#------------------------------------------------------------------------------
#$Date: 2016-06-14 11:04:59 +0300 (Tue, 14 Jun 2016) $
#$Revision: 183455 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/55/7225521.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_7225521
loop_
_publ_author_name
'Jiang, Y.'
'Holmberg, R. J.'
'Habib, F.'
'Ungur, L.'
'Korobkov, I.'
'Chibotaru, L. F.'
'Murugesu, M.'
_publ_section_title
;
 Probing the structural and magnetic properties of a new family of
 centrosymmetric dinuclear lanthanide complexes
;
_journal_issue                   61
_journal_name_full               'RSC Adv.'
_journal_page_first              56668
_journal_paper_doi               10.1039/C6RA12070A
_journal_volume                  6
_journal_year                    2016
_chemical_formula_sum            'C38 H60 Dy2 N6 O14'
_chemical_formula_weight         1149.92
_chemical_name_systematic        2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-09-22 deposited with the CCDC.
2016-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.218(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3404(5)
_cell_length_b                   8.3937(3)
_cell_length_c                   20.8588(8)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.62
_cell_volume                     2282.77(15)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35453
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.407
_diffrn_reflns_theta_min         1.562
_exptl_absorpt_coefficient_mu    3.316
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.207
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0529P)²+6.8197P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4290
_reflns_number_total             5642
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra12070a2.cif
_cod_data_source_block           mm300
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               7225521
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.692
_shelx_estimated_absorpt_t_max   0.826
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Dy1 Dy 0.36511(2) 0.97254(3) 0.52486(2) 0.02302(9) Uani 1 1 d . .
O1 O 0.2954(3) 0.9770(5) 0.6152(2) 0.0309(10) Uani 1 1 d . .
O2 O 0.1453(4) 1.0824(6) 0.6668(3) 0.0481(13) Uani 1 1 d . .
O3 O 0.5317(3) 0.8731(4) 0.5341(2) 0.0233(9) Uani 1 1 d . .
O4 O 0.1984(3) 0.8881(6) 0.4902(2) 0.0383(11) Uani 1 1 d . .
O5 O 0.3512(3) 0.8262(6) 0.4254(2) 0.0336(10) Uani 1 1 d . .
O6 O 0.4557(3) 1.1633(5) 0.5966(2) 0.0358(11) Uani 1 1 d . .
H6A H 0.5253 1.1733 0.5921 0.054 Uiso 1 1 d R U
H6B H 0.4489 1.1979 0.6415 0.054 Uiso 1 1 d R U
O7 O 0.3516(4) 1.2532(6) 0.6849(3) 0.0535(15) Uani 1 1 d . .
H7D H 0.3175 1.1706 0.6722 0.064 Uiso 1 1 calc R U
N1 N 0.4001(4) 0.7155(6) 0.5804(3) 0.0267(11) Uani 1 1 d . .
N2 N 0.4893(4) 0.6303(6) 0.5734(3) 0.0313(12) Uani 1 1 d . .
N3 N 0.7217(4) 0.7709(6) 0.5305(3) 0.0319(13) Uani 1 1 d . .
C1 C 0.2369(4) 0.8690(7) 0.6341(3) 0.0272(13) Uani 1 1 d . .
C2 C 0.1518(5) 0.9190(9) 0.6614(4) 0.0354(15) Uani 1 1 d . .
C3 C 0.0866(5) 0.8111(10) 0.6794(4) 0.050(2) Uani 1 1 d . .
H3A H 0.0295 0.8475 0.6959 0.060 Uiso 1 1 calc R U
C4 C 0.1023(6) 0.6498(10) 0.6742(4) 0.055(2) Uani 1 1 d . .
H4A H 0.0550 0.5761 0.6857 0.066 Uiso 1 1 calc R U
C5 C 0.1856(6) 0.5960(9) 0.6524(4) 0.048(2) Uani 1 1 d . .
