# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Douglas W Stephan'
_publ_contact_author_email       DSTEPHAN@CHEM.UTORONTO.CA

_publ_section_title              
;
Titanium Complexes of Amidophosphinimide Ligands
;
loop_
_publ_author_name
'Douglas W Stephan'
'Osama Alhomaidan'
'Guangcai Bai'
'Chad Beddie'

# Attachment 'CIF.CIF'

data_MeC(CH2NMe)3PNTiCpMe2
_database_code_depnum_ccdc_archive 'CCDC 702181'
_audit_creation_method           SHELXL-97
_chemical_formula_sum            'C15 H29 N4 P Ti'
_chemical_formula_weight         344.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.0818(19)
_cell_length_b                   21.565(6)
_cell_length_c                   8.0593(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.569(14)
_cell_angle_gamma                90.00
_cell_volume                     1899.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      25.0
_exptl_crystal_description       blocks
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.150200
_exptl_absorpt_correction_T_max  0.262695
_diffrn_measurement_device_type  'Bruker SMART system'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_number            9474
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3303
_reflns_number_gt                2627
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3303
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1701
_refine_ls_wR_factor_gt          0.1577
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.65119(4) 0.10385(2) 0.68929(7) 0.0535(2) Uani 1 1 d . . .
P1 P 0.93509(6) 0.13907(3) 0.87430(8) 0.0443(2) Uani 1 1 d . . .
N1 N 0.8066(2) 0.12491(12) 0.7709(3) 0.0614(6) Uani 1 1 d . . .
N2 N 0.9570(2) 0.11851(12) 1.0760(3) 0.0611(7) Uani 1 1 d . . .
N3 N 0.9751(2) 0.21310(11) 0.8845(3) 0.0600(6) Uani 1 1 d . . .
N4 N 1.0504(2) 0.10435(13) 0.8047(3) 0.0635(7) Uani 1 1 d . . .
C1 C 0.5219(8) 0.0999(4) 0.8956(11) 0.143(3) Uani 1 1 d . . .
H1A H 0.5337 0.0722 0.9933 0.172 Uiso 1 1 calc R . .
C2 C 0.5650(6) 0.1571(5) 0.8955(10) 0.131(2) Uani 1 1 d . . .
H2A H 0.6125 0.1776 0.9937 0.158 Uiso 1 1 calc R . .
C3 C 0.5250(7) 0.1846(3) 0.7536(14) 0.138(2) Uani 1 1 d . . .
H3A H 0.5343 0.2287 0.7290 0.166 Uiso 1 1 calc R . .
C4 C 0.4454(7) 0.1413(7) 0.6522(9) 0.177(4) Uani 1 1 d . . .
H4A H 0.3908 0.1496 0.5459 0.213 Uiso 1 1 calc R . .
C5 C 0.4509(6) 0.0877(4) 0.7501(14) 0.153(3) Uani 1 1 d . . .
H5A H 0.4010 0.0504 0.7234 0.183 Uiso 1 1 calc R . .
C6 C 0.6353(4) 0.1211(2) 0.4250(5) 0.0924(12) Uani 1 1 d . . .
H6A H 0.6287 0.1649 0.4045 0.139 Uiso 1 1 calc R . .
H6B H 0.5637 0.1007 0.3665 0.139 Uiso 1 1 calc R . .
H6C H 0.7065 0.1054 0.3854 0.139 Uiso 1 1 calc R . .
C7 C 0.6638(4) 0.0057(2) 0.6876(7) 0.120(2) Uani 1 1 d . . .
H7A H 0.6716 -0.0096 0.8007 0.180 Uiso 1 1 calc R . .
H7B H 0.7342 -0.0064 0.6402 0.180 Uiso 1 1 calc R . .
H7C H 0.5914 -0.0112 0.6211 0.180 Uiso 1 1 calc R . .
C8 C 1.2869(3) 0.17701(18) 1.1462(5) 0.0815(10) Uani 1 1 d . . .
H8A H 1.3296 0.1387 1.1748 0.122 Uiso 1 1 calc R . .
H8B H 1.2795 0.1992 1.2472 0.122 Uiso 1 1 calc R . .
H8C H 1.3317 0.2017 1.0781 0.122 Uiso 1 1 calc R . .
C9 C 1.1583(3) 0.16313(13) 1.0471(4) 0.0535(7) Uani 1 1 d . . .
C10 C 1.0853(3) 0.12400(16) 1.1549(4) 0.0638(8) Uani 1 1 d . . .
H10A H 1.1213 0.0830 1.1706 0.077 Uiso 1 1 calc R . .
H10B H 1.0899 0.1430 1.2648 0.077 Uiso 1 1 calc R . .
C11 C 0.8947(3) 0.06450(14) 1.1291(5) 0.0754(9) Uani 1 1 d . . .
H11A H 0.8114 0.0640 1.0723 0.113 Uiso 1 1 calc R . .
H11B H 0.8962 0.0663 1.2485 0.113 Uiso 1 1 calc R . .
H11C H 0.9355 0.0275 1.1018 0.113 Uiso 1 1 calc R . .
C12 C 1.1700(3) 0.12737(17) 0.8869(4) 0.0669(8) Uani 1 1 d . . .
H12A H 1.2041 0.1543 0.8102 0.080 Uiso 1 1 calc R . .
H12B H 1.2254 0.0927 0.9147 0.080 Uiso 1 1 calc R . .
C13 C 1.0430(4) 0.08891(16) 0.6285(4) 0.0740(10) Uani 1 1 d . . .
H13A H 0.9621 0.0744 0.5846 0.111 Uiso 1 1 calc R . .
H13B H 1.1014 0.0570 0.6166 0.111 Uiso 1 1 calc R . .
