Boron-centered soft ligands based on tetrazole units and their complexes with sodium, potassium and bismuth ions.
Imran, Muhammad; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Monkowius, Uwe; Bleckenwegner, Petra; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14737–14748; doi:10.1039/c4dt01931h

data_7031692
_publ_section_title
;
 Boron-centered soft ligands based on tetrazole units and their complexes
 with sodium, potassium and bismuth ions.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14737
_journal_page_last               14748
_journal_paper_doi               10.1039/c4dt01931h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C28 H20 Bi2 N16 S4, 2(C2 H3 N)'
_chemical_formula_sum            'C32 H26 Bi2 N18 S4'
_chemical_formula_weight         1208.91
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-11-06
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                67.741(3)
_cell_angle_beta                 89.501(2)
_cell_angle_gamma                78.825(2)
_cell_formula_units_Z            1
_cell_length_a                   7.07185(17)
_cell_length_b                   11.5039(4)
_cell_length_c                   13.7591(5)
_cell_measurement_reflns_used    34915
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.9580
_cell_measurement_theta_min      3.0480
_cell_volume                     1013.72(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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
;
SHELXL, 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      100.00(10)
_diffrn_detector_area_resol_mean 8.0951
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9425
_diffrn_measurement_details
;
  1 omega  -42.00   59.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -19.0000  150.0000 101

  2 omega   16.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -134.0000  117.0000 67

  3 omega   -4.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000   90.0000 98

  4 omega   10.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -135.0000  -61.0000 76

  5 omega   -4.00   43.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000 -150.0000 47

  6 omega  -42.00   54.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -77.0000  120.0000 96

  7 omega   -4.00   88.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000  -30.0000 92

  8 omega  -40.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -77.0000  -30.0000 86

  9 omega    7.00   85.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000  -90.0000 78

 10 omega    1.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421    0.0000  -90.0000 89

 11 omega  -97.00  -35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000 -178.0000  -60.0000 62

 12 omega  -92.00   -5.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -57.0000   90.0000 87

 13 omega    3.00   96.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   38.0000 -120.0000 93

 14 omega  -20.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000 -180.0000 86

 15 omega   -4.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000   60.0000 98

 16 omega    8.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -135.0000  -61.0000 78

 17 omega  -46.00   47.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -38.0000  -90.0000 93

 18 omega  -13.00   97.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   19.0000    0.0000 110

 19 omega  -95.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -180.0000 143

 20 omega  -97.00  -35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000 -178.0000 -180.0000 62

 21 omega  -95.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -150.0000 143

 22 omega  -92.00   -5.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -57.0000  150.0000 87

 23 omega  -20.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000   30.0000 86

 24 omega    7.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000    0.0000 86

 25 omega   35.00   99.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  178.0000 -180.0000 64

 26 omega   -4.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000  -60.0000 98

 27 omega  -95.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -120.0000 141
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0008942000
_diffrn_orient_matrix_UB_12      0.0077729000
_diffrn_orient_matrix_UB_13      0.0487204000
_diffrn_orient_matrix_UB_21      -0.0142997000
_diffrn_orient_matrix_UB_22      0.0674702000
_diffrn_orient_matrix_UB_23      -0.0272915000
_diffrn_orient_matrix_UB_31      -0.1014918000
_diffrn_orient_matrix_UB_32      0.0047159000
_diffrn_orient_matrix_UB_33      0.0002552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59206
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.079
_diffrn_reflns_theta_min         2.944
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.924
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.112
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.5349
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.0451
_refine_diff_density_max         3.633
_refine_diff_density_min         -1.461
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+5.4021P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5688
_reflns_number_total             5928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01931h2.cif
_cod_data_source_block           compound6b
_cod_depositor_comments
'Adding full bibliography for 7031686--7031693.cif.'
_cod_database_code               7031692
_chemical_oxdiff_formula         'C16 h18 B Bi N2 O4 S2'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_shelx_res_checksum              7290
_shelxl_version_number           2013-2