#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$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/ # # All data on this site have been placed in the public domain by the # contributors. # data_2002952 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1998 _journal_volume B54 _journal_page_first 417 _journal_page_last 423 _publ_section_title ; Test of tabular results ; loop_ _publ_author_name 'Ross II, C. R.' 'Paulsen, B. L.' 'Nielson, R. M.' 'Abrahams, S. C.' _chemical_name_common 'Aminoguanidinium hexafluorozirconate hydrate' _chemical_formula_moiety 'CN4H8 ZrF6 H2O' _chemical_formula_sum 'C H10 F6 N4 O Zr' _chemical_formula_weight 299.33 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' 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' _cell_length_a 12.3770(7) _cell_length_b 9.7522(6) _cell_length_c 13.8543(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.326(6) _cell_angle_gamma 90.00 _cell_volume 1658.60(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 14 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 12.5 _cell_measurement_temperature 295(2) _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max .36 _exptl_crystal_size_mid .36 _exptl_crystal_size_min .30 _exptl_crystal_density_diffrn 2.397 _exptl_crystal_density_meas 2.31(4) _exptl_crystal_density_method 'pycnometry at 295K' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.402 _exptl_absorpt_correction_T_min .422 _exptl_absorpt_correction_T_max .473 _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method \q-2\q _diffrn_reflns_number 4811 _diffrn_reflns_av_R_equivalents .0220 _diffrn_reflns_av_sigmaI/netI .0331 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 5 _reflns_number_total 3798 _reflns_number_observed 3434 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all .0337 _refine_ls_R_factor_obs .0299 _refine_ls_wR_factor_all .0870 _refine_ls_wR_factor_obs .0842 _refine_ls_goodness_of_fit_all 1.119 _refine_ls_goodness_of_fit_obs 1.143 _refine_ls_restrained_S_all 1.119 _refine_ls_restrained_S_obs 1.143 _refine_ls_number_reflns 3798 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _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_shift/esd_max .005 _refine_ls_shift/esd_mean .000 _refine_diff_density_max .744 _refine_diff_density_min -.692 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 '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' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 .5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_disorder_group _atom_site_type_symbol Zr1 .81610(2) .11839(2) .50967(2) .01500(9) Uani d . 1 . Zr Zr2 1.00976(2) .12107(2) .33245(2) .01572(9) Uani d . 1 . Zr F1 .69060(13) -.0125(2) .44744(13) .0253(4) Uani d . 1 . F F2 .7249(2) .2399(2) .41729(15) .0357(4) Uani d . 1 . F F3 .82696(14) .3029(2) .58486(14) .0314(4) Uani d . 1 . F F4 .9453(2) .0933(2) .63250(14) .0297(4) Uani d . 1 . F F5 .8612(2) -.0943(2) .54993(13) .0288(4) Uani d . 1 . F F6 .71618(15) .0937(2) .61477(13) .0297(4) Uani d . 1 . F F7 .87391(15) .0252(2) .38562(13) .0303(4) Uani d . 1 . F F8 .95740(14) .2174(2) .46324(12) .0277(4) Uani d . 1 . F F9 1.13241(15) .0878(2) .25012(13) .0321(4) Uani d . 1 . F F10 .93397(14) .0228(2) .21130(12) .0273(4) Uani d . 1 . F F11 .89490(15) .2570(2) .26995(13) .0300(4) Uani d . 1 . F F12 1.09076(14) .3069(2) .33685(15) .0315(4) Uani d . 