#------------------------------------------------------------------------------
#$Date: 2016-03-24 13:58:10 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179647 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/00/4510002.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_4510002
loop_
_publ_author_name
'Parker, T. Gannon'
'Cross, Justin N.'
'Polinski, Matthew J.'
'Lin, Jian'
'Albrecht-Schmitt, Thomas E.'
_publ_section_title
;
 Ionothermal and Hydrothermal Flux Syntheses of Five New Uranyl
 Phosphonates
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              228
_journal_paper_doi               10.1021/cg401435w
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C9 H9 O11 P3 U, C6 H11 N2, H2O'
_chemical_formula_sum            'C15 H20 N2 O12 P3 U'
_chemical_formula_weight         751.27
_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                118.0820(10)
_cell_angle_beta                 90.8820(10)
_cell_angle_gamma                91.9230(10)
_cell_formula_units_Z            2
_cell_length_a                   8.8825(5)
_cell_length_b                   11.7704(7)
_cell_length_c                   12.1185(7)
_cell_measurement_reflns_used    6824
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.30
_cell_volume                     1116.51(11)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics
'SHELXP-97 (Sheldrick, 1997), CrystalMaker (Kohn, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '0.5° wide ω exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'I\ms microfocused'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20959
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    7.549
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sheltxprep
_exptl_crystal_colour            Yellow-green
_exptl_crystal_density_diffrn    2.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         6824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0306P)²+0.0636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                6491
_reflns_number_total             6824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401435w_si_002.cif
_cod_data_source_block           '[Emim][UPhDPO]'
_cod_database_code               4510002
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
U1 U 0.022447(9) 0.229699(8) 0.772216(8) 0.00669(3) Uani 1 1 d . . .
P1 P 0.17857(7) 0.06857(6) 0.93291(6) 0.00807(11) Uani 1 1 d . . .
P2 P 0.17559(7) 0.46110(6) 1.09194(6) 0.00760(11) Uani 1 1 d . . .
P3 P 0.17247(7) -0.09080(6) 0.54121(6) 0.00887(12) Uani 1 1 d . . .
O1 O -0.1303(2) 0.15894(18) 0.81501(18) 0.0108(3) Uani 1 1 d . . .
O2 O 0.1768(2) 0.29953(18) 0.73046(18) 0.0112(3) Uani 1 1 d . . .
O3 O 0.2016(2) 0.13969(17) 0.85898(16) 0.0089(3) Uani 1 1 d . . .
O6 O 0.0706(2) 0.37989(17) 0.98254(17) 0.0097(3) Uani 1 1 d . . .
O9 O 0.0806(2) 0.02225(17) 0.61737(17) 0.0105(3) Uani 1 1 d . . .
O7 O -0.1246(2) 0.40902(17) 0.81479(17) 0.0099(3) Uani 1 1 d . . .
O8 O 0.2064(2) 0.38420(18) 1.16715(18) 0.0122(4) Uani 1 1 d . . .
H17 H 0.1611 0.3115 1.1306 0.018 Uiso 1 1 calc R . .
O4 O 0.0998(2) 0.14287(17) 1.05598(17) 0.0104(3) Uani 1 1 d . . .
O5 O 0.0916(2) -0.06365(18) 0.84945(17) 0.0120(4) Uani 1 1 d . . .
H16 H 0.0341 -0.0816 0.8940 0.018 Uiso 1 1 calc R . .
O10 O 0.2051(2) -0.16580(19) 0.61828(18) 0.0145(4) Uani 1 1 d . . .
H18 H 0.1624 -0.1301 0.6870 0.022 Uiso 1 1 calc R . .
O11 O -0.1067(2) 0.19044(18) 0.58383(17) 0.0112(3) Uani 1 1 d . . .
C1 C 0.3576(3) 0.4835(2) 1.0405(2) 0.0100(5) Uani 1 1 d . . .