H5A H 0.1985 0.4848 0.6515 0.058 Uiso 1 1 calc R U
C6 C 0.2532(5) 0.7056(8) 0.6312(3) 0.0316(15) Uani 1 1 d . .
C7 C 0.0772(7) 1.1413(11) 0.7056(5) 0.062(2) Uani 1 1 d . .
H7A H 0.0785 1.2581 0.7056 0.093 Uiso 1 1 calc R U
H7B H 0.0988 1.1022 0.7506 0.093 Uiso 1 1 calc R U
H7C H 0.0074 1.1043 0.6871 0.093 Uiso 1 1 calc R U
C8 C 0.3434(5) 0.6376(8) 0.6122(3) 0.0325(14) Uani 1 1 d . .
H8A H 0.3610 0.5303 0.6240 0.039 Uiso 1 1 calc R U
C9 C 0.5480(4) 0.7220(7) 0.5479(3) 0.0250(12) Uani 1 1 d . .
C10 C 0.6416(5) 0.6509(7) 0.5301(4) 0.0327(15) Uani 1 1 d . .
H10A H 0.6688 0.5655 0.5617 0.039 Uiso 1 1 calc R U
H10B H 0.6226 0.6025 0.4859 0.039 Uiso 1 1 calc R U
C11 C 0.7977(6) 0.7139(10) 0.4944(5) 0.058(2) Uani 1 1 d . .
H11A H 0.7635 0.6886 0.4492 0.087 Uiso 1 1 calc R U
H11B H 0.8312 0.6181 0.5157 0.087 Uiso 1 1 calc R U
H11C H 0.8492 0.7970 0.4941 0.087 Uiso 1 1 calc R U
C12 C 0.7728(6) 0.8084(10) 0.5991(4) 0.051(2) Uani 1 1 d . .
H12A H 0.7216 0.8462 0.6231 0.077 Uiso 1 1 calc R U
H12B H 0.8244 0.8916 0.5993 0.077 Uiso 1 1 calc R U
H12C H 0.8061 0.7124 0.6204 0.077 Uiso 1 1 calc R U
C13 C 0.1497(5) 0.7870(9) 0.4515(4) 0.0370(16) Uani 1 1 d . .
C14 C 0.1856(5) 0.7167(9) 0.4008(4) 0.0396(17) Uani 1 1 d . .
H14A H 0.1411 0.6467 0.3722 0.048 Uiso 1 1 calc R U
C15 C 0.2837(5) 0.7428(8) 0.3892(3) 0.0317(14) Uani 1 1 d . .
C16 C 0.0448(6) 0.7434(12) 0.4628(5) 0.062(2) Uani 1 1 d . .
H16A H 0.0313 0.8029 0.5005 0.093 Uiso 1 1 calc R U
H16B H 0.0424 0.6289 0.4714 0.093 Uiso 1 1 calc R U
H16C H -0.0074 0.7702 0.4236 0.093 Uiso 1 1 calc R U
C17 C 0.3133(6) 0.6679(10) 0.3301(4) 0.049(2) Uani 1 1 d . .
H17A H 0.3840 0.6972 0.3291 0.073 Uiso 1 1 calc R U
H17B H 0.2671 0.7062 0.2901 0.073 Uiso 1 1 calc R U
H17C H 0.3078 0.5518 0.3328 0.073 Uiso 1 1 calc R U
C18 C 0.3699(9) 1.2627(12) 0.7538(5) 0.075(3) Uani 1 1 d . .
H18A H 0.4028 1.1629 0.7730 0.090 Uiso 1 1 calc R U
H18B H 0.3037 1.2741 0.7677 0.090 Uiso 1 1 calc R U
C19 C 0.4349(10) 1.3956(13) 0.7779(6) 0.093(4) Uani 1 1 d . .
H19A H 0.4476 1.3978 0.8259 0.140 Uiso 1 1 calc R U
H19B H 0.4012 1.4948 0.7603 0.140 Uiso 1 1 calc R U
H19C H 0.5002 1.3849 0.7639 0.140 Uiso 1 1 calc R U
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 O4 74.18(16) . .
