#------------------------------------------------------------------------------
#$Date: 2017-09-29 05:58:07 +0300 (Fri, 29 Sep 2017) $
#$Revision: 201490 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/43/7044353.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_7044353
loop_
_publ_author_name
'Perlepes, Spyros P.'
'Polyzou, Christina D.'
'Koumousi, Evangelia S.'
'Lada, Zoi G.'
'Raptopoulou, Catherine P.'
'Psycharis, Vassilis'
'Rouzieres, Mathieu'
'Tsipis, Athanassios C.'
'Mathoniere, Corine'
'Clerac, Rodolphe'
_publ_section_title
;
 “Switching on” the single-molecule magnet properties within
 a series of dinuclear cobalt(III)-dysprosium(III) 2-pyridyloximate
 complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02717F
_journal_year                    2017
_chemical_formula_sum            'C21 H30 Co Dy N12 O15'
_chemical_formula_weight         912.00
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-09-14 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   16.51370(10)
_cell_length_b                   16.51370(10)
_cell_length_c                   20.9946(5)
_cell_measurement_reflns_used    36323
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      71.98
_cell_measurement_theta_min      6.54
_cell_volume                     4958.23(13)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48920
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.981
_diffrn_reflns_theta_min         6.822
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    11.104
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0445P)²+3.1629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2431
_reflns_number_total             2819
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02717f2.cif
_cod_data_source_block           shelx
_cod_database_code               7044353
_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.
;
_shelxl_version_number           2014/6
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, 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
_atom_site_refinement_flags_occupancy
Co Co 0.6667 0.3333 0.05616(3) 0.01550(19) Uani 1 3 d S T P
Dy Dy 0.6667 0.3333 -0.12365(2) 0.01865(12) Uani 1 3 d S T P
O1 O 0.54349(14) 0.26847(12) -0.05240(8) 0.0203(4) Uani 1 1 d . . .
N1 N 0.63423(15) 0.22094(16) 0.10525(10) 0.0184(5) Uani 1 1 d . . .
N2 N 0.56625(14) 0.24699(15) 0.00516(9) 0.0184(5) Uani 1 1 d . . .
N3 N 0.45280(17) 0.09099(16) -0.01074(10) 0.0299(6) Uani 1 1 d . . .
H3A H 0.4353 0.1037 -0.0472 0.036 Uiso 1 1 calc R U .
H3B H 0.4251 0.0332 0.0036 0.036 Uiso 1 1 calc R U .
C1 C 0.6756(2) 0.2133(2) 0.15786(12) 0.0234(6) Uani 1 1 d . . .
C2 C 0.6434(2) 0.1292(2) 0.18941(13) 0.0299(7) Uani 1 1 d . . .
C3 C 0.5648(2) 0.0507(2) 0.16689(14) 0.0336(7) Uani 1 1 d . . .
C4 C 0.5203(2) 0.0574(2) 0.11267(14) 0.0273(7) Uani 1 1 d . . .
C5 C 0.55737(18) 0.1433(2) 0.08264(12) 0.0197(6) Uani 1 1 d . . .
C6 C 0.52182(18) 0.15982(18) 0.02304(11) 0.0198(6) Uani 1 1 d . . .
N11 N 0.82723(18) 0.48080(17) -0.18964(11) 0.0338(6) Uani 1 1 d . . .
O11 O 0.83705(15) 0.43401(14) -0.14620(9) 0.0304(5) Uani 1 1 d . . .
O12 O 0.74327(16) 0.45934(19) -0.20171(11) 0.0435(6) Uani 1 1 d . . .
O13 O 0.89285(17) 0.54242(18) -0.21818(13) 0.0633(8) Uani 1 1 d . . .
O1M O 0.41272(18) 0.31847(16) -0.02649(12) 0.0467(6) Uani 1 1 d . . .
C1M C 0.3473(3) 0.2421(3) 0.0097(2) 0.0745(13) Uani 1 1 d . . .
H1MA H 0.3783 0.2354 0.0465 0.097 Uiso 1 1 d . U .
H1MB H 0.3233 0.1864 -0.0159 0.097 Uiso 1 1 d . U .
H1MC H 0.2979 0.2521 0.0225 0.097 Uiso 1 1 d . U .
H1 H 0.727(2) 0.266(2) 0.1736(15) 0.026(9) Uiso 1 1 d . . .
