#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200833.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_2200833 loop_ _publ_author_name 'Yang, Yang-Yi' 'Chen, Xiao-Ming' 'Ng, Seik Weng' _publ_section_title ; Tetrakis(trimethylammonioacetato-O)copper(II) bis(hexafluorophosphate) ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m61 _journal_page_last m62 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Cu (C5 H11 N O2)4] (P F6)2' _chemical_formula_moiety 'C5 H11 Cu1 N O2 2+, 2F6 P 1-' _chemical_formula_sum 'C20 H44 Cu F12 N4 O8 P2' _chemical_formula_weight 822.07 _chemical_name_systematic ; Tetrakis(trimethylammonioacetato-O)copper(II) bis(hexafluorophosphate) ; _space_group_IT_number 121 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4 2' _symmetry_space_group_name_H-M 'I -4 2 m' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 11.831(6) _cell_length_b 11.831(6) _cell_length_c 11.760(8) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 7 _cell_volume 1646.1(16) _computing_cell_refinement 'R3m Software' _computing_data_collection 'R3m Software (Siemens, 1990)' _computing_data_reduction 'R3m Software' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Siemens R3m four-circle' _diffrn_measurement_method \w _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 .0284 _diffrn_reflns_av_sigmaI/netI .0258 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 1035 _diffrn_reflns_theta_full 25.99 _diffrn_reflns_theta_max 25.99 _diffrn_reflns_theta_min 2.43 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 150 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu .876 _exptl_absorpt_correction_T_max .742 _exptl_absorpt_correction_T_min .657 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '\y scan (North et al., 1968)' _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Polyhedron _exptl_crystal_F_000 846 _exptl_crystal_size_max .50 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .30 _refine_diff_density_max .274 _refine_diff_density_min -.347 _refine_ls_abs_structure_details 'Flack & Schwarzenbach (1988)' _refine_ls_abs_structure_Flack -.01(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 89 _refine_ls_number_reflns 544 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all .0297 _refine_ls_R_factor_gt .0270 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0480P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .0689 _refine_ls_wR_factor_ref .0706 _reflns_number_gt 514 _reflns_number_total 544 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6104.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1646(2) _cod_database_code 2200833 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x, y, -z' 'x, -y, -z' '-y, -x, z' 'y, x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+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 Cu1 .0000 .0000 .0000 .0213(2) Uani d S 1 Cu P1 .0000 .5000 .0000 .0260(3) Uani d S 1 P F1 .0000 .5000 -.1330(2) .0690(10) Uani d S 1 F F2 .1359(2) .5000 .0000 .0480(10) Uani d S 1 F F3 .0000 .3670(2) .0000 .0660(10) Uani d S 1 F O1 .11660(10) .11660(10) -.0013(5) .0300(10) Uani d S 1 O O2 .1128(2) .1128(2) .1884(3) .0470(10) Uani d S 1 O N1 .2871(2) .2871(2) .1964(3) .0290(10) Uani d S 1 N C1 .1481(3) .1481(3) .0977(4) .0280(10) Uani d S 1 C C2 .2393(3) .2393(3) .0885(4) .0280(10) Uani d S 1 C C3 .1984(4) .3448(4) .2654(4) .0470(10) Uani d D 1 C C4 .3734(3) .3734(3) .1641(6) .052(2) Uani d SD 1 C H2 .303(3) .203(3) .051(3) .040(10) Uiso d . 