#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:51:47 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179543 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/12/4501200.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_4501200
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         'C22 H12 O27 P6 U3'
_chemical_formula_sum            'C22 H12 O27 P6 U3'
_chemical_formula_weight         1608.23
_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                111.964(4)
_cell_angle_beta                 107.146(4)
_cell_angle_gamma                105.977(4)
_cell_formula_units_Z            1
_cell_length_a                   10.089(3)
_cell_length_b                   11.712(4)
_cell_length_c                   11.803(4)
_cell_measurement_reflns_used    7039
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      2.34
_cell_volume                     1112.9(6)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17282
_diffrn_reflns_theta_full        24.21
_diffrn_reflns_theta_max         24.21
_diffrn_reflns_theta_min         2.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.187
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SHELXPREP
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.035
_refine_diff_density_max         4.938
_refine_diff_density_min         -4.256
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.297
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3535
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0583
_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)+(0.1018P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1761
_reflns_number_gt                2854
_reflns_number_total             3535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200872a_si_001.cif
_cod_data_source_block           p-1
_cod_database_code               4501200
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 1.0000 0.0000 0.0000 0.0459(3) Uani 1 2 d S . .
U2 U 1.0000 0.5000 0.5000 0.0379(3) Uani 1 2 d S . .
U3 U 0.5000 0.5000 0.0000 0.0332(3) Uani 1 2 d S . .
P1 P 0.8893(5) -0.2656(4) 0.0908(5) 0.0491(11) Uani 1 1 d . . .
P2 P 0.8435(5) 0.1444(4) 0.2342(4) 0.0478(11) Uani 1 1 d . . .
P3 P 0.6971(5) 0.5922(5) 0.3570(4) 0.0461(10) Uani 1 1 d . . .
O1 O 0.8144(13) -0.0447(15) -0.1160(15) 0.078(4) Uani 1 1 d . . .
O2 O 0.8644(14) 0.4352(13) 0.5499(13) 0.066(3) Uani 1 1 d . . .
O3 O 0.5718(13) 0.3847(11) -0.0630(13) 0.056(3) Uani 1 1 d . . .
O4 O 0.9011(17) -0.1949(12) 0.0065(15) 0.072(4) Uani 1 1 d . . .
O5 O 0.7300(13) -0.3204(11) 0.0761(13) 0.054(3) Uani 1 1 d . . .
O6 O 1.0039(17) -0.1672(14) 0.2475(14) 0.089(5) Uani 1 1 d . . .
O7 O 0.9500(12) 0.1065(12) 0.1784(12) 0.063(3) Uani 1 1 d . . .
O8 O 0.8946(15) 0.2979(11) 0.3030(12) 0.067(4) Uani 1 1 d . . .
O9 O 0.8334(17) 0.0871(16) 0.3326(13) 0.091(5) Uani 1 1 d . . .
O10 O 0.8444(12) 0.5779(14) 0.3975(12) 0.057(3) Uani 1 1 d . . .
O11 O 0.5981(14) 0.5086(12) 0.2033(11) 0.066(4) Uani 1 1 d . . .
O12 O 0.7365(19) 0.7463(14) 0.4127(17) 0.089(5) Uani 1 1 d . . .
O13 O 0.593(3) 1.072(3) 0.387(3) 0.081(8) Uani 0.50 1 d PU . 1
O14 O 0.482(3) 0.813(2) 0.404(2) 0.057(6) Uani 0.50 1 d PU A 1
O1W O 1.0000 0.0000 0.5000 0.177(15) Uani 1 2 d S B 1
C1 C 0.9500(15) -0.3976(13) 0.0392(16) 0.035(3) Uani 1 1 d . . .
C2 C 0.9934(18) -0.4256(15) -0.0677(16) 0.044(4) Uani 1 1 d . . .
H2A H 0.9913 -0.3747 -0.1121 0.053 Uiso 1 1 calc R . .
C3 C 0.9608(18) -0.4707(15) 0.1061(18) 0.045(4) Uani 1 1 d . . .
H3A H 0.9368 -0.4500 0.1794 0.054 Uiso 1 1 calc R . .
C4 C 0.6497(16) 0.0638(14) 0.1008(15) 0.035(3) Uani 1 1 d . . .
