#------------------------------------------------------------------------------ #$Date: 2016-02-21 09:56:54 +0000 (Sun, 21 Feb 2016) $ #$Revision: 176809 $ #$URL: svn://www.crystallography.net/cod/cif/2/30/01/2300198.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_2300198 loop_ _publ_author_name 'Morgenroth, Wolfgang' 'Overgaard, Jacob' 'Clausen, Henrik F.' 'Svendsen, Helle' 'J\/orgensen, Mads R. V.' 'Larsen, Finn K.' 'Iversen, Bo B.' _publ_section_title ; Helium cryostat synchrotron charge densities determined using a large CCD detector -- the upgraded beamline D3 at DESY ; _journal_coeditor_code HX5073 _journal_issue 5 _journal_name_full 'Journal of Applied Crystallography' _journal_page_first 846 _journal_page_last 853 _journal_paper_doi 10.1107/S0021889808024643 _journal_volume 41 _journal_year 2008 _space_group_IT_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_creation_method 'XD routine XDCIF' _cell_angle_alpha 94.686 _cell_angle_beta 100.568(2) _cell_angle_gamma 98.884 _cell_length_a 6.2170(10) _cell_length_b 6.9850(10) _cell_length_c 10.5060(10) _cell_volume 440.26(10) _computing_molecular_graphics 'Volkov et al, (2006)' _computing_publication_material 'Volkov et al, (2006)' _computing_structure_refinement 'Volkov et al, (2006)' _exptl_absorpt_correction_type none _refine_diff_density_max 0.414 _refine_diff_density_min -0.507 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.293 _refine_ls_matrix_type full _refine_ls_number_parameters 348 _refine_ls_number_reflns 8807 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.031 _refine_ls_R_factor_gt 0.026 _refine_ls_shift/su_max 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; calc w2 = 1/[s^2^(Fo^2^)] ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.033 _cod_data_source_file hx5073.cif _cod_data_source_block I _cod_database_code 2300198 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z loop_ _atom_rho_multipole_atom_label _atom_rho_multipole_coeff_Pv _atom_rho_multipole_coeff_P00 _atom_rho_multipole_coeff_P10 _atom_rho_multipole_coeff_P11 _atom_rho_multipole_coeff_P1-1 _atom_rho_multipole_coeff_P20 _atom_rho_multipole_coeff_P21 _atom_rho_multipole_coeff_P2-1 _atom_rho_multipole_coeff_P22 _atom_rho_multipole_coeff_P2-2 _atom_rho_multipole_coeff_P30 _atom_rho_multipole_coeff_P31 _atom_rho_multipole_coeff_P3-1 _atom_rho_multipole_coeff_P32 _atom_rho_multipole_coeff_P3-2 _atom_rho_multipole_coeff_P33 _atom_rho_multipole_coeff_P3-3 _atom_rho_multipole_coeff_P40 _atom_rho_multipole_coeff_P41 _atom_rho_multipole_coeff_P4-1 _atom_rho_multipole_coeff_P42 _atom_rho_multipole_coeff_P4-2 _atom_rho_multipole_coeff_P43 _atom_rho_multipole_coeff_P4-3 _atom_rho_multipole_coeff_P44 _atom_rho_multipole_coeff_P4-4 _atom_rho_multipole_kappa _atom_rho_multipole_kappa_prime0 _atom_rho_multipole_kappa_prime1 _atom_rho_multipole_kappa_prime2 _atom_rho_multipole_kappa_prime3 _atom_rho_multipole_kappa_prime4 _atom_rho_multipole_radial_slater_n0 _atom_rho_multipole_radial_slater_zeta0 _atom_rho_multipole_radial_slater_n1 _atom_rho_multipole_radial_slater_zeta1 _atom_rho_multipole_radial_slater_n2 _atom_rho_multipole_radial_slater_zeta2 _atom_rho_multipole_radial_slater_n3 _atom_rho_multipole_radial_slater_zeta3 _atom_rho_multipole_radial_slater_n4 _atom_rho_multipole_radial_slater_zeta4 K(1) 18 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 0 0 0 0 0 0 0 0 0 0 O(1) 6.383(17) 0 0.004(8) -0.034(10) 0.010(8) -0.093(9) -0.005(8) 0.001(8) -0.065(9) 0.025(8) -0.017(8) -0.016(8) 0.001(7) -0.009(7) 0.008(7) 0.041(7) -0.006(7) 0 0 0 0 0 0 0 0 0 0.9723(10) 0.955911 0.955911 0.955911 0.955911 0.955911 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(2) 6.426(19) 0 0.002(9) 0.020(9) -0.039(9) -0.013(9) -0.001(9) -0.012(8) 0.089(9) -0.008(9) -0.007(8) -0.031(8) -0.026(8) -0.010(8) -0.006(7) 0.088(7) -0.021(8) 0 0 0 0 0 0 0 0 0 0.9742(12) 0.957394 0.957394 0.957394 0.957394 0.957394 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(3) 6.371(19) 0 0.007(9) 0.014(9) -0.062(9) -0.037(9) -0.009(9) -0.005(8) 0.063(8) -0.009(9) 0.009(8) -0.029(8) -0.014(8) -0.003(7) 0.003(7) 0.095(7) -0.009(7) 0 0 0 0 0 0 0 0 0 0.9742(12) 0.957394 0.957394 0.957394 0.957394 0.957394 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(4) 6.348(17) 0 0.004(8) -0.045(10) -0.002(8) -0.083(9) 0.011(8) -0.007(8) -0.067(9) -0.029(8) -0.005(8) -0.004(8) -0.001(8) -0.001(7) 0.006(7) 0.054(7) -0.002(7) 0 0 0 0 0 0 0 0 0 0.9723(10) 0.955911 0.955911 0.955911 0.955911 0.955911 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(5) 6.40(2) 0 0.003(9) -0.011(9) -0.033(9) -0.052(9) -0.014(9) -0.011(9) 0.048(9) -0.004(9) -0.001(8) -0.023(8) -0.017(8) -0.009(8) 0.007(8) 0.100(8) -0.020(8) 0 0 0 0 0 0 0 0 0 0.9742(12) 0.957394 0.957394 0.957394 0.957394 0.957394 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(6) 6.387(17) 0 -0.006(8) -0.049(9) -0.005(8) -0.102(9) 0.032(9) -0.011(8) -0.064(8) 0.006(8) -0.005(8) -0.002(8) -0.019(7) 0.007(8) -0.008(7) 0.047(7) -0.003(7) 0 0 0 0 0 0 0 0 0 0.9723(10) 0.955911 0.955911 0.955911 0.955911 0.955911 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(7) 6.423(17) 0 -0.009(8) -0.042(9) -0.012(8) -0.079(9) -0.002(9) -0.022(8) -0.031(9) -0.040(8) 0.002(8) -0.013(8) 0.001(7) -0.013(8) -0.002(7) 0.071(7) -0.012(7) 0 0 0 0 0 0 0 0 0 0.9723(10) 0.955911 0.955911 0.955911 0.955911 0.955911 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(8) 6.403(16) 0 -0.004(8) -0.045(9) -0.012(8) -0.107(9) -0.048(9) 0.016(8) -0.078(8) 0.005(8) 0.006(8) -0.028(8) -0.006(7) -0.002(8) 0.008(7) 0.043(7) -0.004(7) 0 0 0 0 0 0 0 0 0 