#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:23:37 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178897 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/26/4112627.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_4112627
loop_
_publ_author_name
'Pierre Thuéry'
'Claude Villiers'
'Joël Jaud'
'Michel Ephritikhine'
'Bernardo Masci'
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      Bât. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       thuery@drecam.cea.fr
_publ_contact_author_fax         '33 1 69 08 66 40'
_publ_contact_author_name        'P. Thuéry'
_publ_contact_author_phone       '33 01 69 08 63 29'
_publ_section_title
;
 Uranyl-Based Metallamacrocycles: Tri- and Tetranuclear Complexes with
 (2R,3R,4S,5S)-Tetrahydrofurantetracarboxylic Acid
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6838
_journal_page_last               6839
_journal_paper_doi               10.1021/ja0485964
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C82 H156 N8 O48 U4'
_chemical_formula_weight         2974.27
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patter
_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            2
_cell_length_a                   15.9353(16)
_cell_length_b                   15.9353(16)
_cell_length_c                   23.817(3)
_cell_measurement_reflns_used    30120
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      5.14
_cell_volume                     6047.9(11)
_computing_cell_refinement       'Eval-CCD (Duisenberg et al., 2003)'
_computing_data_collection       'Eval-CCD (Duisenberg et al., 2003)'
_computing_data_reduction        'Eval-CCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ 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  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30120
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         5.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.422
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.747
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2774
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0627
_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)+(0.0520P)²+15.0597P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                1669
_reflns_number_total             2774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0485964si20040311_042501.cif
_cod_data_source_block           2
_cod_original_cell_volume        6047.9(10)
_cod_database_code               4112627
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
U U 0.23913(4) 0.77178(4) 0.5000 0.0521(3) Uani 1 2 d S
O1 O 0.1633(7) 0.8538(8) 0.5000 0.058(3) Uani 1 2 d S
O2 O 0.3162(9) 0.6901(7) 0.5000 0.070(4) Uani 1 2 d S
O3 O 0.3566(7) 0.8801(7) 0.5000 0.051(3) Uani 1 2 d S
O4 O 0.2873(6) 0.8182(6) 0.4133(4) 0.065(2) Uani 1 1 d U
O5 O 0.3331(10) 0.9163(10) 0.3552(7) 0.124(5) Uani 1 1 d U
O6 O 0.3100(6) 1.1577(5) 0.4404(4) 0.068(3) Uani 1 1 d U
O7 O 0.4143(17) 1.0871(13) 0.4054(15) 0.063(9) Uani 1 1 d DU
C1 C 0.3640(8) 0.9322(7) 0.4507(7) 0.057(4) Uani 1 1 d .
H1 H 0.4230 0.9446 0.4425 0.068 Uiso 1 1 calc R
C2 C 0.3164(7) 1.0126(7) 0.4665(6) 0.044(3) Uani 1 1 d .