C5 C 0.5772(19) 0.1417(15) 0.0754(15) 0.045(4) Uani 1 1 d . . .
H5A H 0.6276 0.2367 0.1264 0.054 Uiso 1 1 calc R . .
C6 C 0.5730(19) -0.0754(15) 0.0282(16) 0.047(4) Uani 1 1 d . . .
H6A H 0.6218 -0.1270 0.0481 0.057 Uiso 1 1 calc R . .
C7 C 0.5856(16) 0.5391(15) 0.4373(15) 0.034(3) Uani 1 1 d . . .
C8 C 0.6464(18) 0.6087(16) 0.5785(16) 0.044(4) Uani 1 1 d . . .
H8A H 0.7431 0.6829 0.6306 0.053 Uiso 1 1 calc R . .
C9 C 0.4367(17) 0.4323(15) 0.3587(15) 0.041(4) Uani 1 1 d . . .
H9A H 0.3938 0.3890 0.2640 0.049 Uiso 1 1 calc R . .
C10 C 0.317(5) 0.905(4) 0.313(4) 0.063(10) Uani 0.50 1 d PU A 1
C11 C 0.377(5) 0.831(4) 0.275(5) 0.081(13) Uani 0.50 1 d P A 1
C12 C 0.385(7) 0.777(5) 0.451(5) 0.095(16) Uani 0.50 1 d P A 1
C13 C 0.447(6) 0.838(5) 0.578(5) 0.083(13) Uani 0.50 1 d PU . 1
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
O1 U1 O1 179.999(1) . 2_755
O1 U1 O4 88.2(6) . .
O1 U1 O4 91.8(6) 2_755 .
O1 U1 O4 91.8(6) . 2_755
O1 U1 O4 88.2(6) 2_755 2_755
O4 U1 O4 180.0 . 2_755
O1 U1 O7 90.1(6) . .
O1 U1 O7 89.9(6) 2_755 .
O4 U1 O7 87.4(5) . .
O4 U1 O7 92.6(5) 2_755 .
O1 U1 O7 89.9(6) . 2_755
O1 U1 O7 90.1(6) 2_755 2_755
O4 U1 O7 92.6(5) . 2_755
O4 U1 O7 87.4(5) 2_755 2_755
O7 U1 O7 180.0(5) . 2_755
O2 U2 O2 180.000(3) . 2_766
O2 U2 O8 91.8(6) . .
O2 U2 O8 88.2(6) 2_766 .
O2 U2 O8 88.2(6) . 2_766
O2 U2 O8 91.8(6) 2_766 2_766
O8 U2 O8 179.999(3) . 2_766
O2 U2 O10 90.0(5) . .
O2 U2 O10 90.0(5) 2_766 .
O8 U2 O10 91.8(4) . .
O8 U2 O10 88.2(4) 2_766 .
O2 U2 O10 90.0(5) . 2_766
O2 U2 O10 90.0(5) 2_766 2_766
O8 U2 O10 88.2(4) . 2_766
O8 U2 O10 91.8(4) 2_766 2_766
O10 U2 O10 180.000(4) . 2_766
O3 U3 O3 179.999(1) 2_665 .
O3 U3 O11 91.3(6) 2_665 .
O3 U3 O11 88.7(6) . .
O3 U3 O11 88.7(6) 2_665 2_665
O3 U3 O11 91.3(6) . 2_665
O11 U3 O11 180.0(6) . 2_665
O3 U3 O5 89.6(5) 2_665 1_565
O3 U3 O5 90.4(5) . 1_565
O11 U3 O5 87.8(4) . 1_565
O11 U3 O5 92.2(4) 2_665 1_565
O3 U3 O5 90.4(5) 2_665 2_655
O3 U3 O5 89.6(5) . 2_655
O11 U3 O5 92.2(4) . 2_655
O11 U3 O5 87.8(4) 2_665 2_655
O5 U3 O5 179.998(1) 1_565 2_655
O5 P1 O4 111.1(8) . .
O5 P1 O6 108.6(8) . .
O4 P1 O6 112.5(9) . .
O5 P1 C1 111.4(6) . .
O4 P1 C1 108.8(7) . .
O6 P1 C1 104.3(7) . .
O7 P2 O8 111.3(8) . .
O7 P2 O9 108.8(9) . .
