#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:39:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178575 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/85/4068521.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_4068521
loop_
_publ_author_name
'Dietrich, H. Martin'
'Ziller, Joseph W.'
'Anwander, Reiner'
'Evans, William J.'
_publ_section_title
;
 Reactivity of (C5Me5)2UMe2and (C5Me5)2UMeCl toward Group 13 Alkyls
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1173
_journal_paper_doi               10.1021/om800914w
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C52 H90 Al2 Cl2 U2'
_chemical_formula_weight         1316.16
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 106.028(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.730(4)
_cell_length_b                   11.835(3)
_cell_length_c                   18.919(5)
_cell_measurement_temperature    163(2)
_cell_volume                     2739.5(13)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART1K CCD'
_diffrn_measurement_method       'phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22078
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        '< 1.0'
_exptl_absorpt_coefficient_mu    6.064
_exptl_absorpt_correction_T_max  0.7514
_exptl_absorpt_correction_T_min  0.3920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.310
_refine_diff_density_min         -3.834
_refine_diff_density_rms         0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         4661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0877
_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)+(0.0128P)²+158.5257P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1926
_refine_ls_wR_factor_ref         0.2003
_reflns_number_gt                3756
_reflns_number_total             4661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800914w_si_004.cif
_cod_data_source_block           hmd3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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_original_cell_volume        2739.5(14)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4068521
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
U1 U 0.23998(5) 0.84698(6) 0.10308(3) 0.0228(2) Uani 1 1 d .
Al1 Al -0.1087(5) 0.7465(5) -0.0579(4) 0.0394(15) Uani 1 1 d .
Cl1 Cl 0.1458(4) 1.0639(4) 0.0742(3) 0.0431(13) Uani 1 1 d .
C1 C 0.3889(8) 0.9386(10) 0.0438(5) 0.0669(17) Uani 1 1 d G
C2 C 0.3077(8) 0.9077(10) -0.0169(5) 0.0669(17) Uani 1 1 d G
C3 C 0.3049(8) 0.7899(10) -0.0213(5) 0.0669(17) Uani 1 1 d G
C4 C 0.3889(8) 0.7454(10) 0.0392(5) 0.0669(17) Uani 1 1 d G
C5 C 0.4419(8) 0.8365(10) 0.0795(5) 0.0669(17) Uani 1 1 d G
C6 C 0.4270(13) 1.0527(13) 0.0697(8) 0.0669(17) Uani 1 1 d G
H6A H 0.3952 1.1079 0.0311 0.100 Uiso 1 1 calc R
H6B H 0.5069 1.0556 0.0813 0.100 Uiso 1 1 calc R
H6C H 0.4043 1.0705 0.1139 0.100 Uiso 1 1 calc R
C7 C 0.2332(12) 0.9820(14) -0.0763(7) 0.0669(17) Uani 1 1 d G
