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_7032849
_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_sum            'C12 H13 N7 O5 Pb'
_chemical_formula_weight         542.48
_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           SHELXL-2014
_cell_angle_alpha                81.365(2)
_cell_angle_beta                 87.259(2)
_cell_angle_gamma                73.959(2)
_cell_formula_units_Z            4
_cell_length_a                   7.6487(5)
_cell_length_b                   12.2700(7)
_cell_length_c                   18.3447(12)
_cell_measurement_reflns_used    7391
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      2.96
_cell_volume                     1635.82(18)
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18025
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.700
_diffrn_reflns_theta_min         2.640
_exptl_absorpt_coefficient_mu    10.355
_exptl_absorpt_correction_T_max  0.14
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_description       Block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.190
_refine_diff_density_max         2.913
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         5514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+2.3038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4373
_reflns_number_total             5514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02316a2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
Adding full bibliography for 7032845--7032850.cif.

2017-03-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C24 H26 N14 O10 Pb2'
_cod_original_formula_weight         1084.97
_cod_original_formula_units_Z            2
_cod_database_code               7032849
_shelx_estimated_absorpt_t_min   0.111
_shelx_estimated_absorpt_t_max   0.244
_shelxl_version_number           2014-1
_shelx_res_checksum              44305