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_7013444
_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            'C24 H46 N2 P2'
_chemical_formula_weight         424.57
_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                 108.388(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.457(8)
_cell_length_b                   13.908(8)
_cell_length_c                   14.713(8)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     2613(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10896
_diffrn_reflns_theta_full        23.17
_diffrn_reflns_theta_max         23.17
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.488950
_exptl_absorpt_correction_T_min  0.321773
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                2709
_reflns_number_total             3714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b308114a.txt
_cod_data_source_block           m-C6H4(CH2(t-Bu2)PNH)2
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7013444