#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/05/2220547.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_2220547
loop_
_publ_author_name
'Rafizadeh, Masoud'
'Manteghi, Faranak'
_publ_section_title
;Poly[ethylenediaminium
 [di-μ-aqua-(μ₆-benzene-1,2,4,5-tetracarboxylato-κ¹⁰O¹,O^1'^:O²,O^2'^:O^2'^:O⁴,O^4'^:O⁵:O⁵,O^5'^)dithallium(I)]]
;
_journal_coeditor_code           HY2169
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m17
_journal_page_last               m18
_journal_paper_doi               10.1107/S1600536808040282
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C2 H10 N2) [Tl2 (C10 H2 O8) (H2 O)2)]'
_chemical_formula_moiety         'C2 H10 N2 2+ , C10 H2 O8 Tl2 2- , 2H2 O'
_chemical_formula_sum            'C12 H16 N2 O10 Tl2'
_chemical_formula_weight         757.01
_chemical_name_systematic
;
Poly[ethylenediaminium [di-μ-aqua-(μ₆-benzene-1,2,4,5-tetracarboxylato-\
κ¹⁰O¹,O^1'^:O²,O^2'^:O^2'^:O⁴,O^4'^:O⁵:O⁵,O^5'^)dithallium(I)]]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.397(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.925(5)
_cell_length_b                   7.073(4)
_cell_length_c                   11.325(6)
_cell_measurement_reflns_used    1231
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.67
_cell_measurement_theta_min      3.38
_cell_volume                     786.5(7)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al.,  2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5272
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    20.525
_exptl_absorpt_correction_T_max  0.201
_exptl_absorpt_correction_T_min  0.064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.021
_refine_diff_density_min         -1.804
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.031P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                1487
_reflns_number_total             1787
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2169.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2220547
_cod_database_fobs_code          2220547
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_disorder_assembly
_atom_site_disorder_group
Tl Tl1 -0.05121(3) 0.10847(4) 0.68253(2) 0.01266(11) Uani d . 1 . .
O O1 0.1709(5) -0.1391(7) 0.8360(4) 0.0122(11) Uani d . 1 . .
O O2 0.1667(5) 0.1726(8) 0.8595(4) 0.0128(10) Uani d . 1 . .
O O3 0.6799(5) 0.2759(7) 0.7972(4) 0.0130(11) Uani d . 1 . .
O O4 0.8315(5) 0.0925(8) 0.9073(5) 0.0136(11) Uani d . 1 . .
C C1 0.2231(7) 0.0140(11) 0.8761(6) 0.0105(14) Uani d . 1 . .
C C2 0.3648(8) 0.0083(10) 0.9445(6) 0.0098(14) Uani d . 1 . .
C C3 0.4680(7) 0.0882(10) 0.8919(6) 0.0085(8) Uani d . 1 . .
H H1 0.4463 0.1491 0.8168 0.010 Uiso calc R 1 . .
C C4 0.6041(7) 0.0817(10) 0.9465(6) 0.0085(8) Uani d . 1 . .
C C5 0.7143(7) 0.1550(10) 0.8785(6) 0.0085(8) Uani d . 1 . .
C C6 0.5359(8) 0.0285(11) 0.5608(6) 0.0122(15) Uani d . 1 . .
H H2 0.4801 -0.0087 0.6226 0.015 Uiso calc R 1 . .
H H3 0.6244 -0.0381 0.5775 0.015 Uiso calc R 1 . .
N N1 0.5585(6) 0.2319(8) 0.5655(5) 0.0086(12) Uani d . 1 . .
H H4 0.6070 0.2664 0.5067 0.010 Uiso calc R 1 . .
H H5 0.6058 0.2636 0.6378 0.010 Uiso calc R 1 . .
H H6 0.4768 0.2927 0.5550 0.010 Uiso calc R 1 . .
O O1W 0.1899(5) 0.0253(8) 0.5778(5) 0.0167(12) Uani d . 1 . .
H H7 0.2389 -0.0717 0.5965 0.025 Uiso d R 1 . .
H H8 0.2341 0.1244 0.6018 0.025 Uiso d R 1 . .
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'
Tl Tl -2.8358 9.6688 '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
O3 Tl1 O2 2_546 . 114.26(16) ?
O3 Tl1 O1W 2_546 . 106.77(16) ?
O2 Tl1 O1W . . 73.92(15) ?
O3 Tl1 O4 2_546 1_455 69.06(15) ?
O2 Tl1 O4 . 1_455 75.31(15) ?
O1W Tl1 O4 . 1_455 143.40(15) ?
O3 Tl1 O1 2_546 . 76.67(15) ?
O2 Tl1 O1 . . 43.70(14) ?
O1W Tl1 O1 . . 63.61(15) ?
O4 Tl1 O1 1_455 . 80.47(14) ?
C1 O1 Tl1 . . 86.5(4) ?
C1 O2 Tl1 . . 104.3(4) ?
C5 O3 Tl1 . 2_556 127.4(4) ?
C5 O4 Tl1 . 1_655 103.4(4) ?
O2 C1 O1 . . 124.3(6) ?
O2 C1 C2 . . 117.7(7) ?
O1 C1 C2 . . 118.0(7) ?
C3 C2 C4 . 3_657 119.4(7) ?
