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_4315274
_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_absolute_configuration ad
_chemical_formula_moiety         'C20 H46 Co N7, 3(Cl O4),Cl, 3(H2 O)'
_chemical_formula_sum            'C20 H46 Cl4 Co N7 O15 S'
_chemical_formula_weight         857.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5396(3)
_cell_length_b                   14.5424(4)
_cell_length_c                   19.7738(5)
_cell_measurement_reflns_used    38816
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.1002
_cell_measurement_theta_min      2.7074
_cell_volume                     3318.31(15)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
        (compiled Apr 27 2007,17:53:11)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
        (compiled Apr 27 2007,17:53:11)
;
_computing_data_reduction
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        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
        (compiled Apr 27 2007,17:53:11)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
;
 Oxford Diffraction Xcalibur diffractometer

;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0031631732
_diffrn_orient_matrix_UB_12      0.0160779936
_diffrn_orient_matrix_UB_13      0.0337810819
_diffrn_orient_matrix_UB_21      0.0119750888
_diffrn_orient_matrix_UB_22      0.0452641547
_diffrn_orient_matrix_UB_23      -0.011249733
_diffrn_orient_matrix_UB_31      -0.0601398912
_diffrn_orient_matrix_UB_32      0.0082487842
_diffrn_orient_matrix_UB_33      -0.0040282759
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
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_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.94446
_exptl_absorpt_correction_type   multi-scan
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;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.343
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         16695
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                11837
_reflns_number_total             16695
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic9019603_si_004.cif
_cod_data_source_block           gk220
_cod_database_code               4315274