#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:01:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180000 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/94/7029499.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_7029499
loop_
_publ_author_name
'Zhang, Haixia'
'Lin, Shuang-Yan'
'Xue, Shufang'
'Wang, Chao'
'Tang, Jinkui'
_publ_section_title
;
 Acetato-bridged dinuclear lanthanide complexes with single molecule
 magnet behaviour for the Dy2 species.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6262
_journal_page_last               6268
_journal_paper_doi               10.1039/c3dt53366b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C38 H48 Gd2 N6 O16 S2'
_chemical_formula_weight         1223.44
_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                69.60(2)
_cell_angle_beta                 85.69(2)
_cell_angle_gamma                81.48(2)
_cell_formula_units_Z            1
_cell_length_a                   10.198(11)
_cell_length_b                   10.642(11)
_cell_length_c                   11.568(12)
_cell_measurement_reflns_used    1872
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.20
_cell_measurement_theta_min      2.26
_cell_volume                     1163(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  '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  0.0938
_diffrn_reflns_av_unetI/netI     0.1838
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6677
_diffrn_reflns_theta_full        25.58
_diffrn_reflns_theta_max         25.58
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_T_max  0.6463
_exptl_absorpt_correction_T_min  0.5340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sadabs; Bruker,2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.324
_refine_diff_density_min         -3.417
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4223
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.0931
_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)+(0.1481P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2698
_reflns_number_gt                2330
_reflns_number_total             4223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53366b2.cif
_cod_data_source_block           Gd2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7029499
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
O4 O 0.5686(12) 0.3178(13) 0.1552(11) 0.058(3) Uani 1 1 d .
Gd1 Gd 0.47949(8) 0.14877(9) 0.33030(8) 0.0472(4) Uani 1 1 d .
N3 N 0.3923(12) 0.3872(15) 0.3280(12) 0.047(4) Uani 1 1 d .
N2 N 0.2636(14) 0.4341(17) 0.2917(13) 0.059(4) Uani 1 1 d .
H2 H 0.2259 0.5126 0.2897 0.071 Uiso 1 1 calc R
N1 N -0.1183(15) 0.5577(19) 0.1334(15) 0.071(5) Uani 1 1 d .
O2 O 0.6078(11) 0.2191(11) 0.4389(10) 0.048(3) Uani 1 1 d .
O1 O 0.2546(11) 0.2345(14) 0.2699(12) 0.063(4) Uani 1 1 d .
O7 O 0.3920(13) -0.0473(14) 0.3312(11) 0.068(4) Uani 1 1 d U
H7A H 0.4198 -0.1245 0.3972 0.081 Uiso 1 1 calc R
O3 O 0.4676(12) 0.1705(14) 0.1159(11) 0.066(4) Uani 1 1 d .
O6 O 0.6212(10) -0.0646(11) 0.4743(9) 0.047(3) Uani 1 1 d .
O5 O 0.6978(12) 0.0421(14) 0.2872(11) 0.061(3) Uani 1 1 d .
O8 O 0.2703(19) 0.205(2) 0.959(2) 0.117(6) Uani 1 1 d DU
H8 H 0.1915 0.2298 0.9681 0.175 Uiso 1 1 calc R
S1 S 0.0584(5) 0.6668(6) 0.1945(6) 0.0794(17) Uani 1 1 d D
H1 H 0.001(15) 0.7680(19) 0.136(16) 0.119 Uiso 1 1 d D
C13 C 0.6570(15) 0.3283(19) 0.4281(14) 0.047(4) Uani 1 1 d .
C12 C 0.7853(17) 0.322(2) 0.4629(18) 0.067(6) Uani 1 1 d .
H12 H 0.8375 0.2386 0.4931 0.081 Uiso 1 1 calc R
C11 C 0.835(2) 0.436(2) 0.4532(19) 0.070(6) Uani 1 1 d .
H11 H 0.9214 0.4282 0.4789 0.084 Uiso 1 1 calc R
C10 C 0.7642(19) 0.565(2) 0.406(2) 0.070(6) Uani 1 1 d .
H10 H 0.8006 0.6425 0.3989 0.084 Uiso 1 1 calc R
C9 C 0.6439(18) 0.5694(18) 0.3740(16) 0.056(5) Uani 1 1 d .
H9 H 0.5955 0.6547 0.3422 0.067 Uiso 1 1 calc R
C8 C 0.5809(15) 0.4609(19) 0.3820(14) 0.047(4) Uani 1 1 d .
C7 C 0.4480(18) 0.4780(19) 0.3475(14) 0.052(4) Uani 1 1 d .
H7 H 0.3973 0.5609 0.3382 0.063 Uiso 1 1 calc R
C6 C 0.2015(15) 0.3513(19) 0.2601(14) 0.047(4) Uani 1 1 d .
