3/4, z+3/4'
    '-x+1/4, y+3/4, z+3/4'
    'x+1/2, y, z+1/2'
    '-x+1/2, -y, z+1/2'
    'x+3/4, -y+1/4, z+3/4'
    '-x+3/4, y+1/4, z+3/4'
    'x+1/2, y+1/2, z'
    '-x+1/2, -y+1/2, z'
    'x+3/4, -y+3/4, z+1/4'
    '-x+3/4, y+3/4, z+1/4'
_cell_length_a     29.425(5)
_cell_length_b     9.2613(14)
_cell_length_c     13.690(2)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     3730.6(10)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     6486
_cell_measurement_theta_min     2.74
_cell_measurement_theta_max     28.29
_cell_measurement_temperature     293(2)
_cell_special_details
; ?
;
_exptl_crystal_description     prism
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     0.31
_exptl_crystal_size_mid     0.08
_exptl_crystal_size_min     0.05
_exptl_crystal_density_diffrn     1.928
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     2112
_exptl_absorpt_coefficient_mu     4.255
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_correction_T_min     0.290
_exptl_absorpt_correction_T_max     0.808
_exptl_special_details
;
?
;
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker AXS APEX CCD'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     6486
_diffrn_reflns_av_R_equivalents     0.0270
_diffrn_reflns_av_sigmaI/netI     0.0297
_diffrn_reflns_theta_min     2.74
_diffrn_reflns_theta_max     28.29
_diffrn_reflns_theta_full     28.29
_diffrn_measured_fraction_theta_max     1.000
_diffrn_measured_fraction_theta_full     1.000
_diffrn_reflns_limit_h_min     -39
_diffrn_reflns_limit_h_max     39
_diffrn_reflns_limit_k_min     -12
_diffrn_reflns_limit_k_max     8
_diffrn_reflns_limit_l_min     -18
_diffrn_reflns_limit_l_max     17
_diffrn_standards_number     none
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     none
_diffrn_standards_decay_%     0
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     2185
_reflns_number_gt     2065
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0237
_refine_ls_R_factor_gt     0.0222
_refine_ls_wR_factor_gt     0.0541
_refine_ls_wR_factor_ref     0.0548
_refine_ls_goodness_of_fit_ref     1.104
_refine_ls_restrained_S_all     1.101
_refine_ls_number_reflns     2185
_refine_ls_number_parameters     142
_refine_ls_number_restraints     11
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
             'calc w = 1/[σ²(Fo²)+(0.0315P)²] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.427
_refine_diff_density_min     -0.600
_refine_ls_extinction_method     SHELXL97
_refine_ls_extinction_coef     0.00174(7)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details     'Flack (1983)'
_refine_ls_abs_structure_Flack     -0.030(13)
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'
    'Cl' 'Cl' 0.1484 0.1585
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Tb' 'Tb' -0.1723 4.1537
                         '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'
_computing_data_collection     'SMART (Bruker, 2001)'
_computing_cell_refinement     'SMART'
_computing_data_reduction     'SAINT-Plus (Bruker, 1999)'
_computing_structure_solution     'SHELXTL (Sheldrick, 1998)'
_computing_structure_refinement     'SHELXTL'
_computing_molecular_graphics     'PLATON (Spek, 2003)'
_computing_publication_material     'SHELXTL'
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_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Tb 0.0000 0.0000 0.10089(3) 0.01999(9) Uani d S 1 . . Tb
    Cl1 0.16603(4) -0.02478(13) 0.12593(7) 0.0356(2) Uani d . 1 . . Cl
