#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:00:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179088 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/50/4305010.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_4305010
loop_
_publ_author_name
'Andrea N. Alsobrook'
'Wei Zhan'
'Thomas E. Albrecht-Schmitt'
_publ_section_title
;
Use of Bifunctional Phosphonates for the Preparation of Heterobimetallic
5f-3d Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5177
_journal_page_last               5183
_journal_paper_doi               10.1021/ic800192r
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C2 H2 Na O9 P U'
_chemical_formula_sum            'C2 H2 Na O9 P U'
_chemical_formula_weight         462.03
_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                79.1450(10)
_cell_angle_beta                 78.6850(10)
_cell_angle_gamma                63.8860(10)
_cell_formula_units_Z            2
_cell_length_a                   6.8742(4)
_cell_length_b                   7.4167(5)
_cell_length_c                   9.6353(6)
_cell_measurement_reflns_used    2016
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.17
_cell_volume                     429.62(5)
_computing_cell_refinement       SMART,SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '0.3 wide /w exposures'
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4427
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         na
_exptl_absorpt_coefficient_mu    19.153
_exptl_absorpt_correction_T_max  0.7589
_exptl_absorpt_correction_T_min  0.2383
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELXPREP
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    3.572
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.024
_exptl_crystal_size_min          0.012
_refine_diff_density_max         1.620
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.257
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0304P)²+0.0669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                2016
_reflns_number_total             2117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800192r-file005_4.cif
_cod_data_source_block           p-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'nm' 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_sg_symbol_H-M      ' P -1'
_cod_database_code               4305010
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 0.26268(3) 0.61106(2) 0.770764(17) 0.00810(8) Uani 1 1 d . . .
P1 P 0.7918(2) 0.49082(19) 0.84896(13) 0.0085(2) Uani 1 1 d . . .
Na1 Na 0.5597(4) -0.0404(4) 0.8242(2) 0.0190(5) Uani 1 1 d . . .
O1 O 0.8548(5) 0.3376(5) 0.9822(4) 0.0097(7) Uani 1 1 d . . .
O2 O 0.9123(6) 0.6274(5) 0.8187(4) 0.0109(7) Uani 1 1 d . . .
O3 O 0.5473(6) 0.6225(5) 0.8626(4) 0.0108(7) Uani 1 1 d . . .
O4 O 0.8516(6) 0.3909(6) 0.4532(4) 0.0176(8) Uani 1 1 d . . .
O5 O 0.5596(6) 0.5894(6) 0.5844(4) 0.0135(7) Uani 1 1 d . . .
O6 O 0.1571(7) 0.8777(6) 0.7322(4) 0.0152(8) Uani 1 1 d . . .
O7 O 0.3750(7) 0.3427(6) 0.8054(4) 0.0147(8) Uani 1 1 d . . .
O8 O 0.6861(10) -0.0030(9) 0.5900(5) 0.0426(14) Uani 1 1 d . . .
O9 O 0.7365(6) -0.0022(6) 0.9951(4) 0.0161(8) Uani 1 1 d . . .
C1 C 0.8658(8) 0.3439(8) 0.7016(5) 0.0119(10) Uani 1 1 d . . .
H1A H 1.0253 0.2957 0.6724 0.014 Uiso 1 1 calc R . .
H1B H 0.8355 0.2232 0.7360 0.014 Uiso 1 1 calc R . .
C2 C 0.7513(8) 0.4519(8) 0.5709(6) 0.0118(10) 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'
Na Na 0.0362 0.0249 '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'
Cu Cu 0.3201 1.2651 '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
O6 U1 O7 178.33(16) . . ?
O6 U1 O2 90.64(16) . 1_455 ?
O7 U1 O2 90.69(16) . 1_455 ?
O6 U1 O3 87.94(16) . . ?
O7 U1 O3 91.52(16) . . ?
O2 U1 O3 146.06(13) 1_455 . ?
O6 U1 O1 87.18(16) . 2_667 ?
O7 U1 O1 94.15(16) . 2_667 ?
O2 U1 O1 73.99(12) 1_455 2_667 ?
O3 U1 O1 72.07(12) . 2_667 ?
O6 U1 O5 88.05(16) . . ?
O7 U1 O5 90.28(16) . . ?
O2 U1 O5 143.98(12) 1_455 . ?
O3 U1 O5 69.87(12) . . ?
O1 U1 O5 141.78(12) 2_667 . ?
O6 U1 O4 87.01(17) . 2_666 ?
O7 U1 O4 92.45(16) . 2_666 ?
O2 U1 O4 71.80(12) 1_455 2_666 ?
O3 U1 O4 141.86(13) . 2_666 ?
O1 U1 O4 145.20(12) 2_667 2_666 ?
O5 U1 O4 72.19(12) . 2_666 ?
O6 U1 Na1 54.74(13) . 1_565 ?
O7 U1 Na1 124.57(13) . 1_565 ?
O2 U1 Na1 136.18(9) 1_455 1_565 ?
O3 U1 Na1 33.54(9) . 1_565 ?
O1 U1 Na1 77.94(9) 2_667 1_565 ?
O5 U1 Na1 68.51(10) . 1_565 ?
O4 U1 Na1 124.56(10) 2_666 1_565 ?
O3 P1 O2 108.7(2) . . ?
O3 P1 O1 111.2(2) . . ?
