 
data_jjh11
 
_audit_creation_method            SHELXL-2013

#===============================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name      'Prof. Dr. Jin-Xiao Mi'
_publ_contact_author_address
;
Engineering, College of Materials, 
Xiamen University, Xiamen 361005, 
Fujian Province, 
People¡¯s Republic of China
;
_publ_contact_author_phone     ' '
_publ_contact_author_fax       ' '
_publ_contact_author_email     'jxmi@xmu.edu.cn'
_publ_requested_journal         ?
_publ_requested_category        ?
_publ_requested_coeditor_name   ?
_publ_contact_letter
;
Aug. 29, 2016

Please consider this CIF submission for publication in Acta
Crystallographica Section C. All authors have seen and approved this
submission. The authors acknowledge the conditions of publication.

The CIF has passed the enCIFer(V1.1) checking.

Jin-Xiao MI
;
#=============================================================================== 

_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'B F K O4 P' 
_chemical_formula_weight          163.88

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'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 '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'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            9
_space_group_name_H-M_alt         'C c'
_space_group_name_Hall            'C -2yc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 'x, -y, z+1/2'
 'x+1/2, y+1/2, z'
 'x+1/2, -y+1/2, z+1/2'
 
_cell_length_a                    4.2917(9)
_cell_length_b                    7.8624(15)
_cell_length_c                    12.0505(19)
_cell_angle_alpha                 90
_cell_angle_beta                  90.44(3)
_cell_angle_gamma                 90
_cell_volume                      406.61(13)
_cell_formula_units_Z             4
_cell_measurement_temperature     203(2)
_cell_measurement_reflns_used     1249 
_cell_measurement_theta_min       1.690
_cell_measurement_theta_max       28.460 
 
_exptl_crystal_description        'tablet' 
_exptl_crystal_colour             'colorless' 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     2.677          
_exptl_crystal_F_000              320
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.200
_exptl_crystal_size_mid           0.200
_exptl_crystal_size_min           0.050
_exptl_absorpt_coefficient_mu     1.621
_shelx_estimated_absorpt_T_min    0.737
_shelx_estimated_absorpt_T_max    0.923
_exptl_absorpt_correction_type    multi-scan   
_exptl_absorpt_correction_T_min   0.635
_exptl_absorpt_correction_T_max   0.940 
_exptl_absorpt_process_details    'SMART (Bruker, 2001)' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       203(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_measurement_device_type   'Bruker Diffraction CCD area-detector'
_diffrn_measurement_method        
'1265 images,φ=0, 90, 180 degree, and Δω=0.3 degree, χ= 54.74 degree' 
_diffrn_detector_area_resol_mean  .
_diffrn_standards_number          0
_diffrn_standards_interval_count  .
_diffrn_standards_interval_time   .
_diffrn_standards_decay_%         . 
_diffrn_reflns_number             1249
_diffrn_reflns_av_unetI/netI      0.0718
_diffrn_reflns_av_R_equivalents   0.0728
_diffrn_reflns_limit_h_min        -5
_diffrn_reflns_limit_h_max        4
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          1.690
_diffrn_reflns_theta_max          28.460
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.976
_diffrn_measured_fraction_theta_full  0.984
_diffrn_reflns_Laue_measured_fraction_max    0.976
_diffrn_reflns_Laue_measured_fraction_full   0.984
_diffrn_reflns_point_group_measured_fraction_max   0.850
_diffrn_reflns_point_group_measured_fraction_full  0.901
_reflns_number_total              604
_reflns_number_gt                 578
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.733
_reflns_Friedel_fraction_max      0.723
_reflns_Friedel_fraction_full     0.816
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'SMART (Bruker, 2001)' 
_computing_cell_refinement        'SAINT (Bruker, 2001)' 
_computing_data_reduction         'SAINT (Bruker, 2001)' 
_computing_structure_solution     'SHELXS-2013 (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2015)'
_computing_molecular_graphics     
'DIAMOND (Brandenburg, 2011) and ATOMS (Dowty, 2004)' 
_computing_publication_material   
'SHELXL-2013 (Sheldrick, 2015)'
 
