Cobalt(III) Complexes of Monodentate N(9)-Bound Adeninate (ade-), [Co(ade-κN9)Cl(en)2]+ (en = 1,2-Diaminoethane): Syntheses, Crystal Structures, and Protonation Behaviors of the Geometrical Isomers
Takayoshi Suzuki; Yoko Hirai; Hideaki Monjushiro; Sumio Kaizaki; Inorganic Chemistry 43 (2004) 6435–6444; doi:10.1021/ic035336z

data_4311639
_publ_section_title
;
 Cobalt(III) Complexes of Monodentate N(9)-Bound Adeninate (ade-),
 [Co(ade-\kN9)Cl(en)2]+ (en = 1,2-Diaminoethane): Syntheses, Crystal
 Structures, and Protonation Behaviors of the Geometrical Isomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6435
_journal_page_last               6444
_journal_paper_doi               10.1021/ic035336z
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C9 H22 Cl Co N9 3+, 2(Cl 1-), B F4 1-, H2 O'
_chemical_formula_sum            'C9 H24 B Cl3 Co F4 N9 O'
_chemical_formula_weight         526.46
_chemical_name_systematic
; 
cis-(1H,7H-adeninium-\kN^9^)chlorobis(ethane-1,2-diamine)cobalt(III) 
Dichloride Tetrafluoroborate Hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.835(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.432(2)
_cell_length_b                   14.584(2)
_cell_length_c                   15.556(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     2077.7(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan ver. 1.11'
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6368
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0.52
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.618
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         6036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1180P)^2^+2.4091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.2043
_reflns_number_gt                3885
_reflns_number_total             6036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic035336zsi20040226_120107_3.cif
_cod_data_source_block           cis-3
_cod_original_cell_volume        2077.7(7)
_cod_database_code               4311639