#------------------------------------------------------------------------------
#$Date: 2019-06-15 07:15:48 +0300 (Sat, 15 Jun 2019) $
#$Revision: 216000 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021666.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_2021666
loop_
_publ_author_name
'Silverman, Joshua A.'
'Mathivathanan, Logesh'
'Govor, Evgen V.'
'Raptis, Raphael G.'
'Kavallieratos, Konstantinos'
_publ_section_title
;
Coordination polymers of Cd^II^ and Pb^II^ with croconate show remarkable
differences in coordination patterns: a structural and spectroscopic
study
;
_journal_coeditor_code YF3176
_journal_issue 7
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229619007277
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac '[Pb (C5 O5) (H2 O)2], H2 O'
_chemical_formula_moiety 'C5 H4 O7 Pb, H2 O'
_chemical_formula_sum 'C5 H6 O8 Pb'
_chemical_formula_weight 401.29
_chemical_name_systematic
'catena-Poly[[[diaqualead(II)]-\m-croconato-\k^4^O^1^,O^2^:O^3^,O^4^] monohydrate]'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens difmap
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 104.0550(10)
_cell_angle_beta 90.956(2)
_cell_angle_gamma 96.200(2)
_cell_formula_units_Z 2
_cell_length_a 6.4360(4)
_cell_length_b 7.9058(4)
_cell_length_c 8.3495(5)
_cell_measurement_reflns_used 6853
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 28.27
_cell_measurement_theta_min 3.19
_cell_volume 409.30(4)
_computing_cell_refinement
;
APEX2 (Bruker, 2015)
;
_computing_data_collection
;
SAINT (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009) and CrystalMaker (Palmer,
2014)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 296
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method '\f and \w shutterless scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0266
_diffrn_reflns_av_unetI/netI 0.0208
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 8040
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.267
_diffrn_reflns_theta_min 3.187
_exptl_absorpt_coefficient_mu 20.631
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.4153
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 3.256
_exptl_crystal_description needle
_exptl_crystal_F_000 364
_exptl_crystal_size_max 0.127
_exptl_crystal_size_mid 0.035
_exptl_crystal_size_min 0.033
_refine_diff_density_max 0.491
_refine_diff_density_min -1.366
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.219
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 144
_refine_ls_number_reflns 2026
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.218
_refine_ls_R_factor_all 0.0190
_refine_ls_R_factor_gt 0.0171
