#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:09:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179679 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/01/7000113.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_7000113
loop_
_publ_author_name
'Silva, Manuela'
'Antunes, Maria Augusta'
'Dias, Marta'
'Domingos, Angela'
'dos Santos, Isabel Cordeiro'
'Marçalo, Joaquim'
'Marques, Noémia'
_publ_section_title
;
 The uranium-nitrogen bond in U IV complexes supported by the
 hydrotris(3,5-dimethylpyrazolyl)borate ligand.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3353
_journal_page_last               3358
_journal_paper_doi               10.1039/b509229a
_journal_year                    2005
_chemical_formula_moiety         'C27 H32 B Cl2 N7 U'
_chemical_formula_sum            'C27 H32 B Cl2 N7 U'
_chemical_formula_weight         774.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.667(9)
_cell_angle_beta                 88.415(11)
_cell_angle_gamma                78.416(10)
_cell_formula_units_Z            2
_cell_length_a                   8.1647(11)
_cell_length_b                   10.2881(11)
_cell_length_c                   18.947(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      8
_cell_volume                     1510.2(3)
_computing_cell_refinement       'CAD4 Software (Enraf-Nonius,1994) '
_computing_data_collection       'CAD4 Software (Enraf-Nonius,1994) '
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  cad4
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_sigmaI/netI    0.2274
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5697
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.09
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    5.580
_exptl_absorpt_correction_T_max  0.4941
_exptl_absorpt_correction_T_min  0.3314
_exptl_absorpt_correction_type   'psi-scan (North,1968)'
_exptl_crystal_colour            'golden brown'
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.347
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5297
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1762
_refine_ls_R_factor_gt           0.0792
_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)+(0.0109P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                2849
_reflns_number_total             5297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b509229a.txt
_cod_data_source_block           utpclnph
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000113
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
U U 0.51066(9) 0.40175(6) 0.76331(4) 0.03462(18) Uani 1 1 d . . .
Cl1 Cl 0.7967(5) 0.2700(4) 0.7288(2) 0.0526(12) Uani 1 1 d . . .
Cl2 Cl 0.4010(5) 0.1976(4) 0.8476(2) 0.0613(13) Uani 1 1 d . . .
N11 N 0.2997(14) 0.5647(11) 0.8115(6) 0.035(3) Uani 1 1 d . . .
N12 N 0.3360(15) 0.6761(11) 0.8286(6) 0.041(3) Uani 1 1 d . . .
N21 N 0.6487(14) 0.4320(13) 0.8723(7) 0.045(4) Uani 1 1 d . . .
N22 N 0.6167(14) 0.5592(11) 0.8883(6) 0.038(3) Uani 1 1 d . . .
N31 N 0.6072(13) 0.6197(10) 0.7215(6) 0.032(3) Uani 1 1 d . . .
N32 N 0.5962(14) 0.7135(12) 0.7622(6) 0.044(3) Uani 1 1 d . . .
B B 0.522(2) 0.6903(18) 0.8377(10) 0.042(5) Uani 1 1 d . . .
H H 0.509(11) 0.766(8) 0.865(5) 0.01(3) Uiso 1 1 d . . .
C11 C 0.1311(17) 0.5830(16) 0.8084(8) 0.047(4) Uani 1 1 d . . .
C12 C 0.0626(17) 0.7005(14) 0.8255(7) 0.041(4) Uani 1 1 d . . .
H12 H -0.0509 0.7337 0.8297 0.049 Uiso 1 1 calc R . .
C13 C 0.192(2) 0.7635(14) 0.8358(7) 0.043(4) Uani 1 1 d . . .
C14 C 0.0399(16) 0.4811(11) 0.7887(7) 0.048(4) Uani 1 1 d U . .
H14A H 0.1201 0.4059 0.7790 0.072 Uiso 1 1 calc R . .
H14B H -0.0299 0.5255 0.7462 0.072 Uiso 1 1 calc R . .
