#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/77/2207731.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_2207731
loop_
_publ_author_name
'Premkumar, Thattan'
'Govindarajan, Subbiah'
'Starosta, Wojciech'
'Leciejewicz, Janusz'
_publ_section_title
;
 Diaquatetrakis(pyrazine-2-carboxylato-κ²O,N)thorium(IV)
 trihydrate
;
_journal_coeditor_code           BV6020
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m98
_journal_page_last               m100
_journal_paper_doi               10.1107/S1600536805039346
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Th (C5 H3 N2 O2)4 (H2 O)2], 3H2 O'
_chemical_formula_moiety         'C20 H16 N8 O10 Th, 3H2 O'
_chemical_formula_sum            'C20 H22 N8 O13 Th'
_chemical_formula_weight         814.50
_chemical_name_systematic
;
Diaquatetrakis(pyrazine-2-carboxylato-κ²O,N)thorium(IV) trihydrate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9080(16)
_cell_length_b                   18.014(4)
_cell_length_c                   19.391(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     2748.7(10)
_computing_cell_refinement       'KM-4 Software'
_computing_data_collection       'KM-4 Software (Kuma, 1996)'
_computing_data_reduction        'DATAPROC (Kuma, 2001)'
_computing_molecular_graphics    'XP (Siemens, 1992)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.95
_diffrn_measured_fraction_theta_max 0.714
_diffrn_measurement_device_type  'Kuma KM-4'
_diffrn_measurement_method       ω/2θ
_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  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7144
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        9.71
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.504
_exptl_absorpt_correction_T_max  0.37871
_exptl_absorpt_correction_T_min  0.24045
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2000)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.543
_refine_diff_density_min         -3.928
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5768
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0835P)²+2.9776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                4872
_reflns_number_total             5768
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bv6020.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2207731
_cod_database_fobs_code          2207731
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_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_type_symbol
Th1 1.03088(3) 0.943782(13) 0.253092(13) 0.02560(9) Uani d . 1 Th
N11 0.9713(8) 0.8032(3) 0.2023(3) 0.0312(13) Uani d . 1 N
C12 0.8124(10) 0.7804(4) 0.2022(4) 0.0344(16) Uani d . 1 C
C13 0.7640(12) 0.7096(5) 0.1793(5) 0.047(2) Uani d . 1 C
H13 0.6515 0.6951 0.1806 0.056 Uiso calc R 1 H
N12 0.8727(11) 0.6618(5) 0.1555(5) 0.060(2) Uani d . 1 N
C15 1.0309(13) 0.6856(5) 0.1557(5) 0.053(2) Uani d . 1 C
H15 1.1105 0.6539 0.1392 0.063 Uiso calc R 1 H
C16 1.0843(11) 0.7551(5) 0.1793(4) 0.0419(19) Uani d . 1 C
H16 1.1978 0.7686 0.1793 0.050 Uiso calc R 1 H
C17 0.6878(9) 0.8349(4) 0.2270(4) 0.0312(14) Uani d . 1 C
O11 0.7433(7) 0.8987(3) 0.2420(3) 0.0341(11) Uani d . 1 O
