Ti and Zr bidentate bis-phosphinimide complexes
Hollink, Emily; Stewart, Jeffrey C.; Wei, Pingrong; Stephan, Douglas W.; Dalton Transactions  (2003) 3968–; doi:10.1039/b308114a

data_7013445
_publ_section_title
;
 Ti and Zr bidentate bis-phosphinimide complexes
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              3968
_journal_paper_doi               10.1039/b308114a
_journal_year                    2003
_chemical_formula_sum            'C36 H64 N4 P2 Ti'
_chemical_formula_weight         662.75
_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                102.835(11)
_cell_angle_beta                 93.060(12)
_cell_angle_gamma                90.686(12)
_cell_formula_units_Z            2
_cell_length_a                   8.726(5)
_cell_length_b                   12.389(8)
_cell_length_c                   18.381(11)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     1934(2)
_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_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8246
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.256568
_exptl_absorpt_correction_T_min  0.167631
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1975
_refine_ls_wR_factor_ref         0.2154
_reflns_number_gt                3079
_reflns_number_total             5491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b308114a.txt
_cod_data_source_block           m-C6H4(CH2(Cy2)PN)2Ti(NMe2)2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7013445