Coordination Chemistry of a Novel Tetramacrocyclic Ligand Derived from 1,4,7-Triazacyclononane: Synthesis, Structure, and Properties of Nickel(II) and Copper(II) Complexes
Bim Graham; Martin J. Grannas; Milton T. W. Hearn; Christopher M. Kepert; Leone Spiccia; Brian W. Skelton; Allan H. White; Inorganic Chemistry 39 (2000) 1092–1099; doi:10.1021/ic991082z

data_4300191
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   Nedlands
   Western Australia 6907
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_9380_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08-9380_3481
_publ_section_title
;
Coordination Chemistry of a Novel Tetramacrocyclic Ligand Derived from
1,4,7-Triazacyclononane: Synthesis, Structure, and Properties of
Nickel(II) and Copper(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1092
_journal_page_last               1099
_journal_paper_doi               10.1021/ic991082z
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C34 H100 Cl8 Cu4 N12 O49'
_chemical_formula_weight         1999.02
_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'
_cell_angle_alpha                90.00000
_cell_angle_beta                 108.24(5)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   16.713(7)
_cell_length_b                   16.714(6)
_cell_length_c                   14.775(14)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    293
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      9.8
_cell_volume                     3920(4)
_computing_cell_refinement       'Enraf Nonius software'
_computing_data_collection       'Enraf Nonius software'
_computing_data_reduction        'xtal ADDREF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type
;
CAD4 diffractometer
;
_diffrn_measurement_method       '2\q-\w scans'
_diffrn_radiation_detector       'single counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .035
_diffrn_reflns_av_sigmaI/netI    .041
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13768
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  600
_diffrn_standards_number         14
_exptl_absorpt_coefficient_mu    1.45
_exptl_absorpt_correction_T_max  .76
_exptl_absorpt_correction_T_min  .45
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 XTAL absorb
;
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       prism
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.20
_refine_diff_density_max         .881
_refine_diff_density_min         -1.003
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_ref   1.333
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           atomblock
_refine_ls_number_constraints    0
_refine_ls_number_parameters     483
_refine_ls_number_reflns         3259
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          .14
_refine_ls_R_factor_gt           .084
_refine_ls_shift/su_max          .08
_refine_ls_shift/su_mean         .007
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .121
_refine_ls_wR_factor_ref         .099
_reflns_d_resolution_high        .84
_reflns_d_resolution_low         11.51
_reflns_limit_h_max              19
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -17
_reflns_number_gt                6898
_reflns_number_total             6898
_reflns_threshold_expression     'I    > 3 sig(I   )'
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_database_code               4300191