#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:53:33 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180361 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/30/7203002.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_7203002
loop_
_publ_author_name
'Wang, Su-Na'
'Sun, Ran'
'Wang, Xiao-Shi'
'Li, Yi-Zhi'
'Pan, Yi'
'Bai, Junfeng'
'Scheer, Manfred'
'You, Xiao-Zeng'
_publ_section_title
;
 Versatile lanthanide coordination assemblies due to the synergistic
 effect of lanthanide contraction and flexibility of a flexible
 tricarboxylate ligand
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1051
_journal_paper_doi               10.1039/b708104a
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C9 H10 N3 Nd O8 S3, 2(H2 O)'
_chemical_formula_sum            'C9 H14 N3 Nd O10 S3'
_chemical_formula_weight         564.65
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 121.30(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8368(18)
_cell_length_b                   14.529(3)
_cell_length_c                   15.467(3)
_cell_measurement_reflns_used    3884
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.70
_cell_volume                     1696.8(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD 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  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8375
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    3.487
_exptl_absorpt_correction_T_max  0.42
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Brucker(2000)'
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    2.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.614
_refine_diff_density_min         -2.362
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0462
_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)+(0.1P)²+0.8P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1720
_reflns_number_gt                2009
_reflns_number_total             2976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708104a.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7203002
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Nd1 Nd 0.75458(5) 0.50505(3) 0.50327(3) 0.0211(2) Uani 1 1 d . . .
C1 C 0.7653(11) 0.9748(7) 0.4745(7) 0.028(2) Uani 1 1 d . . .
C2 C 0.7468(11) 1.1174(6) 0.4162(6) 0.028(2) Uani 1 1 d . . .
C3 C 0.7277(10) 1.0926(6) 0.5531(6) 0.0260(19) Uani 1 1 d . . .
C4 C 0.7663(11) 0.8049(6) 0.5527(7) 0.035(2) Uani 1 1 d . . .
H4A H 0.8617 0.8225 0.6196 0.053 Uiso 1 1 calc R . .
H4B H 0.6547 0.8234 0.5453 0.053 Uiso 1 1 calc R . .
C5 C 0.7686(11) 0.7007(6) 0.5377(7) 0.031(2) Uani 1 1 d . . .
C6 C 0.7703(10) 1.1264(6) 0.2448(6) 0.028(2) Uani 1 1 d . . .
H6A H 0.8202 1.1630 0.2132 0.041 Uiso 1 1 calc R . .
H6B H 0.8538 1.0776 0.2827 0.041 Uiso 1 1 calc R . .
C7 C 0.5968(11) 1.0827(6) 0.1614(6) 0.0250(19) Uani 1 1 d . . .
C8 C 0.7025(10) 1.0444(6) 0.7211(6) 0.031(2) Uani 1 1 d . . .
H8A H 0.6144 1.0541 0.7397 0.046 Uiso 1 1 calc R . .
H8B H 0.6705 0.9890 0.6804 0.046 Uiso 1 1 calc R . .
C9 C 0.8770(10) 1.0306(6) 0.8141(6) 0.0256(19) Uani 1 1 d . . .
N1 N 0.7676(9) 1.0278(5) 0.4038(5) 0.0297(17) Uani 1 1 d . . .
N2 N 0.7264(9) 1.1541(5) 0.4884(5) 0.0305(19) Uani 1 1 d . . .
N3 N 0.7444(11) 1.0013(4) 0.5495(6) 0.029(2) Uani 1 1 d . . .
O1 O 0.8593(8) 0.6682(4) 0.5038(5) 0.0388(16) Uani 1 1 d . . .
O2 O 0.6809(8) 0.6519(4) 0.5621(5) 0.0447(17) Uani 1 1 d . . .
O3 O 0.6039(7) 1.0414(5) 0.0912(4) 0.0320(15) Uani 1 1 d . . .
O4 O 0.4582(7) 1.0851(4) 0.1638(4) 0.0324(15) Uani 1 1 d . . .
O5 O 1.0162(7) 1.0297(5) 0.8113(4) 0.0383(16) Uani 1 1 d . . .
O6 O 0.8830(8) 1.0139(4) 0.8971(5) 0.0294(15) Uani 1 1 d . . .