O1 Dy1 O3 119.03(15) . .
O4 Dy1 O3 138.87(16) . .
O1 Dy1 O6 72.90(15) . .
O4 Dy1 O6 138.13(16) . .
O3 Dy1 O6 80.72(15) . .
O1 Dy1 O3 142.50(15) . 3_676
O4 Dy1 O3 128.62(16) . 3_676
O3 Dy1 O3 66.37(16) . 3_676
O6 Dy1 O3 71.66(15) . 3_676
O1 Dy1 O5 139.48(15) . .
O4 Dy1 O5 71.07(15) . .
O3 Dy1 O5 77.66(14) . .
O6 Dy1 O5 147.32(14) . .
O3 Dy1 O5 77.32(14) 3_676 .
O1 Dy1 N1 72.09(16) . .
O4 Dy1 N1 87.23(17) . .
O3 Dy1 N1 64.19(14) . .
O6 Dy1 N1 106.24(17) . .
O3 Dy1 N1 130.07(14) 3_676 .
O5 Dy1 N1 85.95(17) . .
O1 Dy1 N3 97.63(16) . 3_676
O4 Dy1 N3 78.77(17) . 3_676
O3 Dy1 N3 131.12(14) . 3_676
O6 Dy1 N3 80.70(18) . 3_676
O3 Dy1 N3 64.93(14) 3_676 3_676
O5 Dy1 N3 95.45(17) . 3_676
N1 Dy1 N3 164.59(16) . 3_676
O1 Dy1 Dy1 140.03(11) . 3_676
O4 Dy1 Dy1 145.27(12) . 3_676
O3 Dy1 Dy1 33.69(9) . 3_676
O6 Dy1 Dy1 73.41(10) . 3_676
O3 Dy1 Dy1 32.68(9) 3_676 3_676
O5 Dy1 Dy1 75.00(10) . 3_676
N1 Dy1 Dy1 97.66(11) . 3_676
N3 Dy1 Dy1 97.53(11) 3_676 3_676
C1 O1 Dy1 127.8(4) . .
C2 O2 C7 116.7(6) . .
C9 O3 Dy1 118.2(3) . .
C9 O3 Dy1 123.2(3) . 3_676
Dy1 O3 Dy1 113.63(15) . 3_676
C13 O4 Dy1 138.3(4) . .
C15 O5 Dy1 136.3(4) . .
C8 N1 N2 113.2(5) . .
C8 N1 Dy1 128.2(4) . .
N2 N1 Dy1 118.3(3) . .
C9 N2 N1 109.6(5) . .
C10 N3 C11 110.8(6) . .
C10 N3 C12 109.7(5) . .
C11 N3 C12 109.8(6) . .
C10 N3 Dy1 108.1(4) . 3_676
C11 N3 Dy1 109.5(4) . 3_676
C12 N3 Dy1 108.9(4) . 3_676
O1 C1 C6 124.1(5) . .
O1 C1 C2 119.2(6) . .
C6 C1 C2 116.7(5) . .
C3 C2 O2 125.7(6) . .
C3 C2 C1 121.2(6) . .
O2 C2 C1 113.0(5) . .
C2 C3 C4 121.0(6) . .
C5 C4 C3 120.1(7) . .
C4 C5 C6 120.3(7) . .
C1 C6 C5 120.5(6) . .
C1 C6 C8 122.9(5) . .
C5 C6 C8 116.4(6) . .
N1 C8 C6 123.4(6) . .
N2 C9 O3 125.6(5) . .
N2 C9 C10 118.3(5) . .
O3 C9 C10 116.0(5) . .
N3 C10 C9 111.7(5) . .
O4 C13 C14 124.4(6) . .
O4 C13 C16 115.8(7) . .
C14 C13 C16 119.8(7) . .
