Structural variation in ethylenediamine and -diphosphine adducts of (2,6-Me2C6H3S)2Pb: a single crystal X-ray diffraction and (207)Pb solid-state NMR spectroscopy study.
Rossini, Aaron J.; Macgregor, Alan W.; Smith, Anita S.; Schatte, Gabriele; Schurko, Robert W.; Briand, Glen G.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 9533–9546; doi:10.1039/c3dt33070b

data_7021402
_publ_section_title
;
 Structural variation in ethylenediamine and -diphosphine adducts of
 (2,6-Me2C6H3S)2Pb: a single crystal X-ray diffraction and (207)Pb
 solid-state NMR spectroscopy study.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9533
_journal_page_last               9546
_journal_paper_doi               10.1039/c3dt33070b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C54 H70 P2 Pb3 S6'
_chemical_formula_sum            'C54 H70 P2 Pb3 S6'
_chemical_formula_weight         1594.97
_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   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-2012 template'
_cell_angle_alpha                90
_cell_angle_beta                 114.6800(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2754(2)
_cell_length_b                   20.1016(2)
_cell_length_c                   18.9169(2)
_cell_measurement_reflns_used    13542
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      1.00
_cell_volume                     7005.65(13)
_computing_cell_refinement       'HKL DENZO and SCALEPACK, Bruker AXS/Nonius'
_computing_data_collection       'COLLECT, Bruker AXS/Nonius'
_computing_data_reduction        'HKL DENZO and SCALEPACK, Bruker AXS/Nonius'
_computing_molecular_graphics    'XP (SHELXTL-NT v6.14, Bruker AXS)'
_computing_publication_material  'WinGX v1.80.05 2009 (L. J. Farrugia)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'KappaCCD (BruKer AXS-Nonius, FR540C)'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Nonius FR590D, fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19559
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         3.119
_exptl_absorpt_coefficient_mu    7.444
_exptl_absorpt_correction_T_max  0.348
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_platon_squeeze_details
;Approximately 23% of the unit cell volume (1576 ^3^) comprises a
region of disordered solvent which could not be modeled as
discrete atomic sites. The program PLATON/SQUEEZE was used to
calculate the contribution from the solvent region to the
diffraction. A total electron count of 148 electrons was found
in the total solvent-accessible void volume within the unit
cell. The eletcron count of 74 e^-^ corresponds to 1.5 molecules
of toluene in each void. Toluene was used as a solvent for growing
the crystals. The data were corrected for disordered electron
density through use of the SQUEEZE procedure as implemented
in PLATON leading to a set of solvent-free diffraction
intensities.
The modified data improved the R-factors (before SQUEEZE:
R~1~ = 0.0361, wR~2~ = 0.1009; largest difference peak and hole,
1.470 and -1.372 e-/ ^3^; after SQUEEZE: R~1~ = 0.0316, wR~2~ = 0.0743;
largest difference peak and hole, 0.996 and -1.392 e^-^/ ^3^).
Derived values (formula weight, density, absorption coefficient)
do not contain the contribution of the disordered solvent.
;
_refine_diff_density_max         0.998
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         10209
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+14.0431P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8098
_reflns_number_total             10209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt33070b.txt
_cod_data_source_block           10
_cod_database_code               7021402
_shelx_estimated_absorpt_t_min   0.279
_shelx_estimated_absorpt_t_max   0.348