Synthesis, structural and photo-physical studies of bismuth(iii) complexes with Janus scorpionate and co-ligands.
Imran, Muhammad; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Monkowius, Uwe; Bleckenwegner, Petra; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 10956–10968; doi:10.1039/c4dt00668b

data_7030982
_publ_section_title
;
 Synthesis, structural and photo-physical studies of bismuth(iii)
 complexes with Janus scorpionate and co-ligands.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10956
_journal_page_last               10968
_journal_paper_doi               10.1039/c4dt00668b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C24.55 H32.32 B2 Bi I2 N14.77 Na O S12, 0.77(H2 O), 0.23(O1), 0.23(C2 H3 N1)'
_chemical_formula_sum            'C25 H35 B2 Bi I2 N15 Na O2 S12'
_chemical_formula_weight         1469.79
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-10-25
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.7276(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.92021(15)
_cell_length_b                   17.08670(14)
_cell_length_c                   20.8514(2)
_cell_measurement_reflns_used    67481
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      31.9860
_cell_measurement_theta_min      3.1470
_cell_volume                     5063.38(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector_area_resol_mean 8.0951
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9991
_diffrn_measurement_details
;
  1 omega  -42.00   84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421    0.0000 -120.0000 126

  2 omega  -40.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -38.0000 -180.0000 87

  3 omega   -4.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000   30.0000 98

  4 omega  -13.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000   60.0000 79

  5 omega   -4.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000 -150.0000 96

  6 omega    8.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000  -60.0000 58

  7 omega    7.00   55.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000  -30.0000 48

  8 omega    7.00   55.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000  150.0000 48

  9 omega    5.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000 -180.0000 61

 10 omega  -32.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421    0.0000   30.0000 118

 11 omega    7.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000  -90.0000 86

 12 omega    7.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000   60.0000 86

 13 omega   34.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -178.0000   60.0000 66

 14 omega   -4.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000  150.0000 98

 15 omega  -20.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000  -90.0000 86

 16 omega   35.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  178.0000  150.0000 64

 17 omega    7.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000    0.0000 86

 18 omega  -43.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -57.0000  120.0000 87

 19 omega  -46.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000   38.0000   60.0000 93

 20 omega   -4.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000   60.0000 98

 21 omega   -4.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000  -90.0000 98

 22 omega  -20.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000    0.0000 86

 23 omega    3.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   38.0000 -120.0000 93

 24 omega  -20.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000 -150.0000 86

 25 omega  -20.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000  -60.0000 86

 26 omega  -20.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000  150.0000 86

 27 omega  -92.00  -35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -57.0000   90.0000 57
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0464486000
_diffrn_orient_matrix_UB_12      -0.0139105000
_diffrn_orient_matrix_UB_13      0.0051268000
_diffrn_orient_matrix_UB_21      0.0117721000
_diffrn_orient_matrix_UB_22      0.0355521000
_diffrn_orient_matrix_UB_23      -0.0130633000
_diffrn_orient_matrix_UB_31      0.0139392500
_diffrn_orient_matrix_UB_32      0.0163145500
_diffrn_orient_matrix_UB_33      0.0328365000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            136600
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.030
_diffrn_reflns_theta_min         2.595
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.249
_exptl_absorpt_correction_T_max  1.171
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.1666
_exptl_crystal_size_mid          0.1059
_exptl_crystal_size_min          0.0886
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7384
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+12.8366P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7028
_reflns_number_total             7384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00668b4.cif
_cod_data_source_block           compound4a
_cod_depositor_comments
;Adding full bibliography for 7030979--7030984.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        5063.37(9)
_cod_database_code               7030982
_chemical_oxdiff_formula         ' C18H20B2BiI2N12S12'
_chemical_oxdiff_usercomment     'Vers.Nr. 288'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Others
 Fixed Sof: Na1(0.5) O1(0.5) H1(0.5) N8(0.5) C12(0.5) C13(0.5) H13A(0.5)
 H13B(0.5) H13C(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 Fixed Uiso: H1(0.054) H2AA(0.041) H2AB(0.041) H11A(0.067) H11B(0.067)
 H11C(0.067) H13A(0.053) H13B(0.053) H13C(0.053) H14A(0.059) H14B(0.059)
 H14C(0.059) H16A(0.052) H16B(0.052) H16C(0.052)
 Fixed X: Bi1(0.75) H1(0.6713) H11A(0.5312) H11B(0.6137) H11C(0.6355)
 H13A(0.8635) H13B(0.8545) H13C(0.9517) H14A(0.5478) H14B(0.577) H14C(0.6435)
 H16A(0.532) H16B(0.4889) H16C(0.4309)
 Fixed Y: Bi1(0.75) H1(0.2781) H11A(0.2532) H11B(0.1898) H11C(0.2748)
 H13A(0.078) H13B(0.0983) H13C(0.1135) H14A(0.3325) H14B(0.4123) H14C(0.3758)
 H16A(0.0324) H16B(0.0173) H16C(0.0671)
 Fixed Z: Bi1(0.5) H1(0.5026) H11A(0.1586) H11B(0.1821) H11C(0.1582)
 H13A(0.4446) H13B(0.5173) H13C(0.5017) H14A(0.5238) H14B(0.4953) H14C(0.564)
 H16A(0.2969) H16B(0.2177) H16C(0.2567)
;
_shelx_hkl_checksum              19426
_shelx_res_checksum              37881
_shelxl_version_number           2013-2