# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Linfeng Rao'
_publ_contact_author_email       LRAO@LBL.GOV

_publ_section_title              
;
A comparative study of the complexation
of Np(V) with N,N-dimethyl-3-oxa-glutaramic acid and related
ligands: thermodynamics, optical properties and structural aspects
;
loop_
_publ_author_name
'Linfeng Rao.'
'Simon J. Teat'
'Guoxin Tian'

# Attachment 'NPDMOGA2.CIF'

data_npdmoga2
_database_code_depnum_ccdc_archive 'CCDC 745530'
#TrackingRef 'NPDMOGA2.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
'Neptunyl(V) N,N-dimethyl-3-oxa-glutaramate monohydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H14 N Np O8'
_chemical_formula_weight         465.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Np Np -7.7000 4.7872
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Cmc2(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   7.161(2)
_cell_length_b                   16.659(5)
_cell_length_c                   9.536(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1137.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    6073
_cell_measurement_theta_min      4.10
_cell_measurement_theta_max      33.49

_exptl_crystal_description       block
_exptl_crystal_colour            'pale blue'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    7.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_process_details   'SADABS 2004/1 Bruker AXS Madison WI USA'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            8249
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.10
_diffrn_reflns_theta_max         33.53
_reflns_number_total             1824
_reflns_number_gt                1758
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v7.34a'
_computing_data_reduction        'Bruker SAINT v7.34a'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
All non-hydrogen atom were refined anisotropically. Hydrogen were placed
geometrical, for the CH2 groups and refined using a riding model. The
methyl and water hydrogens could neither be found in the difference map
nor placed geometrically and were therefore omitted from the refinement.
Displacement parameter restrains were used on the ligand, even with these
the ratio max:min for some atom is a little greater than 4:1.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_number_reflns         1824
_refine_ls_number_parameters     94
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0733
_refine_ls_wR_factor_gt          0.0728
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Np1 Np 0.5000 0.889344(10) 0.66463(11) 0.02246(9) Uani 1 2 d S . .
O1 O 0.7560(7) 0.8883(2) 0.667(2) 0.0383(12) Uani 1 1 d . . .
O3 O 0.5000 0.9586(4) 0.4340(7) 0.0348(15) Uani 1 2 d S . .
O4 O 0.5000 0.9641(5) 0.2005(7) 0.0371(17) Uani 1 2 d S . .
C1 C 0.5000 0.9268(5) 0.3166(9) 0.0229(14) Uani 1 2 d SU . .
C2 C 0.5000 0.8374(6) 0.3045(9) 0.0281(17) Uani 1 2 d SU . .
H2A H 0.3879 0.8194 0.2525 0.034 Uiso 0.50 1 calc PR . .
H2B H 0.6121 0.8194 0.2525 0.034 Uiso 0.50 1 calc PR . .
O5 O 0.5000 0.8033(3) 0.4433(6) 0.0232(11) Uani 1 2 d SU . .
C3 C 0.5000 0.7171(5) 0.4388(8) 0.0233(14) Uani 1 2 d SU . .
H3A H 0.6123 0.6971 0.3893 0.028 Uiso 0.50 1 calc PR . .
H3B H 0.3877 0.6971 0.3893 0.028 Uiso 0.50 1 calc PR . .
C4 C 0.5000 0.6891(4) 0.5901(7) 0.0203(13) Uani 1 2 d SU . .
O6 O 0.5000 0.7412(4) 0.6852(8) 0.0328(17) Uani 1 2 d SU . .
N1 N 0.5000 0.6127(4) 0.6151(11) 0.0274(18) Uani 1 2 d SU . .
C5 C 0.5000 0.5810(7) 0.7566(10) 0.0295(18) Uani 1 2 d SU . .
C6 C 0.5000 0.5511(6) 0.5037(9) 0.0321(17) Uani 1 2 d SU . .
O1W O 0.5000 0.8629(5) 0.9254(9) 0.0412(15) Uani 1 2 d SU . .
O2W O 1.0000 0.7847(4) 0.5368(7) 0.0396(15) Uani 1 2 d SU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Np1 0.03872(15) 0.01144(13) 0.01721(12) -0.0009(2) 0.000 0.000
O1 0.036(2) 0.035(3) 0.044(3) -0.014(4) -0.012(6) 0.0000(13)
O3 0.051(4) 0.027(4) 0.026(3) -0.001(3) 0.000 0.000
O4 0.055(4) 0.025(3) 0.032(4) 0.009(2) 0.000 0.000
C1 0.032(3) 0.013(3) 0.024(3) 0.002(2) 0.000 0.000
C2 0.051(4) 0.016(4) 0.017(3) -0.004(3) 0.000 0.000
O5 0.043(3) 0.009(2) 0.017(2) 0.0014(17) 0.000 0.000
C3 0.043(4) 0.010(3) 0.018(3) -0.001(2) 0.000 0.000
C4 0.030(2) 0.014(2) 0.017(2) 0.0030(19) 0.000 0.000
O6 0.049(2) 0.019(2) 0.031(3) 0.000(2) 0.000 0.000
N1 0.051(5) 0.015(4) 0.016(3) -0.001(2) 0.000 0.000
C5 0.045(4) 0.023(4) 0.020(3) 0.006(3) 0.000 0.000
C6 0.049(4) 0.020(3) 0.027(3) -0.008(3) 0.000 0.000
O1W 0.068(4) 0.024(3) 0.031(3) -0.004(3) 0.000 0.000
O2W 0.065(4) 0.028(3) 0.026(3) -0.005(3) 0.000 0.000

