# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

data_added_by_encifer
#------------------ SUBMISSION DETAILS --------------------------------------#

# Name and address of author for correspondence

_publ_contact_author_name        'Ning Ye'
_publ_contact_author_address     
;
Fujian Institute of Research on the Structure of Matter,
Chinese Academy of Sciences
Fuzhou, Fujian
350002
People's Republic of China
;
_publ_contact_author_email       nye@fjirsm.ac.cn
_publ_contact_author_fax         +86-591-83776076
_publ_contact_author_phone       +86-591-83776076
_publ_requested_journal          CrystEngComm


#------------------ TITLE AND AUTHOR LIST------------------------------------#

_publ_section_title              
;

;
loop_
_publ_author_name
;
Shichao Wang, Ning Ye and Guohong Zou
;
_publ_author_address             
;
Fujian Institute of Research on the Structure of Matter,
Chinese Academy of Sciences
Fuzhou, Fujian
350002
People's Republic of China
;

data_KBe4B3O9_P2/c

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_analytical     ?
_chemical_formula_sum            'B3 Be4 K O9'
_chemical_formula_weight         251.57

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2/c
_symmetry_Int_Tables_number      13
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   6.065(3)
_cell_length_b                   4.463(2)
_cell_length_c                   11.550(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.081(6)
_cell_angle_gamma                90
_cell_volume                     312.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    864
_cell_measurement_theta_min      3.359
_cell_measurement_theta_max      27.3411

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Prism
_exptl_crystal_colour            White
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    2.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             244
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8585
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 14.6306
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_ub_11      0.0289
_diffrn_orient_matrix_ub_12      0.1233
_diffrn_orient_matrix_ub_13      0.1056
_diffrn_orient_matrix_ub_21      -0.2163
_diffrn_orient_matrix_ub_22      0.0007
_diffrn_orient_matrix_ub_23      0.0584
_diffrn_orient_matrix_ub_31      0.0167
_diffrn_orient_matrix_ub_32      -0.0576
_diffrn_orient_matrix_ub_33      0.0625
_diffrn_measurement_device       
;
        Mercury70 (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_reflns_av_R_equivalents  0.0115
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_number            2108
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.36
_diffrn_reflns_theta_max         27.35
_diffrn_reflns_theta_full        27.35
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_reflns_number_total             705
_reflns_number_gt                678
_reflns_threshold_expression     >2sigma(I)
_diffrn_reflns_reduction_process 'Lp corrections applied'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0230P)²+0.2516P] where P=(Fo²+2Fc²)/3'
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.054(10)
_refine_ls_number_reflns         705
_refine_ls_number_parameters     81
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.02
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0548
_refine_ls_wR_factor_gt          0.0544
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.053

