# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
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data_SMOF-4
_database_code_depnum_ccdc_archive 'CCDC 1857584'
_audit_update_record             
;
2018-12-13 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_audit_creation_date             2018-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            '[Pb4(2,6-ndc)3Cl2]n'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H9 Cl O6 Pb2'
_chemical_formula_sum            'C18 H9 Cl O6 Pb2'
_chemical_formula_weight         771.08
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.0559(3)
_cell_length_b                   22.1208(11)
_cell_length_c                   12.1647(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.721(5)
_cell_angle_gamma                90
_cell_volume                     1624.07(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6478
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5160
_cell_measurement_theta_min      3.8290
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.23b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   'Sphere (Rigaku CrystalClear)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    3.154
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13520
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.801
_diffrn_reflns_theta_min         3.485
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     53.00  79.00   0.50    1.49    --    5.00  45.00   0.00   52
  2  ω    -66.00 -40.00   0.50    1.49    --    5.00  45.00 150.00   52
  3  ω     34.00  60.00   0.50    1.49    --  -11.10  45.00 120.00   52
  4  ω   -100.00  78.00   0.50    1.49    --  -11.10  45.00 150.00  356
  5  ω    -24.00   1.00   0.50    1.49    --  -11.10  45.00 120.00   50
  6  ω    -82.00 -29.00   0.50    1.49    --  -11.10  45.00  60.00  106
  7  ω    -99.00 -74.00   0.50    1.49    --  -11.10  45.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0892292000
_diffrn_orient_matrix_UB_12      -0.0204807000
_diffrn_orient_matrix_UB_13      -0.0034895000
_diffrn_orient_matrix_UB_21      -0.0757693000
_diffrn_orient_matrix_UB_22      -0.0245127000
_diffrn_orient_matrix_UB_23      -0.0037973000
_diffrn_orient_matrix_UB_31      -0.0101503000
_diffrn_orient_matrix_UB_32      0.0028844000
_diffrn_orient_matrix_UB_33      -0.0582793000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3267
_reflns_number_total             3725
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.326
_refine_diff_density_min         -1.799
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       0.00124(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3725
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0320
_refine_ls_restrained_S_all      1.065
_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)+(0.0321P)²+2.2071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0691
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C17(H17), C9(H9), C15(H15), C5(H5), C11(H11), C16(H16), C12(H12),
 C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.53296(4) 0.77377(2) 0.58022(2) 0.01736(9) Uani 1 1 d . . . . .
Pb2 Pb 0.97595(4) 0.79370(2) 0.35698(2) 0.01799(9) Uani 1 1 d . . . . .
Cl1 Cl 1.0020(3) 0.76883(9) 0.64730(14) 0.0303(4) Uani 1 1 d . . . . .
O3 O 0.6235(7) 0.81961(18) 0.2282(3) 0.0209(10) Uani 1 1 d . . . . .
O5 O 0.3119(7) 0.35477(19) 0.0218(4) 0.0231(10) Uani 1 1 d . . . . .
O6 O 0.6756(8) 0.3573(2) 0.0543(4) 0.0253(10) Uani 1 1 d . . . . .
O1 O 0.6799(8) 0.71916(19) 0.4369(4) 0.0242(10) Uani 1 1 d . . . . .
O2 O 0.3174(8) 0.7097(2) 0.4048(4) 0.0279(11) Uani 1 1 d . . . . .
O4 O 0.9196(7) 0.8793(2) 0.2377(4) 0.0248(10) Uani 1 1 d . . . . .
C8 C 0.4877(10) 0.3816(3) 0.0595(5) 0.0160(13) Uani 1 1 d . . . . .
C1 C 0.5077(11) 0.6934(3) 0.3889(5) 0.0175(13) Uani 1 1 d . . . . .
C13 C 0.7239(10) 0.8672(3) 0.1999(5) 0.0183(13) Uani 1 1 d . U . . .
C2 C 0.5478(10) 0.6392(2) 0.3200(5) 0.0133(12) Uani 1 1 d . U . . .
C7 C 0.4672(10) 0.4432(3) 0.1073(5) 0.0168(13) Uani 1 1 d . . . . .
C3 C 0.3778(10) 0.6140(3) 0.2537(5) 0.0172(13) Uani 1 1 d . . . . .
H3 H 0.241477 0.633525 0.245238 0.021 Uiso 1 1 calc R . . . .
C17 C 0.7175(10) 0.9612(3) 0.0925(5) 0.0173(13) Uani 1 1 d . . . . .
H17 H 0.864505 0.966938 0.118967 0.021 Uiso 1 1 calc R . . . .
C4 C 0.4073(9) 0.5582(2) 0.1976(5) 0.0134(12) Uani 1 1 d . . . . .
C14 C 0.6067(10) 0.9110(3) 0.1230(5) 0.0189(13) Uani 1 1 d . . . . .
C18 C 0.6110(10) 1.0050(3) 0.0207(5) 0.0147(12) Uani 1 1 d . . . . .
C9 C 0.6420(10) 0.4706(3) 0.1657(5) 0.0167(13) Uani 1 1 d . . . . .
H9 H 0.778459 0.451157 0.174135 0.020 Uiso 1 1 calc R . . . .
C15 C 0.3817(11) 0.9019(3) 0.0849(5) 0.0196(13) Uani 1 1 d . . . . .
H15 H 0.305707 0.868276 0.107951 0.024 Uiso 1 1 calc R . . . .
C5 C 0.2344(10) 0.5302(3) 0.1308(5) 0.0174(13) Uani 1 1 d . . . . .
H5 H 0.100592 0.550414 0.116115 0.021 Uiso 1 1 calc R . . . .
C11 C 0.7890(10) 0.5573(3) 0.2793(5) 0.0180(13) Uani 1 1 d . . . . .
H11 H 0.927244 0.538853 0.288502 0.022 Uiso 1 1 calc R . . . .
C16 C 0.2769(10) 0.9425(3) 0.0144(5) 0.0195(13) Uani 1 1 d . . . . .
H16 H 0.129973 0.935922 -0.011306 0.023 Uiso 1 1 calc R . . . .
C12 C 0.7595(10) 0.6112(3) 0.3293(5) 0.0196(14) Uani 1 1 d . . . . .
H12 H 0.877726 0.629749 0.369714 0.024 Uiso 1 1 calc R . . . .
C10 C 0.6173(9) 0.5284(3) 0.2136(5) 0.0135(12) Uani 1 1 d . . . . .
C6 C 0.2608(10) 0.4745(3) 0.0881(5) 0.0183(13) Uani 1 1 d . . . . .
H6 H 0.144028 0.456367 0.045848 0.022 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Cl1 2.8919(17) . ?
Pb1 O5 2.414(4) 2_655 ?
Pb1 O6 2.710(4) 2_655 ?
Pb1 O1 2.355(4) . ?
Pb2 Cl1 2.9173(17) 4_575 ?
Pb2 O3 2.605(4) . ?
Pb2 O5 2.731(5) 2_655 ?
Pb2 O6 2.687(4) 2_755 ?
Pb2 O1 2.677(4) . ?
Pb2 O4 2.392(4) . ?
Pb2 C13 2.853(6) . ?
O3 C13 1.277(7) . ?
O5 C8 1.271(7) . ?
O6 C8 1.265(7) . ?
O1 C1 1.285(8) . ?
O2 C1 1.238(8) . ?
O4 C13 1.264(7) . ?
C8 C7 1.490(9) . ?
C1 C2 1.495(8) . ?
C13 C14 1.486(8) . ?
C2 C3 1.373(8) . ?
C2 C12 1.420(8) . ?
C7 C9 1.368(8) . ?
C7 C6 1.430(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.430(8) . ?
C17 H17 0.9300 . ?
C17 C14 1.366(9) . ?
C17 C18 1.422(8) . ?
C4 C5 1.414(8) . ?
C4 C10 1.431(8) . ?
C14 C15 1.417(9) . ?
C18 C18 1.413(12) 3_675 ?
C18 C16 1.429(9) 3_675 ?
C9 H9 0.9300 . ?
C9 C10 1.417(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.362(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.353(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.357(8) . ?
C11 C10 1.412(8) . ?
C16 H16 0.9300 . ?
C12 H12 0.9300 . ?
C6 H6 0.9300 . ?

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
O5 Pb1 Cl1 76.02(11) 2_655 . ?
O5 Pb1 O6 50.60(14) 2_655 2_655 ?
O6 Pb1 Cl1 126.45(10) 2_655 . ?
O1 Pb1 Cl1 76.55(12) . . ?
O1 Pb1 O5 79.23(15) . 2_655 ?
O1 Pb1 O6 95.08(15) . 2_655 ?
O3 Pb2 Cl1 71.29(10) . 4_575 ?
O3 Pb2 O5 71.81(13) . 2_655 ?
O3 Pb2 O6 134.73(13) . 2_755 ?
O3 Pb2 O1 79.26(14) . . ?
O3 Pb2 C13 26.55(15) . . ?
