#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:29:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179248 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/68/4316826.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_4316826
loop_
_publ_author_name
'Denise Girnt'
'Peter W. Roesky'
'Andreas Geist'
'Christian M. Ruff'
'Petra J. Panak'
'Melissa A. Denecke'
_publ_contact_author
;
      Prof. Dr. Peter Roesky
      Institut für Anorganische Chemie
      KIT
      Engesserstraße 15
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_publ_contact_author_fax         +49/(0)7216084854
_publ_contact_author_phone       +49/(0)7216086117
_publ_section_title
;
 6-(3,5-Dimethyl-1H-pyrazol-1-yl)-2,2'-bipyridine as Ligand for
 Actinide(III)/Lanthanide(III) Separation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9627
_journal_page_last               9635
_journal_paper_doi               10.1021/ic101309j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C17 H20 N7 O10 S Sm'
_chemical_formula_sum            'C17 H20 N7 O10 S Sm'
_chemical_formula_weight         664.81
_chemical_name_common            '[Sm(dmpbipy)(NO3)3(DMSO)]'
_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                85.30(3)
_cell_angle_beta                 86.30(3)
_cell_angle_gamma                88.61(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4637(19)
_cell_length_b                   10.825(2)
_cell_length_c                   11.554(2)
_cell_measurement_reflns_used    18031
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      1.77
_cell_volume                     1177.0(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'WinGX32, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13712
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    2.651
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.780
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0307
_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)+(0.0390P)²+1.0461P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                5059
_reflns_number_total             5577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101309j_si_001_2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1176.9(4)
_cod_database_code               4316826
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
Sm Sm 0.715576(17) 0.802202(15) 0.771095(14) 0.03086(6) Uani 1 1 d . . .
S1 S 0.61651(10) 0.61919(8) 1.03569(8) 0.04089(19) Uani 1 1 d . . .
O4 O 0.5186(3) 0.9591(3) 0.8161(2) 0.0472(6) Uani 1 1 d . . .
N2 N 0.9523(3) 0.9045(2) 0.6882(2) 0.0312(5) Uani 1 1 d . . .
N4 N 0.8245(3) 0.7407(3) 0.5721(3) 0.0381(6) Uani 1 1 d . . .
N5 N 0.8782(4) 0.5671(3) 0.8142(3) 0.0452(7) Uani 1 1 d . . .
O7 O 0.5111(3) 0.7958(3) 0.6381(3) 0.0488(6) Uani 1 1 d . . .
O5 O 0.6632(3) 1.0110(2) 0.6706(2) 0.0429(6) Uani 1 1 d . . .
N6 N 0.5522(3) 1.0367(3) 0.7318(3) 0.0413(7) Uani 1 1 d . . .
O9 O 0.4833(3) 0.6822(3) 0.7986(3) 0.0549(7) Uani 1 1 d . . .
C6 C 1.0076(3) 0.9980(3) 0.7415(3) 0.0327(6) Uani 1 1 d . . .
O10 O 0.6733(3) 0.7383(3) 0.9714(2) 0.0470(6) Uani 1 1 d . . .
C12 C 0.9095(4) 0.6268(4) 0.4277(3) 0.0449(8) Uani 1 1 d . . .
H12 H 0.9128 0.5703 0.3711 0.054 Uiso 1 1 calc R . .
C7 C 1.1377(4) 1.0492(3) 0.7042(3) 0.0386(7) Uani 1 1 d . . .
H7 H 1.1741 1.1124 0.7427 0.046 Uiso 1 1 calc R . .
C10 C 1.0276(3) 0.8634(3) 0.5968(3) 0.0324(6) Uani 1 1 d . . .
N1 N 0.8148(3) 0.9711(3) 0.8877(3) 0.0346(6) Uani 1 1 d . . .
O8 O 0.3248(4) 0.6815(3) 0.6711(4) 0.0660(9) Uani 1 1 d . . .
O2 O 0.7527(3) 0.5690(2) 0.7818(3) 0.0464(6) Uani 1 1 d . . .
O3 O 0.9337(3) 0.6703(3) 0.8220(3) 0.0510(7) Uani 1 1 d . . .
