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_4310865
_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            'C22 H24 Cu N2 O9 Pb'
_chemical_formula_weight         731.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.96(3)
_cell_angle_beta                 103.97(3)
_cell_angle_gamma                97.73(3)
_cell_formula_units_Z            2
_cell_length_a                   9.990(2)
_cell_length_b                   10.759(2)
_cell_length_c                   12.576(3)
_cell_measurement_reflns_used    4172
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.559
_cell_measurement_theta_min      4.712
_cell_volume                     1188.0(6)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 1K, 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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5168
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    8.027
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.582907
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            crimson
_exptl_crystal_density_diffrn    2.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+0.0265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0509
_reflns_number_gt                3167
_reflns_number_total             3387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035427wsi20040129_114253_4.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multiscan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

2020-11-04
Z value changed to be consistent with given formula
                miguel
;
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1188.0(4)
_cod_original_formula_sum        'C22 H24 Cu1 N2 O9 Pb1'
_cod_database_code               4310865