#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:58:48 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224380 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/92/7049253.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_7049253
loop_
_publ_author_name
'Yang, Zhao-Fu'
'Tian, Yong-Mei'
'Zhang, Wan-Ying'
'Chen, Peng'
'Li, Hong-Feng'
'Zhang, Yi-Quan'
'Sun, Wen-Bin'
_publ_section_title
;
 High local coordination symmetry around the spin center and the alignment
 between magnetic and symmetric axes together play a crucial role in
 single-molecule magnet performance.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4931
_journal_page_last               4940
_journal_paper_doi               10.1039/c9dt00058e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C58 H54 Dy2 F6 N6 O12 S2'
_chemical_formula_weight         1530.19
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-01-30 deposited with the CCDC.    2019-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                99.306(7)
_cell_angle_beta                 96.452(7)
_cell_angle_gamma                105.332(7)
_cell_formula_units_Z            1
_cell_length_a                   11.1327(9)
_cell_length_b                   11.7050(11)
_cell_length_c                   12.3830(10)
_cell_measurement_reflns_used    5627
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      1.00000
_cell_measurement_theta_min      0.73398
_cell_volume                     1515.2(2)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'CrysAlis PRO (Agilent, 2011)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_unetI/netI     0.0963
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17350
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.022
_diffrn_source                   '\w scans'
_exptl_absorpt_coefficient_mu    2.599
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,

Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)

(compiled Jan 23 2012,18:06:46)

Empirical absorption correction using 
spherical harmonics,
 
implemented in SCALE3 ABSPACK 
scaling algorithm.

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       block
_exptl_crystal_F_000             758
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.508
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         6919
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0536
_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)+(0.0590P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5158
_reflns_number_total             6919
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00058e2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7049253--7049258.cif.'
_cod_database_code               7049253
_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_min   0.763
_shelx_estimated_absorpt_t_max   0.781
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
_atom_site_refinement_flags_adp
Dy01 Dy 0.50854(3) 0.62541(2) 0.41407(2) 0.03685(12) Uani 1 1 d D .
S1 S 0.2963(2) 0.2965(3) 0.0780(2) 0.0906(8) Uani 1 1 d . .
O5 O 0.6230(4) 0.5536(4) 0.5512(3) 0.0375(10) Uani 1 1 d . .
O4 O 0.6915(4) 0.6493(4) 0.3396(4) 0.0543(12) Uani 1 1 d . .
O3 O 0.4684(4) 0.4821(4) 0.2495(4) 0.0523(12) Uani 1 1 d . .
O1 O 0.4021(4) 0.6989(4) 0.5557(4) 0.0531(12) Uani 1 1 d D .
H1 H 0.432(4) 0.771(3) 0.594(5) 0.080 Uiso 1 1 d D U
O2 O 0.3572(5) 0.6651(4) 0.2892(4) 0.0525(12) Uani 1 1 d . .
N008 N 0.6845(5) 0.7869(4) 0.5399(4) 0.0374(12) Uani 1 1 d . .
N009 N 0.5330(5) 0.8438(5) 0.3955(4) 0.0410(12) Uani 1 1 d . .
N00A N 0.4457(5) 0.8709(5) 0.3235(5) 0.0463(14) Uani 1 1 d . .
O6 O 0.4742(7) 0.8974(5) 0.7144(5) 0.0756(17) Uani 1 1 d . .
H6 H 0.5106 0.9652 0.7059 0.113 Uiso 1 1 calc R U
C16 C 0.7335(6) 0.6245(6) 0.6097(5) 0.0383(14) Uani 1 1 d . .
C19 C 0.7280(6) 0.5928(6) 0.2587(6) 0.0469(17) Uani 1 1 d . .
C7 C 0.3590(6) 0.7702(6) 0.2735(6) 0.0433(15) Uani 1 1 d . .
C6 C 0.2597(6) 0.7778(6) 0.1849(6) 0.0447(15) Uani 1 1 d . .
C23 C 0.4902(7) 0.3155(6) -0.0270(5) 0.0418(15) Uani 1 1 d . U
H23A H 0.5706 0.3385 -0.0456 0.050 Uiso 1 1 calc R U
C15 C 0.8164(6) 0.5843(6) 0.6722(6) 0.0443(15) Uani 1 1 d . .
