#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:50:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179157 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/18/4311863.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_4311863
loop_
_publ_author_name
'Margaret-Jane Crawford'
'Arkady Ellern'
'Konstantin Karaghiosoff'
'Peter Mayer'
'Heinrich Nöth'
'Max Suter'
_publ_contact_author
;
      Margaret-Jane Crawford
      Institut für anorganische Chemie
      Universität München
      Butenandtstr. 5-13 (Haus D)
      81377 München
      Bundesrepublik Deutschland
;
_publ_contact_author_email       mjc@cup.uni-muenchen.de
_publ_contact_author_fax         '089 2180 77492'
_publ_contact_author_phone       '089 2180 77503'
_publ_section_title
;
 Synthesis and Characterization of Heavier Dioxouranium(VI) Dihalides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7120
_journal_page_last               7126
_journal_paper_doi               10.1021/ic0354926
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C36 H30 I1.01 N0.98 O6.96 P2 U'
_chemical_formula_sum            'C36 H30 I1.01 N0.98 O6.96 P2 U'
_chemical_formula_weight         1015.996
_chemical_melting_point          249.0
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 115.0413(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5834(3)
_cell_length_b                   18.9208(7)
_cell_length_c                   10.8624(5)
_cell_measurement_reflns_used    21358
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.134
_cell_volume                     1784.49(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
'HKL Denzo & Scalepack (Otwinowski & Minor 1997)'
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of Göttingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      202(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1415
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23364
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    5.564
_exptl_absorpt_correction_T_max  0.7823
_exptl_absorpt_correction_T_min  0.5796
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
crystal faces optimized with XShape, rev. 1.02, STOE (Darmstadt, Germany)
Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.89088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.024
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.257
_refine_ls_extinction_coef       0.0027(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0611
_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)+(0.0000P)²+20.0277P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                2205
_reflns_number_total             3137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0354926si20040705_042654_3.cif
_cod_data_source_block           hn018
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4311863
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.0000 0.0000 0.0000 0.0400(3) Uani 1 2 d S . .
I I -0.07708(18) 0.03217(8) 0.23363(17) 0.0485(7) Uani 0.507(4) 1 d P A 1
N N -0.07708(18) 0.03217(8) 0.23363(17) 0.0485(7) Uani 0.49 1 d P A 2
O3 O -0.1730(18) -0.0081(9) 0.1284(16) 0.048(4) Uiso 0.493(4) 1 d P A 2
O4 O 0.007(2) 0.0704(10) 0.208(2) 0.065(6) Uiso 0.493(4) 1 d P A 2
O5 O -0.146(2) 0.0536(10) 0.306(2) 0.069(6) Uiso 0.493(4) 1 d P A 2
P P 0.3099(3) 0.13614(15) 0.1685(3) 0.0333(7) Uani 1 1 d . . .
O1 O 0.2122(8) 0.0737(4) 0.0937(8) 0.0375(19) Uani 1 1 d . A .
O2 O -0.1133(9) 0.0703(4) -0.0972(8) 0.046(2) Uani 1 1 d . A .
C1 C 0.4133(12) 0.1189(6) 0.3456(11) 0.033(3) Uani 1 1 d . A .
C2 C 0.5681(14) 0.0971(6) 0.3965(14) 0.043(3) Uani 1 1 d . . .
H2 H 0.6201 0.0957 0.3390 0.052 Uiso 1 1 calc R A .
C3 C 0.6435(16) 0.0776(7) 0.5321(16) 0.060(4) Uani 1 1 d . A .
H3 H 0.7488 0.0642 0.5686 0.072 Uiso 1 1 calc R . .
C4 C 0.5666(16) 0.0778(7) 0.6132(14) 0.055(4) Uani 1 1 d . . .
H4 H 0.6179 0.0627 0.7050 0.066 Uiso 1 1 calc R A .
C5 C 0.4174(16) 0.0992(7) 0.5637(14) 0.052(4) Uani 1 1 d . A .
H5 H 0.3663 0.1002 0.6219 0.062 Uiso 1 1 calc R . .