O2 P1 O1 112.4(2) . . ?
O3 P1 C1 108.8(2) . . ?
O2 P1 C1 109.2(2) . . ?
O1 P1 C1 106.3(2) . . ?
O3 P1 Na1 52.61(15) . 1_565 ?
O2 P1 Na1 56.14(14) . 1_565 ?
O1 P1 Na1 129.20(15) . 1_565 ?
C1 P1 Na1 124.44(18) . 1_565 ?
O8 Na1 O9 149.4(2) . 2_657 ?
O8 Na1 O9 119.4(2) . . ?
O9 Na1 O9 86.41(15) 2_657 . ?
O8 Na1 O3 104.23(19) . 1_545 ?
O9 Na1 O3 77.39(14) 2_657 1_545 ?
O9 Na1 O3 112.49(16) . 1_545 ?
O8 Na1 O7 86.60(19) . . ?
O9 Na1 O7 80.31(15) 2_657 . ?
O9 Na1 O7 82.83(15) . . ?
O3 Na1 O7 151.82(16) 1_545 . ?
O8 Na1 O2 81.58(18) . 1_545 ?
O9 Na1 O2 122.01(15) 2_657 1_545 ?
O9 Na1 O2 79.10(14) . 1_545 ?
O3 Na1 O2 58.31(12) 1_545 1_545 ?
O7 Na1 O2 149.86(15) . 1_545 ?
O8 Na1 P1 93.49(17) . 1_545 ?
O9 Na1 P1 100.03(12) 2_657 1_545 ?
O9 Na1 P1 96.34(12) . 1_545 ?
O3 Na1 P1 28.97(9) 1_545 1_545 ?
O7 Na1 P1 179.09(14) . 1_545 ?
O2 Na1 P1 29.35(8) 1_545 1_545 ?
O8 Na1 Na1 158.0(2) . 2_657 ?
O9 Na1 Na1 43.22(11) 2_657 2_657 ?
O9 Na1 Na1 43.19(11) . 2_657 ?
O3 Na1 Na1 96.47(13) 1_545 2_657 ?
O7 Na1 Na1 78.40(12) . 2_657 ?
O2 Na1 Na1 103.52(13) 1_545 2_657 ?
P1 Na1 Na1 101.26(10) 1_545 2_657 ?
O8 Na1 U1 94.24(16) . 1_545 ?
O9 Na1 U1 71.14(11) 2_657 1_545 ?
O9 Na1 U1 139.56(13) . 1_545 ?
O3 Na1 U1 31.21(9) 1_545 1_545 ?
O7 Na1 U1 123.76(12) . 1_545 ?
O2 Na1 U1 84.88(10) 1_545 1_545 ?
P1 Na1 U1 57.14(4) 1_545 1_545 ?
Na1 Na1 U1 107.49(9) 2_657 1_545 ?
P1 O1 U1 129.1(2) . 2_667 ?
P1 O2 U1 140.9(2) . 1_655 ?
P1 O2 Na1 94.51(17) . 1_565 ?
U1 O2 Na1 124.50(16) 1_655 1_565 ?
P1 O3 U1 132.1(2) . . ?
P1 O3 Na1 98.42(18) . 1_565 ?
U1 O3 Na1 115.26(15) . 1_565 ?
C2 O4 U1 134.1(3) . 2_666 ?
C2 O5 U1 128.9(3) . . ?
U1 O7 Na1 173.0(2) . . ?
Na1 O9 Na1 93.59(15) 2_657 . ?
C2 C1 P1 116.1(4) . . ?
C2 C1 H1A 108.2 . . ?
P1 C1 H1A 108.2 . . ?
C2 C1 H1B 108.2 . . ?
P1 C1 H1B 108.2 . . ?
H1A C1 H1B 107.4 . . ?
O4 C2 O5 123.0(5) . . ?
O4 C2 C1 117.0(5) . . ?
O5 C2 C1 119.9(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 O6 1.773(4) . ?
U1 O7 1.779(4) . ?
U1 O2 2.314(3) 1_455 ?
U1 O3 2.339(4) . ?
U1 O1 2.404(3) 2_667 ?
U1 O5 2.408(4) . ?
U1 O4 2.442(4) 2_666 ?
U1 Na1 4.083(2) 1_565 ?
P1 O3 1.520(4) . ?
P1 O2 1.527(4) . ?
P1 O1 1.537(4) . ?
P1 C1 1.809(5) . ?
P1 Na1 3.105(3) 1_565 ?
Na1 O8 2.265(5) . ?
Na1 O9 2.351(4) 2_657 ?
Na1 O9 2.352(5) . ?
Na1 O3 2.494(4) 1_545 ?
Na1 O7 2.538(5) . ?
Na1 O2 2.587(4) 1_545 ?
Na1 P1 3.105(3) 1_545 ?
Na1 Na1 3.428(5) 2_657 ?
Na1 U1 4.083(2) 1_545 ?
O1 U1 2.403(3) 2_667 ?
O2 U1 2.314(3) 1_655 ?
O2 Na1 2.587(4) 1_565 ?
O3 Na1 2.494(4) 1_565 ?
O4 C2 1.256(6) . ?
O4 U1 2.442(4) 2_666 ?
O5 C2 1.262(6) . ?
O9 Na1 2.351(4) 2_657 ?
C1 C2 1.517(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
