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_4068988
_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         '(C22 H51 Cl2 N2 P2 Si Zr)(C5H12)'
_chemical_formula_sum            'C27 H63 Cl2 N2 P2 Si Zr'
_chemical_formula_weight         667.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.4150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0595(12)
_cell_length_b                   25.137(3)
_cell_length_c                   13.1081(14)
_cell_measurement_reflns_used    6513
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      3.4
_cell_volume                     3643.0(7)
_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      112(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17454
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         3.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         7042
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                5636
_reflns_number_total             7042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8011932_si_001.cif
_cod_data_source_block           wac4008xs
_cod_original_cell_volume        3642.9(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4068988