#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/25/2012544.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_2012544 loop_ _publ_author_name 'Otieno, Tom' 'Blanton, Jaime R.' 'Hatfield, M. Jason' 'Asher, Sherry L.' 'Parkin, Sean' _publ_section_title ; A copper(II)--pyrazole complex cation with f̱ \/overline 3 imposed symmetry ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m182 _journal_page_last m185 _journal_paper_doi 10.1107/S010827010200152X _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Cu (C3 H4 N2)6] (As F6)2' _chemical_formula_moiety 'C18 H24 Cu N12 2+ , 2As F6 -' _chemical_formula_sum 'C18 H24 As2 Cu F12 N12' _chemical_formula_weight 849.87 _chemical_name_systematic ; hexakis(pyrazole-N^2^)copper(II) bis(hexafluoroarsenate) ; _space_group_IT_number 147 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-P 3' _symmetry_space_group_name_H-M 'P -3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 1 _cell_length_a 10.1780(14) _cell_length_b 10.1780(14) _cell_length_c 8.0980(16) _cell_measurement_reflns_used 3793 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.00 _cell_volume 726.5(2) _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'XP in SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL97 and local procedures' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 18 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .032 _diffrn_reflns_av_sigmaI/netI .026 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 4497 _diffrn_reflns_theta_full 27.42 _diffrn_reflns_theta_max 27.42 _diffrn_reflns_theta_min 2.31 _diffrn_standards_decay_% <1 _exptl_absorpt_coefficient_mu 3.124 _exptl_absorpt_correction_T_max .458 _exptl_absorpt_correction_T_min .409 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SCALEPACK; Otwinowski & Minor, 1997)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular block' _exptl_crystal_F_000 419 _exptl_crystal_size_max .30 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .25 _refine_diff_density_max .973 _refine_diff_density_min -.770 _refine_ls_extinction_coef .011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 70 _refine_ls_number_reflns 1107 _refine_ls_number_restraints 16 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all .045 _refine_ls_R_factor_gt .036 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.9805P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .093 _refine_ls_wR_factor_ref .097 _reflns_number_gt 949 _reflns_number_total 1107 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bj1038.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 2012544 _cod_database_fobs_code 2012544 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu .0000 .0000 .0000 .0203(2) Uani d SU 1 . . Cu N1 .1098(3) -.0880(3) -.1530(3) .0352(6) Uani d U 1 . . N N2 .2597(3) -.0385(3) -.1463(3) .0367(6) Uani d U 1 . . N H2 .3207 .0230 -.0697 .044 Uiso calc R 1 . . H C1 .0610(4) -.1772(4) -.2872(4) .0387(8) Uani d U 1 . . C H1 -.0410 -.2288 -.3250 .046 Uiso calc R 1 . . H C2 .1794(4) -.1839(4) -.3632(4) .0421(8) Uani d U 1 . . C H2A .1749 -.2392 -.4597 .050 Uiso calc R 1 . . H C3 .3045(4) -.0935(4) -.2690(5) .0439(8) Uani