 
data_yar
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'B5 H4 K O10' 
_chemical_formula_weight          257.18

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0106   0.0060
 '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'
 'K'  'K'   0.2009   0.2494
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    9.47340(18)
_cell_length_b                    7.52030(16)
_cell_length_c                    11.4205(2)
_cell_angle_alpha                 90
_cell_angle_beta                  97.3002(17)
_cell_angle_gamma                 90
_cell_volume                      807.03(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     6804
_cell_measurement_theta_min       3.2410 
_cell_measurement_theta_max       32.1870
 
_exptl_crystal_description        'irregular'
_exptl_crystal_colour             'colourless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.117          
_exptl_crystal_F_000              512
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.2652
_exptl_crystal_size_mid           0.2581
_exptl_crystal_size_min           0.1873
_exptl_absorpt_coefficient_mu     0.699
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.97170
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details    
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01) 
; 
_exptl_absorpt_special_details    
; 
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
; 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'
_diffrn_measurement_device_type   'Xcalibur, Sapphire3'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  16.0630
_diffrn_reflns_number             15711
_diffrn_reflns_av_unetI/netI      0.0277
_diffrn_reflns_av_R_equivalents   0.0442
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          3.252
_diffrn_reflns_theta_max          30.499
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              2464
_reflns_number_gt                 2220
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0257P)²+0.4098P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refall
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.0158(17)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          2464
_refine_ls_number_parameters      162
_refine_ls_number_restraints      5
_refine_ls_R_factor_all           0.0394
_refine_ls_R_factor_gt            0.0336
_refine_ls_wR_factor_ref          0.0737
_refine_ls_wR_factor_gt           0.0711
_refine_ls_goodness_of_fit_ref    1.111
_refine_ls_restrained_S_all       1.110
_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 0.32672(4) 0.43043(5) 0.26804(3) 0.02495(10) Uani 1 1 d . . . . .
O1 O 0.45849(10) 0.19876(13) 0.01776(8) 0.01315(19) Uani 1 1 d . . . . .
O2 O 0.63832(10) 0.40612(13) -0.00853(8) 0.0135(2) Uani 1 1 d . . . . .
O3 O 0.81700(11) 0.60402(14) 0.95840(9) 0.0171(2) Uani 1 1 d D . . . .
O4 O 0.60320(10) 0.31809(13) 0.18617(8) 0.0154(2) Uani 1 1 d . . . . .
O5 O 0.77458(10) 0.54786(13) 0.15724(8) 0.0144(2) Uani 1 1 d . . . . .
O6 O 0.61882(10) 0.57767(13) 0.30691(8) 0.0147(2) Uani 1 1 d . . . . .
O7 O 0.80982(10) 0.36331(14) 0.32830(8) 0.0146(2) Uani 1 1 d . . . . .
O8 O 0.73337(10) 0.50008(13) 0.49835(8) 0.0135(2) Uani 1 1 d . . . . .
O9 O 0.93297(11) 0.30529(15) 0.51540(9) 0.0186(2) Uani 1 1 d D . . . .
O10 O 0.94258(12) 0.09249(16) 0.23519(9) 0.0232(2) Uani 1 1 d D . . . .
B1 B 0.56696(15) 0.3086(2) 0.06854(13) 0.0111(3) Uani 1 1 d . . . . .
B2 B 0.74642(15) 0.5204(2) 0.03927(13) 0.0122(3) Uani 1 1 d . . . . .
B3 B 0.70120(15) 0.4510(2) 0.24462(12) 0.0123(3) Uani 1 1 d . . . . .
B4 B 0.63126(15) 0.5931(2) 0.42519(12) 0.0113(3) Uani 1 1 d . . . . .
B5 B 0.82576(16) 0.3889(2) 0.44642(13) 0.0121(3) Uani 1 1 d . . . . .
H3 H 0.8894(16) 0.666(3) 0.9841(18) 0.040(6) Uiso 1 1 d D . . . .
H9 H 0.934(2) 0.336(3) 0.5864(10) 0.043(6) Uiso 1 1 d D . . . .
H10A H 0.912(2) 0.175(2) 0.2760(16) 0.040(6) Uiso 1 1 d D . . . .
H10B H 1.0240(14) 0.062(3) 0.2680(19) 0.052(7) Uiso 1 1 d 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 O3 2.7774(10) 3_666 ?
K1 O10 2.8234(12) 2_655 ?
K1 O8 2.8463(9) 3_666 ?
K1 O6 2.8545(11) 2_645 ?
K1 O6 2.9611(11) . ?
K1 O4 3.0116(11) . ?
K1 O4 3.0208(11) 2_655 ?
K1 O1 3.1194(10) 4_566 ?
K1 O5 3.1835(11) 2_645 ?
K1 O2 3.2640(10) 3_665 ?
K1 B4 3.4188(15) 2_645 ?
K1 B4 3.4240(15) . ?
O1 B4 1.3856(17) 2_645 ?
O1 B1 1.3867(17) . ?
O2 B1 1.3860(17) . ?
O2 B2 1.3939(17) . ?
O3 B2 1.3612(17) 1_556 ?
O3 H3 0.849(10) . ?
O4 B1 1.3456(17) . ?
O4 B3 1.4659(17) . ?
O5 B2 1.3556(17) . ?
O5 B3 1.4785(17) . ?
O6 B4 1.3459(16) . ?
O6 B3 1.4710(17) . ?
O7 B5 1.3520(17) . ?
O7 B3 1.4687(17) . ?
O8 B4 1.3847(16) . ?
O8 B5 1.3959(17) . ?
O9 B5 1.3580(17) . ?
O9 H9 0.843(9) . ?
O10 H10A 0.847(9) . ?
O10 H10B 0.845(9) . ?
 
