#------------------------------------------------------------------------------
#$Date: 2022-07-26 00:53:15 +0300 (Tue, 26 Jul 2022) $
#$Revision: 276922 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/03/7130388.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_7130388
loop_
_publ_author_name
'Li, Yang'
'Chen, Xinglong'
'Ok, Kang Min'
_publ_section_title
;
 KF·B(OH)3: a KBBF-type material with large birefringence and
 remarkable deep-ultraviolet transparency
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03495F
_journal_year                    2022
_chemical_formula_moiety         'B H3 O3. F. K'
_chemical_formula_sum            'B F H3 K O3'
_chemical_formula_weight         119.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-17 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.4454(3)
_cell_length_b                   10.6284(7)
_cell_length_c                   7.0024(4)
_cell_measurement_reflns_used    7511
_cell_measurement_temperature    297.15
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      3.74
_cell_volume                     405.27(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      297.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15066
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_min         3.742
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0604 before and 0.0490 after correction.
The Ratio of minimum to maximum transmission is 0.9001.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_description       block
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.297
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.297
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0236
_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)+(0.0201P)²+0.1742P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0556
_reflns_Friedel_coverage         0.000
_reflns_number_gt                511
_reflns_number_total             547
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc03495f2.cif
_cod_data_source_block           1_pl
_cod_database_code               7130388
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.836
_olex2_refinement_description
;
1.a Riding coordinates:
 O1(H1), O3(H3), O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.4576(2) 0.42825(12) 0.250000 0.0239(3) Uani 1 2 d S T P . .
H1 H 0.528877 0.495604 0.250000 0.049(8) Uiso 1 2 d R . P . .
O3 O 0.0570(2) 0.34343(12) 0.250000 0.0262(3) Uani 1 2 d S T P . .
H3 H 0.133694 0.286304 0.250000 0.047(9) Uiso 1 2 d R . P . .
O2 O 0.1208(2) 0.56537(12) 0.250000 0.0292(4) Uani 1 2 d S T P . .
H2 H -0.019720 0.579342 0.250000 0.055(9) Uiso 1 2 d R . P . .
B1 B 0.2087(4) 0.4450(2) 0.250000 0.0197(4) Uani 1 2 d S T P . .
F1 F 0.32773(19) 0.14199(10) 0.250000 0.0295(3) Uani 1 2 d S T P . .
K1 K 0.66251(7) 0.250000 0.000000 0.02272(14) Uani 1 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
H H 0.0000 0.0000 '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'
O O 0.0106 0.0060 '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
B1 O1 H1 111.0 . . ?
B1 O1 K1 118.79(8) . 6_556 ?
B1 O1 K1 118.79(8) . . ?
K1 O1 H1 113.8 6_556 . ?
K1 O1 H1 113.8 . . ?
K1 O1 K1 77.05(3) 6_556 . ?
B1 O3 H3 108.0 . . ?
B1 O3 K1 135.34(6) . 6_456 ?
B1 O3 K1 135.34(6) . 1_455 ?
K1 O3 H3 97.8 1_455 . ?
K1 O3 H3 97.8 6_456 . ?
K1 O3 K1 72.99(3) 1_455 6_456 ?
B1 O2 H2 121.5 . . ?
B1 O2 K1 119.60(8) . 5_665 ?
B1 O2 K1 119.60(8) . 2_665 ?
K1 O2 H2 105.8 2_665 . ?
K1 O2 H2 105.8 5_665 . ?
K1 O2 K1 74.79(3) 2_665 5_665 ?
O3 B1 O1 119.92(17) . . ?
O3 B1 O2 122.05(17) . . ?
O2 B1 O1 118.03(17) . . ?
K1 F1 K1 78.19(3) 6_556 . ?
O1 K1 O1 133.21(5) . 3 ?
O1 K1 O3 72.05(3) . 1_655 ?
O1 K1 O3 72.05(3) 3 3_655 ?
O1 K1 O3 152.57(4) . 3_655 ?
O1 K1 O3 152.57(4) 3 1_655 ?
O1 K1 O2 94.70(3) 3 7_655 ?
O1 K1 O2 104.08(2) . 7_655 ?