O1W O 0.5458(9) 0.3794(5) 0.3742(6) 0.057(2) Uani 1 1 d . . .
H1WA H 0.5992 0.3283 0.3950 0.069 Uiso 1 1 d R . .
H1WB H 0.4498 0.3774 0.3740 0.069 Uiso 1 1 d R . .
O2W O 0.9027(9) 0.3485(4) 0.5761(5) 0.0509(19) Uani 1 1 d . . .
H2WA H 0.8384 0.3080 0.5329 0.061 Uiso 1 1 d R . .
H2WB H 1.0046 0.3479 0.5834 0.061 Uiso 1 1 d R . .
O3W O 0.2872(17) 0.1851(7) 0.2513(9) 0.132(5) Uani 1 1 d . . .
H3WD H 0.2510 0.2402 0.2452 0.158 Uiso 1 1 d R . .
H3WB H 0.2849 0.1691 0.1977 0.158 Uiso 1 1 d R . .
O4W O 0.187(3) 0.3740(14) 0.2269(11) 0.254(12) Uani 1 1 d . . .
H4WB H 0.1242 0.4016 0.2457 0.305 Uiso 1 1 d R . .
H4WC H 0.1831 0.4033 0.1781 0.305 Uiso 1 1 d R . .
S1 S 0.7943(3) 0.85848(16) 0.45710(19) 0.0385(6) Uani 1 1 d . . .
S2 S 0.7468(3) 1.19747(15) 0.33088(16) 0.0329(6) Uani 1 1 d . . .
S3 S 0.6981(3) 1.14075(16) 0.64612(16) 0.0355(6) 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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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
O3 Nd1 O6 156.8(2) 4_576 4_575 ?
O3 Nd1 O2 73.5(2) 4_576 . ?
O6 Nd1 O2 129.1(2) 4_575 . ?
O3 Nd1 O5 75.82(19) 4_576 2_746 ?
O6 Nd1 O5 113.49(19) 4_575 2_746 ?
O2 Nd1 O5 71.2(2) . 2_746 ?
O3 Nd1 O1 124.0(2) 4_576 . ?
O6 Nd1 O1 79.2(2) 4_575 . ?
O2 Nd1 O1 51.3(2) . . ?
O5 Nd1 O1 77.8(2) 2_746 . ?
O3 Nd1 O4 111.21(18) 4_576 2_645 ?
O6 Nd1 O4 74.15(19) 4_575 2_645 ?
O2 Nd1 O4 77.8(2) . 2_645 ?
O5 Nd1 O4 144.7(2) 2_746 2_645 ?
O1 Nd1 O4 69.7(2) . 2_645 ?
O3 Nd1 O2W 79.2(2) 4_576 . ?
O6 Nd1 O2W 83.5(2) 4_575 . ?
O2 Nd1 O2W 139.0(2) . . ?
O5 Nd1 O2W 72.8(2) 2_746 . ?
O1 Nd1 O2W 136.1(2) . . ?
O4 Nd1 O2W 141.8(2) 2_645 . ?
O3 Nd1 O1W 82.0(2) 4_576 . ?
O6 Nd1 O1W 78.4(2) 4_575 . ?
O2 Nd1 O1W 130.4(2) . . ?
O5 Nd1 O1W 142.3(2) 2_746 . ?
O1 Nd1 O1W 139.6(2) . . ?
O4 Nd1 O1W 72.0(2) 2_645 . ?
O2W Nd1 O1W 73.4(2) . . ?
O3 Nd1 O6 121.03(19) 4_576 2_746 ?
O6 Nd1 O6 64.5(2) 4_575 2_746 ?
O2 Nd1 O6 101.64(19) . 2_746 ?
O5 Nd1 O6 49.00(19) 2_746 2_746 ?
O1 Nd1 O6 68.76(19) . 2_746 ?
O4 Nd1 O6 125.35(19) 2_645 2_746 ?
O2W Nd1 O6 67.4(2) . 2_746 ?
O1W Nd1 O6 127.88(19) . 2_746 ?
O3 Nd1 O3 62.7(2) 4_576 2_645 ?
O6 Nd1 O3 118.04(19) 4_575 2_645 ?
