#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/08/4310862.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4310862
loop_
_publ_author_name
'John H. Thurston'
'Christopher G.-Z. Tang'
'Daniel W. Trahan'
'Kenton H. Whitmire'
_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/[σ²(Fo²)+(0.1012P)²+23.0608P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.0000 0.14455(2) 0.2500 0.0567(3) Uani 1 2 d S . .
Ni1 Ni 0.13171(9) 0.25870(5) 0.34056(14) 0.0526(4) Uani 1 1 d . . .
O1 O 0.1230(5) 0.1986(3) 0.2622(8) 0.0574(19) Uani 1 1 d . . .
O2 O 0.1105(5) 0.2173(3) 0.4291(7) 0.0555(18) Uani 1 1 d . . .
O3 O 0.1419(7) 0.1058(4) 0.2225(11) 0.087(3) Uani 1 1 d . . .
O4 O 0.0848(7) 0.1457(4) 0.5314(10) 0.083(3) Uani 1 1 d . . .
O21 O 0.0664(9) 0.0522(4) 0.3569(12) 0.106(3) Uani 1 1 d . . .
C1 C 0.1444(8) 0.1922(5) 0.1867(12) 0.063(3) Uani 1 1 d . . .
C2 C 0.1548(9) 0.1427(6) 0.1622(13) 0.074(4) Uani 1 1 d . . .
C3 C 0.1757(10) 0.1330(8) 0.0821(16) 0.104(6) Uani 1 1 d . . .
H3A H 0.1825 0.0999 0.0651 0.125 Uiso 1 1 calc R . .
C4 C 0.1864(12) 0.1760(11) 0.0259(17) 0.114(7) Uani 1 1 d . . .
H4A H 0.1984 0.1709 -0.0303 0.137 Uiso 1 1 calc R . .
C5 C 0.1794(11) 0.2206(8) 0.0532(16) 0.095(5) Uani 1 1 d . . .
H5A H 0.1881 0.2473 0.0170 0.115 Uiso 1 1 calc R . .
C6 C 0.1596(8) 0.2325(7) 0.1339(12) 0.074(4) Uani 1 1 d . . .
C7 C 0.1582(9) 0.2836(6) 0.1634(15) 0.077(4) Uani 1 1 d . . .
H7A H 0.1659 0.3083 0.1217 0.092 Uiso 1 1 calc R . .
C8 C 0.1411(13) 0.3535(6) 0.259(2) 0.108(6) Uani 1 1 d . . .
H8A H 0.1807 0.3726 0.2493 0.129 Uiso 1 1 calc R . .
H8B H 0.0739 0.3650 0.1891 0.129 Uiso 1 1 calc R . .
C9 C 0.1776(11) 0.3610(5) 0.397(2) 0.098(5) Uani 1 1 d . . .
H9A H 0.2485 0.3627 0.4645 0.118 Uiso 1 1 calc R . .
H9B H 0.1520 0.3924 0.3997 0.118 Uiso 1 1 calc R . .
C10 C 0.1273(9) 0.3220(7) 0.5047(16) 0.094(5) Uani 1 1 d . . .
H10A H 0.1304 0.3545 0.5343 0.112 Uiso 1 1 calc R . .
C11 C 0.1048(8) 0.2807(6) 0.5522(13) 0.074(4) Uani 1 1 d . . .
C12 C 0.0917(9) 0.2911(9) 0.6445(15) 0.107(7) Uani 1 1 d . . .
H12A H 0.0936 0.3246 0.6684 0.128 Uiso 1 1 calc R . .
C13 C 0.0770(12) 0.2546(10) 0.6960(18) 0.111(7) Uani 1 1 d . . .
H13A H 0.0682 0.2617 0.7552 0.133 Uiso 1 1 calc R . .
C14 C 0.0751(9) 0.2079(8) 0.6607(15) 0.095(5) Uani 1 1 d . . .
H14A H 0.0657 0.1819 0.6978 0.114 Uiso 1 1 calc R . .
C15 C 0.0861(8) 0.1948(7) 0.5717(12) 0.072(4) Uani 1 1 d . . .
C16 C 0.1008(7) 0.2310(5) 0.5162(11) 0.060(3) Uani 1 1 d . . .
C17 C 0.0905(13) 0.1030(7) 0.6049(18) 0.120(7) Uani 1 1 d . . .
H17A H 0.0888 0.0719 0.5659 0.180 Uiso 1 1 calc R . .
H17B H 0.0359 0.1040 0.5982 0.180 Uiso 1 1 calc R . .
H17C H 0.1504 0.1048 0.6993 0.180 Uiso 1 1 calc R . .
C18 C 0.1697(14) 0.0545(6) 0.225(2) 0.121(6) Uani 1 1 d . . .
H18A H 0.1571 0.0328 0.2688 0.181 Uiso 1 1 calc R . .
H18B H 0.2381 0.0535 0.2736 0.181 Uiso 1 1 calc R . .
H18C H 0.1323 0.0430 0.1325 0.181 Uiso 1 1 calc R . .
C21 C 0.0000 0.0303(8) 0.2500 0.091(6) Uani 1 2 d S . .
C22 C 0.0000 -0.0276(8) 0.2500 0.179(16) Uani 1 2 d S . .
H22A H -0.0556 -0.0397 0.1603 0.268 Uiso 0.50 1 calc PR . .
H22B H -0.0033 -0.0397 0.3144 0.268 Uiso 0.50 1 calc PR . .
H22C H 0.0589 -0.0397 0.2753 0.268 Uiso 0.50 1 calc PR . .
N1 N 0.1474(7) 0.2985(4) 0.2424(11) 0.071(3) Uani 1 1 d . . .