O5 Pb2 Cl1 142.11(10) 2_655 4_575 ?
O5 Pb2 C13 75.51(15) 2_655 . ?
O6 Pb2 Cl1 120.16(11) 2_755 4_575 ?
O6 Pb2 O5 92.24(14) 2_755 2_655 ?
O6 Pb2 C13 109.27(16) 2_755 . ?
O1 Pb2 Cl1 96.39(10) . 4_575 ?
O1 Pb2 O5 68.43(13) . 2_655 ?
O1 Pb2 O6 134.73(14) . 2_755 ?
O1 Pb2 C13 104.87(17) . . ?
O4 Pb2 Cl1 81.96(12) . 4_575 ?
O4 Pb2 O3 52.58(14) . . ?
O4 Pb2 O5 82.55(14) . 2_655 ?
O4 Pb2 O6 84.13(14) . 2_755 ?
O4 Pb2 O1 129.88(15) . . ?
O4 Pb2 C13 26.03(16) . . ?
C13 Pb2 Cl1 75.45(12) . 4_575 ?
Pb1 Cl1 Pb2 98.17(5) . 4_576 ?
C13 O3 Pb2 87.6(4) . . ?
Pb1 O5 Pb2 101.73(15) 2_645 2_645 ?
C8 O5 Pb1 100.5(4) . 2_645 ?
C8 O5 Pb2 126.1(4) . 2_645 ?
Pb2 O6 Pb1 101.37(14) 2_745 2_645 ?
C8 O6 Pb1 86.8(4) . 2_645 ?
C8 O6 Pb2 151.9(4) . 2_745 ?
Pb1 O1 Pb2 104.95(15) . . ?
C1 O1 Pb1 102.8(4) . . ?
C1 O1 Pb2 130.6(4) . . ?
C13 O4 Pb2 97.8(4) . . ?
O5 C8 C7 118.3(5) . . ?
O6 C8 O5 120.9(6) . . ?
O6 C8 C7 120.8(5) . . ?
O1 C1 C2 116.5(6) . . ?
O2 C1 O1 122.1(6) . . ?
O2 C1 C2 121.2(6) . . ?
O3 C13 Pb2 65.8(3) . . ?
O3 C13 C14 119.6(6) . . ?
O4 C13 Pb2 56.1(3) . . ?
O4 C13 O3 121.9(6) . . ?
O4 C13 C14 118.4(5) . . ?
C14 C13 Pb2 173.9(4) . . ?
C3 C2 C1 120.4(5) . . ?
C3 C2 C12 119.9(5) . . ?
C12 C2 C1 119.5(5) . . ?
C9 C7 C8 121.5(6) . . ?
C9 C7 C6 119.9(6) . . ?
C6 C7 C8 118.6(5) . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 120.9(5) . . ?
C4 C3 H3 119.5 . . ?
C14 C17 H17 119.6 . . ?
C14 C17 C18 120.8(6) . . ?
C18 C17 H17 119.6 . . ?
C3 C4 C10 118.5(5) . . ?
C5 C4 C3 122.4(5) . . ?
C5 C4 C10 119.0(5) . . ?
C17 C14 C13 118.8(6) . . ?
C17 C14 C15 120.4(5) . . ?
C15 C14 C13 120.7(6) . . ?
C17 C18 C16 122.3(5) . 3_675 ?
C18 C18 C17 118.9(7) 3_675 . ?
C18 C18 C16 118.8(7) 3_675 3_675 ?
C7 C9 H9 119.7 . . ?
C7 C9 C10 120.7(5) . . ?
C10 C9 H9 119.7 . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.9(6) . . ?
C16 C15 H15 120.1 . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 120.9(5) . . ?
C6 C5 H5 119.5 . . ?
C12 C11 H11 118.9 . . ?
C12 C11 C10 122.3(6) . . ?
C10 C11 H11 118.9 . . ?
C18 C16 H16 119.5 3_675 . ?
C15 C16 C18 121.1(6) . 3_675 ?
C15 C16 H16 119.5 . . ?
C2 C12 H12 120.0 . . ?
C11 C12 C2 120.0(5) . . ?
C11 C12 H12 120.0 . . ?
C9 C10 C4 118.8(5) . . ?
C11 C10 C4 118.2(5) . . ?
C11 C10 C9 122.9(5) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 C7 120.5(5) . . ?
C5 C6 H6 119.8 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O5 C8 O6 -12.1(6) 2_645 . . . ?
Pb1 O5 C8 C7 166.3(4) 2_645 . . . ?
Pb1 O6 C8 O5 10.6(6) 2_645 . . . ?
Pb1 O6 C8 C7 -167.7(5) 2_645 . . . ?
Pb1 O1 C1 O2 15.5(7) . . . . ?
Pb1 O1 C1 C2 -159.4(4) . . . . ?
Pb2 O3 C13 O4 1.1(6) . . . . ?
Pb2 O3 C13 C14 -176.8(5) . . . . ?
Pb2 O5 C8 O6 100.9(6) 2_645 . . . ?
Pb2 O5 C8 C7 -80.7(6) 2_645 . . . ?
Pb2 O6 C8 O5 -97.6(9) 2_745 . . . ?
Pb2 O6 C8 C7 84.0(10) 2_745 . . . ?
Pb2 O1 C1 O2 -107.4(6) . . . . ?
Pb2 O1 C1 C2 77.7(7) . . . . ?
Pb2 O4 C13 O3 -1.3(7) . . . . ?
Pb2 O4 C13 C14 176.7(5) . . . . ?
O3 C13 C14 C17 -179.2(6) . . . . ?
O3 C13 C14 C15 2.9(9) . . . . ?
O5 C8 C7 C9 168.8(6) . . . . ?
O5 C8 C7 C6 -13.1(8) . . . . ?
O6 C8 C7 C9 -12.8(9) . . . . ?
O6 C8 C7 C6 165.3(6) . . . . ?
O1 C1 C2 C3 -170.9(5) . . . . ?
O1 C1 C2 C12 13.6(8) . . . . ?
O2 C1 C2 C3 14.2(9) . . . . ?
O2 C1 C2 C12 -161.4(6) . . . . ?
O4 C13 C14 C17 2.8(9) . . . . ?
O4 C13 C14 C15 -175.1(6) . . . . ?
C8 C7 C9 C10 -177.9(5) . . . . ?
C8 C7 C6 C5 179.3(6) . . . . ?
C1 C2 C3 C4 -172.5(5) . . . . ?
C1 C2 C12 C11 170.7(6) . . . . ?
C13 C14 C15 C16 -180.0(6) . . . . ?
C2 C3 C4 C5 178.5(5) . . . . ?
C2 C3 C4 C10 1.2(9) . . . . ?
C7 C9 C10 C4 -1.4(9) . . . . ?
C7 C9 C10 C11 176.8(6) . . . . ?
C3 C2 C12 C11 -4.8(9) . . . . ?
C3 C4 C5 C6 -173.2(6) . . . . ?
C3 C4 C10 C9 174.8(5) . . . . ?
C3 C4 C10 C11 -3.5(8) . . . . ?
C17 C14 C15 C16 2.2(9) . . . . ?
C4 C5 C6 C7 -1.6(9) . . . . ?
C14 C17 C18 C18 -1.3(10) . . . 3_675 ?
C14 C17 C18 C16 -178.9(6) . . . 3_675 ?
C14 C15 C16 C18 -1.1(9) . . . 3_675 ?
C18 C17 C14 C13 -178.9(5) . . . . ?
C18 C17 C14 C15 -1.0(9) . . . . ?
C9 C7 C6 C5 -2.5(10) . . . . ?
C5 C4 C10 C9 -2.6(8) . . . . ?
C5 C4 C10 C11 179.1(5) . . . . ?
C12 C2 C3 C4 3.0(9) . . . . ?
C12 C11 C10 C4 1.7(9) . . . . ?
C12 C11 C10 C9 -176.5(6) . . . . ?
C10 C4 C5 C6 4.1(9) . . . . ?
C10 C11 C12 C2 2.4(10) . . . . ?