O12 0.5403(7) 0.8137(3) 0.2305(4) 0.0458(15) Uani d . 1 O
N21 0.9077(10) 0.9384(4) 0.1146(4) 0.0413(16) Uani d . 1 N
C22 1.0214(12) 0.9177(5) 0.0712(4) 0.0411(18) Uani d . 1 C
C23 0.9713(14) 0.9059(7) 0.0004(5) 0.060(3) Uani d . 1 C
H23 1.0539 0.8924 -0.0281 0.072 Uiso calc R 1 H
N22 0.8153(13) 0.9129(7) -0.0272(5) 0.068(3) Uani d . 1 N
C25 0.7009(16) 0.9340(7) 0.0170(6) 0.064(3) Uani d . 1 C
H25 0.5879 0.9406 -0.0002 0.077 Uiso calc R 1 H
C26 0.7470(13) 0.9457(6) 0.0858(5) 0.056(3) Uani d . 1 C
H26 0.6636 0.9593 0.1139 0.068 Uiso calc R 1 H
C27 1.2021(11) 0.9092(6) 0.1019(5) 0.046(2) Uani d . 1 C
O21 1.2227(7) 0.9143(3) 0.1680(3) 0.0386(12) Uani d . 1 O
O22 1.3152(9) 0.8966(5) 0.0658(4) 0.070(2) Uani d . 1 O
N31 1.2036(9) 1.0643(4) 0.2043(4) 0.0352(14) Uani d . 1 N
N32 1.3387(10) 1.1983(5) 0.1615(4) 0.0457(18) Uani d . 1 N
C32 1.1049(9) 1.1227(4) 0.1864(4) 0.0318(15) Uani d . 1 C
C33 1.1724(11) 1.1898(5) 0.1655(4) 0.0395(18) Uani d . 1 C
H33 1.0997 1.2295 0.1542 0.047 Uiso calc R 1 H
C35 1.4358(10) 1.1374(6) 0.1780(5) 0.046(2) Uani d . 1 C
H35 1.5525 1.1401 0.1755 0.056 Uiso calc R 1 H
C36 1.3656(11) 1.0709(5) 0.1985(5) 0.046(2) Uani d . 1 C
H36 1.4363 1.0302 0.2082 0.055 Uiso calc R 1 H
C37 0.9172(9) 1.1132(4) 0.1891(4) 0.0320(15) Uani d . 1 C
O31 0.8742(7) 1.0537(3) 0.2205(3) 0.0349(11) Uani d . 1 O
O32 0.8185(8) 1.1597(4) 0.1625(4) 0.062(2) Uani d . 1 O
N41 0.8422(7) 0.9956(3) 0.3582(3) 0.0266(12) Uani d . 1 N
C42 0.9275(10) 1.0386(4) 0.4055(4) 0.0304(15) Uani d . 1 C
C43 0.8550(11) 1.0694(5) 0.4612(5) 0.0394(18) Uani d . 1 C
H43 0.9204 1.0989 0.4929 0.047 Uiso calc R 1 H
N42 0.6925(9) 1.0568(4) 0.4696(4) 0.0379(15) Uani d . 1 N
C45 0.6056(10) 1.0161(4) 0.4228(4) 0.0365(17) Uani d . 1 C
H45 0.4908 1.0080 0.4267 0.044 Uiso calc R 1 H
C46 0.6785(10) 0.9842(4) 0.3673(4) 0.0361(17) Uani d . 1 C
H46 0.6123 0.9546 0.3360 0.043 Uiso calc R 1 H
C47 1.1119(11) 1.0529(5) 0.3943(4) 0.0370(16) Uani d . 1 C
O41 1.1650(7) 1.0177(3) 0.3436(3) 0.0381(12) Uani d . 1 O
O42 1.1934(9) 1.0973(5) 0.4307(4) 0.071(3) Uani d . 1 O
O1 1.0106(7) 0.8497(3) 0.3499(3) 0.0413(13) Uani d D 1 O
H11 1.079(11) 0.814(4) 0.357(6) 0.062 Uiso d D 1 H
H12 0.9274 0.8328 0.3702 0.062 Uiso d D 1 H
O2 1.3021(8) 0.8844(4) 0.2961(3) 0.0432(14) Uani d D 1 O
H21 1.364(12) 0.861(5) 0.271(5) 0.065 Uiso d D 1 H
H22 1.323(14) 0.881(6) 0.3398(13) 0.065 Uiso d D 1 H
O3 0.4182(8) 0.8464(4) 0.4251(3) 0.0514(16) Uani d D 1 O
H301 0.5217 0.8430 0.4355 0.077 Uiso d D 1 H
H302 0.4030 0.8647 0.4634 0.077 Uiso d D 1 H
O4 0.7484(13) 0.7966(6) 0.4160(6) 0.131(5) Uani d D 1 O
H402 0.7266 0.7545 0.3910 0.197 Uiso d D 1 H
H401 0.7289 0.7701 0.4530 0.197 Uiso d D 1 H
O5 0.920(2) 0.7488(7) 0.5269(7) 0.172(7) Uani d D 1 O
H502 0.8893 0.7071 0.5417 0.258 Uiso d D 1 H
H501 0.9002 0.7789 0.5587 0.258 Uiso d D 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Th Th -7.2400 8.8979 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O41 Th1 O31 85.0(2) y
O41 Th1 O11 127.31(17) ?
O31 Th1 O11 78.20(18) ?
O41 Th1 O21 111.44(19) ?
O31 Th1 O21 110.3(2) ?
O11 Th1 O21 121.24(19) ?
O41 Th1 O2 71.5(2) ?
O31 Th1 O2 149.3(2) ?
O11 Th1 O2 131.8(2) ?
O21 Th1 O2 63.3(2) ?
