Lanthanide Triangles Sandwiched by Tetranuclear Copper Complexes Afford a Family of Hendecanuclear Heterometallic Complexes [LnIII3CuII8] (Ln = La-Lu): Synthesis and Magnetostructural Studies
Olga Iasco; Ghenadie Novitchi; Erwann Jeanneau; Dominique Luneau; Inorganic Chemistry 52 (2013) 8723–8731; doi:10.1021/ic4009015

data_4335558
_publ_section_title
;
 Lanthanide Triangles Sandwiched by Tetranuclear Copper Complexes Afford a
 Family of Hendecanuclear Heterometallic Complexes [LnIII3CuII8] (Ln =
 La-Lu): Synthesis and Magnetostructural Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8723
_journal_page_last               8731
_journal_paper_doi               10.1021/ic4009015
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C54 H70 Cl6 Cu8 N6 Nd3 O28, 3(Cl)'
_chemical_formula_sum            'C54 H70 Cl9 Cu8 N6 Nd3 O28'
_chemical_formula_weight         2511.33
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   22.135(3)
_cell_length_b                   22.135(3)
_cell_length_c                   21.038(3)
_cell_measurement_reflns_used    2432
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.2175
_cell_measurement_theta_min      3.4075
_cell_volume                     8927(2)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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 0.969
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7413
_diffrn_reflns_theta_full        25.181
_diffrn_reflns_theta_max         29.280
_diffrn_reflns_theta_min         3.414
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.935
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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            'dark green'
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       plate
_exptl_crystal_F_000             3674.988
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.158
_platon_squeeze_details
;
;
_refine_diff_density_max         1.00
_refine_diff_density_min         -1.05
_refine_ls_abs_structure_details 'Flack (1983), 114 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.8845
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         4552
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.0018660
_refine_ls_shift/su_mean         0.0000474
_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: 
 0.176E+05 0.282E+05 0.140E+05 0.476E+04 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0995
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0995
_reflns_limit_h_max              14
_reflns_limit_h_min              -29
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                2946
_reflns_number_total             4552
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.70
_oxford_diffrn_Wilson_scale      15.16
_oxford_refine_ls_r_factor_ref   0.0882
_oxford_refine_ls_scale          3.66(3)
_oxford_reflns_number_all        4552
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic4009015_si_001_03.cif
_cod_data_source_block           '[Nd3Cu]-4'
_cod_original_sg_symbol_H-M      'R 3 2 '
_cod_database_code               4335558
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   (   1,X'S) H   (6623,X'S) H   (  12,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  52,X'S) H   (  53,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE O   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
REM TOO MANY H ATOMS ON O   (   6), - 6 
RIDE O   (   6,X'S) H   (  62,X'S) H   (  63,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;