0.9723(10) 0.955911 0.955911 0.955911 0.955911 0.955911 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(9) 6.55(3) 0 0.002(8) -0.029(8) -0.028(8) 0.001(9) -0.038(8) -0.017(8) -0.017(7) 0.016(8) -0.002(8) -0.034(7) -0.054(7) -0.007(7) 0.016(7) 0.093(7) -0.037(7) 0 0 0 0 0 0 0 0 0 0.9645(16) 0.967312 0.967312 0.967312 0.967312 0.967312 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 O(10) 6.55(3) 0 0.007(8) -0.027(8) -0.031(8) 0.013(9) -0.001(8) 0.012(8) -0.021(7) 0.043(8) 0.006(8) -0.033(7) -0.043(8) 0.008(7) -0.016(7) 0.109(7) -0.040(7) 0 0 0 0 0 0 0 0 0 0.9645(16) 0.967312 0.967312 0.967312 0.967312 0.967312 2 4.466 2 4.466 2 4.466 3 4.466 4 4.466 C(1) 3.83(2) 0 -0.006(9) 0.043(11) -0.018(9) -0.237(10) -0.003(9) -0.006(9) 0.007(11) -0.017(9) 0.008(12) 0.036(11) -0.003(10) -0.002(10) 0.014(11) 0.302(11) 0.010(13) 0 0 0 0 0 0 0 0 0 1.013(2) 1.001788 1.001788 1.001788 1.001788 1.001788 2 3.1762 2 3.1762 2 3.1762 3 3.1762 4 3.1762 C(2) 3.80(2) 0 0.002(9) 0.054(11) -0.008(9) -0.257(10) 0.007(9) -0.003(9) 0.027(11) 0.004(9) 0.007(12) 0.003(11) 0.010(10) -0.009(10) 0.028(11) 0.309(11) 0.018(14) 0 0 0 0 0 0 0 0 0 1.013(2) 1.001788 1.001788 1.001788 1.001788 1.001788 2 3.1762 2 3.1762 2 3.1762 3 3.1762 4 3.1762 C(3) 3.79(2) 0 0.021(9) 0.078(11) -0.044(10) -0.265(10) 0.016(9) 0.001(9) 0.031(10) 0.015(10) -0.014(11) -0.007(11) 0.012(10) 0.003(11) 0.008(11) 0.294(12) -0.001(12) 0 0 0 0 0 0 0 0 0 1.013(2) 1.001788 1.001788 1.001788 1.001788 1.001788 2 3.1762 2 3.1762 2 3.1762 3 3.1762 4 3.1762 C(4) 3.82(2) 0 -0.007(8) 0.032(11) 0.017(10) -0.245(10) -0.030(9) 0.004(9) 0.014(10) -0.036(10) 0.021(11) -0.002(11) -0.003(10) -0.011(11) -0.012(11) 0.293(12) 0.034(12) 0 0 0 0 0 0 0 0 0 1.013(2) 1.001788 1.001788 1.001788 1.001788 1.001788 2 3.1762 2 3.1762 2 3.1762 3 3.1762 4 3.1762 H(2) 0.579(13) 0 0.057(11) 0.001(8) -0.004(8) 0.037(16) 0.018(14) -0.042(14) -0.010(12) 0.003(12) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 2 H(3) 0.593(12) 0 0.023(10) -0.016(9) 0.001(8) 0.089(16) 0.015(14) 0.043(14) 0.017(12) -0.001(12) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 2 H(5) 0.600(13) 0 0.101(11) 0.017(8) -0.003(9) 0.071(16) 0.037(13) -0.011(14) -0.014(12) 0.013(11) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 2 H(9A) 0.689(9) 0 0.110(7) 0 0 0.069(8) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 2 H(9B) 0.6885 0 0.1095 0 0 0.0688 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 2 H(10A) 0.6885 0 0.1095 0 0 0.0688 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 2 H(10B) 0.6885 0 0.1095 0 0 0.0688 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.2 1.2 1.2 1.2 1.2 1.2 0 2 1 2 2 2 3 2 4 2 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 K(1) 0.00580(6) 0.00486(6) 0.00548(6) -0.00018(4) 0.00117(4) 0.00075(4) O(1) 