C6 C 0.3399(14) 0.1195(6) 0.4306(14) 0.045(3) Uani 1 1 d . . .
H6 H 0.2354 0.1341 0.3970 0.054 Uiso 1 1 calc R A .
C7 C 0.1965(12) 0.2151(5) 0.1437(12) 0.032(3) Uani 1 1 d . A .
C8 C 0.2303(14) 0.2666(6) 0.2402(13) 0.044(3) Uani 1 1 d . . .
H8 H 0.3098 0.2591 0.3285 0.053 Uiso 1 1 calc R A .
C9 C 0.1487(15) 0.3306(7) 0.2099(15) 0.054(4) Uani 1 1 d . A .
H9 H 0.1727 0.3662 0.2773 0.065 Uiso 1 1 calc R . .
C10 C 0.0355(15) 0.3412(7) 0.0837(17) 0.059(4) Uani 1 1 d . . .
H10 H -0.0192 0.3847 0.0631 0.071 Uiso 1 1 calc R A .
C11 C -0.0012(16) 0.2901(7) -0.0145(17) 0.057(4) Uani 1 1 d . A .
H11 H -0.0827 0.2980 -0.1017 0.068 Uiso 1 1 calc R . .
C12 C 0.0812(13) 0.2258(6) 0.0127(13) 0.045(3) Uani 1 1 d . . .
H12 H 0.0590 0.1909 -0.0559 0.054 Uiso 1 1 calc R A .
C13 C 0.4508(13) 0.1534(6) 0.1003(14) 0.044(3) Uani 1 1 d . A .
C14 C 0.4707(13) 0.1048(7) 0.0157(14) 0.045(3) Uani 1 1 d . . .
H14 H 0.4080 0.0637 -0.0097 0.054 Uiso 1 1 calc R A .
C15 C 0.5829(16) 0.1151(8) -0.0340(17) 0.067(4) Uani 1 1 d . A .
H15 H 0.6005 0.0800 -0.0884 0.080 Uiso 1 1 calc R . .
C16 C 0.6648(18) 0.1753(10) -0.003(2) 0.081(6) Uani 1 1 d . . .
H16 H 0.7372 0.1839 -0.0402 0.098 Uiso 1 1 calc R A .
C17 C 0.6453(16) 0.2239(8) 0.0792(19) 0.071(5) Uani 1 1 d . A .
H17 H 0.7064 0.2655 0.1008 0.085 Uiso 1 1 calc R . .
C18 C 0.5364(14) 0.2147(6) 0.1348(15) 0.054(4) Uani 1 1 d . . .
H18 H 0.5232 0.2491 0.1927 0.064 Uiso 1 1 calc R A .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
_geom_angle_publ_flag
O2 U O2 180.0(3) 3 . ?
O2 U O1 90.7(3) 3 3 ?
O2 U O1 89.3(3) . 3 ?
O2 U O1 89.3(3) 3 . ?
O2 U O1 90.7(3) . . ?
O1 U O1 180.0(3) 3 . ?
O2 U O3 90.3(5) 3 . ?
O2 U O3 89.7(5) . . ?
O1 U O3 63.7(4) 3 . ?
O1 U O3 116.3(4) . . ?
O2 U O3 89.7(5) 3 3 ?
O2 U O3 90.3(5) . 3 ?
O1 U O3 116.3(4) 3 3 ?
O1 U O3 63.7(4) . 3 ?
O3 U O3 180.0(4) . 3 ?
O2 U O4 85.2(5) 3 3 ?
O2 U O4 94.8(5) . 3 ?
O1 U O4 67.4(5) 3 3 ?
O1 U O4 112.6(5) . 3 ?
O3 U O4 130.8(6) . 3 ?
O3 U O4 49.2(6) 3 3 ?
O2 U O4 94.8(5) 3 . ?
O2 U O4 85.2(5) . . ?
O1 U O4 112.6(5) 3 . ?
O1 U O4 67.4(5) . . ?
O3 U O4 49.2(6) . . ?
O3 U O4 130.8(6) 3 . ?
