#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:17:12 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178807 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/61/4106144.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_4106144
loop_
_publ_author_name
'Hongping Wu'
'Shilie Pan'
'Kenneth R. Poeppelmeier'
'Hongyi Li'
'Dianzeng Jia'
'Zhaohui Chen'
'Xiaoyun Fan'
'Yun Yang'
'James M. Rondinelli'
'Haosu Luo'
_publ_section_title
;
 K3B6O10Cl: A New Structure Analogous to Perovskite with a Large Second
 Harmonic Generation Response and Deep UV Absorption Edge
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7786
_journal_page_last               7790
_journal_paper_doi               10.1021/ja111083x
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'B6 Cl K3 O10'
_chemical_formula_weight         377.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           160
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.0624(14)
_cell_length_b                   10.0624(14)
_cell_length_c                   8.8361(18)
_cell_measurement_temperature    293(2)
_cell_volume                     774.8(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2606
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.428
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_coef       0.066(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         474
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0138
_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)+(0.0129P)²+0.1902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0320
_refine_ls_wR_factor_ref         0.0323
_reflns_number_gt                468
_reflns_number_total             474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja111083x_si_002.cif
_cod_data_source_block           whp
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4106144
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
K1 K -0.17954(2) 0.17954(2) 0.56270(2) 0.00964(12) Uani 1 2 d S
Cl1 Cl 0.0000 0.0000 0.44054(10) 0.01367(18) Uani 1 6 d S
B1 B -0.08739(11) 0.08739(11) 0.8987(2) 0.0043(4) Uani 1 2 d S
B2 B 0.15075(11) 0.3015(2) 0.7840(2) 0.0049(4) Uani 1 2 d S
O1 O -0.00079(10) 0.23426(10) 0.82039(10) 0.0058(2) Uani 1 1 d .
O2 O 0.22323(7) 0.44647(14) 0.72298(14) 0.0061(3) Uani 1 2 d S
O3 O 0.0000 0.0000 0.8896(3) 0.0029(5) Uani 1 6 d S
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 K1 O1 150.33(4) 17_444 14_554
O1 K1 O1 125.02(4) 17_444 .
O1 K1 O1 75.952(15) 14_554 .
O1 K1 O1 75.952(15) 17_444 4
O1 K1 O1 125.02(4) 14_554 4
O1 K1 O1 49.97(4) . 4
O1 K1 O2 49.81(3) 17_444 13_444
O1 K1 O2 119.09(3) 14_554 13_444
O1 K1 O2 157.49(3) . 13_444
O1 K1 O2 115.43(3) 4 13_444
O1 K1 O2 119.09(3) 17_444 14_554
O1 K1 O2 49.81(3) 14_554 14_554
O1 K1 O2 115.43(3) . 14_554
O1 K1 O2 157.49(3) 4 14_554
O2 K1 O2 71.65(5) 13_444 14_554
O1 K1 B2 25.82(4) 17_444 13_444
O1 K1 B2 143.62(4) 14_554 13_444
O1 K1 B2 140.14(4) . 13_444
O1 K1 B2 91.28(4) 4 13_444
O2 K1 B2 26.07(5) 13_444 13_444
O2 K1 B2 97.72(4) 14_554 13_444
O1 K1 B2 143.62(4) 17_444 14_554
O1 K1 B2 25.82(4) 14_554 14_554
O1 K1 B2 91.28(4) . 14_554
O1 K1 B2 140.14(4) 4 14_554
O2 K1 B2 97.72(4) 13_444 14_554
O2 K1 B2 26.07(5) 14_554 14_554
B2 K1 B2 123.78(7) 13_444 14_554
O1 K1 Cl1 101.95(2) 17_444 7_455
O1 K1 Cl1 101.95(2) 14_554 7_455
O1 K1 Cl1 81.44(2) . 7_455
O1 K1 Cl1 81.44(2) 4 7_455
O2 K1 Cl1 79.06(3) 13_444 7_455
O2 K1 Cl1 79.06(3) 14_554 7_455
B2 K1 Cl1 83.97(3) 13_444 7_455
B2 K1 Cl1 83.97(3) 14_554 7_455
O1 K1 Cl1 80.91(2) 17_444 .
O1 K1 Cl1 80.91(2) 14_554 .
O1 K1 Cl1 84.24(2) . .
O1 K1 Cl1 84.24(2) 4 .
O2 K1 Cl1 113.41(3) 13_444 .
O2 K1 Cl1 113.41(3) 14_554 .
B2 K1 Cl1 103.08(3) 13_444 .
B2 K1 Cl1 103.08(3) 14_554 .
Cl1 K1 Cl1 164.19(3) 7_455 .
O1 K1 B1 99.96(2) 17_444 .
O1 K1 B1 99.96(2) 14_554 .
O1 K1 B1 25.157(19) . .
O1 K1 B1 25.157(19) 4 .
O2 K1 B1 139.65(3) 13_444 .
O2 K1 B1 139.65(3) 14_554 .
B2 K1 B1 116.40(4) 13_444 .
B2 K1 B1 116.40(4) 14_554 .
Cl1 K1 B1 83.57(4) 7_455 .
Cl1 K1 B1 80.62(4) . .
