#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/30/4503014.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_4503014
loop_
_publ_author_name
'Mihalcea, Ionut'
'Henry, Natacha'
'Volkringer, Christophe'
'Loiseau, Thierry'
_publ_section_title
;
 Uranyl--Pyromellitate Coordination Polymers: Toward Three-Dimensional
 Open Frameworks with Large Channel Systems
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              526
_journal_paper_doi               10.1021/cg201509v
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety
'1(N H4 1+).  2(U O2 2+).  1(C10 O8 H2 4-).  1(O H 1-);  1(H2 O);  1.75(H2 O)'
_chemical_formula_sum            'C10 H7.5 N O15.75 U2'
_chemical_formula_weight         869.73
_chemical_name_systematic
; 
 ? 
;
_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                 112.7010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1844(2)
_cell_length_b                   21.6150(5)
_cell_length_c                   11.5401(2)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.859
_cell_measurement_theta_min      2.426
_cell_volume                     2113.47(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0806
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            89921
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    15.378
_exptl_absorpt_correction_T_max  0.4797
_exptl_absorpt_correction_T_min  0.1044
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1538
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.779
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.440
_refine_ls_extinction_coef       0.00132(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0296
_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)+(0.0624P)²+5.9123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                3018
_reflns_number_total             3691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201509v_si_003.cif
_cod_data_source_block           upyro001_1
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C10 H7.50 N O15.75 U2'
_cod_database_code               4503014
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_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
U1 U 0.29255(4) 0.246273(14) 0.27919(3) 0.01739(15) Uani 1 1 d .
U2 U -0.08308(4) 0.499504(14) 0.13045(3) 0.02285(15) Uani 1 1 d .
O1W O -0.1900(14) 0.5008(3) 0.2998(10) 0.069(3) Uani 1 1 d .
O102 O 0.1163(7) 0.3360(3) 0.2285(6) 0.0207(14) Uani 1 1 d .
O81 O 0.4809(7) 0.1611(3) 0.3339(6) 0.0191(13) Uani 1 1 d .
O12U O 0.1270(8) 0.1970(3) 0.2294(6) 0.0282(16) Uani 1 1 d .
O11U O 0.4572(8) 0.2964(3) 0.3283(6) 0.0263(15) Uani 1 1 d .
O91 O 0.2466(9) 0.2930(3) 0.4601(6) 0.0339(18) Uani 1 1 d .
O82 O 0.6812(8) 0.0996(3) 0.3514(7) 0.0300(17) Uani 1 1 d .
O101 O -0.0813(9) 0.3996(3) 0.2081(7) 0.0365(19) Uani 1 1 d .
O71 O 0.2359(8) 0.2943(3) 0.0685(6) 0.0269(16) Uani 1 1 d .
O22U O -0.2729(9) 0.4838(3) 0.0162(7) 0.0397(18) Uani 1 1 d .
O72 O 0.3387(9) 0.2019(3) 0.0966(6) 0.0320(17) Uani 1 1 d .
O21U O 0.1059(9) 0.5153(3) 0.2468(7) 0.0361(17) Uani 1 1 d .
O92 O 0.3491(8) 0.2006(3) 0.4921(6) 0.0296(17) Uani 1 1 d .
O1H O 0.0326(9) 0.4405(3) 0.0188(6) 0.0325(19) Uani 1 1 d .
C7 C 0.2872(11) 0.2498(4) 0.0268(8) 0.0167(19) Uani 1 1 d .
C9 C 0.3003(11) 0.2470(4) 0.5297(8) 0.020(2) Uani 1 1 d .
C10 C -0.0205(11) 0.3469(4) 0.2239(8) 0.0182(19) Uani 1 1 d .
C8 C 0.6153(11) 0.1525(4) 0.3353(8) 0.018(2) Uani 1 1 d .
C1 C 0.2899(11) 0.2503(4) -0.1016(9) 0.0187(19) Uani 1 1 d .
C4 C 0.3012(11) 0.2488(4) 0.6613(9) 0.020(2) Uani 1 1 d .
C2 C 0.7097(11) 0.2039(4) 0.3100(8) 0.0172(19) Uani 1 1 d .
