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_7032845
_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
'C37 H30 N22 O21 Pb5, 2(C3 H7 N1 O1), C1 H4 O'
_chemical_formula_sum            'C44 H48 N24 O24 Pb5'
_chemical_formula_weight         2333.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 111.140(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.1919(17)
_cell_length_b                   19.7200(10)
_cell_length_c                   11.8904(8)
_cell_measurement_reflns_used    9486
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.46
_cell_volume                     6165.5(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0498
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            46755
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.408
_diffrn_reflns_theta_min         2.463
_exptl_absorpt_coefficient_mu    13.708
_exptl_absorpt_correction_T_max  0.10
_exptl_absorpt_correction_T_min  0.04
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_description       Block
_exptl_crystal_F_000             4328
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
_platon_squeeze_details
;These disordered dimethylformamide and 
 methanol molecules could not be modelled reliably, were 
 removed from the model but included in the empirical formulae.
 This justify the B-level alert in the checkcif report.The strategy
 improved the R1 factor by 8.20%. The electron count suggests the presence of 
 8 DMF and 4 methanol molecules per unit cell (electron count = 392), 
 2 DMF and one methanol molecules per asymmetric unit.
 Thermogravimetric and elemental analysis data support these results.
;
_refine_diff_density_max         7.152
_refine_diff_density_min         -2.589
_refine_diff_density_rms         0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         5832
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+293.6295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4847
_reflns_number_total             5832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02316a2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7032845--7032850.cif.'
_cod_database_code               7032845
_shelx_estimated_absorpt_t_min   0.114
_shelx_estimated_absorpt_t_max   0.218
_shelxl_version_number           2014/6
_shelx_res_checksum              65359