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_4315271
_publ_contact_author_address
;
School of Biomedical, Biomolecular and Chemical Sciences, 
The University of Western Australia, 
35 Stirling Highway,
 Crawley, 
Western Australia, 6009

;
_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         'C20 H40 Co N7 S, 7(H2 O), 4(Cl) '
_chemical_formula_sum            'C20 H54 Cl4 Co N7 O7 S'
_chemical_formula_weight         737.49
_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             2009-09-06T10:35:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                95.0180(10)
_cell_angle_beta                 93.2580(10)
_cell_angle_gamma                105.5250(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9640(8)
_cell_length_b                   11.9100(10)
_cell_length_c                   14.7250(12)
_cell_measurement_reflns_used    9455
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.37
_cell_volume                     1671.4(2)
_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      170(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.886
_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  0.018
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14430
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             780
_exptl_crystal_size_max          .58
_exptl_crystal_size_mid          .52
_exptl_crystal_size_min          .37
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7599
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.5498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                6600
_reflns_number_total             7599
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic9019603_si_001.cif
_cod_data_source_block           gk173
_cod_original_sg_symbol_Hall     -p_1
_cod_database_code               4315271