#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:20:16 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180008 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/02/7030249.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_7030249
loop_
_publ_author_name
'Lin, Xiao-Ming'
'Li, Ting-Ting'
'Chen, Lian-Fen'
'Zhang, Li'
'Su, Cheng-Yong'
_publ_section_title
;
 Two ligand-functionalized Pb(II) metal-organic frameworks: structures and
 catalytic performances.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10422
_journal_page_last               10429
_journal_paper_doi               10.1039/c2dt30935a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C29 H29 N5 O11 Pb'
_chemical_formula_weight         830.76
_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                 129.724(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   43.753(3)
_cell_length_b                   7.7050(3)
_cell_length_c                   28.326(2)
_cell_measurement_reflns_used    4028
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.5945
_cell_measurement_theta_min      2.6239
_cell_volume                     7344.6(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10303
_diffrn_reflns_theta_full        62.64
_diffrn_reflns_theta_max         62.64
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    9.437
_exptl_absorpt_correction_T_max  0.4521
_exptl_absorpt_correction_T_min  0.2541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.323
_refine_diff_density_min         -2.975
_refine_diff_density_rms         0.228
_refine_ls_extinction_coef       0.000059(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5758
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0911P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1466
_reflns_number_gt                4093
_reflns_number_total             5758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30935a.txt
_cod_data_source_block           compd2
_cod_original_cell_volume        7344.5(13)
_cod_original_sg_symbol_H-M      ' C2/c'
_cod_database_code               7030249
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
Pb1 Pb 0.724221(10) -1.37372(5) 0.721690(16) 0.01648(17) Uani 1 1 d .
C1 C 0.7126(3) -1.5498(13) 0.7991(4) 0.016(2) Uani 1 1 d U
C2 C 0.7070(3) -1.6480(14) 0.8388(4) 0.022(2) Uani 1 1 d .
C3 C 0.7065(3) -1.8295(13) 0.8382(5) 0.024(2) Uani 1 1 d .
H3A H 0.7100 -1.8894 0.8127 0.029 Uiso 1 1 calc R
C4 C 0.7010(3) -1.9221(14) 0.8728(5) 0.026(2) Uani 1 1 d .
H4A H 0.6995 -2.0451 0.8699 0.031 Uiso 1 1 calc R
C5 C 0.6977(3) -1.8345(13) 0.9138(5) 0.024(2) Uani 1 1 d .
C6 C 0.6977(3) -1.6557(13) 0.9139(5) 0.027(3) Uani 1 1 d .
H6A H 0.6949 -1.5955 0.9402 0.033 Uiso 1 1 calc R
C7 C 0.7018(3) -1.5616(14) 0.8765(5) 0.027(3) Uani 1 1 d .
H7A H 0.7010 -1.4384 0.8765 0.033 Uiso 1 1 calc R
N1 N 0.6942(3) -1.9207(11) 0.9532(4) 0.026(2) Uani 1 1 d .
H1A H 0.6880 -1.8547 0.9714 0.031 Uiso 1 1 calc R
C9 C 0.7011(3) -2.1413(15) 1.0204(5) 0.029(3) Uani 1 1 d .
C10 C 0.7108(4) -2.3129(14) 1.0403(5) 0.032(3) Uani 1 1 d .
H10A H 0.7145 -2.3937 1.0189 0.039 Uiso 1 1 calc R
C11 C 0.7152(3) -2.3654(14) 1.0900(5) 0.028(2) Uani 1 1 d .
H11A H 0.7216 -2.4832 1.1026 0.033 Uiso 1 1 calc R
C12 C 0.7004(3) -2.0879(13) 1.1034(5) 0.024(2) Uani 1 1 d .
H12A H 0.6968 -2.0109 1.1257 0.028 Uiso 1 1 calc R
C13 C 0.6952(3) -2.0293(15) 1.0529(5) 0.028(3) Uani 1 1 d .
H13A H 0.6876 -1.9122 1.0400 0.033 Uiso 1 1 calc R
C14 C 0.3599(3) -0.6422(15) 0.4018(5) 0.028(2) Uani 1 1 d .
C15 C 0.4026(3) -0.6761(16) 0.4471(5) 0.034(3) Uani 1 1 d .
