Hemi- and holo-directed lead(II) complexes in a soft ligand environment.
Imran, Muhammad; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Monkowius, Uwe; Gründlinger, Petra; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 924–937; doi:10.1039/c4dt01406e

data_7031672
_publ_section_title
;
 Hemi- and holo-directed lead(II) complexes in a soft ligand environment.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              924
_journal_page_last               937
_journal_paper_doi               10.1039/c4dt01406e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C16 H20 B2 N4 Pb S8'
_chemical_formula_sum            'C16 H20 B2 N4 Pb S8'
_chemical_formula_weight         753.65
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-06-27
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                65.316(2)
_cell_angle_beta                 83.1389(17)
_cell_angle_gamma                66.8959(19)
_cell_formula_units_Z            2
_cell_length_a                   9.93379(19)
_cell_length_b                   12.2627(3)
_cell_length_c                   12.4372(3)
_cell_measurement_reflns_used    43855
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.8410
_cell_measurement_theta_min      3.1840
_cell_volume                     1264.40(6)
_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      100.01(10)
_diffrn_detector_area_resol_mean 10.6228
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9516
_diffrn_measurement_details
;
  1 omega   -8.00   85.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854   77.0000 -150.0000 93

  2 omega   -4.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854   77.0000   60.0000 93

  3 omega   -4.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854   57.0000  -30.0000 90

  4 omega  -27.00   43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -57.0000  -60.0000 70

  5 omega  -51.00   18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -57.0000 -180.0000 69

  6 omega  -20.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -99.0000   60.0000 76

  7 omega   11.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854   38.0000 -180.0000 35

  8 omega   60.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854   38.0000 -180.0000 28

  9 omega   37.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  178.0000 -150.0000 33

 10 omega  -15.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -99.0000  -90.0000 71

 11 omega   55.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854 -153.0000 -134.0374 36

 12 omega  -86.00  -35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  148.0000   14.7631 51

 13 omega  -88.00    4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -38.0000  -90.0000 92

 14 omega  -88.00    4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -38.0000   60.0000 92

 15 omega  -75.00  -27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  131.0000  -82.7173 48

 16 omega  -88.00    4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -38.0000    0.0000 92

 17 omega  -94.00   16.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -19.0000  150.0000 110

 18 omega   35.00  101.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  178.0000   30.0000 66

 19 omega    7.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854 -133.0000  -93.7391 70

 20 omega  -20.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -99.0000   90.0000 76

 21 omega  -90.00  -38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  153.0000 -157.0994 52

 22 omega  -94.00   16.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -19.0000 -120.0000 110

 23 omega  -85.00    8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  -57.0000 -150.0000 93

 24 omega  -90.00  -38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8604  153.0000  -36.0747 52

 25 omega  -68.00    9.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854    0.0000 -180.0000 77

 26 omega  -54.00   38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854  -38.0000   60.0000 92

 27 omega   16.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.4854 -153.0000 -134.0374 75
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0261927000
_diffrn_orient_matrix_UB_12      0.0206612000
_diffrn_orient_matrix_UB_13      0.0357534000
_diffrn_orient_matrix_UB_21      -0.0714087000
_diffrn_orient_matrix_UB_22      0.0464531000
_diffrn_orient_matrix_UB_23      -0.0021418000
_diffrn_orient_matrix_UB_31      -0.0160652000
_diffrn_orient_matrix_UB_32      -0.0463710000
_diffrn_orient_matrix_UB_33      0.0516506000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            74818
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.995
_diffrn_reflns_theta_min         2.795
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.346
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.203
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.3512
_exptl_crystal_size_mid          0.2091
_exptl_crystal_size_min          0.1473
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         7372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0146
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+0.3336P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0321
_refine_ls_wR_factor_ref         0.0327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7025
_reflns_number_total             7372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01406e1.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7031671--7031680.cif.'
_cod_original_cell_volume        1264.40(5)
_cod_database_code               7031672
_chemical_oxdiff_formula         'C8 H24 B N O3 Pb S4'
_chemical_oxdiff_usercomment     'V.Nr 315 vom 15.4.13'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_shelx_res_checksum              40410
_shelxl_version_number           2013-2