#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:50:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179992 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/86/7028622.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_7028622
loop_
_publ_author_name
'Yang, Fen'
'Zhou, Qi'
'Zeng, Guang'
'Li, Guanghua'
'Gao, Lu'
'Shi, Zhan'
'Feng, Shouhua'
_publ_section_title
;
 Anion effects on the structures and magnetic properties of binuclear
 lanthanide single-molecule magnets.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1238
_journal_page_last               1245
_journal_paper_doi               10.1039/c3dt52634h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C44 H48 Cl6 Dy2 N4 O6'
_chemical_formula_sum            'C44 H48 Cl6 Dy2 N4 O6'
_chemical_formula_weight         1266.56
_chemical_melting_point          ?
_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                 105.93(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.910(2)
_cell_length_b                   12.189(2)
_cell_length_c                   18.974(4)
_cell_measurement_reflns_used    5007
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      3.00
_cell_volume                     2426.3(9)
_computing_cell_refinement       Process-auto
_computing_data_collection       Process-auto
_computing_data_reduction        Process-auto
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_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  0.0835
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23355
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.435
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9241
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Process-auto
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5507
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0401
_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)+(0.0184P)²+2.3139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                4055
_reflns_number_total             5507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52634h.txt
_cod_data_source_block           compound-3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2426.3(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7028622
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
Dy1 Dy -0.01867(2) -0.127673(17) 0.055269(13) 0.02837(8) Uani 1 1 d .
Cl1 Cl 0.19489(14) -0.08952(12) 0.15862(8) 0.0561(4) Uani 1 1 d .
Cl2 Cl -0.15440(13) -0.15656(11) 0.14761(8) 0.0497(4) Uani 1 1 d .
Cl3 Cl -0.22351(12) -0.17584(11) -0.05504(8) 0.0452(3) Uani 1 1 d .
N1 N -0.0585(4) -0.3914(3) -0.0896(2) 0.0390(10) Uani 1 1 d .
H1 H -0.0961 -0.3414 -0.0713 0.080 Uiso 1 1 calc .
N2 N 0.3212(4) -0.0997(3) 0.0137(2) 0.0373(10) Uani 1 1 d .
H2 H 0.2819 -0.0562 0.0359 0.080 Uiso 1 1 calc .
O1 O 0.0544(3) -0.2841(2) 0.0362(2) 0.0409(9) Uani 1 1 d .
O2 O 0.0697(3) -0.0549(2) -0.03525(17) 0.0284(7) Uani 1 1 d .
O3 O 0.4147(8) 0.0130(6) 0.2985(4) 0.156(3) Uani 1 1 d D
C1 C -0.1228(6) -0.4363(4) -0.1528(3) 0.0527(15) Uani 1 1 d .
C2 C -0.0595(8) -0.5183(5) -0.1813(4) 0.072(2) Uani 1 1 d .
H2A H -0.1011 -0.5518 -0.2254 0.080 Uiso 1 1 calc .
C3 C 0.0597(9) -0.5495(5) -0.1462(4) 0.075(2) Uani 1 1 d .
H3A H 0.0985 -0.6043 -0.1666 0.080 Uiso 1 1 calc .
C4 C 0.1278(6) -0.5011(4) -0.0790(3) 0.0530(16) Uani 1 1 d .
C5 C 0.2528(7) -0.5270(5) -0.0384(4) 0.072(2) Uani 1 1 d .
H5 H 0.2969 -0.5824 -0.0547 0.080 Uiso 1 1 calc .
C6 C 0.3098(6) -0.4723(5) 0.0243(4) 0.0635(19) Uani 1 1 d .
H6 H 0.3928 -0.4904 0.0500 0.080 Uiso 1 1 calc .
C7 C 0.2458(6) -0.3884(4) 0.0515(3) 0.0521(15) Uani 1 1 d .
H7 H 0.2871 -0.3516 0.0944 0.080 Uiso 1 1 calc .
C8 C 0.1208(5) -0.3607(4) 0.0142(3) 0.0382(12) Uani 1 1 d .
C9 C 0.0643(5) -0.4194(4) -0.0513(3) 0.0402(13) Uani 1 1 d .
C10 C -0.2536(7) -0.3994(5) -0.1886(4) 0.0656(18) Uani 1 1 d .
H10A H -0.2774 -0.3431 -0.1594 0.080 Uiso 1 1 calc .
H10B H -0.3111 -0.4602 -0.1934 0.080 Uiso 1 1 calc .
H10C H -0.2576 -0.3707 -0.2362 0.080 Uiso 1 1 calc .
