#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/60/2216082.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_2216082
loop_
_publ_author_name
'Aghabozorg, Hossein'
'Attar Gharamaleki, Jafar'
'Motyeian, Elham'
'Ghadermazi, Mohammad'
_publ_section_title
;
 Poly[propane-1,3-diammonium
 [diaqua(μ₄-4-benzene-1,2,4,5-tetracarboxylato)cobaltate(II)]
 hemihydrate]
;
_journal_coeditor_code           OM2167
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2793
_journal_page_last               m2794
_journal_paper_doi               10.1107/S1600536807050659
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'(C3 H12 N2) [Co (C10 H2 O8) (H2 O1)2], 0.5H2 O'
_chemical_formula_moiety         'C3 H12 N2 2+, C10 H6 Co O10 -, 0.5(H2 O)'
_chemical_formula_sum            'C13 H19 Co N2 O10.5'
_chemical_formula_weight         430.23
_chemical_name_systematic
;
Poly[propane-1,3-diammonium
[diaqua(μ₄-4-benzene-1,2,4,5-tetracarboxylato)cobaltate(II)]
hemihydrate]
;
_space_group_IT_number           46
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2a'
_symmetry_space_group_name_H-M   'I m a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4011(3)
_cell_length_b                   7.17860(10)
_cell_length_c                   14.2586(2)
_cell_measurement_reflns_used    6735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      46.73
_cell_measurement_theta_min      2.48
_cell_volume                     1678.76(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL Bruker, 2005)'
_computing_publication_material  'SHELXTL Bruker, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19141
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.345
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.375(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2526
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.05P)²+P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                2479
_reflns_number_total             2526
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om2167.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C13 H19 Co1 N2 O10.5'
_cod_database_code               2216082
_cod_database_fobs_code          2216082
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y, z'
'-x+1/2, y, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'
'-x+1, 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
Co Co1 0.5000 0.5000 0.82749(2) 0.00585(4) Uani d S 1
O O1 0.59187(6) 0.93889(14) 1.23336(6) 0.01174(18) Uani d . 1
O O2 0.54019(5) 0.69011(13) 1.15830(6) 0.01297(17) Uani d . 1
O O3 0.56026(5) 0.86184(13) 0.96344(7) 0.01294(16) Uani d . 1
O O4 0.58410(6) 0.55896(14) 0.93363(6) 0.01095(17) Uani d . 1
C C1 0.7500 0.8092(3) 1.17061(12) 0.0095(3) Uani d S 1
H H1A 0.7500 0.8483 1.2343 0.011 Uiso calc SR 1
C C2 0.67589(7) 0.78092(16) 1.12452(9) 0.0090(2) Uani d . 1
C C3 0.67626(7) 0.72442(17) 1.03074(8) 0.0083(2) Uani d . 1
C C4 0.7500 0.6944(2) 0.98435(12) 0.0095(3) Uani d S 1
H H4A 0.7500 0.6535 0.9210 0.011 Uiso calc SR 1
C C5 0.59580(7) 0.80529(17) 1.17606(8) 0.0093(2) Uani d . 1
C C6 0.59980(7) 0.71361(17) 0.97228(8) 0.0090(2) Uani d . 1
O O5 0.45721(5) 0.77721(11) 0.82396(8) 0.01252(15) Uani d . 1
H H5B 0.4770 0.8192 0.8781 0.015 Uiso d R 1
H H5A 0.4806 0.8255 0.7732 0.015 Uiso d R 1
N N1 0.40163(6) 0.73402(16) 0.54638(8) 0.0136(2) Uani d . 1
H H1B 0.4460 0.7422 0.5844 0.020 Uiso calc R 1
H H1C 0.4044 0.8241 0.5016 0.020 Uiso calc R 1
H H1D 0.4006 0.6200 0.5185 0.020 Uiso calc R 1
C C7 0.32604(8) 0.75991(19) 0.60320(9) 0.0136(2) Uani d . 1
H H7A 0.3248 0.8881 0.6288 0.016 Uiso calc R 1
H H7B 0.3264 0.6718 0.6566 0.016 Uiso calc R 1
C C8 0.2500 0.7265(3) 0.54340(14) 0.0133(3) Uani d S 1
H H8A 0.2500 0.5971 0.5195 0.016 Uiso calc SR 1
H H8B 0.2500 0.8123 0.4890 0.016 Uiso calc SR 1
O O6 0.2991(5) 0.9781(12) 0.8219(7) 0.071(2) Uani d P 0.25
H H6A 0.3333 0.8845 0.8105 0.085 Uiso d PR 0.25
H H6B 0.2500 0.9320 0.8101 0.085 Uiso d SPR 0.50
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
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
O1 Co1 O1 8_544 7_464 98.92(5) ?
O1 Co1 O4 8_544 . 174.14(4) y
O1 Co1 O4 7_464 . 86.91(3) ?
O4 Co1 O4 . 2_665 87.26(5) ?
O1 Co1 O5 8_544 2_665 91.54(4) ?
O1 Co1 O5 7_464 2_665 86.68(4) ?
O4 Co1 O5 . 2_665 89.36(4) ?
O4 Co1 O5 2_665 2_665 92.62(4) ?
O1 Co1 O5 7_464 . 91.54(4) ?
O4 Co1 O5 . . 92.62(4) ?
O4 Co1 O5 2_665 . 89.36(4) ?
O5 Co1 O5 2_665 . 177.26(6) y
C5 O1 Co1 . 7_465 128.29(8) ?