O1 K1 B2 135.96(4) 17_444 .
O1 K1 B2 57.61(4) 14_554 .
O1 K1 B2 21.27(4) . .
O1 K1 B2 67.44(4) 4 .
O2 K1 B2 173.66(4) 13_444 .
O2 K1 B2 103.55(4) 14_554 .
B2 K1 B2 158.37(7) 13_444 .
B2 K1 B2 77.576(12) 14_554 .
Cl1 K1 B2 96.10(3) 7_455 .
Cl1 K1 B2 72.09(3) . .
B1 K1 B2 42.54(3) . .
K1 Cl1 K1 90.59(2) 15_444 14_554
K1 Cl1 K1 90.59(2) 15_444 13_544
K1 Cl1 K1 90.59(2) 14_554 13_544
K1 Cl1 K1 164.19(3) 15_444 3
K1 Cl1 K1 78.369(7) 14_554 3
K1 Cl1 K1 78.369(7) 13_544 3
K1 Cl1 K1 78.369(7) 15_444 2
K1 Cl1 K1 164.19(3) 14_554 2
K1 Cl1 K1 78.369(7) 13_544 2
K1 Cl1 K1 109.906(16) 3 2
K1 Cl1 K1 78.370(7) 15_444 .
K1 Cl1 K1 78.370(7) 14_554 .
K1 Cl1 K1 164.19(3) 13_544 .
K1 Cl1 K1 109.906(16) 3 .
K1 Cl1 K1 109.906(16) 2 .
O2 B1 O1 110.94(10) 9_455 4
O2 B1 O1 110.94(10) 9_455 .
O1 B1 O1 107.02(15) 4 .
O2 B1 O3 108.90(16) 9_455 .
O1 B1 O3 109.51(10) 4 .
O1 B1 O3 109.51(10) . .
O2 B1 K1 135.72(11) 9_455 .
O1 B1 K1 54.00(8) 4 .
O1 B1 K1 54.00(8) . .
O3 B1 K1 115.38(13) . .
O1 B2 O1 121.21(17) . 5
O1 B2 O2 119.24(8) . .
O1 B2 O2 119.24(8) 5 .
O1 B2 K1 145.70(13) . 7
O1 B2 K1 62.06(6) 5 7
O2 B2 K1 65.30(6) . 7
O1 B2 K1 62.06(6) . 9_455
O1 B2 K1 145.70(13) 5 9_455
O2 B2 K1 65.30(6) . 9_455
K1 B2 K1 95.97(5) 7 9_455
O1 B2 K1 47.78(8) . .
O1 B2 K1 132.43(11) 5 .
O2 B2 K1 93.44(8) . .
K1 B2 K1 158.37(7) 7 .
K1 B2 K1 77.363(13) 9_455 .
O1 B2 K1 132.43(11) . 3
O1 B2 K1 47.78(8) 5 3
O2 B2 K1 93.44(8) . 3
K1 B2 K1 77.363(13) 7 3
K1 B2 K1 158.37(7) 9_455 3
K1 B2 K1 101.21(5) . 3
B2 O1 B1 124.60(12) . .
B2 O1 K1 92.12(9) . 9_455
B1 O1 K1 128.18(9) . 9_455
B2 O1 K1 110.95(11) . .
B1 O1 K1 100.84(8) . .
K1 O1 K1 97.11(3) 9_455 .
B2 O2 B1 128.98(16) . 14_554
B2 O2 K1 88.63(7) . 7
B1 O2 K1 117.54(4) 14_554 7
B2 O2 K1 88.63(7) . 9_455
B1 O2 K1 117.54(4) 14_554 9_455
K1 O2 K1 109.68(5) 7 9_455
B1 O3 B1 119.72(2) 2 3
B1 O3 B1 119.72(2) 2 .
B1 O3 B1 119.72(2) 3 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O1 2.7621(9) 17_444
K1 O1 2.7621(9) 14_554
K1 O1 2.7808(10) .
K1 O1 2.7808(10) 4
K1 O2 2.8393(8) 13_444
K1 O2 2.8393(8) 14_554
K1 B2 3.1244(14) 13_444
K1 B2 3.1244(14) 14_554
K1 Cl1 3.2660(7) 7_455
K1 Cl1 3.3101(6) .
K1 B1 3.376(2) .
K1 B2 3.5066(14) .
Cl1 K1 3.2659(7) 15_444
Cl1 K1 3.2659(7) 14_554
Cl1 K1 3.2660(7) 13_544
Cl1 K1 3.3101(6) 3
Cl1 K1 3.3101(6) 2
B1 O2 1.448(2) 9_455
B1 O1 1.4611(14) 4
B1 O1 1.4611(14) .
B1 O3 1.5252(19) .
B2 O1 1.3619(14) .
B2 O1 1.3619(14) 5
B2 O2 1.373(2) .
B2 K1 3.1244(14) 7
B2 K1 3.1244(14) 9_455
B2 K1 3.5066(14) 3
O1 K1 2.7621(9) 9_455
O2 B1 1.448(2) 14_554
O2 K1 2.8393(8) 7
O2 K1 2.8394(8) 9_455
O3 B1 1.5252(19) 2
O3 B1 1.5252(19) 3
