#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:30:01 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232880 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/83/4348336.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_4348336
loop_
_publ_author_name
'Martínez-Casado, Francisco J'
'Ramos-Riesco, Miguel'
'Rodríguez-Cheda, José A'
'Cucinotta, Fabio'
'Matesanz, Emilio'
'Miletto, Ivana'
'Gianotti, Enrica'
'Marchese, Leonardo'
'Matěj, Zdeněk'
_publ_section_title
;
 Unraveling the Decomposition Process of Lead(II) Acetate: Anhydrous
 Polymorphs, Hydrates, and Byproducts and Room Temperature
 Phosphorescence.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8576
_journal_page_last               8586
_journal_paper_doi               10.1021/acs.inorgchem.6b01116
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C8 H14 O9 Pb2'
_chemical_formula_sum            'C8 H14 O9 Pb2'
_chemical_formula_weight         668.57
_chemical_name_common            'Lead(II) acetate hemihydrate'
_chemical_name_systematic
; 
 'Lead(II) acetate hemihydrate'
;
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.646(3)
_cell_length_b                   17.632(4)
_cell_length_c                   5.3720(11)
_cell_measurement_reflns_used    3096
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.38
_cell_measurement_theta_min      3.13
_cell_volume                     1387.3(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Mercury (Version 3.1; Macrae et al., 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 13.65
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'MAR225 CCD area-detector'
_diffrn_measurement_method       'f\ scans'
_diffrn_radiation_monochromator  'silicon(111) double crystal monochromator'
_diffrn_radiation_source         'undulator radiation'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            20092
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         31.38
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    27.588
_exptl_absorpt_correction_T_max  0.0595
_exptl_absorpt_correction_T_min  0.0317
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.025
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.269
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.171(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3090
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0462P)²+4.2060P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                2831
_reflns_number_total             3090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01116_si_002.cif
_cod_data_source_block           PbAc2Hemi
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4348336
_exptl_absorpt_correction_t_ave  0.0479
_shelx_f_squared_multiplier      1.000
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.1310(4) 0.4685(4) 0.183(2) 0.0136(13) Uani 1 1 d .
C2 C 0.1976(7) 0.4068(5) 0.2437(17) 0.0257(14) Uani 1 1 d .
H2A H 0.2038 0.4023 0.4248 0.039 Uiso 1 1 calc R
H2B H 0.2571 0.4190 0.1706 0.039 Uiso 1 1 calc R
H2C H 0.1755 0.3587 0.1753 0.039 Uiso 1 1 calc R
C3 C 0.1959(5) 0.7104(5) 0.0868(15) 0.0231(10) Uani 1 1 d .
C4 C 0.1920(7) 0.7756(6) 0.2624(15) 0.033(2) Uani 1 1 d .
H4A H 0.1536 0.7622 0.4053 0.049 Uiso 1 1 calc R
H4B H 0.1660 0.8197 0.1774 0.049 Uiso 1 1 calc R
H4C H 0.2538 0.7877 0.3202 0.049 Uiso 1 1 calc R
C5 C 0.3592(5) 0.4985(5) -0.1000(15) 0.0205(17) Uani 1 1 d .
C6 C 0.4326(6) 0.4571(6) 0.0400(18) 0.035(2) Uani 1 1 d .
H6A H 0.4548 0.4146 -0.0607 0.053 Uiso 1 1 calc R
H6B H 0.4077 0.4378 0.1971 0.053 Uiso 1 1 calc R
H6C H 0.4832 0.4919 0.0749 0.053 Uiso 1 1 calc R
C7 C -0.0185(6) 0.7110(5) 0.6100(15) 0.0229(13) Uani 1 1 d .
C8 C -0.0142(6) 0.7678(5) 0.8166(16) 0.0257(14) Uani 1 1 d .
H8A H -0.0468 0.8139 0.7670 0.039 Uiso 1 1 calc R
H8B H 0.0497 0.7801 0.8520 0.039 Uiso 1 1 calc R
H8C H -0.0427 0.7464 0.9660 0.039 Uiso 1 1 calc R
O1 O 0.0945(4) 0.5023(3) 0.3702(11) 0.0123(11) Uani 1 1 d .
O2 O 0.1115(4) 0.4858(3) -0.0336(11) 0.0143(12) Uani 1 1 d .
