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_1516868
_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
'P C24 H20 1+, C22 H28 Co N4 O4 1-, 1.5(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C49 H56.5 Co N5.5 O6 P'
_chemical_formula_weight         908.40
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.372(3)
_cell_angle_beta                 96.621(3)
_cell_angle_gamma                112.716(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5973(11)
_cell_length_b                   12.2755(11)
_cell_length_c                   18.0998(15)
_cell_measurement_reflns_used    15457
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2289.0(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-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    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku RAXIS-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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20579
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.8731
_exptl_absorpt_correction_T_min  0.8008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         10368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0510
_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^)+(0.1105P)^2^+1.1399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                9016
_reflns_number_total             10368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-399-131-137-2.cif
_cod_data_source_block           PPh4[1]_1.5CH3CN_2H2O
_cod_original_formula_sum        'C49 H56.50 Co N5.50 O6 P'
_cod_database_code               1516868