#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:44:52 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224320 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/87/7048759.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_7048759
loop_
_publ_author_name
'Vignesh, Kuduva R.'
'Alexandropoulos, Dimitris I.'
'Dolinar, Brian S.'
'Dunbar, Kim R.'
_publ_section_title
;
 Hard versus soft: zero-field dinuclear Dy(iii) oxygen bridged SMM and
 theoretical predictions of the sulfur and selenium analogues.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2872
_journal_page_last               2876
_journal_paper_doi               10.1039/c9dt00324j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C46 H58 Dy2 N2 O14, 2(N O3), 4(C2 H3 N)'
_chemical_formula_sum            'C54 H70 Dy2 N8 O20'
_chemical_formula_weight         1476.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-21 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                63.5140(10)
_cell_angle_beta                 85.6460(10)
_cell_angle_gamma                80.8900(10)
_cell_formula_units_Z            1
_cell_length_a                   10.5842(3)
_cell_length_b                   12.0661(4)
_cell_length_c                   12.7702(4)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      25.71
_cell_measurement_theta_min      2.56
_cell_volume                     1441.27(8)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON area detector'
_diffrn_measurement_method       '0.5\ ω and 0.5\ φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24328
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.719
_diffrn_reflns_theta_min         2.528
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.655
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0858 before and 0.0364 after correction.
The Ratio of minimum to maximum transmission is 0.8564.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5474
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0189P)²+0.9572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0381
_refine_ls_wR_factor_ref         0.0385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5271
_reflns_number_total             5474
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00324j2.cif
_cod_data_source_block           vig42_mecn_0m_a
_cod_depositor_comments
'Adding full bibliography for 7048759--7048760.cif.'
_cod_database_code               7048759
_shelx_shelxl_version_number     2014/7
_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   0.619
_shelx_estimated_absorpt_t_min   0.416
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4
 0.87 with sigma of 0.01
 O2-H2
 0.87 with sigma of 0.01
 O3-H3
 0.87 with sigma of 0.01
 C8-H4
 1.919943 with sigma of 0.02
 Dy1-H4
 3.055482 with sigma of 0.02
 C4-H2
 1.916833 with sigma of 0.02
 Dy1-H2
 3.102054 with sigma of 0.02
 C6-H3
 1.920327 with sigma of 0.02
 Dy1-H3
 3.079967 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23)
3.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
3.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Dy1 Dy 0.35457(2) 0.59664(2) 0.41293(2) 0.00757(4) Uani 1 1 d D
O1 O 0.47762(13) 0.55538(12) 0.56733(12) 0.0095(3) Uani 1 1 d .
O2 O 0.36638(13) 0.80053(13) 0.40702(12) 0.0118(3) Uani 1 1 d D
H2 H 0.4419(13) 0.8276(18) 0.3873(18) 0.018 Uiso 1 1 d DR
O3 O 0.13734(14) 0.69681(14) 0.35954(13) 0.0156(3) Uani 1 1 d D
H3 H 0.1040(18) 0.7269(19) 0.2893(12) 0.023 Uiso 1 1 d DR
O4 O 0.24228(14) 0.42213(13) 0.53122(12) 0.0131(3) Uani 1 1 d D
H4 H 0.2764(17) 0.3435(9) 0.5571(17) 0.020 Uiso 1 1 d DR
O5 O 0.35929(14) 0.75119(14) 0.76989(13) 0.0174(3) Uani 1 1 d .
H5 H 0.3655 0.8276 0.7317 0.026 Uiso 1 1 calc GR
O6 O 0.45629(13) 0.71417(13) 0.24387(12) 0.0131(3) Uani 1 1 d .
O7 O 0.28844(13) 0.55005(13) 0.27174(12) 0.0116(3) Uani 1 1 d .
O8 O 0.38019(14) 0.19486(13) 0.59897(14) 0.0182(3) Uani 1 1 d .
O9 O 0.22853(16) 0.08070(18) 0.6709(2) 0.0442(5) Uani 1 1 d .
O10 O 0.41758(15) -0.00327(14) 0.64604(15) 0.0242(4) Uani 1 1 d .
N1 N 0.22090(15) 0.63356(15) 0.57917(14) 0.0098(3) Uani 1 1 d .
