#------------------------------------------------------------------------------
#$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2002952.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_2002952
loop_
_publ_author_name
'Ross, II, C. R.'
'Paulsen, B. L.'
'Nielson, R. M.'
'Abrahams, S. C.'
_publ_section_title
;
 Aminoguanidinium(2+) Hexafluorozirconate Monohydrate: A Co-Product of
 Preparing the Ferroelectric Anhydrous Salt
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              417
_journal_page_last               423
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'CN4H8 ZrF6 H2O'
_chemical_formula_sum            'C H10 F6 N4 O Zr'
_chemical_formula_weight         299.33
_chemical_name_common
'Aminoguanidinium hexafluorozirconate hydrate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.326(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.3770(7)
_cell_length_b                   9.7522(6)
_cell_length_c                   13.8543(11)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      12.0
_cell_volume                     1658.60(19)
_computing_cell_refinement       'XSCANS 2.1 (Siemens, 1993)'
_computing_data_collection       'XSCANS 2.1 (Siemens, 1993)'
_computing_data_reduction        'XSCANS (Siemens, 1993)'
_computing_molecular_graphics    'SHELXTL 5.0 (Siemens, 1995)'
_computing_publication_material  'SHELXTL 5.0 (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \q-2\q
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4811
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_T_max  0.473
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_type   'psi scans (Siemens, 1993)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.397
_exptl_crystal_density_meas      2.31(4)
_exptl_crystal_density_method    'pycnometry at 295K'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.692
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.119
_refine_ls_goodness_of_fit_obs   1.143
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.143
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_obs          0.0299
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+1.7484P] where P=(Fo^2^+2Fc^2^)/3
(Siemens, 1995)
;
_refine_ls_wR_factor_all         0.0870
_refine_ls_wR_factor_obs         0.0842
_reflns_number_observed          3434
_reflns_number_total             3798
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    br0070.cif
_[local]_cod_data_source_block   BR70
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_cod_original_cell_volume        1658.60(4)
_cod_database_code               2002952
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Zr1 0.01204(14) 0.01414(14) 0.01882(14) 0.00051(8) 0.00198(10) -0.00126(8)