O4 U O4 180.0(11) 3 . ?
O2 U N 92.5(3) 3 3 ?
O2 U N 87.5(3) . 3 ?
O1 U N 89.47(19) 3 3 ?
O1 U N 90.53(19) . 3 ?
O3 U N 153.1(4) . 3 ?
O3 U N 26.9(4) 3 3 ?
O4 U N 23.4(5) 3 3 ?
O4 U N 156.6(5) . 3 ?
O2 U I 92.5(3) 3 3 ?
O2 U I 87.5(3) . 3 ?
O1 U I 89.47(19) 3 3 ?
O1 U I 90.53(19) . 3 ?
O3 U I 153.1(4) . 3 ?
O3 U I 26.9(4) 3 3 ?
O4 U I 23.4(5) 3 3 ?
O4 U I 156.6(5) . 3 ?
N U I 0.00(5) 3 3 ?
O2 U I 87.5(3) 3 . ?
O2 U I 92.5(3) . . ?
O1 U I 90.53(19) 3 . ?
O1 U I 89.47(19) . . ?
O3 U I 26.9(4) . . ?
O3 U I 153.1(4) 3 . ?
O4 U I 156.6(5) 3 . ?
O4 U I 23.4(5) . . ?
N U I 180.00(5) 3 . ?
I U I 180.00(5) 3 . ?
O1 P C1 111.8(5) . . ?
O1 P C7 111.8(5) . . ?
C1 P C7 109.8(5) . . ?
O1 P C13 108.6(5) . . ?
C1 P C13 107.6(5) . . ?
C7 P C13 107.1(5) . . ?
P O1 U 159.2(5) . . ?
C6 C1 C2 119.4(11) . . ?
C6 C1 P 120.9(9) . . ?
C2 C1 P 119.3(9) . . ?
C3 C2 C1 118.9(12) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C4 C3 C2 120.2(12) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 120.6(13) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.7(14) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 120.2(12) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C8 C7 C12 120.4(10) . . ?
C8 C7 P 123.0(9) . . ?
C12 C7 P 116.1(9) . . ?
C7 C8 C9 120.5(12) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C10 C9 C8 119.6(13) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 120.9(13) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C10 C11 C12 120.6(14) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C7 C12 C11 118.0(12) . . ?
C7 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
C14 C13 C18 120.7(12) . . ?
C14 C13 P 119.3(9) . . ?
C18 C13 P 119.9(11) . . ?
C13 C14 C15 120.8(13) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C16 C15 C14 119.0(15) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C17 120.7(15) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C16 C17 C18 122.1(14) . . ?
C16 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
C13 C18 C17 116.6(14) . . ?
C13 C18 H18 121.7 . . ?
C17 C18 H18 121.7 . . ?
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
U O2 1.758(8) 3 ?
U O2 1.758(8) . ?
U O1 2.316(7) 3 ?
U O1 2.316(7) . ?
U O3 2.583(16) . ?
U O3 2.583(16) 3 ?
U O4 2.60(2) 3 ?
U O4 2.60(2) . ?
U N 2.9906(16) 3 ?
U I 2.9906(16) 3 ?
U I 2.9906(16) . ?
P O1 1.513(7) . ?
P C1 1.782(12) . ?
P C7 1.799(10) . ?
P C13 1.824(13) . ?
C1 C6 1.377(16) . ?
C1 C2 1.408(16) . ?
C2 C3 1.387(18) . ?
C2 H2 0.9500 . ?
C3 C4 1.37(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.359(18) . ?
C4 H4 0.9500 . ?
C5 C6 1.371(17) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.366(16) . ?
C7 C12 1.398(16) . ?
C8 C9 1.402(16) . ?
C8 H8 0.9500 . ?
C9 C10 1.355(19) . ?
C9 H9 0.9500 . ?
C10 C11 1.37(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.411(17) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.370(17) . ?
C13 C18 1.377(16) . ?
C14 C15 1.405(18) . ?
C14 H14 0.9500 . ?
C15 C16 1.34(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.35(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.42(2) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