C11 C 0.4460(5) -0.1181(4) 0.0450(3) 0.0454(14) Uani 1 1 d .
C12 C 0.5096(5) -0.1887(5) 0.0094(4) 0.0559(16) Uani 1 1 d .
H12 H 0.5957 -0.2034 0.0298 0.080 Uiso 1 1 calc .
C13 C 0.4462(6) -0.2365(5) -0.0553(4) 0.0599(18) Uani 1 1 d .
H13 H 0.4903 -0.2837 -0.0781 0.080 Uiso 1 1 calc .
C14 C 0.3153(5) -0.2164(4) -0.0887(3) 0.0407(13) Uani 1 1 d .
C15 C 0.2433(6) -0.2618(4) -0.1554(3) 0.0480(15) Uani 1 1 d .
H15 H 0.2815 -0.3087 -0.1818 0.080 Uiso 1 1 calc .
C16 C 0.1178(6) -0.2367(4) -0.1809(3) 0.0450(14) Uani 1 1 d .
H16 H 0.0710 -0.2664 -0.2253 0.080 Uiso 1 1 calc .
C17 C 0.0560(5) -0.1665(4) -0.1420(3) 0.0378(12) Uani 1 1 d .
H17 H -0.0304 -0.1518 -0.1609 0.080 Uiso 1 1 calc .
C18 C 0.1211(4) -0.1201(3) -0.0772(3) 0.0291(10) Uani 1 1 d .
C19 C 0.2528(4) -0.1455(3) -0.0508(3) 0.0304(11) Uani 1 1 d .
C20 C 0.5072(5) -0.0615(5) 0.1153(4) 0.0612(17) Uani 1 1 d .
H20A H 0.4452 -0.0169 0.1293 0.080 Uiso 1 1 calc .
H20B H 0.5755 -0.0160 0.1094 0.080 Uiso 1 1 calc .
H20C H 0.5404 -0.1151 0.1528 0.080 Uiso 1 1 calc .
C21 C 0.4094(11) 0.1266(8) 0.2920(7) 0.129(4) Uani 1 1 d D
H21A H 0.4314 0.1585 0.3408 0.080 Uiso 1 1 calc .
H21B H 0.3224 0.1480 0.2676 0.080 Uiso 1 1 calc .
C22 C 0.4930(10) 0.1718(8) 0.2520(5) 0.113(3) Uani 1 1 d .
H22A H 0.4856 0.2502 0.2505 0.080 Uiso 1 1 calc .
H22B H 0.4695 0.1433 0.2029 0.080 Uiso 1 1 calc .
H22C H 0.5795 0.1516 0.2759 0.080 Uiso 1 1 calc .
H99 H 0.371(7) -0.0311(15) 0.267(3) 0.135 Uiso 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'
Dy Dy -0.1892 4.4098 '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'
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 O2 156.99(12) . 3
O1 Dy1 O2 88.06(12) . .
O2 Dy1 O2 69.20(11) 3 .
O1 Dy1 Cl2 107.48(10) . .
O2 Dy1 Cl2 94.89(8) 3 .
O2 Dy1 Cl2 163.58(7) . .
O1 Dy1 Cl1 89.36(10) . .
O2 Dy1 Cl1 94.38(9) 3 .
O2 Dy1 Cl1 91.20(8) . .
Cl2 Dy1 Cl1 94.17(5) . .
O1 Dy1 Cl3 86.67(10) . .
O2 Dy1 Cl3 88.33(8) 3 .
O2 Dy1 Cl3 86.19(8) . .
Cl2 Dy1 Cl3 89.40(5) . .
Cl1 Dy1 Cl3 175.32(4) . .
O1 Dy1 Dy1 122.07(10) . 3
O2 Dy1 Dy1 35.12(7) 3 3
O2 Dy1 Dy1 34.08(7) . 3
Cl2 Dy1 Dy1 129.89(3) . 3
Cl1 Dy1 Dy1 93.36(4) . 3
Cl3 Dy1 Dy1 86.65(3) . 3
C1 N1 C9 124.7(5) . .
C1 N1 H1 117.6 . .
C9 N1 H1 117.6 . .
C11 N2 C19 124.3(4) . .
C11 N2 H2 117.8 . .
C19 N2 H2 117.8 . .
C8 O1 Dy1 161.7(3) . .
C18 O2 Dy1 126.3(3) . 3
C18 O2 Dy1 121.8(2) . .
Dy1 O2 Dy1 110.80(11) 3 .
C21 O3 H99 124(2) . .
N1 C1 C2 116.5(6) . .
N1 C1 C10 119.7(5) . .
C2 C1 C10 123.8(6) . .