H2 H 0.681(2) 0.125(2) 0.2241(15) 0.043(9) Uiso 1 1 d . . .
H3 H 0.537(2) -0.008(2) 0.1874(14) 0.041(9) Uiso 1 1 d . . .
H4 H 0.463(2) 0.008(2) 0.0978(12) 0.024(7) Uiso 1 1 d . . .
H1OM H 0.457(3) 0.306(3) -0.0319(19) 0.074(14) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 '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
N2 Co N2 91.01(9) 2_655 3_665
N2 Co N2 91.01(9) 2_655 .
N2 Co N2 91.01(9) 3_665 .
N2 Co N1 92.73(9) 2_655 .
N2 Co N1 172.15(9) 3_665 .
N2 Co N1 82.03(9) . .
N2 Co N1 82.03(9) 2_655 2_655
N2 Co N1 92.73(9) 3_665 2_655
N2 Co N1 172.15(9) . 2_655
N1 Co N1 94.63(9) . 2_655
N2 Co N1 172.15(9) 2_655 3_665
N2 Co N1 82.03(9) 3_665 3_665
N2 Co N1 92.73(9) . 3_665
N1 Co N1 94.63(9) . 3_665
N1 Co N1 94.63(9) 2_655 3_665
O1 Dy O1 82.65(7) 3_665 .
O1 Dy O1 82.64(7) 3_665 2_655
O1 Dy O1 82.65(7) . 2_655
O1 Dy O12 142.05(7) 3_665 3_665
O1 Dy O12 129.62(7) . 3_665
O1 Dy O12 82.77(8) 2_655 3_665
O1 Dy O12 129.62(7) 3_665 2_655
O1 Dy O12 82.77(8) . 2_655
O1 Dy O12 142.05(7) 2_655 2_655
O12 Dy O12 80.02(10) 3_665 2_655
O1 Dy O12 82.77(8) 3_665 .
O1 Dy O12 142.06(7) . .
O1 Dy O12 129.62(7) 2_655 .
O12 Dy O12 80.02(10) 3_665 .
O12 Dy O12 80.02(10) 2_655 .
O1 Dy O11 72.64(6) 3_665 .
O1 Dy O11 150.38(7) . .
O1 Dy O11 78.31(6) 2_655 .
O12 Dy O11 70.18(7) 3_665 .
O12 Dy O11 125.65(8) 2_655 .
O12 Dy O11 51.31(7) . .
O1 Dy O11 150.38(7) 3_665 3_665
O1 Dy O11 78.31(6) . 3_665
O1 Dy O11 72.64(6) 2_655 3_665
O12 Dy O11 51.31(7) 3_665 3_665
O12 Dy O11 70.18(7) 2_655 3_665
O12 Dy O11 125.65(8) . 3_665
O11 Dy O11 116.49(3) . 3_665
O1 Dy O11 78.31(6) 3_665 2_655
O1 Dy O11 72.64(6) . 2_655
O1 Dy O11 150.38(7) 2_655 2_655
O12 Dy O11 125.65(8) 3_665 2_655
O12 Dy O11 51.31(7) 2_655 2_655
O12 Dy O11 70.18(7) . 2_655
O11 Dy O11 116.49(3) . 2_655
O11 Dy O11 116.49(3) 3_665 2_655
O1 Dy N11 157.03(6) 3_665 3_665
O1 Dy N11 103.84(7) . 3_665
O1 Dy N11 76.50(6) 2_655 3_665
O12 Dy N11 25.78(7) 3_665 3_665
O12 Dy N11 73.33(7) 2_655 3_665
O12 Dy N11 103.18(8) . 3_665
O11 Dy N11 93.57(7) . 3_665
O11 Dy N11 25.54(6) 3_665 3_665
O11 Dy N11 124.64(7) 2_655 3_665
O1 Dy N11 103.84(7) 3_665 2_655
O1 Dy N11 76.50(6) . 2_655
O1 Dy N11 157.04(6) 2_655 2_655
O12 Dy N11 103.18(8) 3_665 2_655
O12 Dy N11 25.78(7) 2_655 2_655
O12 Dy N11 73.33(7) . 2_655
O11 Dy N11 124.64(7) . 2_655
O11 Dy N11 93.57(7) 3_665 2_655
O11 Dy N11 25.54(6) 2_655 2_655
N11 Dy N11 99.10(6) 3_665 2_655
O1 Dy N11 76.50(6) 3_665 .
O1 Dy N11 157.04(6) . .
