#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:20:45 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179056 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/18/4301889.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_4301889
loop_
_publ_author_name
'Pius O. Adelani'
'Thomas E. Albrecht-Schmitt'
_publ_section_title
;
Uranyl Diphosphonates with Pillared Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2732
_journal_page_last               2734
_journal_paper_doi               10.1021/ic900172s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C19 H19 N2 O12 P3 U'
_chemical_formula_sum            'C19 H19 N2 O12 P3 U'
_chemical_formula_weight         798.30
_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                63.5180(10)
_cell_angle_beta                 89.2330(10)
_cell_angle_gamma                89.5900(10)
_cell_formula_units_Z            2
_cell_length_a                   8.8105(6)
_cell_length_b                   12.0084(8)
_cell_length_c                   12.3493(8)
_cell_measurement_reflns_used    4926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      1.84
_cell_volume                     1169.36(14)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'BRUKER APEX'
_diffrn_measurement_method       '0.3 wide /w exposure'
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12094
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         na
_exptl_absorpt_coefficient_mu    7.216
_exptl_absorpt_correction_T_max  0.6230
_exptl_absorpt_correction_T_min  0.4854
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELXPREP
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.096
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.084
_refine_diff_density_max         3.576
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.301
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0497
_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)+(0.0629P)²+0.0106P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                4926
_reflns_number_total             5770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900172s_si_001_3.cif
_cod_data_source_block           final
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'na' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1169.36(13)
_cod_database_code               4301889
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 0.97951(3) 0.55022(3) 0.72784(2) 0.01428(10) Uani 1 1 d . . .
O1 O 1.1362(6) 0.6543(5) 0.6811(5) 0.0187(11) Uani 1 1 d . . .
O2 O 0.8207(6) 0.4502(5) 0.7726(5) 0.0191(11) Uani 1 1 d . . .
P1 P 0.8240(2) 0.86529(19) 0.57694(18) 0.0163(4) Uani 1 1 d . . .
O3 O 0.8045(6) 0.7284(5) 0.6545(5) 0.0230(12) Uani 1 1 d . . .
O4 O 0.9096(6) 0.8997(5) 0.4597(5) 0.0166(11) Uani 1 1 d . . .
O5 O 0.9031(6) 0.9226(5) 0.6531(5) 0.0206(12) Uani 1 1 d . . .
H5A H 0.9604 0.9785 0.6093 0.031 Uiso 1 1 calc R . .
C11 C 0.6406(9) 0.9394(7) 0.5366(7) 0.0166(15) Uani 1 1 d . . .
C12 C 0.6324(10) 1.0692(8) 0.4758(7) 0.0234(17) Uani 1 1 d . . .
H12A H 0.7207 1.1163 0.4594 0.028 Uiso 1 1 calc R . .
C13 C 0.5051(10) 0.8727(8) 0.5596(8) 0.0237(17) Uani 1 1 d . . .
H13A H 0.5084 0.7863 0.6002 0.028 Uiso 1 1 calc R . .
P2 P 0.8264(2) 0.62712(17) 0.41964(16) 0.0110(3) Uani 1 1 d . . .
O6 O 0.9231(6) 0.5984(5) 0.5279(4) 0.0147(10) Uani 1 1 d . . .
O7 O 0.7962(6) 0.7723(5) 0.3551(5) 0.0162(11) Uani 1 1 d . . .
H7B H 0.8356 0.8045 0.3940 0.024 Uiso 1 1 calc R . .
O8 O 0.8884(6) 0.5922(5) 0.3253(4) 0.0134(10) Uani 1 1 d . . .
C14 C 0.6424(8) 0.5582(7) 0.4637(7) 0.0138(14) Uani 1 1 d . . .
C15 C 0.5713(8) 0.5076(7) 0.3956(7) 0.0159(15) Uani 1 1 d . . .
H15A H 0.6188 0.5110 0.3265 0.019 Uiso 1 1 calc R . .