C6 C7 C9 C10 4.0(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.053
_oxdiff_exptl_absorpt_empirical_full_min 0.708
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_SMOF-3
_database_code_depnum_ccdc_archive 'CCDC 1857745'
_audit_update_record             
;
2018-12-13 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_audit_creation_date             2018-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            '[Pb2(2,6-ndc)2H2O]n, nDMF'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H14 O9 Pb2, C3 H7 N O'
_chemical_formula_sum            'C27 H21 N O10 Pb2'
_chemical_formula_weight         933.83
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2143(7)
_cell_length_b                   11.8601(11)
_cell_length_c                   14.6928(18)
_cell_angle_alpha                102.099(18)
_cell_angle_beta                 93.567(14)
_cell_angle_gamma                109.763(12)
_cell_volume                     1303.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4489
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.962
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.23b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   'Sphere (Rigaku CrystalClear)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19770
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         3.050
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4027
_reflns_number_total             5375
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5375
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0273
_refine_ls_restrained_S_all      0.857
_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)+(0.0199P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0572
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H5-H27F_$1
 2.2 with sigma of 0.02
 O1W-H1WA = O1W-H1WB
 0.82 with sigma of 0.01
 H1WA-H1WB
 1.39 with sigma of 0.01
 N1-C27A \\sim N1-C27B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C27A) = Uanis(C27B)
4. Others
 Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(H26A)=Sof(C27B)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=1-FVAR(1)
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(H26)=Sof(C27A)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=FVAR(1)
5.a Me refined with riding coordinates:
 C25(H25D,H25E,H25F)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16),
 C18(H18), C21(H21), C22(H22), C24(H24), C26(H26), C26(H26A)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27A(H27A,H27B,H27C), C27B(H27D,H27E,H27F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.81046(3) 0.84003(2) 0.40800(2) 0.02096(7) Uani 1 1 d . . . . .
Pb2 Pb 0.25462(3) 0.78194(2) 0.32234(2) 0.02359(7) Uani 1 1 d . . . . .
O1 O 0.7925(5) 0.8868(4) 0.2619(3) 0.0294(10) Uani 1 1 d . . . . .
O1W O 0.4409(6) 0.8468(6) 0.2112(3) 0.0557(15) Uani 1 1 d D . . . .
H1WA H 0.398(8) 0.810(7) 0.156(2) 0.084 Uiso 1 1 d DR . . . .
H1WB H 0.546(3) 0.862(7) 0.223(5) 0.084 Uiso 1 1 d DR . . . .
O2 O 1.0703(5) 0.9450(3) 0.3180(3) 0.0247(9) Uani 1 1 d . . . . .
O3 O 0.4956(5) 0.6853(3) 0.3483(4) 0.0365(12) Uani 1 1 d . . . . .
O4 O 0.2190(6) 0.5695(4) 0.3202(4) 0.0441(13) Uani 1 1 d . . . . .
O5 O 0.0774(6) 0.6873(4) 0.1784(3) 0.0373(11) Uani 1 1 d . . . . .
O6 O -0.1105(5) 0.6642(4) 0.2824(3) 0.0331(10) Uani 1 1 d . . . . .
O8 O 0.6058(5) -0.0441(3) 0.4149(3) 0.0281(10) Uani 1 1 d . . . . .
O9 O 0.8818(6) 0.0728(3) 0.4603(3) 0.0363(11) Uani 1 1 d . . . . .
O10 O -0.4021(8) 0.1910(7) -0.0259(4) 0.0787(19) Uani 1 1 d . . . . .
C1 C 0.9533(8) 0.9316(5) 0.2541(5) 0.0257(14) Uani 1 1 d . . . . .
C2 C 0.9989(8) 0.9659(5) 0.1638(4) 0.0278(14) Uani 1 1 d . . . . .
C3 C 0.8707(8) 0.9367(6) 0.0896(5) 0.0307(15) Uani 1 1 d . . . . .
H3 H 0.755074 0.894903 0.095493 0.037 Uiso 1 1 calc R . . . .
C4 C 0.9107(8) 0.9690(6) 0.0041(5) 0.0331(15) Uani 1 1 d . . . . .
C5 C 0.7829(9) 0.9430(7) -0.0725(5) 0.0439(18) Uani 1 1 d . . . . .
H5 H 0.666212 0.903130 -0.067456 0.053 Uiso 1 1 calc DR . . . .
C6 C 0.8247(8) 0.9746(6) -0.1550(5) 0.0350(15) Uani 1 1 d . . . . .
H6 H 0.737110 0.956858 -0.204796 0.042 Uiso 1 1 calc R . . . .
C7 C -0.0787(8) 0.6504(5) 0.1991(5) 0.0301(15) Uani 1 1 d . . . . .
C8 C -0.2205(8) 0.5914(6) 0.1142(5) 0.0365(16) Uani 1 1 d . . . . .
C9 C -0.3882(9) 0.5737(7) 0.1245(5) 0.0456(18) Uani 1 1 d . . . . .
H9 H -0.417054 0.597818 0.183827 0.055 Uiso 1 1 calc R . . . .
C10 C -0.5246(8) 0.5172(6) 0.0436(5) 0.0414(17) Uani 1 1 d . . . . .
C11 C -0.6992(10) 0.4989(8) 0.0524(6) 0.066(3) Uani 1 1 d . . . . .
H11 H -0.730108 0.524572 0.110840 0.079 Uiso 1 1 calc R . . . .
C12 C -0.8234(10) 0.4438(8) -0.0240(6) 0.062(2) Uani 1 1 d . . . . .
H12 H -0.940052 0.428922 -0.016960 0.074 Uiso 1 1 calc R . . . .
C13 C 0.3751(8) 0.5834(5) 0.3435(4) 0.0263(14) Uani 1 1 d . . . . .
C14 C 0.4164(8) 0.4767(5) 0.3651(4) 0.0240(13) Uani 1 1 d . . . . .
C15 C 0.2752(7) 0.3658(5) 0.3614(4) 0.0251(13) Uani 1 1 d . . . . .
H15 H 0.160651 0.361670 0.348844 0.030 Uiso 1 1 calc R . . . .
C16 C 0.3076(7) 0.2646(5) 0.3764(4) 0.0234(13) Uani 1 1 d . . . . .
H16 H 0.214516 0.192058 0.373772 0.028 Uiso 1 1 calc R . . . .
C17 C 0.4807(7) 0.2691(5) 0.3956(4) 0.0225(13) Uani 1 1 d . . . . .
C18 C 0.5190(8) 0.1649(5) 0.4076(4) 0.0240(13) Uani 1 1 d . . . . .
H18 H 0.428052 0.090139 0.402115 0.029 Uiso 1 1 calc R . . . .
C19 C 0.6874(7) 0.1726(5) 0.4271(4) 0.0200(12) Uani 1 1 d . . . . .
C20 C 0.7258(7) 0.0599(5) 0.4352(4) 0.0184(12) Uani 1 1 d . . . . .
C21 C 0.8272(8) 0.2856(5) 0.4358(5) 0.0293(14) Uani 1 1 d . . . . .
H21 H 0.941638 0.291057 0.451285 0.035 Uiso 1 1 calc R . . . .
C22 C 0.7948(7) 0.3870(5) 0.4216(5) 0.0287(14) Uani 1 1 d . . . . .
H22 H 0.887708 0.460142 0.425223 0.034 Uiso 1 1 calc R . . . .
C23 C 0.6206(7) 0.3813(5) 0.4012(4) 0.0223(13) Uani 1 1 d . . . . .
C24 C 0.5835(7) 0.4835(5) 0.3839(4) 0.0238(13) Uani 1 1 d . . . . .
H24 H 0.675041 0.556530 0.385480 0.029 Uiso 1 1 calc R . . . .
N1 N -0.2133(10) 0.2535(7) 0.1079(5) 0.073(2) Uani 1 1 d D . . . .
C25 C -0.0363(16) 0.2892(12) 0.1548(9) 0.124(5) Uani 1 1 d . . . . .
H25A H -0.033774 0.235842 0.195330 0.187 Uiso 0.653(13) 1 calc GR . P A 1
H25B H 0.002323 0.373134 0.191404 0.187 Uiso 0.653(13) 1 calc GR . P A 1
H25C H 0.039809 0.282280 0.108597 0.187 Uiso 0.653(13) 1 calc GR . P A 1
H25D H -0.035480 0.306851 0.221654 0.187 Uiso 0.347(13) 1 calc R . P A 2
H25E H 0.005933 0.222883 0.135705 0.187 Uiso 0.347(13) 1 calc R . P A 2
H25F H 0.037905 0.361522 0.137972 0.187 Uiso 0.347(13) 1 calc R . P A 2
C26 C -0.2580(13) 0.2237(7) 0.0166(6) 0.061(2) Uani 1 1 d . . . . .
H26 H -0.167814 0.228334 -0.019391 0.073 Uiso 0.653(13) 1 calc R . P A 1
H26A H -0.167814 0.228334 -0.019391 0.073 Uiso 0.347(13) 1 calc R . P A 2
C27A C -0.336(2) 0.2919(15) 0.1664(11) 0.100(5) Uani 0.653(13) 1 d D . P A 1
H27A H -0.439497 0.281458 0.126590 0.150 Uiso 0.653(13) 1 calc GR . P A 1
H27B H -0.280438 0.377116 0.199585 0.150 Uiso 0.653(13) 1 calc GR . P A 1
H27C H -0.365898 0.241799 0.210717 0.150 Uiso 0.653(13) 1 calc GR . P A 1
C27B C -0.324(4) 0.166(3) 0.1607(19) 0.100(5) Uani 0.347(13) 1 d D . P A 2
H27D H -0.258341 0.175631 0.220014 0.150 Uiso 0.347(13) 1 calc GR . P A 2
H27E H -0.356863 0.082447 0.124253 0.150 Uiso 0.347(13) 1 calc GR . P A 2
H27F H -0.427440 0.184588 0.171474 0.150 Uiso 0.347(13) 1 calc DGR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.335(4) . ?
