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#$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2003121.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_2003121
loop_
_publ_author_name
'Peterkov\'a, J.'
'Dusek, M.'
'Petr\'icek, V.'
'Loub, J.'
_publ_section_title
;
Structures of Fluoroarsenates KAsF~6n~(OH)~n~, n
= 0, 1, 2: Application of the Heavy-Atom Method for Modulated
Structures
;
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section B'
_journal_page_first 809
_journal_page_last 818
_journal_volume 54
_journal_year 1998
_chemical_formula_moiety 'K As F5 H O'
_chemical_formula_sum 'As F5 H K O'
_chemical_formula_weight 226.02
_chemical_name_systematic
;
potassium hydroxopentafluoroarsenate
;
_space_group_IT_number 60
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2bc 2n'
_symmetry_space_group_name_H-M 'P n a b'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 24
_cell_length_a 9.391(2)
_cell_length_b 11.336(3)
_cell_length_c 28.173(8)
_cell_measurement_reflns_used 33
_cell_measurement_temperature 291
_cell_measurement_theta_max 21
_cell_measurement_theta_min 7
_cell_volume 2999.2(13)
_computing_cell_refinement 'HW Petricek 1994)'
_computing_data_collection 'HW Petricek 1994'
_computing_data_reduction 'JANA96 Petricek&Dusek 1996'
_computing_publication_material ' '
_computing_structure_refinement 'JANA96 Petricek&Dusek 1996'
_computing_structure_solution 'JANA96 Petricek&Dusek 1996'
_diffrn_ambient_temperature 291
_diffrn_measurement_device 'Hilger&Watts diffractometer'
_diffrn_measurement_method \w-2q
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_type 'Ag K\a'
_diffrn_radiation_wavelength 0.5609
_diffrn_reflns_av_R_equivalents 0
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 42
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 5377
_diffrn_reflns_theta_max 25.4
_diffrn_reflns_theta_min 11.2
_diffrn_standards_decay_% 11
_diffrn_standards_interval_count 30
_diffrn_standards_number 9
_exptl_absorpt_coefficient_mu 4.02
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 3.002(3)
_exptl_crystal_density_meas 2.951(6)
_exptl_crystal_density_method flotation
_exptl_crystal_description prism
_exptl_crystal_F_000 2544
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.2
_refine_diff_density_max 1.54
_refine_diff_density_min -1.24
_refine_ls_extinction_coef 53E1(12)
_refine_ls_extinction_method 'B-C type 2 isotropic'
_refine_ls_goodness_of_fit_obs 1.55
_refine_ls_hydrogen_treatment refxyz
_refine_ls_number_parameters 219
_refine_ls_number_reflns 3711
_refine_ls_R_factor_all .080
_refine_ls_R_factor_obs .047
_refine_ls_shift/esd_max .001
_refine_ls_shift/esd_mean .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme 'calc w=1/(\s^2^(F)+0.003F^2^)'
_refine_ls_wR_factor_all .085
_refine_ls_wR_factor_obs .077
_reflns_number_observed 3711
_reflns_number_total 5363
_reflns_observed_criterion F>3.0\s(F)
_[local]_cod_data_source_file sh0109.cif
_[local]_cod_data_source_block B
_[local]_cod_cif_authors_sg_Hall '-p 2bc -2n'
_[local]_cod_chemical_formula_sum_orig 'K As F5 H O'
_cod_original_cell_volume 2999.20(10)
_cod_database_code 2003121
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,1/2+y,1/2+z
+x,1/2+y,1/2-z
1/2-x,+y,-z
-x,-y,-z
1/2+x,1/2-y,1/2-z
-x,1/2-y,1/2+z
1/2+x,-y,+z
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
Ka 0.0369(7) 0.0403(8) 0.0412(8) 0.00000 0.0075(6) 0.00000
Kb 0.0313(5) 0.0366(5) 0.0303(5) -0.0034(4) -0.0013(4) 0.0021(4)
Kc 0.0317(5) 0.0310(5) 0.0323(5) 0.0028(4) 0.0012(4) 0.0012(4)
Kd 0.0314(6) 0.0288(6) 0.0312(7) 0.00000 0.0013(5) 0.00000
As1a 0.0186(2) 0.0182(2) 0.0261(2) -0.00030(10) -0.00050(10) -0.00040(10)
F1a 0.0250(10) 0.041(2) 0.076(3) -0.0130(10) -0.0010(10) 0.0030(10)
O2a 0.0200(10) 0.029(2) 0.059(2) -0.0020(10) 0.0000(10) 0.001(2)
F3a 0.040(2) 0.044(2) 0.054(2) 0.0020(10) 0.0120(10) -0.0240(10)
F4a 0.048(2) 0.048(2) 0.055(2) 0.002(2) -0.003(2) 0.028(2)
