Temperature-Induced Solid-State Valence Tautomeric Interconversion in Two Cobalt-Schiff Base Diquinone Complexes
Olivier Cador; Françoise Chabre; Andrea Dei; Claudio Sangregorio; Joris Van Slageren; Maria G. F. Vaz; Inorganic Chemistry 42 (2003) 6432–6440; doi:10.1021/ic034210z

data_4314345
_publ_contact_author_address
;
 Dipartimento di Chimica, Universita' di Firenze, via della Lastruccia 3,
 50019 Sesto F.no (FI), Italy
;
_publ_contact_author_email       andrea.dei@unifi.it
_publ_contact_author_fax         +39-0554573372
_publ_contact_author_name        'Dei, A.'
_publ_section_title
;
 Temperature-Induced Solid-State Valence Tautomeric Interconversion in Two
 Cobalt-Schiff Base Diquinone Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6432
_journal_page_last               6440
_journal_paper_doi               10.1021/ic034210z
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C67 H71 B Co N4 O2'
_chemical_formula_weight         1034.02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           34
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(2)
_cell_angle_beta                 90.000(2)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            8
_cell_length_a                   41.396(2)
_cell_length_b                   14.383(1)
_cell_length_c                   20.626(1)
_cell_measurement_reflns_used    8532
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.453
_cell_measurement_theta_min      2.34
_cell_volume                     12280.7(12)
_computing_cell_refinement       'Bruker-Smart-NT V5.6'
_computing_data_collection       'Bruker-Smart-NT V5.6'
_computing_data_reduction        'Bruker-Saint V6.02A'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD-1K 3 circles Bruker diffractometer'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  'gobbel mirrors'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_sigmaI/netI    0.1050
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27821
_diffrn_reflns_theta_full        50.49
_diffrn_reflns_theta_max         50.49
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    2.528
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.538987
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.299(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1321
_refine_ls_number_reflns         11803
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                7465
_reflns_number_total             11803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034210zsi20030225_115629.cif
_cod_data_source_block           cotpyrt
_cod_original_cell_volume        12281(1)
_cod_database_code               4314345