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_7032846
_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         'C22 H16 N12 O8 Pb2, 2(C3 H7 N1 O1), H2 O'
_chemical_formula_sum            'C28 H32 N14 O11 Pb2'
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_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
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_cell_angle_gamma                90
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_cell_measurement_reflns_used    9941
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.23
_cell_measurement_theta_min      2.62
_cell_volume                     3787.3(4)
_computing_cell_refinement       'Bruker SAINT'
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_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
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_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
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_diffrn_measured_fraction_theta_max 0.996
_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
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_exptl_crystal_description       Block
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_platon_squeeze_details
;These disordered dimethylformamide and water 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 13.84%.
 The electron count suggest the presence of 8 DMF and 4 water molecules
 per unit cell (electron count = 360), 2 DMF and 1 water molecules per
 asymmetric unit. Thermogravimetric and elemental analysis data support
 these results. 
;
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+8.7097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1269
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_depositor_comments
'Adding full bibliography for 7032845--7032850.cif.'
_cod_database_code               7032846
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_shelx_estimated_absorpt_t_max   0.347
_shelxl_version_number           2014/6
_shelx_res_checksum              68316