N2 N 0.1436(7) 0.3173(4) 0.4237(11) 0.071(3) Uani 1 1 d . . .
O31 O 0.2396(13) 0.0032(7) 0.5597(19) 0.050 Uiso 0.372(14) 1 d P . .
O33 O 0.5515(18) 0.0586(9) 0.983(3) 0.050 Uiso 0.265(14) 1 d P . .
O32 O 0.3594(18) 0.0261(10) 0.835(3) 0.050 Uiso 0.266(14) 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O1 113.9(3) 2 . ?
O1 Pb1 O2 76.7(2) 2 . ?
O1 Pb1 O2 55.6(2) . . ?
O1 Pb1 O2 55.6(2) 2 2 ?
O1 Pb1 O2 76.7(2) . 2 ?
O2 Pb1 O2 86.5(3) . 2 ?
O1 Pb1 O21 113.4(3) 2 2 ?
O1 Pb1 O21 126.9(3) . 2 ?
O2 Pb1 O21 160.6(3) . 2 ?
O2 Pb1 O21 112.8(3) 2 2 ?
O1 Pb1 O21 126.9(3) 2 . ?
O1 Pb1 O21 113.4(3) . . ?
O2 Pb1 O21 112.8(3) . . ?
O2 Pb1 O21 160.6(3) 2 . ?
O21 Pb1 O21 47.8(5) 2 . ?
N2 Ni1 O2 95.7(5) . . ?
N2 Ni1 O1 178.1(4) . . ?
O2 Ni1 O1 83.2(3) . . ?
N2 Ni1 N1 86.6(6) . . ?
O2 Ni1 N1 176.8(4) . . ?
O1 Ni1 N1 94.5(5) . . ?
C1 O1 Ni1 125.9(8) . . ?
C1 O1 Pb1 126.3(7) . . ?
Ni1 O1 Pb1 103.7(3) . . ?
C16 O2 Ni1 127.8(8) . . ?
C16 O2 Pb1 119.9(7) . . ?
Ni1 O2 Pb1 103.0(3) . . ?
C2 O3 C18 117.8(12) . . ?
C15 O4 C17 118.9(13) . . ?
C21 O21 Pb1 94.2(11) . . ?
O1 C1 C2 117.6(12) . . ?
O1 C1 C6 123.7(13) . . ?
C2 C1 C6 118.7(12) . . ?
O3 C2 C1 114.4(11) . . ?
O3 C2 C3 124.7(15) . . ?
C1 C2 C3 120.9(15) . . ?
C2 C3 C4 117.7(17) . . ?
C5 C4 C3 120.0(17) . . ?
C4 C5 C6 124.6(18) . . ?
C5 C6 C7 119.8(15) . . ?
C5 C6 C1 118.0(16) . . ?
C7 C6 C1 122.1(12) . . ?
N1 C7 C6 125.1(13) . . ?
C9 C8 N1 107.3(13) . . ?
N2 C9 C8 107.0(12) . . ?
N2 C10 C11 125.9(13) . . ?
C16 C11 C12 118.7(16) . . ?
C16 C11 C10 121.3(12) . . ?
C12 C11 C10 119.9(16) . . ?
C13 C12 C11 121.7(19) . . ?
C14 C13 C12 117.6(18) . . ?
C13 C14 C15 124.0(18) . . ?
C16 C15 C14 120.3(16) . . ?
C16 C15 O4 113.6(11) . . ?
C14 C15 O4 126.1(15) . . ?
C15 C16 O2 119.0(12) . . ?
C15 C16 C11 117.6(13) . . ?
O2 C16 C11 123.4(12) . . ?
O21 C21 O21 124(2) . 2 ?
O21 C21 C22 118.2(10) . . ?
O21 C21 C22 118.2(10) 2 . ?
C7 N1 C8 119.9(13) . . ?
C7 N1 Ni1 127.4(10) . . ?
C8 N1 Ni1 112.6(11) . . ?
C10 N2 C9 120.7(14) . . ?
C10 N2 Ni1 125.4(11) . . ?
C9 N2 Ni1 113.9(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.613(7) 2 ?
Pb1 O1 2.613(7) . ?
Pb1 O2 2.633(7) . ?
Pb1 O2 2.633(7) 2 ?
Pb1 O21 2.663(10) 2 ?
Pb1 O21 2.663(10) . ?
Ni1 N2 1.826(11) . ?
Ni1 O2 1.841(7) . ?
Ni1 O1 1.844(8) . ?
Ni1 N1 1.854(11) . ?
O1 C1 1.325(14) . ?
O2 C16 1.346(13) . ?
O3 C2 1.387(16) . ?
O3 C18 1.440(16) . ?
O4 C15 1.396(17) . ?
O4 C17 1.451(17) . ?
O21 C21 1.224(13) . ?
C1 C2 1.390(17) . ?
C1 C6 1.409(18) . ?
C2 C3 1.39(2) . ?
C3 C4 1.45(3) . ?
C4 C5 1.26(3) . ?
C5 C6 1.40(2) . ?
C6 C7 1.41(2) . ?
C7 N1 1.267(17) . ?
C8 C9 1.48(3) . ?
C8 N1 1.481(18) . ?
C9 N2 1.476(18) . ?
C10 N2 1.317(19) . ?
C10 C11 1.46(2) . ?
C11 C16 1.378(18) . ?
C11 C12 1.44(2) . ?
C12 C13 1.32(3) . ?
C13 C14 1.31(2) . ?
C14 C15 1.38(2) . ?
C15 C16 1.346(18) . ?
C21 O21 1.224(13) 2 ?
C21 C22 1.52(3) . ?