O1 Dy N11 103.84(7) 2_655 .
O12 Dy N11 73.33(7) 3_665 .
O12 Dy N11 103.18(8) 2_655 .
O12 Dy N11 25.78(6) . .
O11 Dy N11 25.53(6) . .
O11 Dy N11 124.64(7) 3_665 .
O11 Dy N11 93.57(7) 2_655 .
N11 Dy N11 99.10(6) 3_665 .
N11 Dy N11 99.10(6) 2_655 .
N2 O1 Dy 113.62(14) . .
C1 N1 C5 118.6(2) . .
C1 N1 Co 128.1(2) . .
C5 N1 Co 113.31(17) . .
C6 N2 O1 117.8(2) . .
C6 N2 Co 117.91(17) . .
O1 N2 Co 123.93(16) . .
C6 N3 H3A 120.0 . .
C6 N3 H3B 120.0 . .
H3A N3 H3B 120.0 . .
N1 C1 C2 122.2(3) . .
N1 C1 H1 119(2) . .
C2 C1 H1 119(2) . .
C3 C2 C1 119.2(3) . .
C3 C2 H2 121.5(18) . .
C1 C2 H2 118.9(19) . .
C2 C3 C4 119.5(3) . .
C2 C3 H3 123.3(19) . .
C4 C3 H3 117(2) . .
C5 C4 C3 118.4(3) . .
C5 C4 H4 118.7(16) . .
C3 C4 H4 122.7(16) . .
N1 C5 C4 122.2(2) . .
N1 C5 C6 113.2(2) . .
C4 C5 C6 124.6(3) . .
N2 C6 N3 123.7(2) . .
N2 C6 C5 113.3(2) . .
N3 C6 C5 122.9(2) . .
O13 N11 O11 122.6(3) . .
O13 N11 O12 121.9(3) . .
O11 N11 O12 115.5(2) . .
O13 N11 Dy 178.5(2) . .
O11 N11 Dy 58.83(14) . .
O12 N11 Dy 56.67(14) . .
N11 O11 Dy 95.63(16) . .
N11 O12 Dy 97.55(16) . .
C1M O1M H1OM 103(3) . .
O1M C1M H1MA 108.9 . .
O1M C1M H1MB 108.8 . .
H1MA C1M H1MB 109.0 . .
O1M C1M H1MC 109.7 . .
H1MA C1M H1MC 110.2 . .
H1MB C1M H1MC 110.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co N2 1.888(2) 2_655
Co N2 1.888(2) 3_665
Co N2 1.888(2) .
Co N1 1.949(2) .
Co N1 1.949(2) 2_655
Co N1 1.949(2) 3_665
Dy O1 2.3116(19) 3_665
Dy O1 2.3116(19) .
Dy O1 2.3117(19) 2_655
Dy O12 2.446(2) 3_665
Dy O12 2.446(2) 2_655
Dy O12 2.446(2) .
Dy O11 2.495(2) .
Dy O11 2.495(2) 3_665
Dy O11 2.495(2) 2_655
Dy N11 2.902(2) 3_665
Dy N11 2.902(2) 2_655
Dy N11 2.902(2) .
O1 N2 1.364(3) .
N1 C1 1.338(3) .
N1 C5 1.362(4) .
N2 C6 1.302(3) .
N3 C6 1.341(3) .
N3 H3A 0.8800 .
N3 H3B 0.8800 .
C1 C2 1.383(4) .
C1 H1 0.92(3) .
C2 C3 1.381(4) .
C2 H2 0.98(3) .
C3 C4 1.389(4) .
C3 H3 0.94(3) .
C4 C5 1.384(4) .
C4 H4 0.94(3) .
C5 C6 1.465(3) .
N11 O13 1.211(3) .
N11 O11 1.257(3) .
N11 O12 1.273(3) .
O1M C1M 1.404(4) .
O1M H1OM 0.86(4) .
C1M H1MA 0.9630 .
C1M H1MB 0.9622 .
C1M H1MC 0.9490 .
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
O1M H1OM O1 0.86(4) 1.87(4) 2.725(3) 172(4) .
N3 H3B O1M 0.88 2.01 2.847(3) 157.6 8
C3 H3 O11 0.94(3) 2.56(3) 3.216(4) 127(2) 9_545
C4 H4 O11 0.94(3) 2.68(3) 3.231(4) 119(2) 9_545
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.001 2086 372 ' '