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.1389P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.019(3)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          604
_refine_ls_number_parameters      74
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0666
_refine_ls_R_factor_gt            0.0645
_refine_ls_wR_factor_ref          0.1856
_refine_ls_wR_factor_gt           0.1815
_refine_ls_goodness_of_fit_ref    1.093
_refine_ls_restrained_S_all       1.091
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
K1 K 0.1330(4) 0.3480(3) 0.3424(2) 0.0169(7) Uani 1 1 d . . . . .
P1 P 0.7180(5) 0.4835(3) 0.6223(2) 0.0095(7) Uani 1 1 d . . . . .
B1 B 0.225(3) 0.6597(15) 0.5421(11) 0.011(2) Uani 1 1 d . . . . .
F1 F 0.1021(18) 0.6732(9) 0.4333(6) 0.0187(16) Uani 1 1 d . . . . .
O1 O 0.467(2) 0.5319(10) 0.5329(7) 0.0147(17) Uani 1 1 d . . . . .
O2 O 0.9810(18) 0.6177(10) 0.6195(7) 0.0121(16) Uani 1 1 d . . . . .
O3 O 0.8694(19) 0.3206(9) 0.5740(8) 0.0155(18) Uani 1 1 d . . . . .
O4 O 0.603(2) 0.4691(10) 0.7369(8) 0.0183(18) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
K1 F1 2.666(8) 3_545 ?
K1 O2 2.772(9) 2_464 ?
K1 F1 2.785(7) . ?
K1 O4 2.792(9) 2_564 ?
K1 O4 2.802(9) 4_454 ?
K1 F1 2.884(8) 3_445 ?
K1 O4 2.968(9) 2_464 ?
K1 O3 3.027(9) 1_455 ?
K1 O1 3.060(9) . ?
K1 B1 3.333(12) 3_445 ?
K1 P1 3.448(4) 2_464 ?
K1 B1 3.455(13) . ?
P1 O4 1.474(9) . ?
P1 O2 1.546(8) . ?
P1 O3 1.552(8) . ?
P1 O1 1.566(9) . ?
P1 K1 3.448(4) 2_665 ?
P1 K1 3.738(4) 4 ?
B1 F1 1.414(14) . ?
B1 O2 1.447(15) 1_455 ?
B1 O1 1.449(15) . ?
B1 O3 1.458(14) 3_455 ?
B1 K1 3.333(12) 3 ?
F1 K1 2.666(8) 3_455 ?
F1 K1 2.884(8) 3 ?
O2 B1 1.447(15) 1_655 ?
O2 K1 2.772(9) 2_665 ?
O3 B1 1.458(14) 3_545 ?
O3 K1 3.027(9) 1_655 ?
O4 K1 2.792(9) 2_565 ?
O4 K1 2.802(9) 4 ?
O4 K1 2.968(9) 2_665 ?
 
