#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2002962.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_2002962
loop_
_publ_author_name
'Ross, II, C. R.'
'Bauer, M. R.'
'Nielson, R. M.'
'Abrahams, S. C.'
_publ_section_title
;
 Anhydrous ammonioguanidinium(2+) and dihydrated
 bis[aminoguanidinium(1+)] hexafluorosilicates: new co-products of
 preparing ferroelectric ammonioguanidinium(2+) hexafluorozirconate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              246
_journal_page_last               254
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C1 H8 N4,F6 Si'
_chemical_formula_sum            'C H8 F6 N4 Si'
_chemical_formula_weight         218.20
_chemical_name_systematic
;
 aminoguanidinium(2+) hexafluorosilicate
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.42320(10)
_cell_length_b                   17.6675(2)
_cell_length_c                   7.53630(10)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      47.5
_cell_measurement_theta_min      42.5
_cell_volume                     1387.82(3)
_computing_cell_refinement       'CAD4 EXPRESS (Enraf-Nonius, 1988)'
_computing_data_collection       'CAD4 EXPRESS (Enraf-Nonius, 1988)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_molecular_graphics
;
DRAWXTL (Finger and Kroeker, 1997),
ORTEP-III (Burnett and Johnson, 1996)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .856
_diffrn_measured_fraction_theta_max .856
_diffrn_measurement_device_type  MACH3
_diffrn_measurement_method       '\w - 2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  .0191
_diffrn_reflns_av_sigmaI/netI    .0143
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3143
_diffrn_reflns_theta_full        69.73
_diffrn_reflns_theta_max         69.73
_diffrn_reflns_theta_min         4.93
_diffrn_standards_decay_%        7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.888
_exptl_absorpt_correction_T_max  .595
_exptl_absorpt_correction_T_min  .415
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 using ABSPSI -
 Alcock, N.W. and Marks, P.J. (1994). J. Appl. Cryst. 27, 200
;
_exptl_crystal_colour            'colorless, clear'
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_density_meas      2.11(3)
_exptl_crystal_density_method    pycnometry
_exptl_crystal_description       blocky
_exptl_crystal_F_000             880
_exptl_crystal_size_max          .290
_exptl_crystal_size_mid          .170
_exptl_crystal_size_min          .160
_refine_diff_density_max         .215
_refine_diff_density_min         -.307
_refine_ls_extinction_coef       .0076(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          .0268
_refine_ls_R_factor_gt           .0255
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.4906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_ref         .0653
_reflns_number_gt                1267
_reflns_number_total             1315
_reflns_threshold_expression     >2sigma(I)
_[local]_cod_data_source_file    br0080.cif
_[local]_cod_data_source_block   anhydrous
_cod_database_code               2002962
