#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:42:28 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180351 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/20/7202007.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_7202007
loop_
_publ_author_name
'Masci, Bernardo'
'Thuéry, Pierre'
_publ_section_title
;
 Hydrothermal synthesis of uranyl--organic frameworks with
 pyrazine-2,3-dicarboxylate linkers
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1082
_journal_paper_doi               10.1039/b802378f
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C6 H6 N2 O8 U'
_chemical_formula_weight         472.16
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 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                 98.472(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.4220(3)
_cell_length_b                   6.2926(4)
_cell_length_c                   14.5732(10)
_cell_measurement_reflns_used    16192
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.83
_cell_volume                     491.79(5)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and five ω scans with 2° steps'
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16192
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.83
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.540
_exptl_absorpt_correction_T_max  0.516
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    3.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.482(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1786
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0154
_refine_ls_R_factor_gt           0.0151
_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)+(0.0256P)²+0.2330P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0378
_refine_ls_wR_factor_ref         0.0380
_reflns_number_gt                1760
_reflns_number_total             1786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802378f.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7202007
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.56618(11) 0.698714(18) 0.93822(9) 0.00778(6) Uani 1 1 d . . .
O1 O 0.8516(8) 0.8289(6) 0.9684(3) 0.0137(8) Uani 1 1 d . . .
O2 O 0.2779(7) 0.5670(6) 0.9065(3) 0.0145(8) Uani 1 1 d . . .
O3 O 0.5190(8) 0.8569(6) 0.7896(3) 0.0154(8) Uani 1 1 d . . .
O4 O 0.6480(7) 0.9185(6) 0.6529(2) 0.0131(7) Uani 1 1 d . . .
O5 O 0.7389(6) 0.6138(5) 0.5066(2) 0.0112(7) Uani 1 1 d . . .
O6 O 1.1038(9) 0.7630(8) 0.5671(4) 0.0153(8) Uani 1 1 d . . .
O7 O 0.3853(7) 1.0535(5) 0.9505(2) 0.0116(7) Uani 1 1 d . . .
H7A H 0.4875 1.1833 0.9614 0.014 Uiso 1 1 d R . .
H7B H 0.2557 1.0967 0.9817 0.014 Uiso 1 1 d R . .
O8 O 0.4603(8) 0.7298(6) 1.0903(3) 0.0117(8) Uani 1 1 d . . .
H8A H 0.3582 0.6867 1.1294 0.014 Uiso 1 1 d R . .
H8B H 0.5268 0.8630 1.1156 0.014 Uiso 1 1 d R . .
N1 N 0.7615(7) 0.4883(7) 0.8077(3) 0.0102(8) Uani 1 1 d . . .
N2 N 1.0509(9) 0.3567(7) 0.6754(3) 0.0105(8) Uani 1 1 d . . .
C1 C 0.7710(9) 0.6008(8) 0.7298(3) 0.0094(9) Uani 1 1 d . . .
C2 C 0.9119(9) 0.5342(8) 0.6626(4) 0.0091(9) Uani 1 1 d . . .
C3 C 1.0367(10) 0.2416(10) 0.7518(5) 0.0090(10) Uani 1 1 d . . .
H3 H 1.1294 0.1173 0.7619 0.011 Uiso 1 1 calc R . .
C4 C 0.8861(13) 0.3043(7) 0.8167(4) 0.0105(12) Uani 1 1 d . . .
H4 H 0.8720 0.2167 0.8670 0.013 Uiso 1 1 calc R . .
C5 C 0.6340(11) 0.8096(7) 0.7218(4) 0.0105(12) Uani 1 1 d . . .
C6 C 0.9224(10) 0.6522(8) 0.5726(4) 0.0090(10) 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'
U U -9.6767 9.6646 '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
_geom_angle_publ_flag
O1 U O2 179.41(17) . . ?
O1 U O5 90.15(16) . 2_565 ?
O2 U O5 90.02(15) . 2_565 ?
O1 U O3 90.30(18) . . ?
O2 U O3 89.18(16) . . ?
O5 U O3 136.70(13) 2_565 . ?
O1 U O8 93.07(18) . . ?
O2 U O8 87.52(16) . . ?
O5 U O8 78.95(13) 2_565 . ?
O3 U O8 144.21(14) . . ?
O1 U O7 84.49(15) . . ?
O2 U O7 95.63(14) . . ?
O5 U O7 150.83(12) 2_565 . ?
O3 U O7 72.14(12) . . ?
O8 U O7 72.75(13) . . ?
O1 U N1 88.97(16) . . ?
O2 U N1 90.54(15) . . ?
O5 U N1 73.13(13) 2_565 . ?
O3 U N1 63.59(14) . . ?
O8 U N1 152.01(14) . . ?
O7 U N1 135.18(13) . . ?
C5 O3 U 127.7(4) . . ?
C6 O5 U 133.4(3) . 2_564 ?
U O7 H7A 122.9 . . ?
U O7 H7B 129.7 . . ?
H7A O7 H7B 97.2 . . ?
U O8 H8A 145.8 . . ?
U O8 H8B 107.5 . . ?
H8A O8 H8B 104.6 . . ?
C4 N1 C1 117.2(5) . . ?
C4 N1 U 127.5(4) . . ?
C1 N1 U 114.2(3) . . ?
C3 N2 C2 117.7(5) . . ?
N1 C1 C2 121.9(5) . . ?
N1 C1 C5 116.4(5) . . ?
C2 C1 C5 121.6(5) . . ?
N2 C2 C1 120.5(5) . . ?
N2 C2 C6 115.8(4) . . ?
C1 C2 C6 123.8(4) . . ?
N2 C3 C4 121.5(5) . . ?
N2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
N1 C4 C3 121.1(5) . . ?
N1 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
O4 C5 O3 126.8(5) . . ?
O4 C5 C1 117.5(5) . . ?
O3 C5 C1 115.8(5) . . ?
O6 C6 O5 126.6(5) . . ?
O6 C6 C2 118.0(5) . . ?
O5 C6 C2 115.2(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U O1 1.749(4) . ?
U O2 1.769(4) . ?
U O5 2.337(3) 2_565 ?
U O3 2.363(4) . ?
U O8 2.378(4) . ?
U O7 2.456(3) . ?
U N1 2.662(4) . ?
O3 C5 1.278(7) . ?
O4 C5 1.227(7) . ?
O5 C6 1.300(6) . ?
O5 U 2.337(3) 2_564 ?
O6 C6 1.218(7) . ?
O7 H7A 0.9870 . ?
O7 H7B 0.9322 . ?
O8 H8A 0.8932 . ?
O8 H8B 0.9639 . ?
N1 C4 1.337(7) . ?
N1 C1 1.346(7) . ?
N2 C3 1.340(8) . ?
N2 C2 1.345(7) . ?
C1 C2 1.392(7) . ?
C1 C5 1.505(8) . ?
C2 C6 1.516(7) . ?
C3 C4 1.394(9) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
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
O7 H7A O5 0.99 1.91 2.875(5) 164.4 2_575
O7 H7B O6 0.93 1.82 2.705(6) 157.7 2_475
O8 H8A N2 0.89 1.91 2.752(6) 157.6 2_465
O8 H8B O4 0.96 1.59 2.548(5) 176.5 2_575