d U 1 . . C H3 .4049 -.0737 -.2880 .053 Uiso calc R 1 . . H As .3333 -.3333 .13772(7) .0308(2) Uani d SU 1 . . As F1 .4574(2) -.1859(2) .0146(3) .0418(5) Uani d U 1 . . F F2 .3121(3) -.2072(3) .2582(3) .0570(6) Uani d U 1 . . F 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 Cu .0205(3) .0205(3) .0200(4) .01023(15) .000 .000 N1 .0308(14) .0333(14) .0251(13) .0039(12) -.0046(11) .0027(10) N2 .0352(15) .0352(15) .0332(14) .0125(12) -.0095(12) .0017(12) C1 .0362(17) .0383(18) .0283(15) .0088(15) -.0050(14) .0007(13) C2 .053(2) .0390(19) .0308(16) .0209(17) -.0041(15) .0044(14) C3 .0411(19) .043(2) .046(2) .0195(16) -.0022(16) .0108(16) As .0282(2) .0282(2) .0360(3) .01409(12) .000 .000 F1 .0345(10) .0319(10) .0525(11) .0118(8) -.0008(9) .0040(9) F2 .0624(15) .0530(14) .0601(14) .0321(12) .0024(12) -.0180(11) 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' Cu Cu .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As .0499 2.0058 '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 N1 Cu N1 5 . 90.11(10) no N1 Cu N1 5 6 89.89(10) no N1 Cu N1 . 6 90.11(10) yes N1 Cu N1 5 3 90.11(10) no N1 Cu N1 . 3 89.89(10) yes N1 Cu N1 6 3 180.0 no N1 Cu N1 5 4 89.89(10) no N1 Cu N1 . 4 180.00(11) yes N1 Cu N1 6 4 89.89(10) no N1 Cu N1 3 4 90.11(10) no N1 Cu N1 5 2 180.0 no N1 Cu N1 . 2 89.89(10) no N1 Cu N1 6 2 90.11(10) no N1 Cu N1 3 2 89.89(10) no N1 Cu N1 4 2 90.11(10) no C1 N1 N2 . . 104.6(3) no C1 N1 Cu . . 131.1(2) no N2 N1 Cu . . 123.4(2) no C3 N2 N1 . . 112.1(3) no C3 N2 H2 . . 124.0 no N1 N2 H2 . . 124.0 no N1 C1 C2 . . 110.9(3) no N1 C1 H1 . . 124.5 no C2 C1 H1 . . 124.5 no C3 C2 C1 . . 105.0(3) no C3 C2 H2A . . 127.5 no C1 C2 H2A . . 127.5 no N2 C3 C2 . . 107.5(3) no N2 C3 H3 . . 126.3 no C2 C3 H3 . . 126.3 no F2 As F2 2_545 3_655 90.68(12) no F2 As F2 2_545 . 90.68(12) no F2 As F2 3_655 . 90.68(12) no F2 As F1 2_545 2_545 89.38(11) no F2 As F1 3_655 2_545 179.01(10) no F2 As F1 . 2_545 90.31(11) no F2 As F1 2_545 3_655 90.31(11) no F2 As F1 3_655 3_655 89.38(11) no F2 As F1 . 3_655 179.01(10) no F1 As F1 2_545 3_655 89.63(10) no F2 As F1 2_545 . 179.01(10) no F2 As F1 3_655 . 90.31(11) no F2 As F1 . . 89.38(11) no F1 As F1 2_545 . 89.63(10) no F1 As F1 3_655 . 89.63(10) no 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 Cu N1 5 2.142(3) no Cu N1 . 2.142(3) yes Cu N1 6 2.142(3) no Cu N1 3 2.142(3) no Cu N1 4 2.142(3) no Cu N1 2 2.142(3) no N1 C1 . 1.342(4) no N1 N2 . 1.347(4) no N2 C3 . 1.328(5) no N2 H2 . .8800 no C1 C2 . 1.385(5) no C1 H1 . .9500 no C2 C3 . 1.371(5) no C2 H2A . .9500 no C3 H3 . .9500 no As F2 2_545 1.709(2) no As F2 3_655 1.709(2) no As F2 . 1.710(2) no As F1 2_545 1.716(2) no As F1 3_655 1.716(2) no As F1 . 1.716(2) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag N1 Cu N1 C1 5 89.4(2) no N1 Cu N1 C1 6 179.3(3) no N1 Cu N1 C1 3 -.7(3) no N1 Cu N1 C1 2 -90.6(2) no N1 Cu N1 N2 5 -103.2(3) no N1 Cu N1 N2 6 -13.3(2) no N1 Cu N1 N2 3 166.7(2) no N1 Cu N1 N2 2 76.8(3) no C1 N1 N2 C3 . -.3(4) no Cu N1 N2 C3 . -170.5(2) no N2 N1 C1 C2 . .3(4) no Cu N1 C1 C2 . 169.5(2) no N1 C1 C2 C3 . -.2(4) no N1 N2 C3 C2 . .2(4) no C1 C2 C3 N2 . .0(4) no