H14C H -0.0279 0.4476 0.8286 0.072 Uiso 1 1 calc R . .
C15 C 0.1867(17) 0.8963(13) 0.8561(8) 0.072(6) Uani 1 1 d . . .
H15A H 0.2986 0.9106 0.8594 0.108 Uiso 1 1 calc R . .
H15B H 0.1342 0.8932 0.9022 0.108 Uiso 1 1 calc R . .
H15C H 0.1241 0.9701 0.8195 0.108 Uiso 1 1 calc R . .
C21 C 0.747(2) 0.3431(16) 0.9235(9) 0.056(5) Uani 1 1 d . . .
C22 C 0.7853(18) 0.4123(15) 0.9725(8) 0.054(5) Uani 1 1 d . . .
H22 H 0.8564 0.3739 1.0131 0.065 Uiso 1 1 calc R . .
C23 C 0.7031(18) 0.5454(17) 0.9526(8) 0.048(4) Uani 1 1 d . . .
C24 C 0.803(2) 0.1971(13) 0.9248(8) 0.076(6) Uani 1 1 d . . .
H24A H 0.7568 0.1787 0.8832 0.114 Uiso 1 1 calc R . .
H24B H 0.7659 0.1421 0.9685 0.114 Uiso 1 1 calc R . .
H24C H 0.9230 0.1755 0.9236 0.114 Uiso 1 1 calc R . .
C25 C 0.6970(18) 0.6649(14) 0.9864(7) 0.072(6) Uani 1 1 d . . .
H25A H 0.6264 0.7449 0.9569 0.107 Uiso 1 1 calc R . .
H25B H 0.8078 0.6817 0.9893 0.107 Uiso 1 1 calc R . .
H25C H 0.6529 0.6439 1.0345 0.107 Uiso 1 1 calc R . .
C31 C 0.6819(18) 0.6720(14) 0.6582(9) 0.038(4) Uani 1 1 d . . .
C32 C 0.7174(17) 0.7989(12) 0.6578(8) 0.047(4) Uani 1 1 d . . .
H32 H 0.7671 0.8558 0.6213 0.056 Uiso 1 1 calc R . .
C33 C 0.6613(17) 0.8207(13) 0.7247(8) 0.037(4) Uani 1 1 d . . .
C34 C 0.7135(17) 0.5979(12) 0.5994(7) 0.053(5) Uani 1 1 d . . .
H34A H 0.6763 0.5126 0.6143 0.080 Uiso 1 1 calc R . .
H34B H 0.8311 0.5804 0.5901 0.080 Uiso 1 1 calc R . .
H34C H 0.6535 0.6528 0.5558 0.080 Uiso 1 1 calc R . .
C35 C 0.6654(18) 0.9457(12) 0.7529(8) 0.065(5) Uani 1 1 d . . .
H35A H 0.6188 0.9342 0.8006 0.098 Uiso 1 1 calc R . .
H35B H 0.6010 1.0255 0.7205 0.098 Uiso 1 1 calc R . .
H35C H 0.7790 0.9567 0.7554 0.098 Uiso 1 1 calc R . .
N4 N 0.3590(13) 0.4565(10) 0.6605(6) 0.030(3) Uani 1 1 d . . .
C40 C 0.369(2) 0.3308(14) 0.6397(8) 0.040(4) Uani 1 1 d . . .
C41 C 0.2536(17) 0.2487(13) 0.6634(7) 0.042(4) Uani 1 1 d . . .
H41 H 0.1700 0.2764 0.6940 0.051 Uiso 1 1 calc R . .
C42 C 0.2564(19) 0.1275(15) 0.6440(9) 0.059(5) Uani 1 1 d . . .
H42 H 0.1768 0.0744 0.6606 0.071 Uiso 1 1 calc R . .
C43 C 0.380(2) 0.0892(15) 0.5997(9) 0.061(5) Uani 1 1 d . . .