C1 C 0.0660(17) 0.401(2) 0.2112(16) 0.054(5) Uani 1 1 d .
C4 C -0.1810(18) 0.462(3) 0.122(2) 0.078(6) Uani 1 1 d U
H4 H -0.2674 0.4837 0.0937 0.094 Uiso 1 1 calc R
C3 C -0.1231(18) 0.336(3) 0.150(2) 0.083(6) Uani 1 1 d U
H3 H -0.1666 0.2693 0.1403 0.099 Uiso 1 1 calc R
C2 C 0.0054(17) 0.306(2) 0.1937(16) 0.060(5) Uani 1 1 d .
H2A H 0.0497 0.2186 0.2112 0.072 Uiso 1 1 calc R
C16 C 0.309(3) -0.070(3) 0.255(2) 0.106(8) Uani 1 1 d U
H16A H 0.3060 0.0034 0.1770 0.159 Uiso 1 1 calc R
H16B H 0.2221 -0.0751 0.2917 0.159 Uiso 1 1 calc R
H16C H 0.3423 -0.1531 0.2414 0.159 Uiso 1 1 calc R
C14 C 0.5357(18) 0.2666(18) 0.0804(16) 0.050(4) Uani 1 1 d .
C17 C 0.569(2) 0.330(2) -0.0509(17) 0.077(6) Uani 1 1 d .
H17A H 0.5417 0.4258 -0.0756 0.116 Uiso 1 1 calc R
H17B H 0.5237 0.2929 -0.0988 0.116 Uiso 1 1 calc R
H17C H 0.6629 0.3132 -0.0642 0.116 Uiso 1 1 calc R
C15 C 0.7143(16) -0.0419(17) 0.3987(17) 0.050(4) Uani 1 1 d .
C18 C 0.8521(17) -0.104(2) 0.4365(19) 0.074(6) Uani 1 1 d .
H18A H 0.8889 -0.0518 0.4758 0.110 Uiso 1 1 calc R
H18B H 0.9054 -0.1059 0.3650 0.110 Uiso 1 1 calc R
H18C H 0.8507 -0.1947 0.4931 0.110 Uiso 1 1 calc R
C19 C 0.283(3) 0.098(3) 0.909(3) 0.142(8) Uani 1 1 d DU
H19A H 0.3606 0.0352 0.9408 0.213 Uiso 1 1 calc R
H19B H 0.2911 0.1350 0.8206 0.213 Uiso 1 1 calc R
H19C H 0.2060 0.0516 0.9317 0.213 Uiso 1 1 calc R
C5 C 0.0026(17) 0.535(2) 0.1785(15) 0.054(5) Uani 1 1 d 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'
Gd Gd -0.1653 3.9035 '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
C14 O4 Gd1 92.6(10) . .
O2 Gd1 O6 80.6(4) . 2_656
O2 Gd1 O7 141.9(4) . .
O6 Gd1 O7 75.0(4) 2_656 .
O2 Gd1 O1 128.3(5) . .
O6 Gd1 O1 82.6(4) 2_656 .
O7 Gd1 O1 77.1(5) . .
O2 Gd1 O4 83.8(4) . .
O6 Gd1 O4 155.8(5) 2_656 .
O7 Gd1 O4 127.3(4) . .
O1 Gd1 O4 92.9(4) . .
O2 Gd1 O3 135.4(4) . .
O6 Gd1 O3 144.0(4) 2_656 .
O7 Gd1 O3 74.1(4) . .
O1 Gd1 O3 72.8(4) . .
O4 Gd1 O3 53.7(4) . .
O2 Gd1 O5 79.5(4) . .
O6 Gd1 O5 119.8(4) 2_656 .
O7 Gd1 O5 87.7(5) . .
O1 Gd1 O5 148.9(5) . .
O4 Gd1 O5 74.8(4) . .
O3 Gd1 O5 77.0(4) . .
O2 Gd1 N3 68.4(4) . .
O6 Gd1 N3 88.4(4) 2_656 .
O7 Gd1 N3 138.1(4) . .
O1 Gd1 N3 62.6(4) . .
O4 Gd1 N3 68.7(4) . .
O3 Gd1 N3 102.6(4) . .
O5 Gd1 N3 133.1(4) . .
O2 Gd1 O6 72.6(4) . .
O6 Gd1 O6 68.0(4) 2_656 .
O7 Gd1 O6 71.3(4) . .
O1 Gd1 O6 141.2(4) . .
O4 Gd1 O6 124.1(4) . .
O3 Gd1 O6 117.7(4) . .
O5 Gd1 O6 51.8(4) . .
N3 Gd1 O6 137.1(4) . .
C7 N3 N2 111.5(16) . .
