#------------------------------------------------------------------------------
#$Date: 2023-02-14 11:53:17 +0200 (Tue, 14 Feb 2023) $
#$Revision: 280882 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/67/8106777.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_8106777
loop_
_publ_author_name
'Zhang, Rong-Hua'
'Zhao, Dan'
'Ma, Fa-Xue'
_publ_section_title
;
 Crystal structure of
 poly[aqua-ethylenediamine-tetraacetatolead(II)zinc(II)]
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              35
_journal_page_last               36
_journal_paper_doi               10.1515/ncrs-2014-9086
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C10 H12 N2 O8 Pb Zn, H2 O'
_chemical_formula_sum            'C10 H14 N2 O9 Pb Zn'
_chemical_formula_weight         578.79
_chemical_name_systematic
;
catena-((μ5-Ethylenediamine-tetraacetato)-plumbum(ii)-zinc(ii) 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'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                101.6040(10)
_cell_angle_beta                 106.5400(10)
_cell_angle_gamma                98.9310(10)
_cell_formula_units_Z            2
_cell_length_a                   7.4992(6)
_cell_length_b                   8.2890(7)
_cell_length_c                   11.8236(10)
_cell_measurement_reflns_used    203
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.47
_cell_volume                     672.25(10)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'SMART APEX II (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker smart APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8308
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.296
_diffrn_reflns_theta_min         2.575
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    14.345
_exptl_absorpt_correction_T_max  0.514
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.859
_exptl_crystal_density_meas      .
_exptl_crystal_description       prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.947
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0177P)²+0.4967P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0442
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3138
_reflns_number_total             3290
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2014-9086_suppl.cif
_cod_data_source_block           a
_cod_database_code               8106777
_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_estimated_absorpt_t_min   0.162
_shelx_estimated_absorpt_t_max   0.534
_shelxl_version_number           2013-4
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
loop_
_space_group_symop_operation_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_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
Pb1 Pb -0.17742(2) 1.07232(2) 0.60183(2) 0.01840(5) Uani 1 1 d . . . . .
Zn1 Zn 0.09668(5) 0.65477(4) 0.65987(3) 0.01581(8) Uani 1 1 d . . . . .
C1 C 0.4241(5) 0.7591(4) 0.5827(3) 0.0184(6) Uani 1 1 d . . . . .
C2 C 0.5000(5) 0.6365(4) 0.6504(3) 0.0197(6) Uani 1 1 d . . . . .
H2A H 0.5059 0.5384 0.5922 0.024 Uiso 1 1 calc R U . . .
H2B H 0.6290 0.6891 0.7046 0.024 Uiso 1 1 calc R U . . .
C3 C 0.3420(5) 0.3952(4) 0.6999(3) 0.0175(6) Uani 1 1 d . . . . .
H3A H 0.2998 0.3638 0.7643 0.021 Uiso 1 1 calc R U . . .
H3B H 0.4579 0.3559 0.7017 0.021 Uiso 1 1 calc R U . . .
C4 C 0.1896(4) 0.3102(4) 0.5778(3) 0.0155(6) Uani 1 1 d . . . . .
C5 C 0.4786(4) 0.6659(4) 0.8538(3) 0.0183(6) Uani 1 1 d . . . . .
H5A H 0.5359 0.7831 0.8631 0.022 Uiso 1 1 calc R U . . .
H5B H 0.5795 0.6118 0.8879 0.022 Uiso 1 1 calc R U . . .
C6 C 0.3365(5) 0.6584(4) 0.9230(3) 0.0193(6) Uani 1 1 d . . . . .
H6A H 0.2891 0.5419 0.9214 0.023 Uiso 1 1 calc R U . . .
H6B H 0.3992 0.7216 1.0076 0.023 Uiso 1 1 calc R U . . .
C7 C 0.2177(5) 0.9157(4) 0.9056(3) 0.0219(7) Uani 1 1 d . . . . .
H7A H 0.3501 0.9604 0.9152 0.026 Uiso 1 1 calc R U . . .
H7B H 0.1996 0.9514 0.9841 0.026 Uiso 1 1 calc R U . . .
C8 C 0.0886(5) 0.9858(4) 0.8124(3) 0.0218(7) Uani 1 1 d . . . . .
