#------------------------------------------------------------------------------
#$Date: 2021-02-24 12:16:16 +0200 (Wed, 24 Feb 2021) $
#$Revision: 262192 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/06/1560612.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_1560612
loop_
_publ_author_name
'Chen, Yong-Qiang'
'Tian, Yuan'
_publ_section_title
;
 Lead(II) coordination polymers based on rigid-flexible
 3,5-bis-oxyacetate-benzoic acid: Structural transition driven by
 temperature control
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              60
_journal_page_last               66
_journal_paper_doi               10.1016/j.jssc.2016.12.024
_journal_volume                  247
_journal_year                    2017
_chemical_formula_sum            'C22 H20 O20 Pb4'
_chemical_formula_weight         1433.14
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                100.02(3)
_cell_angle_beta                 102.77(3)
_cell_angle_gamma                97.23(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9756(18)
_cell_length_b                   11.556(2)
_cell_length_c                   15.721(3)
_cell_measurement_reflns_used    5416
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     1542.9(6)
_computing_cell_refinement       SMART
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  scx-mini
_diffrn_measurement_method       'ω scan'
_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  0.1178
_diffrn_reflns_av_sigmaI/netI    0.1637
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13345
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    21.844
_exptl_absorpt_correction_T_max  0.004
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.29
_refine_diff_density_max         3.924
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.343
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5416
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0567
_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)+(0.0000P)²+0.2300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                3505
_reflns_number_total             5416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2017-247-60.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        1542.9(5)
_cod_database_code               1560612
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.49562(8) -0.13997(6) 0.87642(5) 0.0247(2) Uani 1 1 d . . .
Pb2 Pb 0.17473(8) -0.38806(6) 0.79627(5) 0.0261(2) Uani 1 1 d . . .
Pb3 Pb 0.28588(8) -0.17968(6) 0.63954(5) 0.0267(2) Uani 1 1 d . . .
Pb4 Pb 0.09550(8) -0.06785(6) 0.83019(5) 0.0258(2) Uani 1 1 d . . .
O1W O 0.2472(11) -0.1943(9) 0.7785(8) 0.017(3) Uani 1 1 d . . .
O11 O 0.4018(13) 0.0681(10) 0.8604(9) 0.034(4) Uani 1 1 d . . .
O12 O 0.4989(12) -0.0035(10) 0.7462(9) 0.028(3) Uani 1 1 d . . .
O13 O 0.8257(13) 0.3971(11) 0.3629(9) 0.032(3) Uani 1 1 d U . .
O1 O 0.3421(14) -0.2730(10) 0.9514(9) 0.033(3) Uani 1 1 d . . .
O5 O -0.1398(13) 0.0198(11) 1.3135(9) 0.033(3) Uani 1 1 d . . .
O6 O -0.1332(15) -0.0729(11) 1.4219(11) 0.047(4) Uani 1 1 d . . .
O2 O 0.2889(14) -0.0936(10) 0.9869(9) 0.036(4) Uani 1 1 d . . .
O14 O 0.9164(15) 0.5871(11) 0.3842(10) 0.047(4) Uani 1 1 d . . .
O2W O -0.1380(16) -0.1695(14) 0.6993(11) 0.068(5) Uani 1 1 d . . .
O3W O 0.0140(17) -0.2172(11) 0.5265(11) 0.072(6) Uani 1 1 d . . .
O16 O 0.7145(14) 0.4149(10) 0.5059(10) 0.039(4) Uani 1 1 d . . .
O15 O 0.5114(12) 0.2030(10) 0.6915(9) 0.027(3) Uani 1 1 d U . .
O8 O 0.0390(15) -0.1139(11) 1.2440(10) 0.039(4) Uani 1 1 d . . .
O7 O 0.1070(13) -0.5140(10) 1.1441(9) 0.032(3) Uani 1 1 d . . .
O10 O 0.5555(13) 0.7349(11) 0.7180(9) 0.030(3) Uani 1 1 d U . .
O9 O 0.4630(12) 0.6333(10) 0.8076(9) 0.028(3) Uani 1 1 d . . .
O3 O 0.0087(14) -0.7331(10) 1.1504(10) 0.037(4) Uani 1 1 d . . .
O4 O 0.1757(13) -0.8044(11) 1.0789(10) 0.037(4) Uani 1 1 d . . .
C11 C -0.096(2) -0.0610(16) 1.3539(13) 0.023(5) Uani 1 1 d . . .
C2 C 0.2097(18) -0.2417(15) 1.0663(12) 0.020(4) Uani 1 1 d U . .
