Synergistic effect of mixed ligands on the anisotropy axis of two dinuclear dysprosium complexes.
Ke, Hongshan; Yang, Yongsheng; Wei, Wen; Jiang, Youdong; Zhang, Yi-Quan; Xie, Gang; Chen, Sanping; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10594–10602; doi:10.1039/d0dt02139c

data_7704901
_publ_section_title
;
 Synergistic effect of mixed ligands on the anisotropy axis of two
 dinuclear dysprosium complexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10594
_journal_page_last               10602
_journal_paper_doi               10.1039/d0dt02139c
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C91 H116 Dy2 N4 O14'
_chemical_formula_sum            'C91 H116 Dy2 N4 O14'
_chemical_formula_weight         1814.87
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-02 deposited with the CCDC.	2020-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   26.065(3)
_cell_length_b                   26.065(3)
_cell_length_c                   36.149(6)
_cell_measurement_reflns_used    9729
_cell_measurement_temperature    296.98
_cell_measurement_theta_max      63.975
_cell_measurement_theta_min      5.005
_cell_volume                     21269(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.98
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.1095
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            20461
_diffrn_reflns_point_group_measured_fraction_full 0.685
_diffrn_reflns_point_group_measured_fraction_max 0.685
_diffrn_reflns_theta_full        63.687
_diffrn_reflns_theta_max         63.687
_diffrn_reflns_theta_min         4.999
_exptl_absorpt_coefficient_mu    8.827
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.5911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1037 before and 0.0749 after correction. The Ratio of minimum to maximum transmission is 0.7856. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       plate
_exptl_crystal_F_000             8406
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.018(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         10693
_refine_ls_number_restraints     894
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+236.5643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.388
_reflns_Friedel_fraction_full    0.383
_reflns_Friedel_fraction_max     0.383
_reflns_number_gt                9272
_reflns_number_total             10693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02139c2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 7704900--7704901.cif.

 Adding full bibliography for 7704900--7704901.cif.
;
_cod_original_cell_volume        21268(6)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7704901
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.472
_shelx_estimated_absorpt_t_min   0.177
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O13-H13
 0.85 with sigma of 0.01
 H21F-H9
 2.2 with sigma of 0.02
 C56-C58
 2.5 with sigma of 0.02
 H55-H58C
 2.2 with sigma of 0.02
 C56-C58A
 2.5 with sigma of 0.02
 H55-H58D
 2.2 with sigma of 0.02
 H64B-H61
 2.2 with sigma of 0.02
 C58-C57 = C60A-C57 = C60-C57 = C59A-C57 = C59-C57 = C58A-C57
 1.5 with sigma of 0.01
 C60A-C59A = C59A-C58A
 2.5 with sigma of 0.02
 C82A-C79 = C82-C79 = C81A-C79 = C81-C79 = C80A-C79 = C80-C79
 1.5 with sigma of 0.01
 O14-C91 = O14-C91A
 1.5 with sigma of 0.01
 O14-H14
 0.85 with sigma of 0.01
 O14-H14D
 0.85 with sigma of 0.01
 H17-H20D
 2.2 with sigma of 0.02
 C22A-C19 = C21-C19 = C21A-C19 = C20-C19 = C20A-C19 = C22-C19
 1.5 with sigma of 0.01
 C89-H13
 1.861366 with sigma of 0.02
 Dy1-H13
 3.045033 with sigma of 0.02
 C91-H14
 1.94932 with sigma of 0.02
 Dy2-H14
 3.138567 with sigma of 0.02
 C91A-H14D
 1.949595 with sigma of 0.02
 Dy2-H14D
 2.934884 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C41 \\sim C44: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C58A \\sim C59A \\sim C60A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C91 \\sim C91A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C79 \\sim C80 \\sim C81 \\sim C82 \\sim C82A \\sim C81A \\sim C80A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
O14 \\sim C91A \\sim C91: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq,
Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq,
Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C21A)
\\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C58A) \\sim Ueq,
Uanis(C59A) \\sim Ueq, Uanis(C60A) \\sim Ueq, Uanis(C82A) \\sim Ueq,
Uanis(C81A) \\sim Ueq, Uanis(C80A) \\sim Ueq, Uanis(C91A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C44, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C57, C58, C59, C60, C58A, C59A, C60A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C91, C91A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O14, C91, C91A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C19, C20, C21, C22, C21A, C20A, C22A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
 Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59A)=Sof(H59D)=Sof(H59E)=
 Sof(H59F)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(2)
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(2)
 Sof(C82A)=Sof(H82D)=Sof(H82E)=Sof(H82F)=Sof(C81A)=Sof(H81D)=Sof(H81E)=
 Sof(H81F)=Sof(C80A)=Sof(H80D)=Sof(H80E)=Sof(H80F)=1-FVAR(3)
 Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=
 Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=FVAR(3)
 Sof(H14D)=Sof(C91A)=Sof(H91D)=Sof(H91E)=Sof(H91F)=1-FVAR(4)
 Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=Sof(H14)=FVAR(4)
6.a Riding coordinates:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C36(H36A,H36B,H36C), C81(H81A,H81B,
 H81C), C91(H91A,H91B,H91C), O14(H14D), O14(H14), C20A(H20D,H20E,H20F),
 C59A(H59D,H59E,H59F), C80A(H80D,H80E,H80F)
6.b Secondary CH2 refined with riding coordinates:
 C89(H89A,H89B)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C9(H9), C17(H17), C26(H26), C27(H27), C28(H28),
 C33(H33), C39(H39), C48(H48), C49(H49), C50(H50), C52(H52), C55(H55), C61(H61),
  C70(H70), C71(H71), C72(H72), C74(H74), C77(H77), C83(H83)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C86(H86A,H86B,H86C),
 C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C21A(H21D,H21E,
 H21F), C22A(H22D,H22E,H22F), C58A(H58D,H58E,H58F), C60A(H60D,H60E,H60F),
 C82A(H82D,H82E,H82F), C81A(H81D,H81E,H81F), C91A(H91D,H91E,H91F)
;
_shelx_res_checksum              97031
_shelx_fab_checksum              46694
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'