1 . F C1A .8714(2) .5836(3) .3628(2) .0243(6) Uani d . 1 . C N1A .7975(2) .4940(3) .3275(2) .0311(6) Uani d . 1 . N H1AA .8170(2) .4135(3) .3113(2) .037 Uiso calc R 1 . H H1AB .7297(2) .5159(3) .3207(2) .037 Uiso calc R 1 . H N2A .9760(2) .5534(3) .3741(2) .0355(6) Uani d . 1 . N H2AA .9973(2) .4734(3) .3583(2) .043 Uiso calc R 1 . H H2AB 1.0231(2) .6136(3) .3973(2) .043 Uiso calc R 1 . H N3A .8421(2) .7123(3) .3859(2) .0321(6) Uani d . 1 . N H3AA .8888(2) .7781(3) .3911(2) .038 Uiso calc R 1 . H N4A .7329(2) .7355(3) .4014(2) .0280(5) Uani d . 1 . N H1NA .7263(2) .8177(3) .4222(2) .042 Uiso calc R 1 . H H2NA .7151(2) .6782(3) .4439(2) .042 Uiso calc R 1 . H H3NA .6908(2) .7245(3) .3476(2) .042 Uiso calc R 1 . H C1B .4462(2) .1623(3) .3476(2) .0249(6) Uani d . 1 . C N1B .5157(2) .2566(3) .3275(2) .0331(6) Uani d . 1 . N H1BA .5846(2) .2417(3) .3398(2) .040 Uiso calc R 1 . H H1BB .4924(2) .3332(3) .3020(2) .040 Uiso calc R 1 . H N2B .4791(2) .0457(3) .3861(3) .0441(8) Uani d . 1 . N H2BA .5477(2) .0291(3) .3989(3) .053 Uiso calc R 1 . H H2BB .4324(2) -.0148(3) .3988(3) .053 Uiso calc R 1 . H N3B .3383(2) .1831(3) .3315(2) .0379(7) Uani d . 1 . N H3BA .2957(2) .1219(3) .3507(2) .045 Uiso calc R 1 . H N4B .2927(2) .2993(3) .2851(2) .0381(7) Uani d . 1 . N H1NB .2232(2) .2976(3) .2849(2) .057 Uiso calc R 1 . H H2NB .3076(2) .3012(3) .2261(2) .057 Uiso calc R 1 . H H3NB .3189(2) .3712(3) .3154(2) .057 Uiso calc R 1 . H O1W1 .6907(3) .5284(4) .5399(3) .0419(9) Uani d P .80 . O O2W1 .7439(15) .5543(18) .5504(13) .044(4) Uani d P .20 . O O1W2 .5191(4) .3162(5) .5584(4) .0723(12) Uiso d P .80 . O O2W2 .5003(17) .390(2) .5397(14) .068(5) Uiso d P .20 . O 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 .01204(14) .01414(14) .01882(14) .00051(8) .00198(10) -.00126(8) Zr2 .01553(14) .01659(14) .01496(14) .00180(8) .00162(10) .00037(8) F1 .0156(7) .0213(8) .0374(9) .0004(6) -.0028(7) -.0053(7) F2 .0283(9) .0278(9) .0469(11) .0033(8) -.0110(8) .0093(8) F3 .0275(9) .0218(8) .0456(11) -.0009(7) .0074(8) -.0115(8) F4 .0301(9) .0196(8) .0351(9) -.0014(7) -.0123(8) .0005(7) F5 .0329(10) .0195(8) .0299(9) .0035(7) -.0123(7) -.0035(7) F6 .0264(9) .0338(9) .0313(9) -.0089(7) .0129(7) -.0087(8) F7 .0330(9) .0286(9) .0321(9) -.0110(8) .0153(8) -.0119(7) F8 .0260(8) .0337(9) .0248(8) -.0121(7) .0091(7) -.0104(7) F9 .0269(9) .0440(11) .0271(9) -.0005(8) .0099(7) -.0032(8) F10 .0284(9) .0282(9) .0237(8) .0017(7) -.0028(7) -.0064(7) F11 .0326(9) .0276(9) .0272(9) .0127(7) -.0055(7) -.0009(7) F12 .0276(9) .0210(8) .0471(11) -.0018(7) .0096(8) .0035(8) C1A .0246(14) .0200(13) .0279(14) -.0008(11) .0013(11) -.0027(11) N1A .0236(12) .0185(12) .050(2) -.0006(10) .0010(11) -.0119(11) N2A .0243(13) .0249(13) .056(2) -.0005(11) .0001(12) -.0077(12) N3A .0251(13) .0190(12) .050(2) -.0025(10) -.0020(11) -.0117(11) N4A .0317(14) .0216(12) .0289(13) .0056(10) -.0030(10) -.0073(10) C1B .0211(13) .0271(14) .0263(13) -.0039(12) .0028(10) .0051(12) N1B .0225(12) .0325(14) .043(2) -.0072(11) .0011(11) .0141(12) N2B .0184(12) .036(2) .077(2) .0000(11) .0039(13) .029(2) N3B .0198(12) .0332(15) .059(2) -.0016(11) .0002(12) .0231(14) N4B .0220(12) .041(2) .049(2) .0008(12) -.0036(12) .0216(14) O1W1 .044(2) .037(2) .046(2) .004(2) .010(2) .007(2) O2W1 .055(10) .035(8) .044(8) .003(8) .011(9) .004(6)