#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/57/2235772.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_2235772
loop_
_publ_author_name
'Lejon, Tore'
'Gorovoy, Alexey S.'
'Khrustalev, Victor N.'
_publ_section_title
;
 Potassium [(1S)-1-azido-2-phenylethyl]trifluoridoborate
;
_journal_coeditor_code           CV5318
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1048
_journal_paper_doi               10.1107/S1600536812030085
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'K +, C8 H8 B F3 N3 -'
_chemical_formula_moiety         'K +, C8 H8 B F3 N3 -'
_chemical_formula_sum            'C8 H8 B F3 K N3'
_chemical_formula_weight         253.08
_chemical_name_systematic
;
Potassium [(1S)-1-azido-2-phenylethyl]trifluoridoborate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.052(2)
_cell_length_b                   6.959(2)
_cell_length_c                   25.120(8)
_cell_measurement_reflns_used    546
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.45
_cell_measurement_theta_min      3.24
_cell_volume                     1058.0(6)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω 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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.1401
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10239
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.402
_refine_ls_abs_structure_details 'Flack (1983), 828 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0191P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                1203
_reflns_number_total             2075
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv5318.cif
_cod_data_source_block           I
_cod_original_cell_volume        1057.9(6)
_cod_database_code               2235772
_cod_database_fobs_code          2235772
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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
_atom_site_occupancy
_atom_site_symmetry_multiplicity
K K1 0.19352(19) 0.92096(16) 0.77175(5) 0.0230(3) Uani d . 1 1
N N1 0.4374(7) 0.6992(6) 0.85281(14) 0.0243(11) Uani d . 1 1
N N2 0.6381(7) 0.7035(6) 0.84172(15) 0.0224(11) Uani d . 1 1
N N3 0.8199(7) 0.7267(7) 0.83058(14) 0.0296(11) Uani d . 1 1
C C1 0.3397(8) 0.5009(6) 0.86075(17) 0.0187(12) Uani d . 1 1
H H1 0.1992 0.5194 0.8811 0.022 Uiso calc R 1 1
C C2 0.4850(8) 0.3714(6) 0.89471(16) 0.0206(13) Uani d . 1 1
H H2A 0.4156 0.2427 0.8965 0.025 Uiso calc R 1 1
H H2B 0.6294 0.3564 0.8766 0.025 Uiso calc R 1 1
C C3 0.5268(8) 0.4407(6) 0.95126(18) 0.0167(11) Uani d . 1 1
C C4 0.3648(8) 0.4141(7) 0.99013(17) 0.0215(12) Uani d . 1 1
H H4 0.2286 0.3546 0.9811 0.026 Uiso calc R 1 1
C C5 0.4030(8) 0.4748(7) 1.04210(19) 0.0227(13) Uani d . 1 1
H H5 0.2922 0.4575 1.0684 0.027 Uiso calc R 1 1
C C6 0.6016(8) 0.5603(7) 1.05561(19) 0.0231(12) Uani d . 1 1
H H6 0.6273 0.5998 1.0913 0.028 Uiso calc R 1 1