C5 C 0.9247(3) 1.0418(3) 0.8439(3) 0.0329(6) Uani 1 1 d . . .
O6 O 0.4817(3) 1.1314(3) 0.7099(3) 0.0615(9) Uani 1 1 d . . .
C11 C 1.0188(4) 0.6988(3) 0.4539(3) 0.0405(7) Uani 1 1 d . . .
C15 C 1.1664(4) 0.6972(4) 0.4000(4) 0.0523(10) Uani 1 1 d . . .
H15A H 1.2216 0.7564 0.4339 0.078 Uiso 1 1 calc R . .
H15B H 1.1647 0.7183 0.3177 0.078 Uiso 1 1 calc R . .
H15C H 1.2078 0.6159 0.4136 0.078 Uiso 1 1 calc R . .
O1 O 0.9410(4) 0.4697(3) 0.8372(4) 0.0752(10) Uani 1 1 d . . .
N3 N 0.9654(3) 0.7678(3) 0.5418(3) 0.0356(6) Uani 1 1 d . . .
C14 C 0.6490(5) 0.5989(4) 0.5055(4) 0.0547(11) Uani 1 1 d . . .
H14A H 0.5884 0.6344 0.5644 0.082 Uiso 1 1 calc R . .
H14B H 0.6569 0.5108 0.5231 0.082 Uiso 1 1 calc R . .
H14C H 0.6095 0.6158 0.4312 0.082 Uiso 1 1 calc R . .
N7 N 0.4361(3) 0.7197(3) 0.7021(3) 0.0430(7) Uiso 1 1 d . . .
C13 C 0.7925(4) 0.6543(4) 0.5019(3) 0.0416(8) Uani 1 1 d . . .
C1 C 0.7414(4) 1.0070(3) 0.9840(3) 0.0387(7) Uani 1 1 d . . .
H1 H 0.6667 0.9585 1.0159 0.046 Uiso 1 1 calc R . .
C8 C 1.2119(4) 1.0045(4) 0.6091(3) 0.0405(8) Uani 1 1 d . . .
H8 H 1.2992 1.0374 0.5831 0.049 Uiso 1 1 calc R . .
C9 C 1.1570(4) 0.9118(4) 0.5529(3) 0.0404(7) Uani 1 1 d . . .
H9 H 1.2045 0.8822 0.4875 0.048 Uiso 1 1 calc R . .
C2 C 0.7715(4) 1.1113(4) 1.0369(3) 0.0428(8) Uani 1 1 d . . .
H2 H 0.7184 1.1321 1.1033 0.051 Uiso 1 1 calc R . .
C3 C 0.8809(4) 1.1845(4) 0.9908(4) 0.0467(9) Uani 1 1 d . . .
H3 H 0.9028 1.2560 1.0249 0.056 Uiso 1 1 calc R . .
C4 C 0.9576(4) 1.1496(4) 0.8928(3) 0.0430(8) Uani 1 1 d . . .
H4 H 1.0315 1.1983 0.8595 0.052 Uiso 1 1 calc R . .
C17 C 0.4536(6) 0.6602(5) 1.1046(6) 0.0696(15) Uani 1 1 d . . .
H17A H 0.3838 0.6730 1.0479 0.104 Uiso 1 1 calc R . .
H17B H 0.4635 0.7351 1.1421 0.104 Uiso 1 1 calc R . .
H17C H 0.4242 0.5948 1.1617 0.104 Uiso 1 1 calc R . .
C16 C 0.7154(7) 0.6012(6) 1.1623(6) 0.095(2) Uani 1 1 d . . .
H16A H 0.8116 0.5782 1.1407 0.143 Uiso 1 1 calc R . .
H16B H 0.6742 0.5376 1.2159 0.143 Uiso 1 1 calc R . .
H16C H 0.7139 0.6780 1.1984 0.143 Uiso 1 1 calc R . .
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'
Sm Sm -0.1638 3.4418 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O10 Sm O5 127.42(10) . . ?
O10 Sm O2 75.81(10) . . ?
O5 Sm O2 154.57(10) . . ?