1 H H3a .153(4) .284(3) .290(4) .06(2) Uiso d D 1 H H3b .232(3) .378(3) .330(2) .040(10) Uiso d D 1 H H3c .161(3) .401(3) .223(3) .040(10) Uiso d D 1 H H4a .426(4) .340(4) .106(4) .10(2) Uiso d D 1 H H4b .402(3) .402(3) .240(3) .020(10) Uiso d SD 1 H 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 Cu1 .0200(3) .0200(3) .0238(5) .000 .000 .000 P1 .0273(6) .0247(6) .0260(7) .000 .000 .000 F1 .068(2) .110(3) .0280(10) .000(4) .000 .000 F2 .0280(10) .0470(10) .070(2) .000 .000 .012(3) F3 .051(2) .0260(10) .120(3) .000 .012(3) .000 O1 .0290(10) .0290(10) .0320(10) -.0050(10) -.005(2) -.005(2) O2 .051(2) .051(2) .039(2) -.017(2) .0070(10) .0070(10) N1 .0290(10) .0290(10) .030(2) .000(2) -.0070(10) -.0070(10) C1 .0220(10) .0220(10) .040(3) .002(2) -.0010(10) -.0010(10) C2 .0280(10) .0280(10) .028(2) -.001(2) -.0050(10) -.0050(10) C3 .050(3) .048(2) .042(2) .018(2) -.007(2) -.016(2) C4 .049(2) .049(2) .059(4) -.019(3) -.012(2) -.012(2) 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' O O .0106 .0060 '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' P P .1023 .0942 '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' 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 O1 Cu1 O1 . 2 179.1(3) no O1 Cu1 O1 . 3 90.003(3) no O1 Cu1 O1 . 4 90.003(3) no O1 Cu1 O1 2 3 90.003(3) no O1 Cu1 O1 2 4 90.003(3) no O1 Cu1 O1 4 3 179.1(3) no F1 P1 F1 5 . 180.0 no F1 P1 F3 5 2_565 90.0 no F1 P1 F3 . 2_565 90.0 no F1 P1 F3 5 . 90.0 no F1 P1 F3 . . 90.0 no F3 P1 F3 2_565 . 180.0 no F1 P1 F2 5 2_565 90.0 no F1 P1 F2 . 2_565 90.0 no F3 P1 F2 2_565 2_565 90.0 no F3 P1 F2 . 2_565 90.0 no F1 P1 F2 5 . 90.0 no F1 P1 F2 . . 90.0 no F3 P1 F2 2_565 . 90.0 no F3 P1 F2 . . 90.0 no F2 P1 F2 2_565 . 180.0 no C1 O1 Cu1 . . 113.9(4) no C3 N1 C3 8 . 110.3(5) no C3 N1 C4 8 . 107.9(3) no C3 N1 C4 . . 107.9(3) no C3 N1 C2 8 . 111.5(3) no C3 N1 C2 . . 111.5(3) no C4 N1 C2 . . 107.5(4) no O2 C1 O1 . . 126.7(4) no O2 C1 C2 . . 123.0(4) no O1 C1 C2 . . 110.3(4) no N1 C2 C1 . . 118.2(4) no N1 C2 H2 . . 105(2) no C1 C2 H2 . . 106(2) no N1 C3 H3a . . 103(3) no N1 C3 H3b . . 109(2) no H3a C3 H3b . . 108(4) no N1 C3 H3c . . 112(2) no H3a C3 H3c . . 116(4) no H3b C3 H3c . . 109(3) no N1 C4 H4a . . 109(3) no N1 C4 H4b . . 103(3) no H4a C4 H4b . . 122(3) 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 Cu1 O1 . 1.951(3) no Cu1 O1 2 1.951(3) no Cu1 O1 3 1.951(3) no Cu1 O1 4 1.951(3) no P1 F1 5 1.565(3) no P1 F1 . 1.565(3) no P1 F3 . 1.573(3) no P1 F3 2_565 1.573(3) no P1 F2 . 1.608(2) no P1 F2 2_565 1.608(2) no O1 C1 . 1.277(8) no O2 C1 . 1.219(6) no N1 C3 8 1.492(5) no N1 C3 . 1.492(5) no N1 C4 . 1.493(7) no N1 C2 . 1.501(6) no C1 C2 . 1.529(6) no C2 H2 . .97(4) no C3 H3a . .94(2) no C3 H3b . .94(2) no C3 H3c . .94(2) no C4 H4a . 1.01(3) no C4 H4b . 1.01(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 O1 Cu1 O1 C1 4 89.6(2) no O1 Cu1 O1 C1 3 -89.6(2) no Cu1 O1 C1 O2 . .0 no Cu1 O1 C1 C2 . 180.0 no C3 N1 C2 C1 8 61.9(3) no C3 N1 C2 C1 . -61.9(3) no C4 N1 C2 C1 . 180.0 no O2 C1 C2 N1 . .0 no O1 C1 C2 N1 . 180.0 no