_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/[\s^2^(Fo^2^)+(0.0217P)^2^+0.0167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0416
_refine_ls_wR_factor_ref 0.0422
_reflns_number_gt 1928
_reflns_number_total 2026
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yf3176sup1.cif
_cod_data_source_block rgr545_a_pl
_cod_database_code 2021666
_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.
;
_shelx_hkl_file
;
-1 0 0 4097.99 131.99
-1 0 0 4891.21 131.49
-1 0 0 3907.81 132.49
-1 0 0 4723.93 131.39
1 0 0 4059.89 132.09
1 0 0 5038.70 131.49
1 0 0 5059.79 131.49
-2 0 0 1552.74 46.10
-2 0 0 1531.95 44.70
-2 0 0 1455.65 44.50
-2 0 0 1414.26 46.70
2 0 0 1541.55 44.60
2 0 0 1409.26 47.00
2 0 0 1506.65 44.60
-3 0 0 2143.59 65.69
-3 0 0 2107.39 63.89
-3 0 0 2276.57 66.79
-3 0 0 2059.09 63.69
3 0 0 1977.90 64.99
3 0 0 2071.99 63.59
3 0 0 2284.57 67.29
3 0 0 2075.69 65.69
3 0 0 2106.59 63.79
-4 0 0 318.07 13.50
-4 0 0 318.17 13.70
4 0 0 312.77 15.80
4 0 0 339.77 17.00
-5 0 0 1411.26 46.70
-5 0 0 1401.16 46.30
5 0 0 1434.96 49.00
5 0 0 1530.15 49.99
-6 0 0 1200.78 42.00
-6 0 0 1200.58 41.50
6 0 0 1269.67 44.60
6 0 0 1207.88 44.10
-7 0 0 293.27 18.70
-7 0 0 251.67 17.50
7 0 0 286.57 20.60
7 0 0 288.77 21.00
-8 0 0 44.40 10.90
-8 0 0 44.80 11.90
8 0 0 62.09 13.00
8 0 0 37.60 10.90
8 0 0 68.19 13.30
8 -1 0 308.47 22.90
8 -1 0 301.77 23.90
8 -1 0 301.57 23.40
-8 1 0 273.87 21.70
-8 1 0 263.47 20.90
7 -1 0 806.62 33.20
7 -1 0 713.33 33.30
7 -1 0 694.73 29.80
-7 1 0 721.53 28.80
-7 1 0 695.03 29.70
6 -1 0 979.30 38.50
6 -1 0 1003.30 38.60
-6 1 0 972.40 35.40
-6 1 0 980.90 34.40
5 -1 0 125.19 13.10
5 -1 0 115.49 14.60
-5 1 0 109.49 10.00
-5 1 0 121.39 9.80
4 -1 0 782.02 28.70
4 -1 0 763.32 29.10
-4 1 0 778.62 25.80
-4 1 0 777.22 26.60
3 -1 0 3989.70 122.69
3 -1 0 3876.51 122.89
3 -1 0 4365.16 121.09
3 -1 0 4103.89 121.59
-3 1 0 4021.40 122.29
-3 1 0 4348.67 121.19
-3 1 0 4172.58 121.69
-3 1 0 4182.18 123.59
2 -1 0 5397.16 151.88
2 -1 0 5292.77 151.28
2 -1 0 5088.69 152.18
-2 1 0 5134.29 152.08
-2 1 0 5264.77 151.38
-2 1 0 4978.60 151.98
-2 1 0 5340.57 151.88
1 -1 0 2813.62 82.69
1 -1 0 2801.82 82.39
1 -1 0 2899.91 82.79
1 -1 0 2863.41 82.39
-1 1 0 2861.01 82.79
-1 1 0 2737.63 82.29
-1 1 0 2826.12 82.79
-1 1 0 2966.40 82.79
-1 -1 0 202.48 7.60
-1 -1 0 201.58 7.50
-1 -1 0 194.98 7.00
1 1 0 203.98 7.60
1 1 0 207.18 7.50
1 1 0 205.68 7.60
1 1 0 204.98 7.50
1 1 0 197.38 7.00
-2 -1 0 2278.87 68.19
-2 -1 0 2367.16 69.29
-2 -1 0 2330.87 69.59
-2 -1 0 2324.37 68.69
2 1 0 2341.97 68.19
2 1 0 2362.56 68.59
2 1 0 2235.98 69.39
2 1 0 2265.97 69.29
2 1 0 2298.67 69.39
-3 -1 0 5661.53 162.68
