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_4069323
_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_sum            'C76 H130 Li2 N4 O5 Si2 Y2'
_chemical_formula_weight         1427.72
_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                 105.134(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.905(6)
_cell_length_b                   18.189(5)
_cell_length_c                   20.000(5)
_cell_measurement_reflns_used    3871
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      18.74
_cell_measurement_theta_min      2.36
_cell_volume                     7692(4)
_computing_cell_refinement       'Bruker SMART, (Bruker, 2004)'
_computing_data_collection       'Bruker SMART, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2004)'
_computing_molecular_graphics    SCHAKAL(Keller,1989),ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      108(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-AXS APEX- CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1448
_diffrn_reflns_av_sigmaI/netI    0.1250
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            80574
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.582
_exptl_absorpt_correction_T_max  0.7859
_exptl_absorpt_correction_T_min  0.7426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS;Sheldrick, 2004'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         7016
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0639P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                3875
_reflns_number_total             7016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9001389_si_001.cif
_cod_data_source_block           compound8
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4069323