Pb1 O2 2.664(4) . ?
Pb1 O3 2.580(4) . ?
Pb1 O8 2.500(4) 1_565 ?
Pb1 O9 2.553(4) 1_565 ?
Pb1 C1 2.858(6) . ?
Pb2 O1W 2.376(5) . ?
Pb2 O3 2.646(4) . ?
Pb2 O4 2.429(4) . ?
Pb2 O5 2.318(4) . ?
O1 C1 1.269(7) . ?
O1W H1WA 0.823(10) . ?
O1W H1WB 0.823(10) . ?
O2 C1 1.246(7) . ?
O3 C13 1.262(7) . ?
O4 C13 1.252(7) . ?
O5 C7 1.286(7) . ?
O6 C7 1.256(8) . ?
O8 C20 1.253(6) . ?
O9 C20 1.259(7) . ?
O10 C26 1.199(10) . ?
C1 C2 1.499(8) . ?
C2 C3 1.367(9) . ?
C2 C6 1.409(8) 2_775 ?
C3 H3 0.9300 . ?
C3 C4 1.415(8) . ?
C4 C4 1.427(12) 2_775 ?
C4 C5 1.398(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.372(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.519(9) . ?
C8 C9 1.345(9) . ?
C8 C12 1.411(11) 2_465 ?
C9 H9 0.9300 . ?
C9 C10 1.452(10) . ?
C10 C10 1.388(14) 2_465 ?
C10 C11 1.394(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.352(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.504(7) . ?
C14 C15 1.417(7) . ?
C14 C24 1.355(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.371(7) . ?
C16 H16 0.9300 . ?
C16 C17 1.413(8) . ?
C17 C18 1.417(7) . ?
C17 C23 1.416(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.363(8) . ?
C19 C20 1.499(7) . ?
C19 C21 1.415(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.370(8) . ?
C22 H22 0.9300 . ?
C22 C23 1.420(8) . ?
C23 C24 1.413(7) . ?
C24 H24 0.9300 . ?
N1 C25 1.451(13) . ?
N1 C26 1.308(11) . ?
N1 C27A 1.485(15) . ?
N1 C27B 1.52(2) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C25 H25D 0.9600 . ?
C25 H25E 0.9600 . ?
C25 H25F 0.9600 . ?
C26 H26 0.9300 . ?
C26 H26A 0.9300 . ?
C27A H27A 0.9600 . ?
C27A H27B 0.9600 . ?
C27A H27C 0.9600 . ?
C27B H27D 0.9600 . ?
C27B H27E 0.9600 . ?
C27B H27F 0.9600 . ?

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 O2 51.61(13) . . ?
O1 Pb1 O3 84.65(15) . . ?
O1 Pb1 O8 74.52(14) . 1_565 ?
O1 Pb1 O9 79.75(15) . 1_565 ?
O1 Pb1 C1 25.86(16) . . ?
O2 Pb1 C1 25.77(15) . . ?
O3 Pb1 O2 132.09(14) . . ?
O3 Pb1 C1 108.48(17) . . ?
O8 Pb1 O2 108.31(12) 1_565 . ?
O8 Pb1 O3 70.88(12) 1_565 . ?
O8 Pb1 O9 51.40(13) 1_565 1_565 ?
O8 Pb1 C1 92.04(15) 1_565 . ?
O9 Pb1 O2 73.39(13) 1_565 . ?
O9 Pb1 O3 122.28(13) 1_565 . ?
O9 Pb1 C1 75.74(15) 1_565 . ?
O1W Pb2 O3 77.95(17) . . ?
O1W Pb2 O4 108.6(2) . . ?
O4 Pb2 O3 50.68(13) . . ?
O5 Pb2 O1W 75.98(16) . . ?
O5 Pb2 O3 112.43(15) . . ?
O5 Pb2 O4 81.79(16) . . ?
C1 O1 Pb1 100.8(4) . . ?
Pb2 O1W H1WA 113(6) . . ?
Pb2 O1W H1WB 119(6) . . ?
H1WA O1W H1WB 115(2) . . ?
C1 O2 Pb1 85.8(3) . . ?
Pb1 O3 Pb2 116.26(13) . . ?
C13 O3 Pb1 151.2(4) . . ?
C13 O3 Pb2 88.9(3) . . ?
C13 O4 Pb2 99.4(3) . . ?
C7 O5 Pb2 104.5(4) . . ?
C20 O8 Pb1 94.1(3) . 1_545 ?
C20 O9 Pb1 91.5(3) . 1_545 ?
O1 C1 Pb1 53.4(3) . . ?
O1 C1 C2 117.7(6) . . ?
O2 C1 Pb1 68.4(3) . . ?
O2 C1 O1 121.7(5) . . ?
O2 C1 C2 120.6(5) . . ?
C2 C1 Pb1 170.3(4) . . ?
C3 C2 C1 120.3(5) . . ?
C3 C2 C6 120.1(5) . 2_775 ?
C6 C2 C1 119.6(6) 2_775 . ?
C2 C3 H3 119.4 . . ?
C2 C3 C4 121.2(5) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 C4 118.5(7) . 2_775 ?
C5 C4 C3 122.8(6) . . ?
C5 C4 C4 118.6(7) . 2_775 ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.9(6) . . ?
C6 C5 H5 119.1 . . ?
C2 C6 H6 120.2 2_775 . ?
C5 C6 C2 119.6(6) . 2_775 ?
C5 C6 H6 120.2 . . ?
O5 C7 C8 114.0(6) . . ?
O6 C7 O5 122.7(6) . . ?
O6 C7 C8 123.2(6) . . ?
C9 C8 C7 120.1(7) . . ?
C9 C8 C12 119.7(7) . 2_465 ?
C12 C8 C7 120.1(6) 2_465 . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.4(7) . . ?
C10 C9 H9 119.8 . . ?
C10 C10 C9 117.8(8) 2_465 . ?
C10 C10 C11 120.7(9) 2_465 . ?
C11 C10 C9 121.5(7) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.1(8) . . ?
C12 C11 H11 120.0 . . ?
C8 C12 H12 119.4 2_465 . ?
C11 C12 C8 121.2(7) . 2_465 ?
C11 C12 H12 119.4 . . ?
O3 C13 C14 120.7(5) . . ?
O4 C13 O3 120.3(5) . . ?
O4 C13 C14 119.0(5) . . ?
C15 C14 C13 118.1(5) . . ?
C24 C14 C13 121.5(5) . . ?
C24 C14 C15 120.3(5) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 119.9(5) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 119.6 . . ?
C15 C16 C17 120.9(5) . . ?
C17 C16 H16 119.6 . . ?
C16 C17 C18 122.3(5) . . ?
C16 C17 C23 118.7(5) . . ?
C23 C17 C18 119.0(5) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.9(5) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C20 120.1(5) . . ?
C18 C19 C21 120.3(5) . . ?
C21 C19 C20 119.6(5) . . ?
O8 C20 O9 121.6(5) . . ?
O8 C20 C19 120.3(5) . . ?
O9 C20 C19 118.1(5) . . ?
C19 C21 H21 119.9 . . ?
C22 C21 C19 120.3(5) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 119.7 . . ?
C21 C22 C23 120.5(5) . . ?
C23 C22 H22 119.7 . . ?
C17 C23 C22 119.0(5) . . ?
C24 C23 C17 119.3(5) . . ?
C24 C23 C22 121.7(5) . . ?
C14 C24 C23 120.9(5) . . ?
C14 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C25 N1 C27A 115.7(10) . . ?
C25 N1 C27B 104.2(15) . . ?
C26 N1 C25 124.5(9) . . ?
C26 N1 C27A 117.0(10) . . ?
C26 N1 C27B 116.1(13) . . ?
N1 C25 H25A 109.5 . . ?
N1 C25 H25B 109.5 . . ?
N1 C25 H25C 109.5 . . ?
N1 C25 H25D 109.5 . . ?
N1 C25 H25E 109.5 . . ?
N1 C25 H25F 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
H25D C25 H25E 109.5 . . ?
H25D C25 H25F 109.5 . . ?
H25E C25 H25F 109.5 . . ?
O10 C26 N1 127.4(9) . . ?
O10 C26 H26 116.3 . . ?
O10 C26 H26A 116.3 . . ?
N1 C26 H26 116.3 . . ?
N1 C26 H26A 116.3 . . ?
N1 C27A H27A 109.5 . . ?
N1 C27A H27B 109.5 . . ?
N1 C27A H27C 109.5 . . ?
H27A C27A H27B 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
N1 C27B H27D 109.5 . . ?
N1 C27B H27E 109.5 . . ?
N1 C27B H27F 109.5 . . ?
H27D C27B H27E 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O1 C1 O2 -3.1(6) . . . . ?
Pb1 O1 C1 C2 175.7(4) . . . . ?