H2 H 0.2583 1.0070 0.4536 0.053 Uiso 1 1 calc R
C3 C 0.3252(11) 0.8878(10) 0.4041(8) 0.078(5) Uani 1 1 d .
C4 C 0.3549(7) 1.0919(8) 0.4388(7) 0.067(4) Uani 1 1 d D
N N 0.4457(9) 1.2244(8) 0.3418(6) 0.069(5) Uani 1 1 d D
H0 H 0.4336 1.1833 0.3670 0.083 Uiso 1 1 calc R
C5 C 0.5154(10) 1.2723(14) 0.3685(8) 0.087(7) Uani 1 1 d DU
H5A H 0.5284 1.3202 0.3449 0.104 Uiso 1 1 calc R
H5B H 0.5648 1.2367 0.3694 0.104 Uiso 1 1 calc R
C6 C 0.4989(16) 1.3038(17) 0.4275(9) 0.092(7) Uani 1 1 d DU
H6A H 0.4475 1.3353 0.4280 0.137 Uiso 1 1 calc R
H6B H 0.5444 1.3391 0.4392 0.137 Uiso 1 1 calc R
H6C H 0.4942 1.2569 0.4526 0.137 Uiso 1 1 calc R
C7 C 0.4721(17) 1.1781(19) 0.2905(10) 0.070(13) Uani 1 1 d DU
H7A H 0.4262 1.1465 0.2743 0.084 Uiso 1 1 calc R
H7B H 0.5189 1.1408 0.2980 0.084 Uiso 1 1 calc R
C8 C 0.498(4) 1.251(3) 0.2537(13) 0.12(2) Uani 1 1 d DU
H8A H 0.4553 1.2942 0.2553 0.177 Uiso 1 1 calc R
H8B H 0.5040 1.2326 0.2156 0.177 Uiso 1 1 calc R
H8C H 0.5501 1.2740 0.2667 0.177 Uiso 1 1 calc R
C9 C 0.3665(10) 1.2715(17) 0.3360(13) 0.115(10) Uani 1 1 d DU
H9A H 0.3749 1.3228 0.3149 0.138 Uiso 1 1 calc R
H9B H 0.3433 1.2854 0.3725 0.138 Uiso 1 1 calc R
C10 C 0.309(3) 1.211(3) 0.305(2) 0.131(16) Uani 1 1 d DU
H10A H 0.2556 1.2372 0.2992 0.196 Uiso 1 1 calc R
H10B H 0.3029 1.1609 0.3261 0.196 Uiso 1 1 calc R
H10C H 0.3337 1.1984 0.2688 0.196 Uiso 1 1 calc R
O8 O 0.5000 0.5000 0.7225(12) 0.093(5) Uani 1 4 d SU
C11 C 0.5000 0.5000 0.6673(15) 0.080(6) Uani 1 4 d SU
O9 O 0.5000 0.5000 0.863(2) 0.178(15) Uiso 1 4 d S
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
O1 U O2 179.4(6) . .
O1 U O6 91.9(4) . 4_465
O2 U O6 88.6(4) . 4_465
O1 U O6 91.9(4) . 11_466
O2 U O6 88.6(4) . 11_466
O6 U O6 75.3(5) 4_465 11_466
O1 U O4 89.4(3) . 10_556
O2 U O4 90.3(3) . 10_556
O6 U O4 155.0(3) 4_465 10_556
O6 U O4 79.6(3) 11_466 10_556
O1 U O4 89.4(3) . .
O2 U O4 90.3(3) . .
O6 U O4 79.6(3) 4_465 .
O6 U O4 155.0(3) 11_466 .
O4 U O4 125.4(5) 10_556 .
O1 U O3 90.1(5) . .
O2 U O3 89.3(5) . .
O6 U O3 142.3(2) 4_465 .
O6 U O3 142.3(2) 11_466 .
O4 U O3 62.7(2) 10_556 .
O4 U O3 62.7(2) . .
C1 O3 C1 108.9(13) 10_556 .
C1 O3 U 116.7(7) 10_556 .
C1 O3 U 116.7(7) . .
C3 O4 U 125.7(10) . .
C4 O6 U 142.8(10) . 3_665
O3 C1 C3 107.8(10) . .
O3 C1 C2 103.9(11) . .
C3 C1 C2 112.6(12) . .
C1 C2 C4 112.3(9) . .
C1 C2 C2 104.2(8) . 10_556
C4 C2 C2 115.2(8) . 10_556
O5 C3 O4 121.3(18) . .
O5 C3 C1 119.2(15) . .
O4 C3 C1 119.4(14) . .
O7 C4 O6 120.1(15) . .
O7 C4 C2 121.6(13) . .
O6 C4 C2 115.9(10) . .
C9 N C7 114.7(9) . .
C9 N C5 114.7(9) . .
C7 N C5 113.2(9) . .
N C5 C6 115.8(16) . .
N C7 C8 100(2) . .
N C9 C10 104(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O1 1.780(12) .
U O2 1.790(13) .
U O6 2.322(9) 4_465
U O6 2.322(9) 11_466
U O4 2.324(10) 10_556
U O4 2.324(10) .
U O3 2.547(11) .
O3 C1 1.443(15) 10_556
O3 C1 1.443(15) .
O4 C3 1.281(17) .
O5 C3 1.26(2) .
O6 C4 1.270(14) .
O6 U 2.322(9) 3_665
O7 C4 1.24(3) .
C1 C3 1.45(2) .
C1 C2 1.536(16) .
C2 C4 1.552(17) .
C2 C2 1.60(3) 10_556
N C9 1.48(2) .
N C7 1.49(3) .
N C5 1.49(2) .
C5 C6 1.52(3) .
C7 C8 1.51(5) .
C9 C10 1.52(5) .
O8 C11 1.31(4) .
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
N H0 O7 0.91 1.81 2.71(2) 168.2
