#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:25:51 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178623 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/34/4073419.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_4073419
loop_
_publ_author_name
'Maynadié, Jérôme'
'Berthet, Jean-Claude'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 Bent and Linear Uranium(IV) Metallocenes with Terminal and Bridging
 Cyanide Ligands
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4585
_journal_page_last               4591
_journal_paper_doi               10.1021/om7003173
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C58 H92 Cl4 Mg N2 O4 U2'
_chemical_formula_weight         1523.51
_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                 106.958(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3093(12)
_cell_length_b                   32.315(4)
_cell_length_c                   10.4798(13)
_cell_measurement_reflns_used    32595
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.97
_cell_volume                     3015.6(7)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and three 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  0.0828
_diffrn_reflns_av_sigmaI/netI    0.0672
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32595
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    5.596
_exptl_absorpt_correction_T_max  0.676
_exptl_absorpt_correction_T_min  0.178
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2003)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.411
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0637
_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)+(0.0539P)²+36.6782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                4080
_reflns_number_total             5703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7003173.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4073419
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
U U 0.62909(5) 0.142357(12) 0.21127(4) 0.03310(16) Uani 1 1 d .
Mg Mg 0.5000 0.0000 0.5000 0.0339(12) Uani 1 2 d S
Cl1 Cl 0.3687(3) 0.14829(9) 0.2629(3) 0.0379(7) Uani 1 1 d .
Cl2 Cl 0.8796(3) 0.09722(9) 0.2688(3) 0.0433(7) Uani 1 1 d .
N1 N 0.5617(10) 0.0460(3) 0.3814(9) 0.034(2) Uani 1 1 d .
O1 O 0.4243(9) 0.0475(2) 0.6030(7) 0.0372(18) Uani 1 1 d .
O2 O 0.2808(8) -0.0022(2) 0.3696(8) 0.0381(19) Uani 1 1 d .
C1 C 0.5849(12) 0.0743(3) 0.3251(11) 0.034(3) Uani 1 1 d .
C2 C 0.8583(14) 0.1991(4) 0.3007(13) 0.044(3) Uani 1 1 d .
C3 C 0.7321(14) 0.2242(3) 0.2323(12) 0.040(3) Uani 1 1 d .
C4 C 0.6267(13) 0.2224(3) 0.3048(12) 0.038(3) Uani 1 1 d .
C5 C 0.6824(14) 0.1981(3) 0.4197(12) 0.040(3) Uani 1 1 d .
C6 C 0.8266(13) 0.1839(3) 0.4172(11) 0.038(3) Uani 1 1 d .
C7 C 1.0041(15) 0.1953(4) 0.2683(14) 0.056(4) Uani 1 1 d .
H7A H 1.0694 0.2176 0.3096 0.084 Uiso 1 1 calc R
H7B H 0.9858 0.1965 0.1733 0.084 Uiso 1 1 calc R
H7C H 1.0505 0.1693 0.3011 0.084 Uiso 1 1 calc R
C8 C 0.7295(19) 0.2545(4) 0.1224(13) 0.066(5) Uani 1 1 d .
H8A H 0.6288 0.2571 0.0645 0.098 Uiso 1 1 calc R
H8B H 0.7939 0.2448 0.0721 0.098 Uiso 1 1 calc R
H8C H 0.7640 0.2810 0.1605 0.098 Uiso 1 1 calc R
C9 C 0.4836(14) 0.2479(4) 0.2730(15) 0.058(4) Uani 1 1 d .
H9A H 0.4158 0.2360 0.3164 0.086 Uiso 1 1 calc R
H9B H 0.4372 0.2482 0.1783 0.086 Uiso 1 1 calc R
H9C H 0.5075 0.2758 0.3040 0.086 Uiso 1 1 calc R
C10 C 0.6168(19) 0.1933(4) 0.5329(15) 0.069(4) Uani 1 1 d .
H10A H 0.6446 0.2166 0.5917 0.103 Uiso 1 1 calc R
H10B H 0.6543 0.1684 0.5809 0.103 Uiso 1 1 calc R
H10C H 0.5094 0.1919 0.4988 0.103 Uiso 1 1 calc R
C11 C 0.9336(16) 0.1585(4) 0.5277(13) 0.060(4) Uani 1 1 d .
H11A H 1.0161 0.1489 0.4979 0.091 Uiso 1 1 calc R
H11B H 0.8810 0.1351 0.5488 0.091 Uiso 1 1 calc R
H11C H 0.9711 0.1754 0.6056 0.091 Uiso 1 1 calc R
C12 C 0.6563(14) 0.1243(4) -0.0356(11) 0.040(3) Uani 1 1 d .
C13 C 0.5515(14) 0.1570(3) -0.0593(11) 0.038(3) Uani 1 1 d .
