#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:17:06 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179569 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/35/4503527.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_4503527
loop_
_publ_author_name
'Masci, Bernardo'
'Thuéry, Pierre'
_publ_section_title
;
 Pyrazinetetracarboxylic Acid as an Assembler Ligand in
 Uranyl−Organic Frameworks
;
_journal_issue                   5
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1689
_journal_paper_doi               10.1021/cg701246j
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C16 H12 N4 O22 Rb2 U'
_chemical_formula_weight         1021.27
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.559(4)
_cell_angle_beta                 107.331(4)
_cell_angle_gamma                90.071(3)
_cell_formula_units_Z            1
_cell_length_a                   8.0501(5)
_cell_length_b                   8.7608(6)
_cell_length_c                   10.3486(5)
_cell_measurement_reflns_used    31961
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.43
_cell_volume                     652.35(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and eight 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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            31961
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.038
_exptl_absorpt_correction_T_max  0.448
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             478
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.844
_refine_diff_density_min         -1.904
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0251(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0310
_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)+(0.0483P)²+5.6272P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                2476
_reflns_number_total             2477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg701246j.cif
_cod_data_source_block           6
_cod_database_code               4503527
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
U U 0.5000 0.5000 0.5000 0.01313(17) Uani 1 2 d S
Rb Rb 0.56068(10) 0.76738(9) 0.98828(7) 0.0316(2) Uani 1 1 d .
O1 O 0.4242(6) 0.7212(5) 0.6853(5) 0.0187(9) Uani 1 1 d .
O2 O 0.2933(6) 0.9384(5) 0.7743(5) 0.0179(9) Uani 1 1 d .
O3 O 0.3729(6) 0.4786(5) 0.2455(4) 0.0162(9) Uani 1 1 d .
O4 O 0.2879(6) 0.5741(5) 0.0635(5) 0.0178(9) Uani 1 1 d .
O5 O 0.2770(6) 0.9465(6) 0.0793(5) 0.0205(9) Uani 1 1 d .
O6 O 0.0125(6) 0.8217(5) 0.0404(5) 0.0175(9) Uani 1 1 d .
H6 H 0.0077 0.8094 -0.0562 0.021 Uiso 1 1 d R
O7 O 0.3607(6) 1.2357(5) 0.7277(5) 0.0175(9) Uani 1 1 d .
O8 O 0.0807(6) 1.2129(5) 0.5899(5) 0.0175(9) Uani 1 1 d .
H8 H 0.0889 1.3137 0.6705 0.021 Uiso 1 1 d R
O9 O 0.3051(6) 0.3857(5) 0.4755(5) 0.0185(9) Uani 1 1 d .
O11 O 0.0483(6) 1.4685(5) 0.7845(5) 0.0209(9) Uani 1 1 d .
H11A H 0.1255 1.4976 0.8741 0.025 Uiso 1 1 d R
H11B H 0.0211 1.5543 0.7683 0.025 Uiso 1 1 d R
N1 N 0.3401(6) 0.7437(6) 0.4346(5) 0.0134(10) Uani 1 1 d .
N2 N 0.2090(6) 1.0117(6) 0.3708(5) 0.0143(10) Uani 1 1 d .
C1 C 0.3180(7) 0.8755(7) 0.5388(6) 0.0141(11) Uani 1 1 d .
C2 C 0.2937(7) 0.7418(7) 0.2995(6) 0.0137(11) Uani 1 1 d .
C3 C 0.2262(7) 0.8773(7) 0.2685(6) 0.0136(11) Uani 1 1 d .
C4 C 0.2549(7) 1.0106(7) 0.5071(6) 0.0136(11) Uani 1 1 d .
C5 C 0.3487(8) 0.8464(7) 0.6798(6) 0.0151(12) Uani 1 1 d .
C6 C 0.3186(8) 0.5861(7) 0.1916(6) 0.0145(11) Uani 1 1 d .
C7 C 0.1752(8) 0.8845(7) 0.1177(6) 0.0143(11) Uani 1 1 d .
C8 C 0.2369(8) 1.1658(7) 0.6215(6) 0.0136(11) Uani 1 1 d .
O10 O 0.0003(6) 0.7819(5) -0.2224(5) 0.0185(9) Uani 1 1 d .