O10 Sm O4 82.48(10) . . ?
O5 Sm O4 50.19(9) . . ?
O2 Sm O4 138.58(9) . . ?
O10 Sm O7 118.36(10) . . ?
O5 Sm O7 68.00(9) . . ?
O2 Sm O7 92.77(10) . . ?
O4 Sm O7 67.24(9) . . ?
O10 Sm O3 75.75(11) . . ?
O5 Sm O3 137.61(9) . . ?
O2 Sm O3 50.02(9) . . ?
O4 Sm O3 152.96(10) . . ?
O7 Sm O3 137.91(10) . . ?
O10 Sm O9 71.21(10) . . ?
O5 Sm O9 107.92(10) . . ?
O2 Sm O9 66.68(10) . . ?
O4 Sm O9 73.10(10) . . ?
O7 Sm O9 49.50(9) . . ?
O3 Sm O9 113.60(10) . . ?
O10 Sm N1 72.73(9) . . ?
O5 Sm N1 71.18(9) . . ?
O2 Sm N1 131.94(10) . . ?
O4 Sm N1 71.00(9) . . ?
O7 Sm N1 134.16(10) . . ?
O3 Sm N1 87.17(10) . . ?
O9 Sm N1 131.51(10) . . ?
O10 Sm N4 145.58(10) . . ?
O5 Sm N4 86.90(10) . . ?
O2 Sm N4 71.19(10) . . ?
O4 Sm N4 129.69(10) . . ?
O7 Sm N4 73.35(10) . . ?
O3 Sm N4 75.75(11) . . ?
O9 Sm N4 103.52(10) . . ?
N1 Sm N4 124.41(9) . . ?
O10 Sm N2 122.19(10) . . ?
O5 Sm N2 70.45(9) . . ?
O2 Sm N2 108.01(9) . . ?
O4 Sm N2 113.41(9) . . ?
O7 Sm N2 118.97(9) . . ?
O3 Sm N2 67.25(9) . . ?
O9 Sm N2 164.94(10) . . ?
N1 Sm N2 62.92(9) . . ?
N4 Sm N2 61.66(9) . . ?
O10 Sm N6 105.69(10) . . ?
O5 Sm N6 25.10(9) . . ?
O2 Sm N6 155.00(9) . . ?
O4 Sm N6 25.12(9) . . ?
O7 Sm N6 64.17(9) . . ?
O3 Sm N6 154.98(9) . . ?
O9 Sm N6 89.85(10) . . ?
N1 Sm N6 70.01(9) . . ?
N4 Sm N6 108.32(10) . . ?
N2 Sm N6 92.46(9) . . ?
O10 Sm N5 73.46(10) . . ?
O5 Sm N5 155.60(9) . . ?
O2 Sm N5 25.11(9) . . ?
O4 Sm N5 154.13(10) . . ?
O7 Sm N5 116.26(10) . . ?
O3 Sm N5 24.94(9) . . ?
O9 Sm N5 89.95(10) . . ?
N1 Sm N5 109.54(10) . . ?
N4 Sm N5 72.53(10) . . ?
N2 Sm N5 87.94(9) . . ?
N6 Sm N5 179.15(9) . . ?
O10 S1 C17 105.9(2) . . ?
O10 S1 C16 103.5(2) . . ?
C17 S1 C16 97.5(4) . . ?
N6 O4 Sm 95.9(2) . . ?
C10 N2 C6 117.3(3) . . ?
C10 N2 Sm 122.0(2) . . ?
C6 N2 Sm 120.6(2) . . ?
C13 N4 N3 105.0(3) . . ?
C13 N4 Sm 133.1(2) . . ?
N3 N4 Sm 118.5(2) . . ?
O1 N5 O3 122.0(4) . . ?
O1 N5 O2 121.1(4) . . ?
O3 N5 O2 116.9(3) . . ?
O1 N5 Sm 176.7(3) . . ?
O3 N5 Sm 58.91(19) . . ?
O2 N5 Sm 58.04(17) . . ?
N7 O7 Sm 97.3(2) . . ?
N6 O5 Sm 97.7(2) . . ?
