#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:35:12 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179797 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/93/7009357.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_7009357
loop_
_publ_author_name
'Venkateswara Rao, P.'
'Rao, Chebrolu P.'
'Sreedhara, Alavattam'
'Wegelius, Elina K.'
'Rissanen, Kari'
'Kolehmainen, Erkki'
_publ_section_title
;
 Synthesis, structure and reactivity of trans-UO22+ complexes of
 OH-containing ligands †
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1213
_journal_paper_doi               10.1039/b000142m
_journal_year                    2000
_chemical_formula_sum            'C17 H25 Br N3 O7 U'
_chemical_formula_weight         701.34
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_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           SHELXL
_cell_angle_alpha                90.000(14)
_cell_angle_beta                 107.86(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   8.142(2)
_cell_length_b                   25.595(5)
_cell_length_c                   10.927(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2167.4(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4093
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    9.374
_exptl_crystal_density_diffrn    2.149
_exptl_crystal_F_000             1324
_refine_diff_density_max         1.940
_refine_diff_density_min         -3.397
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.153
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_restrained_S_obs      1.153
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_obs          0.0486
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0767P)²+19.2521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1308
_refine_ls_wR_factor_obs         0.1254
_reflns_number_observed          3103
_reflns_number_total             3812
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000142m.txt
_cod_data_source_block           6.
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+19.2521P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+19.2521P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2167.5(8)
_cod_database_code               7009357
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
U1 U 0.45891(5) 0.47584(2) 0.15727(3) 0.0207(2) Uani 1 d . .
O3 O 0.2972(9) 0.4324(3) 0.0635(7) 0.029(2) Uani 1 d . .
O5 O 0.2419(9) 0.5283(3) 0.2106(7) 0.028(2) Uani 1 d . .
O4 O 0.6238(10) 0.5171(3) 0.2533(8) 0.038(2) Uani 1 d . .
N1 N 0.6749(10) 0.3986(3) 0.2226(7) 0.020(2) Uani 1 d . .
N2 N 0.0713(11) 0.5624(4) 0.3197(8) 0.025(2) Uani 1 d . .
O1 O 0.4250(12) 0.4346(4) 0.3308(8) 0.060(3) Uani 1 d . .
C6 C 0.6240(12) 0.3682(4) 0.4214(9) 0.021(2) Uani 1 d . .
C7 C 0.7026(13) 0.3670(4) 0.3177(9) 0.022(2) Uani 1 d . .
H7 H 0.7814(13) 0.3403(4) 0.3212(9) 0.026 Uiso 1 calc R .
C5 C 0.6901(14) 0.3332(5) 0.5226(10) 0.027(2) Uani 1 d . .
H5 H 0.7777(14) 0.3102(5) 0.5208(10) 0.033 Uiso 1 calc R .
C12 C 0.1978(14) 0.5334(4) 0.3107(10) 0.024(2) Uani 1 d . .
H12 H 0.2603(14) 0.5150(4) 0.3835(10) 0.029 Uiso 1 calc R .
O2 O 0.6101(10) 0.4613(3) 0.0093(7) 0.026(2) Uani 1 d . .
C1 C 0.4921(14) 0.4030(5) 0.4261(9) 0.029(2) Uani 1 d . .
C3 C 0.4998(14) 0.3673(5) 0.6330(10) 0.029(2) Uani 1 d . .
H3 H 0.4621(14) 0.3680(5) 0.7052(10) 0.034 Uiso 1 calc R .
C9 C 0.6613(15) 0.4073(5) 0.0001(10) 0.031(3) Uani 1 d . .
H9A H 0.7217(15) 0.4042(5) -0.0635(10) 0.038 Uiso 1 calc R .
H9B H 0.5604(15) 0.3849(5) -0.0253(10) 0.038 Uiso 1 calc R .
C2 C 0.4299(15) 0.4011(5) 0.5320(10) 0.034(3) Uani 1 d . .
H2 H 0.3398(15) 0.4230(5) 0.5343(10) 0.041 Uiso 1 calc R .
C13 C -0.0329(15) 0.5928(5) 0.2112(11) 0.037(3) Uani 1 d . .
H13A H -0.1195(15) 0.6116(5) 0.2361(11) 0.056 Uiso 1 calc R .