C7 N3 Gd1 132.3(11) . .
N2 N3 Gd1 116.0(11) . .
C6 N2 N3 115.9(16) . .
C6 N2 H2 122.0 . .
N3 N2 H2 122.0 . .
C5 N1 C4 124.0(19) . .
C13 O2 Gd1 137.9(9) . .
C6 O1 Gd1 123.8(11) . .
C16 O7 Gd1 133.2(14) . .
C16 O7 H7A 113.4 . .
Gd1 O7 H7A 113.4 . .
C14 O3 Gd1 92.5(10) . .
C15 O6 Gd1 156.1(11) . 2_656
C15 O6 Gd1 89.2(9) . .
Gd1 O6 Gd1 112.0(4) 2_656 .
C15 O5 Gd1 95.0(10) . .
C19 O8 H8 109.5 . .
C5 S1 H1 112.2(16) . .
O2 C13 C12 120.7(18) . .
O2 C13 C8 122.2(13) . .
C12 C13 C8 117.1(17) . .
C11 C12 C13 121(2) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C12 C11 C10 123.0(17) . .
C12 C11 H11 118.5 . .
C10 C11 H11 118.5 . .
C9 C10 C11 115.8(18) . .
C9 C10 H10 122.1 . .
C11 C10 H10 122.1 . .
C10 C9 C8 126.6(19) . .
C10 C9 H9 116.7 . .
C8 C9 H9 116.7 . .
C9 C8 C7 121.6(18) . .
C9 C8 C13 116.9(14) . .
C7 C8 C13 121.5(15) . .
N3 C7 C8 124.5(18) . .
N3 C7 H7 117.7 . .
C8 C7 H7 117.7 . .
O1 C6 N2 121.5(15) . .
O1 C6 C1 120.5(17) . .
N2 C6 C1 118.0(17) . .
C2 C1 C5 120.0(16) . .
C2 C1 C6 113.7(18) . .
C5 C1 C6 126.2(17) . .
C3 C4 N1 121.2(18) . .
C3 C4 H4 119.4 . .
N1 C4 H4 119.4 . .
C4 C3 C2 118(2) . .
C4 C3 H3 121.1 . .
C2 C3 H3 121.1 . .
C1 C2 C3 121(2) . .
C1 C2 H2A 119.6 . .
C3 C2 H2A 119.6 . .
O7 C16 H16A 109.5 . .
O7 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
O7 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
O3 C14 O4 120.7(16) . .
O3 C14 C17 120.8(17) . .
O4 C14 C17 118.2(17) . .
C14 C17 H17A 109.5 . .
C14 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C14 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
O6 C15 O5 121.9(14) . .
O6 C15 C18 120.3(16) . .
O5 C15 C18 117.7(16) . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
O8 C19 H19A 109.5 . .
O8 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
O8 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
N1 C5 C1 116.0(17) . .
N1 C5 S1 116.3(16) . .
C1 C5 S1 127.7(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O4 C14 1.26(2) .
O4 Gd1 2.415(11) .
Gd1 O2 2.246(10) .
Gd1 O6 2.340(10) 2_656
Gd1 O7 2.385(13) .
Gd1 O1 2.399(11) .
Gd1 O3 2.420(12) .
Gd1 O5 2.444(12) .
Gd1 N3 2.553(16) .
Gd1 O6 2.602(11) .
N3 C7 1.28(2) .
N3 N2 1.375(18) .
N2 C6 1.32(2) .
N2 H2 0.8600 .
N1 C5 1.33(2) .
N1 C4 1.33(3) .
O2 C13 1.30(2) .
O1 C6 1.25(2) .
O7 C16 1.37(2) .
O7 H7A 0.9300 .
O3 C14 1.25(2) .
O6 C15 1.233(19) .
O6 Gd1 2.340(10) 2_656
O5 C15 1.29(2) .
O8 C19 1.430(10) .
O8 H8 0.8200 .
S1 C5 1.66(2) .
S1 H1 1.1500(14) .
C13 C12 1.38(2) .
C13 C8 1.45(3) .
C12 C11 1.35(3) .
C12 H12 0.9300 .
C11 C10 1.40(3) .
C11 H11 0.9300 .
C10 C9 1.30(3) .
C10 H10 0.9300 .
C9 C8 1.38(2) .
C9 H9 0.9300 .
C8 C7 1.41(2) .
C7 H7 0.9300 .
C6 C1 1.48(2) .
C1 C2 1.34(3) .
C1 C5 1.41(3) .
C4 C3 1.32(3) .
C4 H4 0.9300 .
C3 C2 1.39(2) .
C3 H3 0.9300 .
C2 H2A 0.9300 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C14 C17 1.47(2) .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C15 C18 1.49(2) .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