-3 -1 0 5607.44 164.08
-3 -1 0 5629.44 162.38
3 1 0 5830.02 162.28
3 1 0 5048.49 164.48
3 1 0 5523.35 164.18
-4 -1 0 3445.96 98.79
-4 -1 0 3393.36 98.49
4 1 0 3324.27 100.59
4 1 0 2974.00 101.39
-5 -1 0 175.18 11.60
-5 -1 0 120.69 11.10
5 1 0 168.98 15.40
5 1 0 172.68 13.70
-6 -1 0 449.46 21.70
-6 -1 0 454.35 21.10
6 1 0 489.15 23.60
6 1 0 492.55 24.50
-7 -1 0 489.85 24.50
-7 -1 0 492.75 24.10
7 1 0 510.75 26.10
7 1 0 494.95 26.00
-8 -1 0 255.57 19.70
-8 -1 0 304.77 21.70
8 1 0 224.58 22.00
8 1 0 270.47 22.80
8 -2 0 262.77 24.60
8 -2 0 206.08 24.30
8 -2 0 258.47 21.40
-8 2 0 244.08 20.90
-8 2 0 283.77 20.50
7 -2 0 33.70 13.20
7 -2 0 46.80 12.50
7 -2 0 35.10 9.10
-7 2 0 24.70 9.10
-7 2 0 21.00 8.20
6 -2 0 235.08 19.00
6 -2 0 254.97 19.90
6 -2 0 247.38 14.60
-6 2 0 248.38 14.50
-6 2 0 240.68 15.50
5 -2 0 2552.84 81.59
5 -2 0 2589.24 78.19
5 -2 0 2557.54 81.29
-5 2 0 2579.64 78.29
-5 2 0 2597.44 79.39
4 -2 0 3149.28 94.89
4 -2 0 3256.07 97.29
4 -2 0 3265.67 96.89
-4 2 0 3190.78 95.99
-4 2 0 3130.09 94.89
3 -2 0 1846.42 63.19
3 -2 0 2212.88 62.49
3 -2 0 2130.09 62.39
3 -2 0 2070.19 63.49
3 -2 0 2076.19 63.79
-3 2 0 2175.88 62.49
-3 2 0 2179.78 63.59
-3 2 0 2122.79 63.59
2 -2 0 54.99 4.50
2 -2 0 52.39 3.30
2 -2 0 50.69 3.40
2 -2 0 49.40 4.10
2 -2 0 44.40 4.10
-2 2 0 48.50 4.20
-2 2 0 47.00 4.20
-2 2 0 50.09 4.30
1 -2 0 623.54 19.80
1 -2 0 631.64 19.00
1 -2 0 650.63 19.60
1 -2 0 621.74 19.90
-1 2 0 636.64 19.80
-1 2 0 647.04 19.60
-1 2 0 666.83 19.10
-1 2 0 619.04 19.80
0 -2 0 4148.98 130.89
0 -2 0 4737.03 131.49
0 -2 0 4564.14 131.49
0 2 0 4516.75 131.39
0 2 0 4597.24 131.39
0 2 0 4583.54 130.89
-1 -2 0 4610.44 131.49
-1 -2 0 4378.36 132.59
-1 -2 0 4566.54 132.59
-1 -2 0 4683.83 132.59
1 2 0 4449.45 131.49
1 2 0 4562.44 132.69
1 2 0 4481.45 132.59
1 2 0 4699.63 132.49
1 2 0 4459.75 132.49
-2 -2 0 4817.32 135.79
-2 -2 0 4818.82 135.89
-2 -2 0 4736.83 134.79
-2 -2 0 4248.38 135.79
2 2 0 4742.63 134.79
2 2 0 4538.55 135.59
2 2 0 4478.65 135.79
2 2 0 4733.83 135.69
2 2 0 4545.04 135.89
-3 -2 0 180.88 10.70
-3 -2 0 195.08 9.70
-3 -2 0 188.58 8.70
3 2 0 180.58 10.40
3 2 0 164.28 8.80
3 2 0 184.38 10.60
-4 -2 0 353.06 15.60
-4 -2 0 362.36 14.60
4 2 0 346.17 18.00
4 2 0 339.77 17.50
-5 -2 0 1504.75 46.70
-5 -2 0 1463.15 47.40
5 2 0 1486.25 49.50
5 2 0 1267.67 50.59
-6 -2 0 966.10 35.30
-6 -2 0 958.50 35.70
6 2 0 960.80 39.50
6 2 0 969.70 37.80
-7 -2 0 433.46 22.90
-7 -2 0 411.36 23.40
7 2 0 475.75 26.90
7 2 0 446.96 24.80
-8 -2 0 28.10 12.70
-8 -2 0 17.30 10.80
8 2 0 15.70 13.40
8 2 0 43.80 14.00
8 -3 0 164.78 16.40
8 -3 0 190.98 20.20
8 -3 0 177.08 20.30
-8 3 0 186.78 19.00
7 -3 0 627.64 34.60
