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#$Date: 2017-05-04 09:45:52 +0300 (Thu, 04 May 2017) $
#$Revision: 195974 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/57/4345797.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_4345797
loop_
_publ_author_name
'Hu, Lei'
'Lin, Xiao-Ming'
'Mo, Jun-Ting'
'Lin, Jia'
'Gan, Han-Lin'
'Yang, Xiao-Ling'
'Cai, Yue-Peng'
_publ_section_title
;
 Lead-Based Metal-Organic Framework with Stable Lithium Anodic
 Performance.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4289
_journal_page_last               4295
_journal_paper_doi               10.1021/acs.inorgchem.6b02663
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C24 H16 N2 O6 Pb'
_chemical_formula_sum            'C24 H16 N2 O6 Pb'
_chemical_formula_weight         635.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 97.172(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1289(13)
_cell_length_b                   21.8101(15)
_cell_length_c                   7.6470(3)
_cell_measurement_reflns_used    3986
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      3.08
_cell_volume                     3165.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8204
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.845
_exptl_absorpt_coefficient_mu    5.360
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5612
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0259P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2607
_reflns_number_total             2820
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02663_si_002.cif
_cod_data_source_block           1
_cod_database_code               4345797
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.000000 0.45442(2) 0.250000 0.02147(9) Uani 1 2 d S T P
O1 O 0.07512(17) 0.36720(14) 0.3163(3) 0.0379(7) Uani 1 1 d . . .
O2 O 0.15453(19) 0.44168(15) 0.3078(4) 0.0434(8) Uani 1 1 d . . .
O3 O 0.47195(16) 0.06359(13) 0.0531(3) 0.0305(7) Uani 1 1 d . . .
N1 N 0.43054(19) 0.10776(15) 0.1016(4) 0.0277(8) Uani 1 1 d . . .
C1 C 0.1377(3) 0.3854(2) 0.3104(5) 0.0366(11) Uani 1 1 d . . .
C2 C 0.1931(2) 0.3373(2) 0.2975(5) 0.0315(10) Uani 1 1 d . . .
C3 C 0.1740(2) 0.2759(2) 0.2936(5) 0.0350(11) Uani 1 1 d . . .
H3A H 0.127453 0.264278 0.310587 0.042 Uiso 1 1 calc R U .
C4 C 0.2230(2) 0.2317(2) 0.2649(5) 0.0344(10) Uani 1 1 d . . .
H4A H 0.209409 0.189749 0.261546 0.041 Uiso 1 1 calc R U .
C5 C 0.2915(2) 0.2468(2) 0.2410(5) 0.0320(10) Uani 1 1 d . . .
C6 C 0.3101(3) 0.3084(2) 0.2541(6) 0.0437(12) Uani 1 1 d . . .
H6A H 0.357462 0.319779 0.244817 0.052 Uiso 1 1 calc R U .
C7 C 0.2620(3) 0.3534(2) 0.2802(6) 0.0441(12) Uani 1 1 d . . .
H7A H 0.275859 0.395243 0.286222 0.053 Uiso 1 1 calc R U .
C8 C 0.3420(2) 0.19869(19) 0.1997(5) 0.0286(10) Uani 1 1 d . . .
C9 C 0.3299(2) 0.1369(2) 0.2301(6) 0.0373(11) Uani 1 1 d . . .
H9A H 0.290518 0.125288 0.286772 0.045 Uiso 1 1 calc R U .
C10 C 0.3737(2) 0.0928(2) 0.1798(6) 0.0349(10) Uani 1 1 d . . .
H10A H 0.363952 0.050836 0.200243 0.042 Uiso 1 1 calc R U .
C11 C 0.4461(2) 0.16731(19) 0.0762(5) 0.0301(10) Uani 1 1 d . . .
H11A H 0.487398 0.177816 0.025685 0.036 Uiso 1 1 calc R U .
C12 C 0.4020(2) 0.2129(2) 0.1235(5) 0.0316(10) Uani 1 1 d . . .
H12A H 0.412995 0.254548 0.103481 0.038 Uiso 1 1 calc R U .
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'
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
O1 Pb1 O1 75.12(16) . 2
O1 Pb1 O3 82.98(9) . 7
O1 Pb1 O3 82.56(10) 2 7
O1 Pb1 O3 82.56(10) . 8_456
O1 Pb1 O3 82.98(9) 2 8_456
O3 Pb1 O3 161.73(13) 7 8_456
C1 O1 Pb1 106.7(3) . .
