#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/97/2239786.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_2239786
loop_
_publ_author_name
'Harrison, William T. A.'
'Wardell, James L.'
_publ_section_title
;
 Crystal structures of potassium trifluorido(4-methoxyphenyl)borate and
 potassium trifluorido(4-fluorophenyl)borate
;
_journal_coeditor_code           WM0001
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              68
_journal_page_last               71
_journal_paper_doi               10.1107/S1600536814009684
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'K +, C7 H7 B F3 O -'
_chemical_formula_moiety         'K +, C7 H7 B F3 O -'
_chemical_formula_sum            'C7 H7 B F3 K O'
_chemical_formula_weight         214.04
_chemical_name_systematic
;
Potassium trifluorido(4-methoxyphenyl)borate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 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                   7.1347(2)
_cell_length_b                   17.2819(7)
_cell_length_c                   7.3289(3)
_cell_measurement_reflns_used    4830
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.2
_cell_volume                     903.66(6)
_computing_cell_refinement       'CrystalClear (Rigaku, 2010)'
_computing_data_collection       'CrystalClear (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear (Rigaku, 2010)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5789
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.18
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.9170
_exptl_absorpt_correction_T_min  0.7496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.199
_refine_ls_abs_structure_details 'Flack (1983), 712 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       0.0115(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1833
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0212
_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)+(0.0350P)²+0.1245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0590
_reflns_number_gt                1822
_reflns_number_total             1833
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm0001sup1.cif
_cod_data_source_block           I
_cod_database_code               2239786
_cod_database_fobs_code          2239786
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, 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 0.93636(3) 0.577078(16) 0.49116(4) 0.01659(9) Uani d . 1 1
C C1 0.48663(17) 0.69908(7) 0.3989(2) 0.0159(3) Uani d . 1 1
C C2 0.36313(18) 0.72309(8) 0.2628(2) 0.0195(3) Uani d . 1 1
H H2 0.2718 0.6875 0.2199 0.023 Uiso calc R 1 1
C C3 0.36757(18) 0.79722(8) 0.1867(2) 0.0223(3) Uani d . 1 1
H H3 0.2813 0.8114 0.0938 0.027 Uiso calc R 1 1
C C4 0.5004(2) 0.84983(8) 0.2493(2) 0.0208(3) Uani d . 1 1
C C5 0.62439(19) 0.82828(8) 0.3880(2) 0.0233(3) Uani d . 1 1
H H5 0.7139 0.8643 0.4324 0.028 Uiso calc R 1 1
C C6 0.61673(19) 0.75407(8) 0.4608(2) 0.0206(3) Uani d . 1 1
H H6 0.7018 0.7402 0.5549 0.025 Uiso calc R 1 1
C C7 0.3970(3) 0.94712(11) 0.0422(3) 0.0393(5) Uani d . 1 1
H H7A 0.4278 1.0000 0.0044 0.059 Uiso calc R 1 1
H H7B 0.2674 0.9454 0.0865 0.059 Uiso calc R 1 1
H H7C 0.4105 0.9121 -0.0622 0.059 Uiso calc R 1 1
B B1 0.48502(18) 0.61227(8) 0.4743(2) 0.0153(3) Uani d . 1 1
F F1 0.57562(10) 0.55930(5) 0.35081(13) 0.01754(18) Uani d . 1 1
F F2 0.30347(10) 0.58074(4) 0.50165(17) 0.02096(19) Uani d . 1 1
