#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:01:59 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178930 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/59/4115934.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_4115934
loop_
_publ_author_name
'Li Xu'
'Svilen Bobev'
'Jaouad El-Bahraoui'
'Slavi C. Sevov'
_publ_section_title
;
 A Naked Diatomic Molecule of Bismuth, [Bi2]2-, with a Short Bi-Bi Bond:
 Synthesis and Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1838
_journal_page_last               1839
_journal_paper_doi               10.1021/ja992422i
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C36 H72 Bi2 K2 N4 O12'
_chemical_formula_weight         1249.14
_chemical_name_systematic
;
 (K-crypt)2Bi2
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.220(1)
_cell_length_b                   12.220
_cell_length_c                   28.927(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      12
_cell_volume                     3740.9(5)
_computing_cell_refinement       'CAD4-ARGUS, (Enraf-Nonius, 1994)'
_computing_data_collection       'CAD4-ARGUS, (Enraf-Nonius, 1994)'
_computing_data_reduction        'xcad4 (Harms, 1996)'
_computing_molecular_graphics    'SHELXTL-V5.1 (Siemens, 1994)'
_computing_publication_material  'SHELXTL-V5.1 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega-2theta
_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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1566
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.268
_exptl_absorpt_correction_T_max  0.7360
_exptl_absorpt_correction_T_min  0.1699
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       plate
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00037(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0283
_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)+(0.0466P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                1298
_reflns_number_total             1437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja992422i.cif
_cod_data_source_block           KcrBi2
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4115934
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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'
'-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'
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
Bi Bi 0.0000 0.0000 0.049046(10) 0.06224(16) Uani 1 3 d S
K K 0.0000 0.0000 0.69555(6) 0.0553(4) Uani 1 3 d S
N1 N 0.0000 0.0000 0.7978(3) 0.082(2) Uani 1 3 d S
N2 N 0.0000 0.0000 0.5915(3) 0.0619(15) Uani 1 3 d S
O1 O -0.0134(3) 0.1979(3) 0.74403(14) 0.0757(9) Uani 1 1 d .
O2 O 0.1693(3) -0.0473(3) 0.64803(13) 0.0685(9) Uani 1 1 d .
C1 C -0.0491(10) 0.0808(9) 0.8140(3) 0.110(3) Uani 1 1 d .
H1A H -0.048(6) 0.094(6) 0.839(2) 0.086(19) Uiso 1 1 d .
H1B H -0.163(8) 0.034(7) 0.809(3) 0.14(3) Uiso 1 1 d .
C2 C 0.0138(10) 0.2090(8) 0.7923(3) 0.110(2) Uani 1 1 d .
H2A H -0.023(6) 0.254(7) 0.808(2) 0.11(2) Uiso 1 1 d .
H2B H 0.096(6) 0.241(6) 0.799(2) 0.09(2) Uiso 1 1 d .
C3 C 0.0619(5) 0.3140(5) 0.7212(3) 0.0815(17) Uani 1 1 d .
H3A H 0.143(5) 0.334(5) 0.7262(17) 0.065(13) Uiso 1 1 d .
H3B H 0.057(5) 0.385(6) 0.739(2) 0.090(17) Uiso 1 1 d .
C4 C -0.3053(5) -0.2817(5) 0.6722(2) 0.0770(15) Uani 1 1 d .
H4A H -0.275(5) -0.345(5) 0.6656(19) 0.081(16) Uiso 1 1 d .
H4B H -0.379(5) -0.304(5) 0.6572(17) 0.066(14) Uiso 1 1 d .
C5 C 0.1885(5) -0.0282(6) 0.5999(2) 0.0754(14) Uani 1 1 d .
H5A H 0.217(5) -0.082(5) 0.5857(19) 0.083(16) Uiso 1 1 d .
H5B H 0.246(5) 0.057(5) 0.5917(18) 0.078(16) Uiso 1 1 d .
C6 C 0.0634(6) -0.0683(6) 0.5764(2) 0.0774(14) Uani 1 1 d .
H6A H 0.080(6) -0.056(6) 0.545(3) 0.11(2) Uiso 1 1 d .
H6B H 0.005(5) -0.162(6) 0.578(2) 0.083(16) Uiso 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 0.0033 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'
N N 0.0061 0.0033 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 '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
O2 K O2 97.57(11) . 3
O2 K O2 97.57(11) . 2
O2 K O2 97.57(11) 3 2
O2 K O1 115.80(11) . 2
O2 K O1 60.71(11) 3 2
O2 K O1 141.27(10) 2 2
O2 K O1 60.71(11) . 3
O2 K O1 141.27(10) 3 3
O2 K O1 115.80(11) 2 3
O1 K O1 98.16(11) 2 3
O2 K O1 141.27(11) . .