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Be Be 0.0005 0.0002 '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'
O O 0.0106 0.006 '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_
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0 0.25958(9) 0.25 0.01177(16) Uani 1 2 d S . .
Be1 Be 0.5199(3) 0.3393(4) 0.37289(13) 0.0061(3) Uani 1 1 d . . .
Be2 Be -0.2304(3) 0.8250(4) 0.43886(13) 0.0062(3) Uani 1 1 d . . .
B1 B -0.5 -0.1622(5) 0.25 0.0055(4) Uani 1 2 d S . .
B2 B 0.1923(2) 0.6542(3) 0.46090(11) 0.0056(3) Uani 1 1 d . . .
O1 O -0.5 0.1478(3) 0.25 0.0063(3) Uani 1 2 d S . .
O2 O -0.40084(14) 0.6834(2) 0.33840(7) 0.0064(2) Uani 1 1 d . . .
O3 O -0.28881(14) 0.1784(2) 0.45065(7) 0.0061(2) Uani 1 1 d . . .
O4 O 0.28679(13) 0.3693(2) 0.44171(7) 0.0058(2) Uani 1 1 d . . .
O5 O 0.01706(14) 0.7487(2) 0.40059(8) 0.0073(2) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O5 2.7927(13) . ?
K1 O5 2.7927(13) 2 ?
K1 O4 2.8561(13) . ?
K1 O4 2.8561(13) 2 ?
K1 O5 2.8694(14) 2_545 ?
K1 O5 2.8694(14) 1_545 ?
K1 O3 2.9294(14) . ?
K1 O3 2.9294(14) 2 ?
K1 O1 3.0732(15) . ?
K1 O1 3.0732(15) 1_655 ?
K1 B2 3.2229(17) . ?
K1 B2 3.2229(17) 2 ?
Be1 O4 1.6287(19) . ?
Be1 O3 1.6323(19) 1_655 ?
Be1 O2 1.658(2) 1_655 ?
Be1 O1 1.6609(18) 1_655 ?
Be1 K1 3.260(2) 1_655 ?
Be2 O5 1.6017(19) . ?
Be2 O3 1.622(2) 1_565 ?
Be2 O4 1.6653(19) 3_566 ?
Be2 O2 1.6767(18) . ?
Be2 K1 3.2372(19) 1_565 ?
Be2 K1 3.872(2) 3_566 ?
B1 O2 1.3700(14) 2_445 ?
B1 O2 1.3700(14) 1_545 ?
B1 O1 1.383(2) . ?
B1 K1 3.5692(18) 1_455 ?
B2 O5 1.3380(16) . ?
B2 O3 1.3937(16) 3_566 ?
B2 O4 1.4124(17) . ?
B2 K1 3.559(2) 3_566 ?
O1 Be1 1.6609(18) 1_455 ?
O1 Be1 1.6609(18) 2 ?
O1 K1 3.0732(15) 1_455 ?
O2 B1 1.3700(14) 1_565 ?
O2 Be1 1.658(2) 1_455 ?
O3 B2 1.3937(16) 3_566 ?
O3 Be2 1.622(2) 1_545 ?
O3 Be1 1.6323(19) 1_455 ?
O4 Be2 1.6653(19) 3_566 ?
O5 K1 2.8694(14) 1_565 ?

