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_7021401
_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         'C38 H52 N2 Pb2 S4, C7 H8'
_chemical_formula_sum            'C45 H60 N2 Pb2 S4'
_chemical_formula_weight         1171.57
_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   geom
_audit_creation_method           'manual editing of SHELXL-2012 template'
_cell_angle_alpha                99.7056(8)
_cell_angle_beta                 109.4720(8)
_cell_angle_gamma                90.8606(8)
_cell_formula_units_Z            2
_cell_length_a                   11.91250(10)
_cell_length_b                   14.0434(2)
_cell_length_c                   14.9513(2)
_cell_measurement_reflns_used    10729
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.00
_cell_volume                     2317.59(5)
_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 0.999
_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  0.0185
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.902
_diffrn_reflns_theta_min         2.700
_exptl_absorpt_coefficient_mu    7.467
_exptl_absorpt_correction_T_max  0.31
_exptl_absorpt_correction_T_min  0.31
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.825
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         11047
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0160P)^2^+2.7486P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9667
_reflns_number_total             11047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt33070b.txt
_cod_data_source_block           9
_cod_original_cell_volume        2317.58(5)
_cod_database_code               7021401
_shelx_estimated_absorpt_t_min   0.317
_shelx_estimated_absorpt_t_max   0.317