#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/87/2018763.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2018763
loop_
_publ_author_name
'Lanza, Arianna'
'Gambirasi, Arianna'
'Favaro, Monica'
'Peruzzo, Luca'
'Chiurato, Matteo'
'Nestola, Fabrizio'
_publ_section_title
;
 Re-investigation of lead(II) formate
;
_journal_coeditor_code           SK3452
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              41
_journal_page_last               43
_journal_paper_doi               10.1107/S010827011204913X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Pb (H C O2)2]'
_chemical_formula_moiety         'C2 H2 O4 Pb'
_chemical_formula_sum            'C2 H2 O4 Pb'
_chemical_formula_weight         297.24
_chemical_name_common            'Lead(II) formate'
_chemical_name_systematic
;
Poly[di-μ₄-formato-lead(II)]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5227(8)
_cell_length_b                   7.4153(8)
_cell_length_c                   8.7646(10)
_cell_measurement_reflns_used    2211
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      43.14
_cell_measurement_theta_min      3.60
_cell_volume                     423.92(8)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2005)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2005)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2005)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement
;
WinGX (Farrugia, 1999) and SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
WinGX (Farrugia, 1999) and SUPERFLIP (Palatinus & Chapuis,
2007)
;
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Stoe STADI IV diffractometer equipped with an Oxford Sapphire I CCD area
detector
;
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3678
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    39.681
_exptl_absorpt_correction_T_max  0.0584
_exptl_absorpt_correction_T_min  0.0107
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'[XRED (Stoe & Cie, 1999) and XSHAPE (Stoe & Cie, 2001)]'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.944
_refine_ls_abs_structure_details 'Flack (1983), with 404 Bijvoet pairs'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0321P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0794
_reflns_number_gt                867
_reflns_number_total             1026
_reflns_threshold_expression     I>2σ(I)
_iucr_refine_instructions_details
;
TITL Pb formiato
CELL  0.71073   6.5227   7.4153   8.7646   90.000   90.000   90.000
ZERR     1.00   0.0008   0.0008   0.0010    0.000    0.000    0.000
LATT  -1
SYMM  1/2 - X, - Y, 1/2 + Z
SYMM  1/2 + X, 1/2 - Y, - Z
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    O    PB
UNIT  8    8    16   4
MERG   2
OMIT    -2.00  56.00
TWIN
eqiv $1 2-x, y+0.5, 1.5-z
bind Pb1 O2_$1
bind Pb1 O3_$1
FMAP   2
PLAN   10
ACTA
BOND   $H
temp 24
L.S.  10
WGHT    0.032100
BASF   0.03480
FVAR       0.37745
PB1   4    0.929187    0.259987    0.833752    11.00000    0.02675    0.02346 =
         0.02982   -0.00175   -0.00141    0.00093
C1    1    0.420747    0.109461    0.800139    11.00000    0.03004    0.02953 =
         0.00778    0.00116    0.00183    0.01047
AFIX  43
H1    2    0.495682    0.039148    0.732241    11.00000   -1.20000
AFIX   0
O1    3    0.519258    0.235298    0.862915    11.00000    0.02804    0.02765 =
         0.04406    0.01081    0.00004   -0.00142
O4    3    1.144495    0.425889    0.607727    11.00000    0.04328    0.02814 =
         0.03375   -0.01090    0.01818   -0.00396
O2    3    1.241605    0.066342    0.815340    11.00000    0.03082    0.02626 =
         0.06696    0.00396    0.01317    0.00396
C2    1    1.247261    0.348802    0.506635    11.00000    0.02806    0.03254 =
         0.02414    0.00072    0.00137    0.00293
AFIX  43