O6 N6 O4 122.3(4) . . ?
O6 N6 O5 121.7(4) . . ?
O4 N6 O5 116.0(3) . . ?
O6 N6 Sm 176.3(3) . . ?
O4 N6 Sm 58.99(18) . . ?
O5 N6 Sm 57.16(18) . . ?
N7 O9 Sm 96.6(2) . . ?
N2 C6 C7 122.1(3) . . ?
N2 C6 C5 117.1(3) . . ?
C7 C6 C5 120.8(3) . . ?
S1 O10 Sm 132.84(16) . . ?
C11 C12 C13 107.3(3) . . ?
C8 C7 C6 118.8(3) . . ?
N2 C10 C9 123.9(3) . . ?
N2 C10 N3 115.8(3) . . ?
C9 C10 N3 120.3(3) . . ?
C1 N1 C5 117.4(3) . . ?
C1 N1 Sm 120.0(2) . . ?
C5 N1 Sm 121.4(2) . . ?
N5 O2 Sm 96.8(2) . . ?
N5 O3 Sm 96.2(2) . . ?
N1 C5 C4 121.5(3) . . ?
N1 C5 C6 116.5(3) . . ?
C4 C5 C6 122.0(3) . . ?
N3 C11 C12 105.9(3) . . ?
N3 C11 C15 127.7(3) . . ?
C12 C11 C15 126.4(3) . . ?
C11 N3 N4 111.2(3) . . ?
C11 N3 C10 130.4(3) . . ?
N4 N3 C10 118.2(3) . . ?
O8 N7 O9 121.6(4) . . ?
O8 N7 O7 121.9(4) . . ?
O9 N7 O7 116.6(3) . . ?
O8 N7 Sm 177.0(3) . . ?
O9 N7 Sm 58.67(18) . . ?
O7 N7 Sm 57.92(18) . . ?
N4 C13 C12 110.7(3) . . ?
N4 C13 C14 122.7(3) . . ?
C12 C13 C14 126.7(3) . . ?
N1 C1 C2 123.3(3) . . ?
C9 C8 C7 120.0(3) . . ?
C8 C9 C10 117.8(3) . . ?
C3 C2 C1 119.3(4) . . ?
C2 C3 C4 118.5(3) . . ?
C3 C4 C5 120.1(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
Sm O10 2.372(3) . ?
Sm O5 2.509(3) . ?
Sm O2 2.534(3) . ?
Sm O4 2.549(3) . ?
Sm O7 2.553(3) . ?
Sm O3 2.554(3) . ?
Sm O9 2.569(3) . ?
Sm N1 2.587(3) . ?
Sm N4 2.589(3) . ?
Sm N2 2.613(3) . ?
Sm N6 2.959(3) . ?
Sm N5 2.965(3) . ?
S1 O10 1.526(3) . ?
S1 C17 1.754(5) . ?
S1 C16 1.782(6) . ?
O4 N6 1.263(4) . ?
N2 C10 1.337(4) . ?
N2 C6 1.359(4) . ?
N4 C13 1.339(4) . ?
N4 N3 1.388(4) . ?
N5 O1 1.217(5) . ?
N5 O3 1.258(4) . ?
N5 O2 1.267(5) . ?
O7 N7 1.261(4) . ?
O5 N6 1.267(4) . ?
N6 O6 1.227(4) . ?
O9 N7 1.260(4) . ?
C6 C7 1.391(5) . ?
C6 C5 1.481(5) . ?
C12 C11 1.373(5) . ?
C12 C13 1.397(6) . ?
C7 C8 1.381(5) . ?
C10 C9 1.392(5) . ?
C10 N3 1.417(4) . ?
N1 C1 1.352(5) . ?
N1 C5 1.353(4) . ?
O8 N7 1.227(4) . ?
C5 C4 1.388(5) . ?
C11 N3 1.373(5) . ?
C11 C15 1.493(5) . ?
C14 C13 1.495(5) . ?
C1 C2 1.372(5) . ?
C8 C9 1.369(5) . ?
C2 C3 1.372(6) . ?
C3 C4 1.379(5) . ?
