#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/37/2013761.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_2013761 loop_ _publ_author_name 'C.R. Ross II' 'M. R. Bauer' 'R. M. Nielson' '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_moiety '(C H7 N4)2, F6 Zr' _chemical_formula_sum 'C2 H14 F6 N8 Zr' _chemical_formula_weight 355.43 _chemical_name_systematic ; ? ; _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 _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 99.629(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.3709(3) _cell_length_b 6.3296(3) _cell_length_c 14.5646(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.769 _cell_measurement_theta_min 19.931 _cell_volume 579.05(5) _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., 1994)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0264 _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 3555 _diffrn_reflns_theta_full 29.98 _diffrn_reflns_theta_max 29.98 _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 0.815 _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details 'North et al., 1968' _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 0.590 _exptl_crystal_size_mid 0.370 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.555 _refine_diff_density_min -0.456 _refine_ls_extinction_coef 0.0209(17) _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 1.097 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 81 _refine_ls_number_reflns 1681 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0187 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+0.0641P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0529 _reflns_number_gt 1503 _reflns_number_total 1681 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file fg1714.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 2013761 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Zr 0.0000 0.0000 0.0000 0.02124(7) Uani d S 1 . . Zr F1 0.15005(16) -0.01696(11) 0.13172(7) 0.0367(2) Uani d . 1 . . F F2 -0.11519(11) 0.28480(11) 0.02762(5) 0.03881(17) Uani d . 1 . . F F3 0.25212(11) 0.13923(13) -0.04047(5) 0.04346(19) Uani d . 1 . . F N1 0.0597(2) 0.47446(19) 0.20912(10) 0.0395(3) Uani d . 1 . . N H1A 0.0102 0.4711 0.2605 0.043(2) Uiso calc R 1 . . H H1B -0.0260 0.4799 0.1569 0.043 Uiso calc R 1 . . H N2 0.4039(2) 0.4630(2) 0.28952(9) 0.0373(2) Uani d . 1 . . N H2A 0.3571 0.4595 0.3416 0.043 Uiso calc R 1 . . H H2B 0.5387 0.4610 0.2891 0.043 Uiso calc R 1 . . H N3 0.3382(2) 0.48007(16) 0.12922(10) 0.0327(2) Uani d . 1 . . N H3 0.2492 0.4949 0.0783 0.048(7) Uiso calc R 1 . . H N4 0.5559(2) 0.4651(2) 0.12695(10) 0.0384(3) Uani d . 1 . . N H4A 0.5993 0.5816 0.1014 0.055(4) Uiso calc R 1 . . H H4B 0.5804 0.3532 0.0933 0.055 Uiso calc R 1 . . H C 0.2690(2) 0.47126(17) 0.21042(9) 0.0268(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 0.01877(10) 0.02983(10) 0.01602(10) 0.00160(3) 0.00552(6) 0.00139(3) F1 0.0332(4) 0.0542(5) 0.0212(4) 0.0034(2) 0.0002(3) 0.0023(2) F2 0.0426(4) 0.0402(4) 0.0327(3) 0.0125(3) 0.0035(3) -0.0045(3) F3 0.0353(3) 0.0614(5) 0.0373(4) -0.0141(3) 0.0164(3) -0.0005(3) N1 0.0258(5) 0.0613(7) 0.0327(6) -0.0004(4) 0.0090(5) -0.0043(4) N2 0.0286(5) 0.0578(6) 0.0259(5) -0.0001(4) 0.0057(4) 0.0032(4) N3 0.0278(5) 0.0473(6) 0.0241(5) 0.0038(3) 0.0071(4) 0.0022(3) N4 0.0298(5) 0.0498(6) 0.0389(6) 0.0024(4) 0.0155(5) 0.0050(5) C 0.0259(5) 0.0283(4) 0.0273(6) 0.0006(4) 0.0074(4) -0.0012(4) 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 1.9980(10) no Zr F1 . 1.9980(10) no Zr F3 3 2.0052(6) no Zr F3 . 2.0052(6) no Zr F2 3 2.0121(7) n Zr F2 . 2.0121(7) no N1 C . 1.3304(17) no N1 H1A . 0.8600 no N1 H1B . 0.8600 n N2 C . 1.3181(18) n N2 H2A . 0.8600 no N2 H2B . 0.8600 n N3 C . 1.3307(18) no N3 N4 . 1.3961(16) n N3 H3 . 0.8600 no N4 H4A . 0.8900 no N4 H4B . 0.8900 no 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 F1 3 . 180.00(7) no F1 Zr F3 3 3 91.59(4) no F1 Zr F3 . 3 88.41(4) no F1 Zr F3 3 . 88.41(4) no F1 Zr F3 . . 91.59(4) n F3 Zr F3 3 . 180.00(6) n F1 Zr F2 3 3 89.32(3) n F1 Zr F2 . 3 90.68(3) no F3 Zr F2 3 3 90.11(3) no F3 Zr F2 . 3 89.89(3) no F1 Zr F2 3 . 90.68(3) n F1 Zr F2 . . 89.32(3) no F3 Zr F2 3 . 89.89(3) no F3 Zr F2 . . 90.11(3) n F2 Zr F2 3 . 180.00(5) no C N1 H1A . . 120.0 n C N1 H1B . . 120.0 no H1A N1 H1B . . 120.0 n C N2 H2A . . 120.0 no C N2 H2B . . 120.0 no H2A N2 H2B . . 120.0 no C N3 N4 . . 119.77(12) no 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 N2 C N1 . . 121.22(13) n N2 C N3 . . 120.93(12) n N1 C N3 . . 117.85(13) n _cod_database_fobs_code 2013761