Diamine Bis(phenolate) M(III) (Y, Ti) Complexes: Synthesis, Structures, and Reactivity
Barroso, Sónia; Cui, Jinlan; Carretas, José Manuel; Cruz, Adelaide; Santos, Isabel C.; Duarte, M. Teresa; Telo, João P.; Marques, Noémia; Martins, Ana M.; Organometallics 28 (2009) 3449–; doi:10.1021/om9001389

data_4069316
_publ_section_title
;
 Diamine Bis(phenolate) M(III) (Y, Ti) Complexes: Synthesis, Structures,
 and Reactivity
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3449
_journal_paper_doi               10.1021/om9001389
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C38 H62 Cl N2 O3 Ti, 1.5(C4 H10 O)'
_chemical_formula_sum            'C44 H77 Cl N2 O4.5 Ti'
_chemical_formula_weight         789.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.657(4)
_cell_angle_beta                 90.273(5)
_cell_angle_gamma                90.228(4)
_cell_formula_units_Z            4
_cell_length_a                   9.7830(12)
_cell_length_b                   17.268(2)
_cell_length_c                   27.901(4)
_cell_measurement_reflns_used    17155
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      1.18
_cell_volume                     4697.7(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick,1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            49190
_diffrn_reflns_theta_full        25.58
_diffrn_reflns_theta_max         25.58
_diffrn_reflns_theta_min         1.18
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.9463
_exptl_absorpt_correction_T_min  0.7873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         1.682
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0107(8)
_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   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         17155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.0894
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+15.0078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2351
_refine_ls_wR_factor_ref         0.2496
_reflns_number_gt                11407
_reflns_number_total             17155
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om9001389_si_001.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        4697.7(11)
_cod_depositor_comments
;

2025-11-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C88 H154 Cl2 N4 O9 Ti2'
_cod_original_formula_weight         1578.85
_cod_original_formula_moiety         '2(C38 H62 Cl N2 O3 Ti), 3(C4 H10 O)'
_cod_original_formula_units_Z            2
_cod_database_code               4069316