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#$Date: 2016-03-26 03:40:22 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180191 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/87/7108716.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_7108716
loop_
_publ_author_name
'Ji-Dong Leng'
'Jun-Liang Liu'
'Yan-Zhen Zheng'
'Liviu Ungur'
'Liviu F. Chibotaru'
'Fu-Sheng Guo'
'Ming-Liang Tong'
_publ_section_title
;
 Relaxations in heterolanthanide dinuclear single-molecule magnets
;
_journal_name_full               Chem.Commun.
_journal_page_first              158
_journal_paper_doi               10.1039/c2cc37036k
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C16 H30 Cl4 Dy0.87 N2 O7 Yb1.13'
_chemical_formula_weight         841.13
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 97.463(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.469(4)
_cell_length_b                   9.292(2)
_cell_length_c                   8.889(2)
_cell_measurement_temperature    123(2)
_cell_volume                     1266.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3640
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    7.150
_exptl_absorpt_correction_T_max  0.6345
_exptl_absorpt_correction_T_min  0.4567
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             801
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0218
_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)+(0.0200P)²+1.5604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0499
_reflns_number_gt                1283
_reflns_number_total             1354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37036k.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7108716
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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
Dy1 Dy 0.384587(13) 0.0000 1.02516(2) 0.01533(9) Uani 0.43 2 d SP . 1
Yb1 Yb 0.384587(13) 0.0000 1.02516(2) 0.01533(9) Uani 0.57 2 d SP . 2
Cl1 Cl 0.37090(7) 0.23233(14) 1.19536(13) 0.0431(3) Uani 1 1 d . . .
O1 O 0.4783(2) 0.0000 0.8583(3) 0.0147(7) Uani 1 2 d S . .
O2 O 0.31898(16) 0.1562(3) 0.8356(3) 0.0199(5) Uani 1 1 d . . .
H2O H 0.2669 0.1860 0.8269 0.024 Uiso 1 1 d R . .
C1 C 0.4615(3) 0.0000 0.6957(5) 0.0181(11) Uani 1 2 d S . .
H1 H 0.5188 0.0000 0.6552 0.022 Uiso 1 2 calc SR . .
C2 C 0.4122(2) 0.1359(4) 0.6390(4) 0.0206(8) Uani 1 1 d . . .
H2A H 0.4429 0.2208 0.6876 0.025 Uiso 1 1 calc R . .
H2B H 0.4128 0.1443 0.5281 0.025 Uiso 1 1 calc R . .
C3 C 0.3183(2) 0.1372(4) 0.6721(4) 0.0198(8) Uani 1 1 d . . .
H3 H 0.2877 0.2212 0.6187 0.024 Uiso 1 1 calc R . .
C4 C 0.2700(3) 0.0000 0.6178(6) 0.0229(12) Uani 1 2 d S . .
H4A H 0.2603 0.0000 0.5055 0.027 Uiso 1 2 calc SR . .
H4B H 0.2121 0.0000 0.6541 0.027 Uiso 1 2 calc SR . .
N1 N 0.2284(3) 0.0000 1.0521(5) 0.0342(11) Uani 0.50 2 d SP A 1
C5 C 0.1528(6) 0.0000 1.0575(11) 0.016(2) Uani 0.50 2 d SP A 1
C6 C 0.0576(7) 0.0000 1.0419(15) 0.038(3) Uani 0.50 2 d SP . 1
H6A H 0.0386 0.0000 1.1405 0.057 Uiso 0.50 2 d SPR . 1
H6B H 0.0360 0.0844 0.9873 0.057 Uiso 0.50 1 d PR . 1
O1W O 0.2284(3) 0.0000 1.0521(5) 0.0342(11) Uani 0.50 2 d SP B 2
H1WA H 0.2032 -0.0719 1.0043 0.041 Uiso 0.25 1 d PR B 2
H1WB H 0.2214 0.0000 1.1446 0.041 Uiso 0.50 2 d SPR B 2
N2 N 0.1207(7) 0.0000 1.2855(12) 0.036(2) Uani 0.50 2 d SP . .
C7 C 0.0712(8) 0.0000 1.3658(12) 0.025(2) Uani 0.50 2 d SP . .
C8 C 0.007(2) 0.0000 1.476(3) 0.042(5) Uani 0.50 2 d SP . .
H8A H -0.0254 -0.0813 1.4338 0.063 Uiso 0.50 1 d PR . .
H8B H 0.0266 0.0000 1.5831 0.063 Uiso 0.50 2 d SPR . .
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'
Cl Cl 0.1484 0.1585 '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'
Yb Yb -0.3850 5.5486 '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 O1 69.19(13) . 5_657
O1 Dy1 O2 77.19(9) . 6
O1 Dy1 O2 128.83(8) 5_657 6
O1 Dy1 O2 77.19(9) . .
O1 Dy1 O2 128.83(8) 5_657 .
O2 Dy1 O2 76.20(12) 6 .
O1 Dy1 N1 143.70(13) . .
O1 Dy1 N1 147.11(13) 5_657 .
O2 Dy1 N1 74.43(10) 6 .
O2 Dy1 N1 74.43(10) . .
O1 Dy1 Cl1 119.37(4) . .
O1 Dy1 Cl1 82.94(5) 5_657 .
O2 Dy1 Cl1 148.14(7) 6 .
O2 Dy1 Cl1 81.25(7) . .
N1 Dy1 Cl1 78.05(6) . .