C6 O4 Co1 . . 128.82(8) ?
C2 C1 C2 . 4_655 120.99(16) ?
C2 C1 H1A . . 119.5 ?
C2 C1 H1A 4_655 . 119.5 ?
C1 C2 C3 . . 119.25(13) ?
C1 C2 C5 . . 120.62(11) ?
C3 C2 C5 . . 120.10(12) ?
C4 C3 C2 . . 120.15(13) ?
C4 C3 C6 . . 116.80(11) ?
C2 C3 C6 . . 122.71(12) ?
C3 C4 C3 . 4_655 120.18(15) ?
C3 C4 H4A . . 119.9 ?
C3 C4 H4A 4_655 . 119.9 ?
O2 C5 O1 . . 126.41(11) ?
O2 C5 C2 . . 117.09(11) ?
O1 C5 C2 . . 116.50(11) ?
O3 C6 O4 . . 126.57(11) ?
O3 C6 C3 . . 116.27(11) ?
O4 C6 C3 . . 117.07(11) ?
Co1 O5 H5B . . 100.2 ?
Co1 O5 H5A . . 104.1 ?
H5B O5 H5A . . 114.6 ?
C7 N1 H1B . . 109.5 ?
C7 N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C7 N1 H1D . . 109.5 ?
H1B N1 H1D . . 109.5 ?
H1C N1 H1D . . 109.5 ?
N1 C7 C8 . . 110.80(11) ?
N1 C7 H7A . . 109.5 ?
C8 C7 H7A . . 109.5 ?
N1 C7 H7B . . 109.5 ?
C8 C7 H7B . . 109.5 ?
H7A C7 H7B . . 108.1 ?
C7 C8 C7 . 4 109.24(15) ?
C7 C8 H8A . . 109.8 ?
C7 C8 H8A 4 . 109.8 ?
C7 C8 H8B . . 109.8 ?
C7 C8 H8B 4 . 109.8 ?
H8A C8 H8B . . 108.3 ?
O6 O6 H6A 4 . 129.1 ?
H6A O6 H6B . . 104.9 ?
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
Co1 O1 8_544 2.0650(9) y
Co1 O4 . 2.0910(9) y
Co1 O5 . 2.1107(8) y
O1 C5 . 1.2615(16) ?
O1 Co1 7_465 2.0650(9) ?
O2 C5 . 1.2569(15) ?
O3 C6 . 1.2525(15) ?
O4 C6 . 1.2659(16) ?
C1 C2 . 1.3967(15) ?
C1 C2 4_655 1.3967(15) ?
C1 H1A . 0.9500 ?
C2 C3 . 1.3973(14) ?
C2 C5 . 1.5153(17) ?
C3 C4 . 1.3952(14) ?
C3 C6 . 1.5077(17) ?
C4 C3 4_655 1.3952(14) ?
C4 H4A . 0.9500 ?
O5 H5B . 0.8899 ?
O5 H5A . 0.8901 ?
N1 C7 . 1.4926(16) ?
N1 H1B . 0.9100 ?
N1 H1C . 0.9100 ?
N1 H1D . 0.9100 ?
C7 C8 . 1.5297(17) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C7 4 1.5297(17) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
O6 O6 4 1.612(15) ?
O6 H6A . 0.8900 ?
O6 H6B . 0.8873 ?
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
O5 H5B O3 1_555 0.89 1.85 2.6800(10) 153 y
O5 H5A O2 7_464 0.89 1.91 2.7370(10) 154 y
N1 H1B O2 7_464 0.91 1.93 2.8310(10) 168 y
N1 H1C O4 8_554 0.91 1.95 2.843(2) 166 y
N1 H1D O3 8_544 0.91 2.11 2.988(2) 161 y
C7 H7B Cg 5_545 0.99 2.98 3.767(2) 137 y
C8 H8B Cg 5_555 0.99 2.61 3.439(2) 141 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_4
_geom_torsion
O1 Co1 O4 C6 7_464 . 88.68(11)
O4 Co1 O4 C6 2_665 . -91.95(11)
O5 Co1 O4 C6 2_665 . 175.39(11)
O5 Co1 O4 C6 . . -2.72(11)
C2 C1 C2 C3 4_655 . -0.4(2)
C2 C1 C2 C5 4_655 . 177.80(11)
C1 C2 C3 C4 . . 0.84(16)
C5 C2 C3 C4 . . -177.32(13)
C1 C2 C3 C6 . . -172.23(14)
C5 C2 C3 C6 . . 9.60(15)
C2 C3 C4 C3 . 4_655 -1.3(2)
C6 C3 C4 C3 . 4_655 172.13(10)
Co1 O1 C5 O2 7_465 . 7.22(19)
Co1 O1 C5 C2 7_465 . -172.14(8)
C1 C2 C5 O2 . . -140.38(14)
C3 C2 C5 O2 . . 37.76(15)
C1 C2 C5 O1 . . 39.04(18)
C3 C2 C5 O1 . . -142.82(11)
Co1 O4 C6 O3 . . 10.12(19)
Co1 O4 C6 C3 . . -166.26(8)
C4 C3 C6 O3 . . -114.56(14)
C2 C3 C6 O3 . . 58.73(15)
C4 C3 C6 O4 . . 62.21(17)
C2 C3 C6 O4 . . -124.50(12)
N1 C7 C8 C7 . 4 -178.35(9)