N2 N 0.34016(17) 0.08892(17) 0.63941(16) 0.0169(4) Uani 1 1 d .
N3 N 0.0946(2) 0.0973(2) 0.3398(2) 0.0335(5) Uani 1 1 d .
C1 C 0.44264(18) 0.60804(18) 0.64617(17) 0.0098(4) Uani 1 1 d .
H1A H 0.5097 0.6569 0.6456 0.012 Uiso 1 1 calc R
H1B H 0.4375 0.5400 0.7263 0.012 Uiso 1 1 calc R
C2 C 0.31206(19) 0.69451(18) 0.61477(17) 0.0111(4) Uani 1 1 d .
C3 C 0.26252(19) 0.72030(19) 0.71978(18) 0.0135(4) Uani 1 1 d .
H3A H 0.1910 0.7901 0.6937 0.016 Uiso 1 1 calc R
H3B H 0.2289 0.6453 0.7804 0.016 Uiso 1 1 calc R
C4 C 0.3292(2) 0.81865(19) 0.50986(18) 0.0131(4) Uani 1 1 d D
H4A H 0.2480 0.8766 0.4948 0.016 Uiso 1 1 calc R
H4B H 0.3956 0.8570 0.5277 0.016 Uiso 1 1 calc R
C5 C 0.09305(19) 0.7118(2) 0.53864(19) 0.0161(4) Uani 1 1 d .
H5A H 0.0775 0.7723 0.5726 0.019 Uiso 1 1 calc R
H5B H 0.0254 0.6569 0.5684 0.019 Uiso 1 1 calc R
C6 C 0.0831(2) 0.7831(2) 0.40638(18) 0.0152(4) Uani 1 1 d D
H6A H -0.0075 0.8140 0.3828 0.018 Uiso 1 1 calc R
H6B H 0.1309 0.8555 0.3769 0.018 Uiso 1 1 calc R
C7 C 0.2022(2) 0.50687(19) 0.67163(18) 0.0139(4) Uani 1 1 d .
H7A H 0.1394 0.5154 0.7300 0.017 Uiso 1 1 calc R
H7B H 0.2842 0.4635 0.7123 0.017 Uiso 1 1 calc R
C8 C 0.1550(2) 0.4290(2) 0.62110(18) 0.0142(4) Uani 1 1 d D
H8A H 0.1490 0.3438 0.6837 0.017 Uiso 1 1 calc R
H8B H 0.0687 0.4672 0.5876 0.017 Uiso 1 1 calc R
C9 C 0.64880(19) 0.84231(19) 0.10760(19) 0.0143(4) Uani 1 1 d .
H9 H 0.6559 0.8068 0.1903 0.017 Uiso 1 1 calc R
C10 C 0.7373(2) 0.9176(2) 0.0368(2) 0.0180(5) Uani 1 1 d .
H10 H 0.8060 0.9315 0.0712 0.022 Uiso 1 1 calc R
C11 C 0.7257(2) 0.9724(2) -0.0839(2) 0.0201(5) Uani 1 1 d .
H11 H 0.7860 1.0243 -0.1322 0.024 Uiso 1 1 calc R
C12 C 0.6261(2) 0.9515(2) -0.13390(19) 0.0179(4) Uani 1 1 d .
H12 H 0.6174 0.9899 -0.2166 0.022 Uiso 1 1 calc R
C13 C 0.5388(2) 0.87461(19) -0.06367(18) 0.0140(4) Uani 1 1 d .
H13 H 0.4711 0.8600 -0.0987 0.017 Uiso 1 1 calc R
C14 C 0.54933(19) 0.81853(18) 0.05783(18) 0.0110(4) Uani 1 1 d .
C15 C 0.46086(18) 0.73126(18) 0.13774(17) 0.0105(4) Uani 1 1 d .
C16 C 0.39360(19) 0.66905(18) 0.09464(17) 0.0117(4) Uani 1 1 d .
H16 H 0.4023 0.6881 0.0140 0.014 Uiso 1 1 calc R
C17 C 0.31412(18) 0.58014(18) 0.16434(17) 0.0106(4) Uani 1 1 d .
C18 C 0.25393(19) 0.51205(18) 0.11255(17) 0.0108(4) Uani 1 1 d .
C19 C 0.3105(2) 0.48848(19) 0.02098(18) 0.0132(4) Uani 1 1 d .