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
O5 K1 O5 77.19(5) . 2 ?
O5 K1 O4 50.30(3) . . ?
O5 K1 O4 111.77(4) 2 . ?
O5 K1 O4 111.77(4) . 2 ?
O5 K1 O4 50.30(3) 2 2 ?
O4 K1 O4 160.26(4) . 2 ?
O5 K1 O5 178.79(2) . 2_545 ?
O5 K1 O5 104.02(5) 2 2_545 ?
O4 K1 O5 128.87(3) . 2_545 ?
O4 K1 O5 69.20(3) 2 2_545 ?
O5 K1 O5 104.02(5) . 1_545 ?
O5 K1 O5 178.79(2) 2 1_545 ?
O4 K1 O5 69.20(3) . 1_545 ?
O4 K1 O5 128.87(3) 2 1_545 ?
O5 K1 O5 74.77(5) 2_545 1_545 ?
O5 K1 O3 68.02(3) . . ?
O5 K1 O3 124.59(3) 2 . ?
O4 K1 O3 76.83(5) . . ?
O4 K1 O3 105.68(5) 2 . ?
O5 K1 O3 111.11(4) 2_545 . ?
O5 K1 O3 56.17(3) 1_545 . ?
O5 K1 O3 124.59(3) . 2 ?
O5 K1 O3 68.02(3) 2 2 ?
O4 K1 O3 105.68(5) . 2 ?
O4 K1 O3 76.83(5) 2 2 ?
O5 K1 O3 56.17(3) 2_545 2 ?
O5 K1 O3 111.11(4) 1_545 2 ?
O3 K1 O3 165.79(4) . 2 ?
O5 K1 O1 99.36(3) . . ?
O5 K1 O1 95.23(3) 2 . ?
O4 K1 O1 128.88(3) . . ?
O4 K1 O1 55.11(3) 2 . ?
O5 K1 O1 80.58(3) 2_545 . ?
O5 K1 O1 84.59(3) 1_545 . ?
O3 K1 O1 52.32(3) . . ?
O3 K1 O1 124.82(3) 2 . ?
O5 K1 O1 95.23(3) . 1_655 ?
O5 K1 O1 99.36(3) 2 1_655 ?
O4 K1 O1 55.11(3) . 1_655 ?
O4 K1 O1 128.88(3) 2 1_655 ?
O5 K1 O1 84.59(3) 2_545 1_655 ?
O5 K1 O1 80.58(3) 1_545 1_655 ?
O3 K1 O1 124.82(3) . 1_655 ?
O3 K1 O1 52.32(3) 2 1_655 ?
O1 K1 O1 161.31(5) . 1_655 ?
O5 K1 B2 24.38(3) . . ?
O5 K1 B2 93.25(5) 2 . ?
O4 K1 B2 25.98(3) . . ?
O4 K1 B2 135.36(4) 2 . ?
O5 K1 B2 154.83(3) 2_545 . ?
O5 K1 B2 87.90(5) 1_545 . ?
O3 K1 B2 71.69(4) . . ?
O3 K1 B2 116.70(4) 2 . ?
O1 K1 B2 116.40(3) . . ?
O1 K1 B2 74.50(3) 1_655 . ?
O5 K1 B2 93.25(5) . 2 ?
O5 K1 B2 24.38(3) 2 2 ?
O4 K1 B2 135.36(4) . 2 ?
O4 K1 B2 25.98(3) 2 2 ?
O5 K1 B2 87.90(5) 2_545 2 ?
O5 K1 B2 154.83(3) 1_545 2 ?
O3 K1 B2 116.70(4) . 2 ?
O3 K1 B2 71.69(4) 2 2 ?
O1 K1 B2 74.50(3) . 2 ?
O1 K1 B2 116.40(3) 1_655 2 ?
B2 K1 B2 113.75(6) . 2 ?
O4 Be1 O3 112.61(11) . 1_655 ?
O4 Be1 O2 107.04(10) . 1_655 ?
O3 Be1 O2 109.49(10) 1_655 1_655 ?
O4 Be1 O1 113.40(10) . 1_655 ?
O3 Be1 O1 107.14(10) 1_655 1_655 ?
O2 Be1 O1 106.98(10) 1_655 1_655 ?
O4 Be1 K1 176.33(9) . 1_655 ?
O3 Be1 K1 63.72(7) 1_655 1_655 ?
O2 Be1 K1 74.76(6) 1_655 1_655 ?
O1 Be1 K1 68.65(5) 1_655 1_655 ?
O4 Be1 K1 54.53(6) . . ?
O3 Be1 K1 145.44(9) 1_655 . ?
O2 Be1 K1 105.06(7) 1_655 . ?
O1 Be1 K1 62.18(5) 1_655 . ?
K1 Be1 K1 128.43(6) 1_655 . ?
