#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:45:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179490 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/87/4338772.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_4338772
loop_
_publ_author_name
'Lewis, Andrew J.'
'Mullane, Kimberly C.'
'Nakamaru-Ogiso, Eiko'
'Carroll, Patrick J.'
'Schelter, Eric J.'
_publ_section_title
;
 The inverse trans influence in a family of pentavalent uranium complexes.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6944
_journal_page_last               6953
_journal_paper_doi               10.1021/ic500833s
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C27 H74 N5 O Si6 U'
_chemical_formula_weight         891.48
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.896(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6978(8)
_cell_length_b                   12.8861(7)
_cell_length_c                   23.4364(13)
_cell_measurement_temperature    100(1)
_cell_volume                     4433.1(4)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            99101
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    3.848
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.830
_refine_diff_density_min         -2.168
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         10247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0448
_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)+(0.0437P)²+33.0790P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                8544
_reflns_number_total             10247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500833s_si_002.cif
_cod_data_source_block           2-CN
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

 Adding full bibliography for 4338771--4338772.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c     '
_cod_database_code               4338772
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 0.284787(13) 0.229643(18) 0.108038(8) 0.01995(7) Uani 1 1 d .
O1 O 0.2609(3) 0.3703(3) 0.11001(18) 0.0262(9) Uani 1 1 d .
N1 N 0.1679(3) 0.1870(4) 0.1635(2) 0.0277(11) Uani 1 1 d .
N2 N 0.4283(3) 0.2476(4) 0.1444(2) 0.0232(10) Uani 1 1 d .
N3 N 0.2571(3) 0.2164(4) 0.01157(19) 0.0230(10) Uani 1 1 d .
N4 N 0.3340(4) -0.0466(6) 0.1072(3) 0.0473(16) Uani 1 1 d .
N5 N 0.2156(3) 0.6721(4) 0.0991(2) 0.0277(11) Uani 1 1 d .
Si1 Si 0.06759(13) 0.25716(17) 0.15624(9) 0.0367(4) Uani 1 1 d .
Si2 Si 0.18175(13) 0.09624(16) 0.21849(7) 0.0329(4) Uani 1 1 d .
Si3 Si 0.44707(11) 0.33677(13) 0.20044(7) 0.0244(3) Uani 1 1 d .
Si4 Si 0.51975(11) 0.18148(14) 0.11785(7) 0.0239(3) Uani 1 1 d .
Si5 Si 0.29848(12) 0.31454(14) -0.03077(7) 0.0256(3) Uani 1 1 d .
Si6 Si 0.19375(12) 0.11507(14) -0.01899(7) 0.0271(4) Uani 1 1 d .
C1 C 0.0657(6) 0.3686(7) 0.2076(4) 0.051(2) Uani 1 1 d .
H1a H 0.0572 0.3428 0.2453 0.076 Uiso 1 1 calc R
H1b H 0.0165 0.4145 0.1964 0.076 Uiso 1 1 calc R
H1c H 0.1224 0.4056 0.2072 0.076 Uiso 1 1 calc R
C2 C -0.0373(5) 0.1755(8) 0.1645(4) 0.060(2) Uani 1 1 d .
H2a H -0.0416 0.1243 0.1348 0.090 Uiso 1 1 calc R
H2b H -0.0904 0.2191 0.1619 0.090 Uiso 1 1 calc R
H2c H -0.0334 0.1417 0.2010 0.090 Uiso 1 1 calc R
C3 C 0.0505(5) 0.3162(6) 0.0837(3) 0.0409(17) Uani 1 1 d .
H3a H 0.1028 0.3572 0.0756 0.061 Uiso 1 1 calc R
H3b H -0.0027 0.3594 0.0826 0.061 Uiso 1 1 calc R
H3c H 0.0428 0.2621 0.0557 0.061 Uiso 1 1 calc R
C4 C 0.1282(6) -0.0309(6) 0.1970(3) 0.0445(18) Uani 1 1 d .
H4a H 0.0635 -0.0221 0.1913 0.067 Uiso 1 1 calc R
H4b H 0.1407 -0.0812 0.2267 0.067 Uiso 1 1 calc R
H4c H 0.1530 -0.0546 0.1622 0.067 Uiso 1 1 calc R
C5 C 0.1298(7) 0.1406(8) 0.2858(3) 0.058(2) Uani 1 1 d .
H5a H 0.1612 0.2013 0.3001 0.088 Uiso 1 1 calc R
H5b H 0.1350 0.0864 0.3138 0.088 Uiso 1 1 calc R
H5c H 0.0667 0.1567 0.2778 0.088 Uiso 1 1 calc R
C6 C 0.3049(5) 0.0721(6) 0.2404(3) 0.0394(16) Uani 1 1 d .