C C7 0.7647(8) 0.5888(7) 1.01697(18) 0.0236(12) Uani d . 1 1
H H7 0.9006 0.6489 1.0260 0.028 Uiso calc R 1 1
C C8 0.7250(8) 0.5283(6) 0.96550(18) 0.0219(13) Uani d . 1 1
H H8 0.8356 0.5469 0.9392 0.026 Uiso calc R 1 1
F F1 0.1942(4) 0.5408(3) 0.76697(10) 0.0241(7) Uani d . 1 1
F F2 0.0979(4) 0.2693(4) 0.81157(9) 0.0250(7) Uani d . 1 1
F F3 0.4491(4) 0.3061(4) 0.78057(9) 0.0270(7) Uani d . 1 1
B B1 0.2716(9) 0.4042(8) 0.8047(2) 0.0171(13) Uani d . 1 1
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
F1 K1 F3 . 3_656 71.05(9)
F1 K1 F1 . 3_556 107.25(7)
F3 K1 F1 3_656 3_556 128.98(8)
F1 K1 F2 . 1_565 156.77(10)
F3 K1 F2 3_656 1_565 129.20(9)
F1 K1 F2 3_556 1_565 70.42(8)
F1 K1 F2 . 3_556 66.99(8)
F3 K1 F2 3_656 3_556 91.61(8)
F1 K1 F2 3_556 3_556 47.55(7)
F2 K1 F2 1_565 3_556 117.46(7)
F1 K1 N1 . . 60.53(10)
F3 K1 N1 3_656 . 77.08(10)
F1 K1 N1 3_556 . 148.57(10)
F2 K1 N1 1_565 . 108.83(10)
F2 K1 N1 3_556 . 127.22(11)
F1 K1 N3 . 1_455 64.93(11)
F3 K1 N3 3_656 1_455 135.84(11)
F1 K1 N3 3_556 1_455 70.16(10)
F2 K1 N3 1_565 1_455 93.46(11)
F2 K1 N3 3_556 1_455 74.82(10)
N1 K1 N3 . 1_455 78.62(11)
F1 K1 F3 . 1_565 149.93(9)
F3 K1 F3 3_656 1_565 83.65(6)
F1 K1 F3 3_556 1_565 101.20(8)
F2 K1 F3 1_565 1_565 45.66(7)
F2 K1 F3 3_556 1_565 131.42(8)
N1 K1 F3 . 1_565 98.81(10)
N3 K1 F3 1_455 1_565 136.46(10)
F1 K1 N3 . 3_656 127.01(11)
F3 K1 N3 3_656 3_656 80.25(10)
F1 K1 N3 3_556 3_656 59.97(9)
F2 K1 N3 1_565 3_656 72.92(9)
F2 K1 N3 3_556 3_656 70.44(10)
N1 K1 N3 . 3_656 151.29(11)
N3 K1 N3 1_455 3_656 130.08(7)
F3 K1 N3 1_565 3_656 61.08(9)
N2 N1 C1 . . 115.6(4)
N2 N1 K1 . . 108.7(3)
C1 N1 K1 . . 111.8(3)
N3 N2 N1 . . 173.1(5)
N2 N3 K1 . 1_655 154.2(4)
N2 N3 K1 . 3_646 94.3(3)
K1 N3 K1 1_655 3_646 85.80(9)
N1 C1 C2 . . 112.8(4)
N1 C1 B1 . . 111.4(4)
C2 C1 B1 . . 112.9(4)
N1 C1 H1 . . 106.4
C2 C1 H1 . . 106.4
B1 C1 H1 . . 106.4
C3 C2 C1 . . 115.6(4)
C3 C2 H2A . . 108.4
C1 C2 H2A . . 108.4
C3 C2 H2B . . 108.4
C1 C2 H2B . . 108.4
H2A C2 H2B . . 107.4
C8 C3 C4 . . 118.9(4)
C8 C3 C2 . . 121.4(4)
C4 C3 C2 . . 119.7(4)
C5 C4 C3 . . 120.0(4)
C5 C4 H4 . . 120.0
C3 C4 H4 . . 120.0
C6 C5 C4 . . 120.3(5)
C6 C5 H5 . . 119.8
C4 C5 H5 . . 119.8
C5 C6 C7 . . 120.3(4)
C5 C6 H6 . . 119.9
C7 C6 H6 . . 119.9
C8 C7 C6 . . 118.9(4)
C8 C7 H7 . . 120.5
C6 C7 H7 . . 120.5
C7 C8 C3 . . 121.6(5)
C7 C8 H8 . . 119.2
C3 C8 H8 . . 119.2
B1 F1 K1 . . 129.7(3)
B1 F1 K1 . 3_546 108.9(3)
K1 F1 K1 . 3_546 109.06(9)
B1 F2 K1 . 1_545 113.1(3)
B1 F2 K1 . 3_546 96.9(3)
K1 F2 K1 1_545 3_546 100.87(8)
B1 F3 K1 . 3_646 133.5(3)
B1 F3 K1 . 1_545 94.0(3)
K1 F3 K1 3_646 1_545 129.14(10)
F3 B1 F2 . . 107.2(4)
F3 B1 F1 . . 106.7(4)
F2 B1 F1 . . 106.2(4)
F3 B1 C1 . . 112.5(4)
F2 B1 C1 . . 111.0(4)
F1 B1 C1 . . 112.7(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
K1 F1 . 2.648(3)
K1 F3 3_656 2.654(3)
K1 F1 3_556 2.673(3)