Zr2 0.01553(14) 0.01659(14) 0.01496(14) 0.00180(8) 0.00162(10) 0.00037(8)
F1 0.0156(7) 0.0213(8) 0.0374(9) 0.0004(6) -0.0028(7) -0.0053(7)
F2 0.0283(9) 0.0278(9) 0.0469(11) 0.0033(8) -0.0110(8) 0.0093(8)
F3 0.0275(9) 0.0218(8) 0.0456(11) -0.0009(7) 0.0074(8) -0.0115(8)
F4 0.0301(9) 0.0196(8) 0.0351(9) -0.0014(7) -0.0123(8) 0.0005(7)
F5 0.0329(10) 0.0195(8) 0.0299(9) 0.0035(7) -0.0123(7) -0.0035(7)
F6 0.0264(9) 0.0338(9) 0.0313(9) -0.0089(7) 0.0129(7) -0.0087(8)
F7 0.0330(9) 0.0286(9) 0.0321(9) -0.0110(8) 0.0153(8) -0.0119(7)
F8 0.0260(8) 0.0337(9) 0.0248(8) -0.0121(7) 0.0091(7) -0.0104(7)
F9 0.0269(9) 0.0440(11) 0.0271(9) -0.0005(8) 0.0099(7) -0.0032(8)
F10 0.0284(9) 0.0282(9) 0.0237(8) 0.0017(7) -0.0028(7) -0.0064(7)
F11 0.0326(9) 0.0276(9) 0.0272(9) 0.0127(7) -0.0055(7) -0.0009(7)
F12 0.0276(9) 0.0210(8) 0.0471(11) -0.0018(7) 0.0096(8) 0.0035(8)
C1A 0.0246(14) 0.0200(13) 0.0279(14) -0.0008(11) 0.0013(11) -0.0027(11)
N1A 0.0236(12) 0.0185(12) 0.050(2) -0.0006(10) 0.0010(11) -0.0119(11)
N2A 0.0243(13) 0.0249(13) 0.056(2) -0.0005(11) 0.0001(12) -0.0077(12)
N3A 0.0251(13) 0.0190(12) 0.050(2) -0.0025(10) -0.0020(11) -0.0117(11)
N4A 0.0317(14) 0.0216(12) 0.0289(13) 0.0056(10) -0.0030(10) -0.0073(10)
C1B 0.0211(13) 0.0271(14) 0.0263(13) -0.0039(12) 0.0028(10) 0.0051(12)
N1B 0.0225(12) 0.0325(14) 0.043(2) -0.0072(11) 0.0011(11) 0.0141(12)
N2B 0.0184(12) 0.036(2) 0.077(2) 0.0000(11) 0.0039(13) 0.029(2)
N3B 0.0198(12) 0.0332(15) 0.059(2) -0.0016(11) 0.0002(12) 0.0231(14)
N4B 0.0220(12) 0.041(2) 0.049(2) 0.0008(12) -0.0036(12) 0.0216(14)
O1W1 0.044(2) 0.037(2) 0.046(2) 0.004(2) 0.010(2) 0.007(2)
O2W1 0.055(10) 0.035(8) 0.044(8) 0.003(8) 0.011(9) 0.004(6)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Zr1 0.81610(2) 0.11839(2) 0.50967(2) 0.01500(9) Uani d . 1 Zr
Zr2 1.00976(2) 0.12107(2) 0.33245(2) 0.01572(9) Uani d . 1 Zr
F1 0.69060(13) -0.0125(2) 0.44744(13) 0.0253(4) Uani d . 1 F
F2 0.7249(2) 0.2399(2) 0.41729(15) 0.0357(4) Uani d . 1 F
F3 0.82696(14) 0.3029(2) 0.58486(14) 0.0314(4) Uani d . 1 F
F4 0.9453(2) 0.0933(2) 0.63250(14) 0.0297(4) Uani d . 1 F
F5 0.8612(2) -0.0943(2) 0.54993(13) 0.0288(4) Uani d . 1 F
F6 0.71618(15) 0.0937(2) 0.61477(13) 0.0297(4) Uani d . 1 F
F7 0.87391(15) 0.0252(2) 0.38562(13) 0.0303(4) Uani d . 1 F
F8 0.95740(14) 0.2174(2) 0.46324(12) 0.0277(4) Uani d . 1 F
F9 1.13241(15) 0.0878(2) 0.25012(13) 0.0321(4) Uani d . 1 F
F10 0.93397(14) 0.0228(2) 0.21130(12) 0.0273(4) Uani d . 1 F
F11 0.89490(15) 0.2570(2) 0.26995(13) 0.0300(4) Uani d . 1 F
F12 1.09076(14) 0.3069(2) 0.33685(15) 0.0315(4) Uani d . 1 F
C1A 0.8714(2) 0.5836(3) 0.3628(2) 0.0243(6) Uani d . 1 C
N1A 0.7975(2) 0.4940(3) 0.3275(2) 0.0311(6) Uani d . 1 N
H1AA 0.8170(2) 0.4135(3) 0.3113(2) 0.037 Uiso calc R 1 H
H1AB 0.7297(2) 0.5159(3) 0.3207(2) 0.037 Uiso calc R 1 H
