Benzoxazole-Based Heterometallic Dodecanuclear Complex [DyIII4CuII8] with Single-Molecule-Magnet Behavior
Olga Iasco; Ghenadie Novitchi; Erwann Jeanneau; Wolfgang Wernsdorfer; Dominique Luneau; Inorganic Chemistry 50 (2011) 7373–7375; doi:10.1021/ic201070n

data_4325951
_publ_section_title
;
 Benzoxazole-Based Heterometallic Dodecanuclear Complex [DyIII4CuII8] with
 Single-Molecule-Magnet Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7373
_journal_page_last               7375
_journal_paper_doi               10.1021/ic201070n
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
;
C132 H200 Cl10 Cu8 Gd4 N10 O29, 6(C2 H3 N), 2(Cl)
;
_chemical_formula_sum            'C144 H218 Cl12 Cu8 Gd4 N16 O29'
_chemical_formula_weight         4200.16
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.877(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.478(2)
_cell_length_b                   15.1550(10)
_cell_length_c                   36.220(2)
_cell_measurement_reflns_used    10476
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.8167
_cell_measurement_theta_min      3.4016
_cell_volume                     18923(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full NaN
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.118
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            67804
_diffrn_reflns_theta_full        0.213
_diffrn_reflns_theta_max         66.924
_diffrn_reflns_theta_min         3.404
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.907
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             8472
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.053
_refine_diff_density_max         2.82
_refine_diff_density_min         -1.60
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9538
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1008
_refine_ls_number_reflns         16653
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.0036462
_refine_ls_shift/su_mean         0.0000319
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.139E+04 0.207E+04 0.114E+04 371. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1908
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1908
_reflns_limit_h_max              40
_reflns_limit_h_min              -40
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              42
_reflns_limit_l_min              0
_reflns_number_gt                12627
_reflns_number_total             16656
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.14
_oxford_diffrn_Wilson_scale      41.72
_oxford_refine_ls_r_factor_ref   0.0888
_oxford_refine_ls_scale          0.4111(5)
_oxford_reflns_number_all        16653
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic201070n_si_001_1.cif
_cod_data_source_block           '[Gd4Cu8]'
_cod_original_cell_volume        18923.2(20)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4325951
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE O   (   3,X'S) H   (   1,X'S) 
RIDE O   (   4,X'S) H   (   2,X'S) 
RIDE O   (   7,X'S) H   (   3,X'S) 
RIDE O   (  12,X'S) H   (   4,X'S) 
RIDE O   (  13,X'S) H   (  13,X'S) 
RIDE O   (  14,X'S) H   (   6,X'S) H   ( 141,X'S) 
RIDE O   (  15,X'S) H   (   7,X'S) H   (   8,X'S) 
RIDE C   (   1,X'S) H   (   9,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) H   (  33,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) 
RIDE C   (  13,X'S) H   ( 133,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   (   5,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 233,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 383,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) H   ( 393,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) H   ( 403,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) H   ( 443,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) H   ( 453,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) H   ( 463,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) H   ( 553,X'S) 
RIDE C   (  56,X'S) H   ( 563,X'S) H   ( 561,X'S) H   ( 562,X'S) 
RIDE C   (  57,X'S) H   ( 572,X'S) H   ( 571,X'S) H   ( 573,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  61,X'S) H   ( 613,X'S) H   ( 611,X'S) H   ( 612,X'S) 
RIDE C   (  62,X'S) H   ( 622,X'S) H   ( 621,X'S) H   ( 623,X'S) 
RIDE C   (  63,X'S) H   ( 632,X'S) H   ( 633,X'S) H   ( 631,X'S) 
RIDE C   (  66,X'S) H   ( 662,X'S) H   ( 663,X'S) H   ( 661,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) H   ( 683,X'S) H   ( 682,X'S) 
RIDE C   (  74,X'S) H   ( 746,X'S) H   ( 745,X'S) H   ( 744,X'S) H   ( 743,X'S) 
RIDE C   (  70,X'S) H   ( 703,X'S) H   ( 702,X'S) H   ( 701,X'S) 
RIDE C   (  72,X'S) H   ( 723,X'S) H   ( 722,X'S) H   ( 721,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
DISTANCE 1.150000 , 0.050000 = C(67) TO N(6) 
DISTANCE 1.550000 , 0.050000 = C(67) TO C(68) 
DISTANCE 1.150000 , 0.050000 = C(69) TO N(7) 
DISTANCE 1.550000 , 0.050000 = C(69) TO C(70) 
DISTANCE 1.150000 , 0.050000 = C(73) TO N(9) 
DISTANCE 1.550000 , 0.050000 = C(73) TO C(74) 
DISTANCE 1.150000 , 0.050000 = C(75) TO N(10) 
DISTANCE 1.550000 , 0.050000 = C(75) TO C(74) 
DISTANCE 1.150000 , 0.050000 = C(71) TO N(8) 
DISTANCE 1.550000 , 0.050000 = C(71) TO C(72) 
DISTANCE 1.150000 , 0.050000 = C(65) TO N(5) 
DISTANCE 1.550000 , 0.050000 = C(65) TO C(66) 
U(IJ)'S  0.0, 0.010000 = C(67) TO N(6) 
U(IJ)'S  0.0, 0.010000 = C(68) TO C(67) 
U(IJ)'S  0.0, 0.010000 = C(69) TO N(7) 
U(IJ)'S  0.0, 0.010000 = C(69) TO C(70) 
U(IJ)'S  0.0, 0.010000 = C(73) TO N(9) 
U(IJ)'S  0.0, 0.010000 = C(73) TO C(74) 
U(IJ)'S  0.0, 0.010000 = C(75) TO N(10) 
U(IJ)'S  0.0, 0.010000 = C(75) TO C(74) 
U(IJ)'S  0.0, 0.010000 = C(71) TO N(8) 
U(IJ)'S  0.0, 0.010000 = C(71) TO C(72) 
U(IJ)'S  0.0, 0.010000 = C(65) TO N(5) 
U(IJ)'S  0.0, 0.010000 = C(65) TO C(66) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 0.820000 , 0.010000 = O(13) TO H(13) 
ANGLE 109.000000 , 0.500000 = H(13,2,1,1,0,1) TO O(13) TO H(13) 
END                                                                             
;