H7A H 0.1636 0.9938 -0.0648 0.100 Uiso 1 1 calc R
H7B H 0.2198 0.9445 -0.1242 0.100 Uiso 1 1 calc R
H7C H 0.2686 1.0551 -0.0780 0.100 Uiso 1 1 calc R
C8 C 0.2388(12) 0.7169(13) -0.0838(7) 0.0669(17) Uani 1 1 d G
H8A H 0.1628 0.7428 -0.0984 0.100 Uiso 1 1 calc R
H8B H 0.2417 0.6380 -0.0676 0.100 Uiso 1 1 calc R
H8C H 0.2694 0.7229 -0.1259 0.100 Uiso 1 1 calc R
C9 C 0.4216(13) 0.6262(13) 0.0518(7) 0.0669(17) Uani 1 1 d G
H9A H 0.4875 0.6128 0.0359 0.100 Uiso 1 1 calc R
H9B H 0.3624 0.5776 0.0237 0.100 Uiso 1 1 calc R
H9C H 0.4366 0.6089 0.1043 0.100 Uiso 1 1 calc R
C10 C 0.5490(12) 0.8289(14) 0.1390(7) 0.0669(17) Uani 1 1 d G
H10A H 0.5499 0.7599 0.1679 0.100 Uiso 1 1 calc R
H10B H 0.5569 0.8949 0.1714 0.100 Uiso 1 1 calc R
H10C H 0.6097 0.8270 0.1165 0.100 Uiso 1 1 calc R
C11 C 0.2718(8) 0.9218(10) 0.2455(5) 0.0669(17) Uani 1 1 d G
C12 C 0.1676(8) 0.8794(10) 0.2264(5) 0.0669(17) Uani 1 1 d G
C13 C 0.1740(9) 0.7568(10) 0.2188(5) 0.0669(17) Uani 1 1 d G
C14 C 0.2858(8) 0.7336(10) 0.2320(5) 0.0669(17) Uani 1 1 d G
C15 C 0.3448(8) 0.8280(10) 0.2494(5) 0.0669(17) Uani 1 1 d G
C16 C 0.3026(12) 1.0433(13) 0.2653(8) 0.0669(17) Uani 1 1 d G
H16A H 0.2420 1.0928 0.2402 0.100 Uiso 1 1 calc R
H16B H 0.3678 1.0628 0.2499 0.100 Uiso 1 1 calc R
H16C H 0.3178 1.0532 0.3186 0.100 Uiso 1 1 calc R
C17 C 0.0653(12) 0.9385(13) 0.2220(8) 0.0669(17) Uani 1 1 d G
H17A H 0.0335 0.9094 0.2600 0.100 Uiso 1 1 calc R
H17B H 0.0141 0.9261 0.1734 0.100 Uiso 1 1 calc R
H17C H 0.0797 1.0196 0.2297 0.100 Uiso 1 1 calc R
C18 C 0.0786(12) 0.6810(13) 0.2081(8) 0.0669(17) Uani 1 1 d G
H18A H 0.0839 0.6201 0.1741 0.100 Uiso 1 1 calc R
H18B H 0.0113 0.7241 0.1876 0.100 Uiso 1 1 calc R
H18C H 0.0773 0.6485 0.2555 0.100 Uiso 1 1 calc R
C19 C 0.3282(13) 0.6022(13) 0.2387(8) 0.0669(17) Uani 1 1 d G
H19A H 0.3952 0.5969 0.2230 0.100 Uiso 1 1 calc R
H19B H 0.2716 0.5541 0.2072 0.100 Uiso 1 1 calc R
H19C H 0.3431 0.5772 0.2899 0.100 Uiso 1 1 calc R
C20 C 0.4706(12) 0.8448(14) 0.2865(8) 0.0669(17) Uani 1 1 d G
H20A H 0.4827 0.8619 0.3389 0.100 Uiso 1 1 calc R
H20B H 0.4976 0.9075 0.2626 0.100 Uiso 1 1 calc R
H20C H 0.5098 0.7755 0.2813 0.100 Uiso 1 1 calc R
C21 C 0.040(2) 0.762(2) 0.0160(15) 0.065(3) Uani 1 1 d .
H21A H 0.0866 0.8115 -0.0048 0.079 Uiso 1 1 calc R
H21B H 0.0313 0.7980 0.0611 0.079 Uiso 1 1 calc R
C22 C 0.099(2) 0.644(2) 0.0367(15) 0.065(3) Uani 1 1 d .
H22A H 0.1703 0.6563 0.0724 0.098 Uiso 1 1 calc R
H22B H 0.1095 0.6089 -0.0076 0.098 Uiso 1 1 calc R
H22C H 0.0541 0.5953 0.0583 0.098 Uiso 1 1 calc R
C23 C -0.225(2) 0.669(2) -0.0265(14) 0.065(3) Uani 1 1 d .
H23A H -0.2946 0.7075 -0.0503 0.079 Uiso 1 1 calc R
H23B H -0.2306 0.5911 -0.0463 0.079 Uiso 1 1 calc R
C24 C -0.215(2) 0.661(2) 0.0524(14) 0.065(3) Uani 1 1 d .
H24A H -0.2787 0.6205 0.0596 0.098 Uiso 1 1 calc R
H24B H -0.2128 0.7373 0.0732 0.098 Uiso 1 1 calc R
H24C H -0.1483 0.6203 0.0772 0.098 Uiso 1 1 calc R
C25 C -0.093(2) 0.689(2) -0.1510(14) 0.065(3) Uani 1 1 d .
