#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:14:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179886 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/82/7018260.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_7018260
loop_
_publ_author_name
'Zou, Lifei'
'Zhao, Lang'
'Chen, Peng'
'Guo, Yun-Nan'
'Guo, Yang'
'Li, Yun-Hui'
'Tang, Jinkui'
_publ_section_title
;
 Phenoxido and alkoxido-bridged dinuclear dysprosium complexes showing
 single-molecule magnet behaviour.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2966
_journal_page_last               2971
_journal_paper_doi               10.1039/c2dt12235a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C73 H60 Dy2 N8 O15'
_chemical_formula_weight         1614.29
_chemical_name_common            complex1Dy2
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 125.9080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.1750(18)
_cell_length_b                   14.9170(9)
_cell_length_c                   20.013(2)
_cell_measurement_reflns_used    8441
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      25.84
_cell_measurement_theta_min      2.32
_cell_volume                     7296.3(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19591
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    2.101
_exptl_absorpt_correction_T_max  0.7435
_exptl_absorpt_correction_T_min  0.6217
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.737
_refine_diff_density_min         -1.979
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7140
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0716
_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)+(0.1252P)²+54.5106P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2323
_reflns_number_gt                4963
_reflns_number_total             7140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12235a.txt
_cod_data_source_block           complex1Dy2
_cod_original_cell_volume        7296.1(10)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7018260
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Dy1 Dy 0.01473(2) 0.30263(3) 0.17207(3) 0.0728(2) Uani 1 1 d .
N1 N 0.0339(5) 0.3435(7) 0.0697(5) 0.095(3) Uani 1 1 d .
N2 N -0.0115(5) 0.3812(7) -0.0034(6) 0.104(4) Uani 1 1 d .
H2A H -0.0113 0.3906 -0.0466 0.125 Uiso 1 1 calc R
N3 N 0.0305(3) 0.1375(5) 0.1965(5) 0.0635(18) Uani 1 1 d .
N4 N -0.0062(3) 0.0836(5) 0.1296(5) 0.072(2) Uani 1 1 d .
H4A H -0.0071 0.0250 0.1341 0.086 Uiso 1 1 calc R
O1 O 0.1021(4) 0.2937(7) 0.2271(5) 0.120(4) Uani 1 1 d .
O2 O -0.0520(4) 0.3930(5) 0.0590(5) 0.108(3) Uani 1 1 d .
O3 O 0.0539(3) 0.2679(5) 0.3113(4) 0.0708(16) Uani 1 1 d .
O4 O -0.0394(3) 0.2103(4) 0.0548(4) 0.0689(17) Uani 1 1 d .
O5 O 0.0465(6) 0.4406(9) 0.2343(9) 0.072(3) Uani 0.50 1 d PU
O6 O 0.0719(18) 0.542(3) 0.331(3) 0.30(2) Uani 0.50 1 d PDU
O7 O 0.0001(8) 0.4435(12) 0.2879(11) 0.099(5) Uani 0.50 1 d PU
O8 O 0.9909(7) 0.6038(11) 0.1195(11) 0.200(6) Uani 1 1 d U
O9 O 0.9861(5) 0.9115(7) 0.1720(7) 0.142(4) Uani 1 1 d U
C1 C 0.1382(6) 0.2787(10) 0.2142(7) 0.110(5) Uani 1 1 d .
C2 C 0.1908(6) 0.2455(12) 0.2795(8) 0.121(6) Uani 1 1 d .
H2 H 0.1978 0.2336 0.3316 0.145 Uiso 1 1 calc R
C3 C 0.2289(8) 0.2313(12) 0.2702(9) 0.127(6) Uani 1 1 d .
H3 H 0.2634 0.2113 0.3167 0.153 Uiso 1 1 calc R
C4 C 0.2225(8) 0.2437(11) 0.1942(10) 0.119(5) Uani 1 1 d .
C5 C 0.2608(10) 0.2251(13) 0.1829(14) 0.150(7) Uani 1 1 d .
H5 H 0.2955 0.2041 0.2282 0.179 Uiso 1 1 calc R
C6 C 0.2519(13) 0.235(2) 0.1112(19) 0.182(9) Uani 1 1 d .
H6 H 0.2805 0.2234 0.1056 0.219 Uiso 1 1 calc R
C7 C 0.2020(14) 0.262(2) 0.0441(16) 0.180(10) Uani 1 1 d .
H7 H 0.1956 0.2655 -0.0083 0.216 Uiso 1 1 calc R
C8 C 0.1621(9) 0.2837(13) 0.0510(12) 0.139(6) Uani 1 1 d .
H8 H 0.1281 0.3055 0.0048 0.167 Uiso 1 1 calc .
C9 C 0.1712(8) 0.2738(10) 0.1267(10) 0.109(5) Uani 1 1 d .
