Synthesis, structure, magnetism and theoretical study of a series of complexes with a decanuclear core [Ln(iii)2Cu(ii)8] (Ln = Y, Gd, Tb, Dy)
Borta, Ana; Jeanneau, Erwann; Chumakov, Yuri; Luneau, Dominique; Ungur, Liviu; Chibotaru, Liviu F.; Wernsdorfer, Wolfgang; New Journal of Chemistry 35 (2011) 1270–; doi:10.1039/c0nj00931h

data_7052658
_publ_section_related_literature
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?
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_publ_section_title
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 Synthesis, structure, magnetism and theoretical study of a series of
 complexes with a decanuclear core [Ln(iii)2Cu(ii)8] (Ln = Y, Gd, Tb,
 Dy)
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1270
_journal_paper_doi               10.1039/c0nj00931h
_journal_volume                  35
_journal_year                    2011
_chemical_formula_moiety         'C60 H52 Cl6 Cu8 N12 O16 Y2, (H2 O)13.1'
_chemical_formula_sum            'C60 H78.2 Cl6 Cu8 N12 O29.1 Y2'
_chemical_formula_weight         2332.02
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-01-27
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                90
_cell_angle_beta                 96.870(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   16.5041(16)
_cell_length_b                   19.2258(18)
_cell_length_c                   45.343(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     14284(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      293
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.105
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            127902
_diffrn_reflns_theta_full        20.713
_diffrn_reflns_theta_max         20.713
_diffrn_reflns_theta_min         0.905
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.175
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7002
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         1.41
_refine_diff_density_min         -1.22
_refine_ls_extinction_coef       320(50)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0438
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1406
_refine_ls_number_reflns         14560
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.0015151
_refine_ls_shift/su_mean         0.0002031
_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:
79.3 122. 61.0 16.7
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2221
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.2221
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              44
_reflns_limit_l_min              0
_reflns_number_gt                8705
_reflns_number_total             14676
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.22
_oxford_diffrn_Wilson_scale      77.91
_oxford_refine_ls_r_factor_ref   0.0862
_oxford_refine_ls_scale          0.12371(8)
_oxford_reflns_number_all        14560
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title CRYSTALS_cif
_cod_data_source_file            c0nj00931h.txt
_cod_data_source_block           CuY
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7052658
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 1,X'S) H ( 1,X'S)
RIDE C ( 2,X'S) H ( 2,X'S)
RIDE C ( 3,X'S) H ( 3,X'S)
RIDE C ( 4,X'S) H ( 4,X'S)
RIDE C ( 6,X'S) H ( 6,X'S)
RIDE C ( 7,X'S) H ( 7,X'S)
RIDE C ( 8,X'S) H ( 8,X'S)
RIDE C ( 9,X'S) H ( 9,X'S)
RIDE C ( 11,X'S) H ( 11,X'S)
RIDE C ( 12,X'S) H ( 12,X'S)
RIDE C ( 13,X'S) H ( 13,X'S)
RIDE C ( 14,X'S) H ( 14,X'S)
RIDE C ( 16,X'S) H ( 16,X'S)
RIDE C ( 17,X'S) H ( 17,X'S)
RIDE C ( 18,X'S) H ( 18,X'S)
RIDE C ( 19,X'S) H ( 19,X'S)
RIDE C ( 21,X'S) H ( 21,X'S)
RIDE C ( 22,X'S) H ( 22,X'S)
RIDE C ( 23,X'S) H ( 23,X'S)
RIDE C ( 24,X'S) H ( 24,X'S)
RIDE C ( 26,X'S) H ( 26,X'S)
RIDE C ( 27,X'S) H ( 27,X'S)
RIDE C ( 28,X'S) H ( 28,X'S)
RIDE C ( 29,X'S) H ( 29,X'S)
RIDE C ( 31,X'S) H ( 31,X'S)
RIDE C ( 32,X'S) H ( 32,X'S)
RIDE C ( 33,X'S) H ( 33,X'S)
RIDE C ( 34,X'S) H ( 34,X'S)
RIDE C ( 36,X'S) H ( 36,X'S)
RIDE C ( 37,X'S) H ( 37,X'S)
RIDE C ( 38,X'S) H ( 38,X'S)
RIDE C ( 39,X'S) H ( 39,X'S)
RIDE C ( 41,X'S) H ( 41,X'S)
RIDE C ( 42,X'S) H ( 42,X'S)
RIDE C ( 43,X'S) H ( 43,X'S)
RIDE C ( 44,X'S) H ( 44,X'S)
RIDE C ( 46,X'S) H ( 46,X'S)
RIDE C ( 47,X'S) H ( 47,X'S)
RIDE C ( 48,X'S) H ( 48,X'S)
RIDE C ( 49,X'S) H ( 49,X'S)
RIDE C ( 51,X'S) H ( 51,X'S)
RIDE C ( 52,X'S) H ( 52,X'S)
RIDE C ( 53,X'S) H ( 53,X'S)
RIDE C ( 54,X'S) H ( 54,X'S)
RIDE C ( 56,X'S) H ( 56,X'S)
RIDE C ( 57,X'S) H ( 57,X'S)
RIDE C ( 58,X'S) H ( 58,X'S)
RIDE C ( 59,X'S) H ( 59,X'S)
RIDE C ( 61,X'S) H ( 61,X'S)
RIDE C ( 62,X'S) H ( 62,X'S)
RIDE C ( 63,X'S) H ( 63,X'S)
RIDE C ( 64,X'S) H ( 64,X'S)
RIDE C ( 66,X'S) H ( 66,X'S)
RIDE C ( 67,X'S) H ( 67,X'S)
RIDE C ( 68,X'S) H ( 68,X'S)
RIDE C ( 69,X'S) H ( 69,X'S)
RIDE C ( 71,X'S) H ( 71,X'S)
RIDE C ( 72,X'S) H ( 72,X'S)
RIDE C ( 73,X'S) H ( 73,X'S)
RIDE C ( 74,X'S) H ( 74,X'S)
RIDE C ( 76,X'S) H ( 76,X'S)
RIDE C ( 77,X'S) H ( 77,X'S)
RIDE C ( 78,X'S) H ( 78,X'S)
RIDE C ( 79,X'S) H ( 79,X'S)
RIDE C ( 81,X'S) H ( 81,X'S)
RIDE C ( 82,X'S) H ( 82,X'S)
RIDE C ( 83,X'S) H ( 83,X'S)
RIDE C ( 84,X'S) H ( 84,X'S)
RIDE C ( 86,X'S) H ( 86,X'S)
RIDE C ( 87,X'S) H ( 87,X'S)
RIDE C ( 88,X'S) H ( 88,X'S)
RIDE C ( 89,X'S) H ( 89,X'S)
RIDE O ( 24,X'S) H ( 242,X'S) H ( 241,X'S)
RIDE O ( 15,X'S) H ( 151,X'S) H ( 152,X'S)
RIDE O ( 16,X'S) H ( 162,X'S) H ( 161,X'S)
END
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