O1 K1 O2 94.70(3) . 5_665 ?
O1 K1 O2 104.08(2) 3 5_665 ?
O1 K1 K1 51.474(16) . 6_556 ?
O1 K1 K1 51.475(16) 3 6 ?
O1 K1 K1 128.525(16) . 6 ?
O1 K1 K1 128.525(16) 3 6_556 ?
O3 K1 O3 86.27(4) 1_655 3_655 ?
O3 K1 K1 126.493(16) 1_655 6 ?
O3 K1 K1 53.508(16) 1_655 6_556 ?
O3 K1 K1 126.493(15) 3_655 6_556 ?
O3 K1 K1 53.508(15) 3_655 6 ?
O2 K1 O3 80.37(3) 7_655 3_655 ?
O2 K1 O3 64.51(3) 7_655 1_655 ?
O2 K1 O3 64.51(3) 5_665 3_655 ?
O2 K1 O3 80.37(3) 5_665 1_655 ?
O2 K1 O2 131.66(5) 5_665 7_655 ?
O2 K1 K1 127.398(16) 5_665 6_556 ?
O2 K1 K1 52.603(16) 5_665 6 ?
O2 K1 K1 52.603(16) 7_655 6_556 ?
O2 K1 K1 127.398(16) 7_655 6 ?
F1 K1 O1 81.56(2) 3 . ?
F1 K1 O1 67.99(3) . . ?
F1 K1 O1 81.56(2) . 3 ?
F1 K1 O1 67.99(3) 3 3 ?
F1 K1 O3 104.10(2) . 1_655 ?
F1 K1 O3 135.62(3) . 3_655 ?
F1 K1 O3 104.10(2) 3 3_655 ?
F1 K1 O3 135.62(3) 3 1_655 ?
F1 K1 O2 158.98(4) 3 7_655 ?
F1 K1 O2 66.69(3) 3 5_665 ?
F1 K1 O2 66.69(3) . 7_655 ?
F1 K1 O2 158.98(4) . 5_665 ?
F1 K1 F1 97.90(4) . 3 ?
F1 K1 K1 129.097(15) . 6 ?
F1 K1 K1 129.097(15) 3 6_556 ?
F1 K1 K1 50.903(15) . 6_556 ?
F1 K1 K1 50.903(15) 3 6 ?
K1 K1 K1 180.0 6_556 6 ?
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
O1 H1 0.8143 . ?
O1 B1 1.367(2) . ?
O1 K1 2.8106(10) 6_556 ?
O1 K1 2.8106(10) . ?
O3 H3 0.7371 . ?
O3 B1 1.360(2) . ?
O3 K1 2.9436(11) 6_456 ?
O3 K1 2.9436(11) 1_455 ?
O2 H2 0.7792 . ?
O2 B1 1.366(2) . ?
O2 K1 2.8824(11) 2_665 ?
O2 K1 2.8824(11) 5_665 ?
F1 K1 2.7759(9) 6_556 ?
F1 K1 2.7759(9) . ?
K1 K1 3.5012(2) 6_556 ?
K1 K1 3.5012(2) 6 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 F1 0.81 1.74 2.5549(17) 178.2 4_655 yes
O3 H3 F1 0.74 1.86 2.5995(17) 180.0 . yes
O2 H2 F1 0.78 1.80 2.5743(17) 169.3 4 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K1 O1 B1 O3 45.30(6) . . . . ?
K1 O1 B1 O3 -45.30(6) 6_556 . . . ?
K1 O1 B1 O2 -134.70(6) . . . . ?
K1 O1 B1 O2 134.70(6) 6_556 . . . ?
K1 O3 B1 O1 -122.20(11) 1_455 . . . ?
K1 O3 B1 O1 122.20(11) 6_456 . . . ?
K1 O3 B1 O2 -57.80(11) 6_456 . . . ?
K1 O3 B1 O2 57.80(11) 1_455 . . . ?
K1 O2 B1 O1 -44.31(5) 2_665 . . . ?
K1 O2 B1 O1 44.31(5) 5_665 . . . ?
K1 O2 B1 O3 135.69(5) 2_665 . . . ?
K1 O2 B1 O3 -135.69(5) 5_665 . . . ?
