#------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/68/1546836.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_1546836
loop_
_publ_author_name
'Wang, Jia-Jia'
'Yang, Guo-Yu'
_publ_section_title
;
 A novel supramolecular magnesoborate framework with snowflake-like
 channels built by unprecedented huge B ₆₉ cluster cages
;
_journal_issue                   75
_journal_name_full               'Chemical Communications'
_journal_page_first              10398
_journal_page_last               10401
_journal_paper_doi               10.1039/C7CC05404A
_journal_volume                  53
_journal_year                    2017
_chemical_formula_sum            'C0 H18 B69 Mg7 N0 O126'
_chemical_formula_weight         2950.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           163
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-04-20 deposited with the CCDC.
2017-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   26.1715(2)
_cell_length_b                   26.1715(2)
_cell_length_c                   15.38620(10)
_cell_measurement_reflns_used    18780
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.9425
_cell_measurement_theta_min      3.3746
_cell_volume                     9126.81(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43517
_diffrn_reflns_theta_full        67.05
_diffrn_reflns_theta_max         67.05
_diffrn_reflns_theta_min         4.85
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55308
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2910
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.00030(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0488
_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)+(0.0848P)²+4.4155P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1438
_reflns_number_gt                4847
_reflns_number_total             5399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc05404a2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-31c
_cod_original_formula_sum        'C0 B69 H18 Mg7 N0 O126'
_cod_database_code               1546836
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mg1 Mg 0.6667 0.3333 0.2500 0.0237(3) Uani 1 6 d S
Mg2 Mg 0.52777(3) 0.20704(3) 0.41979(4) 0.02730(18) Uani 1 1 d .
B1 B 0.43717(13) -0.00315(12) 0.3584(2) 0.0525(7) Uani 1 1 d .
B2 B 0.33877(13) 0.14186(17) 0.5670(2) 0.0587(8) Uani 1 1 d .
B3 B 0.51645(11) 0.15880(12) 0.61352(14) 0.0404(6) Uani 1 1 d .
B4 B 0.52333(10) 0.30037(10) 0.53041(14) 0.0314(5) Uani 1 1 d .
B5 B 0.39200(11) 0.12864(12) 0.45137(15) 0.0380(5) Uani 1 1 d .
B6 B 0.49091(10) 0.17012(9) 0.23115(13) 0.0275(4) Uani 1 1 d .
B7 B 0.56377(9) 0.33394(9) 0.38299(12) 0.0250(4) Uani 1 1 d .
B8 B 0.44675(10) 0.19432(11) 0.57513(14) 0.0345(5) Uani 1 1 d .
B9 B 0.55303(13) 0.27652(6) 0.2500 0.0238(6) Uani 1 2 d S
B10 B 0.51529(11) 0.08479(11) 0.42206(16) 0.0374(5) Uani 1 1 d .
B11 B 0.59406(10) 0.17325(11) 0.49771(14) 0.0338(5) Uani 1 1 d .
B12 B 0.43401(10) 0.08806(10) 0.33826(14) 0.0323(5) Uani 1 1 d .
O1 O 0.40931(10) -0.06270(9) 0.3464(3) 0.1177(13) Uani 1 1 d .
H1A H 0.4339 -0.0733 0.3427 0.176 Uiso 1 1 calc R
O2 O 0.28512(10) 0.12823(17) 0.59903(18) 0.1127(12) Uani 1 1 d .
H2C H 0.2659 0.0915 0.6099 0.169 Uiso 1 1 d R
O3 O 0.33955(8) 0.11401(11) 0.49104(13) 0.0688(6) Uani 1 1 d .
O4 O 0.53153(10) 0.12873(13) 0.67091(13) 0.0839(8) Uani 1 1 d .
H4C H 0.5655 0.1523 0.6915 0.126 Uiso 1 1 d R
O5 O 0.49073(8) 0.02559(7) 0.40084(15) 0.0613(5) Uani 1 1 d .
