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_7705660
_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         'C32 H56 Bi2 N12'
_chemical_formula_sum            'C32 H56 Bi2 N12'
_chemical_formula_weight         1026.85
_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     iterative
_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                97.933(3)
_cell_angle_beta                 99.017(3)
_cell_angle_gamma                96.358(3)
_cell_formula_units_Z            1
_cell_length_a                   10.1097(3)
_cell_length_b                   10.1538(3)
_cell_length_c                   10.1748(4)
_cell_measurement_reflns_used    4715
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7520
_cell_measurement_theta_min      3.3680
_cell_volume                     1012.28(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_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 0.9982
_diffrn_measured_fraction_theta_max 0.8603
_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     -1.00  83.00   1.00   13.88    --   15.68  57.00-180.00   84
  2  \w    -54.00  35.00   1.00   13.88    --   15.68 -37.00   0.00   89
  3  \w    -11.00  83.00   1.00   13.88    --   15.68  77.00 -90.00   94
  4  \w     -1.00  83.00   1.00   13.88    --   15.68  57.00 150.00   84
  5  \w    -44.00  50.00   1.00   13.88    --  -17.25  77.00   0.00   94
  6  \w    -25.00  22.00   1.00   13.88    --  -17.25 -99.00 150.00   47
  7  \w    -52.00  34.00   1.00   13.88    --   15.68 -77.00-180.00   86
;
_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      -0.0374916000
_diffrn_orient_matrix_UB_12      0.0550136000
_diffrn_orient_matrix_UB_13      0.0045669000
_diffrn_orient_matrix_UB_21      0.0611113000
_diffrn_orient_matrix_UB_22      0.0450183000
_diffrn_orient_matrix_UB_23      0.0180855000
_diffrn_orient_matrix_UB_31      0.0005564000
_diffrn_orient_matrix_UB_32      0.0037674000
_diffrn_orient_matrix_UB_33      -0.0690084000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11744
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.09
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.546
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3835
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                3185
_reflns_number_total             3835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt03225e2.cif
_cod_data_source_block           20190415-1
_cod_depositor_comments
'Adding full bibliography for 7705659--7705660.cif.'
_cod_database_code               7705660
_reflns_odcompleteness_completeness 99.82
_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. Shared sites
{C11, C11'}
{C14, C14'}
{C15, C15'}
3. Uiso/Uaniso restraints and constraints
C6 \\sim C7 \\sim C8: within 1.7A with sigma of 0.002 and sigma for terminal atoms of 0.002
C10 \\sim C11 \\sim C11' \\sim C10': within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C9) \\sim Ueq, Uanis(C9') \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C16') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C11) = Uanis(C11')
Uanis(C14) = Uanis(C14')
Uanis(C15) = Uanis(C15')
4. Others
 Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(H9'C)=Sof(C10')=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C11')=Sof(H11')=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C11)=Sof(H11)=FVAR(1)
 Sof(C14')=Sof(H14')=Sof(C15')=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16')=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(2)
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C11(H11), C11'(H11'), C14(H14), C14'(H14'), C6(H6)
5.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C9'(H9'A,H9'B,H9'C), C10'(H10D,H10E,
 H10F), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C15'(H15D,H15E,H15F),
 C16'(H16D,H16E,H16F), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.633
_oxdiff_exptl_absorpt_empirical_full_min 0.674