7 -3 0 668.13 28.00
7 -3 0 682.93 32.10
-7 3 0 695.63 28.40
-7 3 0 671.33 28.50
6 -3 0 843.32 36.70
6 -3 0 872.61 31.10
6 -3 0 919.51 34.90
-6 3 0 874.31 31.10
-6 3 0 892.81 32.60
5 -3 0 853.21 31.30
5 -3 0 777.52 27.40
5 -3 0 834.02 29.80
-5 3 0 792.62 27.30
-5 3 0 788.02 29.00
4 -3 0 438.96 16.20
4 -3 0 440.56 16.10
4 -3 0 460.95 17.70
4 -3 0 483.65 18.70
-4 3 0 458.75 17.80
3 -3 0 597.04 18.50
3 -3 0 555.04 20.00
3 -3 0 571.94 18.50
3 -3 0 576.24 19.80
-3 3 0 571.54 19.80
2 -3 0 7849.11 228.88
2 -3 0 7899.71 228.68
2 -3 0 7929.51 227.68
2 -3 0 7891.21 229.08
2 -3 0 7997.80 227.68
-2 3 0 7795.82 228.88
-2 3 0 7920.01 227.68
-2 3 0 7480.75 228.48
-2 3 0 8171.08 228.88
1 -3 0 8446.66 241.68
1 -3 0 8218.28 240.48
1 -3 0 8023.00 240.68
1 -3 0 8213.78 241.58
-1 3 0 8593.04 241.58
-1 3 0 8793.92 240.48
-1 3 0 8664.03 241.68
-1 3 0 7733.33 240.68
0 -3 0 1181.08 35.80
0 -3 0 1189.58 36.50
0 -3 0 1180.88 36.50
0 3 0 1193.98 36.40
0 3 0 1199.78 36.40
0 3 0 1224.88 35.70
-1 -3 0 62.79 5.00
-1 -3 0 57.99 5.00
-1 -3 0 63.89 5.00
-1 -3 0 67.59 3.10
1 3 0 71.99 5.20
1 3 0 65.39 5.10
1 3 0 74.89 5.10
1 3 0 59.09 5.00
1 3 0 71.09 3.30
-2 -3 0 558.24 17.30
-2 -3 0 530.45 19.10
-2 -3 0 546.25 18.90
2 3 0 555.84 17.40
2 3 0 503.65 18.90
2 3 0 547.85 19.10
-3 -3 0 2310.57 68.09
-3 -3 0 2288.77 70.39
-3 -3 0 2264.37 69.49
3 3 0 2202.38 69.89
3 3 0 2294.77 70.39
3 3 0 2283.67 68.09
-4 -3 0 2333.87 73.29
-4 -3 0 2226.58 69.99
-4 -3 0 2299.57 71.49
4 3 0 2368.56 73.19
4 3 0 2306.87 73.09
-5 -3 0 767.62 27.80
-5 -3 0 782.22 29.20
5 3 0 785.22 33.00
5 3 0 749.73 31.20
-6 -3 0 8.60 7.80
-6 -3 0 21.80 8.50
6 3 0 23.30 12.50
6 3 0 2.30 9.20
-7 -3 0 62.89 12.70
-7 -3 0 60.59 10.70
7 3 0 56.09 12.80
7 3 0 67.49 15.00
8 -4 0 353.36 32.30
8 -4 0 359.36 29.30
-8 4 0 394.06 22.90
7 -4 0 183.38 23.70
7 -4 0 231.08 17.20
7 -4 0 232.38 21.80
-7 4 0 246.18 17.80
6 -4 0 22.00 10.70
6 -4 0 21.20 6.80
6 -4 0 26.30 8.90
-6 4 0 20.20 7.30
5 -4 0 566.74 24.00
5 -4 0 537.75 22.20
5 -4 0 559.94 20.20
-5 4 0 532.05 22.00
4 -4 0 2401.26 71.79
4 -4 0 2390.36 73.69
4 -4 0 2466.95 71.99
4 -4 0 2379.66 74.29
-4 4 0 2424.46 73.69
3 -4 0 4687.13 142.59
3 -4 0 5000.50 140.59
3 -4 0 4774.72 142.29
3 -4 0 4929.01 140.59
-3 4 0 4763.12 141.89
2 -4 0 1165.48 37.40
2 -4 0 1190.08 36.50
2 -4 0 1159.58 37.20
2 -4 0 1180.28 35.50
-2 4 0 1245.18 35.50
-2 4 0 1189.78 36.40
1 -4 0 2.90 2.60
1 -4 0 0.60 2.40
1 -4 0 3.00 1.80
1 -4 0 4.20 2.10
-1 4 0 3.30 1.90
-1 4 0 1.90 2.90
-1 4 0 -0.10 1.90
0 -4 0 1344.57 41.70
0 -4 0 1356.96 40.80
0 -4 0 1330.27 41.70
0 4 0 1360.36 40.50
-1 -4 0 2124.79 64.39
-1 -4 0 2121.89 63.89
-1 -4 0 2136.39 64.39
