#------------------------------------------------------------------------------
#$Date: 2019-11-24 16:08:35 +0200 (Sun, 24 Nov 2019) $
#$Revision: 238487 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/76/7237665.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_7237665
loop_
_publ_author_name
'Pournara, Anastasia D.'
'Margariti, Antigoni'
'Tarlas, Georgios D.'
'Kourtelaris, Andreas'
'Petkov, Valeri'
'Kokkinos, Christos'
'Economou, Anastasios'
'Papaefstathiou, Giannis S.'
'Manos, Manolis J.'
_publ_section_title
;
 A Ca2+ MOF combining highly efficient sorption and capability for
 voltammetric determination of heavy metal ions in aqueous media
;
_journal_issue                   25
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              15432
_journal_paper_doi               10.1039/C9TA03337H
_journal_volume                  7
_journal_year                    2019
_chemical_formula_sum            'C9 H4 N O6 Pb'
_chemical_formula_weight         429.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-27 deposited with the CCDC.	2019-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   4.1673(2)
_cell_length_b                   25.707(2)
_cell_length_c                   18.2223(9)
_cell_measurement_reflns_used    1628
_cell_measurement_temperature    106.6(2)
_cell_measurement_theta_max      72.5850
_cell_measurement_theta_min      4.1610
_cell_volume                     1952.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT, (Sheldrick, 2015)'
_diffrn_ambient_temperature      106.6(2)
_diffrn_detector_area_resol_mean 10.4223
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6617
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.964
_diffrn_reflns_theta_max         66.964
_diffrn_reflns_theta_min         4.209
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    33.853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.922
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.674
_refine_diff_density_min         -3.237
_refine_diff_density_rms         0.407
_refine_ls_extinction_coef       0.00063(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1708
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0870
_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)+(0.1820P)²+12.2758P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2808
_refine_ls_wR_factor_ref         0.3049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1053
_reflns_number_total             1708
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ta03337h2.cif
_cod_data_source_block           Pb_MOF
_cod_original_cell_volume        1952.2(2)
_cod_database_code               7237665
_shelx_shelxl_version_number     2018/3
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pb2 Pb 0.000000 0.76032(4) 0.750000 0.0387(7) Uani 1 2 d S TU P . .
Pb1 Pb 1.000000 0.55704(8) 0.250000 0.0718(8) Uani 1 2 d S TU P . .
O4 O 0.557(4) 0.7445(6) 0.6601(9) 0.046(4) Uani 1 1 d . U . . .
O3 O -0.024(4) 0.5307(6) 0.5854(8) 0.056(4) Uani 1 1 d . . . . .
C6 C 0.693(4) 0.6980(9) 0.5262(9) 0.047(5) Uani 1 1 d D . . . .
H6 H 0.795295 0.729259 0.536800 0.057 Uiso 1 1 calc R U . . .
O2 O 0.492(5) 0.5612(7) 0.3434(11) 0.075(7) Uani 1 1 d . . . . .
C3 C 0.380(5) 0.6025(6) 0.4938(9) 0.043(5) Uani 1 1 d D . . . .
C7 C 0.736(5) 0.6741(8) 0.4565(9) 0.046(5) Uani 1 1 d D U . . .
H7 H 0.869766 0.689127 0.421591 0.056 Uiso 1 1 calc R U . . .
C9 C 0.054(5) 0.5208(9) 0.5181(15) 0.049(5) Uani 1 1 d . U . . .
N1 N 0.248(5) 0.5534(6) 0.4790(9) 0.049(4) Uani 1 1 d D U . . .
H1 H 0.300338 0.541370 0.436663 0.059 Uiso 1 1 calc R U . . .
C2 C 0.572(5) 0.6272(7) 0.4413(11) 0.053(6) Uani 1 1 d D U . . .
C4 C 0.350(5) 0.6264(6) 0.5618(10) 0.039(4) Uani 1 1 d D . . . .
H4 H 0.227854 0.609775 0.597541 0.047 Uiso 1 1 calc R U . . .
C5 C 0.493(4) 0.6742(7) 0.5798(9) 0.042(4) Uani 1 1 d D . . . .
C8 C 0.420(6) 0.7025(8) 0.6462(11) 0.050(5) Uani 1 1 d D U . . .
C1 C 0.604(9) 0.6077(12) 0.3679(13) 0.075(8) Uani 1 1 d D U . . .
O5 O 0.193(4) 0.6853(6) 0.6853(7) 0.049(3) Uani 1 1 d . U . . .