H25A H -0.0380 0.7368 -0.1651 0.079 Uiso 1 1 calc R
H25B H -0.0619 0.6121 -0.1421 0.079 Uiso 1 1 calc R
C26 C -0.193(2) 0.683(2) -0.2167(14) 0.065(3) Uani 1 1 d .
H26A H -0.1722 0.6536 -0.2593 0.098 Uiso 1 1 calc R
H26B H -0.2241 0.7591 -0.2280 0.098 Uiso 1 1 calc R
H26C H -0.2475 0.6333 -0.2053 0.098 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'
Al Al 0.0645 0.0514 '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
Cnt1 U1 Cl1 102.2 . .
Cnt1 U1 C21 106.1 . .
Cnt2 U1 Cl1 101.2 . .
Cnt2 U1 C21 109.4 . .
Cnt1 U1 Cnt2 138.1 . .
C1 U1 C14 125.2(3) . .
C1 U1 C5 31.17(14) . .
C14 U1 C5 98.4(3) . .
C1 U1 C15 104.6(3) . .
C14 U1 C15 28.46(13) . .
C5 U1 C15 86.8(3) . .
C1 U1 C2 29.18(14) . .
C14 U1 C2 147.1(3) . .
C5 U1 C2 49.5(2) . .
C15 U1 C2 133.2(3) . .
C1 U1 C11 110.4(3) . .
C14 U1 C11 48.8(2) . .
C5 U1 C11 106.5(3) . .
C15 U1 C11 30.33(14) . .
C2 U1 C11 137.0(3) . .
C1 U1 C12 137.4(3) . .
C14 U1 C12 49.2(2) . .
C5 U1 C12 133.9(3) . .
C15 U1 C12 48.6(2) . .
C2 U1 C12 156.8(3) . .
C11 U1 C12 28.75(14) . .
C1 U1 C13 152.9(3) . .
C14 U1 C13 29.70(14) . .
C5 U1 C13 128.1(3) . .
C15 U1 C13 48.4(2) . .
C2 U1 C13 172.5(3) . .
C11 U1 C13 49.1(2) . .
C12 U1 C13 30.68(14) . .
C1 U1 C3 48.4(2) . .
C14 U1 C3 127.0(3) . .
C5 U1 C3 48.6(2) . .
C15 U1 C3 131.4(3) . .
C2 U1 C3 29.30(13) . .
C11 U1 C3 154.9(3) . .
C12 U1 C3 173.7(3) . .
C13 U1 C3 143.2(3) . .
C1 U1 C4 49.4(2) . .
C14 U1 C4 100.0(3) . .
C5 U1 C4 29.03(13) . .
C15 U1 C4 101.8(3) . .
C2 U1 C4 49.1(2) . .
C11 U1 C4 128.9(3) . .
C12 U1 C4 148.4(3) . .
C13 U1 C4 124.6(3) . .
C3 U1 C4 29.80(14) . .
C1 U1 C21 122.0(6) . .
C14 U1 C21 106.6(7) . .
C5 U1 C21 129.0(6) . .
C15 U1 C21 132.5(6) . .
C2 U1 C21 92.8(6) . .
C11 U1 C21 123.6(6) . .
C12 U1 C21 94.9(6) . .
C13 U1 C21 84.4(6) . .
C3 U1 C21 81.3(6) . .
C4 U1 C21 101.8(6) . .
C1 U1 Cl1 82.1(3) . .
C14 U1 Cl1 126.9(2) . .
C5 U1 Cl1 112.3(3) . .
C15 U1 Cl1 109.5(3) . .
C2 U1 Cl1 79.3(3) . .
C11 U1 Cl1 80.6(3) . .
C12 U1 Cl1 79.3(3) . .
C13 U1 Cl1 107.4(2) . .
C3 U1 Cl1 105.5(3) . .
C4 U1 Cl1 127.7(2) . .
C21 U1 Cl1 86.9(6) . .
C25 Al1 C23 112.6(11) . .
C25 Al1 C21 110.1(11) . .
C23 Al1 C21 118.1(12) . .
C25 Al1 Cl1 106.7(9) . 3_575
C23 Al1 Cl1 110.7(9) . 3_575
C21 Al1 Cl1 97.1(9) . 3_575
Al1 Cl1 U1 167.3(3) 3_575 .
C2 C1 C5 108.3 . .
C2 C1 C6 128.9 . .