H6a H 0.3175 -0.0008 0.2382 0.059 Uiso 1 1 calc R
H6b H 0.3169 0.0956 0.2789 0.059 Uiso 1 1 calc R
H6c H 0.3430 0.1092 0.2153 0.059 Uiso 1 1 calc R
C7 C 0.5343(5) 0.2914(6) 0.2564(3) 0.0383(17) Uani 1 1 d .
H7a H 0.5145 0.2274 0.2727 0.057 Uiso 1 1 calc R
H7b H 0.5414 0.3429 0.2859 0.057 Uiso 1 1 calc R
H7c H 0.5916 0.2808 0.2393 0.057 Uiso 1 1 calc R
C8 C 0.4860(4) 0.4645(5) 0.1718(3) 0.0296(13) Uani 1 1 d .
H8a H 0.5455 0.4565 0.1573 0.044 Uiso 1 1 calc R
H8b H 0.4884 0.5151 0.2019 0.044 Uiso 1 1 calc R
H8c H 0.4441 0.4871 0.1416 0.044 Uiso 1 1 calc R
C9 C 0.3407(5) 0.3570(5) 0.2396(3) 0.0329(14) Uani 1 1 d .
H9a H 0.2923 0.3783 0.2131 0.049 Uiso 1 1 calc R
H9b H 0.3511 0.4098 0.2681 0.049 Uiso 1 1 calc R
H9c H 0.3242 0.2934 0.2577 0.049 Uiso 1 1 calc R
C10 C 0.6225(4) 0.2677(6) 0.1101(3) 0.0372(15) Uani 1 1 d .
H10a H 0.6072 0.3227 0.0837 0.056 Uiso 1 1 calc R
H10b H 0.6716 0.2275 0.0960 0.056 Uiso 1 1 calc R
H10c H 0.6410 0.2966 0.1466 0.056 Uiso 1 1 calc R
C11 C 0.4927(4) 0.1280(5) 0.0442(2) 0.0280(13) Uani 1 1 d .
H11a H 0.4770 0.0559 0.0469 0.042 Uiso 1 1 calc R
H11b H 0.5450 0.1353 0.0216 0.042 Uiso 1 1 calc R
H11c H 0.4424 0.1655 0.0265 0.042 Uiso 1 1 calc R
C12 C 0.5553(5) 0.0701(5) 0.1650(3) 0.0339(15) Uani 1 1 d .
H12a H 0.5706 0.0951 0.2028 0.051 Uiso 1 1 calc R
H12b H 0.6074 0.0367 0.1501 0.051 Uiso 1 1 calc R
H12c H 0.5061 0.0212 0.1662 0.051 Uiso 1 1 calc R
C13 C 0.3443(5) 0.2662(6) -0.0987(3) 0.0391(16) Uani 1 1 d .
H13a H 0.3938 0.2194 -0.0901 0.059 Uiso 1 1 calc R
H13b H 0.3655 0.3239 -0.1203 0.059 Uiso 1 1 calc R
H13c H 0.2970 0.2307 -0.1207 0.059 Uiso 1 1 calc R
C14 C 0.3957(4) 0.3868(5) 0.0058(3) 0.0307(14) Uani 1 1 d .
H14a H 0.3769 0.4139 0.0415 0.046 Uiso 1 1 calc R
H14b H 0.4137 0.4429 -0.0181 0.046 Uiso 1 1 calc R
H14c H 0.4462 0.3404 0.0127 0.046 Uiso 1 1 calc R
C15 C 0.2087(5) 0.4143(6) -0.0490(3) 0.0385(16) Uani 1 1 d .
H15a H 0.1617 0.3838 -0.0735 0.058 Uiso 1 1 calc R
H15b H 0.2355 0.4715 -0.0683 0.058 Uiso 1 1 calc R
H15c H 0.1830 0.4385 -0.0146 0.058 Uiso 1 1 calc R
C16 C 0.1093(6) 0.1609(7) -0.0757(4) 0.055(2) Uani 1 1 d .
H16a H 0.0714 0.2136 -0.0603 0.082 Uiso 1 1 calc R
H16b H 0.0721 0.1036 -0.0889 0.082 Uiso 1 1 calc R
H16c H 0.1409 0.1890 -0.1070 0.082 Uiso 1 1 calc R
C17 C 0.2683(5) 0.0140(6) -0.0497(3) 0.0396(16) Uani 1 1 d .