O41 Th1 O1 83.3(2) y
O31 Th1 O1 132.72(17) ?
O11 Th1 O1 73.3(2) y
O21 Th1 O1 116.63(19) ?
O2 Th1 O1 65.1(2) y
O41 Th1 N11 146.5(2) ?
O31 Th1 N11 127.2(2) ?
O11 Th1 N11 61.86(17) ?
O21 Th1 N11 69.35(19) ?
O2 Th1 N11 80.4(2) y
O1 Th1 N11 68.2(2) ?
O41 Th1 N21 145.9(2) ?
O31 Th1 N21 69.4(2) ?
O11 Th1 N21 70.3(2) ?
O21 Th1 N21 60.8(2) ?
O2 Th1 N21 121.6(2) ?
O1 Th1 N21 130.6(2) ?
N11 Th1 N21 65.6(2) y
O41 Th1 N31 67.3(2) ?
O31 Th1 N31 61.43(19) y
O11 Th1 N31 136.5(2) y
O21 Th1 N31 64.8(2) ?
O2 Th1 N31 90.8(2) y
O1 Th1 N31 147.1(2) ?
N11 Th1 N31 132.19(19) ?
N21 Th1 N31 80.5(2) ?
O41 Th1 N41 60.34(17) y
O31 Th1 N41 67.46(18) ?
O11 Th1 N41 67.08(18) ?
O21 Th1 N41 171.28(18) y
O2 Th1 N41 113.98(19) ?
O1 Th1 N41 66.95(17) ?
N11 Th1 N41 118.96(17) ?
N21 Th1 N41 123.8(2) ?
N31 Th1 N41 107.61(17) ?
C12 N11 C16 117.4(7) ?
C12 N11 Th1 114.6(5) ?
C16 N11 Th1 128.0(5) ?
N11 C12 C13 121.1(7) ?
N11 C12 C17 116.8(7) ?
C13 C12 C17 122.1(7) ?
N12 C13 C12 122.4(9) ?
N12 C13 H13 118.8 ?
C12 C13 H13 118.8 ?
C15 N12 C13 115.7(8) ?
N12 C15 C16 123.5(8) ?
N12 C15 H15 118.3 ?
C16 C15 H15 118.3 ?
N11 C16 C15 119.9(8) ?
N11 C16 H16 120.1 ?
C15 C16 H16 120.1 ?
O12 C17 O11 125.5(7) ?
O12 C17 C12 117.9(7) ?
O11 C17 C12 116.5(6) ?
C17 O11 Th1 129.6(4) ?
C26 N21 C22 115.5(8) ?
C26 N21 Th1 128.9(6) ?
C22 N21 Th1 115.1(6) ?
N21 C22 C23 120.8(9) ?
N21 C22 C27 116.8(8) ?
C23 C22 C27 122.4(8) ?
N22 C23 C22 123.4(9) ?
N22 C23 H23 118.3 ?
C22 C23 H23 118.3 ?
C23 N22 C25 115.5(9) ?
N22 C25 C26 121.9(11) ?
N22 C25 H25 119.0 ?
C26 C25 H25 119.0 ?
N21 C26 C25 122.8(10) ?
N21 C26 H26 118.6 ?
C25 C26 H26 118.6 ?
O22 C27 O21 124.3(9) ?
O22 C27 C22 121.3(9) ?
O21 C27 C22 114.3(7) ?
C27 O21 Th1 132.5(5) ?
C36 N31 C32 117.5(7) ?
C36 N31 Th1 128.4(6) ?
C32 N31 Th1 114.1(5) ?
C33 N32 C35 115.5(7) ?
N31 C32 C33 121.8(7) ?
N31 C32 C37 117.2(6) ?
C33 C32 C37 121.0(7) ?
N32 C33 C32 121.5(8) ?
N32 C33 H33 119.3 ?
C32 C33 H33 119.3 ?
N32 C35 C36 122.0(7) ?
N32 C35 H35 119.0 ?
C36 C35 H35 119.0 ?
N31 C36 C35 121.7(8) ?
N31 C36 H36 119.2 ?
C35 C36 H36 119.2 ?
O32 C37 O31 125.4(7) ?
O32 C37 C32 120.0(7) ?
O31 C37 C32 114.6(6) ?
C37 O31 Th1 131.1(4) ?
C42 N41 C46 115.5(6) ?
C42 N41 Th1 115.1(4) ?
C46 N41 Th1 129.4(5) ?
