Structural and Magnetic Diversity in Cyano-Bridged Bi- and Trimetallic Complexes Assembled from Cyanometalates and [M(rac-CTH)]n+Building Blocks (CTH =d,l-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)
Rodríguez-Diéguez, Antonio; Kivekäs, Raikko; Sillanpää, Reijo; Cano, Joan; Lloret, Francesc; McKee, Vickie; Stoeckli-Evans, Helen; Colacio, Enrique; Inorganic Chemistry 45 (2006) 10537–10551; doi:10.1021/ic061187j

data_4332981
_publ_section_title
;
 Structural and Magnetic Diversity in Cyano-Bridged Bi- and Trimetallic
 Complexes Assembled from Cyanometalates and [M(rac-CTH)]n+Building Blocks
 (CTH =d,l-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10537
_journal_page_last               10551
_journal_paper_doi               10.1021/ic061187j
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C60 H108 Cr2 N24 Ni3, 4(H2 O)'
_chemical_formula_sum            'C60 H116 Cr2 N24 Ni3 O4'
_chemical_formula_weight         1517.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.5615(11)
_cell_angle_beta                 83.7558(12)
_cell_angle_gamma                64.1686(10)
_cell_formula_units_Z            2
_cell_length_a                   14.3480(8)
_cell_length_b                   15.0301(8)
_cell_length_c                   21.5086(11)
_cell_measurement_reflns_used    1373
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.75
_cell_measurement_theta_min      2.48
_cell_volume                     4076.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1461
_diffrn_reflns_av_sigmaI/netI    0.2129
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43810
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  0.9708
_exptl_absorpt_correction_T_min  0.8415
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North, Phillips & Mathews 1968'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         15931
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.2536
_refine_ls_R_factor_gt           0.1122
_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^)+(0.1457P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2634
_refine_ls_wR_factor_ref         0.3203
_reflns_number_gt                5988
_reflns_number_total             15931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061187jsup1.cif
_cod_data_source_block           compound_3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332981