#------------------------------------------------------------------------------
#$Date: 2020-11-05 10:56:28 +0200 (Thu, 05 Nov 2020) $
#$Revision: 258736 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/08/4310865.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_4310865
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            '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/[σ²(Fo²)+(0.0278P)²+0.0265P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.077713(15) 0.456307(14) 0.309665(13) 0.03345(7) Uani 1 1 d . . .
Cu1 Cu 0.08273(5) 0.37756(5) 0.01182(4) 0.03158(12) Uani 1 1 d . . .
O1 O 0.1177(3) 0.5626(3) 0.1287(2) 0.0333(6) Uani 1 1 d . . .
O2 O -0.0330(3) 0.3127(3) 0.0922(2) 0.0329(6) Uani 1 1 d . . .
O3 O -0.2064(3) 0.2824(3) 0.2099(2) 0.0407(7) Uani 1 1 d . . .
O4 O 0.1850(3) 0.7643(3) 0.3389(3) 0.0448(7) Uani 1 1 d . . .
O11 O 0.2735(3) 0.4037(3) 0.2321(3) 0.0531(8) Uani 1 1 d . . .
O12 O 0.3477(3) 0.5542(4) 0.4185(3) 0.0580(9) Uani 1 1 d . . .
O21 O 0.1015(4) 0.2515(3) 0.3323(3) 0.0567(9) Uani 1 1 d . . .
O22 O 0.0859(5) 0.3826(4) 0.5050(3) 0.0737(11) Uani 1 1 d . . .
O100 O 0.5598(5) 0.7748(5) 0.6016(4) 0.0983(14) Uani 1 1 d . . .
N1 N 0.2058(3) 0.4322(3) -0.0688(3) 0.0342(8) Uani 1 1 d . . .
N2 N 0.0540(3) 0.1951(3) -0.1099(3) 0.0329(8) Uani 1 1 d . . .
C1 C 0.2356(4) 0.6574(4) 0.1602(4) 0.0326(9) Uani 1 1 d . . .
C2 C 0.2742(4) 0.7705(4) 0.2730(4) 0.0366(10) Uani 1 1 d . . .
C3 C 0.3920(5) 0.8757(5) 0.3099(4) 0.0547(13) Uani 1 1 d . . .
H3A H 0.4153 0.9487 0.3841 0.066 Uiso 1 1 calc R . .
C4 C 0.4765(6) 0.8734(6) 0.2367(5) 0.0634(16) Uani 1 1 d . . .
H4A H 0.5556 0.9454 0.2614 0.076 Uiso 1 1 calc R . .
C5 C 0.4437(5) 0.7668(5) 0.1296(4) 0.0514(13) Uani 1 1 d . . .
H5A H 0.5014 0.7662 0.0814 0.062 Uiso 1 1 calc R . .
C6 C 0.3240(4) 0.6561(4) 0.0886(4) 0.0372(10) Uani 1 1 d . . .
C7 C 0.2983(4) 0.5467(5) -0.0260(4) 0.0409(11) Uani 1 1 d . . .
H7A H 0.3532 0.5600 -0.0730 0.049 Uiso 1 1 calc R . .
C8 C 0.1809(5) 0.3286(4) -0.1890(4) 0.0432(11) Uani 1 1 d . . .
H8A H 0.2649 0.3393 -0.2139 0.052 Uiso 1 1 calc R . .
H8B H 0.1020 0.3376 -0.2459 0.052 Uiso 1 1 calc R . .
C9 C 0.1471(5) 0.1894(4) -0.1838(4) 0.0418(10) Uani 1 1 d . . .
H9A H 0.1002 0.1187 -0.2639 0.050 Uiso 1 1 calc R . .
H9B H 0.2340 0.1678 -0.1494 0.050 Uiso 1 1 calc R . .
C10 C -0.0328(4) 0.0853(4) -0.1258(4) 0.0359(10) Uani 1 1 d . . .
H10A H -0.0363 0.0043 -0.1881 0.043 Uiso 1 1 calc R . .
C11 C -0.1248(4) 0.0779(4) -0.0548(3) 0.0327(9) Uani 1 1 d . . .
