#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:05:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180025 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/19/7031988.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_7031988
loop_
_publ_author_name
'Zhang, Kun'
'Geng, Jiao'
'Jin, Chao'
'Huang, Wei'
_publ_section_title
;
 Distinguishable Zn(ii) and Pb(ii) template effects on forming
 pendant-armed Schiff-base macrocyclic complexes including a remarkable
 Pb(ii)-π macrocyclic complex.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15351
_journal_page_last               15358
_journal_paper_doi               10.1039/c4dt01927j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C27 H26 Cl2 N3 O2 Pb, N O3'
_chemical_formula_sum            'C27 H26 Cl2 N4 O5 Pb'
_chemical_formula_weight         764.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 98.762(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.254(8)
_cell_length_b                   10.682(3)
_cell_length_c                   13.612(4)
_cell_measurement_reflns_used    3893
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      24.825
_cell_measurement_theta_min      2.548
_cell_volume                     2910.6(17)
_computing_cell_refinement       'SMART APEX2 V2011.4-1'
_computing_data_collection       'SMART (BRUKER 2000)'
_computing_data_reduction        'SAINT V6.02A (BRUKER 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL V6.10 (BRUKER 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7752
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.023
_exptl_absorpt_correction_T_max  0.5842
_exptl_absorpt_correction_T_min  0.5842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            'orange yellow'
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.486
_refine_diff_density_min         -3.031
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2696
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0691
_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)+(0.0498P)²+94.6839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                2349
_reflns_number_total             2696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01927j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7031985--7031989.cif.'
_cod_original_cell_volume        2910.6(16)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7031988
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Pb1 Pb 0.11686(4) 0.0000 0.60010(5) 0.0447(3) Uani 1 2 d S
C1 C 0.2564(6) 0.1539(9) 0.6730(8) 0.036(2) Uani 1 1 d .
C2 C 0.2449(6) 0.1852(10) 0.7718(8) 0.035(2) Uani 1 1 d .
C3 C 0.2979(6) 0.2189(11) 0.8434(9) 0.045(3) Uani 1 1 d .
H3 H 0.2900 0.2436 0.9061 0.053 Uiso 1 1 calc R
C4 C 0.3608(6) 0.2162(13) 0.8227(8) 0.049(3) Uani 1 1 d .
C5 C 0.3745(6) 0.1794(11) 0.7290(9) 0.046(3) Uani 1 1 d .
H5 H 0.4184 0.1767 0.7163 0.055 Uiso 1 1 calc R
C6 C 0.3231(6) 0.1477(10) 0.6567(8) 0.037(3) Uani 1 1 d .
C7 C 0.1785(6) 0.1829(11) 0.8014(9) 0.045(3) Uani 1 1 d .
H7 H 0.1735 0.2248 0.8597 0.054 Uiso 1 1 calc R
C8 C 0.0668(7) 0.1212(14) 0.8071(11) 0.061(4) Uani 1 1 d .
H8A H 0.0266 0.1251 0.7583 0.074 Uiso 1 1 calc R
H8B H 0.0666 0.1922 0.8514 0.074 Uiso 1 1 calc R
C9 C 0.0669(11) 0.0000 0.8667(17) 0.069(6) Uani 1 2 d S
H9A H 0.1059 0.0000 0.9177 0.083 Uiso 1 2 calc SR
H9B H 0.0278 0.0000 0.9000 0.083 Uiso 1 2 calc SR
C10 C 0.3368(6) 0.1193(11) 0.5532(9) 0.045(3) Uani 1 1 d .
H10A H 0.3846 0.1114 0.5545 0.054 Uiso 1 1 calc R
H10B H 0.3213 0.1888 0.5098 0.054 Uiso 1 1 calc R
C11 C 0.2977(8) 0.0000 0.3985(13) 0.058(5) Uani 1 2 d SD
H11A H 0.2735 0.0736 0.3711 0.070 Uiso 0.50 1 calc PR
H11B H 0.2735 -0.0736 0.3711 0.070 Uiso 0.50 1 calc PR
C12 C 0.3680(8) 0.0000 0.3715(12) 0.058(6) Uani 1 2 d SD
H12A H 0.3924 -0.0738 0.3979 0.069 Uiso 0.50 1 calc PR
H12B H 0.3924 0.0738 0.3979 0.069 Uiso 0.50 1 calc PR
C13 C 0.3586(12) 0.0000 0.2575(12) 0.064(6) Uani 1 2 d SD
C14 C 0.2975(12) 0.0000 0.1848(15) 0.060(5) Uani 1 2 d S
H14 H 0.2570 0.0000 0.2091 0.072 Uiso 1 2 calc SR
C15 C 0.2952(16) 0.0000 0.0804(17) 0.078(7) Uani 1 2 d S
H15 H 0.2547 0.0000 0.0377 0.093 Uiso 1 2 calc SR
C16 C 0.355(2) 0.0000 0.0445(18) 0.099(11) Uani 1 2 d S
H16 H 0.3556 0.0000 -0.0237 0.119 Uiso 1 2 calc SR
C17 C 0.4123(19) 0.0000 0.107(2) 0.098(10) Uani 1 2 d S
H17 H 0.4523 0.0000 0.0814 0.117 Uiso 1 2 calc SR
C18 C 0.4141(14) 0.0000 0.2092(17) 0.076(7) Uani 1 2 d S
H18 H 0.4558 0.0000 0.2486 0.091 Uiso 1 2 calc SR
Cl1 Cl 0.4277(2) 0.2580(5) 0.9158(3) 0.0837(14) Uani 1 1 d .