O6 O 0.41058(7) 0.02504(6) 0.32789(10) 0.0435(4) Uani 1 1 d .
O7 O 0.56350(6) 0.10927(7) 0.47342(10) 0.0414(4) Uani 1 1 d .
O8 O 0.54145(7) 0.35697(7) 0.55266(9) 0.0422(4) Uani 1 1 d .
O9 O 0.38817(7) 0.17976(7) 0.60697(9) 0.0418(4) Uani 1 1 d .
O10 O 0.48519(7) 0.25716(7) 0.58451(9) 0.0404(4) Uani 1 1 d .
O11 O 0.44712(7) 0.11497(6) 0.25345(8) 0.0380(4) Uani 1 1 d .
O12 O 0.54957(6) 0.18447(7) 0.54138(8) 0.0375(3) Uani 1 1 d .
O13 O 0.38934(7) 0.09638(7) 0.38193(10) 0.0423(4) Uani 1 1 d .
O14 O 0.46722(7) 0.16211(7) 0.63006(9) 0.0379(3) Uani 1 1 d .
O15 O 0.50968(6) 0.17802(6) 0.14823(8) 0.0321(3) Uani 1 1 d .
O16 O 0.44353(6) 0.17491(6) 0.48223(8) 0.0332(3) Uani 1 1 d .
O17 O 0.54304(6) 0.28761(6) 0.45484(8) 0.0290(3) Uani 1 1 d .
O18 O 0.48978(6) 0.11571(6) 0.39173(8) 0.0321(3) Uani 1 1 d .
O19 O 0.60907(6) 0.21174(6) 0.42188(8) 0.0283(3) Uani 1 1 d .
O20 O 0.59098(5) 0.31705(5) 0.31593(7) 0.0239(3) Uani 1 1 d .
O21 O 0.51374(6) 0.21642(5) 0.29001(7) 0.0259(3) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 '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
O20 Mg1 O20 68.17(6) 5_655 2_655
O20 Mg1 O20 98.06(4) 5_655 6
O20 Mg1 O20 98.92(7) 2_655 6
O20 Mg1 O20 98.92(7) 5_655 3_665
O20 Mg1 O20 98.06(4) 2_655 3_665
O20 Mg1 O20 159.47(7) 6 3_665
O20 Mg1 O20 98.06(4) 5_655 4_665
O20 Mg1 O20 159.47(7) 2_655 4_665
O20 Mg1 O20 98.06(4) 6 4_665
O20 Mg1 O20 68.17(6) 3_665 4_665
O20 Mg1 O20 159.47(7) 5_655 .
O20 Mg1 O20 98.06(4) 2_655 .
O20 Mg1 O20 68.17(6) 6 .
O20 Mg1 O20 98.06(4) 3_665 .
O20 Mg1 O20 98.92(7) 4_665 .
O20 Mg1 B9 34.08(3) 5_655 2_655
O20 Mg1 B9 34.08(3) 2_655 2_655
O20 Mg1 B9 100.27(3) 6 2_655
O20 Mg1 B9 100.27(3) 3_665 2_655
O20 Mg1 B9 130.54(3) 4_665 2_655
O20 Mg1 B9 130.54(3) . 2_655
O20 Mg1 B9 130.54(3) 5_655 .
O20 Mg1 B9 100.27(3) 2_655 .
O20 Mg1 B9 34.08(3) 6 .
O20 Mg1 B9 130.54(3) 3_665 .
O20 Mg1 B9 100.27(3) 4_665 .
O20 Mg1 B9 34.08(3) . .
B9 Mg1 B9 120.0 2_655 .
O20 Mg1 B9 100.27(3) 5_655 3_665
O20 Mg1 B9 130.54(3) 2_655 3_665
O20 Mg1 B9 130.54(3) 6 3_665
O20 Mg1 B9 34.08(3) 3_665 3_665
O20 Mg1 B9 34.08(3) 4_665 3_665
O20 Mg1 B9 100.27(3) . 3_665
B9 Mg1 B9 120.0 2_655 3_665
B9 Mg1 B9 120.0 . 3_665
O17 Mg2 O21 95.07(5) . .
