#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/25/2012545.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_2012545 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] (P F6)1.29 (Cl O4)0.71' _chemical_formula_moiety 'C18 H24 Cu N12 2+ , 1.29P F6 - , 0.714Cl O4 -' _chemical_formula_sum 'C18 H24 Cl0.714 Cu F7.716 N12 O2.86 P1.29' _chemical_formula_weight 729.90 _chemical_name_systematic ; hexakis(pyrazole-N^2^)copper(II) hexafluorophosphate perchlorate ; _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 9.9950(10) _cell_length_b 9.9950(10) _cell_length_c 8.0520(10) _cell_measurement_reflns_used 4084 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.00 _cell_volume 696.63(13) _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 .997 _diffrn_measured_fraction_theta_max .997 _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 .030 _diffrn_reflns_av_sigmaI/netI .025 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 4132 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 2.35 _diffrn_standards_decay_% <1 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_T_max .685 _exptl_absorpt_correction_T_min .623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SCALEPACK; Otwinowski & Minor, 1997)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular block' _exptl_crystal_F_000 369 _exptl_crystal_size_max .4 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .4 _refine_diff_density_max .27 _refine_diff_density_min -.60 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 82 _refine_ls_number_reflns 1072 _refine_ls_number_restraints 93 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all .043 _refine_ls_R_factor_gt .037 _refine_ls_shift/su_max .002 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.3481P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .092 _refine_ls_wR_factor_ref .096 _reflns_number_gt 967 _reflns_number_total 1072 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bj1038.cif _cod_data_source_block II _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 2012545 _cod_database_fobs_code 2012545 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 .0288(2) Uani d SU 1 . . Cu N1 .1117(2) .1999(2) .1531(2) .0448(5) Uani d U 1 . . N N2 .2639(2) .3012(2) .1476(2) .0497(5) Uani d U 1 . . N H2 .3261 .3003 .0708 .060 Uiso calc R 1 . . H C1 .0626(3) .2429(3) .2872(3) .0507(6) Uani d U 1 . . C H1 -.0415 .1924 .3244 .061 Uiso calc R 1 . . H C2 .1822(3) .3694(3) .3641(3) .0522(6) Uani d U 1 . . C H2A .1772 .4218 .4602 .063 Uiso calc R 1 . . H C3 .3099(3) .4026(3) .2708(3) .0571(6) Uani d U 1 . . C H3 .4126 .4835 .2909 .068 Uiso calc R 1 . . H P .6667 .3333 .14457(13) .0431(3) Uani d SPDU .643(6) . 1 P F1 .6445(3) .1946(3) .0207(3) .0465(7) Uani d PDU .643(6) . 1 F F2 .5269(3) .2137(3) .2488(3) .0607(11) Uani d PDU .643(6) . 1 F Cl .6667 .3333 .14457(13) .0431(3) Uani d SPDU .357(6) . 2 Cl O1A .6667 .3333 .3225(15) .155(8) Uani d SPDU .357(6) . 2 O O2A .5774(18) .1831(12) .0960(18) .163(7) Uani d PDU .357(6) . 