C2 C 0.4120(3) 0.6052(3) 1.0640(3) 0.0137(5) Uani 1 1 d . . .
H2 H 0.3523 0.6777 1.1075 0.016 Uiso 1 1 calc R . .
C4 C 0.3599(3) 0.0302(2) 0.9694(2) 0.0096(4) Uani 1 1 d . . .
C7 C 0.3560(3) -0.0384(3) 0.5176(2) 0.0105(5) Uani 1 1 d . . .
C5 C 0.3725(3) -0.0104(3) 1.0599(3) 0.0130(5) Uani 1 1 d . . .
H5 H 0.2852 -0.0178 1.1008 0.016 Uiso 1 1 calc R . .
C8 C 0.4288(3) -0.1119(3) 0.4064(2) 0.0128(5) Uani 1 1 d . . .
H8 H 0.3801 -0.1883 0.3426 0.015 Uiso 1 1 calc R . .
C6 C 0.4887(3) 0.0404(3) 0.9090(3) 0.0125(5) Uani 1 1 d . . .
H6 H 0.4811 0.0677 0.8469 0.015 Uiso 1 1 calc R . .
C3 C 0.5529(3) 0.6216(3) 1.0243(3) 0.0155(5) Uani 1 1 d . . .
H3 H 0.5890 0.7053 1.0414 0.019 Uiso 1 1 calc R . .
C9 C 0.4279(3) 0.0739(3) 0.6112(2) 0.0125(5) Uani 1 1 d . . .
H9 H 0.3787 0.1242 0.6869 0.015 Uiso 1 1 calc R . .
O1W O 0.1135(3) 0.5583(2) 1.4241(2) 0.0298(5) Uani 1 1 d . . .
C10 C 0.2538(4) -0.5621(4) 0.5806(4) 0.0340(9) Uani 1 1 d . . .
H10 H 0.1503 -0.5428 0.5866 0.041 Uiso 1 1 calc R A 1
C11 C 0.4983(5) -0.5625(6) 0.6024(6) 0.0552(15) Uani 1 1 d . . .
H11 H 0.5972 -0.5328 0.6375 0.066 Uiso 1 1 calc R B 1
N2 N 0.3179(12) -0.6757(8) 0.4910(10) 0.033(2) Uani 0.50 1 d P C 1
C12 C 0.4709(9) -0.6605(8) 0.5149(7) 0.0297(15) Uani 0.50 1 d P C 1
H12 H 0.5427 -0.7210 0.4671 0.036 Uiso 0.50 1 calc PR C 1
N1 N 0.3646(7) -0.4896(7) 0.6530(7) 0.0207(13) Uani 0.50 1 d P C 1
C15 C 0.2036(16) -0.3569(14) 0.8232(15) 0.026(2) Uani 0.50 1 d P C 1
H15A H 0.1194 -0.3676 0.7654 0.039 Uiso 0.50 1 calc PR C 1
H15B H 0.1983 -0.2739 0.8990 0.039 Uiso 0.50 1 calc PR C 1
H15C H 0.1978 -0.4269 0.8454 0.039 Uiso 0.50 1 calc PR C 1
C14 C 0.3462(9) -0.3604(7) 0.7628(7) 0.0284(15) Uani 0.50 1 d P C 1
H14A H 0.4310 -0.3406 0.8240 0.034 Uiso 0.50 1 calc PR C 1
H14B H 0.3489 -0.2937 0.7349 0.034 Uiso 0.50 1 calc PR C 1
C13 C 0.222(2) -0.774(3) 0.390(2) 0.099(11) Uani 0.50 1 d P C 1
H13A H 0.2178 -0.8528 0.3975 0.149 Uiso 0.50 1 calc PR C 1
H13B H 0.2635 -0.7913 0.3091 0.149 Uiso 0.50 1 calc PR C 1
H13C H 0.1201 -0.7423 0.3949 0.149 Uiso 0.50 1 calc PR C 1
N2' N 0.3096(10) -0.4607(8) 0.6937(8) 0.0354(17) Uani 0.50 1 d P C 2