H17a H 0.3070 0.0457 -0.0766 0.059 Uiso 1 1 calc R
H17b H 0.2311 -0.0379 -0.0688 0.059 Uiso 1 1 calc R
H17c H 0.3052 -0.0178 -0.0196 0.059 Uiso 1 1 calc R
C18 C 0.1209(5) 0.0465(5) 0.0333(3) 0.0344(15) Uani 1 1 d .
H18a H 0.1587 0.0218 0.0650 0.052 Uiso 1 1 calc R
H18b H 0.0905 -0.0111 0.0147 0.052 Uiso 1 1 calc R
H18c H 0.0764 0.0940 0.0467 0.052 Uiso 1 1 calc R
C19 C 0.3184(4) 0.0403(5) 0.1064(2) 0.0232(12) Uani 1 1 d .
C20 C 0.1857(5) 0.7639(6) 0.0631(3) 0.0381(16) Uani 1 1 d .
H20a H 0.2310 0.8183 0.0685 0.051 Uiso 1 1 calc R
H20b H 0.1290 0.7900 0.0769 0.051 Uiso 1 1 calc R
C21 C 0.1719(7) 0.7420(7) -0.0006(4) 0.060(3) Uani 1 1 d .
H21a H 0.2271 0.7145 -0.0148 0.090 Uiso 1 1 calc R
H21b H 0.1561 0.8052 -0.0204 0.090 Uiso 1 1 calc R
H21c H 0.1236 0.6924 -0.0069 0.090 Uiso 1 1 calc R
C22 C 0.3005(4) 0.6218(5) 0.0778(3) 0.0332(14) Uani 1 1 d .
H22a H 0.2877 0.5988 0.0389 0.044 Uiso 1 1 calc R
H22b H 0.3144 0.5608 0.1009 0.044 Uiso 1 1 calc R
C23 C 0.3844(5) 0.6912(6) 0.0791(3) 0.0402(16) Uani 1 1 d .
H23a H 0.3715 0.7523 0.0567 0.060 Uiso 1 1 calc R
H23b H 0.4342 0.6543 0.0637 0.060 Uiso 1 1 calc R
H23c H 0.4004 0.7109 0.1179 0.060 Uiso 1 1 calc R
C24 C 0.1419(4) 0.5862(5) 0.0960(3) 0.0380(16) Uani 1 1 d .
H24a H 0.1300 0.5672 0.0563 0.051 Uiso 1 1 calc R
H24b H 0.1659 0.5254 0.1160 0.051 Uiso 1 1 calc R
C25 C 0.0542(5) 0.6155(7) 0.1207(6) 0.075(3) Uani 1 1 d .
H25a H 0.0644 0.6305 0.1606 0.113 Uiso 1 1 calc R
H25b H 0.0118 0.5591 0.1160 0.113 Uiso 1 1 calc R
H25c H 0.0297 0.6759 0.1014 0.113 Uiso 1 1 calc R
C26 C 0.2304(5) 0.7111(6) 0.1592(3) 0.0368(16) Uani 1 1 d .
H26a H 0.1747 0.7440 0.1704 0.049 Uiso 1 1 calc R
H26b H 0.2774 0.7640 0.1597 0.049 Uiso 1 1 calc R
C27 C 0.2578(6) 0.6293(7) 0.2036(3) 0.049(2) Uani 1 1 d .
