A Novel Series of CoIII(salen-type) Complexes Containing a Seven-Membered Metallacycle: Synthesis, Structural Characterization and Factors Affecting the Metallacyclization Rate
Siega, Patrizia; Dreos, Renata; Brancatelli, Giovanna; Zangrando, Ennio; Tavagnacco, Claudio; Vrdoljak, Višnja; Hrenar, Tomica; Organometallics 33 (2014) 909–; doi:10.1021/om401038v

data_4082375
_publ_section_title
;
 A Novel Series of CoIII(salen-type) Complexes Containing a Seven-Membered
 Metallacycle: Synthesis, Structural Characterization and Factors
 Affecting the Metallacyclization Rate
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              909
_journal_paper_doi               10.1021/om401038v
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C38 H40 Cl2 Co2 N4 O4'
_chemical_formula_sum            'C38 H40 Cl2 Co2 N4 O4'
_chemical_formula_weight         805.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.917(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.932(2)
_cell_length_b                   12.407(2)
_cell_length_c                   13.1250(13)
_cell_measurement_temperature    293(2)
_cell_volume                     1727.9(5)
_computing_cell_refinement       'Denzo (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius, Supergui'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep3 for Windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.80.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELX97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16174
_diffrn_reflns_theta_full        63.72
_diffrn_reflns_theta_max         63.72
_diffrn_reflns_theta_min         4.74
_exptl_absorpt_coefficient_mu    9.333
_exptl_absorpt_correction_T_max  0.1174
_exptl_absorpt_correction_T_min  0.0545
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0655
_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^)+(0.1376P)^2^+0.4430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1860
_reflns_number_gt                2230
_reflns_number_total             2817
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om401038v_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4082375