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
O3 K1 O10 72.11(3) 3_666 2_655 ?
O3 K1 O8 139.21(3) 3_666 3_666 ?
O10 K1 O8 69.20(3) 2_655 3_666 ?
O3 K1 O6 73.74(3) 3_666 2_645 ?
O10 K1 O6 126.49(3) 2_655 2_645 ?
O8 K1 O6 121.13(3) 3_666 2_645 ?
O3 K1 O6 120.84(3) 3_666 . ?
O10 K1 O6 131.77(3) 2_655 . ?
O8 K1 O6 94.89(3) 3_666 . ?
O6 K1 O6 101.04(2) 2_645 . ?
O3 K1 O4 91.58(3) 3_666 . ?
O10 K1 O4 159.57(3) 2_655 . ?
O8 K1 O4 128.90(3) 3_666 . ?
O6 K1 O4 56.55(3) 2_645 . ?
O6 K1 O4 47.03(3) . . ?
O3 K1 O4 108.79(3) 3_666 2_655 ?
O10 K1 O4 76.35(3) 2_655 2_655 ?
O8 K1 O4 74.12(3) 3_666 2_655 ?
O6 K1 O4 154.78(3) 2_645 2_655 ?
O6 K1 O4 55.42(3) . 2_655 ?
O4 K1 O4 98.27(2) . 2_655 ?
O3 K1 O1 156.08(3) 3_666 4_566 ?
O10 K1 O1 113.72(3) 2_655 4_566 ?
O8 K1 O1 45.95(3) 3_666 4_566 ?
O6 K1 O1 85.30(3) 2_645 4_566 ?
O6 K1 O1 73.84(3) . 4_566 ?
O4 K1 O1 86.20(3) . 4_566 ?
O4 K1 O1 95.09(3) 2_655 4_566 ?
O3 K1 O5 92.09(3) 3_666 2_645 ?
O10 K1 O5 95.22(3) 2_655 2_645 ?
O8 K1 O5 79.14(3) 3_666 2_645 ?
O6 K1 O5 46.58(3) 2_645 2_645 ?
O6 K1 O5 127.27(3) . 2_645 ?
O4 K1 O5 97.67(3) . 2_645 ?
O4 K1 O5 153.24(3) 2_655 2_645 ?
O1 K1 O5 64.70(3) 4_566 2_645 ?
O3 K1 O2 44.27(3) 3_666 3_665 ?
O10 K1 O2 91.23(3) 2_655 3_665 ?
O8 K1 O2 146.87(3) 3_666 3_665 ?
O6 K1 O2 91.99(3) 2_645 3_665 ?
O6 K1 O2 78.15(3) . 3_665 ?
O4 K1 O2 68.36(3) . 3_665 ?
O4 K1 O2 75.42(3) 2_655 3_665 ?
O1 K1 O2 150.74(3) 4_566 3_665 ?
O5 K1 O2 130.73(3) 2_645 3_665 ?
O3 K1 B4 54.08(3) 3_666 2_645 ?
O10 K1 B4 119.41(3) 2_655 2_645 ?
O8 K1 B4 142.64(3) 3_666 2_645 ?
O6 K1 B4 22.56(3) 2_645 2_645 ?
O6 K1 B4 101.01(3) . 2_645 ?
O4 K1 B4 54.14(3) . 2_645 ?
O4 K1 B4 141.89(3) 2_655 2_645 ?
O1 K1 B4 107.04(3) 4_566 2_645 ?
O5 K1 B4 64.29(3) 2_645 2_645 ?
O2 K1 B4 70.11(3) 3_665 2_645 ?
O3 K1 B4 143.33(3) 3_666 . ?
O10 K1 B4 123.53(4) 2_655 . ?
O8 K1 B4 72.46(3) 3_666 . ?
O6 K1 B4 108.47(3) 2_645 . ?
O6 K1 B4 22.89(3) . . ?
O4 K1 B4 63.57(3) . . ?
O4 K1 B4 54.02(3) 2_655 . ?
O1 K1 B4 54.51(3) 4_566 . ?
O5 K1 B4 116.42(3) 2_645 . ?
O2 K1 B4 99.52(3) 3_665 . ?
B4 K1 B4 116.36(3) 2_645 . ?
B4 O1 B1 127.69(11) 2_645 . ?
B4 O1 K1 93.04(7) 2_645 4_565 ?
B1 O1 K1 139.20(8) . 4_565 ?
B1 O2 B2 118.09(11) . . ?
B1 O2 K1 152.86(8) . 3_665 ?
B2 O2 K1 88.24(7) . 3_665 ?