C10 C 0.1276(7) 0.2948(8) 0.1365(8) 0.107(5) Uani 1 1 d .
C11 C 0.0772(7) 0.3317(9) 0.0709(7) 0.107(5) Uani 1 1 d .
H11 H 0.0746 0.3497 0.0232 0.129 Uiso 1 1 calc R
C12 C -0.0534(7) 0.4014(7) -0.0041(8) 0.105(5) Uani 1 1 d .
C13 C -0.1022(5) 0.4382(6) -0.0822(6) 0.121(6) Uani 1 1 d G
C14 C -0.1031(6) 0.4553(6) -0.1509(7) 0.144(7) Uani 1 1 d G
H14 H -0.0714 0.4448 -0.1491 0.173 Uiso 1 1 calc R
C15 C -0.1503(6) 0.4876(7) -0.2222(6) 0.176(10) Uani 1 1 d G
H15 H -0.1509 0.4993 -0.2694 0.211 Uiso 1 1 calc R
C16 C -0.1964(6) 0.5028(7) -0.2247(7) 0.160(8) Uani 1 1 d G
H16 H -0.2288 0.5251 -0.2737 0.191 Uiso 1 1 calc R
C17 C -0.1954(5) 0.4857(7) -0.1560(8) 0.153(7) Uani 1 1 d G
H17 H -0.2271 0.4962 -0.1577 0.183 Uiso 1 1 calc R
C18 C -0.1483(6) 0.4534(7) -0.0847(7) 0.147(7) Uani 1 1 d G
H18 H -0.1476 0.4417 -0.0375 0.176 Uiso 1 1 calc R
C19 C 0.0997(4) 0.2208(8) 0.3611(6) 0.072(3) Uani 1 1 d .
C20 C 0.1406(5) 0.2583(10) 0.4376(7) 0.095(3) Uani 1 1 d .
H20 H 0.1353 0.3161 0.4519 0.114 Uiso 1 1 calc R
C21 C 0.1876(6) 0.2130(12) 0.4914(8) 0.117(5) Uani 1 1 d .
H21 H 0.2142 0.2396 0.5433 0.140 Uiso 1 1 calc R
C22 C 0.1985(5) 0.1299(13) 0.4741(8) 0.114(4) Uani 1 1 d .
C23 C 0.2474(7) 0.0868(18) 0.5305(11) 0.172(9) Uani 1 1 d .
H23 H 0.2733 0.1135 0.5827 0.206 Uiso 1 1 calc R
C24 C 0.2587(8) 0.006(2) 0.5112(15) 0.205(11) Uani 1 1 d .
H24 H 0.2930 -0.0223 0.5499 0.246 Uiso 1 1 calc R
C25 C 0.2194(7) -0.0388(15) 0.4331(13) 0.180(9) Uani 1 1 d .
H25 H 0.2267 -0.0967 0.4218 0.216 Uiso 1 1 calc R
C26 C 0.1705(6) 0.0057(11) 0.3749(11) 0.148(7) Uani 1 1 d .
H26 H 0.1458 -0.0194 0.3215 0.177 Uiso 1 1 calc R
C27 C 0.1578(5) 0.0891(10) 0.3955(7) 0.100(4) Uani 1 1 d .
C28 C 0.1081(4) 0.1375(7) 0.3399(6) 0.076(3) Uani 1 1 d .
C29 C 0.0662(4) 0.0952(7) 0.2617(6) 0.075(3) Uani 1 1 d .
H29 H 0.0657 0.0316 0.2593 0.091 Uiso 1 1 calc R
C30 C -0.0396(3) 0.1259(6) 0.0589(5) 0.062(2) Uani 1 1 d .
C31 C -0.0769(3) 0.0746(5) -0.0187(5) 0.079(3) Uani 1 1 d G
C32 C -0.0660(4) -0.0132(5) -0.0248(6) 0.137(6) Uani 1 1 d G
H32 H -0.0350 -0.0423 0.0212 0.164 Uiso 1 1 calc R
C33 C -0.1000(5) -0.0590(6) -0.0977(7) 0.169(8) Uani 1 1 d G
H33 H -0.0925 -0.1198 -0.1019 0.203 Uiso 1 1 calc R
C34 C -0.1449(5) -0.0170(7) -0.1643(6) 0.151(7) Uani 1 1 d G
H34 H -0.1685 -0.0486 -0.2146 0.181 Uiso 1 1 calc R
C35 C -0.1558(4) 0.0709(7) -0.1581(5) 0.173(9) Uani 1 1 d G
H35 H -0.1869 0.1000 -0.2042 0.207 Uiso 1 1 calc R
C36 C -0.1218(4) 0.1167(5) -0.0853(5) 0.131(6) Uani 1 1 d G
H36 H -0.1294 0.1774 -0.0810 0.157 Uiso 1 1 calc R
C37 C 0.0386(11) 0.4728(12) 0.2835(11) 0.095(8) Uani 0.50 1 d PD
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'
Dy Dy -0.1892 4.4098 '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
O1 Dy1 O5 77.6(4) . .
