Strong direct exchange coupling and single-molecule magnetism in indigo-bridged lanthanide dimers.
Guo, Fu-Sheng; Layfield, Richard A.; Chemical communications (Cambridge, England) 53 (2017) 3130–3133; doi:10.1039/c7cc01046j

data_7119719
_publ_section_title
;
 Strong direct exchange coupling and single-molecule magnetism in
 indigo-bridged lanthanide dimers.
;
_journal_issue                   21
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3130
_journal_page_last               3133
_journal_paper_doi               10.1039/c7cc01046j
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C56 H68 Dy2 N2 O2, C24 H48 K O6, C4 H8 O'
_chemical_formula_sum            'C84 H124 Dy2 K N2 O9'
_chemical_formula_weight         1669.94
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-25
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Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
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2017-02-07 deposited with the CCDC.
2017-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                80.217(3)
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_cell_angle_gamma                81.452(3)
_cell_formula_units_Z            1
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_cell_measurement_theta_max      28.6700
_cell_measurement_theta_min      3.7480
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -7.00   84.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   37.0000  -30.0000 91

  2 omega   34.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000  -60.0000 27

  3 omega  -19.00    8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000   60.0000 27

  4 omega  -34.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -37.0000  150.0000 79

  5 omega  -11.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000   60.0000 97

  6 omega  -10.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000 -180.0000 40

  7 omega  -48.00  -15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000  150.0000 33

  8 omega  -85.00  -58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663 -178.0000 -150.0000 27
;
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_diffrn_orient_matrix_UB_21      0.0484266000
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_diffrn_orient_matrix_UB_23      -0.0198384000
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_diffrn_orient_matrix_UB_33      -0.0347252000
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16458
_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.392
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.833
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'dark red'
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_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0443
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+3.3576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                7164
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_cod_depositor_comments
'Adding full bibliography for 7119716--7119721.cif.'
_cod_original_cell_volume        2140.42(14)
_cod_database_code               7119719
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C42-C41 = C43-C42 = C44-C43
 1.5 with sigma of 0.01
 O5-C44 = O5-C41
 1.43 with sigma of 0.01
 C43-O5 = O5-C42
 2.3 with sigma of 0.01
 C41-C43 = C44-C42
 2.4 with sigma of 0.01
 O4-C40 = O4-C37
 1.43 with sigma of 0.01
 C38-C37 = C39-C38 = C40-C39
 1.5 with sigma of 0.01
 C40-C38 \\sim C39-C37
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C22 \\sim C27: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
C23 \\sim C28: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
C21 \\sim C26: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
C19 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O4 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\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
Uanis(C43) = Uanis(C44)
4. Others
 Fixed Sof: O5(0.5) C41(0.5) H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5) H42B(0.5)
 C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
  C43(H43A,H43B), C44(H44A,H44B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              69298
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'