N1 O3 Pb1 125.7(2) . 7
C10 N1 O3 119.4(3) . .
C10 N1 C11 120.2(3) . .
O3 N1 C11 120.4(3) . .
O1 C1 O2 123.1(4) . .
O1 C1 C2 117.4(4) . .
O2 C1 C2 119.4(5) . .
C3 C2 C1 119.3(4) . .
C3 C2 C7 119.6(4) . .
C1 C2 C7 121.0(4) . .
C4 C3 C2 119.7(4) . .
C4 C3 H3A 120.2 . .
C2 C3 H3A 120.2 . .
C3 C4 C5 121.7(4) . .
C3 C4 H4A 119.1 . .
C5 C4 H4A 119.1 . .
C4 C5 C6 117.4(4) . .
C4 C5 C8 120.6(4) . .
C6 C5 C8 122.0(4) . .
C7 C6 C5 121.9(5) . .
C7 C6 H6A 119.0 . .
C5 C6 H6A 119.0 . .
C6 C7 C2 119.6(4) . .
C6 C7 H7A 120.2 . .
C2 C7 H7A 120.2 . .
C9 C8 C12 116.7(4) . .
C9 C8 C5 121.5(4) . .
C12 C8 C5 121.8(4) . .
C8 C9 C10 121.1(4) . .
C8 C9 H9A 119.4 . .
C10 C9 H9A 119.4 . .
N1 C10 C9 120.9(4) . .
N1 C10 H10A 119.6 . .
C9 C10 H10A 119.6 . .
N1 C11 C12 120.1(4) . .
N1 C11 H11A 120.0 . .
C12 C11 H11A 120.0 . .
C8 C12 C11 121.0(4) . .
C8 C12 H12A 119.5 . .
C11 C12 H12A 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.400(3) .
Pb1 O1 2.400(3) 2
Pb1 O3 2.475(2) 7
Pb1 O3 2.475(2) 8_456
O1 C1 1.267(6) .
O2 C1 1.270(6) .
O3 N1 1.329(4) .
N1 C10 1.345(5) .
N1 C11 1.352(5) .
C1 C2 1.504(6) .
C2 C3 1.388(6) .
C2 C7 1.385(6) .
C3 C4 1.381(6) .
C3 H3A 0.9500 .
C4 C5 1.385(6) .
C4 H4A 0.9500 .
C5 C6 1.390(6) .
C5 C8 1.488(6) .
C6 C7 1.378(6) .
C6 H6A 0.9500 .
C7 H7A 0.9500 .
C8 C9 1.392(6) .
C8 C12 1.385(6) .
C9 C10 1.362(6) .
C9 H9A 0.9500 .
C10 H10A 0.9500 .
C11 C12 1.380(6) .
C11 H11A 0.9500 .
C12 H12A 0.9500 .
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
Pb1 O3 N1 C10 121.8(3) 7
Pb1 O3 N1 C11 -59.5(4) 7
Pb1 O1 C1 O2 13.5(5) .
Pb1 O1 C1 C2 -163.6(3) .
O1 C1 C2 C3 -0.4(5) .
O2 C1 C2 C3 -177.6(4) .
O1 C1 C2 C7 176.2(4) .
O2 C1 C2 C7 -1.0(6) .
C1 C2 C3 C4 173.9(3) .
C7 C2 C3 C4 -2.8(6) .
C2 C3 C4 C5 0.5(6) .
C3 C4 C5 C6 2.6(6) .
C3 C4 C5 C8 -176.3(4) .
C4 C5 C6 C7 -3.5(7) .
C8 C5 C6 C7 175.4(4) .
C5 C6 C7 C2 1.3(7) .
C3 C2 C7 C6 1.9(7) .
C1 C2 C7 C6 -174.7(4) .
C4 C5 C8 C9 -17.6(6) .
C6 C5 C8 C9 163.5(4) .
C4 C5 C8 C12 160.0(4) .
C6 C5 C8 C12 -18.9(6) .
C12 C8 C9 C10 -2.7(6) .
C5 C8 C9 C10 175.0(4) .
O3 N1 C10 C9 -179.6(4) .
C11 N1 C10 C9 1.8(6) .
C8 C9 C10 N1 1.0(7) .
C10 N1 C11 C12 -2.8(6) .
O3 N1 C11 C12 178.6(3) .
C9 C8 C12 C11 1.7(6) .
C5 C8 C12 C11 -176.0(4) .
N1 C11 C12 C8 0.9(6) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.036 626 190 ' '
2 0.500 0.500 0.029 626 190 ' '