H13C H 1.0607 0.1251 0.5673 0.111 Uiso 1 1 calc R . .
C14 C 1.0902(3) 0.22367(13) 1.0012(4) 0.0608(7) Uani 1 1 d . . .
H14A H 1.0726 0.2434 1.1027 0.073 Uiso 1 1 calc R . .
H14B H 1.1419 0.2515 0.9493 0.073 Uiso 1 1 calc R . .
C15 C 0.8823(3) 0.26097(13) 0.8880(4) 0.0608(7) Uani 1 1 d . . .
H15B H 0.8104 0.2507 0.8088 0.091 Uiso 1 1 calc R . .
H15A H 0.9137 0.3002 0.8584 0.091 Uiso 1 1 calc R . .
H15C H 0.8619 0.2635 0.9990 0.091 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0402(4) 0.0603(4) 0.0596(4) -0.0045(2) 0.0074(2) 0.0015(2)
P1 0.0428(4) 0.0483(4) 0.0415(4) -0.0023(3) 0.0062(3) 0.0009(3)
N1 0.0498(15) 0.0679(15) 0.0635(16) -0.0070(13) 0.0010(12) -0.0020(12)
N2 0.0590(16) 0.0703(15) 0.0549(15) 0.0105(12) 0.0119(12) -0.0068(12)
N3 0.0549(14) 0.0516(13) 0.0684(16) -0.0008(11) -0.0052(12) 0.0027(10)
N4 0.0566(16) 0.0849(18) 0.0501(14) -0.0181(12) 0.0122(12) 0.0033(12)
C1 0.130(6) 0.182(7) 0.141(6) 0.035(5) 0.091(5) 0.024(5)
C2 0.102(4) 0.186(7) 0.117(5) -0.053(5) 0.052(4) 0.020(5)
C3 0.134(6) 0.121(4) 0.174(7) 0.001(5) 0.064(5) 0.069(4)
C4 0.085(4) 0.347(13) 0.100(4) 0.005(7) 0.014(4) 0.129(6)
C5 0.059(3) 0.229(9) 0.179(7) -0.058(7) 0.046(4) -0.029(4)
C6 0.065(2) 0.142(4) 0.067(2) 0.007(2) -0.0008(18) -0.025(2)
C7 0.077(3) 0.072(3) 0.196(6) -0.007(3) -0.019(3) -0.0047(19)
C8 0.0522(19) 0.103(3) 0.083(2) -0.009(2) -0.0079(17) 0.0024(17)
C9 0.0421(15) 0.0662(16) 0.0508(16) -0.0034(13) 0.0037(12) 0.0039(12)
C10 0.0614(19) 0.0773(19) 0.0502(16) 0.0123(15) 0.0025(14) 0.0092(15)
C11 0.088(3) 0.070(2) 0.073(2) 0.0162(16) 0.0290(19) -0.0060(17)
C12 0.0487(18) 0.088(2) 0.066(2) -0.0073(17) 0.0149(15) 0.0094(15)
C13 0.099(3) 0.077(2) 0.0500(18) -0.0079(15) 0.0250(18) 0.0138(18)
C14 0.0565(17) 0.0591(16) 0.0624(18) -0.0052(13) -0.0030(14) -0.0063(13)
C15 0.0589(18) 0.0535(16) 0.0703(19) 0.0042(14) 0.0120(15) 0.0106(13)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N1 1.797(3) . ?
Ti1 C7 2.121(4) . ?
Ti1 C6 2.141(4) . ?
Ti1 C3 2.345(4) . ?
Ti1 C2 2.350(5) . ?
Ti1 C1 2.370(5) . ?
Ti1 C5 2.377(5) . ?
Ti1 C4 2.391(5) . ?
P1 N1 1.556(3) . ?
P1 N3 1.655(2) . ?
P1 N4 1.658(3) . ?
P1 N2 1.663(2) . ?
N2 C11 1.454(4) . ?
N2 C10 1.462(4) . ?
N3 C15 1.460(4) . ?
N3 C14 1.472(4) . ?
N4 C13 1.448(4) . ?
N4 C12 1.466(4) . ?
C1 C2 1.323(9) . ?
C1 C5 1.326(10) . ?
C2 C3 1.298(9) . ?
C3 C4 1.441(11) . ?
C4 C5 1.395(10) . ?
C8 C9 1.543(4) . ?
C9 C14 1.522(4) . ?
C9 C12 1.528(4) . ?
C9 C10 1.534(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ti1 C7 101.20(13) . . ?
N1 Ti1 C6 103.60(14) . . ?
C7 Ti1 C6 99.3(2) . . ?
N1 Ti1 C3 107.6(3) . . ?
C7 Ti1 C3 141.7(2) . . ?
C6 Ti1 C3 97.9(3) . . ?
N1 Ti1 C2 95.5(2) . . ?
C7 Ti1 C2 121.8(3) . . ?
C6 Ti1 C2 130.0(3) . . ?
C3 Ti1 C2 32.1(2) . . ?
N1 Ti1 C1 114.0(3) . . ?
C7 Ti1 C1 91.0(3) . . ?
C6 Ti1 C1 138.2(3) . . ?
C3 Ti1 C1 54.5(2) . . ?
C2 Ti1 C1 32.6(2) . . ?
N1 Ti1 C5 146.4(3) . . ?
C7 Ti1 C5 85.4(3) . . ?
C6 Ti1 C5 107.8(3) . . ?
C3 Ti1 C5 56.7(3) . . ?
C2 Ti1 C5 54.7(2) . . ?
C1 Ti1 C5 32.4(2) . . ?
N1 Ti1 C4 142.8(4) . . ?
C7 Ti1 C4 113.5(4) . . ?