Pb1 O2 C1 O1 2.6(5) . . . . ?
Pb1 O2 C1 C2 -176.1(5) . . . . ?
Pb1 O3 C13 O4 160.2(6) . . . . ?
Pb1 O3 C13 C14 -20.2(12) . . . . ?
Pb1 O8 C20 O9 -12.7(6) 1_545 . . . ?
Pb1 O8 C20 C19 165.3(4) 1_545 . . . ?
Pb1 O9 C20 O8 12.4(6) 1_545 . . . ?
Pb1 O9 C20 C19 -165.7(4) 1_545 . . . ?
Pb2 O3 C13 O4 8.0(6) . . . . ?
Pb2 O3 C13 C14 -172.4(5) . . . . ?
Pb2 O4 C13 O3 -8.9(7) . . . . ?
Pb2 O4 C13 C14 171.5(5) . . . . ?
Pb2 O5 C7 O6 -2.3(6) . . . . ?
Pb2 O5 C7 C8 176.5(4) . . . . ?
O1 C1 C2 C3 -7.0(8) . . . . ?
O1 C1 C2 C6 174.7(5) . . . 2_775 ?
O2 C1 C2 C3 171.7(6) . . . . ?
O2 C1 C2 C6 -6.5(8) . . . 2_775 ?
O3 C13 C14 C15 178.0(6) . . . . ?
O3 C13 C14 C24 -4.6(9) . . . . ?
O4 C13 C14 C15 -2.3(9) . . . . ?
O4 C13 C14 C24 175.1(6) . . . . ?
O5 C7 C8 C9 -165.3(6) . . . . ?
O5 C7 C8 C12 14.0(9) . . . 2_465 ?
O6 C7 C8 C9 13.4(9) . . . . ?
O6 C7 C8 C12 -167.2(6) . . . 2_465 ?
C1 C2 C3 C4 179.6(6) . . . . ?
C2 C3 C4 C4 1.2(11) . . . 2_775 ?
C2 C3 C4 C5 -178.6(7) . . . . ?
C3 C4 C5 C6 -179.7(7) . . . . ?
C4 C4 C5 C6 0.5(12) 2_775 . . . ?
C4 C5 C6 C2 0.5(11) . . . 2_775 ?
C6 C2 C3 C4 -2.2(9) 2_775 . . . ?
C7 C8 C9 C10 -179.9(6) . . . . ?
C8 C9 C10 C10 -0.1(13) . . . 2_465 ?
C8 C9 C10 C11 -179.4(7) . . . . ?
C9 C10 C11 C12 -178.7(8) . . . . ?
C10 C10 C11 C12 2.0(15) 2_465 . . . ?
C10 C11 C12 C8 -2.7(14) . . . 2_465 ?
C12 C8 C9 C10 0.8(11) 2_465 . . . ?
C13 C14 C15 C16 177.0(5) . . . . ?
C13 C14 C24 C23 -178.0(5) . . . . ?
C14 C15 C16 C17 0.1(9) . . . . ?
C15 C14 C24 C23 -0.7(9) . . . . ?
C15 C16 C17 C18 -177.3(6) . . . . ?
C15 C16 C17 C23 1.3(9) . . . . ?
C16 C17 C18 C19 -179.3(6) . . . . ?
C16 C17 C23 C22 179.3(6) . . . . ?
C16 C17 C23 C24 -2.4(8) . . . . ?
C17 C18 C19 C20 -177.2(5) . . . . ?
C17 C18 C19 C21 0.1(9) . . . . ?
C17 C23 C24 C14 2.1(9) . . . . ?
C18 C17 C23 C22 -2.0(8) . . . . ?
C18 C17 C23 C24 176.3(5) . . . . ?
C18 C19 C20 O8 7.2(8) . . . . ?
C18 C19 C20 O9 -174.7(6) . . . . ?
C18 C19 C21 C22 -2.3(9) . . . . ?
C19 C21 C22 C23 2.3(9) . . . . ?
C20 C19 C21 C22 175.1(6) . . . . ?
C21 C19 C20 O8 -170.1(5) . . . . ?
C21 C19 C20 O9 8.0(8) . . . . ?
C21 C22 C23 C17 -0.2(9) . . . . ?
C21 C22 C23 C24 -178.4(6) . . . . ?
C22 C23 C24 C14 -179.7(6) . . . . ?
C23 C17 C18 C19 2.0(9) . . . . ?
C24 C14 C15 C16 -0.4(9) . . . . ?
C25 N1 C26 O10 178.3(10) . . . . ?
C27A N1 C26 O10 -22.0(15) . . . . ?
C27B N1 C26 O10 47(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_SMOF-1
_database_code_depnum_ccdc_archive 'CCDC 1878319'
_audit_update_record             
;
2018-12-13 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_audit_creation_date             2018-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            '[Pb(1,4-ndc)DMF]n'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H13 N O5 Pb'
_chemical_formula_sum            'C15 H13 N O5 Pb'
_chemical_formula_weight         494.45
_chemical_absolute_configuration rm
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.9990(3)
_cell_length_b                   14.0842(6)
_cell_length_c                   15.1934(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1497.69(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4785
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7520
_cell_measurement_theta_min      3.9400
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.23b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   'Sphere (Rigaku CrystalClear)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8515
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.676
_diffrn_reflns_theta_min         3.946
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      5.00  32.00   0.50    1.33    --    5.00  45.00   0.00   54
  2  ω    -92.00  45.00   0.50    1.33    --  -11.10  45.00 120.00  274
  3  ω    -47.00   8.00   0.50    1.33    --  -11.10  45.00  30.00  110
  4  ω   -100.00 -74.00   0.50    1.33    --  -11.10  45.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0803211000
_diffrn_orient_matrix_UB_12      -0.0230437000
_diffrn_orient_matrix_UB_13      -0.0187137000
_diffrn_orient_matrix_UB_21      -0.0012205000
_diffrn_orient_matrix_UB_22      0.0337436000
_diffrn_orient_matrix_UB_23      -0.0346636000
_diffrn_orient_matrix_UB_31      0.0618783000
_diffrn_orient_matrix_UB_32      -0.0293980000
_diffrn_orient_matrix_UB_33      -0.0250464000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.744
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.905
_reflns_number_gt                3023
_reflns_number_total             3300
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.254(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0257
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0151P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0454
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.746(12)
 0.254(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C5(H5), C7(H7), C13(H13), C4(H4), C6(H6)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.63554(3) 0.30436(2) 0.55486(2) 0.02540(8) Uani 1 1 d . . . . .
O3 O 0.2206(6) 0.7384(4) 0.0970(3) 0.0325(12) Uani 1 1 d . . . . .
O4 O 0.4816(6) 0.6719(4) 0.0433(3) 0.0307(13) Uani 1 1 d . . . . .
O1 O 0.3911(8) 0.3880(5) 0.4428(4) 0.0633(17) Uani 1 1 d . . . . .
C10 C 0.3501(10) 0.6773(5) 0.1015(4) 0.0245(15) Uani 1 1 d . . . . .
O2 O 0.2062(10) 0.3164(5) 0.3441(4) 0.0649(19) Uani 1 1 d . . . . .
O5 O 0.6419(12) 0.4466(6) 0.6711(5) 0.103(3) Uani 1 1 d . . . . .
C8 C 0.3359(10) 0.6352(5) 0.2649(4) 0.0265(16) Uani 1 1 d . . . . .
C9 C 0.3509(10) 0.6076(5) 0.1749(4) 0.0264(15) Uani 1 1 d . . . . .
C11 C 0.3595(11) 0.5136(5) 0.1537(4) 0.0357(17) Uani 1 1 d . . . . .
H11 H 0.378628 0.495930 0.095412 0.043 Uiso 1 1 calc R . . . .
N1 N 0.6600(10) 0.4507(6) 0.8211(5) 0.055(2) Uani 1 1 d . . . . .
C3 C 0.3316(9) 0.5629(6) 0.3315(4) 0.0290(17) Uani 1 1 d . . . . .
C1 C 0.3075(11) 0.3841(7) 0.3701(6) 0.042(2) Uani 1 1 d . . . . .
C12 C 0.3401(11) 0.4433(5) 0.2181(5) 0.0355(17) Uani 1 1 d . . . . .
H12 H 0.335800 0.379930 0.200955 0.043 Uiso 1 1 calc R . . . .
C5 C 0.3237(12) 0.6858(7) 0.4425(5) 0.057(2) Uani 1 1 d . . . . .
H5 H 0.324187 0.703480 0.501437 0.068 Uiso 1 1 calc R . . . .
C7 C 0.3294(11) 0.7314(6) 0.2908(5) 0.038(2) Uani 1 1 d . . . . .
H7 H 0.330914 0.778682 0.248118 0.045 Uiso 1 1 calc R . . . .
C13 C 0.6431(14) 0.4926(9) 0.7421(8) 0.076(3) Uani 1 1 d . . . . .