F5a 0.036(2) 0.044(2) 0.049(2) 0.0010(10) -0.0100(10) 0.0190(10)
F6a 0.053(2) 0.047(2) 0.053(2) 0.007(2) 0.000(2) -0.027(2)
As2b 0.0266(2) 0.0194(2) 0.0247(2) -0.00150(10) 0.00020(10) -0.00120(10)
F1b 0.101(3) 0.0210(10) 0.052(2) -0.010(2) 0.016(2) -0.0010(10)
O2b 0.053(2) 0.021(2) 0.065(3) -0.001(2) 0.009(2) 0.0030(10)
F4b 0.071(3) 0.071(3) 0.118(4) 0.015(2) -0.058(3) -0.001(3)
F5b 0.092(3) 0.048(2) 0.053(2) 0.003(2) 0.033(2) -0.005(2)
F6b 0.040(2) 0.079(3) 0.096(3) 0.000(2) -0.030(2) -0.013(2)
F3b 0.125(4) 0.046(2) 0.043(2) -0.005(2) 0.037(2) -0.003(2)
As1c 0.0183(2) 0.0215(2) 0.0273(2) -0.00130(10) 0.00120(10) 0.00020(10)
F1c 0.0240(10) 0.049(2) 0.075(2) -0.0140(10) 0.0110(10) -0.011(2)
O2c 0.0190(10) 0.032(2) 0.064(2) 0.0000(10) 0.0000(10) 0.002(2)
F3c 0.036(2) 0.058(2) 0.094(3) -0.004(2) 0.011(2) -0.044(2)
F4c 0.054(2) 0.096(3) 0.098(3) 0.020(2) 0.009(2) 0.070(3)
F5c 0.039(2) 0.129(4) 0.069(3) -0.001(2) -0.006(2) 0.060(3)
F6c 0.050(2) 0.087(3) 0.129(4) -0.018(2) 0.033(2) -0.077(3)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Ka 0.25 0.3420(2) 0.0 0.0395(5) Uani
Kb 0.23040(10) 0.33830(10) 0.16589(4) 0.0327(3) Uani
Kc 0.25120(10) 0.32270(10) 0.33167(4) 0.0317(3) Uani
Kd 0.25 0.31850(10) 0.5 0.0304(4) Uani
As1a 0.07660(4) 0.10448(4) 0.080830(10) 0.02090(10) Uani
F1a -0.0962(3) 0.0503(3) 0.08010(10) 0.0473(11) Uani
O2a 0.2443(4) 0.1693(3) 0.08150(10) 0.0362(11) Uani
Ha 0.306160 0.109150 0.085270 0.0300 Uiso
F3a 0.0174(3) 0.2034(3) 0.12300(10) 0.0462(10) Uani
F4a 0.1167(4) 0.0032(3) 0.12430(10) 0.0501(11) Uani
F5a 0.0222(3) 0.2030(3) 0.03750(10) 0.0433(10) Uani
F6a 0.1201(4) 0.0033(3) 0.03820(10) 0.0509(11) Uani
As2b 0.10687(5) 0.09384(4) 0.415830(10) 0.02350(10) Uani
F1b 0.1286(5) 0.2453(3) 0.41360(10) 0.0579(14) Uani
O2b 0.0942(5) -0.0585(3) 0.41890(10) 0.0461(13) Uani
Hb -0.012800 -0.073670 0.422417 0.0300 Uiso
F4b -0.0554(5) 0.1106(4) 0.3901(2) 0.087(2) Uani
F5b 0.0315(5) 0.1156(3) 0.47050(10) 0.0647(14) Uani
F6b 0.2717(4) 0.0864(4) 0.4431(2) 0.0718(16) Uani
F3b 0.1886(5) 0.0851(3) 0.36170(10) 0.0712(16) Uani
As1c 0.08279(4) 0.10744(4) 0.75732(2) 0.02240(10) Uani
F1c -0.0926(3) 0.0578(3) 0.75930(10) 0.0495(11) Uani
O2c 0.2524(3) 0.1678(3) 0.75510(10) 0.0384(11) Uani
Hc 0.307070 0.118420 0.761312 0.0300 Uiso
F3c 0.0294(4) 0.2147(3) 0.79670(10) 0.0624(13) Uani
F4c 0.1211(4) 0.0157(4) 0.8033(2) 0.0829(18) Uani
F5c 0.0308(4) 0.1964(5) 0.71170(10) 0.0789(17) Uani
F6c 0.1216(4) -0.0046(4) 0.7189(2) 0.0887(19) Uani
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As .196 1.332 International_Tables_Vol_IV_Table_2.2B
K .118 .156 International_Tables_Vol_IV_Table_2.2B
F .006 .006 International_Tables_Vol_IV_Table_2.2B
O .003 .004 International_Tables_Vol_IV_Table_2.2B
H 0 0 International_Tables_Vol_IV_Table_2.2B
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 6 0
0 8 0
0 10 0
4 0 0
6 0 0
8 0 0
0 0 4
0 0 6
0 0 8
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F1a As1a F3a . 86.4(2) yes
O2a As1a F4a . 94.4(2) yes
As1a O2a Ha . 105.4(3) yes
O2a Ha F1a 8_555 162.7(3) yes
F1b As2b F5b . 86.5(2) yes
O2b As2b F5b . 94.0(2) yes
As2b O2b Hb . 103.9(3) yes
O2b Hb F6b 8_455 168.1(2) yes
F1c As1c F3c . 86.1(2) yes
O2c As1c F4c . 94.2(2) yes
As1c O2c Hc . 108.3(3) yes
O2c Hc F1c 8_555 157.6(3) yes
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
As1a F1a . 1.735(3) yes
As1a O2a . 1.737(3) yes
As1a F3a . 1.725(3) yes
As1a F4a . 1.719(4) yes
As1a F5a . 1.732(3) yes
As1a F6a . 1.711(4) yes
O2a Ha . 0.902(3) yes
Ha F1a 8_555 2.032(4) yes
As2b F1b . 1.730(3) yes
As2b O2b . 1.733(3) yes
As2b F3b . 1.710(4) yes
As2b F4b . 1.698(5) yes
As2b F5b . 1.714(4) yes
As2b F6b . 1.730(4) yes
O2b Hb . 1.024(4) yes
Hb F1b 8_455 2.112(4) yes
As1c F1c . 1.742(3) yes
As1c O2c . 1.735(3) yes
As1c F3c . 1.720(4) yes
As1c F4c . 1.700(5) yes
As1c F5c . 1.705(5) yes
As1c F6c . 1.708(5) yes
O2c Hc . 0.779(3) yes
Hc F1c 8_555 2.209(4) yes