C6 Ti1 C4 84.2(2) . . ?
C3 Ti1 C4 35.4(3) . . ?
C2 Ti1 C4 55.4(2) . . ?
C1 Ti1 C4 54.9(2) . . ?
C5 Ti1 C4 34.0(3) . . ?
N1 P1 N3 115.44(13) . . ?
N1 P1 N4 114.73(14) . . ?
N3 P1 N4 103.73(14) . . ?
N1 P1 N2 116.32(14) . . ?
N3 P1 N2 102.36(13) . . ?
N4 P1 N2 102.40(14) . . ?
P1 N1 Ti1 169.05(19) . . ?
C11 N2 C10 114.3(2) . . ?
C11 N2 P1 120.1(2) . . ?
C10 N2 P1 112.15(19) . . ?
C15 N3 C14 114.6(2) . . ?
C15 N3 P1 120.0(2) . . ?
C14 N3 P1 112.19(18) . . ?
C13 N4 C12 114.9(3) . . ?
C13 N4 P1 121.0(2) . . ?
C12 N4 P1 112.56(19) . . ?
C2 C1 C5 110.2(8) . . ?
C2 C1 Ti1 72.9(3) . . ?
C5 C1 Ti1 74.1(4) . . ?
C3 C2 C1 110.8(7) . . ?
C3 C2 Ti1 73.7(3) . . ?
C1 C2 Ti1 74.5(3) . . ?
C2 C3 C4 106.9(7) . . ?
C2 C3 Ti1 74.1(3) . . ?
C4 C3 Ti1 74.0(3) . . ?
C5 C4 C3 104.5(6) . . ?
C5 C4 Ti1 72.5(3) . . ?
C3 C4 Ti1 70.6(3) . . ?
C1 C5 C4 107.4(8) . . ?
C1 C5 Ti1 73.5(3) . . ?
C4 C5 Ti1 73.5(3) . . ?
C14 C9 C12 109.6(3) . . ?
C14 C9 C10 108.8(2) . . ?
C12 C9 C10 109.1(3) . . ?
C14 C9 C8 109.7(2) . . ?
C12 C9 C8 109.5(3) . . ?
C10 C9 C8 110.0(3) . . ?
N2 C10 C9 111.4(2) . . ?
N4 C12 C9 110.9(2) . . ?
N3 C14 C9 111.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.052
#===end
data_[(CH2(Me)NP(tBu2)N)2]Ti(NMe2)2
_database_code_depnum_ccdc_archive 'CCDC 702182'
_audit_creation_method           SHELXL-97
_chemical_formula_sum            'C28 H66 N6 P2 Ti'
_chemical_formula_weight         596.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.458(3)
_cell_length_b                   11.1731(18)
_cell_length_c                   17.430(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.535(2)
_cell_angle_gamma                90.00
_cell_volume                     3591.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      25.0
_exptl_crystal_description       blocks
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.660029
_exptl_absorpt_correction_T_max  1.000000
_diffrn_measurement_device_type  'Bruker SMART system'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_number            33574
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6340
_reflns_number_gt                4665
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1405P)^2^+3.7775P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6340
_refine_ls_number_parameters     343
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0616
_refine_ls_wR_factor_ref         0.2003
_refine_ls_wR_factor_gt          0.1730
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.22678(3) 0.02101(5) 0.42334(3) 0.0443(2) Uani 1 1 d . . .
P1 P 0.34651(5) -0.00351(8) 0.28514(6) 0.0546(3) Uani 1 1 d . . .
P2 P 0.11918(5) -0.21480(8) 0.38422(5) 0.0505(3) Uani 1 1 d . . .
N1 N 0.30361(16) 0.0103(2) 0.35935(17) 0.0537(7) Uani 1 1 d . . .
N2 N 0.15598(14) -0.0920(3) 0.40139(16) 0.0542(7) Uani 1 1 d . . .
N3 N 0.32728(18) -0.1348(3) 0.24233(19) 0.0722(9) Uani 1 1 d . . .
N4 N 0.16212(19) -0.2873(3) 0.3150(2) 0.0712(9) Uani 1 1 d . . .
N5 N 0.26687(17) 0.0091(3) 0.52700(17) 0.0624(8) Uani 1 1 d . . .
N6 N 0.18302(17) 0.1771(3) 0.4194(2) 0.0665(8) Uani 1 1 d . . .
C1 C 0.3220(2) 0.1189(4) 0.2153(2) 0.0779(12) Uani 1 1 d . . .
C2 C 0.3605(4) 0.1201(7) 0.1398(4) 0.156(3) Uani 1 1 d . . .
H2B H 0.3435 0.1867 0.1092 0.235 Uiso 1 1 calc R . .
H2C H 0.3504 0.0469 0.1125 0.235 Uiso 1 1 calc R . .
H2D H 0.4118 0.1274 0.1501 0.235 Uiso 1 1 calc R . .
C3 C 0.2409(3) 0.1030(6) 0.1948(3) 0.118(2) Uani 1 1 d . . .
H3A H 0.2252 0.1638 0.1589 0.177 Uiso 1 1 calc R . .
H3B H 0.2140 0.1096 0.2405 0.177 Uiso 1 1 calc R . .
H3C H 0.2328 0.0255 0.1722 0.177 Uiso 1 1 calc R . .
C4 C 0.3334(4) 0.2368(5) 0.2552(4) 0.137(3) Uani 1 1 d . . .
H4A H 0.3210 0.3007 0.2201 0.205 Uiso 1 1 calc R . .
H4B H 0.3833 0.2442 0.2724 0.205 Uiso 1 1 calc R . .
H4C H 0.3031 0.2411 0.2985 0.205 Uiso 1 1 calc R . .