N1 N 0.1267(5) 0.1291(10) 0.7551(7) 0.045(2) Uani 1 1 d .
N2 N 0.3029(7) 0.0000 0.5114(9) 0.040(3) Uani 1 2 d S
N3 N 0.0000 0.235(2) 0.5000 0.20(3) Uani 1 2 d S
O1 O 0.2082(4) 0.1325(7) 0.5996(6) 0.0411(18) Uani 1 1 d .
H1A H 0.2274 0.1074 0.5519 0.062 Uiso 0.50 1 d PR
O2 O 0.0266(14) 0.192(3) 0.445(2) 0.212(12) Uani 1 1 d .
O3 O 0.0000 0.346(6) 0.5000 0.29(3) Uani 1 2 d S
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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
H H 0.0000 0.0000 '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
O1 Pb1 O1 74.8(4) . 6
O1 Pb1 N1 72.9(3) . .
O1 Pb1 N1 112.1(3) 6 .
O1 Pb1 N1 112.1(3) . 6
O1 Pb1 N1 72.9(3) 6 6
N1 Pb1 N1 66.9(5) . 6
O1 Pb1 O2 89.0(5) . .
O1 Pb1 O2 137.7(5) 6 .
N1 Pb1 O2 99.4(6) . .
N1 Pb1 O2 148.2(5) 6 .
O1 C1 C6 119.7(9) . .
O1 C1 C2 123.2(10) . .
C6 C1 C2 117.1(10) . .
C3 C2 C1 120.0(10) . .
C3 C2 C7 117.3(10) . .
C1 C2 C7 122.7(11) . .
C4 C3 C2 120.3(11) . .
C4 C3 H3 119.8 . .
C2 C3 H3 119.8 . .
C3 C4 C5 121.4(11) . .
C3 C4 Cl1 119.4(9) . .
C5 C4 Cl1 119.1(10) . .
C6 C5 C4 119.4(11) . .
C6 C5 H5 120.3 . .
C4 C5 H5 120.3 . .
C5 C6 C1 121.5(10) . .
C5 C6 C10 119.7(11) . .
C1 C6 C10 118.4(10) . .
N1 C7 C2 126.4(11) . .
N1 C7 H7 116.8 . .
C2 C7 H7 116.8 . .
N1 C8 C9 111.3(12) . .
N1 C8 H8A 109.4 . .
C9 C8 H8A 109.4 . .
N1 C8 H8B 109.4 . .
C9 C8 H8B 109.4 . .
H8A C8 H8B 108.0 . .
C8 C9 C8 115.8(18) 6 .
C8 C9 H9A 108.3 6 .
C8 C9 H9A 108.3 . .
C8 C9 H9B 108.3 6 .
C8 C9 H9B 108.3 . .
H9A C9 H9B 107.4 . .
C6 C10 N2 112.5(9) . .
C6 C10 H10A 109.1 . .
N2 C10 H10A 109.1 . .
C6 C10 H10B 109.1 . .
N2 C10 H10B 109.1 . .
H10A C10 H10B 107.8 . .
N2 C11 C12 108.6(13) . .
N2 C11 H11A 110.0 . .
C12 C11 H11A 110.0 . .
N2 C11 H11B 110.0 . .
C12 C11 H11B 110.0 . .
H11A C11 H11B 108.3 . .
C11 C12 C13 105.5(15) . .
C11 C12 H12A 110.6 . .
C13 C12 H12A 110.6 . .
C11 C12 H12B 110.6 . .
C13 C12 H12B 110.6 . .
H12A C12 H12B 108.8 . .
C18 C13 C14 110.0(17) . .
C18 C13 C12 120(2) . .
C14 C13 C12 130.3(18) . .
C15 C14 C13 125(2) . .
C15 C14 H14 117.4 . .
C13 C14 H14 117.4 . .
C16 C15 C14 117(3) . .
C16 C15 H15 121.3 . .
C14 C15 H15 121.3 . .
C17 C16 C15 120(2) . .
C17 C16 H16 119.9 . .
C15 C16 H16 119.9 . .
C16 C17 C18 122(3) . .
C16 C17 H17 119.0 . .
C18 C17 H17 119.0 . .
C13 C18 C17 125(3) . .
C13 C18 H18 117.4 . .
C17 C18 H18 117.4 . .
C7 N1 C8 117.2(11) . .
C7 N1 Pb1 128.3(8) . .
C8 N1 Pb1 113.6(8) . .
C10 N2 C10 114.3(14) . 6
C10 N2 C11 109.7(7) . .
C10 N2 C11 109.7(7) 6 .
