#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2002963.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_2002963 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 '2(C1 H7 N4),F6 Si,2(H2 O)' _chemical_formula_sum 'C2 H18 F6 N8 O2 Si' _chemical_formula_weight 328.33 _chemical_name_systematic ; diaminoguanidinium hexafluorosilicate dihydrate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL-97 _cell_angle_alpha 70.723(2) _cell_angle_beta 82.745(2) _cell_angle_gamma 89.243(3) _cell_formula_units_Z 1 _cell_length_a 6.51240(10) _cell_length_b 6.6952(2) _cell_length_c 8.0215(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 47.5 _cell_measurement_theta_min 42.5 _cell_volume 327.348(17) _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type MACH3 _diffrn_measurement_method '\w - 2\q scans' _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 .0268 _diffrn_reflns_av_sigmaI/netI .0268 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 2404 _diffrn_reflns_theta_full 69.79 _diffrn_reflns_theta_max 69.79 _diffrn_reflns_theta_min 5.89 _diffrn_standards_decay_% 5 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.487 _exptl_absorpt_correction_T_max .61 _exptl_absorpt_correction_T_min .45 _exptl_absorpt_correction_type analytical _exptl_crystal_colour 'colorless, clear' _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_meas 1.670(10) _exptl_crystal_density_method pycnometry _exptl_crystal_description prismatic _exptl_crystal_F_000 170 _exptl_crystal_size_max .350 _exptl_crystal_size_mid .310 _exptl_crystal_size_min .170 _refine_diff_density_max .284 _refine_diff_density_min -.219 _refine_ls_extinction_coef .043(4) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 125 _refine_ls_number_reflns 1239 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all .0305 _refine_ls_R_factor_gt .0301 _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^)+(0.0295P)^2^+0.1278P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_ref .0745 _reflns_number_gt 1224 _reflns_number_total 1239 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file br0080.cif _[local]_cod_data_source_block hydrous _cod_original_cell_volume 327.348(16) _cod_database_code 2002963 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Si .0000 .0000 .0000 .0310(2) Uani d S 1 Si F1 .04859(14) -.01478(16) .20441(12) .0478(3) Uani d . 1 F F2 .12778(16) .23518(15) -.08741(14) .0543(3) Uani d . 1 F F3 -.22230(14) .12017(16) .03280(13) .0531(3) Uani d . 1 F C .4773(2) .2381(2) .5241(2) .0344(3) Uani d . 1 C N1 .5514(2) .1627(2) .67681(19) .0442(3) Uani d . 1 N H1A .465(3) .116(3) .777(3) .046(5) Uiso d . 1 H H1B .671(3) .151(3) .679(2) .037(5) Uiso d . 1 H N2 .2754(2) .2442(3) .5163(2) .0461(4) Uani d . 1 N H2A .182(3) .193(3) .610(3) .054(5) Uiso d . 1 H H2B .235(3) .294(3) .417(3) .045(5) Uiso d . 1 H N3 .6031(2) .3118(2) .37175(19) .0408(3) Uani d . 1 N H3 .552(3) .357(3) .277(3) .044(5) Uiso d . 1 H N4 .8184(2) .3098(2) .3732(2) .0430(3) Uani d . 1 N H4A .867(3) .443(4) .314(3) .058(6) Uiso d . 1 H H4B .862(3) .227(4) .317(3) .059(6) Uiso d . 1 H O .7298(2) .5611(3) .86215(19) .0541(4) Uani d . 1 O H1W .749(4) .442(5) .912(4) .077(8) Uiso d . 1 H H2W .769(4) .622(4) .919(4) .081(9) 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 .0282(3) .0355(3) .0253(3) .0007(2) .00041(19) -.0063(2) F1 .0444(5) .0667(6) .0305(5) -.0002(4) -.0050(4) -.0136(4) F2 .0635(7) .0458(6) .0461(6) -.0167(5) .0049(5) -.0090(4) F3 .0410(5) .0629(6) .0488(6) .0166(4) .0012(4) -.0129(5) C .0333(7) .0319(7) .0361(8) .0001(5) .0005(6) -.0105(6) N1 .0344(8) .0562(8) .0351(8) .0029(6) -.0005(6) -.0075(6) N2 .0320(7) .0609(9) .0390(8) -.0019(6) -.0001(6) -.0094(7) N3 .0331(7) .0508(8) .0334(7) -.0020(5) -.0004(5) -.0083(6) N4 .0313(7) .0450(8) .0484(8) -.0014(6) .0042(6) -.0130(7) O .0634(8) .0494(8) .0497(8) .0016(6) -.0169(6) -.0131(6) 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' O O .0492 .0322 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag F1 Si F1 . 2 180.0 n F1 Si F2 . . 90.35(5) y F1 Si F2 2 . 89.65(5) n F1 Si F2 . 2 89.65(5) n F1 Si F2 2 2 90.35(5) n F2 Si F2 . 2 180.0 n F1 Si F3 . 2 90.74(5) n F1 Si F3 2 2 89.26(5) n F2 Si F3 . 2 89.24(5) n F2 Si F3 2 2 90.76(5) n F1 Si F3 . . 89.26(5) y F1 Si F3 2 . 90.74(5) n F2 Si F3 . . 90.76(5) y F2 Si F3 2 . 89.24(5) n F3 Si F3 2 . 180.0 n N1 C N2 . . 121.27(15) y N1 C N3 . . 120.98(14) y N2 C N3 . . 117.75(15) y C N1 H1A . . 119.6(12) y C N1 H1B . . 120.4(13) y H1A N1 H1B . . 119.8(19) y C N2 H2A . . 123.3(14) y C N2 H2B . . 118.3(14) y H2A N2 H2B . . 118.3(19) y C N3 N4 . . 119.85(14) y C N3 H3 . . 119.0(13) y N4 N3 H3 . . 121.1(13) y N3 N4 H4A . . 106.8(13) y N3 N4 H4B . . 105.1(15) y H4A N4 H4B . . 111(2) y H1W O H2W . . 105(3) y 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 Si F1 . 1.6797(9) y Si F1 2 1.6797(9) n Si F2 . 1.6798(9) y Si F2 2 1.6798(9) n Si F3 2 1.6808(9) n Si F3 . 1.6808(9) y C N1 . 1.313(2) y C N2 . 1.324(2) y C N3 . 1.329(2) y N1 H1A . .89(2) y N1 H1B . .781(19) y N2 H2A . .88(2) y N2 H2B . .83(2) y N3 N4 . 1.4037(19) y N3 H3 . .83(2) y N4 H4A . .90(2) y N4 H4B . .85(2) y O H1W . .78(3) y O H2W . .77(3) y