H19 H 0.3862 0.5225 -0.0154 0.016 Uiso 1 1 calc R
C20 C 0.2566(2) 0.41536(19) -0.01723(18) 0.0152(4) Uani 1 1 d .
H20 H 0.2972 0.3972 -0.0779 0.018 Uiso 1 1 calc R
C21 C 0.1444(2) 0.3688(2) 0.0325(2) 0.0179(4) Uani 1 1 d .
H21 H 0.1080 0.3188 0.0060 0.021 Uiso 1 1 calc R
C22 C 0.0849(2) 0.3951(2) 0.1209(2) 0.0183(5) Uani 1 1 d .
H22 H 0.0063 0.3653 0.1533 0.022 Uiso 1 1 calc R
C23 C 0.1402(2) 0.46475(19) 0.16197(19) 0.0150(4) Uani 1 1 d .
H23 H 0.1005 0.4805 0.2242 0.018 Uiso 1 1 calc R
C24 C 0.1868(2) 0.1348(2) 0.3408(2) 0.0237(5) Uani 1 1 d .
C25 C 0.3043(2) 0.1836(2) 0.3415(2) 0.0292(6) Uani 1 1 d .
H25A H 0.3371 0.2242 0.2613 0.044 Uiso 1 1 calc GR
H25B H 0.3684 0.1146 0.3899 0.044 Uiso 1 1 calc GR
H25C H 0.2864 0.2446 0.3736 0.044 Uiso 1 1 calc GR
N4 N 0.06010(18) 0.8039(2) 0.12207(18) 0.0242(4) Uani 1 1 d .
C26 C 0.0767(2) 0.8256(2) 0.0266(2) 0.0185(5) Uani 1 1 d .
C27 C 0.0987(3) 0.8519(3) -0.0960(2) 0.0289(6) Uani 1 1 d .
H27A H 0.1318 0.9320 -0.1378 0.043 Uiso 1 1 calc GR
H27B H 0.0180 0.8561 -0.1313 0.043 Uiso 1 1 calc GR
H27C H 0.1612 0.7852 -0.1010 0.043 Uiso 1 1 calc GR
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'
Dy Dy -0.1892 4.4098 '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'
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 Dy1 34.79(3) . 2_666
O1 Dy1 Dy1 34.54(3) 2_666 2_666
O1 Dy1 O1 69.32(5) . 2_666
O1 Dy1 O2 74.57(5) . .
O1 Dy1 O2 126.47(5) 2_666 .
O1 Dy1 O3 132.60(5) . .
O1 Dy1 O3 152.91(5) 2_666 .
O1 Dy1 O4 83.80(5) 2_666 .
O1 Dy1 O4 90.81(5) . .
O1 Dy1 O6 84.42(5) 2_666 .
O1 Dy1 O6 108.89(5) . .
O1 Dy1 O7 152.61(5) . .
O1 Dy1 O7 84.15(5) 2_666 .
O1 Dy1 N1 127.97(5) 2_666 .
O1 Dy1 N1 67.86(5) . .
O2 Dy1 Dy1 101.61(3) . 2_666
O2 Dy1 N1 66.56(5) . .
O3 Dy1 Dy1 162.38(4) . 2_666
O3 Dy1 O2 79.45(5) . .
O3 Dy1 N1 65.57(5) . .
O4 Dy1 Dy1 86.72(4) . 2_666
O4 Dy1 O2 135.29(5) . .
O4 Dy1 O3 80.62(5) . .
O4 Dy1 N1 68.78(5) . .
O6 Dy1 Dy1 97.87(4) . 2_666
O6 Dy1 O2 71.37(5) . .
O6 Dy1 O3 99.10(5) . .
O6 Dy1 O4 151.64(5) . .
O6 Dy1 O7 73.90(5) . .
O6 Dy1 N1 137.07(5) . .
O7 Dy1 Dy1 118.42(4) . 2_666
O7 Dy1 O2 129.63(5) . .
O7 Dy1 O3 71.29(5) . .
O7 Dy1 O4 79.30(5) . .
O7 Dy1 N1 129.30(5) . .
N1 Dy1 Dy1 98.44(4) . 2_666
Dy1 O1 Dy1 110.68(5) . 2_666
C1 O1 Dy1 126.28(11) . 2_666
C1 O1 Dy1 122.63(11) . .