2 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 Cu .0298(2) .0298(2) .0267(3) .01492(11) .000 .000 N1 .0418(10) .0669(13) .0323(9) .0321(10) .0023(7) .0066(8) N2 .0516(11) .0537(12) .0432(11) .0259(10) .0129(9) .0099(9) C1 .0500(13) .0775(17) .0349(11) .0395(13) .0036(10) .0036(11) C2 .0694(16) .0581(14) .0421(13) .0417(13) .0029(11) .0073(11) C3 .0578(15) .0486(14) .0606(15) .0235(12) .0050(12) .0125(12) P .0365(3) .0365(3) .0562(6) .01827(17) .000 .000 F1 .0537(14) .0396(12) .0535(14) .0288(11) -.0050(10) -.0035(10) F2 .0558(16) .0590(16) .0611(18) .0242(12) .0230(12) .0222(12) Cl .0365(3) .0365(3) .0562(6) .01827(17) .000 .000 O1A .200(13) .200(13) .064(6) .100(7) .000 .000 O2A .160(12) .070(5) .167(13) -.011(7) -.085(12) -.016(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P .1023 .0942 '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' Cl Cl .1484 .1585 '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_ _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 . 4 180.0(12) yes N1 Cu N1 . 6 90.20(7) yes N1 Cu N1 4 6 89.80(7) no N1 Cu N1 . 3 89.80(7) yes N1 Cu N1 4 3 90.20(7) no N1 Cu N1 6 3 180.00(12) no N1 Cu N1 . 2 89.80(7) no N1 Cu N1 4 2 90.20(7) no N1 Cu N1 6 2 90.20(7) no N1 Cu N1 3 2 89.80(7) no N1 Cu N1 . 5 90.20(7) no N1 Cu N1 4 5 89.80(7) no N1 Cu N1 6 5 89.80(7) no N1 Cu N1 3 5 90.20(7) no N1 Cu N1 2 5 180.00(12) no N2 N1 C1 . . 104.1(2) no N2 N1 Cu . . 123.64(15) no C1 N1 Cu . . 131.48(18) no C3 N2 N1 . . 112.4(2) no C3 N2 H2 . . 123.8 no N1 N2 H2 . . 123.8 no N1 C1 C2 . . 111.5(2) no N1 C1 H1 . . 124.2 no C2 C1 H1 . . 124.2 no C3 C2 C1 . . 104.5(2) no C3 C2 H2A . . 127.7 no C1 C2 H2A . . 127.7 no N2 C3 C2 . . 107.4(2) no N2 C3 H3 . . 126.3 no C2 C3 H3 . . 126.3 no F2 P F2 3_665 . 93.57(15) no F2 P F2 3_665 2_655 93.57(15) no F2 P F2 . 2_655 93.57(15) no F2 P F1 3_665 . 174.93(16) no F2 P F1 . . 89.34(14) no F2 P F1 2_655 . 90.39(14) no F2 P F1 3_665 2_655 90.39(14) no F2 P F1 . 2_655 174.92(16) no F2 P F1 2_655 2_655 89.34(14) no F1 P F1 . 2_655 86.48(15) no F2 P F1 3_665 3_665 89.34(14) no F2 P F1 . 3_665 90.39(14) no F2 P F1 2_655 3_665 174.92(16) no F1 P F1 . 3_665 86.48(15) no F1 P F1 2_655 3_665 86.48(15) 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 2.128(2) ? Cu N1 . 2.128(2) yes Cu N1 6 2.128(2) ? Cu N1 3 2.128(2) ? Cu N1 4 2.128(2) ? Cu N1 2 2.128(2) ? N1 N2 . 1.342(3) no N1 C1 . 1.342(3) no N2 C3 . 1.326(3) no N2 H2 . .8800 no C1 C2 . 1.378(4) no C1 H1 . .9500 no C2 C3 . 1.371(4) no C2 H2A . .9500 no C3 H3 . .9500 no P F2 3_665 1.554(2) no P F2 . 1.554(2) no P F2 2_655 1.554(2) no P F1 . 1.631(3) no P F1 2_655 1.631(3) no P F1 3_665 1.631(3) 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 N2 6 -103.5(2) no N1 Cu N1 N2 3 76.5(2) no N1 Cu N1 N2 2 166.33(16) no N1 Cu N1 N2 5 -13.67(16) no N1 Cu N1 C1 6 88.62(17) no N1 Cu N1 C1 3 -91.38(17) no N1 Cu N1 C1 2 -1.6(2) no N1 Cu N1 C1 5 178.4(2) no C1 N1 N2 C3 . .2(3) no Cu N1 N2 C3 . -170.45(16) no N2 N1 C1 C2 . .2(3) no Cu N1 C1 C2 . 169.81(16) no N1 C1 C2 C3 . -.5(3) no N1 N2 C3 C2 . -.5(3) no C1 C2 C3 N2 . .6(3) no