#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:40:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179198 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/36/4313640.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_4313640
loop_
_publ_author_name
'Leonor Maria'
'Ângela Domingos'
'Isabel Santos'
_publ_section_title
;
 Synthesis and Structural Characterization of Unprecedented Bis-Asymmetric
 Heteroscorpionate U(III) Complexes: [U{κ3-H2B(pztBu,Me)(pzMe,tBu)}2I]
 and [U{κ3-H2B(pztBu,Me)(pzMe2)}2I]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3323
_journal_page_last               3330
_journal_paper_doi               10.1021/ic026210p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '[UI{k3-H2B(pztBu,Me)(pzMe2)}2]'
_chemical_formula_sum            'C26 H44 B2 I N8 U'
_chemical_formula_weight         855.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 110.810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.762(2)
_cell_length_b                   10.2865(10)
_cell_length_c                   19.579(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      7.7
_cell_volume                     3343.9(7)
_computing_cell_refinement       'CAD4 sofware(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 sofware(Enraf-Nonius,1989)'
_computing_data_reduction        process-MoLEN(Fair,1990)
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  CAD4-Enraf-Nonius
_diffrn_measurement_method       ω/2\qscans
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0773
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7081
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        3.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.805
_exptl_absorpt_correction_T_max  0.100
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.453
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.00105(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6878
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0337P)²+14.4155P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                4398
_reflns_number_total             6878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026210psi20030121_040124_2.cif
_cod_data_source_block           ulassim
_cod_database_code               4313640
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
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
U1 U 0.11128(2) 0.62257(4) 0.25532(2) 0.03600(13) Uani 1 1 d . . .
I1 I 0.25937(5) 0.45948(10) 0.25903(5) 0.0741(3) Uani 1 1 d . . .
N1 N 0.0211(5) 0.4290(8) 0.2392(4) 0.041(2) Uani 1 1 d . . .
N2 N -0.0160(5) 0.7125(9) 0.1616(5) 0.051(2) Uani 1 1 d . . .
N3 N 0.0535(5) 0.7222(8) 0.3433(4) 0.040(2) Uani 1 1 d . . .
N4 N 0.1799(5) 0.8403(8) 0.2690(5) 0.047(2) Uani 1 1 d . . .
N11 N -0.0235(4) 0.4099(8) 0.1659(4) 0.041(2) Uani 1 1 d . . .
N21 N -0.0457(5) 0.6283(9) 0.1037(4) 0.046(2) Uani 1 1 d . . .
N31 N 0.1131(5) 0.7826(8) 0.3997(4) 0.042(2) Uani 1 1 d . . .
N41 N 0.2060(4) 0.8787(8) 0.3405(4) 0.0375(18) Uani 1 1 d . . .
C11 C -0.0758(6) 0.3132(11) 0.1597(6) 0.050(3) Uani 1 1 d . . .
C12 C -0.0667(6) 0.2685(10) 0.2271(6) 0.046(3) Uani 1 1 d . . .
H12 H -0.0962 0.2028 0.2385 0.055 Uiso 1 1 calc R . .
C13 C -0.0044(6) 0.3406(9) 0.2758(5) 0.040(2) Uani 1 1 d . . .
C21 C -0.1073(6) 0.6848(14) 0.0520(6) 0.060(4) Uani 1 1 d . . .
C22 C -0.1190(8) 0.8040(14) 0.0771(7) 0.076(4) Uani 1 1 d . . .
H22 H -0.1590 0.8633 0.0527 0.091 Uiso 1 1 calc R . .
C23 C -0.0600(8) 0.8209(13) 0.1460(7) 0.063(4) Uani 1 1 d . . .
C31 C 0.0810(7) 0.8357(10) 0.4466(5) 0.051(3) Uani 1 1 d . . .
C32 C -0.0010(7) 0.8108(12) 0.4180(6) 0.059(3) Uani 1 1 d . . .
H32 H -0.0389 0.8376 0.4378 0.071 Uiso 1 1 calc R . .
C33 C -0.0162(6) 0.7395(10) 0.3553(6) 0.047(3) Uani 1 1 d . . .
C41 C 0.2360(6) 0.9991(11) 0.3457(6) 0.051(3) Uani 1 1 d . . .