C5 C1 C6 122.7 . .
C2 C1 U1 77.6(3) . .
C5 C1 U1 76.2(3) . .
C6 C1 U1 116.0(3) . .
C1 C2 C3 108.5 . .
C1 C2 C7 129.4 . .
C3 C2 C7 121.9 . .
C1 C2 U1 73.2(3) . .
C3 C2 U1 77.2(3) . .
C7 C2 U1 119.1(3) . .
C2 C3 C4 108.6 . .
C2 C3 C8 127.8 . .
C4 C3 C8 123.0 . .
C2 C3 U1 73.5(3) . .
C4 C3 U1 75.2(3) . .
C8 C3 U1 124.6(3) . .
C5 C4 C3 107.2 . .
C5 C4 C9 125.7 . .
C3 C4 C9 126.7 . .
C5 C4 U1 73.2(3) . .
C3 C4 U1 75.0(3) . .
C9 C4 U1 122.6(3) . .
C4 C5 C1 107.4 . .
C4 C5 C10 124.5 . .
C1 C5 C10 127.0 . .
C4 C5 U1 77.8(3) . .
C1 C5 U1 72.6(3) . .
C10 C5 U1 125.2(3) . .
C12 C11 C15 107.3 . .
C12 C11 C16 125.4 . .
C15 C11 C16 127.1 . .
C12 C11 U1 75.8(3) . .
C15 C11 U1 73.8(3) . .
C16 C11 U1 120.4(3) . .
C11 C12 C17 128.6 . .
C11 C12 C13 108.2 . .
C17 C12 C13 122.9 . .
C11 C12 U1 75.4(3) . .
C17 C12 U1 121.3(3) . .
C13 C12 U1 74.8(3) . .
C14 C13 C12 105.0 . .
C14 C13 C18 131.3 . .
C12 C13 C18 123.3 . .
C14 C13 U1 72.6(3) . .
C12 C13 U1 74.5(3) . .
C18 C13 U1 122.9(3) . .
C15 C14 C13 110.7 . .
C15 C14 C19 128.6 . .
C13 C14 C19 119.7 . .
C15 C14 U1 77.0(3) . .
C13 C14 U1 77.7(3) . .
C19 C14 U1 121.7(3) . .
C14 C15 C11 108.8 . .
C14 C15 C20 130.5 . .
C11 C15 C20 119.4 . .
C14 C15 U1 74.6(3) . .
C11 C15 U1 75.8(3) . .
C20 C15 U1 126.5(3) . .
C22 C21 Al1 112.6(18) . .
C22 C21 U1 83.0(14) . .
Al1 C21 U1 163.4(14) . .
C24 C23 Al1 118.7(19) . .
C26 C25 Al1 118.9(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 Cnt1 2.470 .
U1 Cnt2 2.471 .
U1 C1 2.683(10) .
U1 C14 2.702(9) .
U1 C5 2.730(9) .
U1 C15 2.731(9) .
U1 C2 2.737(8) .
U1 C11 2.757(9) .
U1 C12 2.762(9) .
U1 C13 2.766(9) .
U1 C3 2.783(8) .
U1 C4 2.787(9) .
U1 C21 2.81(3) .
U1 Cl1 2.822(5) .
U1 C22 3.049 .
Al1 C25 1.95(3) .
Al1 C23 1.97(3) .
Al1 C21 2.03(3) .
Al1 Cl1 2.296(8) 3_575
Cl1 Al1 2.296(8) 3_575
C1 C2 1.366(6) .
C1 C5 1.455(6) .
C1 C6 1.472(6) .
C2 C3 1.397(6) .
C2 C7 1.532(6) .
C3 C4 1.432(6) .
C3 C8 1.518(6) .
C4 C5 1.384(6) .
C4 C9 1.471(6) .
C5 C10 1.513(6) .
C11 C12 1.370(6) .
C11 C15 1.436(6) .
C11 C16 1.511(6) .
C12 C17 1.459(6) .
C12 C13 1.463(6) .
C13 C14 1.403(6) .
C13 C18 1.479(6) .
C14 C15 1.336(6) .
C14 C19 1.639(7) .
C15 C20 1.573(7) .
C21 C22 1.57(4) .
C23 C24 1.47(3) .
C25 C26 1.52(3) .