C16 C 0.5709(9) 0.5481(7) 0.5691(7) 0.0194(16) Uani 1 1 d . . .
H16A H 0.6188 0.5791 0.6166 0.023 Uiso 1 1 calc R . .
P3 P 0.8263(2) 0.6270(2) 0.97023(18) 0.0189(4) Uani 1 1 d . . .
O9 O 0.9282(7) 0.5943(6) 0.8910(5) 0.0249(13) Uani 1 1 d . . .
O10 O 0.8849(6) 0.5983(5) 1.0945(5) 0.0177(11) Uani 1 1 d . . .
O11 O 0.7967(7) 0.7712(6) 0.9004(5) 0.0277(13) Uani 1 1 d . . .
H11A H 0.8344 0.7984 0.8324 0.042 Uiso 1 1 calc R . .
C17 C 0.6426(9) 0.5561(8) 0.9884(8) 0.0220(17) Uani 1 1 d . . .
C18 C 0.5479(10) 0.5876(9) 0.8871(8) 0.028(2) Uani 1 1 d . . .
H18A H 0.5803 0.6463 0.8111 0.034 Uiso 1 1 calc R . .
C19 C 0.5908(9) 0.4676(9) 1.0998(7) 0.0242(18) Uani 1 1 d . . .
H19A H 0.6518 0.4452 1.1672 0.029 Uiso 1 1 calc R . .
N1 N 0.5212(7) 0.1521(6) 1.0160(6) 0.0191(14) Uani 1 1 d . . .
H1A H 0.4440 0.1503 0.9749 0.023 Uiso 1 1 calc R . .
C1 C 0.6246(10) 0.2430(8) 0.9696(8) 0.0255(18) Uani 1 1 d . . .
H1B H 0.6112 0.3056 0.8915 0.031 Uiso 1 1 calc R . .
C2 C 0.7524(11) 0.2477(9) 1.0339(9) 0.032(2) Uani 1 1 d . . .
H2A H 0.8229 0.3115 0.9985 0.039 Uiso 1 1 calc R . .
C3 C 0.7718(12) 0.1566(9) 1.1500(9) 0.036(2) Uani 1 1 d . . .
H3B H 0.8544 0.1580 1.1955 0.044 Uiso 1 1 calc R . .
C4 C 0.6651(10) 0.0628(8) 1.1973(8) 0.0275(19) Uani 1 1 d . . .
H4A H 0.6757 -0.0013 1.2750 0.033 Uiso 1 1 calc R . .
C5 C 0.5427(9) 0.0652(7) 1.1280(7) 0.0177(15) Uani 1 1 d . . .
C6 C 0.4240(9) -0.0304(7) 1.1763(7) 0.0174(15) Uani 1 1 d . . .
C7 C 0.4310(9) -0.1396(7) 1.2834(7) 0.0218(17) Uani 1 1 d . . .
H7A H 0.5189 -0.1598 1.3292 0.026 Uiso 1 1 calc R . .
C8 C 0.3065(11) -0.2187(8) 1.3220(8) 0.030(2) Uani 1 1 d . . .
H8A H 0.3094 -0.2899 1.3956 0.036 Uiso 1 1 calc R . .
C9 C 0.1797(10) -0.1923(8) 1.2521(8) 0.0280(19) Uani 1 1 d . . .
H9B H 0.0973 -0.2463 1.2768 0.034 Uiso 1 1 calc R . .
C10 C 0.1754(9) -0.0862(8) 1.1461(8) 0.0256(18) Uani 1 1 d . . .
H10A H 0.0901 -0.0679 1.0975 0.031 Uiso 1 1 calc R . .
N2 N 0.2943(7) -0.0076(6) 1.1113(6) 0.0176(13) Uani 1 1 d . . .
H2B H 0.2879 0.0600 1.0451 0.021 Uiso 1 1 calc R . .
O1W O 0.8382(7) 0.8432(5) 0.0997(5) 0.0254(13) Uani 1 1 d . . .
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
_geom_angle_publ_flag
O2 U1 O1 178.5(3) . . ?