C42 C 0.2295(6) 1.0394(11) 0.2775(7) 0.056(3) Uani 1 1 d . . .
H42 H 0.2458 1.1191 0.2651 0.067 Uiso 1 1 calc R . .
C43 C 0.1944(6) 0.9392(12) 0.2307(6) 0.049(3) Uani 1 1 d . . .
C111 C -0.1296(7) 0.2655(13) 0.0869(7) 0.081(4) Uani 1 1 d . . .
H11A H -0.1222 0.3179 0.0493 0.122 Uiso 1 1 calc R . .
H11B H -0.1847 0.2710 0.0839 0.122 Uiso 1 1 calc R . .
H11C H -0.1166 0.1767 0.0807 0.122 Uiso 1 1 calc R . .
C131 C 0.0334(7) 0.3210(11) 0.3568(6) 0.054(3) Uani 1 1 d . . .
C132 C 0.1124(8) 0.3965(14) 0.3872(6) 0.081(4) Uani 1 1 d . . .
H13A H 0.1360 0.3829 0.4390 0.122 Uiso 1 1 calc R . .
H13B H 0.1021 0.4875 0.3774 0.122 Uiso 1 1 calc R . .
H13C H 0.1489 0.3665 0.3643 0.122 Uiso 1 1 calc R . .
C133 C -0.0233(9) 0.3667(16) 0.3954(7) 0.104(6) Uani 1 1 d . . .
H13D H 0.0020 0.3537 0.4471 0.157 Uiso 1 1 calc R . .
H13E H -0.0724 0.3176 0.3776 0.157 Uiso 1 1 calc R . .
H13F H -0.0350 0.4573 0.3856 0.157 Uiso 1 1 calc R . .
C134 C 0.0509(9) 0.1780(14) 0.3732(8) 0.094(5) Uani 1 1 d . . .
H13G H 0.0754 0.1658 0.4250 0.142 Uiso 1 1 calc R . .
H13H H 0.0868 0.1479 0.3498 0.142 Uiso 1 1 calc R . .
H13I H 0.0015 0.1297 0.3551 0.142 Uiso 1 1 calc R . .
C211 C -0.1535(7) 0.6199(16) -0.0194(6) 0.088(5) Uani 1 1 d . . .
H21A H -0.1308 0.5357 -0.0209 0.132 Uiso 1 1 calc R . .
H21B H -0.1503 0.6720 -0.0590 0.132 Uiso 1 1 calc R . .
H21C H -0.2088 0.6105 -0.0239 0.132 Uiso 1 1 calc R . .
C231 C -0.0443(8) 0.9325(12) 0.1967(8) 0.082(4) Uani 1 1 d . . .
H23A H 0.0013 0.9135 0.2399 0.122 Uiso 1 1 calc R . .
H23B H -0.0907 0.9482 0.2098 0.122 Uiso 1 1 calc R . .
H23C H -0.0331 1.0083 0.1733 0.122 Uiso 1 1 calc R . .
C311 C 0.1313(9) 0.9059(12) 0.5144(6) 0.080(4) Uani 1 1 d . . .
H31A H 0.1866 0.9054 0.5178 0.121 Uiso 1 1 calc R . .
H31B H 0.1267 0.8634 0.5563 0.121 Uiso 1 1 calc R . .
H31C H 0.1129 0.9941 0.5124 0.121 Uiso 1 1 calc R . .
C331 C -0.0936(6) 0.6898(14) 0.3037(7) 0.072(4) Uani 1 1 d . . .
H33A H -0.0843 0.6435 0.2649 0.108 Uiso 1 1 calc R . .
H33B H -0.1293 0.7614 0.2838 0.108 Uiso 1 1 calc R . .
H33C H -0.1173 0.6323 0.3291 0.108 Uiso 1 1 calc R . .
C411 C 0.2737(8) 1.0674(13) 0.4184(7) 0.080(4) Uani 1 1 d . . .
H41A H 0.2682 1.0141 0.4565 0.120 Uiso 1 1 calc R . .
H41B H 0.2470 1.1490 0.4171 0.120 Uiso 1 1 calc R . .
H41C H 0.3297 1.0825 0.4275 0.120 Uiso 1 1 calc R . .