C12 C -0.2212(4) -0.0497(4) -0.0925(4) 0.0388(10) Uani 1 1 d . . .
H12A H -0.2216 -0.1239 -0.1597 0.047 Uiso 1 1 calc R . .
C13 C -0.3133(5) -0.0652(4) -0.0317(4) 0.0439(11) Uani 1 1 d . . .
H13A H -0.3777 -0.1493 -0.0586 0.053 Uiso 1 1 calc R . .
C14 C -0.3120(4) 0.0431(4) 0.0700(4) 0.0395(10) Uani 1 1 d . . .
H14A H -0.3750 0.0318 0.1114 0.047 Uiso 1 1 calc R . .
C15 C -0.2161(4) 0.1689(4) 0.1099(4) 0.0327(9) Uani 1 1 d . . .
C16 C -0.1214(4) 0.1887(4) 0.0484(3) 0.0285(9) Uani 1 1 d . . .
C17 C 0.2387(5) 0.8446(5) 0.4637(4) 0.0539(13) Uani 1 1 d . . .
H17A H 0.1666 0.8316 0.4998 0.081 Uiso 1 1 calc R . .
H17B H 0.2658 0.9397 0.4781 0.081 Uiso 1 1 calc R . .
H17C H 0.3201 0.8171 0.4979 0.081 Uiso 1 1 calc R . .
C18 C -0.2732(5) 0.2634(5) 0.2919(4) 0.0552(13) Uani 1 1 d . . .
H18A H -0.2580 0.3502 0.3571 0.083 Uiso 1 1 calc R . .
H18B H -0.2335 0.2018 0.3223 0.083 Uiso 1 1 calc R . .
H18C H -0.3734 0.2253 0.2519 0.083 Uiso 1 1 calc R . .
C21 C 0.1031(5) 0.2763(5) 0.4385(4) 0.0403(10) Uani 1 1 d . . .
C22 C 0.1315(6) 0.1650(5) 0.4816(5) 0.0632(15) Uani 1 1 d . . .
H22A H 0.1305 0.1932 0.5629 0.095 Uiso 1 1 calc R . .
H22B H 0.2229 0.1493 0.4777 0.095 Uiso 1 1 calc R . .
H22C H 0.0593 0.0818 0.4316 0.095 Uiso 1 1 calc R . .
C31 C 0.3709(5) 0.4910(5) 0.3227(5) 0.0455(11) Uani 1 1 d . . .
C32 C 0.5181(5) 0.5221(6) 0.3141(6) 0.0749(17) Uani 1 1 d . . .
H32A H 0.5798 0.4874 0.3617 0.112 Uiso 1 1 calc R . .
H32B H 0.5532 0.6196 0.3431 0.112 Uiso 1 1 calc R . .
H32C H 0.5154 0.4793 0.2320 0.112 Uiso 1 1 calc R . .
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'
Cu Cu 0.3201 1.2651 '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
O21 Pb1 O11 77.48(12) . . ?
O21 Pb1 O2 86.87(11) . . ?
O11 Pb1 O2 74.23(10) . . ?
O21 Pb1 O12 88.27(12) . . ?
O11 Pb1 O12 51.62(12) . . ?
O2 Pb1 O12 125.32(11) . . ?
O21 Pb1 C31 84.40(13) . . ?
O11 Pb1 C31 25.91(13) . . ?
O2 Pb1 C31 99.47(13) . . ?
O12 Pb1 C31 25.91(12) . . ?
O2 Cu1 O1 89.90(11) . . ?
O2 Cu1 N1 175.87(13) . . ?
O1 Cu1 N1 92.84(13) . . ?
O2 Cu1 N2 93.18(13) . . ?
O1 Cu1 N2 176.92(12) . . ?
N1 Cu1 N2 84.08(14) . . ?
C1 O1 Cu1 123.1(3) . . ?
C16 O2 Cu1 126.0(2) . . ?
C16 O2 Pb1 123.4(2) . . ?
Cu1 O2 Pb1 106.69(11) . . ?
C15 O3 C18 118.0(3) . . ?