C5 C -0.1167(10) 0.2961(4) 0.2498(8) 0.0156(18) Uani 1 1 d .
C6 C -0.1245(10) 0.2948(4) 0.3662(8) 0.0172(19) Uani 1 1 d .
H6 H -0.0711 0.3248 0.4249 0.021 Uiso 1 1 calc R
C3 C 0.2162(11) 0.2941(4) 0.6920(8) 0.0181(19) Uani 1 1 d .
H3 H 0.1625 0.3238 0.6325 0.022 Uiso 1 1 calc R
N1 N 0.3681(16) 0.4247(6) 0.2052(13) 0.083(4) Uiso 1 1 d .
O3W O 0.801(2) 0.4232(9) 0.5057(19) 0.071(6) Uiso 0.50 1 d P
O4W O 0.517(2) 0.5581(9) 0.2623(18) 0.064(5) Uiso 0.50 1 d P
O2W O 0.530(2) 0.3780(8) 0.0638(18) 0.060(5) Uiso 0.50 1 d P
O5W O 0.579(4) 0.5883(17) 0.514(3) 0.059(9) Uiso 0.25 1 d P
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'
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
O12U U1 O11U 179.4(3) . .
O12U U1 O81 93.7(3) . .
O11U U1 O81 86.9(3) . .
O12U U1 O102 89.6(3) . .
O11U U1 O102 89.8(3) . .
O81 U1 O102 176.65(19) . .
O12U U1 O72 84.1(3) . .
O11U U1 O72 96.0(3) . .
O81 U1 O72 66.0(2) . .
O102 U1 O72 114.5(2) . .
O12U U1 O91 96.6(3) . .
O11U U1 O91 83.3(3) . .
O81 U1 O91 114.9(2) . .
O102 U1 O91 64.5(2) . .
O72 U1 O91 178.8(2) . .
O12U U1 O71 96.0(3) . .
O11U U1 O71 83.6(3) . .
O81 U1 O71 115.16(19) . .
O102 U1 O71 64.51(19) . .
O72 U1 O71 51.7(2) . .
O91 U1 O71 127.2(2) . .
O12U U1 O92 84.7(3) . .
O11U U1 O92 95.7(3) . .
O81 U1 O92 65.86(19) . .
O102 U1 O92 114.42(19) . .
O72 U1 O92 129.6(2) . .
O91 U1 O92 51.6(2) . .
O71 U1 O92 178.69(18) . .
O12U U1 C9 90.9(3) . .
O11U U1 C9 89.3(3) . .
O81 U1 C9 90.2(2) . .
O102 U1 C9 89.6(2) . .
O72 U1 C9 155.2(2) . .
O91 U1 C9 25.9(2) . .
O71 U1 C9 153.1(2) . .
O92 U1 C9 25.7(2) . .
O12U U1 C7 90.6(3) . .
O11U U1 C7 89.2(3) . .
O81 U1 C7 90.9(2) . .
O102 U1 C7 89.2(2) . .
O72 U1 C7 26.3(2) . .
O91 U1 C7 152.6(2) . .
O71 U1 C7 25.4(2) . .
O92 U1 C7 155.8(2) . .
C9 U1 C7 178.1(2) . .
O22U U2 O21U 179.1(3) . .
O22U U2 O101 88.2(3) . .
O21U U2 O101 91.6(3) . .
O22U U2 O1H 90.6(3) . .
O21U U2 O1H 90.1(3) . .
O101 U2 O1H 76.7(2) . .
O22U U2 O1H 88.6(3) . 3_565
O21U U2 O1H 92.1(3) . 3_565
O101 U2 O1H 145.2(2) . 3_565
O1H U2 O1H 68.7(3) . 3_565
O22U U2 O82 86.7(3) . 2
O21U U2 O82 93.0(3) . 2
O101 U2 O82 138.8(2) . 2
O1H U2 O82 144.2(2) . 2
O1H U2 O82 75.6(2) 3_565 2
O22U U2 O1W 90.8(4) . .
O21U U2 O1W 88.3(4) . .
O101 U2 O1W 70.0(2) . .
O1H U2 O1W 146.6(2) . .
O1H U2 O1W 144.8(2) 3_565 .
