#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/14/4121414.cif $
#------------------------------------------------------------------------------
#
# 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_4121414
loop_
_publ_author_name
'Debackere, John R.'
'Mercier, Hélène P A'
'Schrobilgen, Gary J.'
_publ_section_title
;
 Noble-Gas Difluoride Complexes of Mercury(II): The Syntheses and
 Structures of Hg(OTeF5)2·1.5NgF2 (Ng = Xe, Kr) and Hg(OTeF5)2.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3888
_journal_page_last               3903
_journal_paper_doi               10.1021/ja412193z
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'F13 Hg Kr1.5 O2 Te2'
_chemical_formula_weight         860.49
_chemical_name_common            'Hg (O Te F5)2, (Kr F2)1.5'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.783(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7981(4)
_cell_length_b                   17.4159(9)
_cell_length_c                   9.2247(4)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71
_cell_volume                     1293.44(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            53615
_diffrn_reflns_theta_full        35.50
_diffrn_reflns_theta_max         35.50
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    21.572
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2.0-2 (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.096
_refine_diff_density_min         -3.371
_refine_diff_density_rms         0.304
_refine_ls_extinction_coef       0.00176(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         5906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0331P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                5263
_reflns_number_total             5906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja412193z_si_002.cif
_cod_data_source_block           Hg(OTeF5)2_1.5KrF2
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'F13 Hg Kr1.50 O2 Te2'
_cod_database_code               4121414
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Hg1 Hg 0.538005(16) 0.108288(7) 0.975559(16) 0.01228(4) Uani 1 1 d .
O1 O 0.5912(4) 0.03025(16) 1.1527(4) 0.0180(5) Uani 1 1 d .
Te1 Te 0.69743(3) 0.049253(13) 1.36592(3) 0.01488(5) Uani 1 1 d .
F1 F 0.5025(4) 0.05778(19) 1.3905(4) 0.0330(7) Uani 1 1 d .
F2 F 0.9038(4) 0.04517(19) 1.3610(4) 0.0303(6) Uani 1 1 d .
F3 F 0.8034(5) 0.06549(19) 1.5802(4) 0.0348(7) Uani 1 1 d .
F4 F 0.7030(4) 0.15393(15) 1.3436(4) 0.0257(5) Uani 1 1 d .
F5 F 0.7081(4) -0.05364(15) 1.4084(3) 0.0251(5) Uani 1 1 d .
O2 O 0.4595(4) 0.17936(17) 0.7869(4) 0.0175(5) Uani 1 1 d .
Te2 Te 0.57269(3) 0.253655(13) 0.73320(3) 0.01218(5) Uani 1 1 d .
F6 F 0.6757(4) 0.33109(18) 0.6723(4) 0.0304(6) Uani 1 1 d .
F7 F 0.3833(3) 0.31341(15) 0.6509(3) 0.0217(5) Uani 1 1 d .
F8 F 0.5214(4) 0.21289(17) 0.5354(3) 0.0238(5) Uani 1 1 d .
F9 F 0.6388(3) 0.30423(15) 0.9238(3) 0.0214(5) Uani 1 1 d .
F10 F 0.7709(3) 0.20065(16) 0.8059(3) 0.0211(5) Uani 1 1 d .
Kr1 Kr 1.0000 0.0000 1.0000 0.02182(11) Uani 1 2 d S
F11 F 0.7796(4) 0.0357(2) 0.9263(5) 0.0363(8) Uani 1 1 d .
Kr2 Kr 0.08087(4) 0.18685(2) 0.73671(5) 0.01444(7) Uani 1 1 d .
F12 F -0.0486(3) 0.26375(17) 0.5979(4) 0.0251(5) Uani 1 1 d .
F13 F 0.2073(3) 0.10863(14) 0.8764(3) 0.0197(5) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 '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
O2 Hg1 O1 173.26(12) .
Te1 O1 Hg1 126.47(15) .
F1 Te1 F5 91.29(15) .
F1 Te1 F3 87.05(18) .
F5 Te1 F3 87.72(14) .
F1 Te1 O1 92.86(16) .
F5 Te1 O1 90.75(13) .
F3 Te1 O1 178.46(14) .
F1 Te1 F2 174.22(17) .
F5 Te1 F2 90.10(14) .
F3 Te1 F2 87.40(17) .
O1 Te1 F2 92.74(15) .
F1 Te1 F4 90.12(14) .
F5 Te1 F4 174.18(14) .
F3 Te1 F4 86.71(14) .
O1 Te1 F4 94.82(13) .
F2 Te1 F4 87.95(14) .
Te2 O2 Hg1 129.55(16) .
O2 Te2 F6 176.80(14) .
O2 Te2 F8 93.07(14) .
F6 Te2 F8 86.18(15) .
O2 Te2 F9 94.41(13) .
F6 Te2 F9 86.35(14) .
F8 Te2 F9 172.52(13) .
O2 Te2 F10 94.95(13) .
F6 Te2 F10 88.14(14) .
F8 Te2 F10 89.13(12) .
F9 Te2 F10 90.24(13) .
O2 Te2 F7 90.60(13) .
F6 Te2 F7 86.28(14) .
F8 Te2 F7 89.43(12) .
F9 Te2 F7 90.47(13) .
F10 Te2 F7 174.33(13) .
F11 Kr1 F11 180.000(1) 3_757
F12 Kr2 F13 178.89(11) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg1 O2 2.017(3) .
Hg1 O1 2.029(3) .
O1 Te1 1.836(3) .
Te1 F1 1.824(3) .
Te1 F5 1.829(3) .
Te1 F3 1.836(3) .
Te1 F2 1.836(3) .
Te1 F4 1.838(3) .
O2 Te2 1.819(3) .
Te2 F6 1.835(3) .
Te2 F8 1.837(3) .
Te2 F9 1.839(3) .
Te2 F10 1.844(2) .
Te2 F7 1.848(2) .
Kr1 F11 1.883(3) 3_757
Kr1 F11 1.883(3) .
Kr2 F12 1.885(3) .
Kr2 F13 1.897(3) .
