#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:41:07 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185311 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/92/7039201.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_7039201
loop_
_publ_author_name
'Zheng, Tao'
'Gao, Yang'
'Gui, Daxiang'
'Chen, Lanhua'
'Sheng, Daopeng'
'Diwu, Juan'
'Chai, Zhifang'
'Albrecht-Schmitt, Thomas E'
'Wang, Shuao'
_publ_section_title
;
 Atypical temperature-dependence of symmetry transformation observed in a
 uranyl phosphonate.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9031
_journal_page_last               9035
_journal_paper_doi               10.1039/c6dt01011c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C12 H11 O16 P4 U2, C4 H12 N'
_chemical_formula_sum            'C16 H23 N O16 P4 U2'
_chemical_formula_weight         1085.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-04-05 deposited with the CCDC.
2016-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7287(17)
_cell_length_b                   15.1632(14)
_cell_length_c                   9.0568(8)
_cell_measurement_reflns_used    9686
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.46
_cell_volume                     2709.3(4)
_computing_cell_refinement       'SMART (Bruker)'
_computing_data_collection       'SMART (Bruker)'
_computing_data_reduction        'SMART (Bruker)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Aperx II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            63489
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         2.463
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    12.251
_exptl_absorpt_correction_T_max  0.613
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.661
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0299P)²+8.3388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2825
_reflns_number_total             3245
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01011c2.cif
_cod_data_source_block           1-98K
_cod_depositor_comments
'Adding full bibliography for 7039201--7039202.cif.'
_cod_database_code               7039201
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.193
_shelx_estimated_absorpt_t_max   0.640
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
'x-1/2, y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.13238(2) 0.03776(2) 0.50298(2) 0.00855(6) Uani 1 1 d . . . . .
P1 P 0.20758(4) 0.06590(6) 0.86816(10) 0.01152(17) Uani 1 1 d . . . . .
P2 P 0.01508(4) -0.06843(6) 0.25515(9) 0.01101(17) Uani 1 1 d . . . . .
O1 O 0.19244(12) 0.08427(16) 0.7077(3) 0.0161(5) Uani 1 1 d . . . . .
O2 O 0.27095(12) 0.01210(16) 0.8926(3) 0.0160(5) Uani 1 1 d . . . . .
O3 O 0.14950(13) 0.01247(17) 0.9437(3) 0.0189(5) Uani 1 1 d . . . . .
H3 H 0.1122 0.0264 0.9057 0.028 Uiso 1 1 calc R U . . .
O4 O 0.06585(12) 0.00162(16) 0.3019(3) 0.0142(5) Uani 1 1 d . . . . .
O5 O -0.03901(12) -0.08723(15) 0.3699(3) 0.0139(5) Uani 1 1 d . . . . .
O6 O -0.02031(12) -0.04234(16) 0.1081(3) 0.0150(5) Uani 1 1 d . . . . .
H6 H 0.0092 -0.0298 0.0446 0.022 Uiso 0.5 1 calc R U P . .
O7 O 0.11991(13) -0.06864(16) 0.5799(3) 0.0177(5) Uani 1 1 d . . . . .
O8 O 0.14378(12) 0.14346(16) 0.4243(3) 0.0154(5) Uani 1 1 d . . . . .
C1 C 0.2059(2) 0.2500 0.8879(5) 0.0118(9) Uani 1 2 d S T P . .
H1 H 0.1943 0.2500 0.7861 0.014 Uiso 1 2 calc R U P . .
C2 C 0.21448(17) 0.1697(2) 0.9626(4) 0.0128(6) Uani 1 1 d . . . . .
C3 C 0.23008(18) 0.1708(2) 1.1127(4) 0.0166(7) Uani 1 1 d . . . . .
H3A H 0.2360 0.1167 1.1640 0.020 Uiso 1 1 calc R U . . .
C4 C 0.2371(3) 0.2500 1.1882(6) 0.0178(10) Uani 1 2 d S T P . .
H4 H 0.2467 0.2500 1.2910 0.021 Uiso 1 2 calc R U P . .
C5 C 0.0273(2) -0.2500 0.2470(5) 0.0127(9) Uani 1 2 d S T P . .
H5 H -0.0190 -0.2500 0.2757 0.015 Uiso 1 2 calc R U P . .
C6 C 0.06036(17) -0.1701(2) 0.2265(4) 0.0121(6) Uani 1 1 d . . . . .
