#------------------------------------------------------------------------------
#$Date: 2019-11-23 02:25:04 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231875 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/66/4346609.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_4346609
loop_
_publ_author_name
'Zhang, Yan'
'Guo, Zhen'
'Xie, Shuang'
'Li, Hui-Li'
'Zhu, Wen-Hua'
'Liu, Li'
'Dong, Xun-Qing'
'He, Wei-Xun'
'Ren, Jin-Chao'
'Liu, Ling-Zhi'
'Powell, Annie K.'
_publ_section_title
;
 Tuning the Origin of Magnetic Relaxation by Substituting the 3d or
 Rare-Earth Ions into Three Isostructural Cyano-Bridged 3d-4f
 Heterodinuclear Compounds.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10316
_journal_page_last               10322
_journal_paper_doi               10.1021/acs.inorgchem.5b01763
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C9 H15 Co0.5 Dy0.5 N4 O4'
_chemical_formula_sum            'C9 H15 Co0.5 Dy0.5 N4 O4'
_chemical_formula_weight         353.96
_chemical_name_common            '[DyCo(CN)6](hep)2(H2O)4,14Jun16d'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.400(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.1741(6)
_cell_length_b                   12.9082(6)
_cell_length_c                   15.2619(7)
_cell_measurement_reflns_used    5077
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.3831
_cell_measurement_theta_min      3.1557
_cell_volume                     2633.8(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.6
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7844
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.382
_diffrn_reflns_theta_min         3.156
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.501
_exptl_absorpt_correction_T_max  0.472
_exptl_absorpt_correction_T_min  0.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.00221(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2608
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0288
_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)+(0.0188P)²+8.4491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2240
_reflns_number_total             2608
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b01763_si_003.cif
_cod_data_source_block           a
_cod_original_formula_sum        'C9 H15 Co0.50 Dy0.50 N4 O4'
_cod_database_code               4346609
_shelxl_version_number           2014/6
_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_max   0.475
_shelx_estimated_absorpt_t_min   0.400
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O4-H4
 0.96 with sigma of 0.02
 O2-H2B = O2-H2A
 0.96 with sigma of 0.02
 H2B-H2A
 1.52 with sigma of 0.02
 O3-H3A = O3-H3B
 0.96 with sigma of 0.02
 H3A-H3B
 1.52 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Dy1 Dy 0.0000 0.81983(2) 0.7500 0.01813(11) Uani 1 2 d S T P
Co1 Co 0.0000 1.24688(5) 0.7500 0.01699(18) Uani 1 2 d S T P
C1 C 0.0000 1.1003(4) 0.7500 0.0214(12) Uani 1 2 d S T P
C2 C 0.0005(3) 1.2453(3) 0.6256(3) 0.0238(9) Uani 1 1 d . . .
C3 C -0.1421(3) 1.2515(3) 0.7058(3) 0.0260(9) Uani 1 1 d . . .
C4 C 0.0000 1.3928(4) 0.7500 0.0168(11) Uani 1 2 d S T P
C5 C -0.2145(3) 0.9361(3) 0.6113(3) 0.0275(9) Uani 1 1 d . . .
C6 C -0.3030(4) 0.9564(5) 0.6406(4) 0.0562(15) Uani 1 1 d . . .
H6A H -0.3412 0.8934 0.6378 0.067 Uiso 1 1 calc R . .
H6B H -0.2824 0.9832 0.7035 0.067 Uiso 1 1 calc R . .
C7 C -0.3624(4) 1.0332(5) 0.5748(5) 0.076(2) Uani 1 1 d . . .
H7A H -0.3757 1.0924 0.6079 0.091 Uiso 1 1 calc R . .
H7B H -0.4258 1.0033 0.5374 0.091 Uiso 1 1 calc R . .
C8 C -0.3043(4) 1.0657(4) 0.5145(4) 0.0481(13) Uani 1 1 d . . .
H8A H -0.3429 1.0559 0.4494 0.058 Uiso 1 1 calc R . .
H8B H -0.2849 1.1380 0.5248 0.058 Uiso 1 1 calc R . .
