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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/13/4301324.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_4301324
loop_
_publ_author_name
'Grigory B. Andreev'
'Nina A. Budantseva'
'Ivan G. Tananaev'
'Boris F. Myasoedov'
_publ_contact_author_address
;
A. N. Frumkin Institute of Physical Chemistry and 
Electrochemistry, 31 Leninskiy pr., Moscow, 119991, Russia
;
_publ_contact_author_email       grigory_andreev@mail.ru
_publ_contact_author_name        'Grigory Andreev'
_publ_section_title
;
Interaction of Transuranium Elements with Biologically Important Molecules:
Structural and Spectroscopic Study of Np(V) Complexes with Imidazole
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1232
_journal_page_last               1235
_journal_paper_doi               10.1021/ic801882p
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C8 H11 N4 Np1 O5'
_chemical_formula_sum            'C8 H11 N4 Np O5'
_chemical_formula_weight         480.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6132(12)
_cell_length_b                   10.5746(8)
_cell_length_c                   7.9019(6)
_cell_measurement_temperature    100(2)
_cell_volume                     1304.63(17)
_computing_cell_refinement       'APEX 2 (Bruker, 2006)'
_computing_data_collection       'APEX 2 (Bruker, 2006)'
_computing_data_reduction        'APEX 2 (Bruker, 2006)'
_computing_molecular_graphics    'APEX 2 (Bruker, 2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Kappa APEX II area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0132
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2511
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    7.984
_exptl_absorpt_correction_T_max  0.29
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'APEX 2 (Bruker, 2006)'
_exptl_crystal_density_diffrn    2.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.408
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1738
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0262
_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)+(0.0550P)²+2.9500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                1623
_reflns_number_total             1738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801882p_si_001_1.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C8 H11 N4 Np1 O5'
_cod_database_code               4301324
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'
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 0.182204(17) 0.44727(3) 0.02472(9) Uani 1 2 d SD . .
C5 C 0.5000 0.4571(4) 0.447(5) 0.0087(6) Uani 1 2 d SU . .
C4 C 0.5000 0.5989(7) 0.441(3) 0.045(2) Uani 1 2 d SU . .
O3 O 0.5000 -0.0447(5) 0.435(3) 0.0324(19) Uani 1 2 d S A .
N1 N 0.3467(3) 0.1334(5) 0.5366(9) 0.0359(10) Uani 1 1 d . A .
C1 C 0.2976(3) 0.0411(7) 0.450(5) 0.070(3) Uani 1 1 d . . .
H1 H 0.3126 -0.0104 0.3594 0.084 Uiso 1 1 calc R A .
N2 N 0.2174(3) 0.0493(5) 0.5429(9) 0.0351(11) Uani 1 1 d . A .
H2A H 0.1772 -0.0062 0.5381 0.042 Uiso 1 1 calc R . .
C3 C 0.2945(4) 0.2085(7) 0.6394(10) 0.0376(12) Uani 1 1 d U . .
H3A H 0.3114 0.2807 0.6977 0.045 Uiso 1 1 calc R A .
C2 C 0.2142(4) 0.1572(8) 0.6391(11) 0.0411(14) Uani 1 1 d U A .
H2B H 0.1663 0.1895 0.6940 0.049 Uiso 1 1 calc R . .
O4 O 0.5684(2) 0.3988(4) 0.457(3) 0.068(2) Uani 1 1 d U A .
O1 O 0.4731(12) 0.1808(9) 0.6721(15) 0.020(4) Uani 0.50 1 d PDU A -1
O2 O 0.5392(14) 0.1837(11) 0.2288(16) 0.030(4) Uani 0.50 1 d PD A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Np Np -11.4937 4.1493 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
O1 Np1 O1 26.6(12) 4_655 . ?
O1 Np1 O2 147.2(6) 4_655 . ?
O1 Np1 O2 173.8(12) . . ?
O1 Np1 O2 173.8(12) 4_655 4_655 ?
O1 Np1 O2 147.2(6) . 4_655 ?
O2 Np1 O2 39.0(14) . 4_655 ?
O1 Np1 O3 91.8(5) 4_655 . ?
O1 Np1 O3 91.8(5) . . ?
O2 Np1 O3 88.3(6) . . ?
O2 Np1 O3 88.3(6) 4_655 . ?
O1 Np1 O4 94.3(6) 4_655 4_655 ?
O1 Np1 O4 83.1(6) . 4_655 ?
O2 Np1 O4 99.3(6) . 4_655 ?
O2 Np1 O4 83.1(6) 4_655 4_655 ?
O3 Np1 O4 155.02(9) . 4_655 ?
O1 Np1 O4 83.1(6) 4_655 . ?
O1 Np1 O4 94.3(6) . . ?
O2 Np1 O4 83.1(6) . . ?
O2 Np1 O4 99.3(6) 4_655 . ?
O3 Np1 O4 155.02(9) . . ?
O4 Np1 O4 49.96(17) 4_655 . ?
O1 Np1 N1 86.9(6) 4_655 . ?
O1 Np1 N1 60.8(6) . . ?
O2 Np1 N1 125.2(7) . . ?
O2 Np1 N1 87.1(7) 4_655 . ?
O3 Np1 N1 78.99(19) . . ?
O4 Np1 N1 77.19(18) 4_655 . ?
O4 Np1 N1 124.9(3) . . ?
