#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:17:06 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179569 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/35/4503548.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_4503548
loop_
_publ_author_name
'Frisch, Mark'
'Cahill, Christopher L.'
_publ_section_title
;
 Thorium(IV) Coordination Polymers in the Pyridine and
 Pyrazinedicarboxylic Acid Systems
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2921
_journal_paper_doi               10.1021/cg800029z
_journal_volume                  8
_journal_year                    2008
_chemical_formula_moiety         'C12 H12 N4 O12 Th'
_chemical_formula_sum            'C12 H12 N4 O12 Th'
_chemical_formula_weight         636.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 117.7440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3951(9)
_cell_length_b                   7.2453(3)
_cell_length_c                   15.2827(9)
_cell_measurement_reflns_used    8009
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      2.65
_cell_volume                     1704.69(15)
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2005)'
_computing_data_collection       'APEX II (Bruker AXS, 2005)'
_computing_data_reduction        'SAINTPLUS (Bruker AXS, 2005)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 2004)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9894
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    8.826
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.874
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1774
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0168P)²+1.9408P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0364
_refine_ls_wR_factor_ref         0.0367
_reflns_number_gt                1727
_reflns_number_total             1774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg800029z-file018.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4503548
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Th1 Th 0.0000 0.22720(2) 0.7500 0.00854(6) Uani 1 2 d S
O1 O 0.04961(15) 0.4846(3) 0.85773(17) 0.0144(5) Uani 1 1 d .
O2 O 0.14088(15) 0.6912(3) 0.96282(17) 0.0160(5) Uani 1 1 d .
O3 O 0.13264(14) -0.2832(3) 0.70932(16) 0.0132(5) Uani 1 1 d .
O4 O 0.08631(15) -0.0385(3) 0.76111(16) 0.0130(5) Uani 1 1 d .
O5 O -0.11831(16) 0.3478(3) 0.77789(19) 0.0156(5) Uani 1 1 d D
O6 O -0.20189(17) 0.1591(4) 0.85327(19) 0.0186(6) Uani 1 1 d D
C1 C 0.1922(2) 0.3862(4) 0.9653(2) 0.0098(7) Uani 1 1 d .
C2 C 0.1234(2) 0.5362(4) 0.9265(2) 0.0114(7) Uani 1 1 d .
C3 C 0.2256(2) 0.0848(4) 0.9564(2) 0.0116(7) Uani 1 1 d .
H3 H 0.2108 -0.0319 0.9281 0.014 Uiso 1 1 calc R
C4 C 0.0430(2) 0.1582(4) 1.0122(2) 0.0114(7) Uani 1 1 d .
H4 H 0.0734 0.2687 1.0236 0.014 Uiso 1 1 calc R
C5 C 0.0391(2) -0.0698(4) 0.5911(2) 0.0108(7) Uani 1 1 d .
C6 C 0.0893(2) -0.1399(4) 0.6955(2) 0.0113(7) Uani 1 1 d .
N1 N 0.16730(17) 0.2213(4) 0.92069(19) 0.0116(5) Uani 1 1 d .
N2 N 0.00443(18) 0.0887(4) 0.9211(2) 0.0113(6) Uani 1 1 d .
HW1 H -0.188(3) 0.202(6) 0.9077(19) 0.040(14) Uiso 1 1 d D
HW2 H -0.2518(15) 0.181(5) 0.815(3) 0.026(12) Uiso 1 1 d D
HW3 H -0.145(3) 0.291(5) 0.800(3) 0.038(14) Uiso 1 1 d D
HW4 H -0.123(3) 0.453(3) 0.789(3) 0.038(14) Uiso 1 1 d 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'
Th Th -7.2400 8.8979 '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
O1 Th1 O1 76.14(11) . 2_556
O1 Th1 O4 134.00(9) . 2_556
O1 Th1 O4 124.70(7) 2_556 2_556
O1 Th1 O4 124.70(7) . .
O1 Th1 O4 134.00(9) 2_556 .
O4 Th1 O4 73.21(11) 2_556 .
O1 Th1 O5 77.08(9) . 2_556
O1 Th1 O5 70.24(8) 2_556 2_556
O4 Th1 O5 145.40(8) 2_556 2_556
O4 Th1 O5 75.50(8) . 2_556
O1 Th1 O5 70.24(8) . .
O1 Th1 O5 77.08(9) 2_556 .
O4 Th1 O5 75.50(8) 2_556 .