N2A 0.9760(2) 0.5534(3) 0.3741(2) 0.0355(6) Uani d . 1 N
H2AA 0.9973(2) 0.4734(3) 0.3583(2) 0.043 Uiso calc R 1 H
H2AB 1.0231(2) 0.6136(3) 0.3973(2) 0.043 Uiso calc R 1 H
N3A 0.8421(2) 0.7123(3) 0.3859(2) 0.0321(6) Uani d . 1 N
H3AA 0.8888(2) 0.7781(3) 0.3911(2) 0.038 Uiso calc R 1 H
N4A 0.7329(2) 0.7355(3) 0.4014(2) 0.0280(5) Uani d . 1 N
H1NA 0.7263(2) 0.8177(3) 0.4222(2) 0.042 Uiso calc R 1 H
H2NA 0.7151(2) 0.6782(3) 0.4439(2) 0.042 Uiso calc R 1 H
H3NA 0.6908(2) 0.7245(3) 0.3476(2) 0.042 Uiso calc R 1 H
C1B 0.4462(2) 0.1623(3) 0.3476(2) 0.0249(6) Uani d . 1 C
N1B 0.5157(2) 0.2566(3) 0.3275(2) 0.0331(6) Uani d . 1 N
H1BA 0.5846(2) 0.2417(3) 0.3398(2) 0.040 Uiso calc R 1 H
H1BB 0.4924(2) 0.3332(3) 0.3020(2) 0.040 Uiso calc R 1 H
N2B 0.4791(2) 0.0457(3) 0.3861(3) 0.0441(8) Uani d . 1 N
H2BA 0.5477(2) 0.0291(3) 0.3989(3) 0.053 Uiso calc R 1 H
H2BB 0.4324(2) -0.0148(3) 0.3988(3) 0.053 Uiso calc R 1 H
N3B 0.3383(2) 0.1831(3) 0.3315(2) 0.0379(7) Uani d . 1 N
H3BA 0.2957(2) 0.1219(3) 0.3507(2) 0.045 Uiso calc R 1 H
N4B 0.2927(2) 0.2993(3) 0.2851(2) 0.0381(7) Uani d . 1 N
H1NB 0.2232(2) 0.2976(3) 0.2849(2) 0.057 Uiso calc R 1 H
H2NB 0.3076(2) 0.3012(3) 0.2261(2) 0.057 Uiso calc R 1 H
H3NB 0.3189(2) 0.3712(3) 0.3154(2) 0.057 Uiso calc R 1 H
O1W1 0.6907(3) 0.5284(4) 0.5399(3) 0.0419(9) Uani d P 0.80 O
O2W1 0.7439(15) 0.5543(18) 0.5504(13) 0.044(4) Uani d P 0.20 O
O1W2 0.5191(4) 0.3162(5) 0.5584(4) 0.0723(12) Uiso d P 0.80 O
O2W2 0.5003(17) 0.390(2) 0.5397(14) 0.068(5) Uiso d P 0.20 O
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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'
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
F2 Zr1 F6 . . 100.59(9)
F2 Zr1 F3 . . 78.54(8)
F6 Zr1 F3 . . 75.57(7)
F2 Zr1 F1 . . 76.67(7)
F6 Zr1 F1 . . 74.83(7)
F3 Zr1 F1 . . 136.69(7)
F2 Zr1 F7 . . 87.52(8)
F6 Zr1 F7 . . 144.62(7)
F3 Zr1 F7 . . 139.68(7)
F1 Zr1 F7 . . 73.71(7)
F2 Zr1 F8 . . 87.51(8)
F6 Zr1 F8 . . 148.22(7)
F3 Zr1 F8 . . 76.07(7)
F1 Zr1 F8 . . 136.82(7)
F7 Zr1 F8 . . 65.59(6)
F2 Zr1 F4 . . 149.73(7)
F6 Zr1 F4 . . 83.20(8)
F3 Zr1 F4 . . 73.34(7)
F1 Zr1 F4 . . 132.49(7)
F7 Zr1 F4 . . 106.82(8)
F8 Zr1 F4 . . 75.16(7)
F2 Zr1 F5 . . 146.11(7)
F6 Zr1 F5 . . 82.24(8)
F3 Zr1 F5 . . 133.78(7)
F1 Zr1 F5 . . 71.51(6)
F7 Zr1 F5 . . 72.79(7)
F8 Zr1 F5 . . 107.89(7)
F4 Zr1 F5 . . 64.05(6)
F2 Zr1 Zr2 . . 85.99(6)
F6 Zr1 Zr2 . . 172.73(6)
F3 Zr1 Zr2 . . 109.03(5)
F1 Zr1 Zr2 . . 104.03(5)
F7 Zr1 Zr2 . . 31.59(5)
F8 Zr1 Zr2 . . 34.03(4)
F4 Zr1 Zr2 . . 92.66(6)
F5 Zr1 Zr2 . . 90.58(5)
F9 Zr2 F10 . . 76.31(7)
F9 Zr2 F11 . . 113.08(8)
F10 Zr2 F11 . . 74.75(7)
F9 Zr2 F12 . . 76.31(8)
F10 Zr2 F12 . . 127.04(8)
F11 Zr2 F12 . . 75.73(7)
F9 Zr2 F7 . . 143.01(7)
F10 Zr2 F7 . . 77.28(7)
F11 Zr2 F7 . . 83.97(8)