C5 C 0.4459(2) -0.0065(4) 0.3127(3) 0.0748(12) Uani 1 1 d . . .
C6 C 0.4637(2) 0.0992(5) 0.3655(3) 0.0977(16) Uani 1 1 d . . .
H6A H 0.5145 0.0984 0.3799 0.147 Uiso 1 1 calc R . .
H6B H 0.4360 0.0932 0.4107 0.147 Uiso 1 1 calc R . .
H6C H 0.4518 0.1725 0.3391 0.147 Uiso 1 1 calc R . .
C7 C 0.4574(3) -0.1216(5) 0.3592(4) 0.1100(19) Uani 1 1 d . . .
H7A H 0.5077 -0.1286 0.3753 0.165 Uiso 1 1 calc R . .
H7B H 0.4434 -0.1892 0.3280 0.165 Uiso 1 1 calc R . .
H7C H 0.4285 -0.1191 0.4036 0.165 Uiso 1 1 calc R . .
C8 C 0.4982(3) -0.0054(6) 0.2455(4) 0.122(2) Uani 1 1 d . . .
H8A H 0.5474 -0.0071 0.2657 0.184 Uiso 1 1 calc R . .
H8B H 0.4904 0.0659 0.2155 0.184 Uiso 1 1 calc R . .
H8C H 0.4892 -0.0744 0.2137 0.184 Uiso 1 1 calc R . .
C9 C 0.3581(3) -0.1812(5) 0.1730(3) 0.1039(18) Uani 1 1 d . . .
H9A H 0.3375 -0.2583 0.1612 0.156 Uiso 1 1 calc R . .
H9B H 0.4097 -0.1885 0.1809 0.156 Uiso 1 1 calc R . .
H9C H 0.3473 -0.1273 0.1311 0.156 Uiso 1 1 calc R . .
C10 C 0.2836(3) -0.2238(4) 0.2855(3) 0.0962(15) Uani 1 1 d . . .
H10A H 0.3000 -0.3043 0.2746 0.115 Uiso 1 1 calc R . .
H10B H 0.2907 -0.2100 0.3403 0.115 Uiso 1 1 calc R . .
C11 C 0.2079(3) -0.2125(5) 0.2634(3) 0.0911(14) Uani 1 1 d . . .
H11A H 0.1999 -0.2384 0.2106 0.109 Uiso 1 1 calc R . .
H11B H 0.1935 -0.1292 0.2667 0.109 Uiso 1 1 calc R . .
C12 C 0.1438(4) -0.4038(5) 0.2839(4) 0.137(3) Uani 1 1 d . . .
H12A H 0.1772 -0.4245 0.2453 0.206 Uiso 1 1 calc R . .
H12B H 0.0954 -0.4021 0.2615 0.206 Uiso 1 1 calc R . .
H12C H 0.1467 -0.4622 0.3243 0.206 Uiso 1 1 calc R . .
C13 C 0.1255(2) -0.3123(4) 0.4716(3) 0.0750(11) Uani 1 1 d . . .
C14 C 0.0903(4) -0.4355(6) 0.4652(4) 0.140(3) Uani 1 1 d . . .
H14A H 0.0970 -0.4769 0.5133 0.210 Uiso 1 1 calc R . .
H14B H 0.1124 -0.4805 0.4256 0.210 Uiso 1 1 calc R . .
H14C H 0.0394 -0.4267 0.4527 0.210 Uiso 1 1 calc R . .
C15 C 0.0926(4) -0.2462(7) 0.5370(3) 0.146(3) Uani 1 1 d . . .
H15A H 0.0954 -0.2953 0.5823 0.218 Uiso 1 1 calc R . .
H15B H 0.0428 -0.2282 0.5238 0.218 Uiso 1 1 calc R . .
H15C H 0.1188 -0.1731 0.5467 0.218 Uiso 1 1 calc R . .
C16 C 0.2055(3) -0.3286(6) 0.4902(4) 0.129(2) Uani 1 1 d . . .
H16A H 0.2122 -0.3783 0.5349 0.194 Uiso 1 1 calc R . .
H16B H 0.2275 -0.2519 0.5001 0.194 Uiso 1 1 calc R . .
H16C H 0.2277 -0.3658 0.4476 0.194 Uiso 1 1 calc R . .
C17 C 0.0235(2) -0.1886(4) 0.3485(3) 0.0792(12) Uani 1 1 d . . .
C18 C 0.0287(3) -0.1286(6) 0.2701(3) 0.119(2) Uani 1 1 d . . .
H18A H -0.0193 -0.1128 0.2489 0.178 Uiso 1 1 calc R . .
H18B H 0.0537 -0.1805 0.2363 0.178 Uiso 1 1 calc R . .
H18C H 0.0548 -0.0546 0.2760 0.178 Uiso 1 1 calc R . .
C19 C -0.0252(3) -0.2986(6) 0.3419(5) 0.158(3) Uani 1 1 d . . .
H19A H -0.0728 -0.2752 0.3231 0.236 Uiso 1 1 calc R . .
H19B H -0.0284 -0.3351 0.3915 0.236 Uiso 1 1 calc R . .
H19C H -0.0052 -0.3549 0.3069 0.236 Uiso 1 1 calc R . .
C20 C -0.0120(3) -0.0989(7) 0.4004(4) 0.137(3) Uani 1 1 d . . .
H20A H -0.0612 -0.0852 0.3821 0.206 Uiso 1 1 calc R . .
H20B H 0.0143 -0.0249 0.4002 0.206 Uiso 1 1 calc R . .
H20C H -0.0118 -0.1300 0.4518 0.206 Uiso 1 1 calc R . .
C21 C 0.3412(3) -0.0070(6) 0.5529(3) 0.1083(19) Uani 1 1 d . . .
