Single molecule magnet behaviour in a rare trinuclear {Cr(III)Dy} methoxo-bridged complex.
Car, Pierre-Emmanuel; Favre, Annaïck; Caneschi, Andrea; Sessoli, Roberta; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15769–15773; doi:10.1039/c5dt02459e

data_7036085
_publ_section_title
;
 Single molecule magnet behaviour in a rare trinuclear {Cr(III)Dy}
 methoxo-bridged complex.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15769
_journal_page_last               15773
_journal_paper_doi               10.1039/c5dt02459e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C60 H111 Cr Dy2 O15, C H4 O'
_chemical_formula_sum            'C61 H115 Cr Dy2 O16'
_chemical_formula_weight         1481.52
_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   mixed
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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2015-06-25 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
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_cell_length_b                   14.788(5)
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_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
  1 omega  -48.00   12.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.6757   77.0000 -120.0000 60

  2 omega  -11.00   38.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.6757 -114.0000  106.0000 49

  3 omega  -77.00   17.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.6757  -38.0000 -120.0000 94

  4 omega  -58.00   42.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7695  -38.0000  120.0000 100

  5 omega  -16.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7695   38.0000   90.0000 105

  6 omega  -46.00   57.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.6757   38.0000   60.0000 103
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
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_diffrn_orient_matrix_UB_11      0.0094957518
_diffrn_orient_matrix_UB_12      0.0121242784
_diffrn_orient_matrix_UB_13      -0.0256546002
_diffrn_orient_matrix_UB_21      0.0190074240
_diffrn_orient_matrix_UB_22      0.0511638129
_diffrn_orient_matrix_UB_23      0.0138834591
_diffrn_orient_matrix_UB_31      0.0670524974
_diffrn_orient_matrix_UB_32      0.0035985814
_diffrn_orient_matrix_UB_33      0.0050384751
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.1478
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28156
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        23.000
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         4.109
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73356
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       prism
_exptl_crystal_F_000             1530
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.613
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.861
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     787
_refine_ls_number_reflns         11696
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0524P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6509
_reflns_number_total             11696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02459e2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7036085.cif.'
_cod_database_code               7036085
_reflns_odcompleteness_completeness 99.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O2-H2
 0.82 with sigma of 0.01
 C58-C59 \\sim C59-C60 \\sim C58-C60
 with sigma of 0.01
 C54A-C55A \\sim C54A-C56A \\sim C55A-C56A
 with sigma of 0.01
 C54B-C55B \\sim C54B-C56B \\sim C55B-C56B
 with sigma of 0.01
 C53-C54A \\sim C53-C55A \\sim C53-C56A \\sim C53-C54B \\sim C53-C55B \\sim
C53-C56B
 with sigma of 0.005
 C50-C54A \\sim C50-C55A \\sim C50-C56A \\sim C50-C54B \\sim C50-C55B \\sim
C50-C56B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C53 \\sim C54A \\sim C55A \\sim C56A \\sim C54B \\sim C55B \\sim C56B: within
2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
C42 \\sim C43 \\sim C44 \\sim C45: within 2.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C35 \\sim C36 \\sim C37 \\sim C38: within 2.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C57 \\sim C58 \\sim C59 \\sim C60: within 2.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C54B)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C55B)=Sof(H55D)=Sof(H55E)=
 Sof(H55F)=Sof(C56B)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(1)
 Sof(C54A)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C55A)=Sof(H55A)=Sof(H55B)=
 Sof(H55C)=Sof(C56A)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(1)
5.a Me refined with riding coordinates:
 C54A(H54A,H54B,H54C), C55A(H55A,H55B,H55C), C56A(H56A,H56B,H56C), C54B(H54D,
 H54E,H54F), C55B(H55D,H55E,H55F), C56B(H56D,H56E,H56F)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C18(H18), C29(H29), C40(H40), C51(H51)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C)
5.d Idealised tetrahedral OH refined as rotating group:
 O16(H16)
;
_shelx_res_checksum              50204
_shelx_shelxl_version_number     2014/7