#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2013762.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_2013762 loop_ _publ_author_name 'Ross II, C. R.' 'Bauer, M. R.' 'Nielson, R. M.' 'Abrahams, S. C.' _publ_section_title ; Bis[aminoguanidinium(1+)] hexafluorozirconate(IV): redeterminations and normal probability analysis ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m24 _journal_page_last m26 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '(C H7 N4)2 [Zr F6]' _chemical_formula_moiety '(C H7 N4)2, F6 Zr' _chemical_formula_sum 'C2 H14 F6 N8 Zr' _chemical_formula_weight 355.43 _chemical_name_systematic ; aminoguanidinium(1+) hexafluorozirconate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 99.606(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.3705(4) _cell_length_b 6.3288(9) _cell_length_c 14.5630(8) _cell_measurement_reflns_used 25 _cell_measurement_temperature 283(2) _cell_measurement_theta_max 28.5 _cell_measurement_theta_min 24.5 _cell_volume 578.91(10) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf--Nonius, 1989)' _computing_data_reduction 'maxus (Mackay et al., 1999)' _computing_molecular_graphics 'OrtepII (Johnson, 1976)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _diffrn_ambient_temperature 283(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 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 3540 _diffrn_reflns_theta_full 29.93 _diffrn_reflns_theta_max 29.93 _diffrn_reflns_theta_min 2.84 _diffrn_standards_decay_% 1 _diffrn_standards_interval_time 60 _diffrn_standards_number 5 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_T_max .815 _exptl_absorpt_correction_T_min .619 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details face-indexed _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_description blocky _exptl_crystal_F_000 352 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.365 _refine_diff_density_min -0.581 _refine_ls_extinction_coef 0.032(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 81 _refine_ls_number_reflns 1674 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.134 _refine_ls_R_factor_all 0.0209 _refine_ls_R_factor_gt 0.0186 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+0.0859P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.0492 _reflns_number_gt 1508 _reflns_number_total 1674 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file fg1714.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M P21/c _cod_database_code 2013762 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, 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_refinement_flags _atom_site_occupancy _atom_site_type_symbol Zr 0.0000 0.0000 0.0000 0.02129(7) Uani d S 1 Zr F1 0.14989(15) -0.01698(11) 0.13163(6) 0.03687(19) Uani d . 1 F F2 -0.11520(12) 0.28481(12) 0.02761(5) 0.03881(17) Uani d . 1 F F3 0.25215(12) 0.13928(14) -0.04050(5) 0.04374(19) Uani d . 1 F N1 0.0601(2) 0.47438(19) 0.20925(10) 0.0393(3) Uani d . 1 N H1A 0.0106 0.4707 0.2607 0.046(2) Uiso calc R 1 H H1B -0.0257 0.4801 0.1570 0.046 Uiso calc R 1 H N2 0.4038(2) 0.4626(2) 0.28934(9) 0.0378(2) Uani d . 1 N H2A 0.3572 0.4588 0.3414 0.046 Uiso calc R 1 H H2B 0.5386 0.4607 0.2888 0.046 Uiso calc R 1 H N3 0.3381(2) 0.47995(16) 0.12923(9) 0.0331(2) Uani d . 1 N H3 0.2490 0.4947 0.0784 0.046(6) Uiso calc R 1 H N4 0.55588(19) 0.4650(2) 0.12684(10) 0.0387(3) Uani d . 1 N H4A 0.5984 0.5795 0.0996 0.060(4) Uiso calc R 1 H H4B 0.5808 0.3507 0.0947 0.060 Uiso calc R 1 H C 0.2689(2) 0.47129(17) 0.21047(9) 0.0269(2) Uani d . 1 C 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 Zr 0.01849(9) 0.02981(10) 0.01669(9) 0.00162(4) 0.00615(6) 0.00139(4) F1 0.0334(4) 0.0542(5) 0.0219(4) 0.0031(3) 0.0011(3) 0.0023(2) F2 0.0420(4) 0.0397(4) 0.0340(3) 0.0126(3) 0.0044(3) -0.0044(3) F3 0.0352(4) 0.0617(5) 0.0383(4) -0.0147(3) 0.0176(3) -0.0007(3) N1 0.0249(5) 0.0618(7) 0.0330(6) -0.0001(4) 0.0095(4) -0.0041(4) N2 0.0291(5) 0.0586(6) 0.0261(5) -0.0006(4) 0.0059(4) 0.0031(4) N3 0.0274(5) 0.0481(6) 0.0247(5) 0.0035(3) 0.0072(4) 0.0021(3) N4 0.0300(5) 0.0498(6) 0.0401(6) 0.0026(4) 0.0165(5) 0.0046(5) C 0.0262(5) 0.0285(4) 0.0272(6) 0.0005(4) 0.0081(4) -0.0012(4) 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' Zr Zr -2.9673 0.5597 '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' 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 Zr F2 . . 89.33(3) y F1 Zr F3 . . 91.59(4) y F2 Zr F3 . . 90.10(3) y F1 Zr F1 3 . 180 n F1 Zr F3 3 3 91.59(4) n F1 Zr F3 . 3 88.41(4) n F1 Zr F3 3 . 88.41(4) n F3 Zr F3 3 . 180 n F1 Zr F2 3 3 89.33(3) n F1 Zr F2 . 3 90.67(3) n F3 Zr F2 3 3 90.10(3) n F3 Zr F2 . 3 89.90(3) n F1 Zr F2 3 . 90.67(3) n F3 Zr F2 3 . 89.90(3) no F2 Zr F2 3 . 180 n C N1 H1A . . 120.0 no C N1 H1B . . 120.0 n H1A N1 H1B . . 120.0 no C N2 H2A . . 120.0 n C N2 H2B . . 120.0 no H2A N2 H2B . . 120.0 no C N3 N4 . . 119.81(12) y C N3 H3 . . 120.1 no N4 N3 H3 . . 120.1 no N3 N4 H4A . . 109.5 no N3 N4 H4B . . 109.5 no H4A N4 H4B . . 109.5 no N1 C N2 . . 121.27(13) y N1 C N3 . . 117.86(13) y N2 C N3 . . 120.86(12) 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 Zr F1 3 1.9967(9) n Zr F1 . 1.9967(9) y Zr F2 3 2.0119(7) no Zr F2 . 2.0119(7) y Zr F3 3 2.0053(7) no Zr F3 . 2.0053(7) y N1 C . 1.3279(17) y N1 H1A . 0.86 n N1 H1B . 0.86 no N2 C . 1.3158(17) y N2 H2A . 0.86 no N2 H2B . 0.86 no N3 C . 1.3307(17) y N3 N4 . 1.3968(16) y N3 H3 . 0.86 no N4 H4A . 0.89 no N4 H4B . 0.89 no