O17 Mg2 O19 105.89(6) . .
O21 Mg2 O19 104.26(5) . .
O17 Mg2 O12 96.61(6) . .
O21 Mg2 O12 166.48(6) . .
O19 Mg2 O12 65.90(5) . .
O17 Mg2 O18 165.71(6) . .
O21 Mg2 O18 85.77(5) . .
O19 Mg2 O18 87.64(6) . .
O12 Mg2 O18 84.59(6) . .
O17 Mg2 O16 85.29(6) . .
O21 Mg2 O16 105.63(6) . .
O19 Mg2 O16 146.92(6) . .
O12 Mg2 O16 82.15(6) . .
O18 Mg2 O16 80.76(6) . .
O17 Mg2 B11 114.57(7) . .
O21 Mg2 B11 132.37(7) . .
O19 Mg2 B11 34.12(6) . .
O12 Mg2 B11 35.09(6) . .
O18 Mg2 B11 74.19(7) . .
O16 Mg2 B11 112.85(6) . .
O6 B1 O1 117.3(3) . .
O6 B1 O5 122.5(2) . .
O1 B1 O5 120.3(3) . .
O9 B2 O2 121.6(3) . .
O9 B2 O3 121.4(2) . .
O2 B2 O3 117.0(3) . .
O14 B3 O12 120.8(2) . .
O14 B3 O4 118.19(19) . .
O12 B3 O4 121.0(2) . .
O8 B4 O10 117.79(17) . .
O8 B4 O17 120.62(18) . .
O10 B4 O17 121.59(19) . .
O13 B5 O16 123.4(2) . .
O13 B5 O3 116.7(2) . .
O16 B5 O3 119.9(2) . .
O15 B6 O11 116.76(17) . .
O15 B6 O21 121.37(17) . .
O11 B6 O21 121.84(16) . .
O20 B7 O19 114.21(15) . 3_665
O20 B7 O15 111.55(14) . 6
O19 B7 O15 110.11(15) 3_665 6
O20 B7 O17 107.96(15) . .
O19 B7 O17 107.84(13) 3_665 .
O15 B7 O17 104.62(15) 6 .
O10 B8 O9 107.77(18) . .
O10 B8 O14 110.45(18) . .
O9 B8 O14 106.98(16) . .
O10 B8 O16 111.65(16) . .
O9 B8 O16 110.77(17) . .
O14 B8 O16 109.10(17) . .
O20 B9 O20 106.9(2) . 6
O20 B9 O21 111.26(7) . 6
O20 B9 O21 109.73(6) 6 6
O20 B9 O21 109.73(6) . .
O20 B9 O21 111.26(7) 6 .
O21 B9 O21 108.0(2) 6 .
O20 B9 Mg1 53.46(10) . .
O20 B9 Mg1 53.46(10) 6 .
O21 B9 Mg1 126.02(10) 6 .
O21 B9 Mg1 126.02(10) . .
O7 B10 O18 122.6(2) . .
O7 B10 O5 118.0(2) . .
O18 B10 O5 119.4(2) . .
O8 B11 O19 115.07(17) 2_655 .
O8 B11 O12 113.43(17) 2_655 .
O19 B11 O12 101.01(16) . .
O8 B11 O7 107.35(17) 2_655 .
O19 B11 O7 112.38(17) . .
O12 B11 O7 107.38(16) . .
O8 B11 Mg2 151.60(17) 2_655 .
O19 B11 Mg2 52.60(9) . .
O12 B11 Mg2 54.76(9) . .
O7 B11 Mg2 101.02(12) . .
O11 B12 O6 108.53(17) . .
O11 B12 O13 110.96(18) . .
O6 B12 O13 107.80(17) . .
O11 B12 O18 108.83(16) . .
O6 B12 O18 111.26(17) . .
O13 B12 O18 109.47(16) . .
B5 O3 B2 120.4(2) . .