O2 Nd1 O3 65.9(2) . 2_645 ?
O5 Nd1 O3 126.43(19) 2_746 2_645 ?
O1 Nd1 O3 98.0(2) . 2_645 ?
O4 Nd1 O3 48.58(18) 2_645 2_645 ?
O2W Nd1 O3 125.7(2) . 2_645 ?
O1W Nd1 O3 64.6(2) . 2_645 ?
O6 Nd1 O3 166.2(2) 2_746 2_645 ?
O3 Nd1 C9 98.5(2) 4_576 2_746 ?
O6 Nd1 C9 89.5(2) 4_575 2_746 ?
O2 Nd1 C9 85.1(2) . 2_746 ?
O5 Nd1 C9 24.01(19) 2_746 2_746 ?
O1 Nd1 C9 70.7(2) . 2_746 ?
O4 Nd1 C9 139.3(2) 2_645 2_746 ?
O2W Nd1 C9 69.1(2) . 2_746 ?
O1W Nd1 C9 141.7(2) . 2_746 ?
O6 Nd1 C9 25.0(2) 2_746 2_746 ?
O3 Nd1 C9 148.4(2) 2_645 2_746 ?
O3 Nd1 C7 87.4(2) 4_576 2_645 ?
O6 Nd1 C7 96.2(2) 4_575 2_645 ?
O2 Nd1 C7 69.3(2) . 2_645 ?
O5 Nd1 C7 140.0(2) 2_746 2_645 ?
O1 Nd1 C7 82.4(2) . 2_645 ?
O4 Nd1 C7 23.85(19) 2_645 2_645 ?
O2W Nd1 C7 139.7(2) . 2_645 ?
O1W Nd1 C7 67.2(2) . 2_645 ?
O6 Nd1 C7 147.4(2) 2_746 2_645 ?
O3 Nd1 C7 24.77(19) 2_645 2_645 ?
C9 Nd1 C7 151.0(2) 2_746 2_645 ?
N3 C1 N1 127.8(9) . . ?
N3 C1 S1 120.9(7) . . ?
N1 C1 S1 111.3(8) . . ?
N2 C2 N1 126.7(8) . . ?
N2 C2 S2 114.6(6) . . ?
N1 C2 S2 118.7(7) . . ?
N2 C3 N3 126.0(8) . . ?
N2 C3 S3 113.9(6) . . ?
N3 C3 S3 120.1(7) . . ?
C5 C4 S1 106.5(7) . . ?
C5 C4 H4A 110.4 . . ?
S1 C4 H4A 110.4 . . ?
C5 C4 H4B 110.4 . . ?
S1 C4 H4B 110.4 . . ?
H4A C4 H4B 108.6 . . ?
O2 C5 O1 123.0(8) . . ?
O2 C5 C4 117.2(8) . . ?
O1 C5 C4 119.8(8) . . ?
C7 C6 S2 114.5(6) . . ?
C7 C6 H6A 108.6 . . ?
S2 C6 H6A 108.6 . . ?
C7 C6 H6B 108.6 . . ?
S2 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
O4 C7 O3 121.7(7) . . ?
O4 C7 C6 122.1(7) . . ?
O3 C7 C6 116.2(7) . . ?
O4 C7 Nd1 56.0(4) . 2_655 ?
O3 C7 Nd1 65.8(4) . 2_655 ?
C6 C7 Nd1 177.2(6) . 2_655 ?
C9 C8 S3 113.2(6) . . ?
C9 C8 H8A 108.9 . . ?
S3 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
S3 C8 H8B 108.9 . . ?
H8A C8 H8B 107.8 . . ?
O5 C9 O6 120.2(7) . . ?
O5 C9 C8 121.0(8) . . ?
O6 C9 C8 118.7(7) . . ?
O5 C9 Nd1 55.4(4) . 2_756 ?
O6 C9 Nd1 64.9(4) . 2_756 ?
C8 C9 Nd1 176.4(6) . 2_756 ?
C2 N1 C1 112.2(8) . . ?
C2 N2 C3 114.1(8) . . ?
C1 N3 C3 113.2(8) . . ?
C5 O1 Nd1 92.4(5) . . ?
C5 O2 Nd1 93.1(5) . . ?