C9 C -0.1407(4) 0.9995(4) 0.4984(3) 0.0430(12) Uani 1 1 d . . .
H9A H -0.0838 0.9587 0.5351 0.052 Uiso 1 1 calc R . .
H9B H -0.1181 1.0701 0.4966 0.052 Uiso 1 1 calc R . .
C10 C -0.1787(4) 0.9571(4) 0.4014(4) 0.0493(13) Uani 1 1 d . . .
H10A H -0.2333 0.9999 0.3634 0.059 Uiso 1 1 calc R . .
H10B H -0.1256 0.9587 0.3744 0.059 Uiso 1 1 calc R . .
N1 N 0.0000 1.0112(4) 0.7500 0.0330(13) Uani 1 2 d S T P
N2 N 0.0031(3) 1.2422(3) 0.5514(3) 0.0376(10) Uani 1 1 d . . .
N3 N -0.2273(3) 1.2607(3) 0.6799(3) 0.0442(11) Uani 1 1 d . . .
N4 N 0.0000 1.4810(4) 0.7500 0.0453(15) Uani 1 2 d S T P
N5 N -0.2164(3) 0.9980(3) 0.5426(2) 0.0316(8) Uani 1 1 d . . .
O1 O -0.1477(2) 0.8700(2) 0.6470(2) 0.0380(8) Uani 1 1 d . . .
O2 O -0.0748(2) 0.8070(2) 0.8626(2) 0.0309(7) Uani 1 1 d D . .
O3 O -0.0902(2) 0.6726(2) 0.6789(3) 0.0483(9) Uani 1 1 d D . .
O4 O -0.2125(3) 0.8538(3) 0.4022(3) 0.0572(11) Uani 1 1 d D . .
H2A H -0.045(3) 0.785(4) 0.9244(18) 0.058(16) Uiso 1 1 d D . .
H2B H -0.1440(16) 0.794(5) 0.846(4) 0.10(2) Uiso 1 1 d D . .
H3A H -0.1603(15) 0.668(4) 0.653(4) 0.08(2) Uiso 1 1 d D . .
H3B H -0.065(4) 0.605(2) 0.695(5) 0.11(3) Uiso 1 1 d D . .
H4 H -0.158(3) 0.808(4) 0.418(5) 0.10(2) 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'
Co Co 0.3494 0.9721 '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 N1 73.31(8) . .
O1 Dy1 N1 73.30(8) 2_556 .
O1 Dy1 O1 146.61(16) . 2_556
O1 Dy1 O2 92.97(11) . 2_556
O1 Dy1 O2 89.39(11) . .
O1 Dy1 O2 92.97(11) 2_556 .
O1 Dy1 O2 89.39(11) 2_556 2_556
O1 Dy1 O3 70.94(11) 2_556 2_556
O1 Dy1 O3 142.39(12) . 2_556
O1 Dy1 O3 70.93(11) . .
O1 Dy1 O3 142.39(12) 2_556 .
O2 Dy1 N1 94.11(8) . .
O2 Dy1 N1 94.11(8) 2_556 .
O2 Dy1 O2 171.78(16) . 2_556
O2 Dy1 O3 88.39(13) 2_556 2_556
O2 Dy1 O3 84.95(13) . 2_556
O2 Dy1 O3 88.39(13) . .
O2 Dy1 O3 84.95(13) 2_556 .
O3 Dy1 N1 144.12(8) 2_556 .
O3 Dy1 N1 144.12(8) . .
O3 Dy1 O3 71.76(17) . 2_556
C1 Co1 C2 89.39(12) . 2_556
C1 Co1 C2 89.39(12) . .
C1 Co1 C3 91.81(13) . .
C1 Co1 C3 91.81(13) . 2_556
C2 Co1 C2 178.8(2) . 2_556
C2 Co1 C3 90.01(17) 2_556 .
C2 Co1 C3 90.03(17) 2_556 2_556
C2 Co1 C3 90.03(17) . .
C2 Co1 C3 90.01(17) . 2_556
C3 Co1 C3 176.4(3) 2_556 .