H13 H 0.631924 0.558377 0.739707 0.091 Uiso 1 1 calc R . . . .
C2 C 0.3272(9) 0.4651(6) 0.3052(4) 0.0303(17) Uani 1 1 d . . . . .
C4 C 0.3255(11) 0.5932(7) 0.4211(5) 0.046(2) Uani 1 1 d . . . . .
H4 H 0.322819 0.547880 0.465650 0.055 Uiso 1 1 calc R . . . .
C14 C 0.6619(16) 0.5073(10) 0.8986(7) 0.095(4) Uani 1 1 d . . . . .
H14A H 0.653416 0.573128 0.882719 0.142 Uiso 1 1 calc GR . . . .
H14B H 0.778510 0.496341 0.930247 0.142 Uiso 1 1 calc GR . . . .
H14C H 0.555067 0.490578 0.935044 0.142 Uiso 1 1 calc GR . . . .
C15 C 0.6733(16) 0.3514(9) 0.8222(9) 0.096(4) Uani 1 1 d . . . . .
H15A H 0.563593 0.325405 0.851546 0.143 Uiso 1 1 calc GR . . . .
H15B H 0.787061 0.332805 0.852995 0.143 Uiso 1 1 calc GR . . . .
H15C H 0.678200 0.328036 0.762928 0.143 Uiso 1 1 calc GR . . . .
C6 C 0.3211(13) 0.7559(7) 0.3775(6) 0.055(3) Uani 1 1 d . . . . .
H6 H 0.313626 0.819563 0.393441 0.066 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O3 2.643(5) 2_565 ?
Pb1 O3 2.683(5) 3_645 ?
Pb1 O4 2.525(5) 3_645 ?
Pb1 O4 2.706(4) 2_665 ?
Pb1 O1 2.685(5) . ?
Pb1 O2 2.344(6) 4_556 ?
Pb1 O5 2.672(7) . ?
O3 C10 1.251(8) . ?
O4 C10 1.278(8) . ?
O1 C1 1.252(9) . ?
C10 C9 1.486(9) . ?
O2 C1 1.251(10) . ?
O5 C13 1.257(12) . ?
C8 C9 1.425(9) . ?
C8 C3 1.435(10) . ?
C8 C7 1.412(10) . ?
C9 C11 1.363(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.399(10) . ?
N1 C13 1.343(13) . ?
N1 C14 1.421(11) . ?
N1 C15 1.402(14) . ?
C3 C2 1.435(10) . ?
C3 C4 1.428(10) . ?
C1 C2 1.514(10) . ?
C12 H12 0.9300 . ?
C12 C2 1.362(10) . ?
C5 H5 0.9300 . ?
C5 C4 1.345(12) . ?
C5 C6 1.396(12) . ?
C7 H7 0.9300 . ?
C7 C6 1.363(10) . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C6 H6 0.9300 . ?

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
O3 Pb1 O3 118.89(11) 2_565 3_645 ?
O3 Pb1 O4 167.88(15) 2_565 2_665 ?
O3 Pb1 O4 67.38(14) 3_645 2_665 ?
O3 Pb1 O1 81.14(16) 3_645 . ?
O3 Pb1 O1 69.68(16) 2_565 . ?
O3 Pb1 O5 91.5(2) 2_565 . ?
O4 Pb1 O3 50.06(14) 3_645 3_645 ?
O4 Pb1 O3 70.64(15) 3_645 2_565 ?
O4 Pb1 O4 111.98(12) 3_645 2_665 ?
O4 Pb1 O1 75.10(19) 3_645 . ?
O4 Pb1 O5 161.82(19) 3_645 . ?
O1 Pb1 O4 122.38(16) . 2_665 ?
O2 Pb1 O3 103.4(2) 4_556 3_645 ?
O2 Pb1 O3 82.8(2) 4_556 2_565 ?
O2 Pb1 O4 85.4(2) 4_556 3_645 ?
O2 Pb1 O4 85.6(2) 4_556 2_665 ?
O2 Pb1 O1 150.2(2) 4_556 . ?
O2 Pb1 O5 96.2(3) 4_556 . ?
O5 Pb1 O3 145.3(2) . 3_645 ?
O5 Pb1 O4 86.2(2) . 2_665 ?
O5 Pb1 O1 95.8(2) . . ?
Pb1 O3 Pb1 102.99(15) 2_564 3_655 ?
C10 O3 Pb1 122.7(4) . 2_564 ?
C10 O3 Pb1 90.8(4) . 3_655 ?
Pb1 O4 Pb1 105.58(16) 3_655 2_664 ?
C10 O4 Pb1 131.4(4) . 2_664 ?
C10 O4 Pb1 97.5(4) . 3_655 ?
C1 O1 Pb1 146.9(6) . . ?
O3 C10 O4 121.6(6) . . ?
O3 C10 C9 119.9(6) . . ?
O4 C10 C9 118.4(6) . . ?
C1 O2 Pb1 117.8(5) . 4_456 ?
C13 O5 Pb1 162.4(8) . . ?
C9 C8 C3 119.0(7) . . ?
C7 C8 C9 122.1(7) . . ?
C7 C8 C3 118.9(6) . . ?
C8 C9 C10 122.6(6) . . ?
C11 C9 C10 117.7(6) . . ?
C11 C9 C8 119.6(6) . . ?
C9 C11 H11 119.4 . . ?
C9 C11 C12 121.2(6) . . ?
C12 C11 H11 119.4 . . ?
C13 N1 C14 119.7(10) . . ?
C13 N1 C15 117.1(10) . . ?
C15 N1 C14 123.3(11) . . ?
C2 C3 C8 119.0(6) . . ?
C4 C3 C8 117.5(7) . . ?
C4 C3 C2 123.4(7) . . ?
O1 C1 C2 119.9(8) . . ?
O2 C1 O1 125.2(8) . . ?
O2 C1 C2 114.8(8) . . ?
C11 C12 H12 119.1 . . ?
C2 C12 C11 121.8(7) . . ?
C2 C12 H12 119.1 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.1(8) . . ?
C6 C5 H5 119.5 . . ?
C8 C7 H7 119.5 . . ?
C6 C7 C8 121.0(8) . . ?
C6 C7 H7 119.5 . . ?
O5 C13 N1 122.7(11) . . ?
O5 C13 H13 118.6 . . ?
N1 C13 H13 118.6 . . ?
C3 C2 C1 123.0(6) . . ?
C12 C2 C3 119.0(7) . . ?
C12 C2 C1 118.0(7) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.3(8) . . ?
C5 C4 H4 119.3 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.2(9) . . ?
C7 C6 H6 119.9 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O3 C10 O4 107.5(6) 2_564 . . . ?
Pb1 O3 C10 O4 1.5(6) 3_655 . . . ?
Pb1 O3 C10 C9 -71.3(7) 2_564 . . . ?
Pb1 O3 C10 C9 -177.3(5) 3_655 . . . ?
Pb1 O4 C10 O3 -1.6(7) 3_655 . . . ?
Pb1 O4 C10 O3 116.9(6) 2_664 . . . ?
Pb1 O4 C10 C9 177.2(5) 3_655 . . . ?
Pb1 O4 C10 C9 -64.3(8) 2_664 . . . ?
Pb1 O1 C1 O2 54.8(13) . . . . ?
Pb1 O1 C1 C2 -124.4(9) . . . . ?
Pb1 O2 C1 O1 7.9(11) 4_456 . . . ?
Pb1 O2 C1 C2 -172.8(4) 4_456 . . . ?
Pb1 O5 C13 N1 8(3) . . . . ?
O3 C10 C9 C8 -51.2(9) . . . . ?
O3 C10 C9 C11 126.3(8) . . . . ?
O4 C10 C9 C8 130.0(7) . . . . ?
O4 C10 C9 C11 -52.5(9) . . . . ?
O1 C1 C2 C3 -38.4(10) . . . . ?
O1 C1 C2 C12 142.0(7) . . . . ?
C10 C9 C11 C12 -173.0(7) . . . . ?
O2 C1 C2 C3 142.3(8) . . . . ?
O2 C1 C2 C12 -37.3(10) . . . . ?
C8 C9 C11 C12 4.6(12) . . . . ?
C8 C3 C2 C1 -175.3(6) . . . . ?
C8 C3 C2 C12 4.3(10) . . . . ?
C8 C3 C4 C5 0.1(11) . . . . ?
C8 C7 C6 C5 1.6(13) . . . . ?
C9 C8 C3 C2 -4.9(9) . . . . ?
C9 C8 C3 C4 177.1(6) . . . . ?
C9 C8 C7 C6 -177.9(7) . . . . ?
C9 C11 C12 C2 -5.4(12) . . . . ?
C11 C12 C2 C3 0.7(11) . . . . ?
C11 C12 C2 C1 -179.7(7) . . . . ?
C3 C8 C9 C10 178.0(6) . . . . ?
C3 C8 C9 C11 0.5(10) . . . . ?
C3 C8 C7 C6 0.6(12) . . . . ?
