#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:50:36 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179542 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/11/4501199.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_4501199
loop_
_publ_author_name
'Adelani, Pius O.'
'Albrecht-Schmitt, Thomas E.'
_publ_section_title
;
 Syntheses of Uranyl Diphosphonate Compounds Using Encapsulated Cations as
 Structure Directing Agents
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4227
_journal_paper_doi               10.1021/cg200872a
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C20 H24 O21 P4 U2'
_chemical_formula_sum            'C20 H24 O21 P4 U2'
_chemical_formula_weight         1200.33
_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                92.6250(10)
_cell_angle_beta                 114.8990(10)
_cell_angle_gamma                110.6280(10)
_cell_formula_units_Z            1
_cell_length_a                   9.7762(8)
_cell_length_b                   9.8409(8)
_cell_length_c                   10.3044(9)
_cell_measurement_reflns_used    4110
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.27
_cell_volume                     819.26(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9711
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.152
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SHELXPREP
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.904
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0262P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                3316
_reflns_number_total             3706
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200872a_si_001.cif
_cod_data_source_block           p-1pius
_cod_database_code               4501199
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
U1 U 0.33142(2) 0.537073(18) 0.556986(19) 0.01114(6) Uani 1 1 d .
P1 P 0.69800(14) 0.77239(13) 0.69867(13) 0.0124(2) Uani 1 1 d .
P2 P 0.88841(14) 1.26922(13) 0.35573(13) 0.0117(2) Uani 1 1 d .
O1 O 0.2921(4) 0.6389(3) 0.4179(3) 0.0142(7) Uani 1 1 d .
O2 O 0.3753(4) 0.4368(3) 0.6964(4) 0.0164(7) Uani 1 1 d .
O3 O 0.5567(4) 0.7707(3) 0.7252(3) 0.0153(7) Uani 1 1 d .
O4 O 0.6269(4) 0.6203(3) 0.5951(3) 0.0138(7) Uani 1 1 d .
O5 O 0.8591(4) 0.8011(4) 0.8409(4) 0.0181(7) Uani 1 1 d .
O6 O 1.0731(4) 1.3486(3) 0.4209(4) 0.0151(7) Uani 1 1 d .
O7 O 0.8103(4) 1.1718(4) 0.1981(4) 0.0190(7) Uani 1 1 d .
O8 O 0.8033(4) 1.3728(3) 0.3502(3) 0.0146(7) Uani 1 1 d .
O9 O 0.8764(4) 0.6161(4) 1.0064(4) 0.0287(9) Uani 1 1 d .
O10 O 0.7911(5) 0.2976(4) 0.9788(4) 0.0284(8) Uani 1 1 d .
O1W O 0.3461(14) 0.1504(12) 0.9604(12) 0.070(3) Uiso 0.50 1 d P
C1 C 0.7599(5) 0.9179(5) 0.6100(5) 0.0127(9) Uani 1 1 d .
C2 C 0.9246(6) 1.0141(5) 0.6598(5) 0.0146(9) Uani 1 1 d .
H2A H 1.0093 1.0077 0.7461 0.018 Uiso 1 1 calc R
C6 C 0.6353(6) 0.9295(5) 0.4853(5) 0.0178(10) Uani 1 1 d .
H6A H 0.5229 0.8642 0.4521 0.021 Uiso 1 1 calc R
C4 C 0.8405(5) 1.1328(5) 0.4573(5) 0.0114(9) Uani 1 1 d .
C3 C 0.9636(6) 1.1198(5) 0.5814(5) 0.0164(10) Uani 1 1 d .
H3A H 1.0760 1.1840 0.6133 0.020 Uiso 1 1 calc R
C5 C 0.6759(6) 1.0363(5) 0.4104(5) 0.0196(10) Uani 1 1 d .
H5A H 0.5909 1.0444 0.3256 0.024 Uiso 1 1 calc R
C7 C 0.7308(7) 0.5100(6) 1.0093(6) 0.0284(12) Uani 1 1 d .
H7A H 0.6421 0.5467 0.9739 0.034 Uiso 1 1 calc R
H7B H 0.7578 0.5002 1.1115 0.034 Uiso 1 1 calc R
C8 C 0.6715(7) 0.3612(6) 0.9139(6) 0.0294(13) Uani 1 1 d .
H8A H 0.5632 0.2939 0.9042 0.035 Uiso 1 1 calc R
H8B H 0.6572 0.3727 0.8146 0.035 Uiso 1 1 calc R
C9 C 0.8330(6) 0.2362(6) 0.8782(6) 0.0236(11) Uani 1 1 d .
H9A H 0.7345 0.1931 0.7803 0.028 Uiso 1 1 calc R
H9B H 0.8653 0.1548 0.9132 0.028 Uiso 1 1 calc R
C10 C 0.9710(6) 0.3512(6) 0.8646(6) 0.0242(11) Uani 1 1 d .
H10A H 0.9765 0.3139 0.7768 0.029 Uiso 1 1 calc R
H10B H 0.9515 0.4430 0.8526 0.029 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'
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 178.68(13) . .
O2 U1 O8 90.70(12) . 2_676
O1 U1 O8 90.26(12) . 2_676
O2 U1 O6 90.36(13) . 1_445
O1 U1 O6 90.65(12) . 1_445
O8 U1 O6 82.95(11) 2_676 1_445
O2 U1 O4 91.41(12) . 2_666
O1 U1 O4 88.01(12) . 2_666
O8 U1 O4 159.52(11) 2_676 2_666
O6 U1 O4 76.66(10) 1_445 2_666
O2 U1 O3 91.76(13) . .
