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_7013448
_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            'C32 H52 Cl2 N2 P2 Ti'
_chemical_formula_weight         645.50
_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                 101.95(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.472(14)
_cell_length_b                   17.37(2)
_cell_length_c                   17.70(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3451(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.2252
_diffrn_reflns_av_sigmaI/netI    0.1787
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14456
_diffrn_reflns_theta_full        23.55
_diffrn_reflns_theta_max         23.55
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  0.256597
_exptl_absorpt_correction_T_min  0.036188
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.2322
_refine_ls_R_factor_gt           0.1585
_refine_ls_shift/su_max          0.083
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1848P)^2^+31.0840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3607
_refine_ls_wR_factor_ref         0.4106
_reflns_number_gt                2608
_reflns_number_total             4995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b308114a.txt
_cod_data_source_block           m-C6H4(CH2PCy2))2TiCl2
_cod_original_cell_volume        3452(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7013448