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_7123679
_publ_section_title
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 Dysprosium Complexes Bearing Unsupported DyIII--GeII/SnII Metal--Metal
 Bonds as Single-Ion Magnets
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00388F
_journal_year                    2019
_chemical_formula_moiety         'C38 H45 Dy Ge O'
_chemical_formula_sum            'C38 H45 Dy Ge O'
_chemical_formula_weight         752.83
_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
_audit_creation_date             2018-08-27
_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                 94.211(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.1320(5)
_cell_length_b                   20.8389(7)
_cell_length_c                   22.9987(9)
_cell_measurement_reflns_used    18918
_cell_measurement_temperature    180
_cell_measurement_theta_max      27.7250
_cell_measurement_theta_min      3.5170
_cell_volume                     6754.7(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24790
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.600
_diffrn_reflns_theta_min         1.776
_exptl_absorpt_coefficient_mu    3.112
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.679
_refine_diff_density_min         -1.548
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         24790
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0874P)^2^+25.2713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16626
_reflns_number_total             24790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00388f2.cif
_cod_data_source_block           6
_cod_database_code               7123679
_shelxl_version_number           2014-3
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.7219(7) 0.2781(7)
2. 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
3. Restrained distances
 C39-C49A = C39-C49 = C49A-C50 = C49A-C51 = C49-C50A = C49-C51A
 1.54 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C49A) = Uanis(C49)
Uanis(C50) = Uanis(C50A)
Uanis(C51) = Uanis(C51A)
Uanis(C28) = Uanis(C23)
5. Others
 Sof(C49)=Sof(H49)=Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(C51A)=Sof(H51D)=
 Sof(H51E)=Sof(H51F)=1-FVAR(1)
 Sof(C49A)=Sof(H49A)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51)=Sof(H51A)=
 Sof(H51B)=Sof(H51C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C52(H52), C49A(H49A), C49(H49), C11(H11), C14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C38(H38A,
 H38B), C37(H37A,H37B), C36(H36A,H36B), C35(H35A,H35B)
6.c Me refined with riding coordinates:
 C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C50A(H50D,H50E,H50F), C51A(H51D,H51E,H51F), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C)
6.d Aromatic/amide H refined with riding coordinates:
 C48(H48), C47(H47), C46(H46), C45(H45), C40(H40), C41(H41), C42(H42),
 C43(H43), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69),
  C70(H70), C71(H71), C72(H72), C60(H60), C59(H59), C58(H58), C57(H57),
 C56(H56), C5(H5), C4(H4), C3(H3), C2(H2), C7(H7), C8(H8), C9(H9), C10(H10),
 C28(H28), C27(H27), C26(H26), C25(H25), C24(H24), C22(H22), C21(H21), C20(H20),
  C19(H19), C18(H18), C34(H34), C33(H33), C32(H32), C31(H31), C30(H30)
;
_shelx_res_checksum              86681
_olex2_submission_special_instructions 'No special instructions were received'