O2 N3 O2 130(4) . 2_556
O2 N3 O3 115.1(19) . .
O2 N3 O3 115.1(19) 2_556 .
C1 O1 Pb1 127.2(6) . .
C1 O1 H1A 105.3 . .
Pb1 O1 H1A 105.4 . .
N3 O2 Pb1 96.2(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.331(8) .
Pb1 O1 2.331(8) 6
Pb1 N1 2.503(10) .
Pb1 N1 2.503(10) 6
Pb1 O2 3.29(3) .
C1 O1 1.306(14) .
C1 C6 1.404(16) .
C1 C2 1.439(14) .
C2 C3 1.383(17) .
C2 C7 1.461(16) .
C3 C4 1.347(17) .
C3 H3 0.9300 .
C4 C5 1.402(17) .
C4 Cl1 1.765(12) .
C5 C6 1.363(17) .
C5 H5 0.9300 .
C6 C10 1.507(15) .
C7 N1 1.275(16) .
C7 H7 0.9300 .
C8 N1 1.497(15) .
C8 C9 1.528(18) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C8 1.528(18) 6
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 N2 1.518(14) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 N2 1.52(2) .
C11 C12 1.524(10) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.534(10) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C18 1.39(3) .
C13 C14 1.46(3) .
C14 C15 1.42(3) .
C14 H14 0.9300 .
C15 C16 1.38(4) .
C15 H15 0.9300 .
C16 C17 1.33(5) .
C16 H16 0.9300 .
C17 C18 1.39(3) .
C17 H17 0.9300 .
C18 H18 0.9300 .
N2 C10 1.518(14) 6
N3 O2 1.09(3) .
N3 O2 1.09(3) 2_556
N3 O3 1.18(6) .
O1 H1A 0.8500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 C1 C2 C3 -173.4(10) . .
C6 C1 C2 C3 6.0(15) . .
O1 C1 C2 C7 6.7(16) . .
C6 C1 C2 C7 -173.9(10) . .
C1 C2 C3 C4 -3.6(18) . .
C7 C2 C3 C4 176.3(11) . .
C2 C3 C4 C5 0(2) . .
C2 C3 C4 Cl1 -179.3(10) . .
C3 C4 C5 C6 1(2) . .
Cl1 C4 C5 C6 -179.7(10) . .
C4 C5 C6 C1 1.6(18) . .
C4 C5 C6 C10 174.5(11) . .
O1 C1 C6 C5 174.4(10) . .
C2 C1 C6 C5 -5.0(16) . .
O1 C1 C6 C10 1.4(15) . .
C2 C1 C6 C10 -178.0(9) . .
C3 C2 C7 N1 -163.3(12) . .
C1 C2 C7 N1 16.5(19) . .
N1 C8 C9 C8 -59(2) . 6
C5 C6 C10 N2 132.6(12) . .
C1 C6 C10 N2 -54.2(15) . .
N2 C11 C12 C13 180.000(2) . .
C11 C12 C13 C18 180.000(2) . .
C11 C12 C13 C14 0.000(2) . .
C18 C13 C14 C15 0.000(2) . .
C12 C13 C14 C15 180.000(2) . .
C13 C14 C15 C16 0.000(1) . .
C14 C15 C16 C17 0.000(2) . .
C15 C16 C17 C18 0.0 . .
C14 C13 C18 C17 0.000(2) . .
C12 C13 C18 C17 180.000(2) . .
C16 C17 C18 C13 0.000(2) . .
C2 C7 N1 C8 170.4(12) . .
C2 C7 N1 Pb1 2.4(18) . .
C9 C8 N1 C7 -91.4(16) . .
C9 C8 N1 Pb1 78.4(15) . .
O1 Pb1 N1 C7 -24.3(10) . .
O1 Pb1 N1 C7 40.8(11) 6 .
N1 Pb1 N1 C7 99.6(10) 6 .
O2 Pb1 N1 C7 -110.4(11) . .
O1 Pb1 N1 C8 167.3(9) . .
O1 Pb1 N1 C8 -127.6(8) 6 .
N1 Pb1 N1 C8 -68.8(9) 6 .
O2 Pb1 N1 C8 81.3(9) . .
C6 C10 N2 C10 -76.1(15) . 6
C6 C10 N2 C11 160.3(11) . .
C12 C11 N2 C10 63.1(9) . .
C12 C11 N2 C10 -63.1(9) . 6
C6 C1 O1 Pb1 131.2(9) . .
C2 C1 O1 Pb1 -49.4(13) . .
O1 Pb1 O1 C1 -72.2(9) 6 .
N1 Pb1 O1 C1 47.1(8) . .
N1 Pb1 O1 C1 -8.2(9) 6 .
O2 Pb1 O1 C1 147.3(10) . .
O2 N3 O2 Pb1 -50.1(5) 2_556 .
O3 N3 O2 Pb1 129.9(5) . .
O1 Pb1 O2 N3 -103(2) . .
O1 Pb1 O2 N3 -168.8(15) 6 .
N1 Pb1 O2 N3 -30(2) . .
N1 Pb1 O2 N3 30(3) 6 .