C7 C 0.12818(16) -0.1706(2) 0.1818(4) 0.0147(7) Uani 1 1 d . . . . .
H7 H 0.1516 -0.1165 0.1674 0.018 Uiso 1 1 calc R U . . .
C8 C 0.1612(2) -0.2500 0.1585(5) 0.0153(10) Uani 1 2 d S T P . .
H8 H 0.2070 -0.2500 0.1262 0.018 Uiso 1 2 calc R U P . .
C10 C 0.4889(3) 0.2500 0.1089(6) 0.0322(14) Uani 1 2 d S T P A .
H10A H 0.5296 0.2811 0.0753 0.048 Uiso 0.5 1 calc R U P . .
H10B H 0.4485 0.2798 0.0705 0.048 Uiso 0.5 1 calc R U P . .
H10C H 0.4899 0.1891 0.0729 0.048 Uiso 0.5 1 calc R U P . .
C9 C 0.4300(6) 0.1886(8) 0.3284(10) 0.042(3) Uani 0.5 1 d . . P A -1
H9A H 0.4331 0.1821 0.4358 0.063 Uiso 0.5 1 calc R U P A -1
H9B H 0.4348 0.1307 0.2815 0.063 Uiso 0.5 1 calc R U P A -1
H9C H 0.3859 0.2140 0.3023 0.063 Uiso 0.5 1 calc R U P A -1
C11 C 0.5529(5) 0.2103(6) 0.3389(9) 0.034(2) Uani 0.5 1 d . . P A -1
H11A H 0.5506 0.2112 0.4470 0.052 Uiso 0.5 1 calc R U P A -1
H11B H 0.5918 0.2452 0.3058 0.052 Uiso 0.5 1 calc R U P A -1
H11C H 0.5580 0.1493 0.3049 0.052 Uiso 0.5 1 calc R U P A -1
C12 C 0.4796(8) 0.3367(6) 0.3237(10) 0.044(3) Uani 0.5 1 d . . P A -1
H12A H 0.5151 0.3735 0.2795 0.066 Uiso 0.5 1 calc R U P A -1
H12B H 0.4838 0.3382 0.4315 0.066 Uiso 0.5 1 calc R U P A -1
H12C H 0.4350 0.3592 0.2948 0.066 Uiso 0.5 1 calc R U P A -1
N1 N 0.4868(2) 0.2500 0.2741(5) 0.0185(9) Uani 1 2 d S T P . .
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
O8 U1 O7 179.11(12) . .
O8 U1 O2 91.00(10) . 4_554
O7 U1 O2 89.23(10) . 4_554
O8 U1 O5 90.46(10) . 5_556
O7 U1 O5 89.37(10) . 5_556
O2 U1 O5 175.89(9) 4_554 5_556
O8 U1 O1 88.94(10) . .
O7 U1 O1 91.91(11) . .
O2 U1 O1 91.37(9) 4_554 .
O5 U1 O1 84.81(9) 5_556 .
O8 U1 O4 88.25(10) . .
O7 U1 O4 90.88(10) . .
O2 U1 O4 92.92(9) 4_554 .
O5 U1 O4 90.97(8) 5_556 .
O1 U1 O4 174.91(8) . .
O2 P1 O1 113.89(15) . .
O2 P1 O3 105.26(15) . .
O1 P1 O3 111.85(15) . .
O2 P1 C2 109.94(15) . .
O1 P1 C2 108.15(15) . .
O3 P1 C2 107.57(16) . .
O5 P2 O4 113.84(14) . .
O5 P2 O6 108.60(14) . .
O4 P2 O6 110.88(14) . .
O5 P2 C6 106.67(14) . .
O4 P2 C6 108.16(15) . .
O6 P2 C6 108.49(15) . .
P1 O1 U1 144.85(15) . .
P1 O2 U1 159.34(16) . 4
P1 O3 H3 109.5 . .
P2 O4 U1 139.40(14) . .
P2 O5 U1 147.77(14) . 5_556
P2 O6 H6 109.5 . .
C2 C1 C2 120.4(5) . 7_565
C2 C1 H1 119.8 . .
C2 C1 H1 119.8 7_565 .
C3 C2 C1 119.1(3) . .
C3 C2 P1 119.4(3) . .
C1 C2 P1 121.4(3) . .
C4 C3 C2 120.8(3) . .
C4 C3 H3A 119.6 . .
C2 C3 H3A 119.6 . .