C431 C 0.1776(8) 0.9356(15) 0.1499(6) 0.073(4) Uani 1 1 d . . .
C432 C 0.1576(11) 0.7980(18) 0.1227(7) 0.123(7) Uani 1 1 d . . .
H43A H 0.1469 0.7952 0.0711 0.185 Uiso 1 1 calc R . .
H43B H 0.1109 0.7692 0.1322 0.185 Uiso 1 1 calc R . .
H43C H 0.2023 0.7422 0.1475 0.185 Uiso 1 1 calc R . .
C433 C 0.1069(9) 1.024(2) 0.1079(9) 0.138(8) Uani 1 1 d . . .
H43D H 0.0975 1.0191 0.0566 0.207 Uiso 1 1 calc R . .
H43E H 0.1194 1.1122 0.1243 0.207 Uiso 1 1 calc R . .
H43F H 0.0595 0.9966 0.1166 0.207 Uiso 1 1 calc R . .
C434 C 0.2503(8) 0.9793(18) 0.1335(7) 0.109(6) Uani 1 1 d . . .
H43G H 0.2386 0.9756 0.0817 0.163 Uiso 1 1 calc R . .
H43H H 0.2949 0.9231 0.1579 0.163 Uiso 1 1 calc R . .
H43I H 0.2637 1.0669 0.1503 0.163 Uiso 1 1 calc R . .
B1 B -0.0053(7) 0.4966(13) 0.1102(6) 0.046(3) Uani 1 1 d D . .
H1A H 0.0524 0.5086 0.1249 0.055 Uiso 1 1 calc RD . .
H1B H -0.0240 0.4542 0.0628 0.055 Uiso 1 1 calc RD . .
B2 B 0.1981(7) 0.7802(13) 0.3972(6) 0.045(3) Uani 1 1 d D . .
H2A H 0.2100 0.6935 0.3844 0.054 Uiso 1 1 calc RD . .
H2B H 0.2367 0.8013 0.4451 0.054 Uiso 1 1 calc RD . .
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'
B B 0.0013 0.0007 '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
_geom_angle_publ_flag
N1 U1 N3 90.7(3) . . ?
N1 U1 N4 169.9(3) . . ?
N3 U1 N4 82.2(3) . . ?
N1 U1 N2 80.4(3) . . ?
N3 U1 N2 82.6(3) . . ?
N4 U1 N2 91.5(3) . . ?
N1 U1 I1 94.13(18) . . ?
N3 U1 I1 138.94(18) . . ?
N4 U1 I1 96.0(2) . . ?
N2 U1 I1 138.4(2) . . ?
N1 U1 B2 128.2(3) . . ?
N3 U1 B2 50.9(3) . . ?
N4 U1 B2 51.3(3) . . ?
N2 U1 B2 119.3(3) . . ?
I1 U1 B2 96.5(2) . . ?
N1 U1 B1 51.1(3) . . ?
N3 U1 B1 119.3(3) . . ?
N4 U1 B1 127.0(3) . . ?
N2 U1 B1 50.3(3) . . ?
I1 U1 B1 94.5(2) . . ?
B2 U1 B1 168.9(3) . . ?
C13 N1 N11 106.4(8) . . ?
C13 N1 U1 143.1(7) . . ?
N11 N1 U1 110.4(6) . . ?
C23 N2 N21 108.4(10) . . ?
C23 N2 U1 140.6(9) . . ?
N21 N2 U1 110.5(6) . . ?
C33 N3 N31 107.0(8) . . ?
C33 N3 U1 142.6(7) . . ?
N31 N3 U1 110.4(5) . . ?
C43 N4 N41 106.9(8) . . ?
C43 N4 U1 142.8(7) . . ?
N41 N4 U1 109.9(6) . . ?
C11 N11 N1 108.8(8) . . ?
C11 N11 B1 133.3(9) . . ?
N1 N11 B1 117.9(8) . . ?
C21 N21 N2 108.9(10) . . ?
C21 N21 B1 133.6(10) . . ?
N2 N21 B1 117.5(8) . . ?
C31 N31 N3 109.7(8) . . ?
C31 N31 B2 133.4(9) . . ?
N3 N31 B2 117.0(8) . . ?
C41 N41 N4 109.0(8) . . ?
