1,2,4-Triazolato paddlewheel dibismuth complexes with very short Bi(II)-Bi(II) bonds: bismuth(III) oxidation of 1,2,4-triazolato anions into neutral <i>N</i>-1,2,4-triazolyl radicals.
Zhao, Ming-Gang; Li, Li; He, Ru-Ru; Zhang, Xiang; Ma, Jian-Ping; Su, Ji-Hu; Zheng, Wenjun; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15190–15194; doi:10.1039/d0dt03225e

data_7705659
_publ_section_title
;
 1,2,4-Triazolato paddlewheel dibismuth complexes with very short
 Bi(II)-Bi(II) bonds: bismuth(III) oxidation of 1,2,4-triazolato anions
 into neutral <i>N</i>-1,2,4-triazolyl radicals.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15190
_journal_page_last               15194
_journal_paper_doi               10.1039/d0dt03225e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C56 H40 Bi2 N12, 0.5(C14 H16)'
_chemical_formula_sum            'C63 H48 Bi2 N12'
_chemical_formula_weight         1391.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-06-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2019-07-01 deposited with the CCDC.	2020-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                97.805(3)
_cell_angle_beta                 104.276(3)
_cell_angle_gamma                107.123(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8511(3)
_cell_length_b                   11.8616(4)
_cell_length_c                   14.2639(4)
_cell_measurement_reflns_used    13368
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9310
_cell_measurement_theta_min      3.3250
_cell_volume                     1351.40(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0251
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.8515
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -52.00  32.00   1.00   20.13    --   15.53 -57.00 -90.00   84
  2  \w    -52.00  32.00   1.00   20.13    --   15.53 -57.00 150.00   84
  3  \w    -67.00   9.00   1.00   20.13    --  -17.17 118.00 -42.72   76
  4  \w    -85.00  10.00   1.00   20.13    --  -17.17 -77.00-180.00   95
  5  \w    -84.00   0.00   1.00   20.13    --  -17.17 -57.00 -90.00   84
  6  \w    -34.00  50.00   1.00   20.13    --  -17.17  58.00  67.00   84
  7  \w    -85.00  10.00   1.00   20.13    --  -17.17 -77.00  30.00   95
  8  \w    -84.00   0.00   1.00   20.13    --  -17.17 -57.00 120.00   84
  9  \w    -74.00  -1.00   1.00   20.13    --  -17.17 130.00  28.07   73
 10  \w    -67.00   9.00   1.00   20.13    --  -17.17 118.00 174.86   76
 11  \w     35.00  88.00   1.00   20.13    --   15.53 178.00 120.00   53
 12  \w    -55.00  27.00   1.00   20.13    --  -17.17  97.00 101.66   82
 13  \w    -75.00  -2.00   1.00   20.13    --  -17.17 133.00 -90.97   73
 14  \w    -44.00  50.00   1.00   20.13    --  -17.17  77.00-120.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0460428000
_diffrn_orient_matrix_UB_12      -0.0227232000
_diffrn_orient_matrix_UB_13      0.0361269000
_diffrn_orient_matrix_UB_21      -0.0742467000
_diffrn_orient_matrix_UB_22      -0.0455622000
_diffrn_orient_matrix_UB_23      -0.0018447000
_diffrn_orient_matrix_UB_31      0.0103974000
_diffrn_orient_matrix_UB_32      -0.0391379000
_diffrn_orient_matrix_UB_33      -0.0382720000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30468
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.80
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.395
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5135
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0510
_reflns_number_gt                4515
_reflns_number_total             5135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt03225e2.cif
_cod_data_source_block           180315-1
_cod_depositor_comments
'Adding full bibliography for 7705659--7705660.cif.'
_cod_original_cell_volume        1351.40(7)
_cod_database_code               7705659
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32-C31
 1.53 with sigma of 0.01
 C30-C29 = C29-C31 = C33-C31 = C34-C33 = C35-C34 = C35-C30
 1.42 with sigma of 0.01
 C32-C29 \\sim C32-C33
 with sigma of 0.01
3. Restrained planarity
 C29, C30, C31, C32, C33, C34, C35
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
5. Others
 Fixed Sof: C29(0.5) H29(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C31(0.5)
 C30(0.5) H30(0.5) C33(0.5) H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35(0.5)
6.a Riding coordinates:
 C29(H29), C32(H32A,H32B,H32C), C30(H30), C33(H33), C34(H34), C35(H35)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 58.989
_oxdiff_exptl_absorpt_empirical_full_min 0.451