#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:28:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179846 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/42/7014272.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_7014272
loop_
_publ_author_name
'Salmon, Lionel'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 Synthesis and crystal structure of tetra- and hexanuclear uranium(IV)
 complexes with hexadentate compartmental Schiff-base ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4139
_journal_page_last               4145
_journal_paper_doi               10.1039/b414626c
_journal_year                    2004
_chemical_formula_sum            'C24 H30 Cl2 N2 O5 U'
_chemical_formula_weight         735.43
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 104.804(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9047(6)
_cell_length_b                   22.5476(15)
_cell_length_c                   11.8755(5)
_cell_measurement_reflns_used    8699
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.23
_cell_volume                     2564.1(3)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8699
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    6.576
_exptl_absorpt_correction_T_max  0.272
_exptl_absorpt_correction_T_min  0.178
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.633
_refine_diff_density_min         -1.482
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2269
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0452P)²+19.7204P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                2127
_reflns_number_total             2269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b414626c.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7014272
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.5000 0.630175(14) 0.7500 0.03219(15) Uani 1 2 d S . .
Cl Cl 0.64755(19) 0.63106(8) 0.97052(17) 0.0448(4) Uani 1 1 d . . .
N N 0.6123(8) 0.5308(3) 0.7041(9) 0.082(3) Uani 1 1 d D . .
O1 O 0.8509(5) 0.7316(2) 0.6351(4) 0.0393(11) Uani 1 1 d . . .
O2 O 0.6853(4) 0.6509(2) 0.6935(4) 0.0339(10) Uani 1 1 d . . .
O3 O 0.5000 0.7386(3) 0.7500 0.0425(17) Uani 1 2 d S . .
C1 C 0.9295(8) 0.7750(4) 0.5905(7) 0.0477(18) Uani 1 1 d . . .
H1A H 1.0254 0.7736 0.6343 0.072 Uiso 1 1 calc R . .
H1B H 0.8921 0.8137 0.5973 0.072 Uiso 1 1 calc R . .
H1C H 0.9235 0.7667 0.5101 0.072 Uiso 1 1 calc R . .
C2 C 0.8798(7) 0.6735(3) 0.6184(6) 0.0342(14) Uani 1 1 d . . .
C3 C 0.7888(7) 0.6321(3) 0.6492(6) 0.0339(14) Uani 1 1 d . . .
C4 C 0.8112(7) 0.5726(3) 0.6331(6) 0.0401(16) Uani 1 1 d D . .
C5 C 0.9227(8) 0.5531(4) 0.5908(8) 0.0503(19) Uani 1 1 d . . .
H5 H 0.9363 0.5128 0.5811 0.060 Uiso 1 1 calc R . .
C6 C 1.0113(8) 0.5937(4) 0.5639(7) 0.053(2) Uani 1 1 d . . .
H6 H 1.0860 0.5810 0.5360 0.064 Uiso 1 1 calc R . .
C7 C 0.9909(7) 0.6541(4) 0.5779(6) 0.0446(17) Uani 1 1 d . . .
H7 H 1.0524 0.6814 0.5598 0.053 Uiso 1 1 calc R . .
C8 C 0.7139(8) 0.5280(3) 0.6536(8) 0.059(2) Uani 1 1 d D . .
H8 H 0.7270 0.4906 0.6251 0.071 Uiso 1 1 calc R . .
C9A C 0.5461(11) 0.4767(4) 0.7395(9) 0.039(3) Uiso 0.50 1 d PD . .
C9B C 0.5036(15) 0.4886(7) 0.6505(11) 0.056(4) Uiso 0.50 1 d PD . .
C10 C 0.4179(10) 0.4622(6) 0.6346(12) 0.053(4) Uani 0.50 1 d PD . .
C11 C 0.6306(15) 0.4205(6) 0.7807(18) 0.084(7) Uani 0.50 1 d PD . .
C12 C 0.6245(8) 0.7755(3) 0.7975(8) 0.052(2) Uani 1 1 d D . .
C13A C 0.6023(13) 0.8355(5) 0.7430(14) 0.048(4) Uiso 0.50 1 d PD . .
C13B C 0.5530(12) 0.8371(5) 0.7639(14) 0.046(4) Uiso 0.50 1 d PD . .