C12' C 0.4548(12) -0.4801(10) 0.6928(9) 0.046(2) Uani 0.50 1 d P C 2
H12' H 0.5202 -0.4289 0.7630 0.055 Uiso 0.50 1 calc PR C 2
N1' N 0.3469(17) -0.6294(9) 0.5199(11) 0.052(3) Uani 0.50 1 d P C 2
C15' C 0.222(3) -0.814(2) 0.390(2) 0.072(8) Uani 0.50 1 d P C 2
H15D H 0.2022 -0.8194 0.4666 0.108 Uiso 0.50 1 calc PR C 2
H15E H 0.2275 -0.9014 0.3197 0.108 Uiso 0.50 1 calc PR C 2
H15F H 0.1415 -0.7695 0.3727 0.108 Uiso 0.50 1 calc PR C 2
C14' C 0.3379(18) -0.7570(16) 0.4023(13) 0.088(5) Uani 0.50 1 d P C 2
H14C H 0.3514 -0.7420 0.3292 0.106 Uiso 0.50 1 calc PR C 2
H14D H 0.4210 -0.8099 0.4047 0.106 Uiso 0.50 1 calc PR C 2
C13' C 0.231(3) -0.364(2) 0.794(2) 0.091(9) Uani 0.50 1 d P C 2
H13D H 0.1939 -0.3991 0.8485 0.136 Uiso 0.50 1 calc PR C 2
H13E H 0.1456 -0.3383 0.7604 0.136 Uiso 0.50 1 calc PR C 2
H13F H 0.2995 -0.2892 0.8428 0.136 Uiso 0.50 1 calc PR C 2
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'
P P 0.1023 0.0942 '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
O2 U1 O1 179.22(8) . .
O2 U1 O6 89.44(8) . .
O1 U1 O6 90.28(8) . .
O2 U1 O9 90.87(8) . .
O1 U1 O9 88.90(8) . .
O6 U1 O9 142.78(6) . .
O2 U1 O7 91.30(8) . .
O1 U1 O7 89.32(8) . .
O6 U1 O7 72.99(6) . .
O9 U1 O7 144.18(6) . .
O2 U1 O11 89.06(8) . .
O1 U1 O11 91.59(8) . .
O6 U1 O11 144.77(6) . .
O9 U1 O11 72.44(6) . .
O7 U1 O11 71.86(6) . .
O2 U1 O3 88.48(8) . .
O1 U1 O3 90.74(7) . .
O6 U1 O3 72.19(6) . .
O9 U1 O3 70.62(6) . .
O7 U1 O3 145.18(6) . .
O11 U1 O3 142.92(6) . .
O3 P1 O4 115.04(11) . .
O3 P1 O5 109.60(11) . .
O4 P1 O5 110.25(10) . .
O3 P1 C4 108.03(11) . .
O4 P1 C4 107.43(11) . .
O5 P1 C4 106.06(11) . .
O6 P2 O7 117.33(10) . 2_567
O6 P2 O8 108.50(11) . .
O7 P2 O8 106.56(11) 2_567 .
O6 P2 C1 110.97(11) . .
O7 P2 C1 108.08(11) 2_567 .
O8 P2 C1 104.57(11) . .
O9 P3 O11 117.56(11) . 2_556
O9 P3 O10 109.22(11) . .
O11 P3 O10 105.88(11) 2_556 .
O9 P3 C7 110.62(12) . .
O11 P3 C7 108.28(11) 2_556 .
O10 P3 C7 104.38(12) . .
P1 O3 U1 131.02(10) . .
P2 O6 U1 152.11(11) . .
P3 O9 U1 159.15(11) . .
P2 O7 U1 148.51(11) 2_567 .
P3 O11 U1 146.52(11) 2_556 .
