The Rare CH3O-/CH3CH2O–Bridged Nine-Coordinated Binuclear DyIII Single-Molecule Magnets (SMMs) Significantly Regulate and Enhance the Effective Energy Barriers
Zhang, Sheng; shen, nan; liu, sha; Ma, Rong; Zhang, Yi-Quan; Hu, Dengwei; Liu, Xiangyu; Zhang, Jiangwei; Yang, Desuo; CrystEngComm  (2020) –; doi:10.1039/C9CE02000D

data_7239838
_publ_section_title
;
 The Rare CH3O-/CH3CH2O--Bridged Nine-Coordinated Binuclear DyIII
 Single-Molecule Magnets (SMMs) Significantly Regulate and Enhance the
 Effective Energy Barriers
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE02000D
_journal_year                    2020
_chemical_formula_moiety         'C34 H37 Dy2 N7 O14'
_chemical_formula_sum            'C34 H37 Dy2 N7 O14'
_chemical_formula_weight         1092.70
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-24 deposited with the CCDC.	2020-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.484(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3326(4)
_cell_length_b                   15.5518(6)
_cell_length_c                   21.8107(8)
_cell_measurement_reflns_used    7201
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      74.6070
_cell_measurement_theta_min      3.4500
_cell_volume                     3811.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -108.00 -71.00   1.00    0.50    --  -48.45-125.00  48.00   37
  2  \w   -115.00 -57.00   1.00    0.50    --  -48.45-145.00-118.00   58
  3  \w    -84.00 -36.00   1.00    0.50    --  -48.45 125.00 125.00   48
  4  \w     48.00  95.00   1.00    0.50    --   48.45-125.00  48.00   47
  5  \w     51.00  76.00   1.00    0.50    --   48.45-145.00-118.00   25
  6  \w   -158.00 -71.00   1.00    5.00    --  -86.25-125.00  48.00   87
  7  \w   -132.00-107.00   1.00    5.00    --  -86.25-145.00-118.00   25
  8  \w    131.00 175.00   1.00    5.00    --  106.49 145.00 -67.00   44
  9  \w     91.00 117.00   1.00    5.00    --  106.49-125.00  48.00   26
 10  \w     62.00  87.00   1.00    5.00    --  106.49-145.00-118.00   25
 11  \w    114.00 178.00   1.00    5.00    --  106.49 125.00 125.00   64
 12  \w   -120.00 -27.00   1.00    0.50    --  -48.45 -77.00-120.00   93
 13  \w    136.00 178.00   1.00    5.00    --  106.49  19.00-120.00   42
 14  \w     34.00 109.00   1.00    5.00    --  106.49 -99.00  60.00   75
 15  \w     94.00 123.00   1.00    5.00    --  106.49  19.00-120.00   29
 16  \w     93.00 177.00   1.00    5.00    --  106.49  38.00 120.00   84
 17  \w     34.00 117.00   1.00    5.00    --  106.49 -38.00-180.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0931729000
_diffrn_orient_matrix_UB_12      -0.0050057000
_diffrn_orient_matrix_UB_13      0.0579713000
_diffrn_orient_matrix_UB_21      0.0019746000
_diffrn_orient_matrix_UB_22      -0.0987380000
_diffrn_orient_matrix_UB_23      -0.0056180000
_diffrn_orient_matrix_UB_31      0.1005221000
_diffrn_orient_matrix_UB_32      0.0065010000
_diffrn_orient_matrix_UB_33      -0.0410213000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21835
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.501
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    21.405
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.073
_refine_diff_density_min         -1.828
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         6638
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0622
_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/[\s^2^(Fo^2^)+(0.1167P)^2^+6.3659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5238
_reflns_number_total             6638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce02000d2.cif
_cod_data_source_block           zhangsheng0516
_cod_database_code               7239838
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         DyCNO
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.481
_reflns_odcompleteness_completeness 97.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Uiso/Uaniso restraints and constraints
O4 \\sim C33 \\sim C34: within 2A with sigma of 0.004 and sigma for terminal
atoms of 0.008
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C28(H28A,H28B), C33(H33A,H33B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C29(H29), C30(H30)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              90942
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.833
_oxdiff_exptl_absorpt_empirical_full_min 0.533