H15 H 0.7957 0.5035 0.6784 0.053 Uiso 1 1 calc R U
C17 C 0.7687(6) 0.7494(6) 0.6030(5) 0.0387(14) Uani 1 1 d . .
C20 C 0.6570(7) 0.5001(6) 0.1757(6) 0.0499(17) Uani 1 1 d . .
H20 H 0.6958 0.4679 0.1204 0.060 Uiso 1 1 calc R U
F3 F 0.9133(5) 0.7502(5) 0.2690(7) 0.132(3) Uani 1 1 d . .
C21 C 0.5267(7) 0.4524(6) 0.1722(6) 0.0470(16) Uani 1 1 d . .
C8 C 0.6257(7) 0.9311(6) 0.4513(6) 0.0507(17) Uani 1 1 d . .
H8 H 0.6343 1.0105 0.4437 0.061 Uiso 1 1 calc R U
C14 C 0.9324(7) 0.6638(7) 0.7268(6) 0.0533(18) Uani 1 1 d . .
H14 H 0.9869 0.6339 0.7690 0.064 Uiso 1 1 calc R U
C9 C 0.7158(6) 0.9014(6) 0.5260(6) 0.0453(16) Uani 1 1 d . .
C13 C 0.9692(6) 0.7827(6) 0.7211(6) 0.0528(18) Uani 1 1 d . .
H13 H 1.0469 0.8332 0.7587 0.063 Uiso 1 1 calc R U
C12 C 0.8868(6) 0.8269(6) 0.6571(6) 0.0459(16) Uani 1 1 d . .
C22 C 0.4515(7) 0.3608(6) 0.0759(6) 0.0489(17) Uani 1 1 d . .
C5 C 0.2363(7) 0.8872(7) 0.1760(6) 0.0556(18) Uani 1 1 d . .
H5 H 0.2831 0.9574 0.2260 0.067 Uiso 1 1 calc R U
C1 C 0.1908(7) 0.6750(7) 0.1093(6) 0.0576(19) Uani 1 1 d . .
H1A H 0.2053 0.6011 0.1135 0.069 Uiso 1 1 calc R U
C10 C 0.8322(7) 0.9847(6) 0.5774(6) 0.059(2) Uani 1 1 d . .
H10 H 0.8517 1.0641 0.5671 0.070 Uiso 1 1 calc R U
C11 C 0.9159(7) 0.9484(6) 0.6421(7) 0.058(2) Uani 1 1 d . .
H11 H 0.9926 1.0033 0.6768 0.070 Uiso 1 1 calc R U
C26 C 0.2743(7) 0.6478(7) 0.5771(7) 0.063(2) Uani 1 1 d D .
H26A H 0.2745 0.6582 0.6564 0.075 Uiso 1 1 calc R U
H26B H 0.2455 0.5619 0.5455 0.075 Uiso 1 1 calc R U
F1 F 0.9097(6) 0.5842(7) 0.1785(8) 0.159(4) Uani 1 1 d . .
C2 C 0.0998(8) 0.6826(9) 0.0271(7) 0.070(2) Uani 1 1 d . .
H2 H 0.0531 0.6132 -0.0240 0.084 Uiso 1 1 calc R U
C4 C 0.1452(8) 0.8927(8) 0.0944(7) 0.066(2) Uani 1 1 d . .
H4 H 0.1298 0.9663 0.0902 0.080 Uiso 1 1 calc R U
C3 C 0.0774(8) 0.7918(9) 0.0199(7) 0.069(2) Uani 1 1 d . .
H3 H 0.0163 0.7961 -0.0358 0.083 Uiso 1 1 calc R U
C24 C 0.3843(9) 0.2317(8) -0.0921(8) 0.078(2) Uani 1 1 d . U
H24 H 0.3875 0.1913 -0.1624 0.094 Uiso 1 1 calc R U
F2 F 0.9298(6) 0.6100(10) 0.3471(8) 0.173(4) Uani 1 1 d . .