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Np1 O1 1.833(5) . ?
Np1 O1 1.833(5) 4_655 ?
Np1 O3 2.484(7) . ?
Np1 O4 2.466(8) 2_675 ?
Np1 O5 2.552(6) . ?
Np1 O6 2.476(7) . ?
Np1 O1W 2.526(8) . ?
O3 C1 1.238(11) . ?
O4 Np1 2.466(8) 2_674 ?
O4 C1 1.269(10) . ?
C1 C2 1.495(13) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 O5 1.440(10) . ?
O5 C3 1.436(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.516(10) . ?
C4 O6 1.255(10) . ?
C4 N1 1.295(9) . ?
N1 C5 1.449(15) . ?
N1 C6 1.476(12) . ?

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
O1 Np1 O1 178.4(10) . 4_655 ?
O1 Np1 O3 90.8(6) . . ?
O1 Np1 O3 90.8(6) 4_655 . ?
O1 Np1 O4 90.44(12) 4_655 2_675 ?
O1 Np1 O4 90.44(12) . 2_675 ?
O1 Np1 O5 90.2(5) . . ?
O1 Np1 O5 90.2(5) 4_655 . ?
O1 Np1 O6 89.43(16) . . ?
O1 Np1 O6 89.43(16) 4_655 . ?
O1 Np1 O1W 89.3(6) . . ?
O1 Np1 O1W 89.3(6) 4_655 . ?
O3 Np1 O4 70.3(2) . 2_675 ?
O3 Np1 O5 61.9(2) . . ?
O3 Np1 O6 122.2(3) . . ?
O3 Np1 O1W 162.4(3) . . ?
O4 Np1 O5 132.2(2) 2_675 . ?
O4 Np1 O6 167.5(3) 2_675 . ?
O4 Np1 O1W 92.1(2) 2_675 . ?
O5 Np1 O6 60.3(2) . . ?
O5 Np1 O1W 135.7(2) . . ?
O6 Np1 O1W 75.4(3) . . ?
Np1 O3 C1 127.1(6) . . ?
Np1 O4 C1 127.2(6) 2_674 . ?
O3 C1 O4 125.5(8) . . ?
O3 C1 C2 119.7(7) . . ?
O4 C1 C2 114.8(7) . . ?
C1 C2 H2A 109.9 . . ?
C1 C2 H2B 109.9 . . ?
C1 C2 O5 108.8(6) . . ?
H2A C2 H2B 108.3 . . ?
H2A C2 O5 109.9 . . ?
H2B C2 O5 109.9 . . ?
Np1 O5 C2 122.6(5) . . ?
Np1 O5 C3 125.9(5) . . ?
C2 O5 C3 111.5(6) . . ?
O5 C3 H3A 110.5 . . ?
O5 C3 H3B 110.5 . . ?
O5 C3 C4 106.2(6) . . ?
H3A C3 H3B 108.7 . . ?
H3A C3 C4 110.5 . . ?
H3B C3 C4 110.5 . . ?
C3 C4 O6 118.3(7) . . ?
C3 C4 N1 118.5(7) . . ?
O6 C4 N1 123.1(8) . . ?
Np1 O6 C4 129.2(6) . . ?
C4 N1 C5 121.9(8) . . ?
C4 N1 C6 123.4(9) . . ?
C5 N1 C6 114.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.029
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.189