#------------------------------------------------------------------------------
#$Date: 2016-03-26 15:36:20 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180345 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/14/7201435.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_7201435
loop_
_publ_author_name
'Deifel, Nicholas P.'
'Cahill, Christopher L.'
_publ_section_title
;
 The uranyl tetrachloride anion as a tecton in the assembly of U(VI)
 hybrid materials
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              2739
_journal_paper_doi               10.1039/b911470j
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C20 H24 Cl6 N4 O4 U'
_chemical_formula_weight         835.18
_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                 102.76
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.0230(2)
_cell_length_b                   15.4120(4)
_cell_length_c                   13.4514(3)
_cell_measurement_temperature    298(2)
_cell_volume                     1420.00(6)
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2005)'
_computing_data_collection       'APEX II (Bruker AXS, 2005)'
_computing_data_reduction        'SAINTPLUS (Bruker AXS, 2005)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 2004)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega 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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0154
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27602
_diffrn_reflns_theta_full        30.32
_diffrn_reflns_theta_max         30.32
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    6.313
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick (2008)'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         4025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0190
_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)+(0.0295P)²+0.9335P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0508
_reflns_number_gt                3333
_reflns_number_total             4025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911470j.txt
_cod_data_source_block           compound7
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7201435
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.0000 0.0000 0.0000 0.02803(4) Uani 1 2 d S . .
Cl1 Cl -0.02084(9) -0.17288(4) 0.01253(4) 0.03785(13) Uani 1 1 d . . .
Cl2 Cl 0.23772(12) 0.45119(4) 0.89536(5) 0.05334(18) Uani 1 1 d . . .
Cl3 Cl -0.14592(18) -0.01153(5) -0.19958(6) 0.0619(2) Uani 1 1 d . . .
O1 O -0.2399(3) 0.00836(10) 0.0201(2) 0.0472(5) Uani 1 1 d . . .
N2 N 0.4658(3) 0.32333(12) 0.04167(14) 0.0326(4) Uani 1 1 d . . .
HN2 H 0.4387 0.3613 -0.0062 0.039 Uiso 1 1 calc R . .
N1 N 0.4967(3) 0.18713(14) -0.28994(14) 0.0379(4) Uani 1 1 d . . .
H1 H 0.4913 0.1755 -0.3530 0.046 Uiso 1 1 calc R . .
C3 C 0.5539(3) 0.28707(15) -0.15511(17) 0.0330(5) Uani 1 1 d . . .
H3 H 0.5893 0.3426 -0.1308 0.040 Uiso 1 1 calc R . .
C5 C 0.4608(3) 0.14084(15) -0.12879(18) 0.0346(5) Uani 1 1 d . . .
H5 H 0.4319 0.0973 -0.0866 0.041 Uiso 1 1 calc R . .
C6 C 0.5097(3) 0.22441(14) -0.09056(16) 0.0276(4) Uani 1 1 d . . .
C7 C 0.5117(3) 0.24266(16) 0.01747(15) 0.0286(4) Uani 1 1 d . . .
C8 C 0.5556(4) 0.18140(17) 0.09434(18) 0.0383(5) Uani 1 1 d . . .
H8 H 0.5893 0.1251 0.0801 0.046 Uiso 1 1 calc R . .
C4 C 0.4563(4) 0.12441(16) -0.22934(19) 0.0397(5) Uani 1 1 d . . .
H4 H 0.4249 0.0691 -0.2556 0.048 Uiso 1 1 calc R . .
C9 C 0.5488(4) 0.20520(19) 0.19324(18) 0.0438(6) Uani 1 1 d . . .
H9 H 0.5757 0.1643 0.2453 0.053 Uiso 1 1 calc R . .
C10 C 0.4599(4) 0.34764(18) 0.13633(18) 0.0416(6) Uani 1 1 d . . .
H10 H 0.4271 0.4044 0.1491 0.050 Uiso 1 1 calc R . .
