#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:12:01 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179561 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/30/4503018.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_4503018
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
'2(U O2 2+).  1(C10 O8 H2 4-).  2(H2 O);  1(H2 O)'
_chemical_formula_sum            'C10 H8 O15 U2'
_chemical_formula_weight         844.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8489(2)
_cell_length_b                   12.7051(2)
_cell_length_c                   9.97360(10)
_cell_measurement_reflns_used    9746
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.228
_cell_measurement_theta_min      3.043
_cell_volume                     1628.16(4)
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            146460
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    19.951
_exptl_absorpt_correction_T_max  0.1562
_exptl_absorpt_correction_T_min  0.0776
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.307
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.00026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0124P)²+5.7726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0348
_refine_ls_wR_factor_ref         0.0377
_reflns_number_gt                2296
_reflns_number_total             2717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201509v_si_011.cif
_cod_data_source_block           upyro001
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4503018
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
U1 U 0.798601(7) 0.813140(8) 0.405113(10) 0.01469(4) Uani 1 1 d .
O1U O 0.80227(18) 0.93220(19) 0.4959(2) 0.0248(5) Uani 1 1 d .
O2U O 0.80059(18) 0.69438(19) 0.3152(3) 0.0262(5) Uani 1 1 d .
O71 O 0.66166(18) 0.88977(18) 0.2669(2) 0.0226(5) Uani 1 1 d .
O81 O 0.98574(17) 0.79115(18) 0.4215(3) 0.0268(5) Uani 1 1 d .
O82 O 0.63774(17) 0.75508(19) 0.4996(3) 0.0245(5) Uani 1 1 d .
O72 O 0.8444(2) 0.7301(2) 0.6063(2) 0.0261(5) Uani 1 1 d .
O1W O 0.8784(2) 0.9119(2) 0.2256(3) 0.0309(6) Uani 1 1 d .
C7 C 0.6304(2) 0.8582(2) 0.1548(3) 0.0153(5) Uani 1 1 d .
C8 C 1.0458(2) 0.7225(2) 0.4694(3) 0.0149(5) Uani 1 1 d .
C2 C 1.0144(2) 0.6086(2) 0.4837(3) 0.0136(5) Uani 1 1 d .
C1 C 0.5603(2) 0.9287(2) 0.0745(3) 0.0136(5) Uani 1 1 d .
C3 C 1.0732(2) 0.5369(2) 0.4102(3) 0.0151(5) Uani 1 1 d .
H3 H 1.1223 0.5619 0.3495 0.018 Uiso 1 1 calc R
O2W O 0.9305(6) 0.1012(6) 0.2771(8) 0.0620(19) Uiso 0.50 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'
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
O2U U1 O1U 177.63(11) . .
O2U U1 O72 92.69(10) . .
O1U U1 O72 86.54(10) . .
O2U U1 O82 87.05(10) . .
O1U U1 O82 94.91(10) . .
O72 U1 O82 74.96(9) . .
O2U U1 O1W 93.55(11) . .
O1U U1 O1W 85.60(10) . .
O72 U1 O1W 139.67(9) . .
O82 U1 O1W 145.14(9) . .
O2U U1 O81 85.46(10) . .
O1U U1 O81 92.17(10) . .
O72 U1 O81 68.99(9) . .
O82 U1 O81 142.72(8) . .
O1W U1 O81 71.86(8) . .
O2U U1 O71 93.72(9) . .
O1U U1 O71 88.11(9) . .
O72 U1 O71 147.74(9) . .
O82 U1 O71 73.85(8) . .
O1W U1 O71 71.32(8) . .
O81 U1 O71 143.05(8) . .
C7 O71 U1 127.43(19) . .
C8 O81 U1 135.5(2) . .
C8 O82 U1 147.4(2) 4_466 .
C7 O72 U1 142.3(2) 2_665 .
O71 C7 O72 122.9(3) . 2_664
O71 C7 C1 118.5(3) . .
O72 C7 C1 118.6(3) 2_664 .
O82 C8 O81 121.0(3) 4_566 .
O82 C8 C2 116.5(3) 4_566 .
O81 C8 C2 122.4(3) . .
C3 C2 C1 119.5(3) . 2_665
C3 C2 C8 115.5(2) . .
C1 C2 C8 124.6(2) 2_665 .
C3 C1 C2 119.0(3) 6_566 2_664
C3 C1 C7 117.3(2) 6_566 .
C2 C1 C7 123.7(3) 2_664 .
C2 C3 C1 121.5(3) . 6_656
C2 C3 H3 119.2 . .
C1 C3 H3 119.2 6_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2U 1.755(2) .
U1 O1U 1.763(2) .
U1 O72 2.342(2) .
U1 O82 2.388(2) .
U1 O1W 2.415(2) .
U1 O81 2.426(2) .
U1 O71 2.438(2) .
O71 C7 1.253(4) .
O81 C8 1.259(4) .
O82 C8 1.253(3) 4_466
O72 C7 1.265(4) 2_665
C7 O72 1.265(4) 2_664
C7 C1 1.501(4) .
C8 O82 1.253(3) 4_566
C8 C2 1.510(4) .
C2 C3 1.392(4) .
C2 C1 1.402(4) 2_665
C1 C3 1.394(4) 6_566
C1 C2 1.402(4) 2_664
C3 C1 1.394(4) 6_656
C3 H3 0.9300 .