C7 O3 Nd1 152.9(5) . 4_575 ?
C7 O3 Nd1 89.5(5) . 2_655 ?
Nd1 O3 Nd1 117.3(2) 4_575 2_655 ?
C7 O4 Nd1 100.1(5) . 2_655 ?
C9 O5 Nd1 100.6(5) . 2_756 ?
C9 O6 Nd1 154.4(5) . 4_576 ?
C9 O6 Nd1 90.0(5) . 2_756 ?
Nd1 O6 Nd1 115.5(2) 4_576 2_756 ?
Nd1 O1W H1WA 106.8 . . ?
Nd1 O1W H1WB 109.5 . . ?
H1WA O1W H1WB 109.3 . . ?
Nd1 O2W H2WA 106.8 . . ?
Nd1 O2W H2WB 109.3 . . ?
H2WA O2W H2WB 109.2 . . ?
H3WD O3W H3WB 109.4 . . ?
H4WB O4W H4WC 109.7 . . ?
C1 S1 C4 101.4(5) . . ?
C2 S2 C6 102.9(4) . . ?
C3 S3 C8 104.9(4) . . ?
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
Nd1 O3 2.442(6) 4_576 ?
Nd1 O6 2.449(6) 4_575 ?
Nd1 O2 2.533(6) . ?
Nd1 O5 2.534(6) 2_746 ?
Nd1 O1 2.542(6) . ?
Nd1 O4 2.553(6) 2_645 ?
Nd1 O2W 2.573(6) . ?
Nd1 O1W 2.626(7) . ?
Nd1 O6 2.742(6) 2_746 ?
Nd1 O3 2.764(5) 2_645 ?
Nd1 C9 3.027(8) 2_746 ?
Nd1 C7 3.031(8) 2_645 ?
C1 N3 1.325(16) . ?
C1 N1 1.346(12) . ?
C1 S1 1.750(10) . ?
C2 N2 1.331(10) . ?
C2 N1 1.341(11) . ?
C2 S2 1.759(9) . ?
C3 N2 1.338(11) . ?
C3 N3 1.338(10) . ?
C3 S3 1.737(9) . ?
C4 C5 1.533(12) . ?
C4 S1 1.798(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O2 1.245(10) . ?
C5 O1 1.256(11) . ?
C6 C7 1.537(11) . ?
C6 S2 1.780(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O4 1.245(9) . ?
C7 O3 1.270(9) . ?
C7 Nd1 3.031(8) 2_655 ?
C8 C9 1.477(11) . ?
C8 S3 1.806(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O5 1.253(9) . ?
C9 O6 1.281(10) . ?
C9 Nd1 3.027(8) 2_756 ?
O3 Nd1 2.442(6) 4_575 ?
O3 Nd1 2.764(5) 2_655 ?
O4 Nd1 2.553(6) 2_655 ?
O5 Nd1 2.534(6) 2_756 ?
O6 Nd1 2.449(6) 4_576 ?
O6 Nd1 2.742(6) 2_756 ?
O1W H1WA 0.8484 . ?
O1W H1WB 0.8473 . ?
O2W H2WA 0.8490 . ?
O2W H2WB 0.8470 . ?
O3W H3WD 0.8486 . ?
O3W H3WB 0.8521 . ?
O4W H4WB 0.8493 . ?
O4W H4WC 0.8515 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WB O4W 0.85 2.25 2.78(2) 120.7 .
O3W H3WD O4W 0.85 2.00 2.85(2) 173.4 .
O2W H2WB O1 0.85 2.24 2.950(9) 142.0 3_766
O1W H1WB O2 0.85 1.92 2.691(9) 151.0 3_666
O4W H4WC N1 0.85 2.38 3.18(2) 156.7 2_645
O4W H4WC S1 0.85 2.30 2.944(14) 133.2 2_645
O4W H4WB O5 0.85 1.98 2.825(16) 170.2 4_475
O2W H2WB O3W 0.85 2.54 3.092(15) 123.3 4_666
O2W H2WA N2 0.85 2.40 3.170(10) 151.7 1_545
O3W H3WB O4 0.85 2.22 2.890(11) 135.2 1_545
O1W H1WA S2 0.85 2.76 3.439(7) 137.7 1_545
