#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:07:55 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/80/7048052.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_7048052
loop_
_publ_author_name
'Saal, Thomas'
'Christe, Karl O.'
'Haiges, Ralf'
_publ_section_title
;
 Lewis adduct formation of hydrogen cyanide and nitriles with arsenic and
 antimony pentafluoride.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              99
_journal_page_last               106
_journal_paper_doi               10.1039/c8dt03970d
_journal_volume                  48
_journal_year                    2018
_chemical_formula_moiety         'C H As F5 N'
_chemical_formula_sum            'C H As F5 N'
_chemical_formula_weight         196.95
_chemical_name_common            AsF5HCN
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   difmap
_audit_update_record
;
2018-10-02 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.4973(15)
_cell_length_b                   5.4973(15)
_cell_length_c                   16.475(5)
_cell_measurement_reflns_used    5287
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.4454
_cell_measurement_theta_min      2.4726
_cell_volume                     497.9(2)
_computing_cell_refinement       'APEX3 v2018.1-0 (Bruker AXS, 2018)'
_computing_data_collection
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2013)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 882)'
_computing_publication_material  'SHELXTL XL 2017/1 (Bruker AXS, 2017)'
_computing_structure_refinement  'SHELXTL XL 2017/1 (Bruker AXS, 2017)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12048
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         3.91
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    6.836
_exptl_absorpt_correction_T_max  0.38
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.472
_refine_ls_abs_structure_details
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         762
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0167P)²+0.5235P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0567
_reflns_number_gt                673
_reflns_number_total             762
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03970d2.cif
_cod_data_source_block           HCNAsF5
_cod_depositor_comments
'Adding full bibliography for 7048050--7048060.cif.'
_cod_original_cell_volume        497.9(3)
_cod_database_code               7048052
_shelx_res_file
;

TITL final in P4(3)2(1)2
    final.res
    created by SHELXL-2017/1 at 11:17:01 on 01-Oct-2018
CELL 0.71073   5.49730   5.49730  16.47470  90.0000  90.0000  90.0000
ZERR    4.00   0.00150   0.00150   0.00460   0.0000   0.0000   0.0000
LATT -1
SYMM  -x, -y, 1/2+z
SYMM  1/2-y, 1/2+x, 1/4+z
SYMM  1/2+y, 1/2-x, 3/4+z
SYMM  1/2-x, 1/2+y, 1/4-z
SYMM  1/2+x, 1/2-y, 3/4-z
SYMM  +y, +x, -z
SYMM  -y, -x, 1/2-z
SFAC C H AS F N
UNIT 4 4 4 20 4
TEMP -173.150
SIZE 0.176 0.232 0.338
L.S. 10
ACTA 58
BOND $H
LIST 4
FMAP 2
DFIX 0.95 C1 H1
PLAN 5
TWIN
WGHT    0.016700    0.523500
BASF   0.48647
FVAR       0.18416
C1    1    0.102598    0.897402    0.250000    10.50000    0.02018    0.02018 =
         0.03035    0.00247    0.00247    0.00038
H1    2   -0.025440    1.025440    0.250000    10.50000   -1.20000
AS1   3    0.503716    0.496284    0.250000    10.50000    0.01828    0.01828 =
         0.01320    0.00090    0.00090    0.00657
F1    4    0.357194    0.366317    0.330014    11.00000    0.03580    0.03295 =
         0.02662    0.01382    0.00778    0.00628
F2    4    0.318380    0.343098    0.184554    11.00000    0.03778    0.02541 =
         0.02955   -0.01202   -0.00759    0.00439
F3    4    0.723948    0.276052    0.250000    10.50000    0.04435    0.04435 =
         0.02828    0.00600    0.00600    0.03294
N1    5    0.248689    0.751311    0.250000    10.50000    0.01763    0.01763 =
         0.01845   -0.00044   -0.00044    0.00113
HKLF 4




REM  final in P4(3)2(1)2
REM R1 =  0.0246 for     673 Fo > 4sig(Fo)  and  0.0288 for all     762 data
REM     41 parameters refined using      1 restraints

END

WGHT      0.0159      0.5646

REM Highest difference peak  0.329,  deepest hole -0.472,  1-sigma level  0.089
Q1    1  -0.1493  1.1493  0.2500  10.50000  0.05    0.33
Q2    1   0.3787  0.2345  0.3096  11.00000  0.05    0.26
Q3    1   0.3917  0.4034  0.1493  11.00000  0.05    0.24
Q4    1   0.9989  0.3586  0.3175  11.00000  0.05    0.24
Q5    1  -0.0256  1.1617  0.3212  11.00000  0.05    0.21
;
_shelx_res_checksum              78754
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
C C1 0.1026(5) 0.8974(5) 0.25 0.0236(8) Uani d T P DS 1
H H1 -0.025(3) 1.025(3) 0.25 0.028 Uiso d U P DS 1
As As1 0.50372(5) 0.49628(5) 0.25 0.01659(13) Uani d T P S 1
F F1 0.3572(5) 0.3663(4) 0.33001(11) 0.0318(4) Uani d . . . 1
F F2 0.3184(4) 0.3431(4) 0.18455(11) 0.0309(4) Uani d . . . 1
F F3 0.7239(3) 0.2761(3) 0.25 0.0390(8) Uani d T P S 1
N N1 0.2487(4) 0.7513(4) 0.25 0.0179(6) Uani d T P S 1
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
C1 0.0202(11) 0.0202(11) 0.030(2) 0.0004(15) 0.0025(14) 0.0025(14)
As1 0.01828(15) 0.01828(15) 0.01320(19) 0.00657(12) 0.00090(10) 0.00090(10)
F1 0.0358(12) 0.0329(12) 0.0266(8) 0.0063(9) 0.0078(9) 0.0138(9)
F2 0.0378(14) 0.0254(11) 0.0296(9) 0.0044(8) -0.0076(9) -0.0120(9)
F3 0.0444(12) 0.0444(12) 0.0283(14) 0.0329(15) 0.0060(15) 0.0060(15)
N1 0.0176(9) 0.0176(9) 0.0184(15) 0.0011(12) -0.0004(14) -0.0004(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'
N N 0.0061 0.0033 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 H1 . . 180.0
F1 As1 F1 . 8_665 175.7(2)
F1 As1 F2 . 8_665 89.70(10)
F1 As1 F2 8_665 8_665 89.98(10)
F1 As1 F2 . . 89.98(10)
F1 As1 F2 8_665 . 89.70(10)
F2 As1 F2 8_665 . 171.60(17)
F1 As1 F3 . . 92.17(10)
F1 As1 F3 8_665 . 92.17(10)
F2 As1 F3 8_665 . 94.20(9)
F2 As1 F3 . . 94.20(9)
F1 As1 N1 . . 87.83(10)
F1 As1 N1 8_665 . 87.83(10)
F2 As1 N1 8_665 . 85.80(9)
F2 As1 N1 . . 85.80(9)
F3 As1 N1 . . 180.00(2)
C1 N1 As1 . . 180.0(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.136(5)
C1 H1 . 1.00(2)
As1 F1 . 1.7020(17)
As1 F1 8_665 1.7021(17)
As1 F2 8_665 1.7058(18)
As1 F2 . 1.7058(18)
As1 F3 . 1.712(2)
As1 N1 . 1.983(3)
