#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:04:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178633 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/44/4074439.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_4074439
loop_
_publ_author_name
'Maynadié, Jérôme'
'Berthet, Jean-Claude'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 From Bent to Linear Uranium Metallocenes: Influence of
 Counterion, Solvent, and Metal Ion Oxidation State
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5603
_journal_page_last               5611
_journal_paper_doi               10.1021/om060642g
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C32 H47 I2 N U'
_chemical_formula_weight         937.54
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   17.0969(6)
_cell_length_b                   12.9933(9)
_cell_length_c                   15.0916(7)
_cell_measurement_reflns_used    136365
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.95
_cell_volume                     3352.5(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and six ω scans with 2° steps'
_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  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            136365
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.703
_exptl_absorpt_correction_T_max  0.342
_exptl_absorpt_correction_T_min  0.191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent dark brown'
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.970
_refine_diff_density_rms         0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0482
_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)+(0.0671P)²+37.3745P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                3072
_reflns_number_total             3312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060642gsi20060718_024903.cif
_cod_data_source_block           4.C~7~H~8~
_cod_database_code               4074439
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
U U 0.32632(2) 0.7500 0.22600(2) 0.02530(16) Uani 1 2 d S
I1 I 0.19762(4) 0.7500 0.36793(5) 0.0330(2) Uani 1 2 d S
I2 I 0.18674(4) 0.7500 0.09769(5) 0.0362(2) Uani 1 2 d S
N1 N 0.3913(5) 0.7500 0.3774(6) 0.027(2) Uani 1 2 d S
C1 C 0.4108(6) 0.7500 0.4492(7) 0.029(2) Uani 1 2 d S
C2 C 0.4314(7) 0.7500 0.5457(7) 0.038(3) Uani 1 2 d S
C3 C 0.3536(9) 0.7500 0.5944(9) 0.053(4) Uani 1 2 d S
H3A H 0.3243 0.6897 0.5787 0.079 Uiso 1 1 d R
H3B H 0.3632 0.7500 0.6570 0.079 Uiso 1 2 d SR
C4 C 0.4798(7) 0.6533(9) 0.5662(6) 0.058(3) Uani 1 1 d .
H4A H 0.4494 0.5931 0.5531 0.087 Uiso 1 1 calc R
H4B H 0.4940 0.6531 0.6277 0.087 Uiso 1 1 calc R
H4C H 0.5263 0.6533 0.5305 0.087 Uiso 1 1 calc R
C5 C 0.4312(4) 0.5912(7) 0.2417(5) 0.0306(18) Uani 1 1 d .
C6 C 0.3608(5) 0.5531(7) 0.2793(5) 0.0311(18) Uani 1 1 d .
C7 C 0.3058(5) 0.5414(7) 0.2098(6) 0.0339(18) Uani 1 1 d .
C8 C 0.3428(5) 0.5703(7) 0.1294(5) 0.0317(18) Uani 1 1 d .
C9 C 0.4197(4) 0.6018(7) 0.1494(5) 0.0304(17) Uani 1 1 d .
C10 C 0.5098(5) 0.6012(8) 0.2881(6) 0.0355(19) Uani 1 1 d .
H10A H 0.5016 0.6117 0.3504 0.053 Uiso 1 1 calc R
H10B H 0.5378 0.6588 0.2640 0.053 Uiso 1 1 calc R
H10C H 0.5396 0.5395 0.2792 0.053 Uiso 1 1 calc R
C11 C 0.3476(6) 0.5162(8) 0.3727(6) 0.041(2) Uani 1 1 d .
H11A H 0.3394 0.4431 0.3725 0.061 Uiso 1 1 calc R
H11B H 0.3024 0.5497 0.3970 0.061 Uiso 1 1 calc R
H11C H 0.3926 0.5322 0.4082 0.061 Uiso 1 1 calc R
C12 C 0.2253(5) 0.4953(8) 0.2211(6) 0.044(2) Uani 1 1 d .
H12A H 0.2292 0.4216 0.2219 0.066 Uiso 1 1 calc R
H12B H 0.1925 0.5162 0.1727 0.066 Uiso 1 1 calc R
H12C H 0.2030 0.5187 0.2759 0.066 Uiso 1 1 calc R
C13 C 0.3130(5) 0.5485(8) 0.0365(6) 0.040(2) Uani 1 1 d .
