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_4327280
_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         'C30 H54 Cl2 Cu2 N6 O11'
_chemical_formula_sum            'C30 H54 Cl2 Cu2 N6 O11'
_chemical_formula_weight         872.77
_chemical_name_common            Cu2-(Me2Bztacn)2(ClO4)2
_chemical_name_systematic
;
 bis(1,4-dimethyl-1,4,7-triazacyclononane)-
bis-(u2-hydroxo)-dicopper(II)-diperchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.748(2)
_cell_length_b                   16.733(3)
_cell_length_c                   20.725(4)
_cell_measurement_reflns_used    35263
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4
_cell_volume                     3704.2(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '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  0.1160
_diffrn_reflns_av_sigmaI/netI    0.1036
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35263
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       'Small Prism'
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         6504
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0701
_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^)+(0.0171P)^2^+9.9554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                4680
_reflns_number_total             6504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0519832Bsi20051117_102848_4.cif
_cod_data_source_block           C2
_cod_original_cell_volume        3704.2(13)
_cod_database_code               4327280