C14 C 0.4189(13) 0.1429(4) -0.0383(11) 0.038(3) Uani 1 1 d .
C15 C 0.4409(13) 0.1010(4) -0.0021(12) 0.037(3) Uani 1 1 d .
C16 C 0.5848(14) 0.0889(3) -0.0002(12) 0.042(3) Uani 1 1 d .
C17 C 0.8091(14) 0.1255(4) -0.0602(13) 0.049(3) Uani 1 1 d .
H17A H 0.8709 0.1037 -0.0109 0.073 Uiso 1 1 calc R
H17B H 0.8560 0.1517 -0.0315 0.073 Uiso 1 1 calc R
H17C H 0.7971 0.1220 -0.1536 0.073 Uiso 1 1 calc R
C18 C 0.5667(18) 0.1967(4) -0.1326(13) 0.058(4) Uani 1 1 d .
H18A H 0.5338 0.1919 -0.2271 0.087 Uiso 1 1 calc R
H18B H 0.6699 0.2054 -0.1066 0.087 Uiso 1 1 calc R
H18C H 0.5061 0.2180 -0.1105 0.087 Uiso 1 1 calc R
C19 C 0.2736(15) 0.1666(4) -0.0665(13) 0.053(4) Uani 1 1 d .
H19A H 0.2948 0.1955 -0.0486 0.080 Uiso 1 1 calc R
H19B H 0.2163 0.1564 -0.0104 0.080 Uiso 1 1 calc R
H19C H 0.2171 0.1631 -0.1583 0.080 Uiso 1 1 calc R
C20 C 0.3225(13) 0.0722(4) 0.0238(12) 0.042(3) Uani 1 1 d .
H20A H 0.2498 0.0882 0.0513 0.063 Uiso 1 1 calc R
H20B H 0.3698 0.0529 0.0928 0.063 Uiso 1 1 calc R
H20C H 0.2732 0.0574 -0.0565 0.063 Uiso 1 1 calc R
C21 C 0.6461(15) 0.0453(3) 0.0145(13) 0.050(3) Uani 1 1 d .
H21A H 0.6207 0.0317 0.0865 0.074 Uiso 1 1 calc R
H21B H 0.7533 0.0461 0.0330 0.074 Uiso 1 1 calc R
H21C H 0.6031 0.0303 -0.0668 0.074 Uiso 1 1 calc R
C22 C 0.4575(14) 0.0909(3) 0.6186(12) 0.042(3) Uani 1 1 d .
H22A H 0.5129 0.0999 0.5583 0.050 Uiso 1 1 calc R
H22B H 0.5161 0.0972 0.7095 0.050 Uiso 1 1 calc R
C23 C 0.3072(14) 0.1113(4) 0.5855(13) 0.046(3) Uani 1 1 d .
H23A H 0.2666 0.1154 0.4900 0.055 Uiso 1 1 calc R
H23B H 0.3135 0.1378 0.6300 0.055 Uiso 1 1 calc R
C24 C 0.2093(14) 0.0806(3) 0.6372(12) 0.041(3) Uani 1 1 d .
H24A H 0.1949 0.0903 0.7203 0.049 Uiso 1 1 calc R
H24B H 0.1120 0.0769 0.5721 0.049 Uiso 1 1 calc R
C25 C 0.2997(15) 0.0408(4) 0.6580(13) 0.047(3) Uani 1 1 d .
H25A H 0.3368 0.0343 0.7522 0.057 Uiso 1 1 calc R
H25B H 0.2377 0.0181 0.6126 0.057 Uiso 1 1 calc R
C26 C 0.1973(14) 0.0332(4) 0.3021(11) 0.041(3) Uani 1 1 d .
H26A H 0.2640 0.0538 0.2834 0.049 Uiso 1 1 calc R
H26B H 0.1395 0.0457 0.3554 0.049 Uiso 1 1 calc R
C27 C 0.0964(13) 0.0156(4) 0.1759(11) 0.041(3) Uani 1 1 d .
H27A H 0.1498 0.0108 0.1104 0.049 Uiso 1 1 calc R
H27B H 0.0108 0.0334 0.1378 0.049 Uiso 1 1 calc R
C28 C 0.0490(14) -0.0248(4) 0.2253(12) 0.047(3) Uani 1 1 d .
H28A H -0.0333 -0.0206 0.2631 0.056 Uiso 1 1 calc R
H28B H 0.0193 -0.0450 0.1539 0.056 Uiso 1 1 calc R
C29 C 0.1887(14) -0.0382(4) 0.3300(14) 0.054(4) Uani 1 1 d .
H29A H 0.1634 -0.0499 0.4060 0.065 Uiso 1 1 calc R
H29B H 0.2415 -0.0590 0.2943 0.065 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'
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'
Na Na 0.0362 0.0249 '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'
Cl Cl 0.1484 0.1585 '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
C1 U Cl1 71.9(3) . .