O2 U1 O6 88.0(2) . . ?
O1 U1 O6 91.4(2) . . ?
O2 U1 O9 88.3(2) . . ?
O1 U1 O9 91.3(2) . . ?
O6 U1 O9 145.8(2) . . ?
O2 U1 O8 89.7(2) . 2_766 ?
O1 U1 O8 91.4(2) . 2_766 ?
O6 U1 O8 71.69(17) . 2_766 ?
O9 U1 O8 142.25(19) . 2_766 ?
O2 U1 O10 89.4(2) . 2_767 ?
O1 U1 O10 91.8(2) . 2_767 ?
O6 U1 O10 143.13(18) . 2_767 ?
O9 U1 O10 70.76(19) . 2_767 ?
O8 U1 O10 71.53(17) 2_766 2_767 ?
O2 U1 O3 88.7(2) . . ?
O1 U1 O3 89.8(2) . . ?
O6 U1 O3 72.79(19) . . ?
O9 U1 O3 73.2(2) . . ?
O8 U1 O3 144.48(18) 2_766 . ?
O10 U1 O3 143.92(19) 2_767 . ?
O3 P1 O4 115.0(3) . . ?
O3 P1 O5 108.6(3) . . ?
O4 P1 O5 110.4(3) . . ?
O3 P1 C11 109.9(3) . . ?
O4 P1 C11 106.4(3) . . ?
O5 P1 C11 106.3(3) . . ?
P1 O3 U1 133.7(3) . . ?
P1 O5 H5A 109.5 . . ?
C13 C11 C12 117.8(7) . . ?
C13 C11 P1 122.9(6) . . ?
C12 C11 P1 119.2(6) . . ?
C13 C12 C11 120.2(8) 2_676 . ?
C13 C12 H12A 119.9 2_676 . ?
C11 C12 H12A 119.9 . . ?
C12 C13 C11 122.0(8) 2_676 . ?
C12 C13 H13A 119.0 2_676 . ?
C11 C13 H13A 119.0 . . ?
O6 P2 O8 117.2(3) . . ?
O6 P2 O7 108.0(3) . . ?
O8 P2 O7 107.1(3) . . ?
O6 P2 C14 111.1(3) . . ?
O8 P2 C14 107.7(3) . . ?
O7 P2 C14 104.9(3) . . ?
P2 O6 U1 157.7(3) . . ?
P2 O7 H7B 109.5 . . ?
P2 O8 U1 150.2(3) . 2_766 ?
C16 C14 C15 118.7(7) . . ?
C16 C14 P2 121.2(6) . . ?
C15 C14 P2 120.0(6) . . ?
C16 C15 C14 120.1(7) 2_666 . ?
C16 C15 H15A 120.0 2_666 . ?
C14 C15 H15A 120.0 . . ?
C14 C16 C15 121.2(7) . 2_666 ?
C14 C16 H16A 119.4 . . ?
C15 C16 H16A 119.4 2_666 . ?
O9 P3 O10 116.7(3) . . ?
O9 P3 O11 106.6(4) . . ?
O10 P3 O11 108.1(3) . . ?
O9 P3 C17 111.5(4) . . ?
O10 P3 C17 108.1(4) . . ?
O11 P3 C17 105.3(4) . . ?
P3 O9 U1 153.8(4) . . ?
P3 O10 U1 146.2(3) . 2_767 ?
P3 O11 H11A 109.5 . . ?
C19 C17 C18 118.0(8) . . ?
C19 C17 P3 121.7(6) . . ?
C18 C17 P3 120.3(7) . . ?
C19 C18 C17 120.5(8) 2_667 . ?
C19 C18 H18A 119.8 2_667 . ?
C17 C18 H18A 119.8 . . ?
C18 C19 C17 121.5(8) 2_667 . ?
C18 C19 H19A 119.2 2_667 . ?
C17 C19 H19A 119.2 . . ?
C5 N1 C1 117.1(7) . . ?
