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_4068989
_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         '(C47 H77 N3 P2 Si Zr)(C5H12)'
_chemical_formula_sum            'C52 H89 N3 P2 Si Zr'
_chemical_formula_weight         937.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 115.02
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.455
_cell_length_b                   18.696
_cell_length_c                   16.811
_cell_measurement_reflns_used    10353
_cell_measurement_temperature    151(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      3.4
_cell_volume                     5256.072
_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      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22057
_diffrn_reflns_theta_full        24.12
_diffrn_reflns_theta_max         24.12
_diffrn_reflns_theta_min         3.42
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         8241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                5725
_reflns_number_total             8241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8011932_si_002.cif
_cod_data_source_block           wac4155
_cod_original_cell_volume        5255.9
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4068989