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_4082377
_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         'C24 H27 Co N3 O3, Cl O4, 1.5(C H Cl3)'
_chemical_formula_sum            'C25.5 H28.5 Cl5.5 Co N3 O7'
_chemical_formula_weight         742.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 94.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.993(3)
_cell_length_b                   12.989(3)
_cell_length_c                   24.117(3)
_cell_measurement_temperature    293(2)
_cell_volume                     6242.0(19)
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37581
_diffrn_reflns_theta_full        63.73
_diffrn_reflns_theta_max         63.73
_diffrn_reflns_theta_min         4.06
_exptl_absorpt_coefficient_mu    9.058
_exptl_absorpt_correction_T_max  0.1344
_exptl_absorpt_correction_T_min  0.0804
_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            orange
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4990
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1973
_reflns_number_gt                3371
_reflns_number_total             4990
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om401038v_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C25.50 H28.50 Cl5.50 Co N3 O7'
_cod_database_code               4082377