C41 N41 B2 133.5(9) . . ?
N4 N41 B2 117.5(8) . . ?
N11 C11 C12 109.1(9) . . ?
N11 C11 C111 121.4(11) . . ?
C12 C11 C111 129.5(11) . . ?
C11 C12 C13 106.1(9) . . ?
N1 C13 C12 109.6(9) . . ?
N1 C13 C131 123.4(9) . . ?
C12 C13 C131 127.0(10) . . ?
N21 C21 C22 107.9(11) . . ?
N21 C21 C211 122.9(12) . . ?
C22 C21 C211 129.2(11) . . ?
C21 C22 C23 107.6(11) . . ?
N2 C23 C22 107.2(12) . . ?
N2 C23 C231 122.7(13) . . ?
C22 C23 C231 130.1(12) . . ?
N31 C31 C32 106.7(10) . . ?
N31 C31 C311 122.2(11) . . ?
C32 C31 C311 131.1(11) . . ?
C33 C32 C31 107.7(10) . . ?
N3 C33 C32 109.0(10) . . ?
N3 C33 C331 121.6(10) . . ?
C32 C33 C331 129.4(10) . . ?
N41 C41 C42 108.3(10) . . ?
N41 C41 C411 122.2(11) . . ?
C42 C41 C411 129.4(11) . . ?
C41 C42 C43 106.6(10) . . ?
N4 C43 C42 109.2(9) . . ?
N4 C43 C431 124.3(11) . . ?
C42 C43 C431 126.4(11) . . ?
C13 C131 C134 109.6(10) . . ?
C13 C131 C132 110.3(9) . . ?
C134 C131 C132 108.7(11) . . ?
C13 C131 C133 110.7(9) . . ?
C134 C131 C133 108.3(11) . . ?
C132 C131 C133 109.0(11) . . ?
C43 C431 C434 110.7(11) . . ?
C43 C431 C432 109.1(10) . . ?
C434 C431 C432 108.5(14) . . ?
C43 C431 C433 111.6(13) . . ?
C434 C431 C433 108.1(12) . . ?
C432 C431 C433 108.8(13) . . ?
N21 B1 N11 111.5(8) . . ?
N21 B1 U1 81.2(6) . . ?
N11 B1 U1 80.4(5) . . ?
N31 B2 N41 110.9(8) . . ?
N31 B2 U1 81.7(6) . . ?
N41 B2 U1 81.0(5) . . ?
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
U1 N1 2.504(8) . ?
U1 N3 2.516(8) . ?
U1 N4 2.519(8) . ?
U1 N2 2.527(8) . ?
U1 I1 3.0989(9) . ?
U1 B2 3.111(12) . ?
U1 B1 3.141(11) . ?
N1 C13 1.332(11) . ?
N1 N11 1.386(10) . ?
N2 C23 1.334(14) . ?
N2 N21 1.375(12) . ?
N3 C33 1.350(12) . ?
N3 N31 1.377(10) . ?
N4 C43 1.341(12) . ?
N4 N41 1.368(10) . ?
N11 C11 1.337(13) . ?
N11 B1 1.530(14) . ?
N21 C21 1.331(12) . ?
N21 B1 1.517(15) . ?
N31 C31 1.355(12) . ?
N31 B2 1.528(14) . ?
N41 C41 1.337(13) . ?
N41 B2 1.546(14) . ?
C11 C12 1.351(14) . ?
C11 C111 1.489(14) . ?
C12 C13 1.391(13) . ?
C13 C131 1.500(14) . ?
C21 C22 1.365(18) . ?
C21 C211 1.502(16) . ?
C22 C23 1.394(18) . ?
C23 C231 1.478(17) . ?
C31 C32 1.386(15) . ?
C31 C311 1.496(16) . ?
C32 C33 1.373(15) . ?
C33 C331 1.477(15) . ?
C41 C42 1.364(14) . ?
C41 C411 1.513(15) . ?
C42 C43 1.372(15) . ?
C43 C431 1.504(15) . ?
C131 C134 1.513(17) . ?
C131 C132 1.528(16) . ?
C131 C133 1.531(16) . ?
C431 C434 1.505(16) . ?
C431 C432 1.51(2) . ?
C431 C433 1.533(19) . ?