F12 Zr2 F7 . . 140.68(7)
F9 Zr2 F5 . 3_756 82.55(8)
F10 Zr2 F5 . 3_756 141.43(7)
F11 Zr2 F5 . 3_756 143.78(7)
F12 Zr2 F5 . 3_756 76.91(7)
F7 Zr2 F5 . 3_756 103.13(8)
F9 Zr2 F4 . 3_756 77.69(8)
F10 Zr2 F4 . 3_756 79.24(7)
F11 Zr2 F4 . 3_756 148.01(7)
F12 Zr2 F4 . 3_756 135.87(7)
F7 Zr2 F4 . 3_756 72.30(7)
F5 Zr2 F4 3_756 3_756 64.82(7)
F9 Zr2 F8 . . 147.55(7)
F10 Zr2 F8 . . 135.85(7)
F11 Zr2 F8 . . 79.14(7)
F12 Zr2 F8 . . 78.17(7)
F7 Zr2 F8 . . 65.00(6)
F5 Zr2 F8 3_756 . 72.37(7)
F4 Zr2 F8 3_756 . 108.37(7)
F9 Zr2 Zr1 . . 167.71(6)
F10 Zr2 Zr1 . . 106.04(5)
F11 Zr2 Zr1 . . 79.00(5)
F12 Zr2 Zr1 . . 110.15(5)
F7 Zr2 Zr1 . . 31.77(5)
F5 Zr2 Zr1 3_756 . 88.70(6)
F4 Zr2 Zr1 3_756 . 90.80(5)
F8 Zr2 Zr1 . . 33.26(4)
Zr1 F4 Zr2 . 3_756 114.54(8)
Zr2 F5 Zr1 3_756 . 116.56(8)
Zr2 F7 Zr1 . . 116.64(8)
Zr1 F8 Zr2 . . 112.71(7)
N1A C1A N2A . . 121.5(3)
N1A C1A N3A . . 120.6(3)
N2A C1A N3A . . 117.9(3)
C1A N1A H1AA . . 120.0(2)
C1A N1A H1AB . . 120.0(2)
H1AA N1A H1AB . . 120.0
C1A N2A H2AA . . 120.0(2)
C1A N2A H2AB . . 120.0(2)
H2AA N2A H2AB . . 120.0
C1A N3A N4A . . 118.3(2)
C1A N3A H3AA . . 120.9(2)
N4A N3A H3AA . . 120.86(15)
N3A N4A H1NA . . 109.47(14)
N3A N4A H2NA . . 109.5(2)
H1NA N4A H2NA . . 109.5
N3A N4A H3NA . . 109.5(2)
H1NA N4A H3NA . . 109.5
H2NA N4A H3NA . . 109.5
N2B C1B N1B . . 121.3(3)
N2B C1B N3B . . 117.0(3)
N1B C1B N3B . . 121.7(3)
C1B N1B H1BA . . 120.0(2)
C1B N1B H1BB . . 120.0(2)
H1BA N1B H1BB . . 120.0
C1B N2B H2BA . . 120.0(2)
C1B N2B H2BB . . 120.0(2)
H2BA N2B H2BB . . 120.0
C1B N3B N4B . . 122.6(3)
C1B N3B H3BA . . 118.7(2)
N4B N3B H3BA . . 118.7(2)
N3B N4B H1NB . . 109.5(2)
N3B N4B H2NB . . 109.5(2)
H1NB N4B H2NB . . 109.5
N3B N4B H3NB . . 109.5(2)
H1NB N4B H3NB . . 109.5
H2NB N4B H3NB . . 109.5
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
Zr1 F2 . 1.987(2) yes
Zr1 F6 . 2.041(2) yes
Zr1 F3 . 2.075(2) yes
Zr1 F1 . 2.108(2) yes
Zr1 F7 . 2.146(2) yes
Zr1 F8 . 2.166(2) yes
Zr1 F4 . 2.195(2) yes
Zr1 F5 . 2.201(2) yes
Zr1 Zr2 . 3.6434(4) ?
Zr2 F9 . 2.038(2) yes
Zr2 F10 . 2.053(2) yes
Zr2 F11 . 2.053(2) yes
Zr2 F12 . 2.068(2) yes
Zr2 F7 . 2.135(2) yes
Zr2 F5 3_756 2.147(2) yes
Zr2 F4 3_756 2.202(2) yes
Zr2 F8 . 2.210(2) yes
F4 Zr2 3_756 2.202(2) ?
F5 Zr2 3_756 2.147(2) ?
C1A N1A . 1.313(4) yes
C1A N2A . 1.318(4) yes
C1A N3A . 1.356(4) yes
N1A H1AA . 0.86 ?
N1A H1AB . 0.86 ?
N2A H2AA . 0.86 ?
N2A H2AB . 0.86 ?
N3A N4A . 1.414(4) yes
N3A H3AA . 0.86 ?
N4A H1NA . 0.86 ?
N4A H2NA . 0.86 ?
N4A H3NA . 0.86 ?
C1B N2B . 1.299(4) yes
C1B N1B . 1.313(4) yes
C1B N3B . 1.340(4) yes
N1B H1BA . 0.86 ?
N1B H1BB . 0.86 ?
N2B H2BA . 0.86 ?
N2B H2BB . 0.86 ?
N3B N4B . 1.387(4) yes
N3B H3BA . 0.86 ?
N4B H1NB . 0.86 ?
N4B H2NB . 0.86 ?
N4B H3NB . 0.86 ?
O1W1 O2W1 . 0.70(2) ?
O1W2 O2W2 . 0.79(2) ?