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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_occupancy
_atom_site_type_symbol
Si .45067(3) .36631(2) .61337(5) .01893(15) Uani d 1 Si
F1 .53956(8) .42962(5) .72439(12) .0304(2) Uani d 1 F
F2 .39434(9) .43412(5) .48043(12) .0324(2) Uani d 1 F
F3 .32849(8) .38265(6) .75852(12) .0357(2) Uani d 1 F
F4 .50423(9) .29678(5) .75149(12) .0357(2) Uani d 1 F
F5 .35997(8) .30235(5) .50833(11) .0311(2) Uani d 1 F
F6 .57320(9) .34800(6) .47477(12) .0376(3) Uani d 1 F
C .61530(13) .40105(8) .10974(18) .0236(3) Uani d 1 C
N1 .66326(14) .33835(8) .0451(2) .0353(3) Uani d 1 N
H1A .744(3) .3375(13) .028(3) .051(6) Uiso d 1 H
H1B .617(3) .3107(16) -.008(4) .074(8) Uiso d 1 H
N2 .68857(15) .45801(9) .1506(3) .0457(4) Uani d 1 N
H2A .773(3) .4530(13) .133(3) .055(6) Uiso d 1 H
H2B .657(2) .4968(15) .181(3) .055(7) Uiso d 1 H
N3 .48640(12) .40978(7) .13244(17) .0236(3) Uani d 1 N
H3 .4682(18) .4359(11) .206(3) .030(5) Uiso d 1 H
N4 .40871(12) .34376(7) .12861(19) .0258(3) Uani d 1 N
H4A .396(2) .3328(12) .025(3) .042(6) Uiso d 1 H
H4B .332(2) .3565(13) .173(3) .052(6) Uiso d 1 H
H4C .441(2) .3017(14) .186(3) .057(6) Uiso 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
Si .0159(2) .0211(2) .0198(2) -.00130(13) .00007(12) .00067(12)
F1 .0303(4) .0288(4) .0322(5) -.0101(3) -.0057(3) -.0001(3)
F2 .0338(5) .0288(4) .0347(5) .0043(4) -.0062(4) .0060(3)
F3 .0246(4) .0508(5) .0318(5) -.0060(4) .0101(4) -.0084(4)
F4 .0447(5) .0269(5) .0356(5) -.0031(4) -.0162(4) .0071(4)
F5 .0303(5) .0287(4) .0342(5) -.0045(3) -.0092(4) -.0046(3)
F6 .0219(4) .0586(6) .0323(5) .0075(4) .0049(4) -.0032(4)
C .0201(6) .0266(7) .0241(7) .0000(5) -.0012(5) .0001(5)
N1 .0189(6) .0376(7) .0494(9) .0000(5) .0018(6) -.0158(6)
N2 .0260(8) .0304(7) .0808(12) -.0038(6) -.0019(7) -.0134(7)
N3 .0209(6) .0229(6) .0270(6) .0013(5) .0008(5) -.0054(5)
N4 .0192(6) .0287(6) .0296(7) -.0026(5) .0006(5) .0026(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0727 .0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si .2541 .3302 '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
_geom_angle_publ_flag
F2 Si F5 90.11(5) y
F2 Si F1 90.87(5) y
F5 Si F1 178.29(5) y
F2 Si F6 91.86(5) y
F5 Si F6 90.30(5) y
F1 Si F6 91.07(5) y
F2 Si F3 90.05(5) y
F5 Si F3 89.76(5) y
F1 Si F3 88.84(5) y
F6 Si F3 178.09(5) y
F2 Si F4 178.48(5) y
F5 Si F4 89.26(4) y
F1 Si F4 89.72(5) y
F6 Si F4 89.53(5) y
F3 Si F4 88.56(5) y
N2 C N1 121.24(14) y
N2 C N3 117.48(14) y
N1 C N3 121.25(13) y
C N1 H1A 116.7(15) y
C N1 H1B 118(2) y
H1A N1 H1B 121(3) y
C N2 H2A 117.8(15) y
C N2 H2B 119.2(18) y
H2A N2 H2B 123(2) y
C N3 N4 117.80(12) y
C N3 H3 114.5(15) y
N4 N3 H3 112.2(15) y
N3 N4 H4A 107.8(15) y
N3 N4 H4B 107.3(14) y
H4A N4 H4B 106(2) y
N3 N4 H4C 116.4(15) y
H4A N4 H4C 109(2) y
H4B N4 H4C 111(2) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Si F2 1.6684(9) y
Si F5 1.6727(8) y
Si F1 1.6761(8) y
Si F6 1.6813(9) y
Si F3 1.7034(9) y
Si F4 1.7043(9) y
C N2 1.300(2) y
C N1 1.309(2) y
C N3 1.3632(19) y
N1 H1A .85(3) y
N1 H1B .80(3) y
N2 H2A .89(3) y
N2 H2B .80(3) y
N3 N4 1.4203(17) y
N3 H3 .74(2) y
N4 H4A .82(2) y
N4 H4B .90(3) y
N4 H4C .92(3) y