H21A H 0.3444 -0.0097 0.6080 0.162 Uiso 1 1 calc R . .
H21B H 0.3697 0.0586 0.5353 0.162 Uiso 1 1 calc R . .
H21C H 0.3592 -0.0806 0.5327 0.162 Uiso 1 1 calc R . .
C22 C 0.2217(3) 0.0201(6) 0.5915(3) 0.120(2) Uani 1 1 d . . .
H22A H 0.2508 0.0118 0.6382 0.180 Uiso 1 1 calc R . .
H22B H 0.1853 -0.0414 0.5890 0.180 Uiso 1 1 calc R . .
H22C H 0.1987 0.0972 0.5904 0.180 Uiso 1 1 calc R . .
C23 C 0.2211(4) 0.2798(5) 0.4511(4) 0.140(3) Uani 1 1 d . . .
H23A H 0.1914 0.3498 0.4441 0.209 Uiso 1 1 calc R . .
H23B H 0.2656 0.2906 0.4253 0.209 Uiso 1 1 calc R . .
H23C H 0.2317 0.2673 0.5049 0.209 Uiso 1 1 calc R . .
C24 C 0.1175(3) 0.2144(5) 0.3809(4) 0.113(2) Uani 1 1 d . . .
H24A H 0.1103 0.2983 0.3897 0.136 Uiso 1 1 calc R . .
H24B H 0.0776 0.1701 0.4002 0.170 Uiso 1 1 calc R . .
H24C H 0.1203 0.2000 0.3268 0.170 Uiso 1 1 calc R . .
C25 C 0.4274(13) -0.1057(13) -0.0274(10) 0.154(8) Uani 0.50 1 d PD . .
C26 C 0.3884(7) -0.017(2) -0.0631(9) 0.130(6) Uani 0.50 1 d PD . .
C27 C 0.4279(9) 0.0856(17) -0.0486(8) 0.185(11) Uani 0.50 1 d PD . .
C28 C 0.4962(7) 0.1049(8) -0.0141(5) 0.155(4) Uani 1 1 d D . .
C29 C 0.4626(8) -0.0212(17) -0.0223(7) 0.163(9) Uani 0.50 1 d PD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0409(3) 0.0438(3) 0.0479(3) -0.0045(2) 0.0004(2) 0.0001(2)
P1 0.0477(5) 0.0572(6) 0.0597(6) 0.0009(4) 0.0116(4) -0.0029(4)
P2 0.0442(5) 0.0492(5) 0.0580(5) -0.0037(4) 0.0019(4) -0.0055(4)
N1 0.0494(16) 0.0531(17) 0.0590(17) -0.0021(13) 0.0064(13) -0.0023(12)
N2 0.0455(15) 0.0536(17) 0.0636(17) -0.0096(13) 0.0021(13) -0.0037(13)
N3 0.075(2) 0.070(2) 0.075(2) -0.0159(17) 0.0314(17) -0.0162(17)
N4 0.079(2) 0.0571(19) 0.080(2) -0.0204(16) 0.0274(18) -0.0192(16)
N5 0.0598(19) 0.077(2) 0.0494(16) -0.0020(14) -0.0042(14) -0.0063(15)
N6 0.0616(19) 0.0487(17) 0.089(2) -0.0084(16) -0.0039(16) 0.0094(14)
C1 0.077(3) 0.086(3) 0.071(3) 0.022(2) 0.013(2) 0.002(2)
C2 0.166(6) 0.196(8) 0.113(5) 0.082(5) 0.064(4) 0.051(6)
C3 0.087(4) 0.149(6) 0.116(4) 0.048(4) -0.020(3) 0.008(4)
C4 0.193(7) 0.066(3) 0.147(5) 0.025(4) -0.044(5) 0.000(4)
C5 0.045(2) 0.084(3) 0.096(3) 0.003(2) 0.014(2) 0.0033(19)
C6 0.060(3) 0.105(4) 0.127(4) -0.024(3) -0.008(3) -0.006(3)
C7 0.070(3) 0.099(4) 0.161(5) 0.029(4) -0.003(3) 0.019(3)
C8 0.057(3) 0.184(7) 0.128(5) -0.005(4) 0.031(3) 0.006(3)
C9 0.107(4) 0.117(4) 0.090(3) -0.039(3) 0.038(3) -0.021(3)
C10 0.111(4) 0.072(3) 0.105(4) -0.030(3) 0.003(3) 0.008(3)
C11 0.102(4) 0.096(4) 0.075(3) -0.026(3) 0.001(3) -0.001(3)
C12 0.168(6) 0.089(4) 0.161(6) -0.067(4) 0.082(5) -0.061(4)
C13 0.072(3) 0.074(3) 0.079(3) 0.019(2) 0.001(2) -0.007(2)
C14 0.150(6) 0.098(4) 0.169(6) 0.058(4) -0.020(5) -0.049(4)
C15 0.195(7) 0.174(7) 0.070(3) 0.013(4) 0.032(4) 0.028(6)
C16 0.089(4) 0.150(6) 0.146(5) 0.081(4) -0.029(3) -0.003(4)
C17 0.051(2) 0.083(3) 0.102(3) 0.001(3) -0.018(2) -0.012(2)
C18 0.105(4) 0.126(5) 0.121(5) 0.027(4) -0.046(3) -0.004(4)
C19 0.095(4) 0.123(5) 0.246(9) 0.033(5) -0.075(5) -0.054(4)
C20 0.063(3) 0.166(6) 0.182(7) -0.026(5) 0.003(4) 0.036(4)
C21 0.084(3) 0.159(6) 0.080(3) 0.020(3) -0.016(3) 0.014(3)
C22 0.100(4) 0.191(7) 0.071(3) -0.036(4) 0.016(3) -0.022(4)
C23 0.142(5) 0.068(3) 0.203(7) -0.032(4) -0.062(5) 0.008(3)
C24 0.081(3) 0.075(3) 0.180(6) 0.005(3) -0.028(4) 0.015(3)
C25 0.186(17) 0.145(14) 0.138(14) -0.073(12) 0.107(13) -0.072(15)
C26 0.087(10) 0.20(2) 0.109(11) -0.017(11) 0.034(8) -0.031(11)
C27 0.140(14) 0.32(3) 0.096(10) 0.058(15) 0.051(10) 0.11(2)
C28 0.217(10) 0.133(7) 0.122(7) 0.026(5) 0.087(7) 0.047(7)
C29 0.24(3) 0.152(15) 0.112(14) -0.047(11) 0.123(16) -0.052(17)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N2 1.845(3) . ?
