Cobalt(III) complexes with tridentate hydrazone ligands: protonation state and hydrogen bonds competition
Vrdoljak, Visnja; Pavlović, Gordana; Hrenar, Tomica; Rubčić, Mirta; Siega, Patrizia; Dreos, Renata; Cindric, Marina; RSC Adv.  (2015) –; doi:10.1039/C5RA22068H

data_7223392
_publ_section_title
;
 Cobalt(III) complexes with tridentate hydrazone ligands: protonation
 state and hydrogen bonds competition
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA22068H
_journal_year                    2015
_chemical_formula_moiety         'C30.72 H25 Co N4 O8.72'
_chemical_formula_sum            'C30.72 H25 Co N4 O8.72'
_chemical_formula_weight         648.64
_chemical_name_systematic
;
(2-oxy-3-methoxybenzaldehyde 4-hydroxybenzoylhydrazonato-O,N,O)
(2-oxy-3-methoxybenzaldehyde 4-hydroxybenzoylhydrazidato-O,N,O)
cobalt(III) methanol solvate (1/0.7)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-10-21 deposited with the CCDC.
2015-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                102.995(6)
_cell_angle_beta                 107.619(5)
_cell_angle_gamma                96.756(6)
_cell_formula_units_Z            2
_cell_length_a                   10.1424(6)
_cell_length_b                   12.2350(10)
_cell_length_c                   13.1652(8)
_cell_measurement_reflns_used    1665
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.9080
_cell_measurement_theta_min      4.2910
_cell_volume                     1486.54(19)
_computing_cell_refinement
'CrysAlisPro, Agilent  Technologies, Version 1.171.36.28'
_computing_data_collection
'CrysAlisPro, Agilent  Technologies, Version 1.171.36.28'
_computing_data_reduction
'CrysAlisPro, Agilent  Technologies, Version 1.171.36.28'
_computing_molecular_graphics    'MERCURY 3.3. (CCDC, 2013)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.1497
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13542
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         4.116
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35.
Empirical absorption correction using spherical 
harmonics,implemented in SCALE3 ABSPACK 
scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6447
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.0910
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3899
_reflns_number_total             6447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra22068h2.cif
_cod_data_source_block           2(150)
_cod_original_cell_volume        1486.54(18)
_cod_database_code               7223392
_shelxl_version_number           2014-3
_shelx_res_checksum              17538