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_4315275
_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         'C19 H40 Co N8 S, Cl O4, 4(Cl),3(H2 O)'
_chemical_formula_sum            'C19 H46 Cl5 Co N8 O7 S'
_chemical_formula_weight         766.88
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
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_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.631(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9924(3)
_cell_length_b                   14.0651(5)
_cell_length_c                   16.3511(5)
_cell_measurement_reflns_used    20734
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.6594
_cell_measurement_theta_min      2.6362
_cell_volume                     3113.62(17)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
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        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
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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)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_orient_matrix_UB_11      -0.0171953322
_diffrn_orient_matrix_UB_12      0.0474648488
_diffrn_orient_matrix_UB_13      -0.0045020206
_diffrn_orient_matrix_UB_21      -0.032541523
_diffrn_orient_matrix_UB_22      -0.0115974996
_diffrn_orient_matrix_UB_23      -0.0392797423
_diffrn_orient_matrix_UB_31      -0.0370909221
_diffrn_orient_matrix_UB_32      -0.0117360431
_diffrn_orient_matrix_UB_33      0.0207769237
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
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_exptl_absorpt_correction_T_min  0.64019
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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    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.069
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.16
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         17471
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.1
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1147P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.2181
_reflns_number_gt                10507
_reflns_number_total             17471
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic9019603_si_005.cif
_cod_data_source_block           gk229
_cod_original_cell_volume        3113.62(16)
_cod_original_sg_symbol_Hall     -P_2yn
_cod_database_code               4315275