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_7031678
_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         'C6 H6 N4 Pb S4'
_chemical_formula_sum            'C6 H6 N4 Pb S4'
_chemical_formula_weight         469.58
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-07-03
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.931(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3192(4)
_cell_length_b                   11.7420(4)
_cell_length_c                   7.72600(19)
_cell_measurement_reflns_used    11084
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1950
_cell_measurement_theta_min      4.9660
_cell_volume                     1205.46(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      100.00(10)
_diffrn_detector_area_resol_mean 5.3114
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -37.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000    0.0000 70

  2 omega  -46.00   35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   30.0000   90.0000 81

  3 omega  -64.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   61.0000  -90.0000 94

  4 omega  -63.00   28.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   61.0000 -180.0000 91

  5 omega   55.00  104.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -60.0000 49

  6 omega   80.00  106.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -180.0000 26

  7 omega   13.00   93.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -150.0000 80

  8 omega   24.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000  150.0000 60

  9 omega   43.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988 -110.0000   42.0000 44

 10 omega   13.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   30.0000 82

 11 omega   16.00   80.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -60.0000 64

 12 omega   11.00   38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   83.0000  107.2156 27

 13 omega   19.00   47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -60.0000 28

 14 omega   18.00   53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -180.0000 35

 15 omega   81.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 26

 16 omega  142.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 36

 17 omega   32.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 77

 18 omega   85.00  118.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 33

 19 omega   54.00  101.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 47

 20 omega   40.00  140.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   60.0000 100

 21 omega   86.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   60.0000  -86.1190 26

 22 omega   82.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 25

 23 omega   81.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 33

 24 omega   86.00  116.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 30

 25 omega   81.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 26

 26 omega   81.00  137.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 56

 27 omega   86.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 25

 28 omega   81.00  176.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 95

 29 omega   85.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 27

 30 omega   86.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 25

 31 omega   86.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 26

 32 omega   56.00   99.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 43

 33 omega  121.00  152.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   69.0000 -178.4082 31

 34 omega   81.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 30

 35 omega   61.00  121.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 60

 36 omega   85.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 26

 37 omega   96.00  122.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 26

 38 omega  122.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 56

 39 omega   86.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 92

 40 omega   81.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 96

 41 omega   81.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 97

 42 omega   85.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 92

 43 omega   43.00   78.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 35

 44 omega   85.00  162.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 77

 45 omega  125.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 52

 46 omega   82.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 25

 47 omega  119.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 58

 48 omega   85.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 30

 49 omega   81.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 33

 50 omega  125.00  176.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 51

 51 omega   81.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 34

 52 omega   84.00  117.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   69.0000 -178.4082 33

 53 omega   84.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000 -116.2067 28

 54 omega  -56.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   45.0000 -150.0000 87

 55 omega -107.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -61.0000   90.0000 95

 56 omega   18.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -150.0000 94

 57 omega   57.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  -30.0000 70

 58 omega   18.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000   90.0000 94

 59 omega  -34.00   76.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  -19.0000 -120.0000 110

 60 omega   57.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  -60.0000 70

 61 omega   11.00   40.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   83.0000  107.2156 29

 62 omega   18.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000    0.0000 94

 63 omega   13.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -120.0000 102

 64 omega   13.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -30.0000 102

 65 omega   23.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000   90.0000 91

 66 omega   57.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  150.0000 70

 67 omega   57.00  127.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000 -150.0000 70

 68 omega   38.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000    0.0000 53

 69 omega   85.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 93

 70 omega   85.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 93

 71 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -60.0000 89

 72 omega   82.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.0000  147.7038 96

 73 omega   71.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  120.0000 107

 74 omega   41.00  122.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 81

 75 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -120.0000 89

 76 omega   38.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 53

 77 omega   31.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 78

 78 omega   38.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -60.0000 53

 79 omega   31.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   90.0000 78

 80 omega   31.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 78

 81 omega   41.00   99.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   60.0000 58

 82 omega   81.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 97

 83 omega   85.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 93

 84 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   30.0000 89

 85 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -30.0000 89

 86 omega   38.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -150.0000 53

 87 omega   85.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 93

 88 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -90.0000 89

 89 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   60.0000 89

 90 omega   89.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   90.0000 89

 91 omega   90.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000    0.0000 88
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0007375000
_diffrn_orient_matrix_UB_12      0.0215967000
_diffrn_orient_matrix_UB_13      -0.1967856000
_diffrn_orient_matrix_UB_21      0.1134064000
_diffrn_orient_matrix_UB_22      -0.0267290000
_diffrn_orient_matrix_UB_23      0.0052664000
_diffrn_orient_matrix_UB_31      -0.0240637000
_diffrn_orient_matrix_UB_32      -0.1266807000
_diffrn_orient_matrix_UB_33      -0.0345730000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            44530
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.996
_diffrn_reflns_theta_min         3.326
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    33.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25323
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.2026
_exptl_crystal_size_mid          0.0587
_exptl_crystal_size_min          0.022
_refine_diff_density_max         1.479
_refine_diff_density_min         -1.798
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         4649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0552P)^2^+18.2097P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4189
_reflns_number_total             4649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01406e1.cif
_cod_data_source_block           compound8
_cod_depositor_comments
'Adding full bibliography for 7031671--7031680.cif.'
_cod_database_code               7031678
_chemical_oxdiff_formula         'C6 H6 N4 Pb S4'
_shelx_res_checksum              46800
_shelxl_version_number           2013-2