C5 N1 H1A 121.4 . . ?
C1 N1 H1A 121.4 . . ?
N1 C1 C2 122.7(8) . . ?
N1 C1 H1B 118.6 . . ?
C2 C1 H1B 118.6 . . ?
C3 C2 C1 119.0(9) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 118.1(9) . . ?
C2 C3 H3B 121.0 . . ?
C4 C3 H3B 121.0 . . ?
C5 C4 C3 119.3(8) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
N1 C5 C4 123.9(7) . . ?
N1 C5 C6 115.2(7) . . ?
C4 C5 C6 121.0(7) . . ?
N2 C6 C7 117.4(7) . . ?
N2 C6 C5 116.6(7) . . ?
C7 C6 C5 125.9(7) . . ?
C6 C7 C8 119.8(8) . . ?
C6 C7 H7A 120.1 . . ?
C8 C7 H7A 120.1 . . ?
C9 C8 C7 120.3(8) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
C10 C9 C8 119.3(8) . . ?
C10 C9 H9B 120.3 . . ?
C8 C9 H9B 120.3 . . ?
N2 C10 C9 120.1(8) . . ?
N2 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 N2 C6 122.9(7) . . ?
C10 N2 H2B 118.5 . . ?
C6 N2 H2B 118.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.765(5) . ?
U1 O1 1.778(5) . ?
U1 O6 2.331(5) . ?
U1 O9 2.338(5) . ?
U1 O8 2.380(5) 2_766 ?
U1 O10 2.444(5) 2_767 ?
U1 O3 2.457(6) . ?
P1 O3 1.498(6) . ?
P1 O4 1.509(6) . ?
P1 O5 1.563(6) . ?
P1 C11 1.805(8) . ?
O5 H5A 0.8200 . ?
C11 C13 1.396(11) . ?
C11 C12 1.398(11) . ?
C12 C13 1.370(12) 2_676 ?
C12 H12A 0.9300 . ?
C13 C12 1.370(12) 2_676 ?
C13 H13A 0.9300 . ?
P2 O6 1.499(5) . ?
P2 O8 1.498(5) . ?
P2 O7 1.583(6) . ?
P2 C14 1.790(7) . ?
O7 H7B 0.8200 . ?
O8 U1 2.380(5) 2_766 ?
C14 C16 1.393(11) . ?
C14 C15 1.395(10) . ?
C15 C16 1.394(11) 2_666 ?
C15 H15A 0.9300 . ?
C16 C15 1.394(11) 2_666 ?
C16 H16A 0.9300 . ?
P3 O9 1.494(6) . ?
P3 O10 1.512(5) . ?
P3 O11 1.575(7) . ?
P3 C17 1.799(8) . ?
O10 U1 2.444(5) 2_767 ?
O11 H11A 0.8200 . ?
C17 C19 1.384(12) . ?
C17 C18 1.417(11) . ?
C18 C19 1.367(12) 2_667 ?
C18 H18A 0.9300 . ?
C19 C18 1.367(12) 2_667 ?
C19 H19A 0.9300 . ?
N1 C5 1.324(10) . ?
N1 C1 1.339(10) . ?
N1 H1A 0.8600 . ?
C1 C2 1.402(13) . ?
C1 H1B 0.9300 . ?
C2 C3 1.374(14) . ?
C2 H2A 0.9300 . ?
C3 C4 1.381(12) . ?
C3 H3B 0.9300 . ?
C4 C5 1.378(12) . ?
C4 H4A 0.9300 . ?
C5 C6 1.469(10) . ?
C6 N2 1.360(10) . ?
C6 C7 1.388(11) . ?
C7 C8 1.389(12) . ?
C7 H7A 0.9300 . ?
C8 C9 1.367(13) . ?
C8 H8A 0.9300 . ?
C9 C10 1.362(12) . ?
C9 H9B 0.9300 . ?
C10 N2 1.346(10) . ?
C10 H10A 0.9300 . ?
N2 H2B 0.8600 . ?