O8 P2 O9 112.3(8) . .
O7 P2 C4 111.2(6) . .
O8 P2 C4 107.7(7) . .
O9 P2 C4 105.4(8) . .
O10 P3 O11 111.6(8) . .
O10 P3 O12 108.7(9) . .
O11 P3 O12 111.9(8) . .
O10 P3 C7 111.7(6) . .
O11 P3 C7 108.3(7) . .
O12 P3 C7 104.5(7) . .
P1 O4 U1 148.7(9) . .
P1 O5 U3 151.3(7) . 1_545
P2 O7 U1 151.6(7) . .
P2 O8 U2 148.2(8) . .
P3 O10 U2 150.9(7) . .
P3 O11 U3 149.5(7) . .
C12 O14 C11 104(3) . .
C3 C1 C2 118.6(13) . .
C3 C1 P1 120.5(12) . .
C2 C1 P1 120.8(11) . .
C3 C2 C1 119.5(15) 2_745 .
C3 C2 H2A 120.2 2_745 .
C1 C2 H2A 120.2 . .
C1 C3 C2 121.8(15) . 2_745
C1 C3 H3A 119.1 . .
C2 C3 H3A 119.1 2_745 .
C6 C4 C5 120.1(14) . .
C6 C4 P2 119.4(12) . .
C5 C4 P2 120.5(11) . .
C4 C5 C6 118.7(13) . 2_655
C4 C5 H5A 120.7 . .
C6 C5 H5A 120.7 2_655 .
C4 C6 C5 121.2(15) . 2_655
C4 C6 H6A 119.4 . .
C5 C6 H6A 119.4 2_655 .
C8 C7 C9 120.0(13) . .
C8 C7 P3 119.3(11) . .
C9 C7 P3 120.7(11) . .
C9 C8 C7 119.9(14) 2_666 .
C9 C8 H8A 120.1 2_666 .
C7 C8 H8A 120.1 . .
C8 C9 C7 120.1(14) 2_666 .
C8 C9 H9A 120.0 2_666 .
C7 C9 H9A 120.0 . .
C10 C11 O14 111(4) . .
C13 C12 O14 112(5) . .
O13 C13 C12 106(5) 2_676 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.752(12) .
U1 O1 1.752(12) 2_755
U1 O4 2.267(11) .
U1 O4 2.267(11) 2_755
U1 O7 2.292(12) .
U1 O7 2.292(12) 2_755
U2 O2 1.741(12) .
U2 O2 1.741(12) 2_766
U2 O8 2.276(10) .
U2 O8 2.276(10) 2_766
U2 O10 2.292(11) .
U2 O10 2.292(11) 2_766
U3 O3 1.734(10) 2_665
U3 O3 1.734(10) .
U3 O11 2.261(10) .
U3 O11 2.261(10) 2_665
U3 O5 2.300(10) 1_565
U3 O5 2.300(10) 2_655
P1 O5 1.486(11) .
P1 O4 1.523(13) .
P1 O6 1.580(15) .
P1 C1 1.781(14) .
P2 O7 1.498(12) .
P2 O8 1.519(11) .
P2 O9 1.558(14) .
P2 C4 1.803(15) .
P3 O10 1.497(11) .
P3 O11 1.521(12) .
P3 O12 1.553(14) .
P3 C7 1.799(14) .
O5 U3 2.300(10) 1_545
O13 C13 1.20(5) 2_676
O14 C12 1.30(5) .
O14 C11 1.70(6) .
C1 C3 1.37(2) .
C1 C2 1.41(2) .
C2 C3 1.38(2) 2_745
C2 H2A 0.9300 .
C3 C2 1.38(2) 2_745
C3 H3A 0.9300 .
C4 C6 1.36(2) .
C4 C5 1.38(2) .
C5 C6 1.39(2) 2_655
C5 H5A 0.9300 .
C6 C5 1.39(2) 2_655
C6 H6A 0.9300 .
C7 C8 1.39(2) .
C7 C9 1.40(2) .
C8 C9 1.38(2) 2_666
C8 H8A 0.9300 .
C9 C8 1.38(2) 2_666
C9 H9A 0.9300 .
C10 C11 1.22(5) .
C12 C13 1.25(6) .
C13 O13 1.20(5) 2_676
