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_4327278
_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         'C8 H14 Cl2 N2 O2'
_chemical_formula_sum            'C4 H7 Cl N O'
_chemical_formula_weight         120.56
_chemical_name_common
N,N'-bis(2-chloroacetyl)-N,N'-dimethylethylenediamine
_chemical_name_systematic
;
 N,N'-bis(2-chloroacetyl)-N,N'-dimethylethylenediamine
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 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                   9.975(2)
_cell_length_b                   8.0632(16)
_cell_length_c                   13.679(3)
_cell_measurement_reflns_used    15798
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     1100.2(4)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'non-profiled 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  0.0865
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15798
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       'Rectangular Prism'
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0336P)^2^+0.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                892
_reflns_number_total             1299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0519832Bsi20051117_102848_2.cif
_cod_data_source_block           bis-(chloroacetamide)
_cod_database_code               4327278