1 4 0 2157.18 64.39
1 4 0 2074.79 63.59
-2 -4 0 4661.93 135.09
-2 -4 0 4601.54 132.79
-2 -4 0 4534.55 135.49
2 4 0 4594.74 132.89
2 4 0 4463.65 135.39
-3 -4 0 1734.63 53.39
-3 -4 0 1681.43 53.79
-3 -4 0 1586.84 50.79
3 4 0 1733.83 51.19
3 4 0 1672.93 53.59
-4 -4 0 9.80 7.10
-4 -4 0 7.00 5.90
-4 -4 0 17.30 5.10
4 4 0 20.80 7.00
4 4 0 1.60 6.80
-5 -4 0 614.54 23.60
-5 -4 0 618.64 25.50
-5 -4 0 608.84 27.90
5 4 0 590.84 27.80
5 4 0 597.84 27.90
-6 -4 0 568.34 25.50
-6 -4 0 589.04 27.00
6 4 0 608.34 33.20
6 4 0 589.14 29.70
-7 -4 0 359.76 24.00
-7 -4 0 404.76 24.40
7 4 0 358.26 27.10
7 4 0 352.56 30.60
7 -5 0 443.26 26.60
7 -5 0 492.55 29.70
-7 5 0 396.36 23.30
6 -5 0 1108.29 40.50
6 -5 0 1085.69 37.70
6 -5 0 1172.08 43.70
-6 5 0 1150.78 39.90
5 -5 0 949.40 31.60
5 -5 0 991.00 35.60
5 -5 0 956.50 34.00
-5 5 0 962.00 33.90
4 -5 0 406.06 16.90
4 -5 0 392.16 17.70
4 -5 0 366.96 14.50
4 -5 0 389.96 14.30
-4 5 0 409.46 16.80
3 -5 0 24.60 5.30
3 -5 0 31.80 3.60
3 -5 0 26.60 5.20
3 -5 0 29.10 3.20
-3 5 0 22.10 4.30
2 -5 0 587.84 20.90
2 -5 0 578.04 21.20
2 -5 0 595.84 18.80
2 -5 0 592.14 19.60
-2 5 0 603.44 19.40
-2 5 0 588.74 18.60
1 -5 0 3440.56 101.19
1 -5 0 3418.86 99.39
1 -5 0 3319.57 101.09
-1 5 0 3271.07 98.49
-1 5 0 3509.95 99.09
0 -5 0 4795.12 143.39
0 -5 0 4839.62 142.29
0 -5 0 4815.72 143.39
0 5 0 4988.50 141.79
-1 -5 0 1583.04 48.80
-1 -5 0 1597.94 49.70
-1 -5 0 1553.54 49.60
1 5 0 1577.14 49.70
-2 -5 0 -0.50 4.60
-2 -5 0 6.30 4.60
2 5 0 6.50 4.60
2 5 0 7.50 2.30
-3 -5 0 923.01 32.20
-3 -5 0 928.11 28.90
-3 -5 0 948.81 33.10
3 5 0 912.71 32.80
3 5 0 898.11 29.40
-4 -5 0 1168.98 38.70
-4 -5 0 1166.38 41.60
-4 -5 0 1244.18 43.10
4 5 0 1205.48 42.70
4 5 0 1232.68 43.10
-5 -5 0 887.51 36.10
-5 -5 0 822.52 31.20
-5 -5 0 848.82 33.80
5 5 0 858.41 35.70
5 5 0 935.41 36.30
-6 -5 0 268.77 20.50
-6 -5 0 224.08 19.20
6 5 0 221.88 24.60
6 5 0 237.08 23.00
7 -6 0 626.34 31.00
7 -6 0 632.34 34.10
-7 6 0 619.24 28.70
6 -6 0 522.95 24.90
6 -6 0 541.15 27.50
-6 6 0 508.35 24.50
5 -6 0 39.80 8.00
5 -6 0 50.59 10.20
-5 6 0 40.30 8.00
4 -6 0 1213.38 39.90
4 -6 0 1185.58 40.50
4 -6 0 1138.79 36.40
-4 6 0 1174.28 38.70
3 -6 0 2785.42 83.69
3 -6 0 2754.12 83.29
3 -6 0 2512.95 80.19
3 -6 0 2775.62 80.29
-3 6 0 2796.32 81.59
2 -6 0 1645.54 49.30
2 -6 0 1622.94 51.99
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_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 95071
_shelx_res_file
;
TITL RGR545_a.res in P-1 New: P-1
rgr545_a_pl.res
created by SHELXL-2018/3 at 16:47:22 on 23-Mar-2019
CELL 0.71073 6.436 7.9058 8.3495 104.055 90.956 96.2
ZERR 2 0.0004 0.0004 0.0005 0.001 0.002 0.002
LATT 1
SFAC C H O Pb