    Cl2 0.0000 0.5000 0.1976(2) 0.0492(5) Uani d S 1 . . Cl
    O1 0.04611(10) 0.1990(3) 0.1609(2) 0.0318(6) Uani d D 1 . . O
    H11 0.0568(18) 0.199(7) 0.216(2) 0.048(16) Uiso d D 1 . . H
    H12 0.032(2) 0.275(5) 0.155(6) 0.07(2) Uiso d D 1 . . H
    O2 0.00361(10) 0.1841(5) -0.0176(3) 0.0485(11) Uani d D 1 . . O
    H21 0.0287(11) 0.214(6) -0.033(4) 0.042(16) Uiso d D 1 . . H
    H22 -0.016(2) 0.200(9) -0.059(5) 0.07(2) Uiso d D 1 . . H
    O3 0.07309(11) -0.0297(4) 0.0302(3) 0.0350(7) Uani d D 1 . . O
    H31 0.079(2) -0.092(6) -0.010(4) 0.059(18) Uiso d D 1 . . H
    H32 0.0965(15) -0.026(7) 0.062(5) 0.06(2) Uiso d D 1 . . H
    C1 0.06201(13) -0.1393(5) 0.3052(3) 0.0287(8) Uani d . 1 . . C
    C2 0.12159(13) -0.1881(4) 0.4076(3) 0.0285(8) Uani d . 1 . . C
    N1 0.04525(11) -0.1007(4) 0.2344(3) 0.0354(8) Uani d . 1 . . N
    N2 0.07682(12) -0.1836(5) 0.3896(3) 0.0358(8) Uani d . 1 . . N
    N3 0.15310(12) -0.1520(5) 0.3449(3) 0.0439(10) Uani d D 1 . . N
    H33 0.1797(9) -0.156(5) 0.369(4) 0.039(14) Uiso d D 1 . . H
    H34 0.1485(19) -0.120(6) 0.287(2) 0.050(16) Uiso d D 1 . . H
    N4 0.13413(16) -0.2305(5) 0.4966(4) 0.0440(11) Uani d D 1 . . N
    H41 0.1621(10) -0.254(6) 0.507(7) 0.06(2) Uiso d D 1 . . H
    H42 0.116(2) -0.232(6) 0.545(4) 0.05(2) Uiso d D 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
    Tb 0.01711(11) 0.02478(12) 0.01808(12) -0.00021(10) 0.000 0.000
    Cl1 0.0266(5) 0.0518(6) 0.0284(6) -0.0048(4) -0.0025(3) -0.0053(5)
    Cl2 0.0298(8) 0.0351(9) 0.0825(16) 0.0034(6) 0.000 0.000
    O1 0.0363(16) 0.0269(15) 0.0322(16) -0.0005(12) -0.0099(13) -0.0014(13)
    O2 0.0232(16) 0.073(3) 0.050(2) -0.0123(16) -0.0092(14) 0.037(2)
    O3 0.0196(14) 0.0504(19) 0.0352(18) 0.0024(13) 0.0000(12) -0.0114(15)
    C1 0.0239(18) 0.031(2) 0.031(2) -0.0048(15) 0.0011(15) 0.0074(16)
    C2 0.0295(19) 0.0258(18) 0.0301(19) -0.0023(15) -0.0072(15) 0.0067(16)
    N1 0.0309(17) 0.040(2) 0.0353(19) -0.0024(15) -0.0085(15) 0.0104(16)
    N2 0.0291(18) 0.046(2) 0.033(2) -0.0032(15) -0.0023(14) 0.0156(18)
    N3 0.0256(17) 0.064(3) 0.042(2) -0.0072(17) -0.0039(17) 0.018(2)
    N4 0.035(2) 0.055(3) 0.042(3) 0.0040(18) -0.0104(19) 0.0144(19)
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
 PLAT731 Type_1 Test for consistency of Bond su's and Coordinate su's in CIF
 A large ratio of the reported and calculated bond s.u.'s is found.
 The use of a DFIX instruction might cause such a warning since
 calculated s.u.'s are based on reported variances only.
 Note_1: su's on the unitcell dimensions are taken into account in the
 calculation of expected su's. This may result in large differences
 between expected and reported su's when this contribution is not included
 in the reported su's, in particular for inaccurate unitcells.
 Note_2: Another source for the discrepancy between calculated and
 reported su's can be that the validation software has access only to
 the variances of the refined parameters as opposed to the full co-variance
 matrix used by e.g. SHELXL for the calculation of derived parameters
 with associated su's. Constrained/restrained refinement may cause largei
 co-variances.
;
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
    Tb O1 . 2.432(3) yes
    Tb O1 2 2.432(3) ?
    Tb O2 . 2.356(4) yes
    Tb O2 2 2.356(4) ?
    Tb O3 . 2.374(3) yes
    Tb O3 2 2.374(3) ?
    Tb N1 . 2.446(4) yes
    Tb N1 2 2.446(4) ?
    O1 H11 . 0.82(2) ?
    O1 H12 . 0.82(2) ?
    O2 H21 . 0.82(2) ?
