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_7031679
_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         'C4 H6 N8 Pb S2'
_chemical_formula_sum            'C4 H6 N8 Pb S2'
_chemical_formula_weight         437.48
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-06-26
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5552(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.94447(19)
_cell_length_b                   4.92209(8)
_cell_length_c                   23.5863(5)
_cell_measurement_reflns_used    41146
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.6460
_cell_measurement_theta_min      3.3300
_cell_volume                     1037.37(4)
_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      100.00(10)
_diffrn_detector_area_resol_mean 10.6228
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9732
_diffrn_measurement_details
;
  1 omega  -90.00  -59.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000  -25.3815 31

  2 omega  -90.00  -63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000 -127.3463 27

  3 omega  -36.00   45.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672   38.0000  -30.0000 81

  4 omega   14.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922 -130.0000 -133.8619 61

  5 omega   -8.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   57.0000   90.0000 94

  6 omega   37.00   65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  178.0000 -180.0000 28

  7 omega  -13.00   89.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   77.0000  -60.0000 102

  8 omega  -48.00    7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  -38.0000  150.0000 55

  9 omega  -51.00   24.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  -38.0000   30.0000 75

 10 omega   40.00   82.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  178.0000  -30.0000 42

 11 omega   -3.00   88.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   38.0000 -150.0000 91

 12 omega  -37.00   54.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672   38.0000   90.0000 91

 13 omega  -42.00   52.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672   57.0000 -120.0000 94

 14 omega  -88.00    4.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  -38.0000  150.0000 92

 15 omega  -85.00    8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  -57.0000   90.0000 93

 16 omega  -88.00    4.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  -38.0000  -90.0000 92

 17 omega  -72.00  -26.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  128.0000   56.0000 46

 18 omega    6.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922 -130.0000 -133.8619 69

 19 omega   34.00  102.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922 -178.0000   90.0000 68

 20 omega  -54.00   38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  -38.0000   90.0000 92

 21 omega  -90.00  -38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000 -176.0073 52

 22 omega -101.00  -55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  178.0000   30.0000 46

 23 omega  -90.00  -38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000 -127.3463 52

 24 omega  -88.00   13.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  -77.0000  -30.0000 101

 25 omega  -68.00   51.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -150.0000 119

 26 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -180.0000 171

 27 omega  -90.00  -38.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000  -63.9193 52

 28 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -150.0000 171

 29 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000    0.0000 171

 30 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000  -90.0000 171

 31 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000  -60.0000 171

 32 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000  -30.0000 171

 33 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -120.0000 171

 34 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000   30.0000 171

 35 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000   60.0000 171

 36 omega  -68.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000   90.0000 171

 37 omega  -68.00   23.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000  120.0000 91

 38 omega  -68.00   82.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -180.0000 150
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0071239000
_diffrn_orient_matrix_UB_12      0.0468669000
_diffrn_orient_matrix_UB_13      0.0284510000
_diffrn_orient_matrix_UB_21      0.0014875000
_diffrn_orient_matrix_UB_22      -0.1362075000
_diffrn_orient_matrix_UB_23      0.0097623000
_diffrn_orient_matrix_UB_31      0.0790491000
_diffrn_orient_matrix_UB_32      -0.0017261000
_diffrn_orient_matrix_UB_33      -0.0013960000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77856
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.376
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.646
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.026
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.4898
_exptl_crystal_size_mid          0.0895
_exptl_crystal_size_min          0.0297
_refine_diff_density_max         3.320
_refine_diff_density_min         -3.082
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+17.8915P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1740
_reflns_number_total             1819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01406e1.cif
_cod_data_source_block           compound9
_cod_depositor_comments
'Adding full bibliography for 7031671--7031680.cif.'
_cod_original_cell_volume        1037.36(4)
_cod_database_code               7031679
_chemical_oxdiff_formula         'C4 H6 N8 Pb S2'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_shelx_res_checksum              67718
_shelxl_version_number           2013-2