O82 U2 O1W 69.2(2) 2 .
O22U U2 U2 89.6(2) . 3_565
O21U U2 U2 91.4(2) . 3_565
O101 U2 U2 110.95(16) . 3_565
O1H U2 U2 34.35(16) . 3_565
O1H U2 U2 34.33(16) 3_565 3_565
O82 U2 U2 109.86(15) 2 3_565
O1W U2 U2 179.01(17) . 3_565
C10 O102 U1 135.6(5) . .
C8 O81 U1 136.0(5) . .
C9 O91 U1 93.6(5) . .
C8 O82 U2 130.8(6) . 2_545
C10 O101 U2 146.6(6) . .
C7 O71 U1 94.9(5) . .
C7 O72 U1 94.4(5) . .
C9 O92 U1 93.3(5) . .
U2 O1H U2 111.3(3) . 3_565
O71 C7 O72 118.9(8) . .
O71 C7 C1 122.1(8) . .
O72 C7 C1 119.0(7) . .
O71 C7 U1 59.7(4) . .
O72 C7 U1 59.3(4) . .
C1 C7 U1 177.9(6) . .
O92 C9 O91 121.5(8) . .
O92 C9 C4 120.4(8) . .
O91 C9 C4 118.1(8) . .
O92 C9 U1 61.0(4) . .
O91 C9 U1 60.5(4) . .
C4 C9 U1 178.5(6) . .
O101 C10 O102 123.9(8) . .
O101 C10 C5 115.4(8) . .
O102 C10 C5 120.5(8) . .
O81 C8 O82 123.4(8) . .
O81 C8 C2 122.1(8) . .
O82 C8 C2 114.4(8) . .
C6 C1 C2 119.4(8) 4_665 4_565
C6 C1 C7 119.3(8) 4_665 .
C2 C1 C7 121.3(7) 4_565 .
C3 C4 C5 120.2(8) . 4_666
C3 C4 C9 119.3(8) . .
C5 C4 C9 120.5(8) 4_666 .
C3 C2 C1 118.7(8) 4_665 4_666
C3 C2 C8 117.4(8) 4_665 .
C1 C2 C8 123.9(7) 4_666 .
C6 C5 C4 119.0(8) . 4_565
C6 C5 C10 117.6(8) . .
C4 C5 C10 123.4(7) 4_565 .
C5 C6 C1 121.7(8) . 4_566
C5 C6 H6 119.2 . .
C1 C6 H6 119.2 4_566 .
C4 C3 C2 121.1(8) . 4_566
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 4_566 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O12U 1.762(7) .
U1 O11U 1.766(6) .
U1 O81 2.436(6) .
U1 O102 2.448(6) .
U1 O72 2.496(6) .
U1 O91 2.497(6) .
U1 O71 2.507(6) .
U1 O92 2.510(6) .
U1 C9 2.864(9) .
U1 C7 2.895(8) .
U2 O22U 1.766(8) .
U2 O21U 1.770(7) .
U2 O101 2.335(6) .
U2 O1H 2.340(6) .
U2 O1H 2.341(6) 3_565
U2 O82 2.384(6) 2
U2 O1W 2.503(9) .
U2 U2 3.8652(7) 3_565
O102 C10 1.259(10) .
O81 C8 1.242(10) .
O91 C9 1.252(11) .
O82 C8 1.274(11) .
O82 U2 2.384(6) 2_545
O101 C10 1.252(11) .
O71 C7 1.246(10) .
O72 C7 1.286(11) .
O92 C9 1.243(10) .
O1H U2 2.341(6) 3_565
C7 C1 1.492(12) .
C9 C4 1.516(11) .
C10 C5 1.510(12) .
C8 C2 1.504(12) .
C1 C6 1.389(12) 4_665
C1 C2 1.410(12) 4_565
C4 C3 1.381(12) .
C4 C5 1.399(12) 4_666
C2 C3 1.387(11) 4_665
C2 C1 1.410(13) 4_666
C5 C6 1.372(11) .
C5 C4 1.399(12) 4_565
C6 C1 1.389(12) 4_566
C6 H6 0.9300 .
C3 C2 1.387(11) 4_566
C3 H3 0.9300 .