O2 K O1 115.80(11) 3 .
O2 K O1 60.71(11) 2 .
O1 K O1 98.16(11) 2 .
O1 K O1 98.16(11) 3 .
O2 K N1 119.70(8) . .
O2 K N1 119.70(8) 3 .
O2 K N1 119.70(8) 2 .
O1 K N1 60.76(9) 2 .
O1 K N1 60.76(9) 3 .
O1 K N1 60.75(9) . .
O2 K N2 60.30(8) . .
O2 K N2 60.30(8) 3 .
O2 K N2 60.30(8) 2 .
O1 K N2 119.24(9) 2 .
O1 K N2 119.24(9) 3 .
O1 K N2 119.25(9) . .
N1 K N2 180.000(2) . .
C1 N1 C1 110.3(4) 2 3
C1 N1 C1 110.3(4) 2 .
C1 N1 C1 110.3(4) 3 .
C1 N1 K 108.7(4) 2 .
C1 N1 K 108.7(4) 3 .
C1 N1 K 108.7(4) . .
C6 N2 C6 111.4(3) . 3
C6 N2 C6 111.4(3) . 2
C6 N2 C6 111.4(3) 3 2
C6 N2 K 107.4(4) . .
C6 N2 K 107.4(4) 3 .
C6 N2 K 107.4(4) 2 .
C3 O1 C2 111.0(5) . .
C3 O1 K 109.6(3) . .
C2 O1 K 116.7(4) . .
C5 O2 C4 112.5(4) . 2
C5 O2 K 122.3(3) . .
C4 O2 K 117.1(3) 2 .
N1 C1 C2 113.7(7) . .
N1 C1 H1A 119(5) . .
C2 C1 H1A 104(5) . .
N1 C1 H1B 113(4) . .
C2 C1 H1B 108(4) . .
H1A C1 H1B 96(6) . .
O1 C2 C1 109.8(6) . .
O1 C2 H2A 111(4) . .
C1 C2 H2A 105(4) . .
O1 C2 H2B 115(4) . .
C1 C2 H2B 103(4) . .
H2A C2 H2B 112(6) . .
O1 C3 C4 110.6(4) . 3
O1 C3 H3A 106(3) . .
C4 C3 H3A 116(3) 3 .
O1 C3 H3B 109(3) . .
C4 C3 H3B 113(3) 3 .
H3A C3 H3B 102(4) . .
O2 C4 C3 110.2(4) 3 2
O2 C4 H4A 104(3) 3 .
C3 C4 H4A 117(3) 2 .
O2 C4 H4B 103(3) 3 .
C3 C4 H4B 110(3) 2 .
H4A C4 H4B 111(4) . .
O2 C5 C6 109.4(4) . .
O2 C5 H5A 113(3) . .
C6 C5 H5A 104(3) . .
O2 C5 H5B 113(3) . .
C6 C5 H5B 108(3) . .
H5A C5 H5B 109(5) . .
N2 C6 C5 114.7(5) . .
N2 C6 H6A 110(5) . .
C5 C6 H6A 106(4) . .
N2 C6 H6B 111(3) . .
C5 C6 H6B 112(3) . .
H6A C6 H6B 102(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi Bi 2.8377(7) 10
K O2 2.774(3) .
K O2 2.774(3) 3
K O2 2.774(3) 2
K O1 2.870(4) 2
K O1 2.870(4) 3
K O1 2.870(4) .
K N1 2.958(8) .
K N2 3.010(7) .
N1 C1 1.465(8) 2
N1 C1 1.465(8) 3
N1 C1 1.466(8) .
N2 C6 1.462(6) .
N2 C6 1.462(6) 3
N2 C6 1.462(6) 2
O1 C3 1.410(7) .
O1 C2 1.426(8) .
O2 C5 1.412(7) .
O2 C4 1.436(6) 2
C1 C2 1.495(12) .
C1 H1A 0.75(7) .
C1 H1B 1.22(8) .
C2 H2A 0.98(7) .
C2 H2B 0.90(6) .
C3 C4 1.482(10) 3
C3 H3A 0.90(5) .
C3 H3B 1.03(6) .
C4 O2 1.436(6) 3
C4 C3 1.482(10) 2
C4 H4A 1.03(5) .
C4 H4B 0.91(5) .
C5 C6 1.513(8) .
C5 H5A 0.98(6) .
C5 H5B 0.95(6) .
C6 H6A 0.92(7) .
C6 H6B 1.01(6) .