Ti1 N1 1.846(3) . ?
Ti1 N6 1.922(3) . ?
Ti1 N5 1.926(3) . ?
P1 N1 1.554(3) . ?
P1 N3 1.677(3) . ?
P1 C1 1.874(4) . ?
P1 C5 1.876(4) . ?
P2 N2 1.554(3) . ?
P2 N4 1.680(3) . ?
P2 C17 1.869(4) . ?
P2 C13 1.872(4) . ?
N3 C9 1.453(5) . ?
N3 C10 1.503(6) . ?
N4 C12 1.444(5) . ?
N4 C11 1.513(6) . ?
N5 C22 1.434(6) . ?
N5 C21 1.437(6) . ?
N6 C24 1.419(6) . ?
N6 C23 1.443(6) . ?
C1 C4 1.501(7) . ?
C1 C2 1.523(7) . ?
C1 C3 1.533(6) . ?
C5 C6 1.524(6) . ?
C5 C7 1.530(6) . ?
C5 C8 1.550(7) . ?
C10 C11 1.439(7) . ?
C13 C15 1.508(7) . ?
C13 C16 1.509(6) . ?
C13 C14 1.524(7) . ?
C17 C20 1.520(7) . ?
C17 C19 1.525(6) . ?
C17 C18 1.528(7) . ?
C25 C29 1.15(2) . ?
C25 C26 1.361(10) . ?
C25 C28 1.56(2) 3_655 ?
C26 C27 1.372(10) . ?
C26 C29 1.515(10) . ?
C27 C28 1.389(9) . ?
C27 C29 1.42(3) . ?
C28 C29 1.346(19) 3_655 ?
C28 C29 1.54(2) . ?
C28 C25 1.56(2) 3_655 ?
C29 C28 1.346(19) 3_655 ?
C29 C29 1.62(3) 3_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ti1 N1 112.72(13) . . ?
N2 Ti1 N6 108.71(13) . . ?
N1 Ti1 N6 111.71(14) . . ?
N2 Ti1 N5 112.71(13) . . ?
N1 Ti1 N5 106.78(14) . . ?
N6 Ti1 N5 103.89(14) . . ?
N1 P1 N3 110.59(16) . . ?
N1 P1 C1 110.56(18) . . ?
N3 P1 C1 108.0(2) . . ?
N1 P1 C5 108.50(19) . . ?
N3 P1 C5 106.49(19) . . ?
C1 P1 C5 112.6(2) . . ?
N2 P2 N4 110.34(15) . . ?
N2 P2 C17 108.94(18) . . ?
N4 P2 C17 107.8(2) . . ?
N2 P2 C13 110.23(18) . . ?
N4 P2 C13 106.8(2) . . ?
C17 P2 C13 112.7(2) . . ?
P1 N1 Ti1 160.5(2) . . ?
P2 N2 Ti1 160.68(19) . . ?
C9 N3 C10 114.7(4) . . ?
C9 N3 P1 126.8(3) . . ?
C10 N3 P1 117.6(3) . . ?
C12 N4 C11 113.7(4) . . ?
C12 N4 P2 126.4(3) . . ?
C11 N4 P2 117.0(3) . . ?
C22 N5 C21 110.2(4) . . ?
C22 N5 Ti1 121.1(3) . . ?
C21 N5 Ti1 128.7(3) . . ?
C24 N6 C23 109.7(4) . . ?
C24 N6 Ti1 129.2(3) . . ?
C23 N6 Ti1 120.7(3) . . ?
C4 C1 C2 109.4(5) . . ?
C4 C1 C3 109.0(5) . . ?
C2 C1 C3 106.7(5) . . ?
C4 C1 P1 108.3(3) . . ?
C2 C1 P1 117.4(4) . . ?
C3 C1 P1 105.8(3) . . ?
C6 C5 C7 108.0(5) . . ?
C6 C5 C8 109.0(4) . . ?
C7 C5 C8 109.3(4) . . ?
C6 C5 P1 108.9(3) . . ?
C7 C5 P1 105.2(3) . . ?
C8 C5 P1 116.2(4) . . ?
C11 C10 N3 110.1(4) . . ?
C10 C11 N4 110.7(4) . . ?
C15 C13 C16 108.6(5) . . ?
C15 C13 C14 108.3(5) . . ?
C16 C13 C14 108.4(5) . . ?
C15 C13 P2 108.6(4) . . ?
C16 C13 P2 105.7(3) . . ?
C14 C13 P2 117.1(4) . . ?
C20 C17 C19 107.9(5) . . ?
C20 C17 C18 106.7(5) . . ?
C19 C17 C18 110.3(5) . . ?
C20 C17 P2 109.4(3) . . ?
C19 C17 P2 116.4(4) . . ?
C18 C17 P2 105.8(3) . . ?