F F3 0.58402(11) 0.60460(5) 0.64078(13) 0.02023(19) Uani d . 1 1
O O1 0.52053(18) 0.92364(6) 0.1842(2) 0.0297(3) 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
F3 K1 F2 3_654 1_655 94.59(3)
F3 K1 F1 3_654 3_655 173.67(3)
F2 K1 F1 1_655 3_655 90.34(3)
F3 K1 F1 3_654 4_565 79.00(3)
F2 K1 F1 1_655 4_565 70.82(2)
F1 K1 F1 3_655 4_565 106.45(2)
F3 K1 F3 3_654 . 107.78(2)
F2 K1 F3 1_655 . 152.47(3)
F1 K1 F3 3_655 . 66.40(3)
F1 K1 F3 4_565 . 128.21(2)
F3 K1 F1 3_654 . 66.83(3)
F2 K1 F1 1_655 . 159.35(3)
F1 K1 F1 3_655 . 108.89(2)
F1 K1 F1 4_565 . 95.79(2)
F3 K1 F1 . . 47.98(3)
F3 K1 F2 3_654 4_565 100.35(3)
F2 K1 F2 1_655 4_565 110.489(19)
F1 K1 F2 3_655 4_565 81.59(3)
F1 K1 F2 4_565 4_565 47.24(3)
F3 K1 F2 . 4_565 81.63(2)
F1 K1 F2 . 4_565 66.60(3)
C2 C1 C6 . . 116.59(12)
C2 C1 B1 . . 121.46(12)
C6 C1 B1 . . 121.90(12)
C1 C2 C3 . . 122.95(12)
C1 C2 K1 . 3_654 86.24(8)
C3 C2 K1 . 3_654 114.99(10)
C1 C2 H2 . . 118.5
C3 C2 H2 . . 118.5
K1 C2 H2 3_654 . 68.1
C4 C3 C2 . . 118.88(13)
C4 C3 H3 . . 120.6
C2 C3 H3 . . 120.6
O1 C4 C3 . . 124.43(14)
O1 C4 C5 . . 115.78(13)
C3 C4 C5 . . 119.79(13)
C6 C5 C4 . . 119.99(13)
C6 C5 H5 . . 120.0
C4 C5 H5 . . 120.0
C5 C6 C1 . . 121.78(14)
C5 C6 H6 . . 119.1
C1 C6 H6 . . 119.1
O1 C7 H7A . . 109.5
O1 C7 H7B . . 109.5
H7A C7 H7B . . 109.5
O1 C7 H7C . . 109.5
H7A C7 H7C . . 109.5
H7B C7 H7C . . 109.5
F3 B1 F2 . . 107.30(13)
F3 B1 F1 . . 104.95(10)
F2 B1 F1 . . 104.73(10)
F3 B1 C1 . . 112.45(11)
F2 B1 C1 . . 114.56(11)
F1 B1 C1 . . 112.10(12)
B1 F1 K1 . 3_654 122.39(8)
B1 F1 K1 . 4_465 98.47(7)
K1 F1 K1 3_654 4_465 117.24(3)
B1 F1 K1 . . 96.46(7)
K1 F1 K1 3_654 . 112.53(3)
K1 F1 K1 4_465 . 106.81(3)
B1 F2 K1 . 1_455 156.48(8)
B1 F2 K1 . 4_465 93.39(6)
K1 F2 K1 1_455 4_465 107.73(2)
B1 F3 K1 . 3_655 146.64(8)
B1 F3 K1 . . 97.29(7)
K1 F3 K1 3_655 . 113.95(3)
C4 O1 C7 . . 117.09(13)
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
K1 F3 3_654 2.6156(10) y
K1 F2 1_655 2.6211(7) y
K1 F1 3_655 2.6550(10) y
K1 F1 4_565 2.7568(10) y
K1 F3 . 2.7836(8) y
K1 F1 . 2.7887(8) y
K1 F2 4_565 2.8885(8) y
K1 F3 4_565 3.4886(9) y
C1 C2 . 1.3940(19) ?
C1 C6 . 1.4036(18) ?
C1 B1 . 1.5987(18) ?
C2 C3 . 1.398(2) ?
C2 K1 3_654 3.5183(15) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.3910(19) ?
C3 H3 . 0.9500 ?
C4 O1 . 1.3696(17) ?
C4 C5 . 1.398(2) ?
C5 C6 . 1.390(2) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 O1 . 1.423(2) ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
B1 F3 . 1.4162(19) y
B1 F2 . 1.4196(14) y
B1 F1 . 1.4403(17) y
B1 K1 4_465 3.2930(14) ?
F1 K1 3_654 2.6550(10) ?
F1 K1 4_465 2.7568(10) ?
F2 K1 1_455 2.6211(7) ?
F2 K1 4_465 2.8885(8) ?
F3 K1 3_655 2.6157(10) ?
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
C2 H2 F2 3_554 0.95 2.50 3.3359(17) 147
C7 H7a O1 2_674 0.98 2.72 3.4960(10) 137
C3 H3 Cg1 3_554 0.95 2.85 3.7171(15) 152
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
C6 C1 C2 C3 . . 1.2(2)
B1 C1 C2 C3 . . -176.35(14)
C6 C1 C2 K1 . 3_654 118.72(12)
B1 C1 C2 K1 . 3_654 -58.84(12)
C1 C2 C3 C4 . . -0.2(2)
K1 C2 C3 C4 3_654 . -102.69(14)
C2 C3 C4 O1 . . 179.10(14)
C2 C3 C4 C5 . . -0.9(2)
O1 C4 C5 C6 . . -178.99(14)
C3 C4 C5 C6 . . 1.0(2)
C4 C5 C6 C1 . . 0.0(2)
C2 C1 C6 C5 . . -1.1(2)
B1 C1 C6 C5 . . 176.46(14)
C2 C1 B1 F3 . . -164.66(12)
C6 C1 B1 F3 . . 17.90(18)
C2 C1 B1 F2 . . -41.81(19)
C6 C1 B1 F2 . . 140.76(15)
C2 C1 B1 F1 . . 77.36(16)
C6 C1 B1 F1 . . -100.07(15)
C3 C4 O1 C7 . . -0.4(2)
C5 C4 O1 C7 . . 179.62(15)