0.00492(10) 0.00590(10) 0.00412(10) -0.00124(9) 0.00006(8) 0.00131(8) O(2) 0.00534(10) 0.00783(11) 0.00281(10) 0.00008(9) -0.00020(8) 0.00221(8) O(3) 0.00589(11) 0.00639(10) 0.00255(9) -0.00078(9) -0.00129(8) 0.00151(8) O(4) 0.00407(10) 0.00692(10) 0.00415(10) -0.00080(9) -0.00043(8) 0.00110(8) O(5) 0.01056(12) 0.00447(10) 0.00202(9) 0.00162(9) -0.00066(8) 0.00014(8) O(6) 0.00916(11) 0.00319(9) 0.00390(10) 0.00083(9) 0.00042(8) 0.00057(8) O(7) 0.00869(11) 0.00503(10) 0.00201(9) 0.00022(9) -0.00072(8) 0.00039(8) O(8) 0.01088(12) 0.00320(10) 0.00404(10) 0.00093(9) 0.00033(9) 0.00082(8) O(9) 0.00744(11) 0.00578(10) 0.00342(10) 0.00201(9) 0.00017(8) 0.00092(8) O(10) 0.00519(10) 0.00768(11) 0.00403(10) 0.00022(9) -0.00021(8) 0.00195(8) C(1) 0.00434(10) 0.00406(9) 0.00242(9) 0.00007(9) -0.00017(8) 0.00071(7) C(2) 0.00385(10) 0.00468(9) 0.00258(9) 0.00031(9) -0.00020(7) 0.00070(8) C(3) 0.00560(10) 0.00338(10) 0.00237(9) 0.00080(8) 0.00018(8) 0.00060(8) C(4) 0.00558(10) 0.00341(10) 0.00235(9) 0.00098(8) 0.00012(8) 0.00067(8) H(2) 0.016856 0.015465 0.010833 0.001305 0.002878 0.002567 H(3) 0.017916 0.014655 0.012989 0.000409 0.002267 0.001235 H(5) 0.021878 0.01346 0.009357 0.002214 0.002341 0.002375 H(9A) 0.02769 0.011247 0.014467 0.005424 0.003393 0.005786 H(9B) 0.02526 0.016044 0.011832 0.005915 0.005609 -0.001987 H(10A) 0.021866 0.020196 0.01426 0.000856 0.010276 0.005935 H(10B) 0.012474 0.021665 0.018989 -0.002279 -0.002242 0.000645 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy K(1) 0.166902(10) 0.146531(9) 0.272299(6) 0.005 1 O(1) 0.32768(6) 0.32887(5) 0.06605(3) 0.005 1 O(2) -0.49600(6) -0.07104(5) 0.15539(3) 0.005 1 O(3) 0.65294(6) 0.51936(5) 0.15900(3) 0.005 1 O(4) -0.23141(6) 0.11365(5) 0.07737(3) 0.005 1 O(5) 0.18091(6) -0.44219(5) 0.30600(3) 0.006 1 O(6) 0.28126(6) -0.15314(5) 0.42892(3) 0.006 1 O(7) 0.35630(6) -0.34409(5) 0.64478(3) 0.006 1 O(8) 0.21781(6) -0.62730(5) 0.51715(3) 0.006 1 O(9) -0.21285(6) -0.05175(5) 0.35666(3) 0.006 1 O(10) 0.05496(6) -0.23947(5) 0.12958(3) 0.006 1 C(1) 0.48896(5) 0.45360(5) 0.06365(3) 0.004 1 C(2) -0.41627(5) 0.01568(5) 0.06547(3) 0.004 1 C(3) 0.24662(5) -0.33147(5) 0.41668(3) 0.004 1 C(4) 0.27615(5) -0.44739(5) 0.53688(3) 0.004 1 H(2) -0.37051 -0.060957 0.243925 0.014 1 H(3) 0.643304 0.443508 0.247473 0.016 1 H(5) 0.137889 -0.357491 0.22923 0.015 1 H(9A) -0.214791 -0.179727 0.389357 0.017 1 H(9B) -0.252828 0.033091 0.424914 0.017 1 H(10A) 0.142382 -0.202357 0.064608 0.018 1 H(10B) -0.094466 -0.290244 0.081178 0.019 1 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C(2) O(2) H(2) 1_555 1_555 1_555 111.54(3) yes C(1) O(3) H(3) 1_555 1_555 1_555 112.99(3) yes C(3) O(5) H(5) 1_555 1_555 1_555 110.49(3) yes C(4) O(7) H(3) 1_555 1_555 2_656 114.80(3) yes H(2) O(9) H(9A) 1_555 1_555 1_555 111.54(3) yes