C1 C 0.2811(18) -0.2001(15) 0.9961(12) 0.016(3) Uani 1 1 d U . .
C7 C 0.1911(18) -0.3613(15) 1.0704(13) 0.022(4) Uani 1 1 d U . .
H7A H 0.2226 -0.4159 1.0301 0.027 Uiso 1 1 calc R . .
C15 C 0.5499(18) 0.3147(15) 0.6739(13) 0.023(3) Uani 1 1 d U . .
C20 C 0.452(2) 0.0777(16) 0.7917(14) 0.026(5) Uani 1 1 d U . .
C19 C 0.4579(19) 0.2028(15) 0.7698(12) 0.021(4) Uani 1 1 d U . .
H19A H 0.3553 0.2241 0.7609 0.025 Uiso 1 1 calc R . .
H19B H 0.5270 0.2611 0.8192 0.025 Uiso 1 1 calc R . .
C22 C 0.848(2) 0.5006(18) 0.4066(14) 0.031(5) Uani 1 1 d U . .
C3 C 0.1520(17) -0.1608(15) 1.1217(12) 0.018(4) Uani 1 1 d U . .
H3A H 0.1530 -0.0828 1.1138 0.022 Uiso 1 1 calc R . .
C21 C 0.7758(19) 0.5192(15) 0.4847(13) 0.022(5) Uani 1 1 d . . .
H21A H 0.8537 0.5656 0.5364 0.027 Uiso 1 1 calc R . .
H21B H 0.6939 0.5656 0.4717 0.027 Uiso 1 1 calc R . .
C16 C 0.6120(18) 0.3180(16) 0.6014(13) 0.023(4) Uani 1 1 d U . .
H16A H 0.6288 0.2469 0.5698 0.028 Uiso 1 1 calc R . .
C4 C 0.093(2) -0.1974(17) 1.1886(15) 0.033(5) Uani 1 1 d . . .
C17 C 0.6490(19) 0.4188(15) 0.5746(13) 0.023(5) Uani 1 1 d . . .
C5 C 0.0762(18) -0.3170(15) 1.1955(13) 0.024(5) Uani 1 1 d . . .
H5A H 0.0335 -0.3433 1.2390 0.029 Uiso 1 1 calc R . .
C6 C 0.1280(19) -0.3975(16) 1.1320(13) 0.025(4) Uani 1 1 d U . .
C10 C -0.009(2) -0.1497(16) 1.3185(13) 0.027(5) Uani 1 1 d . . .
H10A H 0.0812 -0.1541 1.3643 0.033 Uiso 1 1 calc R . .
H10B H -0.0739 -0.2278 1.2994 0.033 Uiso 1 1 calc R . .
C18 C 0.6165(17) 0.5254(16) 0.6227(12) 0.022(4) Uani 1 1 d U . .
H18A H 0.6370 0.5964 0.6039 0.026 Uiso 1 1 calc R . .
C14 C 0.5153(17) 0.4219(14) 0.7221(12) 0.019(3) Uani 1 1 d U . .
H14A H 0.4678 0.4214 0.7690 0.022 Uiso 1 1 calc R . .
C13 C 0.5575(18) 0.5267(14) 0.6940(12) 0.021(3) Uani 1 1 d DU . .
C8 C 0.1639(18) -0.6040(14) 1.0901(13) 0.022(4) Uani 1 1 d U . .
H8A H 0.2761 -0.5855 1.1030 0.026 Uiso 1 1 calc R . .
H8B H 0.1223 -0.6051 1.0274 0.026 Uiso 1 1 calc R . .
C12 C 0.5235(17) 0.6366(15) 0.7410(12) 0.019(4) Uani 1 1 d D . .
C9 C 0.117(2) -0.7217(15) 1.1090(14) 0.026(5) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1W Pb1 O1 75.3(4) . .
O1W Pb1 O9 73.4(4) . 1_545
O1 Pb1 O9 66.5(4) . 1_545
O1W Pb1 O11 75.6(4) . .
O1 Pb1 O11 116.1(4) . .
O9 Pb1 O11 146.8(4) 1_545 .
O1W Pb1 Pb2 39.1(2) . .
O1 Pb1 Pb2 45.6(3) . .
O9 Pb1 Pb2 44.2(2) 1_545 .
O11 Pb1 Pb2 111.6(2) . .
O1W Pb2 O3 73.0(4) . 2_547
O1W Pb2 O13 71.9(4) . 2_656
O3 Pb2 O13 114.4(4) 2_547 2_656
O1W Pb2 O9 75.2(3) . 1_545
O3 Pb2 O9 138.0(4) 2_547 1_545
O13 Pb2 O9 80.0(4) 2_656 1_545
O1W Pb2 O1 74.7(4) . .