C16 C 0.4264(3) -0.6559(14) 0.4310(5) 0.027(3) Uani 1 1 d .
H16A H 0.4148 -0.6172 0.3909 0.032 Uiso 1 1 calc R
C17 C 0.4673(3) -0.6915(15) 0.4729(5) 0.031(3) Uani 1 1 d .
H17A H 0.4833 -0.6727 0.4616 0.038 Uiso 1 1 calc R
C18 C 0.4842(3) -0.7543(19) 0.5308(5) 0.040(3) Uani 1 1 d .
C19 C 0.4617(4) -0.775(2) 0.5487(7) 0.063(4) Uani 1 1 d U
H19A H 0.4735 -0.8160 0.5888 0.075 Uiso 1 1 calc R
C20 C 0.4205(4) -0.734(2) 0.5064(7) 0.062(4) Uani 1 1 d U
H20A H 0.4048 -0.7470 0.5186 0.074 Uiso 1 1 calc R
C21 C 0.5474(3) -0.8710(16) 0.6246(5) 0.033(3) Uani 1 1 d .
C22 C 0.5895(3) -0.9086(14) 0.6506(5) 0.030(3) Uani 1 1 d .
C23 C 0.6108(3) -0.8094(16) 0.6412(5) 0.030(3) Uani 1 1 d .
H23A H 0.5998 -0.7056 0.6178 0.036 Uiso 1 1 calc R
C24 C 0.6495(3) -0.8610(14) 0.6660(4) 0.022(2) Uani 1 1 d .
H24A H 0.6648 -0.7902 0.6606 0.027 Uiso 1 1 calc R
C25 C 0.6450(3) -1.1083(14) 0.7107(5) 0.025(2) Uani 1 1 d .
H25A H 0.6570 -1.2097 0.7352 0.030 Uiso 1 1 calc R
C26 C 0.6074(3) -1.0569(15) 0.6877(5) 0.029(3) Uani 1 1 d .
H26A H 0.5936 -1.1229 0.6972 0.034 Uiso 1 1 calc R
C8 C 0.6988(4) -2.0873(14) 0.9675(5) 0.034(3) Uani 1 1 d .
N2 N 0.7106(2) -2.2564(11) 1.1215(4) 0.0206(19) Uani 1 1 d .
N3 N 0.5254(3) -0.7948(15) 0.5703(5) 0.042(3) Uani 1 1 d .
H3B H 0.5380 -0.7650 0.5567 0.051 Uiso 1 1 calc R
N4 N 0.6644(2) -1.0089(11) 0.6971(4) 0.0208(19) Uani 1 1 d .
O1 O 0.7071(2) -1.3885(9) 0.7928(3) 0.0232(15) Uani 1 1 d U
O2 O 0.7244(2) -1.6291(9) 0.7744(3) 0.0234(15) Uani 1 1 d .
O3 O 0.7017(4) -2.1984(13) 0.9396(5) 0.073(3) Uani 1 1 d U
O4 O 0.7173(2) -2.3057(9) 1.1720(3) 0.0192(15) Uani 1 1 d .
O5 O 0.34659(19) -0.5872(9) 0.3496(3) 0.0237(17) Uani 1 1 d .
O6 O 0.3375(2) -0.6736(11) 0.4151(4) 0.036(2) Uani 1 1 d .
O7 O 0.5357(2) -0.9157(13) 0.6519(4) 0.050(3) Uani 1 1 d U
O8 O 0.7001(2) -1.0588(9) 0.7171(3) 0.0236(16) Uani 1 1 d .