H(2) O(9) H(9B) 1_555 1_555 1_555 108.01(3) yes H(9A) O(9) H(9B) 1_555 1_555 1_555 105.63(3) yes H(5) O(10) H(10A) 1_555 1_555 1_555 119.94(3) yes H(5) O(10) H(10B) 1_555 1_555 1_555 114.53(3) yes H(10A) O(10) H(10B) 1_555 1_555 1_555 105.78(3) yes O(1) C(1) O(3) 1_555 1_555 1_555 126.41(3) yes O(1) C(1) C(1) 1_555 1_555 2_665 120.25(4) yes O(3) C(1) C(1) 1_555 1_555 2_665 113.33(3) yes O(2) C(2) O(4) 1_555 1_555 1_555 126.43(3) yes O(2) C(2) C(2) 1_555 1_555 2_455 112.39(3) yes O(4) C(2) C(2) 1_555 1_555 2_455 121.18(4) yes O(5) C(3) O(6) 1_555 1_555 1_555 125.02(3) yes O(5) C(3) C(4) 1_555 1_555 1_555 113.58(3) yes O(6) C(3) C(4) 1_555 1_555 1_555 121.40(3) yes O(7) C(4) O(8) 1_555 1_555 1_555 127.74(3) yes O(7) C(4) C(3) 1_555 1_555 1_555 114.90(3) yes O(8) C(4) C(3) 1_555 1_555 1_555 117.36(3) yes O(2) H(2) O(9) 1_555 1_555 1_555 178.91(2) yes O(3) H(3) O(7) 1_555 1_555 2_656 176.05(2) yes O(5) H(5) O(10) 1_555 1_555 1_555 173.22(2) yes O(9) H(9A) H(9B) 1_555 1_555 1_555 37.22(2) yes O(9) H(9B) H(9A) 1_555 1_555 1_555 37.152(19) yes O(10) H(10A) H(10B) 1_555 1_555 1_555 37.03(2) yes O(10) H(10B) H(10A) 1_555 1_555 1_555 37.19(2) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O(1) C(1) 1_555 1_555 1.2281(4) yes O(2) C(2) 1_555 1_555 1.2952(4) yes O(2) H(2) 1_555 1_555 1.0885(3) yes O(3) C(1) 1_555 1_555 1.2882(4) yes O(3) H(3) 1_555 1_555 1.1133(3) yes O(4) C(2) 1_555 1_555 1.2228(4) yes O(5) C(3) 1_555 1_555 1.3033(4) yes O(5) H(5) 1_555 1_555 1.0582(3) yes O(6) C(3) 1_555 1_555 1.2229(4) yes O(7) C(4) 1_555 1_555 1.2657(4) yes O(7) H(3) 1_555 2_656 1.3754(3) yes O(8) C(4) 1_555 1_555 1.2421(4) yes O(9) H(2) 1_555 1_555 1.3820(3) yes O(9) H(9A) 1_555 1_555 0.9827(3) yes O(9) H(9B) 1_555 1_555 0.9842(3) yes O(10) H(5) 1_555 1_555 1.4546(3) yes O(10) H(10A) 1_555 1_555 0.9747(3) yes O(10) H(10B) 1_555 1_555 0.9710(3) yes C(1) C(1) 1_555 2_665 1.5521(6) yes C(2) C(2) 1_555 2_455 1.5425(6) yes C(3) C(4) 1_555 1_555 1.5530(4) yes H(9A) H(9B) 1_555 1_555 1.5670031389722 yes H(10A) H(10B) 1_555 1_555 1.551664258724 yes #BEGIN Loops that were not found in dictionaries: loop_ _atom_site_anharm_gc_d_label _atom_site_anharm_gc_d_1111 _atom_site_anharm_gc_d_2222 _atom_site_anharm_gc_d_3333 _atom_site_anharm_gc_d_1112 _atom_site_anharm_gc_d_1222 _atom_site_anharm_gc_d_1113 _atom_site_anharm_gc_d_1333 _atom_site_anharm_gc_d_2223 _atom_site_anharm_gc_d_2333 _atom_site_anharm_gc_d_1122 _atom_site_anharm_gc_d_1133 _atom_site_anharm_gc_d_2233 _atom_site_anharm_gc_d_1123 _atom_site_anharm_gc_d_1223 _atom_site_anharm_gc_d_1233 K(1) 0.00014(5) 0.00033(3) 0.000127(6) -0.00043(3) -0.000264(16) 0.000384(14) 0.000027(5) 0.000095(9) 0.000007(4) -0.000129(17) 0.000164(7) 0.000111(5) 0.000138(7) 0.000082(6) 0.000038(4) #END Loops that were not found in dictionaries