#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:05:15 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178933 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/62/4116260.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_4116260
loop_
_publ_author_name
'William J. Evans'
'Gregory W. Nyce'
'Matthew A. Johnston'
'Joseph W. Ziller'
_publ_section_title
;
 How Much Steric Crowding Is Possible in
 Tris(η5-pentamethylcyclopentadienyl) Complexes? Synthesis and Structure
 of (C5Me5)3UCl and (C5Me5)3UF1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12019
_journal_page_last               12020
_journal_paper_doi               10.1021/ja002486p
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C30 H45 F U'
_chemical_formula_weight         662.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   9.9804(5)
_cell_length_b                   9.9804(5)
_cell_length_c                   15.4529(11)
_cell_measurement_temperature    153(2)
_cell_volume                     1333.02(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14417
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    6.110
_exptl_absorpt_correction_T_max  0.6744
_exptl_absorpt_correction_T_min  0.4609
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.965
_refine_diff_density_min         -6.108
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0626P)²+6.4158P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                916
_reflns_number_total             1146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja002486p_2.cif
_cod_data_source_block           gn13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4116260
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
U1 U 0.3333 0.6667 0.2500 0.0417(3) Uani 1 6 d S
F1 F 0.3333 0.6667 0.0924(16) 0.134(7) Uani 1 3 d S
C1 C 0.3880(6) 0.9604(6) 0.2043(4) 0.0260(10) Uani 1 1 d .
C2 C 0.1380(9) 0.8062(9) 0.2500 0.0302(18) Uani 1 2 d S
C3 C 0.1388(7) 0.3722(7) 0.1756(4) 0.0329(13) Uani 1 1 d .
C4 C 0.5120(8) 1.0711(8) 0.1438(6) 0.0465(18) Uani 1 1 d .
H4A H 0.5060 1.1658 0.1387 0.070 Uiso 1 1 calc R
H4B H 0.4973 1.0230 0.0867 0.070 Uiso 1 1 calc R
H4C H 0.6138 1.0966 0.1666 0.070 Uiso 1 1 calc R
C5 C -0.0331(11) 0.7512(12) 0.2500 0.058(3) Uani 1 2 d S
H5A H -0.0485 0.8407 0.2500 0.087 Uiso 1 2 calc SR
H5B H -0.0808 0.6885 0.3018 0.087 Uiso 0.50 1 calc PR
H5C H -0.0808 0.6885 0.1982 0.087 Uiso 0.50 1 calc PR
C6 C 0.1526(9) 0.3341(13) 0.0848(6) 0.073(3) Uani 1 1 d .
H6A H 0.0743 0.2263 0.0730 0.110 Uiso 1 1 calc R
H6B H 0.2559 0.3480 0.0753 0.110 Uiso 1 1 calc R
H6C H 0.1369 0.4026 0.0460 0.110 Uiso 1 1 calc R
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'
F F 0.0171 0.0103 '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
F1 U1 F1 180.000(5) . 10_556
F1 U1 C1 104.65(13) . 10_556
F1 U1 C1 75.35(13) 10_556 10_556
F1 U1 C1 75.35(13) . .
F1 U1 C1 104.65(13) 10_556 .
C1 U1 C1 29.3(3) 10_556 .