H27a H 0.2121 0.5761 0.2036 0.073 Uiso 1 1 calc R
H27b H 0.2636 0.6609 0.2407 0.073 Uiso 1 1 calc R
H27c H 0.3151 0.5992 0.1946 0.073 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'
Si Si 0.0817 0.0704 '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
O1 U1 N2 93.73(18)
O1 U1 N1 94.19(19)
N2 U1 N1 121.98(19)
O1 U1 N3 94.20(18)
N2 U1 N3 120.04(18)
N1 U1 N3 116.50(18)
O1 U1 C19 179.29(19)
N2 U1 C19 85.63(18)
N1 U1 C19 85.9(2)
N3 U1 C19 86.39(18)
O1 U1 Si3 73.50(13)
N2 U1 Si3 27.03(13)
N1 U1 Si3 104.94(13)
N3 U1 Si3 137.62(13)
C19 U1 Si3 105.80(13)
O1 U1 Si5 74.48(13)
N2 U1 Si5 103.13(13)
N1 U1 Si5 134.28(14)
N3 U1 Si5 26.53(13)
C19 U1 Si5 105.97(13)
Si3 U1 Si5 113.34(4)
O1 U1 Si1 73.25(14)
N2 U1 Si1 136.87(14)
N1 U1 Si1 26.01(15)
N3 U1 Si1 102.11(13)
C19 U1 Si1 107.01(14)
Si3 U1 Si1 112.12(4)
Si5 U1 Si1 112.00(5)
Si1 N1 Si2 119.3(3)
Si1 N1 U1 118.8(3)
Si2 N1 U1 121.4(3)
Si4 N2 Si3 119.6(3)
Si4 N2 U1 122.9(3)
Si3 N2 U1 117.4(2)
Si5 N3 Si6 120.5(3)
Si5 N3 U1 117.5(2)
Si6 N3 U1 122.0(3)
C26 N5 C20 106.7(5)
C26 N5 C22 111.7(5)
C20 N5 C22 111.9(5)
C26 N5 C24 110.6(5)
C20 N5 C24 110.6(5)
C22 N5 C24 105.4(5)
N1 Si1 C3 112.1(3)
N1 Si1 C1 112.2(3)
C3 Si1 C1 105.5(4)
N1 Si1 C2 113.3(4)
C3 Si1 C2 104.4(4)
C1 Si1 C2 108.8(4)
N1 Si1 U1 35.17(18)
C3 Si1 U1 80.1(2)
C1 Si1 U1 109.4(3)
C2 Si1 U1 138.6(3)
N1 Si2 C5 112.3(4)
N1 Si2 C4 110.9(3)
C5 Si2 C4 108.0(4)
N1 Si2 C6 112.8(3)
C5 Si2 C6 104.3(4)
C4 Si2 C6 108.3(4)
N2 Si3 C9 110.7(3)
N2 Si3 C8 110.2(3)
C9 Si3 C8 109.3(3)
N2 Si3 C7 113.2(3)
C9 Si3 C7 105.0(3)
C8 Si3 C7 108.2(3)
N2 Si3 U1 35.55(16)
C9 Si3 U1 78.1(2)
C8 Si3 U1 110.0(2)
C7 Si3 U1 138.0(2)
N2 Si4 C12 111.3(3)
N2 Si4 C11 112.2(3)
C12 Si4 C11 107.5(3)
N2 Si4 C10 112.6(3)
C12 Si4 C10 107.9(3)
C11 Si4 C10 105.0(3)
N3 Si5 C13 113.4(3)
N3 Si5 C14 112.4(3)
C13 Si5 C14 104.9(3)
N3 Si5 C15 111.5(3)
C13 Si5 C15 108.3(3)
C14 Si5 C15 106.0(3)
N3 Si5 U1 35.97(15)
C13 Si5 U1 137.7(3)
C14 Si5 U1 78.8(2)
C15 Si5 U1 111.0(2)
N3 Si6 C16 112.2(3)
N3 Si6 C17 111.7(3)
C16 Si6 C17 109.1(4)
N3 Si6 C18 113.2(3)
C16 Si6 C18 103.4(4)
C17 Si6 C18 106.7(3)
N4 C19 U1 178.1(5)
N5 C20 C21 115.1(6)
N5 C22 C23 115.0(6)
C25 C24 N5 114.7(6)
N5 C26 C27 115.5(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
U1 O1 1.847(4)
U1 N2 2.246(5)
U1 N1 2.273(5)
U1 N3 2.283(4)
U1 C19 2.491(7)
U1 Si3 3.4296(16)
U1 Si5 3.4476(16)
U1 Si1 3.4580(18)
N1 Si1 1.731(6)
N1 Si2 1.745(6)
N2 Si4 1.734(5)
N2 Si3 1.756(5)
N3 Si5 1.736(5)
N3 Si6 1.738(5)
N4 C19 1.142(9)
N5 C26 1.501(9)
N5 C20 1.505(8)
N5 C22 1.513(8)
N5 C24 1.547(8)
Si1 C3 1.868(8)
Si1 C1 1.874(8)
Si1 C2 1.885(8)
Si2 C5 1.875(8)
Si2 C4 1.876(8)
Si2 C6 1.882(8)
Si3 C9 1.870(7)
Si3 C8 1.877(7)
Si3 C7 1.881(6)
Si4 C12 1.870(7)
Si4 C11 1.882(6)
Si4 C10 1.891(7)
Si5 C13 1.867(7)
Si5 C14 1.876(7)
Si5 C15 1.876(7)
Si6 C16 1.868(7)
Si6 C17 1.870(7)
Si6 C18 1.887(7)
C20 C21 1.524(11)
C22 C23 1.523(10)
C24 C25 1.489(11)
C26 C27 1.522(11)