C18 C 0.8710(8) 0.6354(10) 0.2649(9) 0.077(3) Uani 1 1 d . .
C25 C 0.2783(10) 0.2116(8) -0.0495(8) 0.082(3) Uani 1 1 d . .
H25 H 0.2023 0.1567 -0.0861 0.099 Uiso 1 1 calc R U
C28 C 0.4691(10) 0.8997(11) 0.8283(10) 0.101(4) Uani 1 1 d . .
H28A H 0.5093 0.8412 0.8508 0.122 Uiso 1 1 calc R U
H28B H 0.5194 0.9789 0.8694 0.122 Uiso 1 1 calc R U
C27 C 0.1876(9) 0.7083(9) 0.5279(9) 0.091(3) Uani 1 1 d . .
H27A H 0.1949 0.7062 0.4511 0.136 Uiso 1 1 calc R U
H27B H 0.2090 0.7907 0.5666 0.136 Uiso 1 1 calc R U
H27C H 0.1025 0.6672 0.5339 0.136 Uiso 1 1 calc R U
C29 C 0.3496(12) 0.8756(12) 0.8603(12) 0.137(5) Uani 1 1 d . .
H29A H 0.3036 0.9252 0.8302 0.206 Uiso 1 1 calc R U
H29B H 0.3589 0.8932 0.9398 0.206 Uiso 1 1 calc R U
H29C H 0.3043 0.7919 0.8329 0.206 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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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
O4 Dy01 O3 71.57(16) . .
O4 Dy01 O2 108.18(18) . .
O3 Dy01 O2 71.91(17) . .
O4 Dy01 O5 127.77(16) . 2_666
O3 Dy01 O5 74.06(16) . 2_666
O2 Dy01 O5 96.83(15) . 2_666
O4 Dy01 O1 147.46(17) . .
O3 Dy01 O1 140.76(17) . .
O2 Dy01 O1 85.67(18) . .
O5 Dy01 O1 77.27(15) 2_666 .
O4 Dy01 O5 82.78(16) . .
O3 Dy01 O5 106.53(16) . .
O2 Dy01 O5 167.18(15) . .
O5 Dy01 O5 70.76(15) 2_666 .
O1 Dy01 O5 88.32(16) . .
O4 Dy01 N008 69.86(16) . .
O3 Dy01 N008 141.33(17) . .
O2 Dy01 N008 123.52(16) . .
O5 Dy01 N008 130.09(15) 2_666 .
O1 Dy01 N008 77.91(16) . .
O5 Dy01 N008 65.90(15) . .
O4 Dy01 N009 84.54(18) . .
O3 Dy01 N009 116.83(17) . .
O2 Dy01 N009 61.54(16) . .
O5 Dy01 N009 146.88(16) 2_666 .
O1 Dy01 N009 76.39(17) . .
O5 Dy01 N009 127.76(15) . .
N008 Dy01 N009 62.13(16) . .
O4 Dy01 Dy01 107.09(13) . 2_666
O3 Dy01 Dy01 90.54(12) . 2_666
O2 Dy01 Dy01 132.54(12) . 2_666
O5 Dy01 Dy01 35.79(10) 2_666 2_666
O1 Dy01 Dy01 81.26(12) . 2_666
O5 Dy01 Dy01 34.98(9) . 2_666
N008 Dy01 Dy01 97.94(11) . 2_666
N009 Dy01 Dy01 152.59(12) . 2_666
C25 S1 C22 91.3(4) . .
C16 O5 Dy01 128.9(4) . 2_666
C16 O5 Dy01 120.4(4) . .
Dy01 O5 Dy01 109.24(15) 2_666 .
C19 O4 Dy01 136.1(4) . .
C21 O3 Dy01 138.4(5) . .
C26 O1 Dy01 129.3(4) . .
C7 O2 Dy01 124.1(4) . .
C9 N008 C17 119.0(6) . .
C9 N008 Dy01 122.0(4) . .
C17 N008 Dy01 116.6(4) . .
C8 N009 N00A 118.0(5) . .
C8 N009 Dy01 121.8(4) . .
N00A N009 Dy01 120.2(4) . .
C7 N00A N009 109.1(5) . .
O5 C16 C15 124.2(6) . .