C2 C 0.5452(4) 0.26698(16) -0.25598(18) 0.0371(5) Uani 1 1 d . . .
H2 H 0.5731 0.3091 -0.3001 0.044 Uiso 1 1 calc R . .
C11 C 0.5024(4) 0.2890(2) 0.21459(18) 0.0460(6) Uani 1 1 d . . .
H11 H 0.4999 0.3054 0.2808 0.055 Uiso 1 1 calc R . .
OW1 O 0.0851(3) 0.61659(12) 0.97984(14) 0.0537(5) Uani 1 1 d . . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O1 U1 O1 180.00(16) . 3 ?
O1 U1 Cl3 89.50(9) . . ?
O1 U1 Cl3 90.50(9) 3 . ?
O1 U1 Cl3 90.50(9) . 3 ?
O1 U1 Cl3 89.50(9) 3 3 ?
Cl3 U1 Cl3 180.00(5) . 3 ?
O1 U1 Cl1 90.25(5) . 3 ?
O1 U1 Cl1 89.75(5) 3 3 ?
Cl3 U1 Cl1 90.983(19) . 3 ?
Cl3 U1 Cl1 89.017(19) 3 3 ?
O1 U1 Cl1 89.75(5) . . ?
O1 U1 Cl1 90.25(5) 3 . ?
Cl3 U1 Cl1 89.017(19) . . ?
Cl3 U1 Cl1 90.983(19) 3 . ?
Cl1 U1 Cl1 180.000(2) 3 . ?
C10 N2 C7 123.4(2) . . ?
C10 N2 HN2 118.3 . . ?
C7 N2 HN2 118.3 . . ?
C2 N1 C4 122.2(2) . . ?
C2 N1 H1 118.9 . . ?
C4 N1 H1 118.9 . . ?
C6 C3 C2 119.7(2) . . ?
C6 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C4 C5 C6 118.9(2) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C3 C6 C5 118.9(2) . . ?
C3 C6 C7 122.1(2) . . ?
C5 C6 C7 119.0(2) . . ?
N2 C7 C8 118.5(2) . . ?
N2 C7 C6 117.67(19) . . ?
C8 C7 C6 123.9(2) . . ?
C7 C8 C9 119.1(2) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
N1 C4 C5 120.5(2) . . ?
N1 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C11 C9 C8 120.4(2) . . ?
C11 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
N2 C10 C11 120.0(2) . . ?
N2 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
N1 C2 C3 119.8(2) . . ?
N1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C10 C11 C9 118.7(2) . . ?
C10 C11 H11 120.7 . . ?
C9 C11 H11 120.7 . . ?
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
U1 O1 1.769(2) . ?
U1 O1 1.769(2) 3 ?
U1 Cl3 2.6597(8) . ?
U1 Cl3 2.6597(8) 3 ?
U1 Cl1 2.6758(6) 3 ?
U1 Cl1 2.6758(6) . ?
N2 C10 1.337(3) . ?
N2 C7 1.342(3) . ?
N2 HN2 0.8600 . ?
N1 C2 1.330(3) . ?
N1 C4 1.335(3) . ?
N1 H1 0.8600 . ?
C3 C6 1.379(3) . ?
C3 C2 1.380(3) . ?
C3 H3 0.9300 . ?
C5 C4 1.369(3) . ?
C5 C6 1.401(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.477(3) . ?
C7 C8 1.384(3) . ?
C8 C9 1.391(3) . ?
C8 H8 0.9300 . ?
C4 H4 0.9300 . ?
C9 C11 1.377(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.370(4) . ?
C10 H10 0.9300 . ?
C2 H2 0.9300 . ?
C11 H11 0.9300 . ?
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
N2 HN2 Cl2 0.86 2.20 2.9880(19) 152.4 1_554
N1 H1 OW1 0.86 1.90 2.718(3) 157.9 2_545