H43 H 0.3827 0.0080 0.5860 0.073 Uiso 1 1 calc R . .
C44 C 0.501(2) 0.1625(16) 0.5738(9) 0.073(6) Uani 1 1 d . . .
H44 H 0.5839 0.1339 0.5432 0.088 Uiso 1 1 calc R . .
C45 C 0.4915(18) 0.2826(14) 0.5964(8) 0.053(5) Uani 1 1 d . . .
H45 H 0.5739 0.3335 0.5811 0.064 Uiso 1 1 calc R . .
C46 C 0.2610(18) 0.5720(14) 0.6124(8) 0.040(4) Uani 1 1 d . . .
C47 C 0.2339(16) 0.6987(12) 0.6295(8) 0.039(4) Uani 1 1 d . . .
H47 H 0.2785 0.7061 0.6726 0.047 Uiso 1 1 calc R . .
C48 C 0.141(2) 0.8132(13) 0.5830(8) 0.056(5) Uani 1 1 d . . .
H48 H 0.1225 0.8965 0.5958 0.067 Uiso 1 1 calc R . .
C49 C 0.0749(19) 0.8065(14) 0.5161(8) 0.056(5) Uani 1 1 d . . .
H49 H 0.0171 0.8850 0.4840 0.067 Uiso 1 1 calc R . .
C410 C 0.0972(18) 0.6829(15) 0.5000(8) 0.053(5) Uani 1 1 d . . .
H410 H 0.0501 0.6749 0.4575 0.064 Uiso 1 1 calc R . .
C411 C 0.1899(17) 0.5691(14) 0.5468(7) 0.040(4) Uani 1 1 d . . .
H411 H 0.2060 0.4859 0.5341 0.047 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'
B B 0.0013 0.0007 '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'
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
_geom_angle_publ_flag
N4 U N31 88.4(4) . . ?
N4 U N11 89.3(4) . . ?
N31 U N11 76.7(4) . . ?
N4 U N21 159.1(4) . . ?
N31 U N21 74.8(4) . . ?
N11 U N21 75.0(4) . . ?
N4 U Cl2 105.3(3) . . ?
N31 U Cl2 160.9(3) . . ?
N11 U Cl2 90.0(3) . . ?
N21 U Cl2 88.7(3) . . ?
N4 U Cl1 103.2(3) . . ?
N31 U Cl1 90.1(3) . . ?
N11 U Cl1 161.6(3) . . ?
N21 U Cl1 89.4(3) . . ?
Cl2 U Cl1 99.37(13) . . ?
N4 U C40 27.8(3) . . ?
N31 U C40 110.3(4) . . ?
N11 U C40 110.5(4) . . ?
N21 U C40 173.0(4) . . ?
Cl2 U C40 87.1(3) . . ?
Cl1 U C40 85.8(3) . . ?
C11 N11 N12 106.9(11) . . ?
C11 N11 U 128.7(10) . . ?
N12 N11 U 122.4(9) . . ?
N11 N12 C13 109.4(12) . . ?
N11 N12 B 121.3(12) . . ?
C13 N12 B 129.2(13) . . ?
C21 N21 N22 109.4(12) . . ?
C21 N21 U 131.0(10) . . ?
N22 N21 U 119.5(9) . . ?
C23 N22 N21 107.3(12) . . ?
C23 N22 B 127.8(13) . . ?
N21 N22 B 124.4(12) . . ?
N32 N31 C31 106.2(11) . . ?
N32 N31 U 123.4(9) . . ?
C31 N31 U 130.4(9) . . ?
C33 N32 N31 109.1(12) . . ?
C33 N32 B 129.0(13) . . ?
N31 N32 B 121.9(13) . . ?
N32 B N22 111.2(13) . . ?
N32 B N12 106.9(13) . . ?
N22 B N12 108.8(13) . . ?
C12 C11 N11 109.7(13) . . ?