C29 C25 C26 73.8(9) . . ?
C29 C25 C28 57.3(13) . 3_655 ?
C26 C25 C28 131.1(15) . 3_655 ?
C25 C26 C27 105.0(14) . . ?
C25 C26 C29 46.6(9) . . ?
C27 C26 C29 58.7(12) . . ?
C26 C27 C28 132.3(15) . . ?
C26 C27 C29 65.7(8) . . ?
C28 C27 C29 66.6(11) . . ?
C29 C28 C27 125.4(12) 3_655 . ?
C29 C28 C29 68.0(11) 3_655 . ?
C27 C28 C29 57.7(12) . . ?
C29 C28 C25 45.8(9) 3_655 3_655 ?
C27 C28 C25 171.2(11) . 3_655 ?
C29 C28 C25 113.6(10) . 3_655 ?
C25 C29 C28 76.8(16) . 3_655 ?
C25 C29 C27 114.8(11) . . ?
C28 C29 C27 166.5(14) 3_655 . ?
C25 C29 C26 59.6(7) . . ?
C28 C29 C26 136.4(16) 3_655 . ?
C27 C29 C26 55.6(7) . . ?
C25 C29 C28 169.1(15) . . ?
C28 C29 C28 112.0(11) 3_655 . ?
C27 C29 C28 55.7(9) . . ?
C26 C29 C28 111.3(14) . . ?
C25 C29 C29 138(2) . 3_655 ?
C28 C29 C29 61.8(12) 3_655 3_655 ?
C27 C29 C29 105.7(19) . 3_655 ?
C26 C29 C29 161(2) . 3_655 ?
C28 C29 C29 50.2(11) . 3_655 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.076
#===end

data_[tBu2(Me2N)PN]2Ti(NMe2)2
_database_code_depnum_ccdc_archive 'CCDC 702183'
_audit_creation_method           SHELXL-97
_chemical_formula_sum            'C24 H60 N6 P2 Ti'
_chemical_formula_weight         542.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.6174(13)
_cell_length_b                   16.0036(15)
_cell_length_c                   16.7941(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.2890(10)
_cell_angle_gamma                90.00
_cell_volume                     3386.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      25.0
_exptl_crystal_description       blocks
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.839549
_exptl_absorpt_correction_T_max  1.000000
_diffrn_measurement_device_type  'Bruker SMART system'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_number            31894
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5930
_reflns_number_gt                4988
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1609P)^2^+2.0474P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5930
_refine_ls_number_parameters     288
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0784
_refine_ls_wR_factor_ref         0.2583
_refine_ls_wR_factor_gt          0.2399
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.20351(5) 0.70625(4) 0.19846(4) 0.0406(3) Uani 1 1 d . . .
P1 P 0.38109(7) 0.85974(6) 0.22393(6) 0.0493(3) Uani 1 1 d . . .
P2 P -0.05475(7) 0.75842(6) 0.11700(6) 0.0482(3) Uani 1 1 d D . .
N1 N 0.2953(3) 0.7908(2) 0.1962(2) 0.0530(8) Uani 1 1 d . . .
N2 N 0.3403(3) 0.9437(2) 0.1589(3) 0.0748(11) Uani 1 1 d . . .
N3 N 0.0642(2) 0.7416(2) 0.1680(2) 0.0529(8) Uani 1 1 d . . .
N4 N -0.1329(3) 0.6790(3) 0.1368(3) 0.0933(14) Uani 1 1 d D . .
N5 N 0.2170(3) 0.6180(2) 0.1254(2) 0.0629(9) Uani 1 1 d . . .
N6 N 0.2438(3) 0.6552(2) 0.3104(2) 0.0608(9) Uani 1 1 d . . .
C1 C 0.5050(3) 0.8204(3) 0.2118(3) 0.0696(12) Uani 1 1 d . . .
C2 C 0.5208(4) 0.7307(4) 0.2416(5) 0.0920(17) Uani 1 1 d . . .
H2A H 0.5839 0.7091 0.2364 0.138 Uiso 1 1 calc R . .
H2B H 0.4607 0.6981 0.2066 0.138 Uiso 1 1 calc R . .
H2C H 0.5278 0.7279 0.3006 0.138 Uiso 1 1 calc R . .
C3 C 0.6068(4) 0.8683(4) 0.2592(4) 0.0965(18) Uani 1 1 d . . .
H3A H 0.6643 0.8427 0.2484 0.145 Uiso 1 1 calc R . .
H3B H 0.6218 0.8675 0.3199 0.145 Uiso 1 1 calc R . .
H3C H 0.5986 0.9251 0.2393 0.145 Uiso 1 1 calc R . .
C4 C 0.4829(6) 0.8186(5) 0.1146(5) 0.107(2) Uani 1 1 d . . .
H4A H 0.5448 0.7990 0.1061 0.161 Uiso 1 1 calc R . .
H4B H 0.4657 0.8739 0.0913 0.161 Uiso 1 1 calc R . .
H4C H 0.4244 0.7818 0.0859 0.161 Uiso 1 1 calc R . .
C5 C 0.4055(4) 0.8986(3) 0.3339(3) 0.0773(13) Uani 1 1 d . . .
C6 C 0.2923(6) 0.9190(5) 0.3310(5) 0.114(2) Uani 1 1 d . . .
H6A H 0.2973 0.9397 0.3861 0.171 Uiso 1 1 calc R . .
H6B H 0.2498 0.8691 0.3174 0.171 Uiso 1 1 calc R . .
H6C H 0.2599 0.9605 0.2878 0.171 Uiso 1 1 calc R . .
C7 C 0.4515(7) 0.8276(5) 0.3996(4) 0.116(2) Uani 1 1 d . . .