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'
Cl Cl 0.1484 0.1585 '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
O2 U O2 155.0(3) . 2_656 ?
O2 U O3 77.49(13) . . ?
O2 U O3 77.49(13) 2_656 . ?
O2 U N 133.58(19) . 2_656 ?
O2 U N 71.40(19) 2_656 2_656 ?
O3 U N 148.78(15) . 2_656 ?
O2 U N 71.40(19) . . ?
O2 U N 133.58(19) 2_656 . ?
O3 U N 148.78(15) . . ?
N U N 62.4(3) 2_656 . ?
O2 U Cl 90.44(13) . . ?
O2 U Cl 89.37(13) 2_656 . ?
O3 U Cl 89.57(4) . . ?
N U Cl 87.5(2) 2_656 . ?
N U Cl 93.2(2) . . ?
O2 U Cl 89.37(13) . 2_656 ?
O2 U Cl 90.44(13) 2_656 2_656 ?
O3 U Cl 89.57(4) . 2_656 ?
N U Cl 93.2(2) 2_656 2_656 ?
N U Cl 87.5(2) . 2_656 ?
Cl U Cl 179.14(8) . 2_656 ?
C8 N C9B 109.9(9) . . ?
C8 N C9A 122.6(7) . . ?
C2 O1 C1 116.6(6) . . ?
C12 O3 C12 111.3(7) . 2_656 ?
O1 C2 C7 124.8(7) . . ?
O1 C2 C3 115.2(6) . . ?
C7 C2 C3 120.0(7) . . ?
O2 C3 C4 122.0(6) . . ?
O2 C3 C2 119.8(6) . . ?
C4 C3 C2 118.2(6) . . ?
C3 C4 C5 121.7(7) . . ?
C3 C4 C8 120.8(6) . . ?
C5 C4 C8 117.4(7) . . ?
C6 C5 C4 119.3(7) . . ?
C5 C6 C7 120.5(7) . . ?
C2 C7 C6 120.4(7) . . ?
N C8 C4 131.9(7) . . ?
C10 C9A N 117.0(10) 2_656 . ?
N C9A C11 121.5(8) . . ?
N C9A C9B 110.9(10) . 2_656 ?
C11 C9A C9B 98.2(11) . 2_656 ?
N C9A C10 105.7(7) . . ?
C11 C9A C10 110.3(8) . . ?
C9B C9A C10 110.0(10) 2_656 . ?
N C9B C9A 96.0(8) . 2_656 ?
O3 C12 C13A 109.3(8) . . ?
O3 C12 C13B 97.1(7) . . ?
C12 C13A C13B 94.6(9) . 2_656 ?
C13A C13B C12 112.2(10) 2_656 . ?
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 O2 2.160(4) . ?
U O2 2.160(4) 2_656 ?
U O3 2.444(7) . ?
U N 2.621(7) 2_656 ?
U N 2.621(7) . ?
U Cl 2.6530(19) . ?
U Cl 2.6531(19) 2_656 ?
N C8 1.298(10) . ?
N C9B 1.455(10) . ?
N C9A 1.495(9) . ?
N N 2.717(14) 2_656 ?
N O2 2.815(8) . ?
O1 C2 1.365(9) . ?
O1 C1 1.434(8) . ?
O2 C3 1.336(8) . ?
O2 O2 4.218(8) 2_656 ?
O3 C12 1.475(8) . ?
O3 C12 1.475(8) 2_656 ?
C2 C7 1.380(10) . ?
C2 C3 1.410(10) . ?
C3 C4 1.380(10) . ?
C4 C5 1.396(10) . ?
C4 C8 1.456(8) . ?
C5 C6 1.362(12) . ?
C6 C7 1.392(13) . ?
C9A C11 1.528(9) . ?
C9A C9B 1.533(10) 2_656 ?
C9A C10 1.570(9) . ?
C9B C9A 1.533(10) 2_656 ?
C10 C9A 1.48(2) 2_656 ?
C10 C11 1.54(3) 2_656 ?
C11 C10 1.54(3) 2_656 ?
C12 C13A 1.491(10) . ?
C12 C13B 1.564(10) . ?
C13A C13B 1.520(11) 2_656 ?
C13B C13A 1.520(11) 2_656 ?