K1 F2 1_565 2.685(3)
K1 F2 3_556 2.933(3)
K1 N1 . 2.951(4)
K1 N3 1_455 3.020(4)
K1 F3 1_565 3.102(3)
K1 N3 3_656 3.338(4)
N1 N2 . 1.246(5)
N1 C1 . 1.515(6)
N2 N3 . 1.147(5)
C1 C2 . 1.521(6)
C1 B1 . 1.614(7)
C1 H1 . 1.0000
C2 C3 . 1.521(6)
C2 H2A . 0.9900
C2 H2B . 0.9900
C3 C8 . 1.392(6)
C3 C4 . 1.396(6)
C4 C5 . 1.391(6)
C4 H4 . 0.9500
C5 C6 . 1.383(6)
C5 H5 . 0.9500
C6 C7 . 1.399(6)
C6 H6 . 0.9500
C7 C8 . 1.381(6)
C7 H7 . 0.9500
C8 H8 . 0.9500
F1 B1 . 1.422(6)
F2 B1 . 1.420(6)
F3 B1 . 1.410(6)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C4 H4 C3 4_457 0.95 2.93 3.528(6) 122 yes
C4 H4 C4 4_457 0.95 2.98 3.823(6) 149 yes
C4 H4 C5 4_457 0.95 3.08 3.974(7) 158 yes
C4 H4 C6 4_457 0.95 3.13 3.841(7) 133 yes
C4 H4 C7 4_457 0.95 3.09 3.556(7) 112 yes
C4 H4 C8 4_457 0.95 2.98 3.382(6) 107 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
F1 K1 N1 N2 . . 101.9(3)
F3 K1 N1 N2 3_656 . 26.6(3)
F1 K1 N1 N2 3_556 . 176.1(3)
F2 K1 N1 N2 1_565 . -100.8(3)
F2 K1 N1 N2 3_556 . 108.6(3)
N3 K1 N1 N2 1_455 . 169.4(3)
F3 K1 N1 N2 1_565 . -54.8(3)
N3 K1 N1 N2 3_656 . -12.2(5)
F1 K1 N1 C1 . . -26.9(3)
F3 K1 N1 C1 3_656 . -102.3(3)
F1 K1 N1 C1 3_556 . 47.3(4)
F2 K1 N1 C1 1_565 . 130.4(3)
F2 K1 N1 C1 3_556 . -20.2(3)
N3 K1 N1 C1 1_455 . 40.6(3)
F3 K1 N1 C1 1_565 . 176.4(3)
N3 K1 N1 C1 3_656 . -141.0(3)
N2 N1 C1 C2 . . 44.7(5)
K1 N1 C1 C2 . . 169.7(3)
N2 N1 C1 B1 . . -83.6(5)
K1 N1 C1 B1 . . 41.5(4)
N1 C1 C2 C3 . . 61.4(5)
B1 C1 C2 C3 . . -171.2(4)
C1 C2 C3 C8 . . -101.8(5)
C1 C2 C3 C4 . . 79.0(5)
C8 C3 C4 C5 . . 0.0(7)
C2 C3 C4 C5 . . 179.2(4)
C3 C4 C5 C6 . . -0.5(7)
C4 C5 C6 C7 . . 0.9(7)
C5 C6 C7 C8 . . -0.8(7)
C6 C7 C8 C3 . . 0.3(7)
C4 C3 C8 C7 . . 0.1(7)
C2 C3 C8 C7 . . -179.0(4)
F3 K1 F1 B1 3_656 . 95.3(4)
F1 K1 F1 B1 3_556 . -138.5(4)
F2 K1 F1 B1 1_565 . -58.1(5)
F2 K1 F1 B1 3_556 . -164.4(4)
N1 K1 F1 B1 . . 9.8(4)
N3 K1 F1 B1 1_455 . -81.1(4)
F3 K1 F1 B1 1_565 . 61.1(4)
N3 K1 F1 B1 3_656 . 156.4(3)
F3 K1 F1 K1 3_656 3_546 -127.74(10)
F1 K1 F1 K1 3_556 3_546 -1.60(5)
F2 K1 F1 K1 1_565 3_546 78.8(3)
F2 K1 F1 K1 3_556 3_546 -27.48(8)
N1 K1 F1 K1 . 3_546 146.70(13)
N3 K1 F1 K1 1_455 3_546 55.89(11)
F3 K1 F1 K1 1_565 3_546 -161.99(14)
N3 K1 F1 K1 3_656 3_546 -66.63(15)
K1 F3 B1 F2 3_646 . 161.9(2)
K1 F3 B1 F2 1_545 . 2.3(4)
K1 F3 B1 F1 3_646 . 48.4(5)
K1 F3 B1 F1 1_545 . -111.2(3)
K1 F3 B1 C1 3_646 . -75.8(5)
K1 F3 B1 C1 1_545 . 124.6(4)
K1 F2 B1 F3 1_545 . -2.8(4)
K1 F2 B1 F3 3_546 . -107.8(3)
K1 F2 B1 F1 1_545 . 111.0(3)
K1 F2 B1 F1 3_546 . 6.1(4)
K1 F2 B1 C1 1_545 . -126.1(3)
K1 F2 B1 C1 3_546 . 128.9(3)
K1 F1 B1 F3 . . -115.8(3)
K1 F1 B1 F3 3_546 . 107.2(3)
K1 F1 B1 F2 . . 130.0(3)
K1 F1 B1 F2 3_546 . -7.0(4)
K1 F1 B1 C1 . . 8.2(6)
K1 F1 B1 C1 3_546 . -128.8(3)
N1 C1 B1 F3 . . 86.5(5)
C2 C1 B1 F3 . . -41.7(6)
N1 C1 B1 F2 . . -153.3(4)
C2 C1 B1 F2 . . 78.5(5)
N1 C1 B1 F1 . . -34.3(6)
C2 C1 B1 F1 . . -162.5(4)