C9 C -0.0975(4) 0.4824(4) 0.7959(3) 0.0204(7) Uani 1 1 d . . . . .
C10 C 0.0000(5) 0.6539(4) 0.8865(3) 0.0215(7) Uani 1 1 d . . . . .
H10A H -0.0875 0.7289 0.8783 0.026 Uiso 1 1 calc R U . . .
H10B H 0.0315 0.6403 0.9690 0.026 Uiso 1 1 calc R U . . .
O1 O 0.5134(4) 0.8145(3) 0.5190(2) 0.0263(5) Uani 1 1 d . . . . .
O2 O 0.2725(3) 0.8030(3) 0.5935(2) 0.0213(5) Uani 1 1 d . . . . .
O3 O 0.1281(3) 0.3983(3) 0.5085(2) 0.0210(5) Uani 1 1 d . . . . .
O4 O 0.1328(3) 0.1506(3) 0.5580(2) 0.0194(5) Uani 1 1 d . . . . .
O5 O -0.0602(3) 0.4511(3) 0.6967(2) 0.0231(5) Uani 1 1 d . . . . .
O6 O -0.2128(4) 0.3880(3) 0.8246(3) 0.0330(6) Uani 1 1 d . . . . .
O7 O -0.0121(4) 0.8795(3) 0.7108(2) 0.0252(5) Uani 1 1 d . . . . .
O8 O 0.0892(5) 1.1379(3) 0.8366(3) 0.0394(7) Uani 1 1 d . . . . .
O9 O -0.4051(6) 0.0657(4) 0.7786(3) 0.0578(10) Uani 1 1 d . . . . .
H9A H -0.3372 0.1816 0.7916 0.069 Uiso 1 1 d R U . . .
H9B H -0.5364 0.0739 0.7302 0.069 Uiso 1 1 d R U . . .
N1 N 0.3837(4) 0.5804(3) 0.7226(2) 0.0145(5) Uani 1 1 d . . . . .
N2 N 0.1748(4) 0.7305(3) 0.8665(2) 0.0159(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'
N N 0.0061 0.0033 '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'
Zn Zn 0.2839 1.4301 '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
O4 Pb1 O7 73.41(8) 2_566 .
O4 Pb1 O4 66.35(8) 2_566 1_565
O7 Pb1 O4 84.35(8) . 1_565
O4 Pb1 O2 78.54(7) 2_566 2_576
O7 Pb1 O2 150.16(8) . 2_576
O4 Pb1 O2 75.17(7) 1_565 2_576
O4 Pb1 O1 71.43(7) 2_566 1_455
O7 Pb1 O1 85.32(8) . 1_455
O4 Pb1 O1 137.76(7) 1_565 1_455
O2 Pb1 O1 95.34(7) 2_576 1_455
O2 Zn1 O5 164.05(10) . .
O2 Zn1 O3 89.95(9) . 2_566
O5 Zn1 O3 86.89(9) . 2_566
O2 Zn1 O7 86.83(9) . .
O5 Zn1 O7 108.42(10) . .
O3 Zn1 O7 84.88(9) 2_566 .
O2 Zn1 N2 113.73(10) . .
O5 Zn1 N2 76.59(9) . .
O3 Zn1 N2 145.04(9) 2_566 .
O7 Zn1 N2 71.88(9) . .
O2 Zn1 N1 76.23(9) . .
O5 Zn1 N1 95.14(9) . .
O3 Zn1 N1 135.24(9) 2_566 .
O7 Zn1 N1 135.15(9) . .
N2 Zn1 N1 77.56(9) . .
O1 C1 O2 123.1(3) . .
O1 C1 C2 118.2(3) . .
O2 C1 C2 118.7(3) . .
N1 C2 C1 113.4(3) . .
N1 C2 H2A 108.9 . .
C1 C2 H2A 108.9 . .
N1 C2 H2B 108.9 . .
C1 C2 H2B 108.9 . .
H2A C2 H2B 107.7 . .
N1 C3 C4 111.7(2) . .
N1 C3 H3A 109.3 . .
C4 C3 H3A 109.3 . .
N1 C3 H3B 109.3 . .
C4 C3 H3B 109.3 . .
H3A C3 H3B 107.9 . .
O3 C4 O4 126.2(3) . .
O3 C4 C3 119.0(3) . .
O4 C4 C3 114.8(3) . .
