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_4068990
_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         'C25 H60 N2 P2 Si Zr'
_chemical_formula_sum            'C25 H60 N2 P2 Si Zr'
_chemical_formula_weight         570.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                94.477(3)
_cell_angle_beta                 96.876(3)
_cell_angle_gamma                111.824(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0482(17)
_cell_length_b                   9.626(2)
_cell_length_c                   23.012(5)
_cell_measurement_reflns_used    3734
_cell_measurement_temperature    155(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      3.3
_cell_volume                     1628.5(6)
_computing_cell_refinement       'Bruker SAINT v7.07'
_computing_data_collection       'Bruker SMART v5.054d'
_computing_data_reduction        'Bruker SAINT v7.07'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      155(2)
_diffrn_measured_fraction_theta_full 0.882
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'SMART 1000'
_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  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8844
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade-like
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                4833
_reflns_number_total             5854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8011932_si_003.cif
_cod_data_source_block           wac5100xs
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068990