O1 Dy1 O3 145.2(3) . 2
O5 Dy1 O3 104.0(4) . 2
O1 Dy1 O3 76.7(3) . .
O5 Dy1 O3 78.2(4) . .
O3 Dy1 O3 69.9(3) 2 .
O1 Dy1 O4 113.1(3) . .
O5 Dy1 O4 152.2(4) . .
O3 Dy1 O4 81.8(2) 2 .
O3 Dy1 O4 128.4(2) . .
O1 Dy1 O2 127.8(3) . .
O5 Dy1 O2 81.9(4) . .
O3 Dy1 O2 86.3(3) 2 .
O3 Dy1 O2 143.8(3) . .
O4 Dy1 O2 71.3(3) . .
O1 Dy1 O7 107.0(5) . 2
O5 Dy1 O7 29.6(5) . 2
O3 Dy1 O7 78.0(5) 2 2
O3 Dy1 O7 81.9(5) . 2
O4 Dy1 O7 133.8(5) . 2
O2 Dy1 O7 66.3(5) . 2
O1 Dy1 N3 78.9(3) . .
O5 Dy1 N3 143.4(4) . .
O3 Dy1 N3 80.6(2) 2 .
O3 Dy1 N3 69.3(2) . .
O4 Dy1 N3 64.0(2) . .
O2 Dy1 N3 134.6(3) . .
O7 Dy1 N3 148.7(4) 2 .
O1 Dy1 N1 68.9(3) . .
O5 Dy1 N1 90.2(4) . .
O3 Dy1 N1 144.8(3) 2 .
O3 Dy1 N1 145.3(3) . .
O4 Dy1 N1 71.7(2) . .
O2 Dy1 N1 63.7(4) . .
O7 Dy1 N1 103.8(5) 2 .
N3 Dy1 N1 106.9(3) . .
O1 Dy1 Dy1 112.9(2) . 2
O5 Dy1 Dy1 76.9(3) . 2
O3 Dy1 Dy1 38.04(15) 2 2
O3 Dy1 Dy1 37.65(17) . 2
O4 Dy1 Dy1 117.92(16) . 2
O2 Dy1 Dy1 108.3(2) . 2
O7 Dy1 Dy1 62.2(4) 2 2
N3 Dy1 Dy1 86.97(17) . 2
N1 Dy1 Dy1 165.9(2) . 2
C11 N1 N2 115.2(10) . .
C11 N1 Dy1 131.3(8) . .
N2 N1 Dy1 113.4(9) . .
C12 N2 N1 117.0(11) . .
C29 N3 N4 114.8(8) . .
C29 N3 Dy1 129.7(6) . .
N4 N3 Dy1 115.4(6) . .
C30 N4 N3 115.6(8) . .
C1 O1 Dy1 145.9(7) . .
C12 O2 Dy1 122.0(10) . .
C19 O3 Dy1 128.8(6) . 2
C19 O3 Dy1 125.3(6) . .
Dy1 O3 Dy1 104.3(3) 2 .
C30 O4 Dy1 123.0(6) . .
O7 O5 C37 63.4(15) 2 .
O7 O5 Dy1 78.9(11) 2 .
C37 O5 Dy1 124.4(15) . .
O5 O7 C37 59.7(19) 2 2
O5 O7 C37 153.0(19) 2 .
C37 O7 C37 94(2) 2 .
O5 O7 O7 108(2) 2 2
C37 O7 O7 54.3(17) 2 2
C37 O7 O7 53.5(13) . 2
O5 O7 Dy1 71.5(11) 2 2
C37 O7 Dy1 116.6(17) 2 2
C37 O7 Dy1 132.4(14) . 2
O7 O7 Dy1 116.5(5) 2 2
O1 C1 C10 121.6(15) . .
O1 C1 C2 119.8(12) . .
C10 C1 C2 118.7(16) . .
C3 C2 C1 122.2(15) . .
C2 C3 C4 123.9(19) . .
C5 C4 C9 118.7(17) . .
C5 C4 C3 124(2) . .
C9 C4 C3 116.8(17) . .
C6 C5 C4 122(3) . .
C5 C6 C7 121(3) . .
C8 C7 C6 121(2) . .
C7 C8 C9 119(2) . .
C8 C9 C4 119.1(17) . .
C8 C9 C10 120.4(18) . .
C4 C9 C10 120.5(13) . .
C1 C10 C11 121.0(15) . .
C1 C10 C9 117.8(16) . .
C11 C10 C9 121.2(13) . .