UNIT 10 12 16 2
EQIV $1 1-X,1-Y,-Z
EQIV $2 1-X,1-Y,1-Z
EQIV $3 +X,1+Y,1+Z
EQIV $4 -X,1-Y,1-Z
EQIV $5 -X,1-Y,-Z
EQIV $6 -1+X,+Y,+Z
DFIX 0.878 O7 H7a
DFIX 0.878 O7 H7b
DFIX 0.878 H8b O8
DFIX 0.878 H8a O8
L.S. 10
PLAN -5
TEMP 0
HTAB O6 O3_$1
HTAB O6 O5_$2
HTAB O7 O3_$3
HTAB O7 O8_$4
HTAB O8 O2_$5
HTAB O8 O6_$6
BOND $H
HTAB
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.021700 0.016700
FVAR 0.62645
PB1 4 0.099120 0.709683 0.350629 11.00000 0.02980 0.01489 =
0.02673 0.00310 0.00083 0.00468
O1 3 0.180484 0.430071 0.422009 11.00000 0.04354 0.01580 =
0.01560 0.00299 0.00416 0.00594
O2 3 0.208913 0.471731 0.092961 11.00000 0.04448 0.01658 =
0.02032 0.00771 0.00312 0.00496
O3 3 0.247160 0.121728 -0.131833 11.00000 0.05361 0.02464 =
0.01343 -0.00052 0.00827 -0.00082
O4 3 0.239115 -0.131088 0.078923 11.00000 0.05833 0.01709 =
0.02945 0.00133 0.00214 0.01059
O5 3 0.203177 0.062598 0.419519 11.00000 0.04564 0.01633 =
0.01995 0.00878 0.00038 0.00177
O6 3 0.488344 0.738892 0.335292 11.00000 0.02765 0.03181 =
0.01903 0.00600 0.00199 0.00296
AFIX 7
H6A 2 0.548854 0.801583 0.429182 11.00000 -1.50000
H6B 2 0.528764 0.800381 0.264501 11.00000 -1.50000
AFIX 0
O7 3 0.273104 0.803034 0.638241 11.00000 0.04265 0.01985 =
0.02333 0.00424 0.00063 0.00431
O8 3 -0.257569 0.467831 0.218092 11.00000 0.04312 0.03212 =
0.01920 0.00719 0.00347 0.01213
C1 1 0.205434 0.309145 0.298300 11.00000 0.02067 0.01475 =
0.01566 0.00298 0.00122 0.00278
C2 1 0.219462 0.329515 0.130805 11.00000 0.02323 0.01473 =
0.01531 0.00394 0.00181 0.00135
C3 1 0.237011 0.158225 0.020387 11.00000 0.02532 0.02073 =
0.01874 0.00471 0.00328 0.00426
C4 1 0.235219 0.028684 0.125493 11.00000 0.02384 0.01533 =
0.01917 0.00158 0.00098 0.00580
C5 1 0.214326 0.127394 0.296393 11.00000 0.02175 0.01478 =
0.01744 0.00332 0.00085 0.00194
H7A 2 0.248047 0.902421 0.705747 11.00000 0.06021
H7B 2 0.273790 0.720509 0.691734 11.00000 0.04280
H8A 2 -0.350603 0.537337 0.253875 11.00000 0.04631
H8B 2 -0.270349 0.467477 0.115953 11.00000 0.07235
HKLF 4
REM RGR545_a.res in P-1 New: P-1
REM wR2 = 0.0422, GooF = S = 1.219, Restrained GooF = 1.218 for all data
REM R1 = 0.0171 for 1928 Fo > 4sig(Fo) and 0.0190 for all 2026 data
REM 144 parameters refined using 4 restraints
END
WGHT 0.0217 0.0167
REM Instructions for potential hydrogen bonds
HTAB O6 O5_$2
HTAB O6 O3_$1
EQIV $8 x, y+1, z
HTAB O6 O4_$8
HTAB O7 O3_$3
HTAB O7 O8_$4
HTAB O8 O6_$6
HTAB O8 O2_$5
REM Highest difference peak 0.491, deepest hole -1.366, 1-sigma level 0.201
Q1 1 -0.2370 0.8556 0.2945 11.00000 0.05 0.49
Q2 1 0.4628 0.6422 0.6808 11.00000 0.05 0.49
Q3 1 -0.0722 0.4096 0.2188 11.00000 0.05 0.49