C4 Co1 C1 180.0 . .
C4 Co1 C2 90.61(12) . .
C4 Co1 C2 90.61(12) . 2_556
C4 Co1 C3 88.19(13) . .
C4 Co1 C3 88.19(13) . 2_556
N1 C1 Co1 180.0 . .
N2 C2 Co1 177.9(4) . .
N3 C3 Co1 175.9(4) . .
N4 C4 Co1 180.0 . .
N5 C5 C6 109.7(4) . .
O1 C5 C6 125.3(4) . .
O1 C5 N5 125.0(4) . .
C5 C6 H6A 110.7 . .
C5 C6 H6B 110.7 . .
H6A C6 H6B 108.8 . .
C7 C6 C5 105.3(4) . .
C7 C6 H6A 110.7 . .
C7 C6 H6B 110.7 . .
C6 C7 H7A 110.1 . .
C6 C7 H7B 110.1 . .
C6 C7 C8 107.9(4) . .
H7A C7 H7B 108.4 . .
C8 C7 H7A 110.1 . .
C8 C7 H7B 110.1 . .
C7 C8 H8A 111.0 . .
C7 C8 H8B 111.0 . .
H8A C8 H8B 109.0 . .
N5 C8 C7 104.0(4) . .
N5 C8 H8A 111.0 . .
N5 C8 H8B 111.0 . .
H9A C9 H9B 107.9 . .
C10 C9 H9A 109.2 . .
C10 C9 H9B 109.2 . .
N5 C9 H9A 109.2 . .
N5 C9 H9B 109.2 . .
N5 C9 C10 112.2(4) . .
C9 C10 H10A 109.6 . .
C9 C10 H10B 109.6 . .
H10A C10 H10B 108.1 . .
O4 C10 C9 110.2(4) . .
O4 C10 H10A 109.6 . .
O4 C10 H10B 109.6 . .
C1 N1 Dy1 180.0 . .
C5 N5 C8 112.8(4) . .
C5 N5 C9 124.0(4) . .
C9 N5 C8 123.1(4) . .
C5 O1 Dy1 152.7(3) . .
Dy1 O2 H2A 127(3) . .
Dy1 O2 H2B 120(3) . .
H2A O2 H2B 107(3) . .
Dy1 O3 H3A 126(3) . .
Dy1 O3 H3B 122(4) . .
H3A O3 H3B 108(3) . .
C10 O4 H4 110(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 N1 2.471(5) .
Dy1 O1 2.256(3) .
Dy1 O1 2.256(3) 2_556
Dy1 O2 2.306(3) 2_556
Dy1 O2 2.306(3) .
Dy1 O3 2.346(3) 2_556
Dy1 O3 2.346(3) .
Co1 C1 1.892(6) .
Co1 C2 1.900(4) .
Co1 C2 1.900(4) 2_556
Co1 C3 1.900(4) 2_556
Co1 C3 1.900(4) .
Co1 C4 1.884(5) .
C1 N1 1.150(7) .
C2 N2 1.147(5) .
C3 N3 1.146(5) .
C4 N4 1.139(7) .
C5 C6 1.488(6) .
C5 N5 1.312(5) .
C5 O1 1.255(5) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C7 1.462(8) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 C8 1.484(8) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 N5 1.465(6) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C9 C10 1.501(7) .
C9 N5 1.445(6) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C10 O4 1.418(6) .
O2 H2A 0.941(19) .
O2 H2B 0.944(19) .
O3 H3A 0.941(19) .
O3 H3B 0.946(19) .
O4 H4 0.94(2) .
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 H2A N2 0.941(19) 1.86(2) 2.795(5) 171(5) 6_576
O2 H2B N3 0.944(19) 1.78(2) 2.726(5) 176(5) 4_446
O3 H3A O4 0.941(19) 1.74(2) 2.678(5) 173(6) 7_466
O3 H3B N4 0.946(19) 1.89(2) 2.829(6) 169(6) 1_545
O4 H4 N2 0.94(2) 2.19(3) 3.075(5) 158(6) 5_576