O3 Pb2 O1 78.7(4) 2_547 .
O13 Pb2 O1 137.7(4) 2_656 .
O9 Pb2 O1 66.9(4) 1_545 .
O1W Pb2 Pb1 39.4(3) . .
O3 Pb2 Pb1 92.5(3) 2_547 .
O13 Pb2 Pb1 93.6(3) 2_656 .
O9 Pb2 Pb1 46.0(3) 1_545 .
O1 Pb2 Pb1 44.5(3) . .
O1W Pb3 O5 71.7(4) . 2_557
O1W Pb3 O13 70.5(4) . 2_656
O5 Pb3 O13 118.3(4) 2_557 2_656
O1W Pb3 O3W 108.1(5) . .
O5 Pb3 O3W 71.3(5) 2_557 .
O13 Pb3 O3W 76.4(4) 2_656 .
O1W Pb3 O12 78.1(4) . .
O5 Pb3 O12 74.6(4) 2_557 .
O13 Pb3 O12 138.3(4) 2_656 .
O3W Pb3 O12 140.9(4) . .
O1W Pb4 O3 74.0(4) . 2_547
O1W Pb4 O5 71.8(4) . 2_557
O3 Pb4 O5 125.2(4) 2_547 2_557
O1W Pb4 O2W 90.9(5) . .
O3 Pb4 O2W 69.3(5) 2_547 .
O5 Pb4 O2W 69.8(4) 2_557 .
Pb4 O1W Pb3 114.8(4) . .
Pb4 O1W Pb2 111.7(4) . .
Pb3 O1W Pb2 115.2(5) . .
Pb4 O1W Pb1 107.2(5) . .
Pb3 O1W Pb1 105.0(4) . .
Pb2 O1W Pb1 101.5(4) . .
C20 O11 Pb1 95.2(10) . .
C20 O12 Pb3 117.2(10) . .
C22 O13 Pb2 112.9(12) . 2_656
C22 O13 Pb3 143.1(12) . 2_656
Pb2 O13 Pb3 101.7(5) 2_656 2_656
C1 O1 Pb1 102.7(10) . .
C1 O1 Pb2 117.1(11) . .
Pb1 O1 Pb2 89.9(4) . .
C11 O5 Pb3 128.6(12) . 2_557
C11 O5 Pb4 130.1(11) . 2_557
Pb3 O5 Pb4 101.3(5) 2_557 2_557
C17 O16 C21 120.6(15) . .
C15 O15 C19 115.1(14) . .
C4 O8 C10 117.7(13) . .
C6 O7 C8 119.4(13) . .
C12 O9 Pb2 124.0(11) . 1_565
C12 O9 Pb1 101.1(9) . 1_565
Pb2 O9 Pb1 89.8(3) 1_565 1_565
C9 O3 Pb4 119.8(11) . 2_547
C9 O3 Pb2 138.1(11) . 2_547
Pb4 O3 Pb2 101.2(4) 2_547 2_547
O6 C11 O5 120.5(17) . .
O6 C11 C10 116.5(15) . .
O5 C11 C10 122.9(17) . .
C7 C2 C3 120.6(16) . .
C7 C2 C1 119.9(16) . .
C3 C2 C1 119.4(14) . .
O2 C1 O1 120.9(15) . .
O2 C1 C2 121.0(16) . .
O1 C1 C2 117.9(14) . .
C6 C7 C2 119.7(17) . .
C6 C7 H7A 120.2 . .
C2 C7 H7A 120.2 . .
C16 C15 O15 116.2(16) . .
C16 C15 C14 120.3(15) . .
O15 C15 C14 123.2(15) . .
O12 C20 O11 125.0(16) . .
O12 C20 C19 121.1(17) . .
O11 C20 C19 113.9(16) . .
O15 C19 C20 109.4(14) . .
O15 C19 H19A 109.8 . .
C20 C19 H19A 109.8 . .
O15 C19 H19B 109.8 . .
C20 C19 H19B 109.8 . .
H19A C19 H19B 108.2 . .
O14 C22 O13 122.5(19) . .
O14 C22 C21 120.9(18) . .
O13 C22 C21 116.4(16) . .
C4 C3 C2 119.4(16) . .
C4 C3 H3A 120.3 . .
C2 C3 H3A 120.3 . .
O16 C21 C22 114.4(16) . .
O16 C21 H21A 108.6 . .
C22 C21 H21A 108.6 . .
O16 C21 H21B 108.6 . .
C22 C21 H21B 108.6 . .
H21A C21 H21B 107.6 . .
