Tuning the Spin Ground State in Heterononanuclear Nickel(II)-Copper(II) Cylinders with a Triangular Metallacyclophane Core
Marie-Claire Dul; Jesús Ferrando-Soria; Emilio Pardo; Rodrigue Lescouëzec; Yves Journaux; Rafael Ruiz-García; Joan Cano; Miguel Julve; Francesc Lloret; Oscar Fabelo; Jorge Pasán; Catalina Ruiz-Pérez; Inorganic Chemistry 49 (2010) 11264–11266; doi:10.1021/ic102037m

data_4317363
_publ_contact_author_address
;Laboratorio de Rayos X y Materiales Moleculares
 Dpto. F\'isica Fundamental II. Facultad de F\'isica
 Universidad de La Laguna
 E-38204. La Laguna. Tenerife
 Spain
;
_publ_contact_author_email       caruiz@ull.es
_publ_contact_author_fax         +34922318320
_publ_contact_author_name        'Professor Catalina Ruiz-P\'erez'
_publ_contact_author_phone       +34922318300
_publ_section_title
;
 Tuning the Spin Ground State in Heterononanuclear Nickel(II)-Copper(II)
 Cylinders with a Triangular Metallacyclophane Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11264
_journal_page_last               11266
_journal_paper_doi               10.1021/ic102037m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C78 H158 Cl6 Cu8 N24 Ni O55'
_chemical_formula_weight         3092.01
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      73
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.653(5)
_cell_length_b                   27.605(6)
_cell_length_c                   36.879(7)
_cell_measurement_temperature    100(2)
_cell_volume                     26116(9)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'MxCube (ESRF, 2006)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9.6
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_detector       'ADSC Q210r CCD (binned mode)'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.75130
_diffrn_reflns_av_R_equivalents  0.1392
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            334069
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.64
_diffrn_source                   synchrotron
_diffrn_source_type              'ESRF-CRG BM16'
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_T_max  0.8804
_exptl_absorpt_correction_T_min  0.8669
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             12768
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.155
_refine_diff_density_min         -2.341
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.00059(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         12819
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.1058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1441P)^2^+359.1875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2749
_refine_ls_wR_factor_ref         0.2956
_reflns_number_gt                10124
_reflns_number_total             12819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102037m_si_003.cif
_cod_data_source_block           final
_cod_database_code               4317363