Q4 1 0.3467 0.1064 0.6198 11.00000 0.05 0.47
Q5 1 0.2715 0.8635 0.3609 11.00000 0.05 0.47
;
_shelx_res_checksum 93808
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_occupancy
Pb Pb1 0.09912(2) 0.70968(2) 0.35063(2) 0.02400(6) Uani d 1
O O1 0.1805(4) 0.4301(3) 0.4220(3) 0.0249(5) Uani d 1
O O2 0.2089(4) 0.4717(3) 0.0930(3) 0.0265(5) Uani d 1
O O3 0.2472(5) 0.1217(3) -0.1318(3) 0.0318(6) Uani d 1
O O4 0.2391(5) -0.1311(3) 0.0789(3) 0.0352(6) Uani d 1
O O5 0.2032(4) 0.0626(3) 0.4195(3) 0.0267(5) Uani d 1
O O6 0.4883(4) 0.7389(3) 0.3353(3) 0.0262(5) Uani d 1
H H6A 0.548854 0.801583 0.429182 0.039 Uiso d 1
H H6B 0.528764 0.800381 0.264501 0.039 Uiso d 1
O O7 0.2731(4) 0.8030(3) 0.6382(3) 0.0288(5) Uani d 1
O O8 -0.2576(5) 0.4678(4) 0.2181(3) 0.0307(6) Uani d 1
C C1 0.2054(5) 0.3091(4) 0.2983(4) 0.0171(6) Uani d 1
C C2 0.2195(5) 0.3295(4) 0.1308(4) 0.0178(6) Uani d 1
C C3 0.2370(5) 0.1582(4) 0.0204(4) 0.0215(7) Uani d 1
C C4 0.2352(5) 0.0287(4) 0.1255(4) 0.0196(6) Uani d 1
C C5 0.2143(5) 0.1274(4) 0.2964(4) 0.0181(6) Uani d 1
H H7A 0.248(9) 0.902(5) 0.706(6) 0.060(16) Uiso d 1
H H7B 0.274(7) 0.721(5) 0.692(5) 0.043(13) Uiso d 1
H H8A -0.351(6) 0.537(6) 0.254(6) 0.046(15) Uiso d 1
H H8B -0.270(9) 0.467(8) 0.116(3) 0.072(19) Uiso d 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 0.02980(8) 0.01489(8) 0.02673(8) 0.00468(5) 0.00083(5) 0.00310(5)
O1 0.0435(15) 0.0158(11) 0.0156(11) 0.0059(10) 0.0042(10) 0.0030(9)
O2 0.0445(15) 0.0166(12) 0.0203(12) 0.0050(10) 0.0031(11) 0.0077(9)
O3 0.0536(17) 0.0246(13) 0.0134(11) -0.0008(12) 0.0083(11) -0.0005(10)
O4 0.0583(19) 0.0171(13) 0.0294(14) 0.0106(12) 0.0021(13) 0.0013(10)
O5 0.0456(16) 0.0163(12) 0.0200(12) 0.0018(10) 0.0004(10) 0.0088(9)
O6 0.0277(13) 0.0318(14) 0.0190(12) 0.0030(10) 0.0020(9) 0.0060(10)
O7 0.0427(15) 0.0198(13) 0.0233(13) 0.0043(11) 0.0006(11) 0.0042(10)
O8 0.0431(16) 0.0321(15) 0.0192(13) 0.0121(12) 0.0035(11) 0.0072(11)
C1 0.0207(15) 0.0147(15) 0.0157(14) 0.0028(11) 0.0012(11) 0.0030(11)
C2 0.0232(15) 0.0147(15) 0.0153(14) 0.0014(11) 0.0018(11) 0.0039(11)
C3 0.0253(16) 0.0207(17) 0.0187(15) 0.0043(13) 0.0033(12) 0.0047(13)
C4 0.0238(16) 0.0153(15) 0.0192(15) 0.0058(12) 0.0010(12) 0.0016(12)
C5 0.0218(15) 0.0148(14) 0.0174(15) 0.0019(11) 0.0009(12) 0.0033(12)
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_3
_geom_angle
_geom_angle_publ_flag
O1 Pb1 O2 . 66.73(7) y
O1 Pb1 O5 1_565 144.36(8) y
O1 Pb1 O7 . 74.06(8) y
O2 Pb1 O5 1_565 127.18(7) y
O6 Pb1 O1 . 79.20(8) y
O6 Pb1 O2 . 70.11(8) y
O6 Pb1 O5 1_565 77.15(8) y
O6 Pb1 O7 . 69.40(8) y
O7 Pb1 O2 . 127.50(9) y
O7 Pb1 O5 1_565 72.84(8) y
C1 O1 Pb1 . 113.6(2) ?