O1 Np1 N1 60.8(6) 4_655 4_655 ?
O1 Np1 N1 86.9(6) . 4_655 ?
O2 Np1 N1 87.1(7) . 4_655 ?
O2 Np1 N1 125.2(7) 4_655 4_655 ?
O3 Np1 N1 79.00(19) . 4_655 ?
O4 Np1 N1 124.9(3) 4_655 4_655 ?
O4 Np1 N1 77.19(18) . 4_655 ?
N1 Np1 N1 139.9(3) . 4_655 ?
O1 Np1 C5 90.6(8) 4_655 . ?
O1 Np1 C5 90.6(8) . . ?
O2 Np1 C5 89.4(8) . . ?
O2 Np1 C5 89.4(8) 4_655 . ?
O3 Np1 C5 177.5(7) . . ?
O4 Np1 C5 25.06(10) 4_655 . ?
O4 Np1 C5 25.06(10) . . ?
N1 Np1 C5 101.7(2) . . ?
N1 Np1 C5 101.7(2) 4_655 . ?
O4 C5 O4 119.5(7) 4_655 . ?
O4 C5 C4 120.0(3) 4_655 . ?
O4 C5 C4 120.0(3) . . ?
O4 C5 Np1 60.1(2) 4_655 . ?
O4 C5 Np1 60.1(2) . . ?
C4 C5 Np1 178(3) . . ?
C3 N1 C1 110.8(8) . . ?
C3 N1 Np1 126.4(4) . . ?
C1 N1 Np1 120.9(10) . . ?
N1 C1 N2 100.5(19) . . ?
C2 N2 C1 111.1(9) . . ?
C2 C3 N1 108.0(6) . . ?
C3 C2 N2 107.3(6) . . ?
C5 O4 Np1 94.9(3) . . ?
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 1.826(11) 4_655 ?
Np1 O1 1.826(11) . ?
Np1 O2 1.831(11) . ?
Np1 O2 1.831(11) 4_655 ?
Np1 O3 2.402(5) . ?
Np1 O4 2.528(4) 4_655 ?
Np1 O4 2.528(4) . ?
Np1 N1 2.548(5) . ?
Np1 N1 2.548(5) 4_655 ?
Np1 C5 2.906(4) . ?
C5 O4 1.235(5) 4_655 ?
C5 O4 1.235(5) . ?
C5 C4 1.500(9) . ?
N1 C3 1.399(9) . ?
N1 C1 1.42(2) . ?
C1 N2 1.454(18) . ?
N2 C2 1.372(10) . ?
C3 C2 1.365(9) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Np1 C5 O4 -72(2) . . . 4_655 ?
O2 Np1 C5 O4 114(2) . . . 4_655 ?
O4 Np1 C5 O4 -171(4) . . . 4_655 ?
N1 Np1 C5 O4 -12(2) . . . 4_655 ?
N1 Np1 C5 O4 -159(2) 4_655 . . 4_655 ?
O1 Np1 C5 O4 72(2) 4_655 . . . ?
O1 Np1 C5 O4 99(2) . . . . ?
O2 Np1 C5 O4 -75(2) . . . . ?
O2 Np1 C5 O4 -114(2) 4_655 . . . ?
N1 Np1 C5 O4 159(2) . . . . ?
N1 Np1 C5 O4 12(2) 4_655 . . . ?
O1 Np1 N1 C3 60.7(7) 4_655 . . . ?
O1 Np1 N1 C3 54.8(6) . . . . ?
O2 Np1 N1 C3 -126.9(7) . . . . ?
O2 Np1 N1 C3 -118.1(7) 4_655 . . . ?
O4 Np1 N1 C3 -34.4(8) 4_655 . . . ?
O4 Np1 N1 C3 -18.7(9) . . . . ?
C5 Np1 N1 C3 -29.3(9) . . . . ?
O1 Np1 N1 C1 -136.0(11) 4_655 . . . ?
O1 Np1 N1 C1 -141.9(11) . . . . ?
O2 Np1 N1 C1 36.4(12) . . . . ?
O2 Np1 N1 C1 45.3(11) 4_655 . . . ?
O3 Np1 N1 C1 -43.5(12) . . . . ?
O4 Np1 N1 C1 128.9(12) 4_655 . . . ?
O4 Np1 N1 C1 144.6(12) . . . . ?
N1 Np1 N1 C1 -101.4(11) 4_655 . . . ?
C5 Np1 N1 C1 134.0(13) . . . . ?
C3 N1 C1 N2 -13.4(15) . . . . ?
Np1 N1 C1 N2 -179.1(6) . . . . ?
N1 C1 N2 C2 15.0(16) . . . . ?
C1 N1 C3 C2 7.7(14) . . . . ?
Np1 N1 C3 C2 172.4(5) . . . . ?
N1 C3 C2 N2 2.2(9) . . . . ?
C1 N2 C2 C3 -11.2(14) . . . . ?
O4 C5 O4 Np1 9(4) 4_655 . . . ?
O1 Np1 O4 C5 -106(2) 4_655 . . . ?
O1 Np1 O4 C5 -82(2) . . . . ?
O2 Np1 O4 C5 103(2) . . . . ?
O3 Np1 O4 C5 174.2(17) . . . . ?
O4 Np1 O4 C5 -5(2) 4_655 . . . ?