C13 C14 C15 123.6(6) . .
O5 C15 C14 124.1(6) . .
O5 C15 C17 116.4(6) . .
C14 C15 C17 119.5(6) . .
O7 C18 C19 111.2(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.271(4) .
Dy1 O4 2.301(4) .
Dy1 O3 2.344(4) .
Dy1 O6 2.345(4) .
Dy1 O3 2.408(4) 3_676
Dy1 O5 2.385(4) .
Dy1 N1 2.446(5) .
Dy1 N3 2.597(5) 3_676
Dy1 Dy1 3.9775(5) 3_676
O1 C1 1.311(7) .
O2 C2 1.380(9) .
O2 C7 1.427(8) .
O3 C9 1.308(7) .
O3 Dy1 2.408(4) 3_676
O4 C13 1.253(9) .
O5 C15 1.258(7) .
O7 C18 1.408(10) .
N1 C8 1.286(7) .
N1 N2 1.422(7) .
N2 C9 1.290(7) .
N3 C10 1.467(8) .
N3 C11 1.465(8) .
N3 C12 1.484(9) .
N3 Dy1 2.597(5) 3_676
C1 C6 1.392(9) .
C1 C2 1.437(8) .
C2 C3 1.363(9) .
C3 C4 1.377(11) .
C4 C5 1.363(10) .
C5 C6 1.423(9) .
C6 C8 1.460(8) .
C9 C10 1.501(8) .
C13 C14 1.384(10) .
C13 C16 1.512(9) .
C14 C15 1.397(9) .
C15 C17 1.508(9) .
C18 C19 1.437(13) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C8 N1 N2 C9 -172.6(6) .
Dy1 N1 N2 C9 12.4(7) .
Dy1 O1 C1 C6 41.3(9) .
Dy1 O1 C1 C2 -140.4(5) .
C7 O2 C2 C3 12.5(11) .
C7 O2 C2 C1 -167.3(7) .
O1 C1 C2 C3 177.5(7) .
C6 C1 C2 C3 -4.1(11) .
O1 C1 C2 O2 -2.7(9) .
C6 C1 C2 O2 175.7(6) .
O2 C2 C3 C4 -177.6(8) .
C1 C2 C3 C4 2.2(13) .
C2 C3 C4 C5 1.9(14) .
C3 C4 C5 C6 -4.0(14) .
O1 C1 C6 C5 -179.6(7) .
C2 C1 C6 C5 2.0(10) .
O1 C1 C6 C8 5.9(11) .
C2 C1 C6 C8 -172.4(6) .
C4 C5 C6 C1 1.9(12) .
C4 C5 C6 C8 176.7(8) .
N2 N1 C8 C6 173.9(6) .
Dy1 N1 C8 C6 -11.8(10) .
C1 C6 C8 N1 -19.4(11) .
C5 C6 C8 N1 166.0(7) .
N1 N2 C9 O3 3.9(9) .
N1 N2 C9 C10 -174.1(6) .
Dy1 O3 C9 N2 -19.1(8) .
Dy1 O3 C9 N2 -172.6(5) 3_676
Dy1 O3 C9 C10 158.9(4) .
Dy1 O3 C9 C10 5.4(7) 3_676
C11 N3 C10 C9 -162.6(6) .
C12 N3 C10 C9 76.1(7) .
Dy1 N3 C10 C9 -42.5(6) 3_676
N2 C9 C10 N3 -154.2(6) .
O3 C9 C10 N3 27.6(8) .
Dy1 O4 C13 C14 -19.5(12) .
Dy1 O4 C13 C16 160.9(6) .
O4 C13 C14 C15 4.3(12) .
C16 C13 C14 C15 -176.1(7) .
Dy1 O5 C15 C14 1.7(11) .
Dy1 O5 C15 C17 -178.2(5) .
C13 C14 C15 O5 3.7(12) .
C13 C14 C15 C17 -176.4(7) .