H13A H 0.3279 0.6038 -0.0022 0.060 Uiso 1 1 calc R
H13B H 0.2571 0.5426 0.0376 0.060 Uiso 1 1 calc R
H13C H 0.3353 0.4853 0.0154 0.060 Uiso 1 1 calc R
C14 C 0.4834(5) 0.6208(8) 0.0821(6) 0.041(2) Uani 1 1 d .
H14A H 0.5052 0.5562 0.0635 0.061 Uiso 1 1 calc R
H14B H 0.5238 0.6623 0.1082 0.061 Uiso 1 1 calc R
H14C H 0.4619 0.6560 0.0317 0.061 Uiso 1 1 calc R
C15 C 0.4451(8) 0.2500 0.1711(9) 0.044(3) Uani 1 2 d S
C16 C 0.4866(5) 0.1590(8) 0.1682(6) 0.043(2) Uani 1 1 d .
H16 H 0.4599 0.0968 0.1709 0.051 Uiso 1 1 calc R
C17 C 0.5683(6) 0.1586(8) 0.1613(6) 0.043(2) Uani 1 1 d .
H17 H 0.5952 0.0964 0.1588 0.052 Uiso 1 1 calc R
C18 C 0.6088(8) 0.2500 0.1583(9) 0.050(4) Uani 1 2 d S
H18 H 0.6631 0.2500 0.1542 0.060 Uiso 1 2 calc SR
C19 C 0.3584(9) 0.2500 0.1754(15) 0.069(5) Uani 1 2 d S
H19A H 0.3386 0.1897 0.1464 0.103 Uiso 1 1 d R
H19C H 0.3419 0.2500 0.2362 0.103 Uiso 1 2 d SR
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'
I I -0.4742 1.8119 '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'
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
N1 U I1 71.7(2) . .
N1 U I2 155.0(2) . .
I1 U I2 83.29(2) . .
C1 N1 U 171.1(9) . .
N1 C1 C2 176.5(12) . .
C1 C2 C3 105.3(10) . .
C1 C2 C4 108.8(7) . .
C3 C2 C4 112.0(7) . .
C1 C2 C4 108.8(7) . 7_575
C3 C2 C4 112.0(7) . 7_575
C4 C2 C4 109.8(12) . 7_575
C9 C5 C6 108.1(7) . .
C9 C5 C10 124.6(7) . .
C6 C5 C10 126.5(7) . .
C7 C6 C5 107.7(7) . .
C7 C6 C11 124.1(8) . .
C5 C6 C11 127.7(7) . .
C8 C7 C6 108.0(7) . .
C8 C7 C12 127.5(8) . .
C6 C7 C12 124.2(8) . .
C9 C8 C7 108.1(7) . .
C9 C8 C13 124.3(7) . .
C7 C8 C13 126.2(8) . .
C8 C9 C5 108.2(7) . .
C8 C9 C14 125.2(7) . .
C5 C9 C14 125.4(7) . .
C16 C15 C16 118.0(12) . 7_565
C16 C15 C19 121.0(6) . .
C16 C15 C19 121.0(6) 7_565 .
C15 C16 C17 121.3(10) . .
C18 C17 C16 120.1(10) . .
C17 C18 C17 119.4(12) . 7_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U N1 2.541(9) .
U C5 2.743(9) 7_575
U C5 2.743(9) .
U C6 2.746(9) 7_575
U C6 2.746(9) .
U C7 2.744(10) .
U C7 2.744(10) 7_575
U C9 2.756(8) 7_575
U C9 2.756(8) .
U C8 2.767(9) .
U C8 2.767(9) 7_575
U I1 3.0707(8) .
U I2 3.0732(8) .
N1 C1 1.134(14) .
C1 C2 1.498(15) .
C2 C3 1.521(18) .
C2 C4 1.536(13) .
C2 C4 1.536(13) 7_575
C5 C9 1.414(11) .
C5 C6 1.420(11) .
C5 C10 1.521(10) .
C6 C7 1.417(12) .
C6 C11 1.506(11) .
C7 C8 1.418(12) .
C7 C12 1.511(12) .
C8 C9 1.410(10) .
C8 C13 1.518(11) .
C9 C14 1.510(11) .
C15 C16 1.379(12) .
C15 C16 1.379(12) 7_565
C15 C19 1.485(19) .
C16 C17 1.400(13) .
C17 C18 1.376(12) .
C18 C17 1.376(12) 7_565
