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_7239837
_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         'C33 H35 Dy2 N7 O14'
_chemical_formula_sum            'C33 H35 Dy2 N7 O14'
_chemical_formula_weight         1078.68
_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
_audit_creation_date             2019-06-21
_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                 96.828(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2742(3)
_cell_length_b                   15.1845(5)
_cell_length_c                   21.7739(8)
_cell_measurement_reflns_used    4535
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.3650
_cell_measurement_theta_min      2.8970
_cell_volume                     3701.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 1.000
_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    -92.00 -59.00   1.00    8.00    --  -33.50 136.00 -32.00   33
  2  \w    -94.00 -58.00   1.00    8.00    --  -33.50 -57.00 120.00   36
  3  \w      9.00  34.00   1.00    8.00    --  -33.50  57.00 -90.00   25
  4  \w    -52.00 -26.00   1.00    8.00    --  -33.50 136.00 -32.00   26
  5  \w    -30.00  55.00   1.00    8.00    --   36.37 -77.00   0.00   85
  6  \w     18.00  90.00   1.00    8.00    --   36.37-125.00 150.00   72
  7  \w    -28.00  56.00   1.00    8.00    --   36.37 -37.00-180.00   84
  8  \w    -29.00  52.00   1.00    8.00    --   36.37 -57.00 120.00   81
  9  \w    -31.00  48.00   1.00    8.00    --   36.37 -57.00 -90.00   79
 10  \w     43.00  89.00   1.00    8.00    --   36.37-125.00 -90.00   46
 11  \w    -26.00  56.00   1.00    8.00    --   36.37 -37.00   0.00   82
 12  \w     49.00  75.00   1.00    8.00    --   36.37-125.00-180.00   26
 13  \w     45.00 108.00   1.00   35.00    --  108.00 -94.00-120.00   63
 14  \w     78.00 106.00   1.00   35.00    --  108.00 -94.00-180.00   28
 15  \w     56.00 108.00   1.00   35.00    --  108.00 -94.00  90.00   52
 16  \w     41.00 124.00   1.00   35.00    --  108.00 -45.00-150.00   83
 17  \w     63.00 112.00   1.00   35.00    --  108.00 -45.00   0.00   49
 18  \w     56.00 123.00   1.00   35.00    --  108.00 -45.00  60.00   67
 19  \w    123.00 175.00   1.00   35.00    --  108.00 111.00-180.00   52
 20  \w     42.00 117.00   1.00   35.00    --  108.00 -30.00 150.00   75
 21  \w     67.00 106.00   1.00   35.00    --  108.00 -77.00 -90.00   39
 22  \w     67.00 106.00   1.00   35.00    --  108.00 -94.00 150.00   39
 23  \w     85.00 113.00   1.00   35.00    --  108.00 -45.00  90.00   28
 24  \w     40.00 104.00   1.00   35.00    --  108.00 -45.00 -60.00   64
 25  \w    123.00 173.00   1.00   35.00    --  108.00  30.00-120.00   50
 26  \w     68.00 114.00   1.00   35.00    --  108.00-111.00  30.00   46
 27  \w     39.00 176.00   1.00   35.00    --  108.00   0.00-150.00  137
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0581396000
_diffrn_orient_matrix_UB_12      0.0781524000
_diffrn_orient_matrix_UB_13      0.0302479000
_diffrn_orient_matrix_UB_21      -0.0456585000
_diffrn_orient_matrix_UB_22      0.0364854000
_diffrn_orient_matrix_UB_23      -0.0645237000
_diffrn_orient_matrix_UB_31      -0.1160350000
_diffrn_orient_matrix_UB_32      -0.0534696000
_diffrn_orient_matrix_UB_33      0.0001847000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24201
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.243
_diffrn_reflns_theta_min         3.557
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.936
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.781
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         6644
_refine_ls_number_restraints     1897
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0678P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5017
_reflns_number_total             6644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce02000d2.cif
_cod_data_source_block           exp_9960
_cod_database_code               7239837
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.272
_shelx_estimated_absorpt_t_min   0.242
_reflns_odcompleteness_completeness 99.96
_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. Restrained distances
 O15-C33
 1.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
 C24(H24A,H24B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C20(H20),
 C21(H21), C22(H22), C23(H23), C26(H26), C28(H28), C31(H31)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              27136
_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 2.367
_oxdiff_exptl_absorpt_empirical_full_min 0.584