O1W O 0.3491(4) 0.6350(3) -0.5630(10) 0.0217(12) Uani 1 1 d D
O3 O 0.2446(4) 0.7179(3) -0.1048(10) 0.0211(11) Uani 1 1 d .
O4 O 0.1533(3) 0.6494(3) 0.1356(8) 0.0153(11) Uani 1 1 d .
O5 O 0.3311(3) 0.4751(3) -0.2999(19) 0.0269(10) Uani 1 1 d .
O6 O 0.3286(4) 0.5596(4) -0.0029(12) 0.0303(9) Uani 1 1 d .
O7 O -0.0606(4) 0.7296(3) 0.4095(10) 0.0254(13) Uani 1 1 d .
O8 O 0.0199(4) 0.6473(3) 0.6330(9) 0.0160(11) Uani 1 1 d .
Pb01 Pb 0.218102(18) 0.594183(14) -0.30057(9) 0.01884(11) Uani 1 1 d .
Pb02 Pb -0.001533(17) 0.598247(14) 0.20359(7) 0.01665(11) Uani 1 1 d .
H1W H 0.373(5) 0.6832(18) -0.606(11) 0.017 Uiso 1 1 d D
H2W H 0.347(6) 0.605(3) -0.711(6) 0.015 Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0043 0.0021 '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'
O O 0.0143 0.0079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -7.2391 10.5669 '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
O2 C1 O1 121.8(7) . .
O2 C1 C2 122.2(8) . .
O1 C1 C2 116.0(9) . .
O3 C3 O4 122.3(8) . .
O3 C3 C4 117.4(8) . .
O4 C3 C4 120.3(7) . .
O5 C5 O6 121.7(8) . .
O5 C5 C6 121.2(8) . .
O6 C5 C6 117.1(8) . .
O8 C7 O7 121.5(8) . .
O8 C7 C8 120.2(7) . .
O7 C7 C8 118.2(8) . .
C1 O1 Pb02 106.4(5) . .
C1 O2 Pb02 120.9(4) . 2_564
C3 O3 Pb01 99.7(5) . .
C3 O4 Pb02 142.3(5) . .
C3 O4 Pb01 87.4(5) . .
Pb02 O4 Pb01 108.57(17) . .
C5 O5 Pb01 86.8(5) . .
C5 O6 Pb01 100.5(5) . .
C7 O7 Pb02 88.4(5) . .
C7 O8 Pb02 99.4(5) . .
O6 Pb01 O3 80.2(2) . .
O6 Pb01 O1W 86.0(2) . .
O3 Pb01 O1W 82.17(19) . .
O6 Pb01 O5 51.0(2) . .
O3 Pb01 O5 126.85(19) . .
O1W Pb01 O5 75.5(2) . .
O6 Pb01 O4 75.32(19) . .
O3 Pb01 O4 50.56(17) . .
O1W Pb01 O4 131.04(16) . .
O5 Pb01 O4 119.9(2) . .
O1 Pb02 O4 76.83(17) . .
O1 Pb02 O8 79.83(18) . .
O4 Pb02 O8 83.91(16) . .
O1 Pb02 O2 75.93(16) . 2_565
O4 Pb02 O2 148.94(16) . 2_565
O8 Pb02 O2 76.87(17) . 2_565
O1 Pb02 O7 130.11(18) . .
O4 Pb02 O7 92.37(18) . .
O8 Pb02 O7 50.43(17) . .
O2 Pb02 O7 93.86(19) 2_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.237(13) .
C1 O1 1.283(11) .
C1 C2 1.498(11) .
C3 O3 1.259(10) .
C3 O4 1.271(10) .
C3 C4 1.488(13) .
C5 O5 1.221(12) .
C5 O6 1.278(10) .
C5 C6 1.502(11) .
C7 O8 1.262(10) .
C7 O7 1.283(10) .
C7 C8 1.495(12) .
O1 Pb02 2.376(6) .
O2 Pb02 2.604(6) 2_564
O1W Pb01 2.487(5) .
O3 Pb01 2.452(5) .
O4 Pb02 2.468(5) .
O4 Pb01 2.709(5) .
O5 Pb01 2.673(5) .
O6 Pb01 2.356(6) .
O7 Pb02 2.708(6) .
O8 Pb02 2.484(5) .
Pb02 O2 2.604(6) 2_565
