Toward Rational Control of Metal Stoichiometry in Heterobimetallic Coordination Complexes: Synthesis and Characterization of Pb(Hsal)2(Cu(salen*))2, [Pb(NO3)(Cu(salen*))2](NO3), Pb(OAc)2(Cu(salen*)), and [Pb(OAc)(Ni(salen*))2](OAc)
John H. Thurston; Christopher G.-Z. Tang; Daniel W. Trahan; Kenton H. Whitmire; Inorganic Chemistry 43 (2004) 2708–2713; doi:10.1021/ic035427w

data_4310862
_publ_contact_author
;
      Kenton H. Whitmire
      Department of Chemistry MS-60
      Rice University
      1600 Main St. 
      Houtson Tx. 77005
      United States of America
;
_publ_contact_author_email       whitmir@rice.edu
_publ_contact_author_fax         '713 737 5652'
_publ_contact_author_phone       '713 737 5650'
_publ_section_title
;
 Toward Rational Control of Metal Stoichiometry in Heterobimetallic
 Coordination Complexes: Synthesis and Characterization of
 Pb(Hsal)2(Cu(salen*))2, [Pb(NO3)(Cu(salen*))2](NO3),
 Pb(OAc)2(Cu(salen*)), and [Pb(OAc)(Ni(salen*))2](OAc)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2708
_journal_page_last               2713
_journal_paper_doi               10.1021/ic035427w
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C38 H39 N4 Ni2 O11.7 Pb'
_chemical_formula_weight         1064.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 133.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.688(4)
_cell_length_b                   26.355(5)
_cell_length_c                   13.377(3)
_cell_measurement_reflns_used    4707
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.778
_cell_measurement_theta_min      5.186
_cell_volume                     4818(3)
_computing_cell_refinement       'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_data_collection       'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_data_reduction        'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART 1000, CCD'
_diffrn_measurement_method       '2theta, omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9835
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    4.314
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.873851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (sheldrick, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2109
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.579
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+23.0608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                2617
_reflns_number_total             3444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035427wsi20040129_114253_1.cif
_cod_data_source_block           compound4
_cod_original_cell_volume        4818.0(17)
_cod_original_formula_sum        'C38 H39 N4 Ni2 O11.7 Pb1'
_cod_database_code               4310862