C3 C2 C1 . . 117.7(6) ?
C4 C2 C1 3_657 . 122.8(6) ?
C2 C3 C4 . . 121.6(7) ?
C2 C3 H1 . . 119.2 ?
C4 C3 H1 . . 119.2 ?
C2 C4 C3 3_657 . 118.9(6) ?
C2 C4 C5 3_657 . 121.8(6) ?
C3 C4 C5 . . 119.0(6) ?
O4 C5 O3 . . 125.0(6) ?
O4 C5 C4 . . 117.5(6) ?
O3 C5 C4 . . 117.5(6) ?
N1 C6 C6 . 3_656 110.3(8) ?
N1 C6 H2 . . 109.6 ?
C6 C6 H2 3_656 . 109.6 ?
N1 C6 H3 . . 109.6 ?
C6 C6 H3 3_656 . 109.6 ?
H2 C6 H3 . . 108.1 ?
C6 N1 H4 . . 109.5 ?
C6 N1 H5 . . 109.5 ?
H4 N1 H5 . . 109.5 ?
C6 N1 H6 . . 109.5 ?
H4 N1 H6 . . 109.5 ?
H5 N1 H6 . . 109.5 ?
Tl1 O1W H7 . . 122.8 ?
Tl1 O1W H8 . . 96.9 ?
H7 O1W H8 . . 109.6 ?
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
Tl1 O3 2_546 2.702(5) y
Tl1 O2 . 2.763(5) y
Tl1 O1W . 2.882(5) y
Tl1 O4 1_455 2.952(5) y
Tl1 O1 . 3.135(5) y
Tl1 O1W 3_556 3.209(5) y
Tl1 O3 1_455 3.350(5) y
O1 C1 . 1.257(9) ?
O2 C1 . 1.256(9) ?
O3 C5 . 1.266(8) ?
O4 C5 . 1.242(9) ?
C1 C2 . 1.503(10) ?
C2 C3 . 1.378(10) ?
C2 C4 3_657 1.384(10) ?
C3 C4 . 1.402(10) ?
C3 H1 . 0.9500 ?
C4 C2 3_657 1.384(10) ?
C4 C5 . 1.518(10) ?
C6 N1 . 1.456(10) ?
C6 C6 3_656 1.510(14) ?
C6 H2 . 0.9900 ?
C6 H3 . 0.9900 ?
N1 H4 . 0.9100 ?
N1 H5 . 0.9100 ?
N1 H6 . 0.9100 ?
O1W H7 . 0.8500 ?
O1W H8 . 0.8500 ?
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
N1 H4 O2 4_665 0.91 1.900 2.791(8) 166 y
N1 H5 O3 1_555 0.91 1.850 2.741(8) 166 y
N1 H6 O1 2_556 0.91 2.105 2.828(8) 136 y
N1 H6 O4 4_565 0.91 2.199 2.942(8) 138 y
O1W H7 O2 2_546 0.85 2.064 2.909(8) 172 y
O1W H8 O1 2_556 0.85 1.997 2.846(8) 177 y
C3 H1 O1 2_556 0.95 2.4500 3.353(9) 159 y
C6 H3 O3 2_646 0.99 2.5900 3.523(9) 157 y
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_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O3 Tl1 O1 C1 2_546 . . . -155.0(4) ?
O2 Tl1 O1 C1 . . . . -5.8(4) ?
O1W Tl1 O1 C1 . . . . 88.3(4) ?
O4 Tl1 O1 C1 1_455 . . . -84.5(4) ?
O3 Tl1 O2 C1 2_546 . . . 39.1(4) ?
O1W Tl1 O2 C1 . . . . -62.4(4) ?
O4 Tl1 O2 C1 1_455 . . . 97.5(4) ?
O1 Tl1 O2 C1 . . . . 6.0(4) ?
Tl1 O2 C1 O1 . . . . -12.6(8) ?
Tl1 O2 C1 C2 . . . . 164.9(5) ?
Tl1 O1 C1 O2 . . . . 10.7(6) ?
Tl1 O1 C1 C2 . . . . -166.7(6) ?
O2 C1 C2 C3 . . . . -67.2(8) ?
O1 C1 C2 C3 . . . . 110.4(8) ?
O2 C1 C2 C4 . . . 3_657 116.3(8) ?
O1 C1 C2 C4 . . . 3_657 -66.1(9) ?
C4 C2 C3 C4 3_657 . . . -0.4(11) ?
C1 C2 C3 C4 . . . . -177.0(6) ?
C2 C3 C4 C2 . . . 3_657 0.4(11) ?
C2 C3 C4 C5 . . . . 174.0(6) ?
Tl1 O4 C5 O3 1_655 . . . -30.4(8) ?
Tl1 O4 C5 C4 1_655 . . . 150.1(5) ?
Tl1 O3 C5 O4 2_556 . . . -125.2(6) ?
Tl1 O3 C5 C4 2_556 . . . 54.4(8) ?
C2 C4 C5 O4 3_657 . . . 17.5(10) ?
C3 C4 C5 O4 . . . . -156.0(6) ?
C2 C4 C5 O3 3_657 . . . -162.1(7) ?
C3 C4 C5 O3 . . . . 24.5(10) ?
