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#$Date: 2016-03-23 04:09:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179278 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/98/4319843.cif $
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#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4319843
loop_
_publ_author_name
'John F. Lehmann'
'David A. Dixon'
'Gary J. Schrobilgen'
_publ_section_title
;
 X-ray Crystal Structures of α-KrF2, [KrF][MF6] (M = As, Sb, Bi),
 [Kr2F3][SbF6].KrF2, [Kr2F3]2[SbF6]2.KrF2, and [Kr2F3][AsF6].[KrF][AsF6];
 Synthesis and Characterization of [Kr2F3][PF6].nKrF2; and Theoretical
 Studies of KrF2, KrF+, Kr2F3+, and the [KrF][MF6] (M = P, As, Sb, Bi) Ion
 Pairs
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3002
_journal_page_last               3017
_journal_paper_doi               10.1021/ic001167w
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'F20 Kr5 Sb2'
_chemical_formula_weight         1042.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 111.945(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0416(16)
_cell_length_b                   30.814(6)
_cell_length_c                   8.1365(16)
_cell_measurement_temperature    148(2)
_cell_volume                     1870.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      148(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18251
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    14.816
_exptl_crystal_density_diffrn    3.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.00071(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0328P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                2764
_reflns_number_total             4033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001167w_5.cif
_cod_data_source_block           Kr2F3+SbF6-KrF2a
_cod_database_code               4319843
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb2 Sb 0.78981(6) 0.075810(15) 0.94253(6) 0.01874(13) Uani 1 d . . .
Sb1 Sb 1.31493(6) 0.324051(15) 0.96179(6) 0.01876(13) Uani 1 d . . .
Kr3 Kr 0.75338(9) 0.22000(2) 1.01920(9) 0.02254(18) Uani 1 d . . .
Kr1 Kr 1.24253(9) 0.02975(2) 1.49194(10) 0.02524(19) Uani 1 d . . .
Kr4 Kr 1.14574(9) 0.19517(2) 0.90389(9) 0.02202(18) Uani 1 d . . .
Kr2 Kr 1.34178(9) 0.05885(2) 1.10222(10) 0.02491(18) Uani 1 d . . .
F14 F 1.5355(5) 0.32723(13) 1.1524(5) 0.0287(10) Uani 1 d . . .
F20 F 0.6803(5) 0.11789(13) 1.0343(5) 0.0297(10) Uani 1 d . . .
F19 F 0.9037(6) 0.03351(15) 0.8551(6) 0.0362(11) Uani 1 d . . .
F13 F 1.4066(6) 0.27903(15) 0.8659(6) 0.0429(13) Uani 1 d . . .
F18 F 0.9133(6) 0.11958(15) 0.8748(6) 0.0399(12) Uani 1 d . . .
F12 F 1.3914(6) 0.36515(15) 0.8344(6) 0.0444(13) Uani 1 d . . .
F17 F 0.6661(6) 0.03223(13) 1.0127(6) 0.0326(11) Uani 1 d . . .
F16 F 0.6014(5) 0.07751(14) 0.7208(5) 0.0327(11) Uani 1 d . . .
F15 F 0.9818(5) 0.07311(14) 1.1632(5) 0.0305(10) Uani 1 d . . .
F11 F 1.2314(6) 0.28320(13) 1.0837(5) 0.0289(10) Uani 1 d . . .
F10 F 1.0967(5) 0.31944(15) 0.7669(5) 0.0367(11) Uani 1 d . . .
F5 F 1.3570(5) 0.17098(14) 0.9334(6) 0.0374(12) Uani 1 d . . .
F6 F 0.9024(5) 0.22377(14) 0.8628(6) 0.0319(11) Uani 1 d . . .
F3 F 1.3992(5) 0.02879(15) 1.3441(6) 0.0350(11) Uani 1 d . . .
F4 F 0.6259(6) 0.21763(15) 1.1593(6) 0.0402(12) Uani 1 d . . .
F2 F 1.2985(6) 0.08387(15) 0.8905(6) 0.0413(12) Uani 1 d . . .
F1 F 1.1099(6) 0.02939(16) 1.6284(6) 0.0459(13) Uani 1 d . . .
F9 F 1.2202(5) 0.36893(13) 1.0553(6) 0.0325(11) Uani 1 d . . .
Kr5 Kr 0.80366(9) 0.37603(2) 0.95542(9) 0.02345(17) Uani 1 d . . .
F8 F 0.8656(6) 0.31759(15) 1.0182(6) 0.0381(12) Uani 1 d . . .
F7 F 0.7423(6) 0.43413(14) 0.8895(6) 0.0392(12) Uani 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Kr Kr -0.5574 2.7079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F20 Sb2 F16 91.89(18) . . ?
F20 Sb2 F18 89.9(2) . . ?
F16 Sb2 F18 91.34(19) . . ?
F20 Sb2 F19 178.80(18) . . ?
F16 Sb2 F19 89.31(19) . . ?
F18 Sb2 F19 90.0(2) . . ?
F20 Sb2 F17 89.57(19) . . ?
F16 Sb2 F17 89.03(19) . . ?
F18 Sb2 F17 179.4(2) . . ?
F19 Sb2 F17 90.4(2) . . ?
F20 Sb2 F15 89.46(18) . . ?
F16 Sb2 F15 178.65(19) . . ?
F18 Sb2 F15 88.66(18) . . ?
F19 Sb2 F15 89.33(18) . . ?
F17 Sb2 F15 90.99(19) . . ?
F9 Sb1 F14 91.61(18) . . ?
F9 Sb1 F13 179.21(19) . . ?
F14 Sb1 F13 89.17(19) . . ?
F9 Sb1 F11 90.0(2) . . ?
F14 Sb1 F11 90.71(18) . . ?
F13 Sb1 F11 89.9(2) . . ?
F9 Sb1 F12 89.6(2) . . ?
F14 Sb1 F12 91.02(19) . . ?
F13 Sb1 F12 90.5(2) . . ?
F11 Sb1 F12 178.23(18) . . ?
F9 Sb1 F10 90.30(19) . . ?
F14 Sb1 F10 178.1(2) . . ?
F13 Sb1 F10 88.9(2) . . ?
F11 Sb1 F10 89.40(19) . . ?
F12 Sb1 F10 88.88(19) . . ?
F4 Kr3 F6 178.7(2) . . ?
F1 Kr1 F3 177.9(2) . . ?
F5 Kr4 F6 178.3(2) . . ?
F2 Kr2 F3 177.8(2) . . ?
Kr3 F6 Kr4 128.0(2) . . ?
Kr1 F3 Kr2 126.0(2) . . ?
F7 Kr5 F8 179.1(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb2 F20 1.872(4) . ?
Sb2 F16 1.874(4) . ?
Sb2 F18 1.876(4) . ?
Sb2 F19 1.880(4) . ?
Sb2 F17 1.882(4) . ?
Sb2 F15 1.882(4) . ?
Sb1 F9 1.872(4) . ?
Sb1 F14 1.872(4) . ?
Sb1 F13 1.873(4) . ?
Sb1 F11 1.876(4) . ?
Sb1 F12 1.879(4) . ?
Sb1 F10 1.880(4) . ?
Kr3 F4 1.797(5) . ?
Kr3 F6 2.052(5) . ?
Kr1 F1 1.805(5) . ?
Kr1 F3 2.041(5) . ?
Kr4 F5 1.787(4) . ?
Kr4 F6 2.056(4) . ?
Kr2 F2 1.799(4) . ?
Kr2 F3 2.065(4) . ?
Kr5 F7 1.881(4) . ?
Kr5 F8 1.887(4) . ?