O1 O 0.842(7) 0.6285(8) 0.3215(11) 0.086(6) Uani 1 1 d . U . . .
O6 O 0.500000 0.5712(11) 0.750000 0.066(8) Uani 1 2 d S TU P A 1
O7 O 0.500000 0.5428(13) 0.750000 0.079(9) Uani 1 2 d S TU P . .
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 Pb2 O5 73.1(7) . 3_556
O5 Pb2 O4 78.2(5) . 1_455
O5 Pb2 O4 86.8(5) 3_556 1_455
O5 Pb2 O4 86.8(5) . 3_656
O5 Pb2 O4 78.2(5) 3_556 3_656
O4 Pb2 O4 161.3(8) 1_455 3_656
O1 Pb1 O1 77.0(10) . 3_755
O1 Pb1 O2 80.2(8) . 1_655
O1 Pb1 O2 96.1(8) 3_755 1_655
O1 Pb1 O2 96.1(8) . 3_655
O1 Pb1 O2 80.2(8) 3_755 3_655
O2 Pb1 O2 175.4(8) 1_655 3_655
O1 Pb1 O2 122.4(7) . 3_755
O1 Pb1 O2 53.3(7) 3_755 3_755
O2 Pb1 O2 78.4(7) 1_655 3_755
O2 Pb1 O2 101.4(7) 3_655 3_755
O1 Pb1 O2 53.3(7) . .
O1 Pb1 O2 122.4(7) 3_755 .
O2 Pb1 O2 101.4(7) 1_655 .
O2 Pb1 O2 78.4(7) 3_655 .
O2 Pb1 O2 175.4(8) 3_755 .
C8 O4 Pb2 127.8(15) . 1_655
C5 C6 C7 120.1(19) . .
C5 C6 H6 120.0 . .
C7 C6 H6 120.0 . .
C1 O2 Pb1 120.7(19) . 1_455
C1 O2 Pb1 88.4(16) . .
Pb1 O2 Pb1 101.4(7) 1_455 .
C4 C3 C2 117.5(17) . .
C4 C3 N1 122.3(16) . .
C2 C3 N1 120.0(16) . .
C2 C7 C6 118.9(19) . .
C2 C7 H7 120.6 . .
C6 C7 H7 120.6 . .
O3 C9 C9 123(3) . 5_566
O3 C9 N1 121(2) . .
C9 C9 N1 116(3) 5_566 .
C9 N1 C3 133.2(18) . .
C9 N1 H1 113.4 . .
C3 N1 H1 113.4 . .
C3 C2 C7 121.9(18) . .
C3 C2 C1 122(2) . .
C7 C2 C1 115.9(19) . .
C3 C4 C5 123.8(18) . .
C3 C4 H4 118.1 . .
C5 C4 H4 118.1 . .
C4 C5 C6 117.8(17) . .
C4 C5 C8 123.1(17) . .
C6 C5 C8 118.7(17) . .
O4 C8 O5 122.0(18) . .
O4 C8 C5 121(2) . .
O5 C8 C5 117.0(19) . .
O2 C1 O1 112(2) . .
O2 C1 C2 126(2) . .
O1 C1 C2 119(2) . .
C8 O5 Pb2 104.4(12) . .
C1 O1 Pb1 103.5(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb2 O5 2.399(13) .
Pb2 O5 2.399(14) 3_556
Pb2 O4 2.500(14) 1_455
Pb2 O4 2.500(14) 3_656
Pb1 O1 2.35(2) .
Pb1 O1 2.35(2) 3_755
Pb1 O2 2.67(2) 1_655
Pb1 O2 2.67(2) 3_655
Pb1 O2 2.72(2) 3_755
Pb1 O2 2.72(2) .
O4 C8 1.25(3) .
O3 C9 1.29(3) .
C6 C5 1.421(17) .
C6 C7 1.422(17) .
C6 H6 0.9300 .
O2 C1 1.36(3) .
C3 C4 1.388(16) .
C3 C2 1.401(18) .
C3 N1 1.403(17) .
C7 C2 1.414(17) .
C7 H7 0.9300 .
C9 C9 1.33(5) 5_566
C9 N1 1.37(3) .
N1 H1 0.8600 .
C2 C1 1.435(19) .
C4 C5 1.404(17) .
C4 H4 0.9300 .
C5 C8 1.445(17) .
C8 O5 1.26(3) .
C1 O1 1.41(3) .
O6 O7 0.73(3) .