C2 O4 C17 117.3(3) . . ?
C31 O11 Pb1 96.4(3) . . ?
C31 O12 Pb1 89.4(3) . . ?
C21 O21 Pb1 104.4(3) . . ?
C7 N1 C8 121.9(4) . . ?
C7 N1 Cu1 125.6(3) . . ?
C8 N1 Cu1 112.5(3) . . ?
C10 N2 C9 120.5(4) . . ?
C10 N2 Cu1 126.3(3) . . ?
C9 N2 Cu1 113.1(3) . . ?
O1 C1 C6 124.6(4) . . ?
O1 C1 C2 118.0(4) . . ?
C6 C1 C2 117.4(4) . . ?
O4 C2 C3 124.2(4) . . ?
O4 C2 C1 114.4(3) . . ?
C3 C2 C1 121.4(4) . . ?
C2 C3 C4 120.2(5) . . ?
C5 C4 C3 119.9(4) . . ?
C4 C5 C6 121.7(5) . . ?
C1 C6 C5 119.4(4) . . ?
C1 C6 C7 122.9(4) . . ?
C5 C6 C7 117.7(4) . . ?
N1 C7 C6 125.2(4) . . ?
N1 C8 C9 107.1(3) . . ?
N2 C9 C8 108.1(4) . . ?
N2 C10 C11 125.3(4) . . ?
C16 C11 C12 119.7(4) . . ?
C16 C11 C10 123.5(4) . . ?
C12 C11 C10 116.8(4) . . ?
C13 C12 C11 120.7(4) . . ?
C12 C13 C14 120.5(4) . . ?
C13 C14 C15 119.7(4) . . ?
O3 C15 C14 124.1(4) . . ?
O3 C15 C16 114.7(3) . . ?
C14 C15 C16 121.2(4) . . ?
O2 C16 C15 117.6(4) . . ?
O2 C16 C11 124.2(3) . . ?
C15 C16 C11 118.2(3) . . ?
O22 C21 O21 123.7(4) . . ?
O22 C21 C22 120.6(4) . . ?
O21 C21 C22 115.7(4) . . ?
O12 C31 O11 121.6(4) . . ?
O12 C31 C32 119.4(5) . . ?
O11 C31 C32 119.0(5) . . ?
O12 C31 Pb1 64.7(2) . . ?
O11 C31 Pb1 57.7(2) . . ?
C32 C31 Pb1 169.4(3) . . ?
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 O21 2.356(3) . ?
Pb1 O11 2.433(3) . ?
Pb1 O2 2.479(3) . ?
Pb1 O12 2.584(3) . ?
Pb1 C31 2.860(5) . ?
Cu1 O2 1.923(3) . ?
Cu1 O1 1.928(3) . ?
Cu1 N1 1.929(3) . ?
Cu1 N2 1.940(3) . ?
O1 C1 1.322(4) . ?
O2 C16 1.336(4) . ?
O3 C15 1.376(5) . ?
O3 C18 1.413(5) . ?
O4 C2 1.366(5) . ?
O4 C17 1.413(5) . ?
O11 C31 1.257(5) . ?
O12 C31 1.249(6) . ?
O21 C21 1.261(5) . ?
O22 C21 1.214(6) . ?
N1 C7 1.281(5) . ?
N1 C8 1.459(5) . ?
N2 C10 1.287(5) . ?
N2 C9 1.457(5) . ?
C1 C6 1.402(6) . ?
C1 C2 1.420(6) . ?
C2 C3 1.373(6) . ?
C3 C4 1.387(7) . ?
C4 C5 1.348(7) . ?
C5 C6 1.413(6) . ?
C6 C7 1.433(6) . ?
C8 C9 1.519(6) . ?
C10 C11 1.442(6) . ?
C11 C16 1.402(6) . ?
C11 C12 1.413(5) . ?
C12 C13 1.361(6) . ?
C13 C14 1.383(6) . ?
C14 C15 1.391(5) . ?
C15 C16 1.399(5) . ?
C21 C22 1.514(6) . ?
C31 C32 1.502(7) . ?
