Synthesis, structure and catalytic application of lead(II) complexes in cyanosilylation reactions.
Karmakar, Anirban; Hazra, Susanta; Guedes da Silva, M Fátima C; Pombeiro, Armando J. L.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 268–280; doi:10.1039/c4dt02316a

data_7032850
_publ_section_title
;
 Synthesis, structure and catalytic application of lead(II) complexes in
 cyanosilylation reactions.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              268
_journal_page_last               280
_journal_paper_doi               10.1039/c4dt02316a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C20 H18 N12 O9 Pb2, 2.5(C3 H7 N1 O1)'
_chemical_formula_sum            'C27.5 H35.5 N14.5 O11.5 Pb2'
_chemical_formula_weight         1167.58
_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   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90.964(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.468(3)
_cell_length_b                   13.261(2)
_cell_length_c                   19.861(4)
_cell_measurement_reflns_used    9564
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.47
_cell_volume                     3810.0(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66637
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.312
_exptl_absorpt_coefficient_mu    8.903
_exptl_absorpt_correction_T_max  0.175
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_description       Block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.190
_platon_squeeze_details
;These disordered dimethylformamide molecules could not be 
 modelled reliably,were removed from the model but included in the 
 empirical formulae. This justify the A-level alert in the checkcif report.
 The strategy improved the R1 factor by 29.12%. The electron count suggests 
 the presence of 10 DMF molecules per unit cell (electron count= 400), 
 2.5 DMF molecules per asymmetric unit.Thermogravimetric and elemental 
 analysis data support these results. 
;
_refine_diff_density_max         3.527
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7794
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0625P)^2^+5.3545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6291
_reflns_number_total             7794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02316a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7032845--7032850.cif.'
_cod_original_cell_volume        3809.9(12)
_cod_original_formula_sum        'C27.50 H35.50 N14.50 O11.50 Pb2'
_cod_database_code               7032850
_shelx_estimated_absorpt_t_min   0.163
_shelx_estimated_absorpt_t_max   0.283
_shelxl_version_number           2014/6
_shelx_res_checksum              56488