Dysprosium Complexes Bearing Unsupported DyIII–GeII/SnII Metal–Metal Bonds as Single-Ion Magnets
Chen, Shiming; Xiong, Jin; Zhang, Yi-Quan; Ma, Fang; Sun, Hao-Ling; Wang, Bingwu; Gao, Song; Chemical Communications  (2019) –; doi:10.1039/C9CC00388F

data_7123680
_publ_section_title
;
 Dysprosium Complexes Bearing Unsupported DyIII--GeII/SnII Metal--Metal
 Bonds as Single-Ion Magnets
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00388F
_journal_year                    2019
_chemical_formula_moiety         'C22 H23 Dy O Sn, 2(C10 H15)'
_chemical_formula_sum            'C42 H53 Dy O Sn'
_chemical_formula_weight         855.03
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2018-08-31 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 132.134(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6271(4)
_cell_length_b                   17.0698(2)
_cell_length_c                   23.3096(8)
_cell_measurement_reflns_used    25991
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.1530
_cell_measurement_theta_min      3.4940
_cell_volume                     3725.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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    -22.00  14.00   0.50    1.00    --  -15.70 -82.00 -60.00   72
  2  \w    -57.00  -9.00   0.50    1.00    --  -15.70  77.00 -60.00   96
  3  \w     -2.00  58.00   0.50    1.00    --  -15.70  19.00 -30.00  120
  4  \w    -40.00 -14.00   0.50    1.00    --  -15.70  77.00   0.00   52
  5  \w    -52.00 -21.00   0.50    1.00    --  -15.70  77.00-180.00   62
  6  \w    -48.00  -9.00   0.50    1.00    --  -15.70  77.00-120.00   78
  7  \w    -70.00  50.00   0.50    1.00    --   15.80 -57.00-180.00  240
  8  \w    -34.00  52.00   0.50    1.00    --   15.80 -82.00  90.00  172
  9  \w    -30.00  33.00   0.50    1.00    --   15.80 -82.00  60.00  126
 10  \w     24.00  74.00   0.50    1.00    --   15.80  57.00 -60.00  100
 11  \w     58.00  84.00   0.50    1.00    --   15.80  38.00-120.00   52
 12  \w    -38.00  38.00   0.50    1.00    --   15.80  38.00-120.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0469765000
_diffrn_orient_matrix_UB_12      -0.0212467000
_diffrn_orient_matrix_UB_13      -0.0010665000
_diffrn_orient_matrix_UB_21      0.0501591000
_diffrn_orient_matrix_UB_22      -0.0027090000
_diffrn_orient_matrix_UB_23      0.0409032000
_diffrn_orient_matrix_UB_31      -0.0318969000
_diffrn_orient_matrix_UB_32      -0.0356244000
_diffrn_orient_matrix_UB_33      -0.0025440000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46799
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_min         3.483
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.690
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7326
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+4.2670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6687
_reflns_number_total             7326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00388f2.cif
_cod_data_source_block           1_reducted
_cod_original_cell_volume        3725.8(3)
_cod_database_code               7123680
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C48 H60 Sn1 Dy1'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
 C1-C2 \\sim C2-C3
 with sigma of 0.02
 C2-C3 \\sim C3-C4
 with sigma of 0.02
 C3-C4 \\sim C4-C5
 with sigma of 0.02
 C4-C5 \\sim C5-C1
 with sigma of 0.02
 C5-C1 \\sim C1-C2
 with sigma of 0.02
 C6-C7 \\sim C7-C8
 with sigma of 0.02
 C7-C8 \\sim C8-C9
 with sigma of 0.02
 C8-C9 \\sim C9-C10
 with sigma of 0.02
 C9-C10 \\sim C10-C6
 with sigma of 0.02
 C10-C6 \\sim C6-C7
 with sigma of 0.02
 C21-C22 \\sim C22-C23
 with sigma of 0.02
 C22-C23 \\sim C23-C24
 with sigma of 0.02
 C23-C24 \\sim C24-C25
 with sigma of 0.02
 C24-C25 \\sim C25-C26
 with sigma of 0.02
 C25-C26 \\sim C26-C21
 with sigma of 0.02
 C26-C21 \\sim C21-C22
 with sigma of 0.02
 C27-C28 \\sim C28-C29
 with sigma of 0.02
 C28-C29 \\sim C29-C30
 with sigma of 0.02
 C29-C30 \\sim C30-C31
 with sigma of 0.02
 C30-C31 \\sim C31-C32
 with sigma of 0.02
 C31-C32 \\sim C32-C27
 with sigma of 0.02
 C32-C27 \\sim C27-C28
 with sigma of 0.02
 C33-C34 \\sim C34-C35
 with sigma of 0.02
 C34-C35 \\sim C35-C36
 with sigma of 0.02
 C35-C36 \\sim C36-C37
 with sigma of 0.02
 C36-C37 \\sim C37-C38
 with sigma of 0.02
 C37-C38 \\sim C38-C33
 with sigma of 0.02
 C38-C33 \\sim C33-C34
 with sigma of 0.02
3. Restrained planarity
 C13, C3, C4, C5, C1, C2, C12, C11, C15, C14
 with sigma of 0.1
 C10, C9, C8, C7, C6, C16, C20, C19, C18, C17
 with sigma of 0.1
 C21, C26, C25, C24, C23, C22
 with sigma of 0.1
 C33, C34, C35, C36, C37, C38
 with sigma of 0.1
 C27, C28, C29, C30, C31, C32
 with sigma of 0.1
4. Rigid bond restraints
 C9, C10, C6, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C4, C5, C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C28, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, C26, C25, C24, C23, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C34, C33, C38, C37, C36, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C1 \\sim C5 \\sim C4 \\sim C3 \\sim C2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C6 \\sim C10 \\sim C9 \\sim C8 \\sim C7: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C21: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C33 \\sim C38 \\sim C37 \\sim C36 \\sim C35 \\sim C34: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.015 and sigma for
terminal atoms of 0.015
Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6.a Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
6.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C26(H26), C22(H22), C30(H30), C36(H36), C25(H25), C34(H34),
 C32(H32), C24(H24), C29(H29), C38(H38), C31(H31), C37(H37), C28(H28), C23(H23)
6.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C12(H12A,H12B,
 H12C), C19(H19A,H19B,H19C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              58801
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.808