H13B H -0.0874(15) 0.5697(5) 0.1412(11) 0.056 Uiso 1 calc R .
H13C H 0.0395(15) 0.6170(5) 0.1847(11) 0.056 Uiso 1 calc R .
C4 C 0.6247(16) 0.3329(4) 0.6260(10) 0.030(3) Uani 1 d . .
C10 C 0.9327(14) 0.4266(6) 0.1735(11) 0.039(3) Uani 1 d . .
H10A H 0.9916(14) 0.4267(6) 0.1086(11) 0.047 Uiso 1 calc R 1
H10B H 0.8948(14) 0.4620(6) 0.1817(11) 0.047 Uiso 1 calc R 1
O6A O 1.0456(13) 0.4109(5) 0.2892(10) 0.053(3) Uani 0.80 d P 1
H6A H 1.1419(18) 0.4225(13) 0.2966(19) 0.080 Uiso 0.80 calc PR 1
O6B O 0.9622(35) 0.3134(5) 0.2189(17) 0.043(11) Uani 0.20 d PR 2
H6B H 1.0305(36) 0.3365(5) 0.2535(16) 0.064 Uiso 0.20 calc PR 2
C11 C 0.8310(16) 0.3345(5) 0.1172(11) 0.039(3) Uani 1 d . .
H11A H 0.7294(16) 0.3127(5) 0.1034(11) 0.047 Uiso 1 calc R 2
H11B H 0.8663(16) 0.3322(5) 0.0402(11) 0.047 Uiso 1 calc R 2
C8 C 0.7788(13) 0.3913(5) 0.1315(9) 0.026(2) Uani 1 d . .
C14 C 0.0188(15) 0.5637(5) 0.4352(11) 0.036(3) Uani 1 d . .
H14A H -0.0764(15) 0.5874(5) 0.4228(11) 0.054 Uiso 1 calc R .
H14B H 0.1137(15) 0.5753(5) 0.5063(11) 0.054 Uiso 1 calc R .
H14C H -0.0156(15) 0.5294(5) 0.4527(11) 0.054 Uiso 1 calc R .
Br1 Br 0.7205(2) 0.28676(5) 0.76636(12) 0.0460(4) Uani 1 d . .
N3 N 0.2445(13) 0.2420(5) 0.4827(11) 0.048(3) Uani 1 d . .
C15 C 0.1528(25) 0.2823(8) 0.4952(23) 0.094(8) Uani 1 d . .
H15 H 0.1486(25) 0.3106(8) 0.4409(23) 0.112 Uiso 1 calc R .
C16 C 0.3358(32) 0.2427(10) 0.3874(19) 0.106(8) Uani 1 d . .
H16A H 0.3965(32) 0.2103(10) 0.3908(19) 0.159 Uiso 1 calc R .
H16B H 0.4166(32) 0.2711(10) 0.4052(19) 0.159 Uiso 1 calc R .
H16C H 0.2546(32) 0.2471(10) 0.3034(19) 0.159 Uiso 1 calc R .
C17 C 0.2680(25) 0.1957(6) 0.5592(18) 0.074(5) Uani 1 d . .
H17A H 0.3405(25) 0.1717(6) 0.5319(18) 0.111 Uiso 1 calc R .
H17B H 0.1579(25) 0.1797(6) 0.5492(18) 0.111 Uiso 1 calc R .
H17C H 0.3214(25) 0.2045(6) 0.6479(18) 0.111 Uiso 1 calc R .
O7 O 0.0719(21) 0.2860(9) 0.5724(21) 0.149(9) Uani 1 d . .
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'
O O 0.0106 0.0060 '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'
Br Br -0.2901 2.4595 '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
O4 U1 O3 178.0(4) . . ?
O4 U1 O1 92.7(4) . . ?
O3 U1 O1 86.1(4) . . ?
O4 U1 O2 92.3(3) . . ?
O3 U1 O2 87.5(3) . . ?
O1 U1 O2 136.9(3) . . ?
O4 U1 O2 90.5(4) . 3_665 ?
O3 U1 O2 91.3(3) . 3_665 ?
O1 U1 O2 154.5(3) . 3_665 ?
O2 U1 O2 68.2(3) . 3_665 ?
O4 U1 O5 90.2(3) . . ?
O3 U1 O5 91.1(3) . . ?