C7 C8 C9 C10 -3.5(11) . . . . ?
C7 C8 C9 C11 179.0(8) . . . . ?
C7 C8 C3 C2 176.5(7) . . . . ?
C7 C8 C3 C4 -1.5(10) . . . . ?
C2 C3 C4 C5 -177.8(8) . . . . ?
C4 C3 C2 C1 2.6(11) . . . . ?
C4 C3 C2 C12 -177.8(7) . . . . ?
C4 C5 C6 C7 -3.1(13) . . . . ?
C14 N1 C13 O5 179.5(9) . . . . ?
C15 N1 C13 O5 -1.1(16) . . . . ?
C6 C5 C4 C3 2.2(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.797
_oxdiff_exptl_absorpt_empirical_full_min 0.654
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.746(12)
2 0.254(12)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_SMOF-2
_database_code_depnum_ccdc_archive 'CCDC 1878320'
_audit_update_record             
;
2018-12-17 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_audit_creation_date             2018-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            '[Pb(1,4-ndc)DMA]n'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H15 N O5 Pb'
_chemical_formula_sum            'C16 H15 N O5 Pb'
_chemical_formula_weight         508.48
_chemical_absolute_configuration rm
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.036(2)
_cell_length_b                   14.584(5)
_cell_length_c                   15.051(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1544.4(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6181
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.949
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.23b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   'Sphere (Rigaku CrystalClear)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16497
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         3.046
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                3217
_reflns_number_total             3510
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 
;
 Flack x determined using 1290 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(8)
_refine_ls_extinction_coef       0.0048(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3510
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0239
_refine_ls_restrained_S_all      0.917
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0504
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C13A) = Uanis(C13B)
Uanis(C14A) = Uanis(C14B)
Uanis(C15A) = Uanis(C15B)
Uanis(N1A) = Uanis(N1B)
3. Others
 Sof(N1B)=Sof(C13B)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15B)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(N1A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15A)=
 Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
4.b Idealised Me refined as rotating group:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C14B(H14D,H14E,H14F), C15B(H15D,
 H15E,H15F), C16(H16A,H16B,H16C), C16(H16D,H16E,H16F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.60960(4) 0.30889(2) 0.45455(2) 0.02016(9) Uani 1 1 d . . . . .
O1 O 0.7364(8) 0.2024(4) 0.5754(3) 0.0273(13) Uani 1 1 d . . . . .
O2 O 0.4742(8) 0.1422(4) 0.5163(4) 0.0277(13) Uani 1 1 d . . . . .
O3 O 0.4742(11) -0.0897(5) 0.9286(4) 0.0499(19) Uani 1 1 d . . . . .
O4 O 0.6523(10) -0.1981(5) 0.8650(4) 0.0519(17) Uani 1 1 d . . . . .
O5 O 0.6125(15) 0.4373(6) 0.3420(6) 0.079(3) Uani 1 1 d . . . . .
C1 C 0.6059(13) 0.1412(5) 0.5727(4) 0.0198(15) Uani 1 1 d . . . . .
C2 C 0.6096(12) 0.0696(5) 0.6438(4) 0.0187(14) Uani 1 1 d . . . . .
C3 C 0.6071(14) 0.0980(5) 0.7310(5) 0.0263(16) Uani 1 1 d . . . . .
H3 H 0.615083 0.160181 0.744053 0.032 Uiso 1 1 calc R . . . .
C4 C 0.5925(13) 0.0342(5) 0.8007(5) 0.0277(18) Uani 1 1 d . . . . .
H4 H 0.582383 0.055423 0.858758 0.033 Uiso 1 1 calc R . . . .
C5 C 0.5929(12) -0.0586(5) 0.7854(5) 0.0242(16) Uani 1 1 d . . . . .
C6 C 0.6103(12) -0.0909(5) 0.6958(5) 0.0216(15) Uani 1 1 d . . . . .
C7 C 0.6199(13) -0.1864(6) 0.6724(6) 0.0361(19) Uani 1 1 d . . . . .
H7 H 0.619191 -0.230368 0.717099 0.043 Uiso 1 1 calc R . . . .
C8 C 0.6299(17) -0.2135(6) 0.5866(6) 0.046(3) Uani 1 1 d . . . . .
H8 H 0.636280 -0.275707 0.573482 0.055 Uiso 1 1 calc R . . . .
C9 C 0.6310(18) -0.1498(6) 0.5172(6) 0.046(3) Uani 1 1 d . . . . .
H9 H 0.637578 -0.169896 0.458608 0.055 Uiso 1 1 calc R . . . .
C10 C 0.6224(13) -0.0584(5) 0.5351(5) 0.0336(18) Uani 1 1 d . . . . .
H10 H 0.623403 -0.016392 0.488585 0.040 Uiso 1 1 calc R . . . .
C11 C 0.6119(12) -0.0264(5) 0.6240(4) 0.0201(14) Uani 1 1 d . . . . .
C12 C 0.5747(12) -0.1219(6) 0.8653(6) 0.033(2) Uani 1 1 d . . . . .
N1A N 0.610(4) 0.5628(17) 0.2559(12) 0.055(5) Uani 0.568(14) 1 d . . P A 1
C13A C 0.613(3) 0.5254(13) 0.3350(12) 0.042(3) Uani 0.568(14) 1 d . . P A 1
C14A C 0.620(5) 0.591(2) 0.4166(15) 0.062(6) Uani 0.568(14) 1 d . . P A 1
H14A H 0.517280 0.634028 0.412950 0.093 Uiso 0.568(14) 1 calc GR . P A 1
H14B H 0.738781 0.623121 0.416845 0.093 Uiso 0.568(14) 1 calc GR . P A 1
H14C H 0.608156 0.555679 0.470224 0.093 Uiso 0.568(14) 1 calc GR . P A 1
C15A C 0.587(5) 0.493(3) 0.185(2) 0.101(12) Uani 0.568(14) 1 d . . P A 1
H15A H 0.678355 0.504323 0.138684 0.151 Uiso 0.568(14) 1 calc GR . P A 1
H15B H 0.461164 0.496666 0.160708 0.151 Uiso 0.568(14) 1 calc GR . P A 1
H15C H 0.607630 0.433047 0.209293 0.151 Uiso 0.568(14) 1 calc GR . P A 1
N1B N 0.612(6) 0.575(2) 0.2993(16) 0.055(5) Uani 0.432(14) 1 d . . P A 2
C13B C 0.611(4) 0.4914(17) 0.2762(15) 0.042(3) Uani 0.432(14) 1 d . . P A 2
C14B C 0.616(8) 0.469(3) 0.171(3) 0.062(6) Uani 0.432(14) 1 d . . P A 2
H14D H 0.531596 0.510204 0.140702 0.093 Uiso 0.432(14) 1 calc GR . P A 2
H14E H 0.575716 0.407081 0.161648 0.093 Uiso 0.432(14) 1 calc GR . P A 2
H14F H 0.742744 0.477111 0.149509 0.093 Uiso 0.432(14) 1 calc GR . P A 2
C15B C 0.627(7) 0.600(5) 0.388(2) 0.101(12) Uani 0.432(14) 1 d . . P A 2
H15D H 0.704967 0.654159 0.392399 0.151 Uiso 0.432(14) 1 calc GR . P A 2
H15E H 0.685036 0.551226 0.420931 0.151 Uiso 0.432(14) 1 calc GR . P A 2
H15F H 0.503443 0.612736 0.411441 0.151 Uiso 0.432(14) 1 calc GR . P A 2
C16 C 0.609(2) 0.6547(8) 0.2348(10) 0.087(5) Uani 1 1 d . . . . .
H16A H 0.652890 0.662528 0.174788 0.130 Uiso 0.568(14) 1 calc GR . P A 1
H16B H 0.692477 0.687009 0.274506 0.130 Uiso 0.568(14) 1 calc GR . P A 1
H16C H 0.482797 0.678513 0.240258 0.130 Uiso 0.568(14) 1 calc GR . P A 1
H16D H 0.563246 0.708496 0.264465 0.130 Uiso 0.432(14) 1 calc GR . P A 2
H16E H 0.527682 0.640399 0.185608 0.130 Uiso 0.432(14) 1 calc GR . P A 2
H16F H 0.735936 0.665666 0.213383 0.130 Uiso 0.432(14) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.669(5) 4_456 ?
Pb1 O1 2.552(5) . ?
Pb1 O2 2.699(6) 4_556 ?
Pb1 O3 2.372(6) 3_656 ?
Pb1 O4 2.690(6) 2_654 ?
Pb1 O5 2.525(7) . ?
O1 C1 1.281(10) . ?
O2 C1 1.257(9) . ?
O3 C12 1.276(11) . ?
O4 C12 1.237(10) . ?
O5 C13A 1.29(2) . ?
O5 C13B 1.27(2) . ?
C1 C2 1.495(9) . ?
C2 C3 1.377(10) . ?
C2 C11 1.432(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.405(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.373(11) . ?