C4 O2 Dy1 118.57(11) . .
C6 O3 Dy1 117.55(12) . .
C8 O4 Dy1 119.64(11) . .
C15 O6 Dy1 137.28(13) . .
C17 O7 Dy1 136.01(13) . .
C2 N1 Dy1 100.55(11) . .
C5 N1 Dy1 113.27(12) . .
C5 N1 C2 114.07(15) . .
C7 N1 Dy1 105.76(11) . .
C7 N1 C2 113.04(15) . .
C7 N1 C5 109.63(15) . .
O9 N2 O8 119.51(18) . .
O9 N2 O10 122.28(19) . .
O10 N2 O8 118.21(17) . .
O1 C1 C2 112.26(15) . .
N1 C2 C1 108.62(15) . .
N1 C2 C3 112.83(16) . .
N1 C2 C4 107.47(16) . .
C3 C2 C1 109.49(16) . .
C4 C2 C1 109.58(16) . .
C4 C2 C3 108.79(16) . .
O5 C3 C2 112.65(16) . .
O2 C4 C2 110.91(15) . .
N1 C5 C6 113.14(16) . .
O3 C6 C5 106.89(16) . .
N1 C7 C8 111.72(17) . .
O4 C8 C7 109.56(16) . .
C10 C9 C14 120.3(2) . .
C11 C10 C9 120.2(2) . .
C12 C11 C10 119.9(2) . .
C11 C12 C13 120.2(2) . .
C12 C13 C14 120.6(2) . .
C9 C14 C15 118.23(18) . .
C13 C14 C9 118.77(19) . .
C13 C14 C15 122.98(18) . .
O6 C15 C14 116.61(17) . .
O6 C15 C16 124.04(18) . .
C16 C15 C14 119.27(18) . .
C15 C16 C17 123.49(19) . .
O7 C17 C16 125.12(18) . .
O7 C17 C18 115.29(17) . .
C16 C17 C18 119.58(18) . .
C19 C18 C17 122.36(18) . .
C19 C18 C23 118.96(19) . .
C23 C18 C17 118.59(18) . .
C20 C19 C18 120.15(19) . .
C21 C20 C19 120.4(2) . .
C20 C21 C22 120.01(19) . .
C23 C22 C21 119.9(2) . .
C22 C23 C18 120.5(2) . .
N3 C24 C25 179.7(3) . .
N4 C26 C27 179.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 Dy1 3.7418(2) 2_666
Dy1 O1 2.2674(13) .
Dy1 O1 2.2818(13) 2_666
Dy1 O2 2.4503(13) .
Dy1 O3 2.4157(14) .
Dy1 O4 2.4106(14) .
Dy1 O6 2.2871(13) .
Dy1 O7 2.2971(13) .
Dy1 N1 2.6258(16) .
O1 Dy1 2.2818(13) 2_666
O1 C1 1.412(2) .
O2 C4 1.441(2) .
O3 C6 1.444(2) .
O4 C8 1.441(2) .
O5 C3 1.425(2) .
O6 C15 1.275(2) .
O7 C17 1.272(2) .
O8 N2 1.277(2) .
O9 N2 1.223(2) .
O10 N2 1.246(2) .
N1 C2 1.506(2) .
N1 C5 1.502(3) .
N1 C7 1.490(3) .
N3 C24 1.142(3) .
C1 C2 1.554(3) .
C2 C3 1.544(3) .
C2 C4 1.527(3) .
C5 C6 1.519(3) .
C7 C8 1.512(3) .
C9 C10 1.389(3) .
C9 C14 1.398(3) .
C10 C11 1.386(3) .
C11 C12 1.383(3) .
C12 C13 1.386(3) .
C13 C14 1.394(3) .
C14 C15 1.495(3) .
C15 C16 1.404(3) .
C16 C17 1.404(3) .
C17 C18 1.494(3) .
C18 C19 1.394(3) .
C18 C23 1.398(3) .
C19 C20 1.388(3) .
C20 C21 1.381(3) .
C21 C22 1.386(3) .
C22 C23 1.385(3) .
C24 C25 1.460(3) .
N4 C26 1.133(3) .
C26 C27 1.459(3) .