O4 Th1 O5 145.40(8) . .
O5 Th1 O5 138.20(12) 2_556 .
O1 Th1 N2 141.53(9) . 2_556
O1 Th1 N2 77.75(8) 2_556 2_556
O4 Th1 N2 84.31(8) 2_556 2_556
O4 Th1 N2 61.13(8) . 2_556
O5 Th1 N2 67.73(8) 2_556 2_556
O5 Th1 N2 129.61(8) . 2_556
O1 Th1 N2 77.75(8) . .
O1 Th1 N2 141.53(9) 2_556 .
O4 Th1 N2 61.13(8) 2_556 .
O4 Th1 N2 84.31(8) . .
O5 Th1 N2 129.61(8) 2_556 .
O5 Th1 N2 67.73(8) . .
N2 Th1 N2 137.49(11) 2_556 .
O1 Th1 N1 59.46(7) . .
O1 Th1 N1 122.12(8) 2_556 .
O4 Th1 N1 112.93(7) 2_556 .
O4 Th1 N1 65.57(7) . .
O5 Th1 N1 65.42(8) 2_556 .
O5 Th1 N1 115.25(8) . .
N2 Th1 N1 115.12(8) 2_556 .
N2 Th1 N1 64.19(8) . .
O1 Th1 N1 122.12(7) . 2_556
O1 Th1 N1 59.46(7) 2_556 2_556
O4 Th1 N1 65.57(7) 2_556 2_556
O4 Th1 N1 112.93(7) . 2_556
O5 Th1 N1 115.25(8) 2_556 2_556
O5 Th1 N1 65.42(8) . 2_556
N2 Th1 N1 64.19(8) 2_556 2_556
N2 Th1 N1 115.12(8) . 2_556
N1 Th1 N1 178.29(11) . 2_556
C2 O1 Th1 134.7(2) . .
C6 O4 Th1 131.8(2) . .
Th1 O5 HW3 126(3) . .
Th1 O5 HW4 124(4) . .
HW3 O5 HW4 105(5) . .
HW1 O6 HW2 112(5) . .
N1 C1 C3 122.1(3) . 7_557
N1 C1 C2 115.4(3) . .
C3 C1 C2 122.5(3) 7_557 .
O2 C2 O1 125.7(3) . .
O2 C2 C1 119.6(3) . .
O1 C2 C1 114.7(3) . .
N1 C3 C1 121.4(3) . 7_557
N1 C3 H3 119.3 . .
C1 C3 H3 119.3 7_557 .
N2 C4 C5 121.8(3) . 6_556
N2 C4 H4 119.1 . .
C5 C4 H4 119.1 6_556 .
N2 C5 C4 121.7(3) 2_556 6
N2 C5 C6 116.6(3) 2_556 .
C4 C5 C6 121.6(3) 6 .
O3 C6 O4 126.6(3) . .
O3 C6 C5 117.9(3) . .
O4 C6 C5 115.3(3) . .
C3 N1 C1 116.5(3) . .
C3 N1 Th1 129.7(2) . .
C1 N1 Th1 113.58(19) . .
C4 N2 C5 116.5(3) . 2_556
C4 N2 Th1 129.0(2) . .
C5 N2 Th1 114.5(2) 2_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Th1 O1 2.368(2) .
Th1 O1 2.368(2) 2_556
Th1 O4 2.398(2) 2_556
Th1 O4 2.398(2) .
Th1 O5 2.449(3) 2_556
Th1 O5 2.449(3) .
Th1 N2 2.769(3) 2_556
Th1 N2 2.769(3) .
Th1 N1 2.865(3) .
Th1 N1 2.865(3) 2_556
O1 C2 1.279(4) .
O2 C2 1.226(4) .
O3 C6 1.242(4) .
O4 C6 1.263(4) .
O5 HW3 0.805(19) .
O5 HW4 0.792(19) .
O6 HW1 0.811(19) .
O6 HW2 0.805(19) .
C1 N1 1.343(4) .
C1 C3 1.388(5) 7_557
C1 C2 1.519(4) .
C3 N1 1.338(4) .
C3 C1 1.388(5) 7_557
C3 H3 0.9300 .
C4 N2 1.332(4) .
C4 C5 1.393(5) 6_556
C4 H4 0.9300 .
C5 N2 1.340(4) 2_556
C5 C4 1.393(5) 6
C5 C6 1.507(4) .
N2 C5 1.340(4) 2_556