C5 C6 1.433(10) . ?
C5 C12 1.521(10) . ?
C6 C7 1.438(11) . ?
C6 C11 1.433(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.352(12) . ?
C8 H8 0.9300 . ?
C8 C9 1.398(13) . ?
C9 H9 0.9300 . ?
C9 C10 1.362(11) . ?
C10 H10 0.9300 . ?
C10 C11 1.418(10) . ?
N1A C13A 1.31(2) . ?
N1A C15A 1.48(4) . ?
N1A C16 1.38(3) . ?
C13A C14A 1.56(3) . ?
C14A H14A 0.9600 . ?
C14A H14B 0.9600 . ?
C14A H14C 0.9600 . ?
C15A H15A 0.9600 . ?
C15A H15B 0.9600 . ?
C15A H15C 0.9600 . ?
N1B C13B 1.27(4) . ?
N1B C15B 1.39(4) . ?
N1B C16 1.52(3) . ?
C13B C14B 1.61(5) . ?
C14B H14D 0.9600 . ?
C14B H14E 0.9600 . ?
C14B H14F 0.9600 . ?
C15B H15D 0.9600 . ?
C15B H15E 0.9600 . ?
C15B H15F 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 H16D 0.9600 . ?
C16 H16E 0.9600 . ?
C16 H16F 0.9600 . ?

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 115.24(14) . 4_456 ?
O1 Pb1 O2 73.31(17) . 4_556 ?
O1 Pb1 O2 168.21(17) 4_456 4_556 ?
O1 Pb1 O4 119.41(19) 4_456 2_654 ?
O1 Pb1 O4 76.9(2) . 2_654 ?
O3 Pb1 O1 86.4(2) 3_656 . ?
O3 Pb1 O1 85.4(2) 3_656 4_456 ?
O3 Pb1 O2 87.2(2) 3_656 4_556 ?
O3 Pb1 O4 154.3(2) 3_656 2_654 ?
O3 Pb1 O5 92.1(3) 3_656 . ?
O4 Pb1 O2 69.41(18) 2_654 4_556 ?
O5 Pb1 O1 86.6(3) . 4_456 ?
O5 Pb1 O1 157.9(3) . . ?
O5 Pb1 O2 84.6(3) . 4_556 ?
O5 Pb1 O4 96.0(3) . 2_654 ?
Pb1 O1 Pb1 105.14(18) . 4_556 ?
C1 O1 Pb1 131.1(5) . 4_556 ?
C1 O1 Pb1 98.7(4) . . ?
C1 O2 Pb1 126.4(5) . 4_456 ?
C12 O3 Pb1 117.5(6) . 3_646 ?
C12 O4 Pb1 144.3(6) . 2_655 ?
C13A O5 Pb1 142.5(10) . . ?
C13B O5 Pb1 170.6(14) . . ?
O1 C1 C2 116.9(7) . . ?
O2 C1 O1 122.8(6) . . ?
O2 C1 C2 120.3(7) . . ?
C3 C2 C1 118.1(6) . . ?
C3 C2 C11 119.5(6) . . ?
C11 C2 C1 122.3(6) . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.9(7) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.8(7) . . ?
C5 C4 H4 119.1 . . ?
C4 C5 C6 118.8(6) . . ?
C4 C5 C12 117.7(7) . . ?
C6 C5 C12 123.5(7) . . ?
C5 C6 C7 123.5(6) . . ?
C11 C6 C5 119.7(6) . . ?
C11 C6 C7 116.8(6) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.3(7) . . ?
C8 C7 H7 119.4 . . ?
C7 C8 H8 119.3 . . ?
C7 C8 C9 121.3(8) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.1(8) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.6 . . ?
C9 C10 C11 120.7(7) . . ?
C11 C10 H10 119.6 . . ?
C2 C11 C6 119.0(6) . . ?
C10 C11 C2 121.2(6) . . ?
C10 C11 C6 119.8(6) . . ?
O3 C12 C5 114.4(8) . . ?
O4 C12 O3 125.2(8) . . ?
O4 C12 C5 120.3(8) . . ?
C13A N1A C15A 112(3) . . ?
C13A N1A C16 128(2) . . ?
C16 N1A C15A 120(2) . . ?
O5 C13A N1A 119(2) . . ?
O5 C13A C14A 123.2(15) . . ?
N1A C13A C14A 117(2) . . ?
C13A C14A H14A 109.5 . . ?
C13A C14A H14B 109.5 . . ?
C13A C14A H14C 109.5 . . ?
H14A C14A H14B 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
N1A C15A H15A 109.5 . . ?
N1A C15A H15B 109.5 . . ?
N1A C15A H15C 109.5 . . ?
H15A C15A H15B 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C13B N1B C15B 121(4) . . ?
C13B N1B C16 124(2) . . ?
C15B N1B C16 114(4) . . ?
O5 C13B C14B 130(2) . . ?
N1B C13B O5 113(2) . . ?
N1B C13B C14B 118(2) . . ?
C13B C14B H14D 109.5 . . ?
C13B C14B H14E 109.5 . . ?
C13B C14B H14F 109.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
N1B C15B H15D 109.5 . . ?
N1B C15B H15E 109.5 . . ?
N1B C15B H15F 109.5 . . ?
H15D C15B H15E 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
N1A C16 H16A 109.5 . . ?
N1A C16 H16B 109.5 . . ?
N1A C16 H16C 109.5 . . ?
N1B C16 H16D 109.5 . . ?
N1B C16 H16E 109.5 . . ?
N1B C16 H16F 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
H16D C16 H16E 109.5 . . ?
H16D C16 H16F 109.5 . . ?
H16E C16 H16F 109.5 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O1 C1 O2 5.1(7) . . . . ?
Pb1 O1 C1 O2 -113.8(7) 4_556 . . . ?
Pb1 O1 C1 C2 69.4(8) 4_556 . . . ?
Pb1 O1 C1 C2 -171.7(6) . . . . ?
Pb1 O2 C1 O1 -104.7(7) 4_456 . . . ?
Pb1 O2 C1 C2 72.0(8) 4_456 . . . ?
Pb1 O3 C12 O4 -9.7(12) 3_646 . . . ?
Pb1 O3 C12 C5 169.5(5) 3_646 . . . ?
Pb1 O4 C12 O3 -54.5(14) 2_655 . . . ?
Pb1 O4 C12 C5 126.3(9) 2_655 . . . ?
Pb1 O5 C13A N1A -178.2(18) . . . . ?
Pb1 O5 C13A C14A 3(4) . . . . ?
O1 C1 C2 C3 55.8(11) . . . . ?
O1 C1 C2 C11 -125.5(8) . . . . ?
O2 C1 C2 C3 -121.1(9) . . . . ?
O2 C1 C2 C11 57.6(11) . . . . ?
C1 C2 C3 C4 174.0(9) . . . . ?
C1 C2 C11 C6 -178.3(8) . . . . ?
C1 C2 C11 C10 3.9(13) . . . . ?
C2 C3 C4 C5 4.4(15) . . . . ?
C3 C2 C11 C6 0.4(13) . . . . ?
C3 C2 C11 C10 -177.4(9) . . . . ?
C3 C4 C5 C6 0.5(14) . . . . ?
C3 C4 C5 C12 -179.5(8) . . . . ?
C4 C5 C6 C7 177.4(9) . . . . ?
C4 C5 C6 C11 -4.8(13) . . . . ?
C4 C5 C12 O3 32.3(12) . . . . ?
C4 C5 C12 O4 -148.5(9) . . . . ?
C5 C6 C7 C8 177.8(10) . . . . ?
C5 C6 C11 C2 4.3(13) . . . . ?
C5 C6 C11 C10 -177.8(8) . . . . ?
C6 C5 C12 O3 -147.7(9) . . . . ?
C6 C5 C12 O4 31.5(13) . . . . ?
C6 C7 C8 C9 -0.1(19) . . . . ?
C7 C6 C11 C2 -177.7(8) . . . . ?
C7 C6 C11 C10 0.1(13) . . . . ?
C7 C8 C9 C10 0(2) . . . . ?
C8 C9 C10 C11 -0.1(18) . . . . ?
C9 C10 C11 C2 177.8(10) . . . . ?
C9 C10 C11 C6 0.0(15) . . . . ?
C11 C2 C3 C4 -4.8(14) . . . . ?
C11 C6 C7 C8 0.0(15) . . . . ?
C12 C5 C6 C7 -2.6(14) . . . . ?
C12 C5 C6 C11 175.2(8) . . . . ?
C15A N1A C13A O5 6(4) . . . . ?
C15A N1A C13A C14A -175(3) . . . . ?
C15B N1B C13B O5 4(5) . . . . ?
C15B N1B C13B C14B -173(4) . . . . ?
C16 N1A C13A O5 -180(2) . . . . ?
C16 N1A C13A C14A -1(4) . . . . ?
C16 N1B C13B O5 -180(3) . . . . ?
C16 N1B C13B C14B 3(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