N41 C42 C43 123.2(7) ?
N41 C42 C47 115.4(6) ?
C43 C42 C47 121.4(7) ?
N42 C43 C42 120.4(8) ?
N42 C43 H43 119.8 ?
C42 C43 H43 119.8 ?
C45 N42 C43 117.3(7) ?
N42 C45 C46 122.5(7) ?
N42 C45 H45 118.8 ?
C46 C45 H45 118.8 ?
N41 C46 C45 121.2(8) ?
N41 C46 H46 119.4 ?
C45 C46 H46 119.4 ?
O42 C47 O41 125.6(8) ?
O42 C47 C42 119.5(7) ?
O41 C47 C42 114.9(7) ?
C47 O41 Th1 133.9(5) ?
Th1 O1 H11 123(8) ?
Th1 O1 H12 133.2 ?
H11 O1 H12 99 ?
Th1 O2 H21 124(8) ?
Th1 O2 H22 116(8) ?
H21 O2 H22 119(10) ?
H301 O3 H302 92.3 ?
H402 O4 H401 86.8 ?
H502 O5 H501 103.9 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Th1 O41 2.369(6) y
Th1 O31 2.388(5) y
Th1 O11 2.405(6) y
Th1 O21 2.409(5) y
Th1 O2 2.466(6) y
Th1 O1 2.545(6) y
Th1 N11 2.742(6) y
Th1 N21 2.766(7) y
Th1 N31 2.781(6) y
Th1 N41 2.804(5) y
N11 C12 1.322(10) ?
N11 C16 1.352(9) ?
C12 C13 1.392(11) ?
C12 C17 1.503(10) ?
C13 N12 1.330(11) ?
C13 H13 0.9300 ?
N12 C15 1.322(13) ?
C15 C16 1.384(12) ?
C15 H15 0.9300 ?
C16 H16 0.9300 ?
C17 O12 1.235(9) ?
C17 O11 1.254(9) ?
N21 C26 1.343(13) ?
N21 C22 1.343(10) ?
C22 C23 1.407(13) ?
C22 C27 1.500(14) ?
C23 N22 1.301(15) ?
C23 H23 0.9300 ?
N22 C25 1.361(15) ?
C25 C26 1.363(15) ?
C25 H25 0.9300 ?
C26 H26 0.9300 ?
C27 O22 1.211(10) ?
C27 O21 1.278(10) ?
N31 C36 1.303(11) ?
N31 C32 1.334(10) ?
N32 C33 1.334(11) ?
N32 C35 1.359(13) ?
C32 C33 1.399(10) ?
C32 C37 1.501(10) ?
C33 H33 0.9300 ?
C35 C36 1.395(12) ?
C35 H35 0.9300 ?
C36 H36 0.9300 ?
C37 O32 1.223(9) ?
C37 O31 1.295(9) ?
N41 C42 1.331(9) ?
N41 C46 1.339(9) ?
C42 C43 1.388(10) ?
C42 C47 1.517(11) ?
C43 N42 1.331(11) ?
C43 H43 0.9300 ?
N42 C45 1.308(11) ?
C45 C46 1.394(10) ?
C45 H45 0.9300 ?
C46 H46 0.9300 ?
C47 O42 1.210(10) ?
C47 O41 1.274(9) ?
O1 H11 0.85(2) ?
O1 H12 0.856(5) ?
O2 H21 0.84(2) ?
O2 H22 0.85(2) ?
O3 H301 0.825(6) ?
O3 H302 0.832(6) ?
O4 H402 0.908(12) ?
O4 H401 0.888(9) ?
O5 H502 0.849(12) ?
O5 H501 0.848(13) ?
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
O1 H11 N32 2_745 0.85(2) 2.22(6) 2.994(9) 152(10)
O1 H12 O4 . 0.856 1.86 2.718(10) 179
O2 H21 O12 1_655 0.84(2) 1.87(3) 2.696(8) 167(11)
O2 H22 O3 1_655 0.85(2) 1.86(5) 2.668(9) 159(11)
O3 H301 O4 . 0.83 2.05 2.783(12) 148
O3 H302 N42 3_676 0.83 2.11 2.886(9) 155
O4 H402 O32 2_645 0.91 2.01 2.919(14) 179
O4 H401 O5 . 0.89 2.01 2.574(19) 120
O5 H502 O22 4_576 0.85 2.03 2.871(15) 174
O5 H501 O42 3_776 0.85 2.36 3.051(15) 138