N1 C11 C10 126.1(11) . .
O2 C12 N2 120.9(14) . .
O2 C12 C13 121.8(16) . .
N2 C12 C13 117.2(13) . .
C18 C13 C14 120.0 . .
C18 C13 C12 117.1(11) . .
C14 C13 C12 122.9(11) . .
C13 C14 C15 120.0 . .
C14 C15 C16 120.0 . .
C17 C16 C15 120.0 . .
C16 C17 C18 120.0 . .
C13 C18 C17 120.0 . .
O3 C19 C28 122.7(8) . .
O3 C19 C20 117.8(11) . .
C28 C19 C20 119.5(11) . .
C21 C20 C19 120.6(13) . .
C20 C21 C22 122.8(12) . .
C21 C22 C23 120.7(16) . .
C21 C22 C27 118.5(13) . .
C23 C22 C27 120.8(18) . .
C24 C23 C22 120(2) . .
C23 C24 C25 121.5(19) . .
C26 C25 C24 118(2) . .
C25 C26 C27 120.1(16) . .
C26 C27 C28 123.3(12) . .
C26 C27 C22 118.6(12) . .
C28 C27 C22 117.9(13) . .
C19 C28 C27 120.7(10) . .
C19 C28 C29 121.3(9) . .
C27 C28 C29 118.0(10) . .
N3 C29 C28 124.5(10) . .
O4 C30 N4 121.1(8) . .
O4 C30 C31 118.4(8) . .
N4 C30 C31 120.5(8) . .
C32 C31 C36 120.0 . .
C32 C31 C30 120.6(6) . .
C36 C31 C30 119.3(6) . .
C31 C32 C33 120.0 . .
C34 C33 C32 120.0 . .
C35 C34 C33 120.0 . .
C34 C35 C36 120.0 . .
C31 C36 C35 120.0 . .
O5 C37 O7 56.9(13) . 2
O5 C37 O7 121.6(18) . .
O7 C37 O7 72(2) 2 .
O5 C37 O6 117(3) . .
O7 C37 O6 149(3) 2 .
O7 C37 O6 122(3) . .
O5 C37 C37 99.7(15) . 2
O7 C37 C37 43.1(11) 2 2
O7 C37 C37 42.6(15) . 2
O6 C37 C37 126(3) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.185(11) .
Dy1 O5 2.303(13) .
Dy1 O3 2.339(7) 2
Dy1 O3 2.360(6) .
Dy1 O4 2.362(6) .
Dy1 O2 2.376(8) .
Dy1 O7 2.383(18) 2
Dy1 N3 2.502(8) .
Dy1 N1 2.508(10) .
Dy1 Dy1 3.7112(10) 2
N1 C11 1.305(19) .
N1 N2 1.407(15) .
N2 C12 1.292(18) .
N3 C29 1.270(12) .
N3 N4 1.388(10) .
N4 C30 1.321(12) .
O1 C1 1.278(19) .
O2 C12 1.245(15) .
O3 C19 1.335(12) .
O3 Dy1 2.339(7) 2
O4 C30 1.261(10) .
O5 O7 1.20(2) 2
O5 C37 1.24(3) .
O6 C37 1.365(19) .
O7 O5 1.20(2) 2
O7 C37 1.28(2) 2
O7 C37 1.29(3) .
O7 O7 1.52(3) 2
O7 Dy1 2.383(18) 2
C1 C10 1.413(17) .
C1 C2 1.43(2) .
C2 C3 1.29(2) .
C3 C4 1.43(2) .
C4 C5 1.33(2) .
C4 C9 1.40(2) .
C5 C6 1.31(3) .
C6 C7 1.36(4) .
C7 C8 1.33(3) .
C8 C9 1.38(2) .
C9 C10 1.47(2) .
C10 C11 1.41(2) .
C12 C13 1.486(16) .
C13 C18 1.382(6) .
C13 C14 1.382(6) .
C14 C15 1.382(6) .
C15 C16 1.382(6) .
C16 C17 1.382(6) .
C17 C18 1.382(6) .
C19 C28 1.383(15) .
C19 C20 1.402(14) .
C20 C21 1.356(19) .
C21 C22 1.38(2) .
C22 C23 1.38(2) .
C22 C27 1.444(17) .
C23 C24 1.37(3) .
C24 C25 1.45(3) .
C25 C26 1.40(2) .
C26 C27 1.43(2) .
C27 C28 1.433(15) .
C28 C29 1.457(13) .
C30 C31 1.487(10) .
C31 C32 1.374(5) .
C31 C36 1.374(5) .
C32 C33 1.374(5) .
C33 C34 1.374(5) .
C34 C35 1.374(5) .
C35 C36 1.374(5) .
C37 O7 1.28(2) 2
C37 C37 1.89(5) 2
