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_4082376
_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'
_chemical_formula_sum            'C24 H27 Cl Co N3 O7'
_chemical_formula_weight         563.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.8500(18)
_cell_length_b                   16.2010(11)
_cell_length_c                   12.761(9)
_cell_measurement_temperature    100(2)
_cell_volume                     4931(4)
_computing_cell_refinement       'Denzo (Otwinowski & Minor 1997)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'thick slices'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.00000
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20493
_diffrn_reflns_theta_full        29.66
_diffrn_reflns_theta_max         29.66
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    2.090
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.0142(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         2463
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+5.4829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                2235
_reflns_number_total             2464
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om401038v_si_002.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               4082376