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_4315273
_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 H39 Co N7S, 1.375(Cl O4), 1.625(Cl), H2 O'
_chemical_formula_sum            'C20 H41 Cl3 Co N7 O6.5 S'
_chemical_formula_weight         680.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-08-25T13:56:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.8880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.3458(2)
_cell_length_b                   22.6817(3)
_cell_length_c                   18.2093(2)
_cell_measurement_reflns_used    63564
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.9197
_cell_measurement_theta_min      2.5788
_cell_volume                     5917.55(13)
_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
;
        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, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
 Oxford Diffraction Xcalibur diffractometer

;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.01774473
_diffrn_orient_matrix_UB_12      0.0241098767
_diffrn_orient_matrix_UB_13      -0.0213053526
_diffrn_orient_matrix_UB_21      0.0412339087
_diffrn_orient_matrix_UB_22      0.000203448
_diffrn_orient_matrix_UB_23      -0.019942836
_diffrn_orient_matrix_UB_31      -0.0210497947
_diffrn_orient_matrix_UB_32      -0.0199527138
_diffrn_orient_matrix_UB_33      -0.0259518917
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.052
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            201121
_diffrn_reflns_theta_full        35
_diffrn_reflns_theta_max         35
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.87572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
        (compiled Apr 27 2007,17:53:11)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.67
_refine_diff_density_min         -1.591
_refine_diff_density_rms         0.15
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         26026
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1204P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.176
_refine_ls_wR_factor_ref         0.2009
_reflns_number_gt                16521
_reflns_number_total             26026
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic9019603_si_003.cif
_cod_data_source_block           gk219
_cod_original_sg_symbol_Hall     -P_2yn
_cod_original_formula_sum        'C20 H41 Cl3 Co N7 O6.50 S'
_cod_database_code               4315273