Synthesis and Reactivity of Titanium and Zirconium Complexes Supported by a Multidentate Monoanionic [N2P2] Ligand
Chomitz, Wayne A.; Sutton, Andrew D.; Krinsky, Jamin L.; Arnold, John; Organometallics 28 (2009) 3338–; doi:10.1021/om8011932

data_4068992
_publ_section_title
;
 Synthesis and Reactivity of Titanium and Zirconium Complexes Supported by
 a Multidentate Monoanionic [N2P2] Ligand
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3338
_journal_paper_doi               10.1021/om8011932
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C26 H60 Cl N3 P2 Si Ti'
_chemical_formula_sum            'C26 H60 Cl N3 P2 Si Ti'
_chemical_formula_weight         588.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                   18.935(3)
_cell_length_b                   17.017(2)
_cell_length_c                   21.658(3)
_cell_measurement_reflns_used    5221
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      21.2
_cell_measurement_theta_min      2.2
_cell_volume                     6978.6(17)
_computing_cell_refinement       'Bruker SAINT v7.07'
_computing_data_collection       'Bruker SMART v5.631'
_computing_data_reduction        'Bruker SAINT v7.07'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scans'
_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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31515
_diffrn_reflns_theta_full        23.83
_diffrn_reflns_theta_max         23.83
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         10000
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                7887
_reflns_number_total             10000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8011932_si_005.cif
_cod_data_source_block           wac7207xs
_cod_original_cell_volume        6979.0(17)
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               4068992