C3 C2 C1 121.5(7) . .
C3 C2 H2A 119.3 . .
C1 C2 H2A 119.3 . .
C2 C3 C4 121.7(6) . .
C2 C3 H3A 119.2 . .
C4 C3 H3A 119.2 . .
C9 C4 C5 117.5(6) . .
C9 C4 C3 116.4(6) . .
C5 C4 C3 126.1(6) . .
C6 C5 C4 120.8(5) . .
C6 C5 H5 119.6 . .
C4 C5 H5 119.6 . .
C5 C6 C7 121.5(6) . .
C5 C6 H6 119.3 . .
C7 C6 H6 119.3 . .
C8 C7 C6 120.2(6) . .
C8 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
O1 C8 C7 123.8(5) . .
O1 C8 C9 119.3(5) . .
C7 C8 C9 116.8(5) . .
N1 C9 C4 119.2(5) . .
N1 C9 C8 117.5(4) . .
C4 C9 C8 123.2(5) . .
C1 C10 H10A 109.5 . .
C1 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C1 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N2 C11 C12 117.9(5) . .
N2 C11 C20 117.9(5) . .
C12 C11 C20 124.2(5) . .
C13 C12 C11 120.2(5) . .
C13 C12 H12 119.9 . .
C11 C12 H12 119.9 . .
C12 C13 C14 122.0(5) . .
C12 C13 H13 119.0 . .
C14 C13 H13 119.0 . .
C15 C14 C19 118.0(5) . .
C15 C14 C13 125.5(5) . .
C19 C14 C13 116.4(5) . .
C16 C15 C14 119.5(5) . .
C16 C15 H15 120.3 . .
C14 C15 H15 120.3 . .
C15 C16 C17 121.9(5) . .
C15 C16 H16 119.0 . .
C17 C16 H16 119.0 . .
C18 C17 C16 121.1(5) . .
C18 C17 H17 119.5 . .
C16 C17 H17 119.5 . .
O2 C18 C17 125.3(4) . .
O2 C18 C19 117.6(4) . .
C17 C18 C19 117.0(4) . .
N2 C19 C14 119.0(4) . .
N2 C19 C18 118.5(4) . .
C14 C19 C18 122.4(5) . .
C11 C20 H20A 109.5 . .
C11 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C11 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
O3 C21 C22 114.0(10) . .
O3 C21 H21A 108.7 . .
C22 C21 H21A 108.7 . .
O3 C21 H21B 108.7 . .
C22 C21 H21B 108.7 . .
H21A C21 H21B 107.6 . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.135(3) .
Dy1 O2 2.300(3) 3
Dy1 O2 2.361(3) .
Dy1 Cl2 2.6098(14) .
Dy1 Cl1 2.6424(17) .
Dy1 Cl3 2.6743(16) .
Dy1 Dy1 3.8368(7) 3
N1 C1 1.329(7) .
N1 C9 1.380(7) .
N1 H1 0.8600 .
N2 C11 1.347(6) .
N2 C19 1.366(6) .
N2 H2 0.8600 .
O1 C8 1.318(5) .
O2 C18 1.351(5) .
O2 Dy1 2.300(3) 3
O3 C21 1.391(10) .
O3 H99 0.850(10) .
C1 C2 1.405(9) .
C1 C10 1.472(9) .
C2 C3 1.343(10) .
C2 H2A 0.9300 .
C3 C4 1.416(9) .
C3 H3A 0.9300 .
C4 C9 1.396(7) .
C4 C5 1.406(9) .
C5 C6 1.358(10) .
C5 H5 0.9300 .
C6 C7 1.412(8) .
C6 H6 0.9300 .
C7 C8 1.394(8) .
C7 H7 0.9300 .
C8 C9 1.420(7) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 C12 1.391(8) .
C11 C20 1.488(8) .
C12 C13 1.363(9) .
C12 H12 0.9300 .
C13 C14 1.416(8) .
C13 H13 0.9300 .
C14 C15 1.407(8) .
C14 C19 1.414(6) .
C15 C16 1.356(8) .
C15 H15 0.9300 .
C16 C17 1.417(7) .
C16 H16 0.9300 .
C17 C18 1.362(7) .
C17 H17 0.9300 .
C18 C19 1.420(6) .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 C22 1.447(13) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
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
N1 H1 Cl3 0.86 2.52 3.350(4) 163.5 .
N2 H2 Cl1 0.86 2.78 3.399(4) 130.6 .
N2 H2 Cl3 0.86 2.94 3.672(4) 143.7 3
O3 H99 Cl1 0.850(10) 2.50(2) 3.295(7) 157(4) .