N1 C5 C6 110.8(3) . .
N1 C5 H5A 109.5 . .
C6 C5 H5A 109.5 . .
N1 C5 H5B 109.5 . .
C6 C5 H5B 109.5 . .
H5A C5 H5B 108.1 . .
N2 C6 C5 110.0(3) . .
N2 C6 H6A 109.7 . .
C5 C6 H6A 109.7 . .
N2 C6 H6B 109.7 . .
C5 C6 H6B 109.7 . .
H6A C6 H6B 108.2 . .
N2 C7 C8 110.7(3) . .
N2 C7 H7A 109.5 . .
C8 C7 H7A 109.5 . .
N2 C7 H7B 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 108.1 . .
O8 C8 O7 124.3(3) . .
O8 C8 C7 119.6(3) . .
O7 C8 C7 116.0(3) . .
O6 C9 O5 125.8(3) . .
O6 C9 C10 116.2(3) . .
O5 C9 C10 117.9(3) . .
N2 C10 C9 111.7(3) . .
N2 C10 H10A 109.3 . .
C9 C10 H10A 109.3 . .
N2 C10 H10B 109.3 . .
C9 C10 H10B 109.3 . .
H10A C10 H10B 107.9 . .
C1 O1 Pb1 125.6(2) . 1_655
C1 O2 Zn1 118.9(2) . .
C1 O2 Pb1 99.01(19) . 2_576
Zn1 O2 Pb1 128.99(10) . 2_576
C4 O3 Zn1 133.3(2) . 2_566
C4 O4 Pb1 126.42(19) . 2_566
C4 O4 Pb1 112.17(19) . 1_545
Pb1 O4 Pb1 113.65(8) 2_566 1_545
C9 O5 Zn1 116.4(2) . .
C8 O7 Zn1 116.1(2) . .
C8 O7 Pb1 99.83(19) . .
Zn1 O7 Pb1 136.40(11) . .
H9A O9 H9B 98.6 . .
C2 N1 C3 111.0(2) . .
C2 N1 C5 110.4(2) . .
C3 N1 C5 112.0(2) . .
C2 N1 Zn1 108.13(18) . .
C3 N1 Zn1 106.97(18) . .
C5 N1 Zn1 108.24(18) . .
C7 N2 C10 112.0(3) . .
C7 N2 C6 113.0(3) . .
C10 N2 C6 110.8(2) . .
C7 N2 Zn1 107.40(19) . .
C10 N2 Zn1 103.00(19) . .
C6 N2 Zn1 110.10(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O4 2.499(2) 2_566
Pb1 O7 2.507(2) .
Pb1 O4 2.541(2) 1_565
Pb1 O2 2.676(2) 2_576
Pb1 O1 2.689(3) 1_455
Zn1 O2 2.083(2) .
Zn1 O5 2.096(2) .
Zn1 O3 2.123(2) 2_566
Zn1 O7 2.190(2) .
Zn1 N2 2.272(3) .
Zn1 N1 2.291(3) .
C1 O1 1.248(4) .
C1 O2 1.278(4) .
C1 C2 1.498(4) .
C2 N1 1.470(4) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 N1 1.471(4) .
C3 C4 1.512(4) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 O3 1.244(4) .
C4 O4 1.276(4) .
C5 N1 1.480(4) .
C5 C6 1.518(4) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 N2 1.483(4) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 N2 1.466(4) .
C7 C8 1.522(5) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 O8 1.234(4) .
C8 O7 1.281(4) .
C9 O6 1.241(4) .
C9 O5 1.267(4) .
C9 C10 1.524(5) .
C10 N2 1.468(4) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
O1 Pb1 2.689(2) 1_655
O2 Pb1 2.676(2) 2_576
O3 Zn1 2.123(2) 2_566
O4 Pb1 2.499(2) 2_566
O4 Pb1 2.541(2) 1_545
O9 H9A 0.9748 .
O9 H9B 1.0088 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O6 0.97 1.73 2.700(4) 176.3 .
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{d4037911-febf-4a6c-bd92-ad823d93412d} y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{d4037911-febf-4a6c-bd92-ad823d93412d} '_publcif_info_datablock.publ_exptl'
{d4037911-febf-4a6c-bd92-ad823d93412d} '_geom_hbond_atom_site_label_D'