H10A H 0.0861 0.8434 -0.2192 0.022 Uiso 1 1 d R
H10B H -0.0911 0.7958 -0.2970 0.022 Uiso 1 1 d R
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O9 U O9 180.0 . 2_666
O9 U O1 87.46(18) . .
O9 U O1 92.54(18) 2_666 .
O9 U O1 92.54(18) . 2_666
O9 U O1 87.46(18) 2_666 2_666
O1 U O1 180.0 . 2_666
O9 U O3 86.66(17) . .
O9 U O3 93.34(17) 2_666 .
O1 U O3 118.14(14) . .
O1 U O3 61.86(14) 2_666 .
O9 U O3 93.34(17) . 2_666
O9 U O3 86.66(17) 2_666 2_666
O1 U O3 61.86(14) . 2_666
O1 U O3 118.14(14) 2_666 2_666
O3 U O3 180.000(1) . 2_666
O9 U N1 94.90(17) . .
O9 U N1 85.10(17) 2_666 .
O1 U N1 59.65(14) . .
O1 U N1 120.35(14) 2_666 .
O3 U N1 59.66(14) . .
O3 U N1 120.34(14) 2_666 .
O9 U N1 85.10(17) . 2_666
O9 U N1 94.90(17) 2_666 2_666
O1 U N1 120.35(14) . 2_666
O1 U N1 59.65(14) 2_666 2_666
O3 U N1 120.34(14) . 2_666
O3 U N1 59.66(14) 2_666 2_666
N1 U N1 180.000(1) . 2_666
O7 Rb O3 125.21(13) 2_677 2_666
O7 Rb O2 61.10(13) 2_677 2_677
O3 Rb O2 144.18(13) 2_666 2_677
O7 Rb O1 168.48(14) 2_677 .
O3 Rb O1 52.45(12) 2_666 .
O2 Rb O1 128.41(13) 2_677 .
O7 Rb O5 79.28(12) 2_677 1_556
O3 Rb O5 142.78(13) 2_666 1_556
O2 Rb O5 69.85(13) 2_677 1_556
O1 Rb O5 97.55(12) . 1_556
O7 Rb O4 81.96(12) 2_677 2_666
O3 Rb O4 43.28(11) 2_666 2_666
O2 Rb O4 126.60(12) 2_677 2_666
O1 Rb O4 94.41(11) . 2_666
O5 Rb O4 142.38(12) 1_556 2_666
O7 Rb O4 60.84(12) 2_677 1_556
O3 Rb O4 102.30(12) 2_666 1_556
O2 Rb O4 109.09(12) 2_677 1_556
O1 Rb O4 107.82(12) . 1_556
O5 Rb O4 62.69(12) 1_556 1_556
O4 Rb O4 79.70(12) 2_666 1_556
O7 Rb O5 122.03(12) 2_677 2_676
O3 Rb O5 92.71(12) 2_666 2_676
O2 Rb O5 63.14(12) 2_677 2_676
O1 Rb O5 69.14(12) . 2_676
O5 Rb O5 95.86(12) 1_556 2_676
O4 Rb O5 121.71(12) 2_666 2_676
O4 Rb O5 158.19(11) 1_556 2_676
O7 Rb O2 138.78(12) 2_677 .
O3 Rb O2 93.69(11) 2_666 .
O2 Rb O2 96.48(11) 2_677 .
O1 Rb O2 41.24(11) . .
O5 Rb O2 59.98(11) 1_556 .
O4 Rb O2 134.44(11) 2_666 .
O4 Rb O2 101.51(11) 1_556 .
O5 Rb O2 61.34(11) 2_676 .
O7 Rb O6 89.28(11) 2_677 1_656
O3 Rb O6 72.95(11) 2_666 1_656
O2 Rb O6 71.92(11) 2_677 1_656
O1 Rb O6 99.84(12) . 1_656
O5 Rb O6 140.96(12) 1_556 1_656
O4 Rb O6 70.40(11) 2_666 1_656
O4 Rb O6 140.49(11) 1_556 1_656
O5 Rb O6 59.16(11) 2_676 1_656
O2 Rb O6 117.81(11) . 1_656
C6 Rb O6 71.28(12) 2_666 1_656
C5 Rb O6 106.74(12) . 1_656
C5 O1 U 131.6(4) . .