O5 C16 C17 117.8(6) . .
C15 C16 C17 118.0(6) . .
O4 C19 C20 128.3(6) . .
O4 C19 C18 112.0(7) . .
C20 C19 C18 119.6(7) . .
O2 C7 N00A 125.1(6) . .
O2 C7 C6 116.8(6) . .
N00A C7 C6 117.9(6) . .
C1 C6 C5 118.9(7) . .
C1 C6 C7 119.7(6) . .
C5 C6 C7 121.4(6) . .
C24 C23 C22 106.8(7) . .
C16 C15 C14 120.3(6) . .
N008 C17 C12 122.7(6) . .
N008 C17 C16 116.7(5) . .
C12 C17 C16 120.5(6) . .
C19 C20 C21 121.2(6) . .
O3 C21 C20 123.7(7) . .
O3 C21 C22 116.8(6) . .
C20 C21 C22 119.5(6) . .
N009 C8 C9 117.3(6) . .
C13 C14 C15 123.1(7) . .
N008 C9 C10 121.7(6) . .
N008 C9 C8 115.5(6) . .
C10 C9 C8 122.8(6) . .
C14 C13 C12 118.1(7) . .
C13 C12 C17 119.9(6) . .
C13 C12 C11 123.4(7) . .
C17 C12 C11 116.6(6) . .
C23 C22 C21 129.0(7) . .
C23 C22 S1 112.3(5) . .
C21 C22 S1 118.7(5) . .
C4 C5 C6 120.7(8) . .
C6 C1 C2 119.6(8) . .
C11 C10 C9 119.5(6) . .
C10 C11 C12 120.3(7) . .
O1 C26 C27 110.2(7) . .
C3 C2 C1 120.8(8) . .
C3 C4 C5 120.5(8) . .
C4 C3 C2 119.6(8) . .
C25 C24 C23 117.0(9) . .
F2 C18 F3 108.2(10) . .
F2 C18 F1 104.5(10) . .
F3 C18 F1 105.2(9) . .
F2 C18 C19 112.7(8) . .
F3 C18 C19 112.7(8) . .
F1 C18 C19 113.0(8) . .
C24 C25 S1 112.5(8) . .
C29 C28 O6 117.3(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy01 O4 2.298(5) .
Dy01 O3 2.337(5) .
Dy01 O2 2.347(5) .
Dy01 O5 2.352(4) 2_666
Dy01 O1 2.395(5) .
Dy01 O5 2.399(4) .
Dy01 N008 2.498(5) .
Dy01 N009 2.549(5) .
Dy01 Dy01 3.8732(6) 2_666
S1 C25 1.685(9) .
S1 C22 1.697(8) .
O5 C16 1.339(7) .
O5 Dy01 2.352(4) 2_666
O4 C19 1.275(8) .
O3 C21 1.269(8) .
O1 C26 1.463(8) .
O2 C7 1.271(7) .
N008 C9 1.337(8) .
N008 C17 1.359(8) .
N009 C8 1.280(8) .
N009 N00A 1.378(7) .
N00A C7 1.316(8) .
O6 C28 1.414(12) .
C16 C15 1.364(9) .
C16 C17 1.429(8) .
C19 C20 1.365(10) .
C19 C18 1.526(11) .
C7 C6 1.498(9) .
C6 C1 1.378(10) .
C6 C5 1.391(9) .
C23 C24 1.386(11) .
C23 C22 1.455(9) .
C15 C14 1.398(9) .
C17 C12 1.406(9) .
C20 C21 1.403(10) .
F3 C18 1.292(11) .
C21 C22 1.470(10) .
C8 C9 1.436(9) .
C14 C13 1.359(10) .
C9 C10 1.408(9) .
C13 C12 1.399(9) .
C12 C11 1.420(9) .
C5 C4 1.371(10) .
C1 C2 1.384(11) .
C10 C11 1.357(10) .
C26 C27 1.473(12) .
F1 C18 1.312(11) .
C2 C3 1.380(11) .
C4 C3 1.356(12) .
C24 C25 1.326(13) .
F2 C18 1.267(12) .
C28 C29 1.402(14) .