H2    2    1.243610    0.223427    0.506235    11.00000   -1.20000
AFIX   0
O3    3    0.852381    0.079324    0.592074    11.00000    0.02445    0.03197 =
         0.03254   -0.00055   -0.00654    0.00186
HKLF 4
REM  palmitato
REM R1 =  0.0354 for    867 Fo > 4sig(Fo)  and  0.0440 for all   1026 data
REM     65 parameters refined using      0 restraints
END
WGHT      0.0383      0.0000
REM Highest difference peak  1.297,  deepest hole -1.944,  1-sigma level  0.366
Q1    1   0.8241  0.2607  0.9039  11.00000  0.05    1.30
Q2    1   0.9300 -0.0968  0.5802  11.00000  0.05    1.26
Q3    1   0.8177  0.2607  0.7594  11.00000  0.05    1.23
Q4    1   1.0727  0.3975  0.7588  11.00000  0.05    1.23
Q5    1   0.4335  0.3240  0.9963  11.00000  0.05    1.18
Q6    1   0.7322  0.1404  0.9581  11.00000  0.05    1.17
Q7    1   1.0605  0.1075  0.9100  11.00000  0.05    1.04
Q8    1   1.0350  0.2567  0.9215  11.00000  0.05    1.02
Q9    1   1.0623  0.5244  0.7455  11.00000  0.05    1.01
Q10   1   0.9261  0.1205  0.9086  11.00000  0.05    1.00
;
_cod_data_source_file            sk3452.cif
_cod_data_source_block           I
_cod_database_code               2018763
_cod_database_fobs_code          2018763
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Pb Pb1 0.92919(8) 0.25999(6) 0.83375(7) 0.02668(16) Uani d . 1 1
O O1 0.5193(15) 0.2353(14) 0.8629(12) 0.033(2) Uani d . 1 1
O O2 1.2416(17) 0.0663(13) 0.8153(18) 0.041(3) Uani d . 1 1
O O3 0.8524(18) 0.0793(14) 0.5921(13) 0.030(2) Uani d . 1 1
O O4 1.144(2) 0.4259(13) 0.6077(13) 0.035(3) Uani d . 1 1
C C1 0.421(3) 0.1095(17) 0.8001(14) 0.022(3) Uani d . 1 1
C C2 1.247(2) 0.349(2) 0.5066(19) 0.028(3) Uani d . 1 1
H H1 0.4957 0.0391 0.7322 0.027 Uiso calc R 1 1
H H2 1.2436 0.2234 0.5062 0.034 Uiso calc R 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pb1 0.0267(2) 0.0235(2) 0.0298(3) 0.0009(3) -0.0014(2) -0.0018(3)
C1 0.030(7) 0.030(6) 0.008(6) 0.010(7) 0.002(6) 0.001(4)
O1 0.028(5) 0.028(5) 0.044(6) -0.001(5) 0.000(4) 0.011(6)
O4 0.043(7) 0.028(5) 0.034(6) -0.004(5) 0.018(5) -0.011(5)
O2 0.031(7) 0.026(5) 0.067(9) 0.004(4) 0.013(6) 0.004(6)
C2 0.028(7) 0.033(8) 0.024(8) 0.003(6) 0.001(6) 0.001(7)
O3 0.024(6) 0.032(5) 0.033(6) 0.002(4) -0.007(5) -0.001(5)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Pb1 O3 . . 78.8(4) y
O2 Pb1 O4 . 4_746 67.2(4) y
O3 Pb1 O4 . 4_746 67.9(4) y
O2 Pb1 O1 . . 141.0(3) y
O3 Pb1 O1 . . 81.3(3) y
O4 Pb1 O1 4_746 . 74.4(4) y
O2 Pb1 O4 . . 78.0(4) y
O3 Pb1 O4 . . 74.6(4) y
O4 Pb1 O4 4_746 . 132.5(3) y
O1 Pb1 O4 . . 127.7(4) y
O2 Pb1 O1 . 3_557 83.9(4) y
O3 Pb1 O1 . 3_557 149.1(3) y
O4 Pb1 O1 4_746 3_557 81.8(4) y
O1 Pb1 O1 . 3_557 97.0(3) y
O4 Pb1 O1 . 3_557 126.4(3) y
O2 Pb1 O3 . 4_756 94.9(3) y
O3 Pb1 O3 . 4_756 136.5(2) y
O4 Pb1 O3 4_746 4_756 148.3(4) y
O1 Pb1 O3 . 4_756 122.2(3) y
O4 Pb1 O3 . 4_756 62.0(3) y
O1 Pb1 O3 3_557 4_756 70.0(3) y
O2 Pb1 O2 . 4_756 138.42(19) y
O3 Pb1 O2 . 4_756 87.8(4) y
O4 Pb1 O2 4_746 4_756 141.8(4) y
O1 Pb1 O2 . 4_756 73.1(3) y
O4 Pb1 O2 . 4_756 60.5(4) y
O1 Pb1 O2 3_557 4_756 121.5(4) y
O3 Pb1 O2 4_756 4_756 68.7(3) y
O2 C1 O1 1_455 . 129.5(14) y
O2 C1 H1 1_455 . 115.3 n
O1 C1 H1 . . 115.3 n
C1 O1 Pb1 . . 121.0(10) n
C1 O1 Pb1 . 3_457 109.0(9) n
Pb1 O1 Pb1 . 3_457 107.8(3) n
C2 O4 Pb1 . 4_756 133.0(10) n
C2 O4 Pb1 . . 125.9(9) n
Pb1 O4 Pb1 4_756 . 101.2(3) n
C1 O2 Pb1 1_655 . 129.7(9) n
O3 C2 O4 3_556 . 127.0(14) y
O3 C2 H2 3_556 . 116.5 n
O4 C2 H2 . . 116.5 n
C2 O3 Pb1 3_456 . 117.8(10) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 O1 . 2.692(10) y
Pb1 O2 . 2.498(11) y
Pb1 O3 . 2.556(11) y
Pb1 O4 . 2.722(11) y
Pb1 O1 3_557 2.723(10) y
Pb1 O2 4_756 2.848(12) y
Pb1 O3 4_756 2.839(10) y
Pb1 O4 4_746 2.575(10) y
C1 O1 . 1.259(17) y
C1 O2 1_455 1.22(2) y
C1 H1 . 0.9300 n
C2 O3 3_556 1.226(19) y
C2 O4 . 1.249(19) y
C2 H2 . 0.9300 n
