Synthesis and characterization of new Co(III) mixed-ligand complexes, containing 2-hydroxy-aryloximes and α-diimines. Crystal and molecular strucutre of [Co(saox)(bipy)~2~]Br
Maria Lalia-Kantouri; Christos D. Papadopoulos; Antonios G. Hatzidimitriou; Miguel Quirós; Polyhedron 26 (2007) 1292–1302; doi:10.1016/j.poly.2006.10.047

data_1500022
_publ_contact_author_address
;
     Departamento de Qu\'imica Inorg\'anica
     Facultad de Ciencias
     Universidad de Granada
     18071 Granada
     SPAIN
;
_publ_contact_author_email       mquiros@ugr.es
_publ_contact_author_fax         34-58-248526
_publ_contact_author_name        'Miguel Quir\'os'
_publ_contact_author_phone       34-58-240441
_publ_section_title
;
 Synthesis and characterization of new Co(III) mixed-ligand complexes,
 containing 2-hydroxy-aryloximes and \a-diimines. Crystal and molecular
 strucutre of [Co(saox)(bipy)~2~]Br
;
_journal_name_full               Polyhedron
_journal_page_first              1292
_journal_page_last               1302
_journal_paper_doi               10.1016/j.poly.2006.10.047
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C28.81 H26.43 Br Co N5.33 O3.9'
_chemical_formula_weight         648.87
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-07-06
_audit_creation_method           CRYSTALS_ver_12.83
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.7483(10)
_cell_length_b                   36.829(2)
_cell_length_c                   17.3196(10)
_cell_measurement_reflns_used    6423
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.33
_cell_volume                     11320.9(11)
_computing_cell_refinement       'Bruker SMART (Bruker, 1999)'
_computing_data_collection       'Bruker SMART (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69254
_diffrn_reflns_theta_full        26.919
_diffrn_reflns_theta_max         28.336
_diffrn_reflns_theta_min         1.106
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.07
_diffrn_standards_number         767
_exptl_absorpt_coefficient_mu    2.062
_exptl_absorpt_correction_T_max  0.8522
_exptl_absorpt_correction_T_min  0.4232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       laminae
_exptl_crystal_F_000             5277.647
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.80
_refine_diff_density_min         -1.59
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0498
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         8040
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.000604
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 9.68 13.3 4.23 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0870
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0728
_reflns_limit_h_max              23
_reflns_limit_h_min              0
_reflns_limit_k_max              49
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                8040
_reflns_number_total             13502
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            teloxime4.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_formula_sum        'C28.81 H26.43 Br Co N5.33 O3.90'
_cod_database_code               1500022