C2 C1 C3 118.7(2) . 2_667
C2 C1 P2 120.86(19) . .
C3 C1 P2 120.4(2) 2_667 .
C3 C2 C1 120.4(2) . .
C5 C4 C6 119.5(2) . .
C5 C4 P1 119.11(19) . .
C6 C4 P1 121.39(19) . .
C8 C7 C9 119.7(2) . .
C8 C7 P3 119.9(2) . .
C9 C7 P3 120.39(19) . .
C6 C5 C4 120.7(2) 2_657 .
C9 C8 C7 120.3(2) 2_656 .
C5 C6 C4 119.8(2) 2_657 .
C2 C3 C1 120.9(2) . 2_667
C8 C9 C7 120.1(2) 2_656 .
N1' C10 N1 85.5(7) . .
N1' C10 N2' 113.5(8) . .
N1 C10 N2' 28.8(4) . .
N1' C10 N2 21.8(7) . .
N1 C10 N2 106.1(6) . .
N2' C10 N2 132.6(7) . .
C12' C11 C12 147.0(8) . .
C12' C11 N1 38.4(6) . .
C12 C11 N1 112.6(6) . .
C12' C11 N1' 103.3(8) . .
C12 C11 N1' 46.5(6) . .
N1 C11 N1' 66.2(6) . .
C12 N2 C10 107.2(7) . .
C12 N2 C13 133.2(11) . .
C10 N2 C13 119.2(12) . .
C11 C12 N2 109.1(7) . .
C10 N1 C11 105.0(6) . .
C10 N1 C14 123.9(6) . .
C11 N1 C14 131.1(7) . .
C15 C14 N1 111.1(8) . .
C12' N2' C10 103.6(8) . .
C12' N2' C13' 126.4(13) . .
C10 N2' C13' 129.8(12) . .
C11 C12' N2' 116.5(10) . .
C10 N1' C14' 131.9(13) . .
C10 N1' C11 102.8(8) . .
C14' N1' C11 124.9(13) . .
C15' C14' N1' 112.4(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.7742(18) .
U1 O1 1.7767(18) .
U1 O6 2.3405(18) .
U1 O9 2.3560(18) .
U1 O7 2.3680(18) .
U1 O11 2.3731(18) .
U1 O3 2.4230(18) .
P1 O3 1.4984(19) .
P1 O4 1.5245(19) .
P1 O5 1.5669(19) .
P1 C4 1.792(3) .
P2 O6 1.5001(19) .
P2 O7 1.5017(19) 2_567
P2 O8 1.585(2) .
P2 C1 1.797(3) .
P3 O9 1.4930(19) .
P3 O11 1.5056(19) 2_556
P3 O10 1.588(2) .
P3 C7 1.798(3) .
O7 P2 1.5017(18) 2_567
O11 P3 1.5056(19) 2_556
C1 C2 1.390(4) .
C1 C3 1.396(4) 2_667
C2 C3 1.387(4) .
C4 C5 1.392(4) .
C4 C6 1.399(3) .
C7 C8 1.396(4) .
C7 C9 1.396(4) .
C5 C6 1.387(4) 2_657
C8 C9 1.388(4) 2_656
C6 C5 1.387(4) 2_657
C3 C1 1.396(4) 2_667
C9 C8 1.388(4) 2_656
C10 N1' 1.169(14) .
C10 N1 1.296(8) .
C10 N2' 1.396(9) .
C10 N2 1.412(10) .
C11 C12' 1.152(11) .
C11 C12 1.156(10) .
C11 N1 1.456(8) .
C11 N1' 1.604(15) .
N2 C12 1.373(14) .
N2 C13 1.46(3) .
N1 C14 1.493(11) .
C15 C14 1.464(13) .
N2' C12' 1.316(12) .
N2' C13' 1.43(2) .
N1' C14' 1.506(16) .
C15' C14' 1.17(3) .