C3 C4 C3 119.7(5) 7_565 .
C3 C4 H4 120.1 7_565 .
C3 C4 H4 120.1 . .
C6 C5 C6 121.5(4) 7 .
C6 C5 H5 119.3 7 .
C6 C5 H5 119.3 . .
C5 C6 C7 119.0(3) . .
C5 C6 P2 119.6(3) . .
C7 C6 P2 121.4(3) . .
C8 C7 C6 119.9(3) . .
C8 C7 H7 120.1 . .
C6 C7 H7 120.1 . .
C7 C8 C7 120.8(5) . 7
C7 C8 H8 119.6 . .
C7 C8 H8 119.6 7 .
N1 C10 H10A 109.5 . .
N1 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
N1 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N1 C9 H9A 109.5 . .
N1 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N1 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N1 C11 H11A 109.5 . .
N1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N1 C12 H12A 109.5 . .
N1 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N1 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C12 N1 C10 108.9(4) . .
C12 N1 C9 113.2(9) . .
C10 N1 C9 109.8(5) . .
C12 N1 C11 109.2(7) . .
C10 N1 C11 110.8(5) . .
C9 N1 C11 104.9(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O8 1.768(2) .
U1 O7 1.775(2) .
U1 O2 2.282(2) 4_554
U1 O5 2.298(2) 5_556
U1 O1 2.311(2) .
U1 O4 2.311(2) .
P1 O2 1.509(2) .
P1 O1 1.510(2) .
P1 O3 1.561(3) .
P1 C2 1.797(4) .
P2 O5 1.517(2) .
P2 O4 1.520(2) .
P2 O6 1.555(3) .
P2 C6 1.801(3) .
O2 U1 2.282(2) 4
O3 H3 0.8400 .
O5 U1 2.298(2) 5_556
O6 H6 0.8400 .
C1 C2 1.403(4) .
C1 C2 1.403(4) 7_565
C1 H1 0.9500 .
C2 C3 1.395(5) .
C3 C4 1.389(4) .
C3 H3A 0.9500 .
C4 C3 1.389(4) 7_565
C4 H4 0.9500 .
C5 C6 1.388(4) 7
C5 C6 1.388(4) .
C5 H5 0.9500 .
C6 C7 1.398(5) .
C7 C8 1.385(4) .
C7 H7 0.9500 .
C8 C7 1.385(4) 7
C8 H8 0.9500 .
C10 N1 1.497(7) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C9 N1 1.537(9) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C11 N1 1.552(9) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 N1 1.396(8) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 P1 O1 U1 95.1(3) . .
O3 P1 O1 U1 -24.1(3) . .
C2 P1 O1 U1 -142.4(2) . .
O1 P1 O2 U1 146.5(4) . 4
O3 P1 O2 U1 -90.6(5) . 4
C2 P1 O2 U1 25.0(5) . 4
O5 P2 O4 U1 47.4(3) . .
O6 P2 O4 U1 170.21(19) . .
C6 P2 O4 U1 -71.0(2) . .
O4 P2 O5 U1 68.2(3) . 5_556
O6 P2 O5 U1 -55.9(3) . 5_556
C6 P2 O5 U1 -172.6(3) . 5_556
C2 C1 C2 C3 1.4(6) 7_565 .
C2 C1 C2 P1 -177.2(2) 7_565 .
O2 P1 C2 C3 -53.5(3) . .
O1 P1 C2 C3 -178.4(3) . .
O3 P1 C2 C3 60.6(3) . .
O2 P1 C2 C1 125.1(3) . .
O1 P1 C2 C1 0.2(4) . .
O3 P1 C2 C1 -120.8(3) . .
C1 C2 C3 C4 0.0(6) . .
P1 C2 C3 C4 178.7(3) . .
C2 C3 C4 C3 -1.4(7) . 7_565
C6 C5 C6 C7 1.1(7) 7 .
C6 C5 C6 P2 -179.8(3) 7 .
O5 P2 C6 C5 29.0(4) . .
O4 P2 C6 C5 151.8(3) . .
O6 P2 C6 C5 -87.8(3) . .
O5 P2 C6 C7 -151.9(3) . .
O4 P2 C6 C7 -29.1(3) . .
O6 P2 C6 C7 91.3(3) . .
C5 C6 C7 C8 0.1(6) . .
P2 C6 C7 C8 -179.0(3) . .
C6 C7 C8 C7 -1.3(7) . 7
