Structural and Electrochemical Studies of Co(III) Cage Amine Complexes with Pendent Thienylmethylamino Groups
Jack M. Harrowfield; George A. Koutsantonis; Nigel A. Lengkeek; Brian W. Skelton; Allan H. White; Inorganic Chemistry 49 (2010) 3152–3161; doi:10.1021/ic9019603

data_4315272
_publ_contact_author_address
;
   Chemistry
   University of Western Australia
   35 Stirling Highway
   Crawley
   Western Australia 6009
   Australia
;
_publ_contact_author_email       brian.skelton@uwa.edu.au
_publ_contact_author_fax         (+61)_08_6488_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08_6488_7107
_publ_section_title
;
 Structural and Electrochemical Studies of Co(III) Cage Amine Complexes
 with Pendent Thienylmethylamino Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3152
_journal_page_last               3161
_journal_paper_doi               10.1021/ic9019603
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C24 H44 Co N8 S2, 5(H2 O), 5(Cl)'
_chemical_formula_sum            'C24 H54 Cl5 Co N8 O5 S2'
_chemical_formula_weight         835.05
_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_date             2009-08-23T18:50:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                73.433(2)
_cell_angle_beta                 89.839(2)
_cell_angle_gamma                79.880(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4870(10)
_cell_length_b                   12.1800(10)
_cell_length_c                   14.986(2)
_cell_measurement_reflns_used    7005
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.4
_cell_measurement_theta_min      2.57
_cell_volume                     1803.9(3)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    OrtepII
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.92
_diffrn_measurement_device_type
;
        Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27427
_diffrn_reflns_theta_full        32
_diffrn_reflns_theta_max         33.5
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flat_rod
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         13026
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+1.3091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                11017
_reflns_number_total             13026
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic9019603_si_002.cif
_cod_data_source_block           gk178
_cod_original_sg_symbol_Hall     -P_1
_cod_database_code               4315272