O5 Be2 O3 115.78(11) . 1_565 ?
O5 Be2 O4 108.15(10) . 3_566 ?
O3 Be2 O4 113.06(10) 1_565 3_566 ?
O5 Be2 O2 107.81(10) . . ?
O3 Be2 O2 106.86(10) 1_565 . ?
O4 Be2 O2 104.45(10) 3_566 . ?
O5 Be2 K1 62.36(6) . 1_565 ?
O3 Be2 K1 64.45(6) 1_565 1_565 ?
O4 Be2 K1 163.64(9) 3_566 1_565 ?
O2 Be2 K1 91.48(8) . 1_565 ?
O5 Be2 K1 47.34(5) . . ?
O3 Be2 K1 144.43(9) 1_565 . ?
O4 Be2 K1 102.48(8) 3_566 . ?
O2 Be2 K1 63.77(6) . . ?
K1 Be2 K1 81.03(5) 1_565 . ?
O5 Be2 K1 84.17(7) . 3_566 ?
O3 Be2 K1 95.48(7) 1_565 3_566 ?
O4 Be2 K1 41.83(5) 3_566 3_566 ?
O2 Be2 K1 145.77(8) . 3_566 ?
K1 Be2 K1 121.89(5) 1_565 3_566 ?
K1 Be2 K1 110.63(5) . 3_566 ?
O2 B1 O2 119.62(16) 2_445 1_545 ?
O2 B1 O1 120.19(8) 2_445 . ?
O2 B1 O1 120.19(8) 1_545 . ?
O2 B1 K1 129.59(4) 2_445 . ?
O2 B1 K1 83.87(5) 1_545 . ?
O1 B1 K1 58.17(3) . . ?
O2 B1 K1 83.87(5) 2_445 1_455 ?
O2 B1 K1 129.59(4) 1_545 1_455 ?
O1 B1 K1 58.17(3) . 1_455 ?
K1 B1 K1 116.34(7) . 1_455 ?
O5 B2 O3 123.04(12) . 3_566 ?
O5 B2 O4 121.61(11) . . ?
O3 B2 O4 115.30(11) 3_566 . ?
O5 B2 K1 59.49(7) . . ?
O3 B2 K1 176.37(8) 3_566 . ?
O4 B2 K1 62.35(6) . . ?
O5 B2 K1 101.15(8) . 3_566 ?
O3 B2 K1 52.58(6) 3_566 3_566 ?
O4 B2 K1 112.21(7) . 3_566 ?
K1 B2 K1 130.50(5) . 3_566 ?
B1 O1 Be1 120.96(7) . 1_455 ?
B1 O1 Be1 120.96(7) . 2 ?
Be1 O1 Be1 118.08(14) 1_455 2 ?
B1 O1 K1 99.34(3) . . ?
Be1 O1 K1 81.13(6) 1_455 . ?
Be1 O1 K1 89.26(6) 2 . ?
B1 O1 K1 99.34(3) . 1_455 ?
Be1 O1 K1 89.26(6) 1_455 1_455 ?
Be1 O1 K1 81.13(6) 2 1_455 ?
K1 O1 K1 161.31(5) . 1_455 ?
B1 O2 Be1 121.19(10) 1_565 1_455 ?
B1 O2 Be2 126.56(11) 1_565 . ?
Be1 O2 Be2 111.20(9) 1_455 . ?
B1 O2 K1 112.75(6) 1_565 . ?
Be1 O2 K1 75.71(7) 1_455 . ?
Be2 O2 K1 88.62(7) . . ?
B2 O3 Be2 119.40(10) 3_566 1_545 ?
B2 O3 Be1 117.71(10) 3_566 1_455 ?
Be2 O3 Be1 122.45(10) 1_545 1_455 ?
B2 O3 K1 105.22(8) 3_566 . ?
Be2 O3 K1 85.58(7) 1_545 . ?
Be1 O3 K1 86.30(7) 1_455 . ?
B2 O4 Be1 120.23(10) . . ?
B2 O4 Be2 104.77(9) . 3_566 ?
Be1 O4 Be2 122.75(10) . 3_566 ?
B2 O4 K1 91.67(7) . . ?
Be1 O4 K1 97.80(8) . . ?
Be2 O4 K1 115.29(7) 3_566 . ?
B2 O5 Be2 131.85(10) . . ?
B2 O5 K1 96.13(8) . . ?
Be2 O5 K1 107.71(7) . . ?
B2 O5 K1 126.43(8) . 1_565 ?
Be2 O5 K1 88.01(7) . 1_565 ?
K1 O5 K1 104.02(5) . 1_565 ?

#===END


_database_code_depnum_ccdc_archive 'CCDC 981520'
