Titanium and Zirconium Benzyl Complexes Bearing Bulky Bis(amido)cyclodiphosph(III)azanes: Synthesis, Structure, Activation, and Ethene Polymerization Studies
Axenov, Kirill V.; Kilpeläinen, Ilkka; Klinga, Martti; Leskelä, Markku; Repo, Timo; Organometallics 25 (2006) 463–; doi:10.1021/om050725h

data_4074660
_publ_section_title
;
 Titanium and Zirconium Benzyl Complexes Bearing Bulky
 Bis(amido)cyclodiphosph(III)azanes:&#x00A0; Synthesis, Structure,
 Activation, and Ethene Polymerization Studies
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              463
_journal_paper_doi               10.1021/om050725h
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C27 H53 N4 O P2 Zr, C25 H7 B F15'
_chemical_formula_sum            'C52 H60 B F15 N4 O P2 Zr'
_chemical_formula_weight         1206.01
_chemical_name_systematic
; 
[N,N'-1,3-tetrakis(1,1-dimethylethyl)-
1,3,2,4-diazadiphosphetidine-2,4-diaminato(2-)-\kN2,\kN4]
[1,1-oxybis(ethane)]phenylmethylzirconium(1+)
tetrakis(pentafluorophenyl)borate(1-)
;
_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                 100.66(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.870(1)
_cell_length_b                   33.707(3)
_cell_length_c                   15.506(1)
_cell_measurement_temperature    173(2)
_cell_volume                     5583.3(8)
_computing_cell_refinement       'COLLECT (Nonius, 2002)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction        'COLLECT (Nonius, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- and omega-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  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57532
_diffrn_reflns_theta_full        25.53
_diffrn_reflns_theta_max         25.53
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.345
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10263
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0500P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                6898
_reflns_number_total             10263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050725hsi20050822_073745.cif
_cod_data_source_block           axi503
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4074660