O9 O 0.4518(3) -0.2384(16) 0.5043(6) 0.080(3) Uani 1 1 d DU
N5 N 0.4337(5) -0.2483(19) 0.5570(9) 0.155(6) Uani 1 1 d DU
C27 C 0.4750(7) -0.265(4) 0.6119(9) 0.191(8) Uani 1 1 d DU
H27A H 0.4908 -0.1744 0.6118 0.287 Uiso 1 1 calc R
H27B H 0.4850 -0.3792 0.6125 0.287 Uiso 1 1 calc R
H27C H 0.4772 -0.2511 0.6483 0.287 Uiso 1 1 calc R
C28 C 0.3927(7) -0.240(4) 0.5378(13) 0.187(8) Uani 1 1 d DU
H28A H 0.3781 -0.1422 0.5097 0.280 Uiso 1 1 calc R
H28B H 0.3948 -0.2247 0.5741 0.280 Uiso 1 1 calc R
H28C H 0.3785 -0.3483 0.5170 0.280 Uiso 1 1 calc R
C29 C 0.4288(6) -0.2363(17) 0.5061(9) 0.123(6) Uani 1 1 d DU
H29 H 0.4024 -0.2251 0.4685 0.148 Uiso 1 1 calc R
O1W O 0.6580(2) 0.6661(10) 0.4826(4) 0.038(2) Uani 1 1 d U
O2W O 0.5832(7) 0.710(3) 0.3631(12) 0.086(7) Uani 0.50 1 d PU
O3W O 0.5770(7) 0.382(3) 0.2628(11) 0.078(6) Uani 0.50 1 d PU
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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
O5 Pb1 O2 85.0(2) 5_636 .
O5 Pb1 O1 77.7(2) 5_636 .
O2 Pb1 O1 51.5(2) . .
O5 Pb1 O8 79.2(2) 5_636 .
O2 Pb1 O8 127.9(2) . .
O1 Pb1 O8 76.6(2) . .
O1 C1 O2 120.9(9) . .
O1 C1 C2 119.6(9) . .
O2 C1 C2 119.4(9) . .
C7 C2 C3 118.5(10) . .
C7 C2 C1 121.2(9) . .
C3 C2 C1 120.3(9) . .
C4 C3 C2 122.0(10) . .
C4 C3 H3A 119.0 . .
C2 C3 H3A 119.0 . .
C3 C4 C5 119.8(10) . .
C3 C4 H4A 120.1 . .
C5 C4 H4A 120.1 . .
C6 C5 N1 118.5(10) . .
C6 C5 C4 118.2(10) . .
N1 C5 C4 123.3(9) . .
C5 C6 C7 121.5(10) . .
C5 C6 H6A 119.2 . .
C7 C6 H6A 119.2 . .
C6 C7 C2 119.9(10) . .
C6 C7 H7A 120.0 . .
C2 C7 H7A 120.0 . .
C8 N1 C5 129.5(9) . .
C8 N1 H1A 115.2 . .
C5 N1 H1A 115.2 . .
C10 C9 C13 117.2(10) . .
C10 C9 C8 118.5(10) . .
C13 C9 C8 124.3(10) . .
C11 C10 C9 120.4(10) . .
C11 C10 H10A 119.8 . .
C9 C10 H10A 119.8 . .
N2 C11 C10 121.8(10) . .
N2 C11 H11A 119.1 . .
C10 C11 H11A 119.1 . .
N2 C12 C13 120.1(9) . .
N2 C12 H12A 120.0 . .
C13 C12 H12A 120.0 . .
C12 C13 C9 120.3(10) . .
C12 C13 H13A 119.9 . .
C9 C13 H13A 119.9 . .
O5 C14 O6 122.8(10) . .
O5 C14 C15 117.3(9) . .
O6 C14 C15 119.9(10) . .
C16 C15 C20 118.0(11) . .
C16 C15 C14 120.0(10) . .
C20 C15 C14 121.9(10) . .
C15 C16 C17 121.3(10) . .
C15 C16 H16A 119.4 . .
C17 C16 H16A 119.4 . .
C18 C17 C16 119.8(10) . .
C18 C17 H17A 120.1 . .
C16 C17 H17A 120.1 . .
C19 C18 C17 120.8(11) . .
C19 C18 N3 122.1(11) . .
C17 C18 N3 117.1(10) . .
C18 C19 C20 118.9(13) . .
C18 C19 H19A 120.6 . .
C20 C19 H19A 120.6 . .
C15 C20 C19 121.1(12) . .
C15 C20 H20A 119.4 . .
C19 C20 H20A 119.4 . .
O7 C21 N3 125.2(10) . .
O7 C21 C22 120.8(10) . .
N3 C21 C22 113.9(9) . .
C23 C22 C26 118.5(10) . .