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
F1 K1 O2 128.3(2) 3_545 2_464 ?
F1 K1 F1 110.5(3) 3_545 . ?
O2 K1 F1 106.3(2) 2_464 . ?
F1 K1 O4 84.6(2) 3_545 2_564 ?
O2 K1 O4 71.0(3) 2_464 2_564 ?
F1 K1 O4 75.1(2) . 2_564 ?
F1 K1 O4 76.1(2) 3_545 4_454 ?
O2 K1 O4 68.7(3) 2_464 4_454 ?
F1 K1 O4 173.4(3) . 4_454 ?
O4 K1 O4 106.4(3) 2_564 4_454 ?
F1 K1 F1 101.2(2) 3_545 3_445 ?
O2 K1 F1 103.5(2) 2_464 3_445 ?
F1 K1 F1 104.4(2) . 3_445 ?
O4 K1 F1 173.8(3) 2_564 3_445 ?
O4 K1 F1 73.4(2) 4_454 3_445 ?
F1 K1 O4 177.8(2) 3_545 2_464 ?
O2 K1 O4 50.5(2) 2_464 2_464 ?
F1 K1 O4 71.6(2) . 2_464 ?
O4 K1 O4 96.3(3) 2_564 2_464 ?
O4 K1 O4 101.8(3) 4_454 2_464 ?
F1 K1 O4 77.8(2) 3_445 2_464 ?
F1 K1 O3 82.6(2) 3_545 1_455 ?
O2 K1 O3 144.4(2) 2_464 1_455 ?
F1 K1 O3 71.6(2) . 1_455 ?
O4 K1 O3 137.1(3) 2_564 1_455 ?
O4 K1 O3 109.8(2) 4_454 1_455 ?
F1 K1 O3 46.7(2) 3_445 1_455 ?
O4 K1 O3 98.0(2) 2_464 1_455 ?
F1 K1 O1 65.6(2) 3_545 . ?
O2 K1 O1 141.8(2) 2_464 . ?
F1 K1 O1 45.1(2) . . ?
O4 K1 O1 76.3(3) 2_564 . ?
O4 K1 O1 141.3(3) 4_454 . ?
F1 K1 O1 107.9(2) 3_445 . ?
O4 K1 O1 116.4(2) 2_464 . ?
O3 K1 O1 61.2(2) 1_455 . ?
F1 K1 B1 82.7(3) 3_545 3_445 ?
O2 K1 B1 128.4(3) 2_464 3_445 ?
F1 K1 B1 95.6(3) . 3_445 ?
O4 K1 B1 160.5(3) 2_564 3_445 ?
O4 K1 B1 84.8(3) 4_454 3_445 ?
F1 K1 B1 25.0(3) 3_445 3_445 ?
O4 K1 B1 96.9(3) 2_464 3_445 ?
O3 K1 B1 25.9(3) 1_455 3_445 ?
O1 K1 B1 85.0(3) . 3_445 ?
F1 K1 P1 153.90(17) 3_545 2_464 ?
O2 K1 P1 25.98(16) 2_464 2_464 ?
F1 K1 P1 85.63(17) . 2_464 ?
O4 K1 P1 79.8(2) 2_564 2_464 ?
O4 K1 P1 88.4(2) 4_454 2_464 ?
F1 K1 P1 94.03(17) 3_445 2_464 ?
O4 K1 P1 25.16(17) 2_464 2_464 ?
O3 K1 P1 122.82(19) 1_455 2_464 ?
O1 K1 P1 129.18(16) . 2_464 ?
B1 K1 P1 117.1(2) 3_445 2_464 ?
F1 K1 B1 89.9(3) 3_545 . ?
O2 K1 B1 129.1(3) 2_464 . ?
F1 K1 B1 23.2(2) . . ?
O4 K1 B1 82.7(3) 2_564 . ?
O4 K1 B1 162.2(3) 4_454 . ?
F1 K1 B1 99.2(3) 3_445 . ?
O4 K1 B1 92.2(3) 2_464 . ?
O3 K1 B1 56.6(2) 1_455 . ?
O1 K1 B1 24.8(3) . . ?
B1 K1 B1 82.5(3) 3_445 . ?
P1 K1 B1 108.6(2) 2_464 . ?
O4 P1 O2 108.8(5) . . ?
O4 P1 O3 115.6(5) . . ?
O2 P1 O3 104.3(4) . . ?
O4 P1 O1 115.5(5) . . ?
O2 P1 O1 108.6(5) . . ?
O3 P1 O1 103.3(5) . . ?
O4 P1 K1 58.9(4) . 2_665 ?
O2 P1 K1 51.8(3) . 2_665 ?
O3 P1 K1 113.0(4) . 2_665 ?
O1 P1 K1 141.7(3) . 2_665 ?
O4 P1 K1 41.1(3) . 4 ?
O2 P1 K1 124.5(3) . 4 ?
O3 P1 K1 74.6(3) . 4 ?
O1 P1 K1 126.0(3) . 4 ?
K1 P1 K1 76.99(7) 2_665 4 ?
F1 B1 O2 110.3(9) . 1_455 ?
F1 B1 O1 104.1(9) . . ?
O2 B1 O1 114.4(9) 1_455 . ?
F1 B1 O3 109.5(8) . 3_455 ?
O2 B1 O3 109.6(10) 1_455 3_455 ?
O1 B1 O3 108.6(10) . 3_455 ?
F1 B1 K1 59.5(5) . 3 ?
O2 B1 K1 162.5(8) 1_455 3 ?
O1 B1 K1 82.7(6) . 3 ?
O3 B1 K1 65.2(6) 3_455 3 ?
F1 B1 K1 50.7(5) . . ?
O2 B1 K1 102.0(6) 1_455 . ?
O1 B1 K1 62.2(6) . . ?
O3 B1 K1 147.7(8) 3_455 . ?
K1 B1 K1 82.5(3) 3 . ?
B1 F1 K1 134.0(6) . 3_455 ?
B1 F1 K1 106.1(6) . . ?
K1 F1 K1 110.5(3) 3_455 . ?
B1 F1 K1 95.6(6) . 3 ?
K1 F1 K1 101.2(2) 3_455 3 ?
K1 F1 K1 104.4(2) . 3 ?
B1 O1 P1 127.2(8) . . ?
B1 O1 K1 93.1(7) . . ?
P1 O1 K1 135.9(4) . . ?
B1 O2 P1 134.6(8) 1_655 . ?
B1 O2 K1 115.9(7) 1_655 2_665 ?
P1 O2 K1 102.2(4) . 2_665 ?
B1 O3 P1 129.6(8) 3_545 . ?
B1 O3 K1 88.8(7) 3_545 1_655 ?
P1 O3 K1 116.6(4) . 1_655 ?
P1 O4 K1 129.5(5) . 2_565 ?
P1 O4 K1 118.6(5) . 4 ?
K1 O4 K1 106.4(3) 2_565 4 ?
P1 O4 K1 95.9(4) . 2_665 ?
K1 O4 K1 96.3(3) 2_565 2_665 ?
K1 O4 K1 101.8(3) 4 2_665 ?
 
_refine_diff_density_max    1.493
_refine_diff_density_min   -0.804
_refine_diff_density_rms    0.292

_shelxl_version_number 2013-2