B2 O3 K1 111.33(8) 1_556 3_666 ?
B2 O3 H3 117.6(15) 1_556 . ?
K1 O3 H3 130.7(15) 3_666 . ?
B1 O4 B3 123.87(11) . . ?
B1 O4 K1 101.73(8) . . ?
B3 O4 K1 101.12(7) . . ?
B1 O4 K1 98.29(8) . 2_645 ?
B3 O4 K1 117.82(8) . 2_645 ?
K1 O4 K1 113.43(3) . 2_645 ?
B2 O5 B3 123.06(11) . . ?
B2 O5 K1 112.10(8) . 2_655 ?
B3 O5 K1 94.63(7) . 2_655 ?
B4 O6 B3 123.84(11) . . ?
B4 O6 K1 103.00(8) . 2_655 ?
B3 O6 K1 109.25(8) . 2_655 ?
B4 O6 K1 98.26(8) . . ?
B3 O6 K1 103.20(7) . . ?
K1 O6 K1 120.24(3) 2_655 . ?
B5 O7 B3 124.44(11) . . ?
B4 O8 B5 118.28(11) . . ?
B4 O8 K1 105.38(7) . 3_666 ?
B5 O8 K1 135.98(8) . 3_666 ?
B5 O9 H9 110.2(16) . . ?
K1 O10 H10A 87.4(15) 2_645 . ?
K1 O10 H10B 131.4(17) 2_645 . ?
H10A O10 H10B 107.8(17) . . ?
O4 B1 O2 121.52(12) . . ?
O4 B1 O1 122.05(12) . . ?
O2 B1 O1 116.42(11) . . ?
O4 B1 K1 59.21(7) . 2_645 ?
O2 B1 K1 129.93(9) . 2_645 ?
O1 B1 K1 83.46(7) . 2_645 ?
O4 B1 K1 56.42(7) . . ?
O2 B1 K1 132.62(9) . . ?
O1 B1 K1 85.44(7) . . ?
K1 B1 K1 91.85(3) 2_645 . ?
O5 B2 O3 123.52(12) . 1_554 ?
O5 B2 O2 121.69(12) . . ?
O3 B2 O2 114.77(12) 1_554 . ?
O5 B2 K1 165.17(10) . 3_665 ?
O3 B2 K1 47.49(6) 1_554 3_665 ?
O2 B2 K1 68.37(7) . 3_665 ?
O4 B3 O7 109.94(11) . . ?
O4 B3 O6 108.51(11) . . ?
O7 B3 O6 110.30(10) . . ?
O4 B3 O5 110.70(10) . . ?
O7 B3 O5 108.05(11) . . ?
O6 B3 O5 109.34(11) . . ?
O6 B4 O8 121.84(12) . . ?
O6 B4 O1 122.72(12) . 2_655 ?
O8 B4 O1 115.43(11) . 2_655 ?
O6 B4 K1 54.44(7) . 2_655 ?
O8 B4 K1 129.38(9) . 2_655 ?
O1 B4 K1 90.37(8) 2_655 2_655 ?
O6 B4 K1 58.85(7) . . ?
O8 B4 K1 127.84(9) . . ?
O1 B4 K1 85.69(7) 2_655 . ?
K1 B4 K1 94.94(4) 2_655 . ?
O6 B4 K1 172.01(10) . 3_666 ?
O8 B4 K1 52.06(6) . 3_666 ?
O1 B4 K1 63.53(6) 2_655 3_666 ?
K1 B4 K1 132.82(4) 2_655 3_666 ?
K1 B4 K1 119.38(4) . 3_666 ?
O7 B5 O9 119.56(12) . . ?
O7 B5 O8 120.84(12) . . ?
O9 B5 O8 119.60(12) . . ?
 
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
O3 H3 O9  0.849(10) 1.983(12) 2.7948(14) 160(2) 2_756 yes
O9 H9 O10  0.843(9) 1.773(10) 2.6156(15) 177(2) 4_566 yes
O10 H10A O7  0.847(9) 1.859(10) 2.6835(15) 164(2) . yes
O10 H10B O5  0.845(9) 1.992(11) 2.8222(14) 167(2) 2_745 yes
 
_refine_diff_density_max    0.307
_refine_diff_density_min   -0.482
_refine_diff_density_rms    0.061