C23 C22 C21 125.0(11) . .
C26 C22 C21 116.5(10) . .
C22 C23 C24 119.9(11) . .
C22 C23 H23A 120.0 . .
C24 C23 H23A 120.0 . .
N4 C24 C23 119.8(10) . .
N4 C24 H24A 120.1 . .
C23 C24 H24A 120.1 . .
N4 C25 C26 118.1(10) . .
N4 C25 H25A 120.9 . .
C26 C25 H25A 120.9 . .
C25 C26 C22 120.9(11) . .
C25 C26 H26A 119.6 . .
C22 C26 H26A 119.6 . .
O3 C8 N1 122.6(10) . .
O3 C8 C9 118.9(10) . .
N1 C8 C9 118.5(9) . .
O4 N2 C11 121.5(9) . .
O4 N2 C12 118.3(8) . .
C11 N2 C12 120.2(9) . .
C21 N3 C18 128.7(10) . .
C21 N3 H3B 115.7 . .
C18 N3 H3B 115.7 . .
C24 N4 O8 118.4(8) . .
C24 N4 C25 122.4(9) . .
O8 N4 C25 119.2(8) . .
C1 O1 Pb1 91.5(5) . .
C1 O2 Pb1 96.0(6) . .
C14 O5 Pb1 108.8(6) . 5_636
N4 O8 Pb1 127.9(5) . .
C29 N5 C27 113.4(16) . .
C29 N5 C28 106.1(15) . .
C27 N5 C28 141(2) . .
N5 C27 H27A 109.5 . .
N5 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
N5 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
N5 C28 H28A 109.5 . .
N5 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
N5 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
O9 C29 N5 125(2) . .
O9 C29 H29 117.7 . .
N5 C29 H29 117.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O5 2.402(6) 5_636
Pb1 O2 2.468(7) .
Pb1 O1 2.562(6) .
Pb1 O8 2.616(7) .
C1 O1 1.257(12) .
C1 O2 1.257(11) .
C1 C2 1.502(13) .
C2 C7 1.396(14) .
C2 C3 1.398(15) .
C3 C4 1.348(14) .
C3 H3A 0.9500 .
C4 C5 1.431(14) .
C4 H4A 0.9500 .
C5 C6 1.378(14) .
C5 N1 1.390(13) .
C6 C7 1.385(14) .
C6 H6A 0.9500 .
C7 H7A 0.9500 .
N1 C8 1.322(14) .
N1 H1A 0.8800 .
C9 C10 1.393(16) .
C9 C13 1.402(15) .
C9 C8 1.495(14) .
C10 C11 1.357(14) .
C10 H10A 0.9500 .
C11 N2 1.330(13) .
C11 H11A 0.9500 .
C12 N2 1.363(13) .
C12 C13 1.373(14) .
C12 H12A 0.9500 .
C13 H13A 0.9500 .
C14 O5 1.266(13) .
C14 O6 1.280(12) .
C14 C15 1.465(15) .
C15 C16 1.383(14) .
C15 C20 1.400(18) .
C16 C17 1.403(15) .
C16 H16A 0.9500 .
C17 C18 1.384(16) .
C17 H17A 0.9500 .
C18 C19 1.373(17) .
C18 N3 1.424(14) .
C19 C20 1.424(17) .
C19 H19A 0.9500 .
C20 H20A 0.9500 .
C21 O7 1.219(13) .
C21 N3 1.322(14) .
C21 C22 1.510(14) .
C22 C23 1.361(15) .
C22 C26 1.404(15) .
C23 C24 1.412(14) .
C23 H23A 0.9500 .
C24 N4 1.328(13) .
C24 H24A 0.9500 .
C25 N4 1.368(13) .
C25 C26 1.385(14) .
C25 H25A 0.9500 .
C26 H26A 0.9500 .
C8 O3 1.226(13) .
N2 O4 1.319(10) .
N3 H3B 0.8800 .
N4 O8 1.333(10) .
O5 Pb1 2.402(6) 5_636
O9 C29 1.040(15) .
N5 C29 1.319(16) .
N5 C27 1.452(14) .
N5 C28 1.506(14) .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 H29 0.9500 .