C17 C16 C15 122.8(18) . .
C17 C16 H16A 118.6 . .
C15 C16 H16A 118.6 . .
C3 C4 O8 118.0(15) . .
C3 C4 C5 120.8(18) . .
O8 C4 C5 120.9(16) . .
O16 C17 C16 119.0(17) . .
O16 C17 C18 124.0(15) . .
C16 C17 C18 117.0(17) . .
C4 C5 C6 116.7(17) . .
C4 C5 H5A 121.7 . .
C6 C5 H5A 121.7 . .
C7 C6 O7 124.9(17) . .
C7 C6 C5 122.5(16) . .
O7 C6 C5 112.6(15) . .
O8 C10 C11 108.3(14) . .
O8 C10 H10A 110.0 . .
C11 C10 H10A 110.0 . .
O8 C10 H10B 110.0 . .
C11 C10 H10B 110.0 . .
H10A C10 H10B 108.4 . .
C13 C18 C17 122.3(16) . .
C13 C18 H18A 118.8 . .
C17 C18 H18A 118.8 . .
C13 C14 C15 115.9(15) . .
C13 C14 H14A 122.1 . .
C15 C14 H14A 122.1 . .
C18 C13 C14 121.5(16) . .
C18 C13 C12 121.1(15) . .
C14 C13 C12 117.2(15) . .
O7 C8 C9 109.8(14) . .
O7 C8 H8A 109.7 . .
C9 C8 H8A 109.7 . .
O7 C8 H8B 109.7 . .
C9 C8 H8B 109.7 . .
H8A C8 H8B 108.2 . .
O10 C12 O9 120.1(15) . .
O10 C12 C13 120.9(15) . .
O9 C12 C13 119.0(15) . .
O4 C9 O3 124.1(16) . .
O4 C9 C8 117.6(17) . .
O3 C9 C8 118.2(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1W 2.352(11) .
Pb1 O1 2.542(11) .
Pb1 O9 2.608(11) 1_545
Pb1 O11 2.680(11) .
Pb1 Pb2 3.6280(17) .
Pb2 O1W 2.333(10) .
Pb2 O3 2.482(12) 2_547
Pb2 O13 2.485(13) 2_656
Pb2 O9 2.531(11) 1_545
Pb2 O1 2.592(13) .
Pb3 O1W 2.317(11) .
Pb3 O5 2.498(11) 2_557
Pb3 O13 2.575(12) 2_656
Pb3 O3W 2.617(14) .
Pb3 O12 2.651(12) .
Pb4 O1W 2.287(10) .
Pb4 O3 2.467(12) 2_547
Pb4 O5 2.519(13) 2_557
Pb4 O2W 2.577(15) .
O11 C20 1.28(2) .
O12 C20 1.25(2) .
O13 C22 1.24(2) .
O13 Pb2 2.485(13) 2_656
O13 Pb3 2.575(12) 2_656
O1 C1 1.258(19) .
O5 C11 1.27(2) .
O5 Pb3 2.498(11) 2_557
O5 Pb4 2.519(13) 2_557
O6 C11 1.21(2) .
O2 C1 1.260(19) .
O14 C22 1.25(2) .
O16 C17 1.34(2) .
O16 C21 1.386(18) .
O15 C15 1.384(18) .
O15 C19 1.417(19) .
O8 C4 1.39(2) .
O8 C10 1.439(19) .
O7 C6 1.387(19) .
O7 C8 1.443(19) .
O10 C12 1.268(19) .
O9 C12 1.287(18) .
O9 Pb2 2.531(11) 1_565
O9 Pb1 2.608(11) 1_565
O3 C9 1.29(2) .
O3 Pb4 2.467(12) 2_547
O3 Pb2 2.482(12) 2_547
O4 C9 1.22(2) .
C11 C10 1.47(2) .
C2 C7 1.39(2) .
C2 C3 1.39(2) .
C2 C1 1.51(2) .
C7 C6 1.33(2) .
C7 H7A 0.9300 .
C15 C16 1.38(2) .
C15 C14 1.44(2) .
C20 C19 1.54(2) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C22 C21 1.51(2) .
C3 C4 1.38(2) .
C3 H3A 0.9300 .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C16 C17 1.33(2) .
C16 H16A 0.9300 .
C4 C5 1.40(2) .
C17 C18 1.43(2) .
C5 C6 1.44(2) .
C5 H5A 0.9300 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C18 C13 1.34(2) .
C18 H18A 0.9300 .
C14 C13 1.40(2) .
C14 H14A 0.9300 .
C13 C12 1.457(16) .
C8 C9 1.47(2) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