C12 C11 C14 127.2(13) . . ?
N11 C11 C14 123.1(13) . . ?
C11 C12 C13 107.5(13) . . ?
N12 C13 C12 106.4(12) . . ?
N12 C13 C15 123.4(14) . . ?
C12 C13 C15 130.0(14) . . ?
N21 C21 C22 107.6(14) . . ?
N21 C21 C24 124.0(15) . . ?
C22 C21 C24 128.4(16) . . ?
C23 C22 C21 109.8(14) . . ?
C22 C23 N22 105.9(13) . . ?
C22 C23 C25 132.3(15) . . ?
N22 C23 C25 121.8(14) . . ?
N31 C31 C32 110.9(13) . . ?
N31 C31 C34 121.7(13) . . ?
C32 C31 C34 127.4(15) . . ?
C33 C32 C31 103.9(13) . . ?
N32 C33 C32 109.9(12) . . ?
N32 C33 C35 123.3(14) . . ?
C32 C33 C35 126.8(13) . . ?
C46 N4 C40 114.2(11) . . ?
C46 N4 U 140.2(8) . . ?
C40 N4 U 105.5(8) . . ?
C45 C40 C41 115.6(13) . . ?
C45 C40 N4 123.2(14) . . ?
C41 C40 N4 121.2(14) . . ?
C45 C40 U 111.5(10) . . ?
C41 C40 U 110.8(10) . . ?
N4 C40 U 46.6(6) . . ?
C40 C41 C42 123.3(14) . . ?
C43 C42 C41 117.1(15) . . ?
C42 C43 C44 124.2(16) . . ?
C43 C44 C45 115.5(16) . . ?
C40 C45 C44 124.2(16) . . ?
C47 C46 C411 116.4(14) . . ?
C47 C46 N4 119.4(13) . . ?
C411 C46 N4 124.2(13) . . ?
C48 C47 C46 120.6(14) . . ?
C47 C48 C49 121.3(13) . . ?
C410 C49 C48 118.4(14) . . ?
C49 C410 C411 119.8(14) . . ?
C410 C411 C46 123.5(14) . . ?
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
U N4 2.225(10) . ?
U N31 2.465(11) . ?
U N11 2.474(11) . ?
U N21 2.493(12) . ?
U Cl2 2.603(4) . ?
U Cl1 2.608(4) . ?
U C40 2.949(13) . ?
N11 C11 1.352(15) . ?
N11 N12 1.354(12) . ?
N12 C13 1.355(15) . ?
N12 B 1.575(19) . ?
N21 C21 1.317(16) . ?
N21 N22 1.389(13) . ?
N22 C23 1.388(15) . ?
N22 B 1.522(19) . ?
N31 N32 1.365(12) . ?
N31 C31 1.369(16) . ?
N32 C33 1.354(15) . ?
N32 B 1.52(2) . ?
C11 C12 1.338(16) . ?
C11 C14 1.521(16) . ?
C12 C13 1.387(17) . ?
C13 C15 1.500(16) . ?
C21 C22 1.378(17) . ?
C21 C24 1.473(16) . ?
C22 C23 1.363(17) . ?
C23 C25 1.512(16) . ?
C31 C32 1.391(16) . ?
C31 C34 1.488(16) . ?
C32 C33 1.391(17) . ?
C33 C35 1.516(15) . ?
N4 C46 1.417(15) . ?
N4 C40 1.430(14) . ?
C40 C45 1.372(18) . ?
C40 C41 1.380(18) . ?
C41 C42 1.381(15) . ?
C42 C43 1.354(18) . ?
C43 C44 1.369(19) . ?
C44 C45 1.393(16) . ?
C46 C47 1.393(15) . ?
C46 C411 1.395(17) . ?
C47 C48 1.378(16) . ?
C48 C49 1.414(17) . ?
C49 C410 1.357(15) . ?
C410 C411 1.377(16) . ?