B1 O5 B10 119.8(2) . .
B1 O6 B12 123.4(2) . .
B10 O7 B11 121.80(17) . .
B4 O8 B11 122.36(16) . 3_665
B2 O9 B8 122.84(19) . .
B4 O10 B8 133.78(16) . .
B6 O11 B12 127.88(16) . .
B3 O12 B11 129.49(18) . .
B3 O12 Mg2 131.47(14) . .
B11 O12 Mg2 90.15(10) . .
B5 O13 B12 131.95(18) . .
B3 O14 B8 123.92(16) . .
B6 O15 B7 124.17(15) . 6
B5 O16 B8 119.45(16) . .
B5 O16 Mg2 123.62(13) . .
B8 O16 Mg2 114.72(12) . .
B4 O17 B7 116.47(15) . .
B4 O17 Mg2 125.25(13) . .
B7 O17 Mg2 116.34(10) . .
B10 O18 B12 123.07(17) . .
B10 O18 Mg2 120.37(14) . .
B12 O18 Mg2 116.55(12) . .
B7 O19 B11 115.65(15) 2_655 .
B7 O19 Mg2 150.77(11) 2_655 .
B11 O19 Mg2 93.29(11) . .
B7 O20 B9 117.62(15) . .
B7 O20 Mg1 148.75(11) . .
B9 O20 Mg1 92.45(11) . .
B6 O21 B9 114.48(11) . .
B6 O21 Mg2 123.50(11) . .
B9 O21 Mg2 116.58(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 O20 2.0713(12) 5_655
Mg1 O20 2.0713(12) 2_655
Mg1 O20 2.0713(12) 6
Mg1 O20 2.0713(12) 3_665
Mg1 O20 2.0713(12) 4_665
Mg1 O20 2.0713(12) .
Mg1 B9 2.576(3) 2_655
Mg1 B9 2.575(3) .
Mg1 B9 2.575(3) 3_665
Mg2 O17 2.0133(14) .
Mg2 O21 2.0670(13) .
Mg2 O19 2.0693(15) .
Mg2 O12 2.1240(14) .
Mg2 O18 2.1243(15) .
Mg2 O16 2.1533(15) .
Mg2 B11 2.601(2) .
B1 O6 1.327(3) .
B1 O1 1.363(4) .
B1 O5 1.379(4) .
B2 O9 1.323(4) .
B2 O2 1.357(4) .
B2 O3 1.383(4) .
B3 O14 1.358(3) .
B3 O12 1.361(3) .
B3 O4 1.366(3) .
B4 O8 1.354(3) .
B4 O10 1.356(3) .
B4 O17 1.379(2) .
B5 O13 1.342(3) .
B5 O16 1.370(3) .
B5 O3 1.370(3) .
B6 O15 1.345(2) .
B6 O11 1.364(3) .
B6 O21 1.386(2) .
B7 O20 1.443(2) .
B7 O19 1.449(2) 3_665
B7 O15 1.468(2) 6
B7 O17 1.526(2) .
B8 O10 1.443(3) .
B8 O9 1.467(3) .
B8 O14 1.471(3) .
B8 O16 1.505(2) .
B9 O20 1.445(2) .
B9 O20 1.445(2) 6
B9 O21 1.514(2) 6
B9 O21 1.514(2) .
B10 O7 1.349(3) .
B10 O18 1.363(3) .
B10 O5 1.387(3) .
B11 O8 1.438(3) 2_655
B11 O19 1.461(2) .
B11 O12 1.495(3) .
B11 O7 1.498(3) .
B12 O11 1.440(2) .
B12 O6 1.453(3) .
B12 O13 1.456(3) .
B12 O18 1.508(3) .
O8 B11 1.438(3) 3_665
O15 B7 1.468(3) 6
O19 B7 1.449(2) 2_655
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 -0.005 4408.5 703.4
2 0.333 0.667 0.250 215.1 53.3
3 0.667 0.333 0.750 215.1 53.6
