Synthesis, X-ray Crystal Structures, Magnetism, and Phosphate Ester Cleavage Properties of Copper(II) Complexes of N-Substituted Derivatives of 1,4,7-Triazacyclononane
Matthew J. Belousoff; Martin B. Duriska; Bim Graham; Stuart R. Batten; Boujemaa Moubaraki; Keith S. Murray; Leone Spiccia; Inorganic Chemistry 45 (2006) 3746–3755; doi:10.1021/ic051983+

data_4327277
_publ_contact_author_address
;School of Chemistry
Wellington Rd
Clayton
Victoria, Australia, 3800
;
_publ_contact_author_email       leone.spiccia@sci.monash.edu.au
_publ_contact_author_fax         +610399054597
_publ_contact_author_name        'Leone Spiccia'
_publ_contact_author_phone       +610399054526
_publ_section_title
;
 Synthesis, X-ray Crystal Structures, Magnetism, and Phosphate Ester
 Cleavage Properties of Copper(II) Complexes of N-Substituted Derivatives
 of 1,4,7-Triazacyclononane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3746
_journal_page_last               3755
_journal_paper_doi               10.1021/ic051983+
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C66 H66 Cl2 Cu2 N12 O12'
_chemical_formula_sum            'C248 H263 Cl8 Cu8 N52 O49'
_chemical_formula_weight         5547.58
_chemical_name_common            '[Cu2((BzCN)3tacn)(u-OH)](ClO4)2(H2O)2'
_chemical_name_systematic
;
bis(1,4,7-tris-(3-tolunitrile)-1,4,7-triazacyclononane)-bis
-(u2- hydroxo)-dicopper(II)-diperchlorate monohydrate dihydrate
;
_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                75.79(3)
_cell_angle_beta                 78.78(3)
_cell_angle_gamma                88.31(3)
_cell_formula_units_Z            1
_cell_length_a                   17.358(4)
_cell_length_b                   17.588(4)
_cell_length_c                   23.239(5)
_cell_measurement_reflns_used    98487
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4
_cell_volume                     6745(3)
_computing_cell_refinement       'HKL Scalepack (Otwinoswski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius, 2000)'
_computing_data_reduction        'HKL Denzo (Otwinoswski & Minor, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method
'non-profiled thick slice omega/phi/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            98487
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.8292
_exptl_absorpt_correction_T_min  0.8001
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'Dark Green'
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       'Rectangle Prism'
_exptl_crystal_F_000             2875
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1748
_refine_ls_number_reflns         27900
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+9.5285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1992
_reflns_number_gt                16781
_reflns_number_total             27900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0519832Bsi20051117_102848_1.cif
_cod_data_source_block           C3
_cod_original_cell_volume        6745(2)
_cod_database_code               4327277