C5 O1 Rb 105.3(3) . .
U O1 Rb 122.27(16) . .
C5 O2 Rb 133.6(4) . 2_677
C5 O2 Rb 83.9(3) . .
Rb O2 Rb 83.52(11) 2_677 .
C6 O3 U 130.5(4) . .
C6 O3 Rb 102.6(4) . 2_666
U O3 Rb 123.42(16) . 2_666
C6 O4 Rb 87.3(3) . 2_666
C6 O4 Rb 117.8(4) . 1_554
Rb O4 Rb 100.30(12) 2_666 1_554
C7 O5 Rb 121.0(4) . 1_554
C7 O5 Rb 154.8(4) . 2_676
Rb O5 Rb 84.14(11) 1_554 2_676
C7 O6 Rb 153.4(4) . 1_454
C8 O7 Rb 129.3(4) . 2_677
C2 N1 C1 119.0(5) . .
C2 N1 U 120.0(4) . .
C1 N1 U 120.7(4) . .
C3 N2 C4 117.0(5) . .
N1 C1 C4 120.5(5) . .
N1 C1 C5 112.0(5) . .
C4 C1 C5 127.1(5) . .
N1 C2 C3 119.8(5) . .
N1 C2 C6 114.3(5) . .
C3 C2 C6 125.9(5) . .
N2 C3 C2 122.3(5) . .
N2 C3 C7 115.3(5) . .
C2 C3 C7 122.3(5) . .
N2 C4 C1 121.3(5) . .
N2 C4 C8 115.9(5) . .
C1 C4 C8 122.9(5) . .
O2 C5 O1 126.2(6) . .
O2 C5 C1 119.5(5) . .
O1 C5 C1 114.2(5) . .
O4 C6 O3 126.5(6) . .
O4 C6 C2 119.7(5) . .
O3 C6 C2 113.7(5) . .
O5 C7 O6 126.2(6) . .
O5 C7 C3 121.0(5) . .
O6 C7 C3 112.8(5) . .
O7 C8 O8 126.2(6) . .
O7 C8 C4 120.8(5) . .
O8 C8 C4 113.0(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O9 1.765(4) .
U O9 1.765(4) 2_666
U O1 2.453(4) .
U O1 2.453(4) 2_666
U O3 2.466(4) .
U O3 2.466(4) 2_666
U N1 2.670(5) .
U N1 2.670(5) 2_666
Rb O7 2.826(4) 2_677
Rb O3 2.840(4) 2_666
Rb O2 2.845(4) 2_677
Rb O1 2.880(4) .
Rb O5 2.978(5) 1_556
Rb O4 3.170(4) 2_666
Rb O4 3.191(5) 1_556
Rb O5 3.192(5) 2_676
Rb O2 3.342(4) .
Rb O6 3.521(4) 1_656
O1 C5 1.265(8) .
O2 C5 1.240(8) .
O2 Rb 2.845(4) 2_677
O3 C6 1.264(8) .
O3 Rb 2.840(4) 2_666
O4 C6 1.241(8) .
O4 Rb 3.170(4) 2_666
O4 Rb 3.192(5) 1_554
O5 C7 1.209(8) .
O5 Rb 2.978(5) 1_554
O5 Rb 3.192(5) 2_676
O6 C7 1.318(8) .
O6 Rb 3.522(4) 1_454
O7 C8 1.213(8) .
O7 Rb 2.826(4) 2_677
O8 C8 1.305(7) .
N1 C2 1.329(8) .
N1 C1 1.345(8) .
N2 C3 1.333(8) .
N2 C4 1.351(8) .
C1 C4 1.389(8) .
C1 C5 1.513(8) .
C2 C3 1.400(8) .
C2 C6 1.504(8) .
C3 C7 1.514(8) .
C4 C8 1.516(8) .
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
O6 H6 O10 0.96 1.64 2.596(6) 178.1 .
O8 H8 O11 0.98 1.58 2.536(6) 165.0 .
O10 H10A O2 0.86 1.89 2.741(6) 168.4 1_554
O10 H10B N2 0.94 2.18 2.965(7) 140.5 2_575
O11 H11A O4 0.90 1.90 2.793(6) 176.0 1_566
O11 H11B O10 0.84 1.97 2.795(6) 165.9 1_566
