#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:28:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179972 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/66/7026623.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_7026623
loop_
_publ_author_name
'Knope, Karah E.'
'Cahill, Christopher L.'
_publ_section_title
;
 Homometallic UO2(2+) diphosphonates assembled under ambient and
 hydrothermal conditions.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8319
_journal_page_last               8324
_journal_paper_doi               10.1039/c0dt00538j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C H5 O9 P2 U, 3(H2O), NH4'
_chemical_formula_sum            'C H15 N O12 P2 U'
_chemical_formula_weight         533.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.9310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1984(5)
_cell_length_b                   13.4771(9)
_cell_length_c                   13.3650(9)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.38
_cell_measurement_theta_min      2.17
_cell_volume                     1263.71(15)
_computing_cell_refinement       'APEX2 v2008.3-0 Software Suite (Bruker AXS)'
_computing_data_collection       'SMART v5.05 (Bruker AXS)'
_computing_data_reduction        'APEX2 v2008.3-0 Software Suite (Bruker AXS)'
_computing_molecular_graphics    'SHELX-97 (Sheldrick, 2008)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008 )'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'omega and phi 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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24630
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.38
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    13.152
_exptl_absorpt_correction_T_max  0.591
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.030
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0193
_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)+(0.0149P)²+5.7509P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0443
_reflns_number_gt                3274
_reflns_number_total             3585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00538j.txt
_cod_data_source_block           CH15NO12P2U
_cod_original_cell_volume        1263.70(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7026623
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.162142(16) 0.689993(8) 0.538024(8) 0.00531(4) Uani 1 1 d . . .
P1 P 0.30334(12) 0.72657(6) 0.81667(6) 0.00592(14) Uani 1 1 d . . .
O1 O -0.0514(3) 0.68040(18) 0.58288(19) 0.0116(5) Uani 1 1 d . . .
O2 O 0.3754(4) 0.69975(19) 0.4925(2) 0.0134(5) Uani 1 1 d . . .
O3 O 0.1647(5) 0.87212(19) 0.5660(2) 0.0236(6) Uani 1 1 d . . .
O4 O 0.3298(3) 0.72669(17) 0.70690(17) 0.0090(4) Uani 1 1 d . . .
O5 O 0.2637(3) 0.53317(17) 0.60713(18) 0.0094(4) Uani 1 1 d . . .
O6 O 0.0349(3) 0.57335(17) 0.40967(17) 0.0082(4) Uani 1 1 d . . .
O7 O -0.0045(3) 0.77981(17) 0.39268(17) 0.0077(4) Uani 1 1 d . . .
O8 O 0.3446(4) 0.97519(17) 0.73477(18) 0.0106(5) Uani 1 1 d . . .
O9 O 0.1687(3) 0.64342(17) 0.83562(19) 0.0106(5) Uani 1 1 d . . .
C1 C 0.1900(5) 0.8408(2) 0.8417(3) 0.0090(6) Uani 1 1 d . . .
H1A H 0.0754 0.8499 0.7883 0.011 Uiso 1 1 calc R . .
H1B H 0.1514 0.8341 0.9064 0.011 Uiso 1 1 calc R . .
N1 N 0.7745(10) 0.9194(5) 0.5429(4) 0.079(2) Uani 1 1 d . . .
OW1 O 0.6648(5) 0.5355(3) 0.6503(3) 0.0356(8) Uani 1 1 d . . .
OW2 O 0.7112(6) 0.7781(4) 0.6900(4) 0.0272(13) Uani 0.677(9) 1 d P A 1
OW3 O 0.7895(7) 0.5929(4) 0.8555(4) 0.0255(14) Uani 0.605(8) 1 d P B 1
OW4 O 0.7613(12) 0.6972(7) 0.7605(7) 0.035(3) Uani 0.395(8) 1 d P B 2
OW5 O 0.6970(15) 0.8978(9) 0.6979(9) 0.037(3) Uani 0.323(9) 1 d P A 2
P2 P 0.33572(12) 0.95015(6) 0.84732(6) 0.00692(15) 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'
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'
N N 0.0061 0.0033 '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 O2 179.74(12) . .
O1 U1 O6 88.41(10) . .
O2 U1 O6 91.45(10) . .
O1 U1 O5 91.05(10) . .
O2 U1 O5 89.12(10) . .
O6 U1 O5 73.91(8) . .
O1 U1 O4 89.33(10) . .
O2 U1 O4 90.90(10) . .
O6 U1 O4 150.23(8) . .
O5 U1 O4 76.46(8) . .
O1 U1 O7 89.78(10) . .
O2 U1 O7 89.97(10) . .
O6 U1 O7 72.63(8) . .
O5 U1 O7 146.49(8) . .
O4 U1 O7 137.05(8) . .
O1 U1 O3 89.93(11) . .
O2 U1 O3 90.04(11) . .
O6 U1 O3 139.30(8) . .
O5 U1 O3 146.79(8) . .
O4 U1 O3 70.35(8) . .
O7 U1 O3 66.71(8) . .
O4 P1 O7 110.62(14) . 4_676
O4 P1 O9 112.26(14) . .
O7 P1 O9 111.12(14) 4_676 .
O4 P1 C1 109.65(15) . .
O7 P1 C1 107.74(14) 4_676 .
O9 P1 C1 105.21(14) . .
P1 O4 U1 140.74(14) . .
P2 O5 U1 133.00(14) 2_546 .
P2 O6 U1 134.66(13) 4_575 .
P1 O7 U1 137.19(13) 4_575 .
P2 C1 P1 114.95(18) . .
P2 C1 H1A 108.5 . .
P1 C1 H1A 108.5 . .
P2 C1 H1B 108.5 . .
P1 C1 H1B 108.5 . .
H1A C1 H1B 107.5 . .
O6 P2 O5 113.73(13) 4_676 2_556
O6 P2 O8 109.70(14) 4_676 .
O5 P2 O8 110.53(13) 2_556 .
O6 P2 C1 108.73(14) 4_676 .
O5 P2 C1 107.24(14) 2_556 .
O8 P2 C1 106.63(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.775(2) .
U1 O2 1.778(2) .
U1 O6 2.356(2) .
U1 O5 2.356(2) .
U1 O4 2.361(2) .
U1 O7 2.374(2) .
U1 O3 2.482(3) .
P1 O4 1.521(2) .
P1 O7 1.524(2) 4_676
P1 O9 1.539(2) .
P1 C1 1.808(3) .
O5 P2 1.526(2) 2_546
O6 P2 1.522(2) 4_575
O7 P1 1.524(2) 4_575
O8 P2 1.557(2) .
C1 P2 1.801(3) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
P2 O6 1.522(2) 4_676
P2 O5 1.526(2) 2_556
