#------------------------------------------------------------------------------
#$Date: 2016-03-26 12:57:08 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180241 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/27/7112752.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_7112752
loop_
_publ_author_name
'Brianna C. Hughes'
'Zheng Lu'
'David M. Jenkins'
_publ_section_title
;
 The final unadorned tris(azolyl)borate: finishing what Trofimenko started
 in 1966
;
_journal_name_full               Chem.Commun.
_journal_page_first              5273
_journal_paper_doi               10.1039/C3CC47151A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C6 H7 B N9 Na'
_chemical_formula_weight         239.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           212
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 4acd 2ab 3'
_symmetry_space_group_name_H-M   'P 43 3 2'
_atom_sites_solution_hydrogens   geom
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.1478(6)
_cell_length_b                   13.1478(6)
_cell_length_c                   13.1478(6)
_cell_measurement_temperature    100(2)
_cell_volume                     2272.79(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'ω scan'
_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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4942
_diffrn_reflns_theta_full        26.26
_diffrn_reflns_theta_max         26.26
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.9806
_exptl_absorpt_correction_T_min  0.9617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0238
_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)+(0.0416P)²+0.3906P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0662
_reflns_number_gt                748
_reflns_number_total             774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47151a.txt
_cod_data_source_block           Ligand
_cod_original_sg_symbol_H-M      'p 43 3 2'
_cod_database_code               7112752
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'y+3/4, -x+3/4, z+1/4'
'-y+3/4, x+1/4, z+3/4'
'x+1/4, z+3/4, -y+3/4'
'-x+3/4, z+1/4, y+3/4'
'-x+1/4, -z+1/4, -y+1/4'
'x+3/4, -z+3/4, y+1/4'
'z+1/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+1/4'
'-z+3/4, y+1/4, x+3/4'
'-z+1/4, -y+1/4, -x+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
Na1 Na 0.1250 0.1250 0.1250 0.0151(2) Uani 1 6 d S
N1 N 0.31084(7) 0.16329(7) 0.12890(7) 0.0169(2) Uani 1 1 d .
N2 N 0.34738(7) 0.23103(7) 0.19669(7) 0.0150(2) Uani 1 1 d .
N3 N 0.38518(7) 0.13882(8) 0.06602(7) 0.0187(2) Uani 1 1 d .
C3 C 0.46972(9) 0.19159(9) 0.09366(9) 0.0211(3) Uani 1 1 d .
H3 H 0.5328 0.1885 0.0618 0.025 Uiso 1 1 calc R
C2 C 0.44609(9) 0.25008(9) 0.17642(9) 0.0192(3) Uani 1 1 d .
H2 H 0.4892 0.2939 0.2114 0.023 Uiso 1 1 calc R
Na2 Na 0.3750 0.1250 -0.1250 0.0179(3) Uani 1 6 d S
B2 B 0.28050(9) 0.28050(9) 0.28050(9) 0.0155(4) Uani 1 3 d S
H4 H 0.3285(11) 0.3285(11) 0.3285(11) 0.019 Uiso 1 3 d S
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Na1 0.0151(2) 0.0151(2) 0.0151(2) -0.0016(2) -0.0016(2) -0.0016(2)
N1 0.0175(5) 0.0170(5) 0.0162(5) -0.0019(4) 0.0000(3) -0.0008(4)
N2 0.0149(5) 0.0140(4) 0.0160(4) 0.0006(4) -0.0012(4) -0.0010(3)
N3 0.0171(5) 0.0211(5) 0.0178(5) -0.0005(4) 0.0027(4) 0.0011(4)
C3 0.0149(5) 0.0262(6) 0.0221(6) 0.0011(5) 0.0026(4) -0.0017(5)
C2 0.0146(5) 0.0210(6) 0.0219(6) 0.0016(4) -0.0007(4) -0.0034(4)
Na2 0.0179(3) 0.0179(3) 0.0179(3) -0.0018(2) 0.0018(2) -0.0018(2)
B2 0.0155(4) 0.0155(4) 0.0155(4) -0.0016(5) -0.0016(5) -0.0016(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
N1 Na1 N1 94.64(4) 24 .
N1 Na1 N1 113.30(4) 24 5
N1 Na1 N1 77.19(3) . 5
N1 Na1 N1 165.28(4) 24 9
N1 Na1 N1 77.19(3) . 9
N1 Na1 N1 77.19(3) 5 9
N1 Na1 N1 77.19(3) 24 14
N1 Na1 N1 113.30(4) . 14
N1 Na1 N1 165.28(4) 5 14
N1 Na1 N1 94.64(4) 9 14
N1 Na1 N1 77.19(3) 24 19
N1 Na1 N1 165.28(4) . 19
N1 Na1 N1 94.64(4) 5 19
N1 Na1 N1 113.30(4) 9 19
N1 Na1 N1 77.19(3) 14 19
N3 N1 N2 108.13(9) . .
N3 N1 Na1 131.53(7) . .
N2 N1 Na1 119.71(7) . .
C2 N2 N1 109.57(9) . .
C2 N2 B2 127.42(11) . .
N1 N2 B2 122.96(11) . .
N1 N3 C3 108.27(9) . .
N1 N3 Na2 127.02(7) . .
C3 N3 Na2 110.27(7) . .
N3 C3 C2 108.28(10) . .
N3 C3 H3 125.9 . .
C2 C3 H3 125.9 . .
N2 C2 C3 105.75(11) . .
N2 C2 H2 127.1 . .
C3 C2 H2 127.1 . .
N3 Na2 N3 96.37(4) 24 .
N3 Na2 N3 91.30(3) 24 18_554
N3 Na2 N3 81.91(5) . 18_554
N3 Na2 N3 81.91(5) 24 12_554
N3 Na2 N3 91.30(3) . 12_554
N3 Na2 N3 169.84(4) 18_554 12_554
N3 Na2 N3 91.30(3) 24 13_544
N3 Na2 N3 169.84(4) . 13_544
N3 Na2 N3 91.30(3) 18_554 13_544
N3 Na2 N3 96.37(4) 12_554 13_544
N3 Na2 N3 169.84(4) 24 6
N3 Na2 N3 91.30(3) . 6
N3 Na2 N3 96.37(4) 18_554 6
N3 Na2 N3 91.30(3) 12_554 6
N3 Na2 N3 81.91(5) 13_544 6
N2 B2 N2 110.00(8) . 9
N2 B2 N2 110.00(8) . 5
N2 B2 N2 110.00(8) 9 5
N2 B2 H4 108.9(8) . .
N2 B2 H4 108.9(8) 9 .
N2 B2 H4 108.9(8) 5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na1 N1 2.4953(10) 24
Na1 N1 2.4953(10) .
Na1 N1 2.4953(10) 5
Na1 N1 2.4953(10) 9
Na1 N1 2.4953(10) 14
Na1 N1 2.4953(10) 19
N1 N3 1.3200(14) .
N1 N2 1.3486(13) .
N2 C2 1.3483(15) .
N2 B2 1.5526(11) .
N3 C3 1.3598(15) .
N3 Na2 2.5216(10) .
C3 C2 1.3682(17) .
C3 H3 0.9300 .
C2 H2 0.9300 .
Na2 N3 2.5216(10) 24
Na2 N3 2.5216(10) 18_554
Na2 N3 2.5216(10) 12_554
Na2 N3 2.5216(10) 13_544
Na2 N3 2.5216(10) 6
B2 N2 1.5526(11) 9
B2 N2 1.5526(11) 5
B2 H4 1.09(2) .