C2 O2 Pb1 . 110.12(19) ?
C5 O5 Pb1 1_545 115.4(2) ?
Pb1 O6 H6A . 111.0 ?
Pb1 O6 H6B . 110.7 ?
H6A O6 H6B . 103.2 ?
Pb1 O7 H7A . 120(4) ?
Pb1 O7 H7B . 116(3) ?
H7A O7 H7B . 110(5) ?
H8A O8 H8B . 98(5) ?
O1 C1 C2 . 124.7(3) ?
O1 C1 C5 . 126.3(3) ?
C5 C1 C2 . 108.9(3) ?
O2 C2 C1 . 123.6(3) ?
O2 C2 C3 . 127.8(3) ?
C1 C2 C3 . 108.6(3) ?
O3 C3 C2 . 127.7(3) ?
O3 C3 C4 . 125.2(3) ?
C2 C3 C4 . 107.1(3) ?
O4 C4 C3 . 127.5(3) ?
O4 C4 C5 . 125.7(3) ?
C5 C4 C3 . 106.7(3) ?
O5 C5 C1 . 126.0(3) ?
O5 C5 C4 . 125.2(3) ?
C1 C5 C4 . 108.7(3) ?
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 . 2.529(2) y
Pb1 O2 . 2.653(2) y
Pb1 O5 1_565 2.714(2) y
Pb1 O6 . 2.499(2) y
Pb1 O7 . 2.537(3) y
O1 C1 . 1.251(4) ?
O2 C2 . 1.248(4) ?
O3 C3 . 1.238(4) ?
O4 C4 . 1.231(4) ?
O5 C5 . 1.255(4) ?
O6 H6A . 0.8782 ?
O6 H6B . 0.8779 ?
O7 H7A . 0.88(2) ?
O7 H7B . 0.876(19) ?
O8 H8A . 0.864(19) ?
O8 H8B . 0.85(2) ?
C1 C2 . 1.449(4) ?
C1 C5 . 1.440(4) ?
C2 C3 . 1.458(4) ?
C3 C4 . 1.501(5) ?
C4 C5 . 1.467(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O6 H6A O5 2_666 0.88 2.05 2.868(4) 154.8 yes
O6 H6B O3 2_665 0.88 1.97 2.757(3) 148.5 yes
O7 H7A O3 1_566 0.88(2) 1.92(2) 2.795(4) 169(5) yes
O7 H7B O8 2_566 0.876(19) 1.82(2) 2.691(4) 173(5) yes
O8 H8A O6 1_455 0.864(19) 1.98(2) 2.831(4) 167(5) yes
O8 H8B O2 2_565 0.85(2) 1.95(3) 2.769(4) 159(6) yes
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_site_symmetry_1
_geom_torsion
Pb1 O1 C1 C2 . 9.0(4)
Pb1 O1 C1 C5 . -167.6(3)
Pb1 O2 C2 C1 . -8.9(4)
Pb1 O2 C2 C3 . 168.0(3)
Pb1 O5 C5 C1 1_545 160.7(2)
Pb1 O5 C5 C4 1_545 -18.3(4)
O1 C1 C2 O2 . 0.4(5)
O1 C1 C2 C3 . -177.0(3)
O1 C1 C5 O5 . -1.7(6)
O1 C1 C5 C4 . 177.3(3)
O2 C2 C3 O3 . 0.9(6)
O2 C2 C3 C4 . -177.7(3)
O3 C3 C4 O4 . -1.6(6)
O3 C3 C4 C5 . -178.0(3)
O4 C4 C5 O5 . 2.0(6)
O4 C4 C5 C1 . -177.0(3)
C1 C2 C3 O3 . 178.1(3)
C1 C2 C3 C4 . -0.4(4)
C2 C1 C5 O5 . -178.8(3)
C2 C1 C5 C4 . 0.2(4)
C2 C3 C4 O4 . 177.0(3)
C2 C3 C4 C5 . 0.6(4)
C3 C4 C5 O5 . 178.6(3)
C3 C4 C5 C1 . -0.5(4)
C5 C1 C2 O2 . 177.5(3)
C5 C1 C2 C3 . 0.1(4)
_cod_database_fobs_code 2021666