Hydrogen-bonding interactions, geometrical selectivity and spectroscopic properties of cobalt(III) complexes with unsymmetrical tridentate amine-amidato-phenolato type ligands
Ryoji Mitsuhashi; Takayoshi Suzuki; Yukinari Sunatsuki; Masaaki Kojima; Inorganica Chimica Acta 399 (2013) 131–137; doi:

data_1516869
_publ_section_title
;
 Hydrogen-bonding interactions, geometrical selectivity and spectroscopic
 properties of cobalt(III) complexes with unsymmetrical tridentate
 amine-amidato-phenolato type ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              131
_journal_page_last               137
_journal_volume                  399
_journal_year                    2013
_chemical_formula_moiety
'K 1+, C20 H24 Co N4 O4 1-, 0.5(C H4 O), 4.5(H2 O)'
_chemical_formula_sum            'C20.5 H35 Co K N4 O9'
_chemical_formula_weight         579.55
_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
_cell_angle_alpha                104.694(4)
_cell_angle_beta                 110.228(4)
_cell_angle_gamma                103.872(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8385(12)
_cell_length_b                   11.9261(16)
_cell_length_c                   14.2124(18)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.13
_cell_volume                     1268.2(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'CrystalStructure 3.8'
_computing_molecular_graphics    'ortep-3 for win'
_computing_publication_material  SHELXL97
_computing_structure_refinement  SHELXL97
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12556
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.494
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0758P)^2^+1.9104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                5179
_reflns_number_total             5785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-399-131-137-3.cif
_cod_data_source_block           K[2]_0.5CH3OH_4.5H2O
_cod_original_formula_sum        'C20.50 H35 Co K N4 O9'
_cod_database_code               1516869