#------------------------------------------------------------------------------
#$Date: 2016-02-21 11:56:54 +0200 (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'
'Jørgensen, 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/[s²(Fo²)]
;
_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_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