O1 U1 O3 87.54(12) . .
O8 U1 O3 78.90(10) 2_676 .
O6 U1 O3 161.75(10) 1_445 .
O4 U1 O3 121.39(10) 2_666 .
O2 U1 O4 89.71(12) . .
O1 U1 O4 88.97(12) . .
O8 U1 O4 136.26(10) 2_676 .
O6 U1 O4 140.79(10) 1_445 .
O4 U1 O4 64.14(12) 2_666 .
O3 U1 O4 57.37(10) . .
O2 U1 P1 92.82(10) . .
O1 U1 P1 86.04(10) . .
O8 U1 P1 107.14(8) 2_676 .
O6 U1 P1 169.37(8) 1_445 .
O4 U1 P1 93.11(7) 2_666 .
O3 U1 P1 28.28(7) . .
O4 U1 P1 29.22(7) . .
O3 P1 O4 104.01(18) . .
O3 P1 O5 114.22(18) . .
O4 P1 O5 112.96(18) . .
O3 P1 C1 112.28(19) . .
O4 P1 C1 109.20(19) . .
O5 P1 C1 104.3(2) . .
O3 P1 U1 50.07(13) . .
O4 P1 U1 54.22(11) . .
O5 P1 U1 135.13(13) . .
C1 P1 U1 120.58(16) . .
O6 P2 O8 113.69(17) . .
O6 P2 O7 111.51(18) . .
O8 P2 O7 108.97(19) . .
O6 P2 C4 108.78(19) . .
O8 P2 C4 110.70(19) . .
O7 P2 C4 102.63(19) . .
P1 O3 U1 101.65(16) . .
P1 O4 U1 146.65(18) . 2_666
P1 O4 U1 96.56(14) . .
U1 O4 U1 115.86(12) 2_666 .
P2 O6 U1 157.59(19) . 1_665
P2 O8 U1 147.86(19) . 2_676
C10 O9 C7 114.7(4) 2_767 .
C9 O10 C8 115.1(4) . .
C2 C1 C6 120.5(4) . .
C2 C1 P1 122.5(3) . .
C6 C1 P1 117.1(3) . .
C3 C2 C1 119.1(4) . .
C3 C2 H2A 120.4 . .
C1 C2 H2A 120.4 . .
C5 C6 C1 119.6(4) . .
C5 C6 H6A 120.2 . .
C1 C6 H6A 120.2 . .
C3 C4 C5 119.0(4) . .
C3 C4 P2 121.5(3) . .
C5 C4 P2 119.5(3) . .
C4 C3 C2 120.9(4) . .
C4 C3 H3A 119.5 . .
C2 C3 H3A 119.5 . .
C6 C5 C4 120.9(4) . .
C6 C5 H5A 119.5 . .
C4 C5 H5A 119.5 . .
O9 C7 C8 110.2(4) . .
O9 C7 H7A 109.6 . .
C8 C7 H7A 109.6 . .
O9 C7 H7B 109.6 . .
C8 C7 H7B 109.6 . .
H7A C7 H7B 108.1 . .
O10 C8 C7 109.4(5) . .
O10 C8 H8A 109.8 . .
C7 C8 H8A 109.8 . .
O10 C8 H8B 109.8 . .
C7 C8 H8B 109.8 . .
H8A C8 H8B 108.2 . .
O10 C9 C10 111.9(4) . .
O10 C9 H9A 109.2 . .
C10 C9 H9A 109.2 . .
O10 C9 H9B 109.2 . .
C10 C9 H9B 109.2 . .
H9A C9 H9B 107.9 . .
O9 C10 C9 109.4(4) 2_767 .
O9 C10 H10A 109.8 2_767 .
C9 C10 H10A 109.8 . .
O9 C10 H10B 109.8 2_767 .
C9 C10 H10B 109.8 . .
H10A C10 H10B 108.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.769(3) .
U1 O1 1.773(3) .
U1 O8 2.290(3) 2_676
U1 O6 2.294(3) 1_445
U1 O4 2.404(3) 2_666
U1 O3 2.448(3) .
U1 O4 2.553(3) .
U1 P1 3.1264(12) .
P1 O3 1.512(3) .
P1 O4 1.536(3) .
P1 O5 1.553(3) .
P1 C1 1.796(4) .
P2 O6 1.503(3) .
P2 O8 1.516(3) .
P2 O7 1.561(3) .
P2 C4 1.793(4) .
O4 U1 2.404(3) 2_666
O6 U1 2.294(3) 1_665
O8 U1 2.290(3) 2_676
O9 C10 1.432(6) 2_767
O9 C7 1.453(6) .
O10 C9 1.443(6) .
O10 C8 1.450(6) .
C1 C2 1.392(6) .
C1 C6 1.394(6) .
C2 C3 1.392(6) .
C2 H2A 0.9500 .
C6 C5 1.377(6) .
C6 H6A 0.9500 .
C4 C3 1.388(6) .
C4 C5 1.397(6) .
C3 H3A 0.9500 .
C5 H5A 0.9500 .
C7 C8 1.496(8) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.490(7) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 O9 1.432(6) 2_767
C10 H10A 0.9900 .
C10 H10B 0.9900 .