O1 Dy1 Cl1 119.37(4) . 6
O1 Dy1 Cl1 82.94(5) 5_657 6
O2 Dy1 Cl1 81.25(7) 6 6
O2 Dy1 Cl1 148.14(7) . 6
N1 Dy1 Cl1 78.05(6) . 6
Cl1 Dy1 Cl1 108.48(6) . 6
O1 Dy1 Dy1 34.87(8) . 5_657
O1 Dy1 Dy1 34.32(8) 5_657 5_657
O2 Dy1 Dy1 104.46(6) 6 5_657
O2 Dy1 Dy1 104.46(6) . 5_657
N1 Dy1 Dy1 178.57(10) . 5_657
Cl1 Dy1 Dy1 102.75(3) . 5_657
Cl1 Dy1 Dy1 102.75(3) 6 5_657
C1 O1 Dy1 128.9(3) . .
C1 O1 Yb1 120.3(3) . 5_657
Dy1 O1 Yb1 110.81(13) . 5_657
C1 O1 Dy1 120.3(3) . 5_657
Dy1 O1 Dy1 110.81(13) . 5_657
Yb1 O1 Dy1 0.000(11) 5_657 5_657
C3 O2 Dy1 125.8(2) . .
C3 O2 H2O 93.7 . .
Dy1 O2 H2O 125.8 . .
O1 C1 C2 110.5(2) . 6
O1 C1 C2 110.5(2) . .
C2 C1 C2 111.7(4) 6 .
O1 C1 Yb1 37.00(18) . 5_657
C2 C1 Yb1 122.9(2) 6 5_657
C2 C1 Yb1 122.9(2) . 5_657
O1 C1 H1 108.0 . .
C2 C1 H1 108.0 6 .
C2 C1 H1 108.0 . .
Yb1 C1 H1 71.0 5_657 .
C3 C2 C1 113.0(3) . .
C3 C2 H2A 109.0 . .
C1 C2 H2A 109.0 . .
C3 C2 H2B 109.0 . .
C1 C2 H2B 109.0 . .
H2A C2 H2B 107.8 . .
O2 C3 C2 108.0(3) . .
O2 C3 C4 110.8(3) . .
C2 C3 C4 112.0(3) . .
O2 C3 H3 108.7 . .
C2 C3 H3 108.7 . .
C4 C3 H3 108.7 . .
C3 C4 C3 113.5(4) . 6
C3 C4 H4A 108.9 . .
C3 C4 H4A 108.9 6 .
C3 C4 H4B 108.9 . .
C3 C4 H4B 108.9 6 .
H4A C4 H4B 107.7 . .
C5 N1 Dy1 176.8(6) . .
C5 N1 H1WA 68.3 . .
Dy1 N1 H1WA 109.9 . .
C5 N1 H1WB 72.9 . .
Dy1 N1 H1WB 110.3 . .
H1WA N1 H1WB 112.1 . .
N1 C5 C6 172.3(11) . .
N1 C5 H1WA 42.8 . .
C6 C5 H1WA 132.6 . .
N1 C5 H1WB 41.0 . .
C6 C5 H1WB 146.7 . .
H1WA C5 H1WB 71.9 . .
C5 C6 C6 161.7(14) . 5_557
C5 C6 H6A 109.8 . .
C6 C6 H6A 88.5 5_557 .
C5 C6 H6B 109.1 . .
C6 C6 H6B 62.6 5_557 .
H6A C6 H6B 109.5 . .
N2 C7 C8 178.5(19) . .
N2 C7 C8 174.6(16) . 5_558
C8 C7 C8 4(3) . 5_558
C8 C8 C7 165(10) 5_558 .
C8 C8 C7 11(8) 5_558 5_558
C7 C8 C7 176(3) . 5_558
C8 C8 H8A 93.4 5_558 .
C7 C8 H8A 95.9 . .
C7 C8 H8A 86.4 5_558 .
C8 C8 H8B 44.3 5_558 .
C7 C8 H8B 120.6 . .
C7 C8 H8B 55.6 5_558 .
H8A C8 H8B 118.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.205(3) .
Dy1 O1 2.236(3) 5_657
Dy1 O2 2.352(2) 6
Dy1 O2 2.352(2) .
Dy1 N1 2.459(4) .
Dy1 Cl1 2.6604(12) .
Dy1 Cl1 2.6604(12) 6
Dy1 Dy1 3.6556(9) 5_657
O1 C1 1.435(5) .
O1 Yb1 2.236(3) 5_657
O1 Dy1 2.236(3) 5_657
O2 C3 1.463(4) .
O2 H2O 0.8461 .
C1 C2 1.527(4) 6
C1 C2 1.527(4) .
C1 Yb1 3.208(5) 5_657
C1 H1 1.0000 .
C2 C3 1.520(5) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.524(5) .
C3 H3 1.0000 .
C4 C3 1.524(5) 6
C4 H4A 0.9900 .
C4 H4B 0.9900 .
N1 C5 1.176(10) .
N1 H1WA 0.8573 .
N1 H1WB 0.8440 .
C5 C6 1.461(14) .
C5 H1WA 1.1716 .
C5 H1WB 1.2292 .
C6 C6 1.84(2) 5_557
C6 H6A 0.9603 .
C6 H6B 0.9596 .
N2 C7 1.112(14) .
C7 C8 1.481(19) .
C7 C8 1.97(2) 5_558
C8 C8 0.50(3) 5_558
C8 C7 1.97(2) 5_558
C8 H8A 0.9587 .
C8 H8B 0.9587 .
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
O2 H2O Cl1 0.85 2.25 3.093(3) 179.3 7_557
O1W H1WB N2 0.84 2.12 2.825(11) 140.6 .