O1 U1 O5 76.8(3) . . ?
O2 U1 O5 145.9(3) . . ?
O2 U1 O5 77.8(2) 3_665 . ?
O4 U1 N1 88.0(3) . . ?
O3 U1 N1 90.1(3) . . ?
O1 U1 N1 70.2(3) . . ?
O2 U1 N1 67.3(2) . . ?
O2 U1 N1 135.3(2) 3_665 . ?
O5 U1 N1 146.8(2) . . ?
O4 U1 U1 91.7(3) . 3_665 ?
O3 U1 U1 89.3(2) . 3_665 ?
O1 U1 U1 170.4(2) . 3_665 ?
O2 U1 U1 34.3(2) . 3_665 ?
O2 U1 U1 33.9(2) 3_665 3_665 ?
O5 U1 U1 111.7(2) . 3_665 ?
N1 U1 U1 101.5(2) . 3_665 ?
C12 O5 U1 133.5(7) . . ?
C7 N1 C8 117.6(8) . . ?
C7 N1 U1 129.8(6) . . ?
C8 N1 U1 112.6(6) . . ?
C12 N2 C14 122.1(10) . . ?
C12 N2 C13 121.5(9) . . ?
C14 N2 C13 116.3(9) . . ?
C1 O1 U1 146.5(7) . . ?
C5 C6 C1 119.3(9) . . ?
C5 C6 C7 116.5(9) . . ?
C1 C6 C7 124.1(9) . . ?
N1 C7 C6 127.2(9) . . ?
C4 C5 C6 119.9(10) . . ?
O5 C12 N2 124.7(10) . . ?
C9 O2 U1 114.9(5) . . ?
C9 O2 U1 126.8(6) . 3_665 ?
U1 O2 U1 111.8(3) . 3_665 ?
O1 C1 C2 121.0(10) . . ?
O1 C1 C6 120.2(9) . . ?
C2 C1 C6 118.7(10) . . ?
C4 C3 C2 119.4(9) . . ?
O2 C9 C8 107.6(9) . . ?
C3 C2 C1 121.3(10) . . ?
C3 C4 C5 121.3(10) . . ?
C3 C4 Br1 118.9(7) . . ?
C5 C4 Br1 119.7(9) . . ?
O6A C10 C8 111.4(11) . . ?
O6B C11 C8 117.0(12) . . ?
C10 C8 N1 108.1(9) . . ?
C10 C8 C9 110.6(9) . . ?
N1 C8 C9 105.9(8) . . ?
C10 C8 C11 111.8(10) . . ?
N1 C8 C11 114.5(9) . . ?
C9 C8 C11 105.8(9) . . ?
C15 N3 C17 124.9(17) . . ?
C15 N3 C16 120.0(19) . . ?
C17 N3 C16 115.0(15) . . ?
O7 C15 N3 125.4(23) . . ?
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 O4 1.777(8) . ?
U1 O3 1.787(7) . ?
U1 O1 2.259(8) . ?
U1 O2 2.343(7) . ?
U1 O2 2.365(7) 3_665 ?
U1 O5 2.429(7) . ?
U1 N1 2.596(8) . ?
U1 U1 3.8989(9) 3_665 ?
O5 C12 1.258(12) . ?
N1 C7 1.282(13) . ?
N1 C8 1.502(11) . ?
N2 C12 1.298(14) . ?
N2 C14 1.451(13) . ?
N2 C13 1.454(14) . ?
O1 C1 1.299(13) . ?
C6 C5 1.396(15) . ?
C6 C1 1.410(15) . ?
C6 C7 1.462(13) . ?
C5 C4 1.389(13) . ?
O2 C9 1.456(14) . ?
O2 U1 2.365(7) 3_665 ?
C1 C2 1.399(14) . ?
C3 C4 1.37(2) . ?
C3 C2 1.38(2) . ?
C9 C8 1.517(15) . ?
C4 Br1 1.902(11) . ?
C10 O6A 1.38(2) . ?
C10 C8 1.50(2) . ?
O6B C11 1.39(2) . ?
C11 C8 1.54(2) . ?
N3 C15 1.30(2) . ?
N3 C17 1.43(2) . ?
N3 C16 1.45(2) . ?
C15 O7 1.22(3) . ?