C1 U Cl2 71.2(3) . .
Cl1 U Cl2 142.00(9) . .
O2 Mg O2 180.0 . 3_656
O2 Mg O1 92.8(3) . 3_656
O2 Mg O1 87.2(3) 3_656 3_656
O2 Mg O1 87.2(3) . .
O2 Mg O1 92.8(3) 3_656 .
O1 Mg O1 179.998(1) 3_656 .
O2 Mg N1 88.8(3) . 3_656
O2 Mg N1 91.2(3) 3_656 3_656
O1 Mg N1 88.8(3) 3_656 3_656
O1 Mg N1 91.2(3) . 3_656
O2 Mg N1 91.2(3) . .
O2 Mg N1 88.8(3) 3_656 .
O1 Mg N1 91.2(3) 3_656 .
O1 Mg N1 88.8(3) . .
N1 Mg N1 179.998(1) 3_656 .
C1 N1 Mg 170.9(10) . .
C22 O1 C25 105.7(9) . .
C22 O1 Mg 132.5(7) . .
C25 O1 Mg 121.3(6) . .
C29 O2 C26 108.0(8) . .
C29 O2 Mg 127.0(7) . .
C26 O2 Mg 124.9(7) . .
N1 C1 U 175.1(10) . .
C6 C2 C3 106.2(11) . .
C6 C2 C7 126.5(12) . .
C3 C2 C7 126.7(12) . .
C4 C3 C2 107.8(10) . .
C4 C3 C8 125.5(12) . .
C2 C3 C8 125.3(12) . .
C5 C4 C3 110.2(10) . .
C5 C4 C9 125.0(12) . .
C3 C4 C9 124.3(12) . .
C4 C5 C6 106.2(11) . .
C4 C5 C10 127.2(12) . .
C6 C5 C10 126.0(12) . .
C2 C6 C5 109.7(10) . .
C2 C6 C11 125.6(12) . .
C5 C6 C11 124.6(12) . .
C13 C12 C16 107.2(11) . .
C13 C12 C17 125.7(11) . .
C16 C12 C17 126.7(12) . .
C14 C13 C12 109.0(10) . .
C14 C13 C18 124.9(12) . .
C12 C13 C18 124.0(12) . .
C13 C14 C15 107.0(10) . .
C13 C14 C19 126.1(11) . .
C15 C14 C19 126.5(11) . .
C16 C15 C14 109.8(10) . .
C16 C15 C20 124.7(11) . .
C14 C15 C20 125.4(11) . .
C15 C16 C12 107.0(10) . .
C15 C16 C21 126.6(11) . .
C12 C16 C21 125.7(12) . .
O1 C22 C23 104.4(9) . .
C22 C23 C24 104.1(9) . .
C25 C24 C23 103.5(10) . .
O1 C25 C24 106.9(10) . .
O2 C26 C27 103.9(9) . .
C26 C27 C28 101.3(10) . .
C29 C28 C27 102.8(10) . .
O2 C29 C28 107.2(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U C1 2.591(11) .
U Cl1 2.640(3) .
U Cl2 2.666(3) .
U C12 2.735(12) .
U C6 2.743(11) .
U C16 2.744(12) .
U C15 2.751(12) .
U C13 2.755(12) .
U C2 2.761(12) .
U C5 2.762(12) .
U C4 2.769(11) .
U C14 2.772(11) .
U C3 2.799(11) .
Mg O2 2.100(7) .
Mg O2 2.100(7) 3_656
Mg O1 2.112(7) 3_656
Mg O1 2.112(7) .
Mg N1 2.121(9) 3_656
Mg N1 2.121(9) .
N1 C1 1.143(13) .
O1 C22 1.436(13) .
O1 C25 1.453(14) .
O2 C29 1.432(13) .
O2 C26 1.448(13) .
C2 C6 1.425(17) .
C2 C3 1.436(17) .
C2 C7 1.497(17) .
C3 C4 1.407(17) .
C3 C8 1.508(16) .
C4 C5 1.405(16) .
C4 C9 1.519(16) .
C5 C6 1.426(17) .
C5 C10 1.491(18) .
C6 C11 1.528(16) .
C12 C13 1.411(17) .
C12 C16 1.424(16) .
C12 C17 1.519(17) .
C13 C14 1.393(17) .
C13 C18 1.524(16) .
C14 C15 1.406(15) .
C14 C19 1.507(17) .
C15 C16 1.390(16) .
C15 C20 1.526(15) .
C16 C21 1.512(16) .
C22 C23 1.493(16) .
C23 C24 1.547(17) .
C24 C25 1.517(16) .
C26 C27 1.494(15) .
C27 C28 1.517(17) .
C28 C29 1.500(16) .