F1 U1 C1 75.35(13) . 2_665
F1 U1 C1 104.65(13) 10_556 2_665
C1 U1 C1 122.14(4) 10_556 2_665
C1 U1 C1 113.83(10) . 2_665
F1 U1 C1 104.65(13) . 11_666
F1 U1 C1 75.35(13) 10_556 11_666
C1 U1 C1 113.83(10) 10_556 11_666
C1 U1 C1 122.14(4) . 11_666
C1 U1 C1 29.3(3) 2_665 11_666
F1 U1 C1 104.65(13) . 12_566
F1 U1 C1 75.35(13) 10_556 12_566
C1 U1 C1 113.83(10) 10_556 12_566
C1 U1 C1 122.14(4) . 12_566
C1 U1 C1 122.14(4) 2_665 12_566
C1 U1 C1 113.83(10) 11_666 12_566
F1 U1 C1 75.35(13) . 3_565
F1 U1 C1 104.65(13) 10_556 3_565
C1 U1 C1 122.14(4) 10_556 3_565
C1 U1 C1 113.83(10) . 3_565
C1 U1 C1 113.83(10) 2_665 3_565
C1 U1 C1 122.14(4) 11_666 3_565
C1 U1 C1 29.3(3) 12_566 3_565
F1 U1 C3 113.96(13) . 12_566
F1 U1 C3 66.04(13) 10_556 12_566
C1 U1 C3 29.33(17) 10_556 12_566
C1 U1 C3 48.21(17) . 12_566
C1 U1 C3 96.29(17) 2_665 12_566
C1 U1 C3 84.51(16) 11_666 12_566
C1 U1 C3 131.26(18) 12_566 12_566
C1 U1 C3 149.87(17) 3_565 12_566
F1 U1 C3 66.04(13) . 3_565
F1 U1 C3 113.96(13) 10_556 3_565
C1 U1 C3 48.21(17) 10_556 3_565
C1 U1 C3 29.33(17) . 3_565
C1 U1 C3 84.51(16) 2_665 3_565
C1 U1 C3 96.29(17) 11_666 3_565
C1 U1 C3 149.87(17) 12_566 3_565
C1 U1 C3 131.26(18) 3_565 3_565
C3 U1 C3 47.9(3) 12_566 3_565
F1 U1 C3 66.04(14) . .
F1 U1 C3 113.96(14) 10_556 .
C1 U1 C3 149.87(17) 10_556 .
C1 U1 C3 131.26(18) . .
C1 U1 C3 29.33(17) 2_665 .
C1 U1 C3 48.21(17) 11_666 .
C1 U1 C3 96.29(17) 12_566 .
C1 U1 C3 84.51(16) 3_565 .
C3 U1 C3 125.62(6) 12_566 .
C3 U1 C3 104.63(16) 3_565 .
F1 U1 C3 113.96(14) . 10_556
F1 U1 C3 66.04(14) 10_556 10_556
C1 U1 C3 131.26(18) 10_556 10_556
C1 U1 C3 149.87(17) . 10_556
C1 U1 C3 48.21(17) 2_665 10_556
C1 U1 C3 29.33(17) 11_666 10_556
C1 U1 C3 84.51(16) 12_566 10_556
C1 U1 C3 96.29(17) 3_565 10_556
C3 U1 C3 104.63(16) 12_566 10_556
C3 U1 C3 125.62(6) 3_565 10_556
C3 U1 C3 47.9(3) . 10_556
C1 C1 C3 108.2(4) 10_556 3_565
C1 C1 C4 128.4(4) 10_556 .
C3 C1 C4 121.6(6) 3_565 .
C1 C1 U1 75.35(13) 10_556 .
C3 C1 U1 77.0(3) 3_565 .
C4 C1 U1 125.9(4) . .
C3 C2 C3 108.5(7) 12_566 3_565
C3 C2 C5 124.0(4) 12_566 .
C3 C2 C5 124.0(4) 3_565 .
C3 C2 U1 72.8(4) 12_566 .
C3 C2 U1 72.8(4) 3_565 .
C5 C2 U1 137.1(6) . .
C2 C3 C1 107.5(6) 2_665 2_665
C2 C3 C6 126.7(7) 2_665 .
C1 C3 C6 124.7(7) 2_665 .
C2 C3 U1 78.7(4) 2_665 .
C1 C3 U1 73.7(3) 2_665 .
C6 C3 U1 123.3(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 F1 2.43(3) .
U1 F1 2.43(3) 10_556
U1 C1 2.791(5) 10_556
U1 C1 2.791(5) .
U1 C1 2.791(5) 2_665
U1 C1 2.791(5) 11_666
U1 C1 2.791(5) 12_566
U1 C1 2.791(5) 3_565
U1 C3 2.833(6) 12_566
U1 C3 2.833(6) 3_565
U1 C3 2.833(6) .
U1 C3 2.833(6) 10_556
C1 C1 1.412(12) 10_556
C1 C3 1.424(8) 3_565
C1 C4 1.504(8) .
C2 C3 1.417(8) 12_566
C2 C3 1.417(8) 3_565
C2 C5 1.509(12) .
C3 C2 1.417(8) 2_665
C3 C1 1.424(8) 2_665
C3 C6 1.477(11) .