    O2 H22 . 0.82(2) ?
    O3 H31 . 0.81(2) ?
    O3 H32 . 0.81(2) ?
    C1 N1 . 1.145(5) ?
    C1 N2 . 1.301(5) ?
    C2 N2 . 1.341(5) ?
    C2 N3 . 1.307(5) ?
    C2 N4 . 1.332(6) ?
    N3 H33 . 0.853(19) ?
    N3 H34 . 0.86(2) ?
    N4 H41 . 0.86(2) ?
    N4 H42 . 0.85(2) ?
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
    O2 Tb O2 2 . 93.0(3) yes
    O2 Tb O3 2 2 76.25(13) ?
    O2 Tb O3 . 2 71.12(11) ?
    O2 Tb O3 2 . 71.12(11) ?
    O2 Tb O3 . . 76.25(13) ?
    O3 Tb O3 2 . 131.88(17) yes
    O2 Tb O1 2 . 143.75(11) ?
    O2 Tb O1 . . 70.06(13) ?
    O3 Tb O1 2 . 123.74(12) ?
    O3 Tb O1 . . 73.75(12) ?
    O2 Tb O1 2 2 70.06(13) ?
    O2 Tb O1 . 2 143.75(12) ?
    O3 Tb O1 2 2 73.75(12) ?
    O3 Tb O1 . 2 123.74(12) ?
    O1 Tb O1 . 2 140.49(16) yes
    O2 Tb N1 2 . 105.24(16) ?
    O2 Tb N1 . . 139.99(12) yes
    O3 Tb N1 2 . 147.33(12) ?
    O3 Tb N1 . . 76.55(13) yes
    O1 Tb N1 . . 74.50(11) yes
    O1 Tb N1 2 . 76.24(11) ?
    O2 Tb N1 2 2 139.99(12) ?
    O2 Tb N1 . 2 105.24(16) ?
    O3 Tb N1 2 2 76.55(13) ?
    O3 Tb N1 . 2 147.33(12) ?
    O1 Tb N1 . 2 76.24(11) ?
    O1 Tb N1 2 2 74.50(11) ?
    N1 Tb N1 . 2 83.32(19) yes
    Tb O1 H11 . . 122(4) ?
    Tb O1 H12 . . 110(6) ?
    H11 O1 H12 . . 107(7) ?
    Tb O2 H21 . . 118(4) ?
    Tb O2 H22 . . 125(6) ?
    H21 O2 H22 . . 113(8) ?
    Tb O3 H31 . . 123(4) ?
    Tb O3 H32 . . 123(5) ?
    H31 O3 H32 . . 102(6) ?
    N1 C1 N2 . . 174.0(4) ?
    N3 C2 N4 . . 118.7(4) ?
    N3 C2 N2 . . 124.6(4) ?
    N4 C2 N2 . . 116.7(4) ?
    C1 N1 Tb . . 170.5(4) ?
    C1 N2 C2 . . 120.2(4) ?
    C2 N3 H33 . . 113(4) ?
    C2 N3 H34 . . 126(4) ?
    H33 N3 H34 . . 121(5) ?
    C2 N4 H41 . . 119(6) ?
    C2 N4 H42 . . 123(5) ?
    H41 N4 H42 . . 117(8) ?
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
    _geom_hbond_publ_flag
    O1 H11 Cl1 4 0.82(2) 2.34(2) 3.156(3) 174(6) yes
    O1 H12 Cl2 . 0.82(2) 2.36(3) 3.141(3) 159(8) yes
    O2 H21 N2 5_554 0.82(2) 2.00(3) 2.785(5) 160(6) yes
    O2 H22 Cl1 11_454 0.82(2) 2.29(4) 3.077(3) 159(8) yes
    O3 H31 Cl1 8_544 0.81(2) 2.31(2) 3.117(4) 172(6) yes
    O3 H32 Cl1 . 0.81(2) 2.23(2) 3.033(3) 171(7) yes
    N3 H33 Cl2 3 0.853(19) 2.49(2) 3.306(4) 161(4) yes
    N3 H34 Cl1 . 0.86(2) 2.43(3) 3.243(5) 159(5) yes
    N4 H41 Cl2 3 0.86(2) 2.71(5) 3.480(5) 149(7) yes
    N4 H42 O1 5_545 0.85(2) 2.67(3) 3.492(6) 161(6) yes