H7A H 0.4639 0.8479 0.4565 0.174 Uiso 1 1 calc R . .
H7B H 0.5172 0.8087 0.3972 0.174 Uiso 1 1 calc R . .
H7C H 0.4020 0.7820 0.3862 0.174 Uiso 1 1 calc R . .
C8 C 0.4742(7) 0.9773(5) 0.3622(5) 0.129(3) Uani 1 1 d . . .
H8A H 0.4817 0.9920 0.4196 0.193 Uiso 1 1 calc R . .
H8B H 0.4409 1.0224 0.3238 0.193 Uiso 1 1 calc R . .
H8C H 0.5429 0.9667 0.3608 0.193 Uiso 1 1 calc R . .
C9 C 0.2338(5) 0.9480(4) 0.0966(4) 0.109(2) Uani 1 1 d . . .
H9A H 0.2242 0.9994 0.0650 0.164 Uiso 1 1 calc R . .
H9B H 0.1850 0.9460 0.1255 0.164 Uiso 1 1 calc R . .
H9C H 0.2209 0.9017 0.0577 0.164 Uiso 1 1 calc R . .
C10 C 0.4058(6) 1.0148(4) 0.1562(5) 0.117(2) Uani 1 1 d . . .
H10A H 0.3637 1.0539 0.1136 0.176 Uiso 1 1 calc R . .
H10B H 0.4639 0.9959 0.1418 0.176 Uiso 1 1 calc R . .
H10C H 0.4329 1.0416 0.2115 0.176 Uiso 1 1 calc R . .
C11 C 0.2534(5) 0.6258(4) 0.0550(4) 0.0965(18) Uani 1 1 d . . .
H11A H 0.2526 0.5719 0.0297 0.145 Uiso 1 1 calc R . .
H11B H 0.3244 0.6477 0.0764 0.145 Uiso 1 1 calc R . .
H11C H 0.2073 0.6631 0.0123 0.145 Uiso 1 1 calc R . .
C12 C 0.1726(5) 0.5362(3) 0.1262(4) 0.0890(16) Uani 1 1 d . . .
H12A H 0.1871 0.5005 0.0860 0.133 Uiso 1 1 calc R . .
H12B H 0.0973 0.5409 0.1103 0.133 Uiso 1 1 calc R . .
H12C H 0.2040 0.5127 0.1829 0.133 Uiso 1 1 calc R . .
C13 C 0.3376(4) 0.6051(4) 0.3473(4) 0.0846(15) Uani 1 1 d . . .
H13A H 0.3436 0.5858 0.4030 0.127 Uiso 1 1 calc R . .
H13B H 0.3988 0.6380 0.3528 0.127 Uiso 1 1 calc R . .
H13C H 0.3332 0.5580 0.3107 0.127 Uiso 1 1 calc R . .
C14 C 0.1979(5) 0.6708(4) 0.3727(3) 0.0903(17) Uani 1 1 d . . .
H14A H 0.2326 0.6369 0.4227 0.135 Uiso 1 1 calc R . .
H14B H 0.1236 0.6573 0.3485 0.135 Uiso 1 1 calc R . .
H14C H 0.2065 0.7287 0.3888 0.135 Uiso 1 1 calc R . .
C15 C -0.0846(4) 0.7626(3) 0.0020(3) 0.0699(12) Uani 1 1 d . . .
C16 C -0.0035(7) 0.8148(9) -0.0162(5) 0.190(6) Uani 1 1 d . . .
H16A H -0.0206 0.8166 -0.0771 0.286 Uiso 1 1 calc R . .
H16B H 0.0656 0.7905 0.0120 0.286 Uiso 1 1 calc R . .
H16C H -0.0038 0.8705 0.0051 0.286 Uiso 1 1 calc R . .
C17 C -0.0675(11) 0.6760(7) -0.0293(6) 0.197(6) Uani 1 1 d . . .
H17A H -0.0831 0.6780 -0.0900 0.295 Uiso 1 1 calc R . .
H17B H -0.1136 0.6365 -0.0180 0.295 Uiso 1 1 calc R . .
H17C H 0.0050 0.6594 0.0005 0.295 Uiso 1 1 calc R . .
C18 C -0.1951(5) 0.7892(6) -0.0588(4) 0.123(3) Uani 1 1 d . . .
H18A H -0.1984 0.7887 -0.1169 0.184 Uiso 1 1 calc R . .
H18B H -0.2097 0.8445 -0.0441 0.184 Uiso 1 1 calc R . .
H18C H -0.2468 0.7510 -0.0537 0.184 Uiso 1 1 calc R . .
C19 C -0.0924(4) 0.8548(3) 0.1511(4) 0.0774(13) Uani 1 1 d . . .
C20 C -0.0510(14) 0.8586(9) 0.2488(8) 0.236(8) Uani 1 1 d . . .
H20A H -0.0714 0.9108 0.2662 0.354 Uiso 1 1 calc R . .
H20B H 0.0250 0.8543 0.2718 0.354 Uiso 1 1 calc R . .
H20C H -0.0804 0.8133 0.2700 0.354 Uiso 1 1 calc R . .
C21 C -0.0234(8) 0.9232(6) 0.1523(11) 0.215(7) Uani 1 1 d . . .
H21A H -0.0467 0.9727 0.1721 0.322 Uiso 1 1 calc R . .
H21B H -0.0252 0.9323 0.0953 0.322 Uiso 1 1 calc R . .
H21C H 0.0478 0.9101 0.1903 0.322 Uiso 1 1 calc R . .
C22 C -0.2043(6) 0.8841(5) 0.1185(6) 0.134(3) Uani 1 1 d . . .
H22A H -0.2081 0.9364 0.1452 0.201 Uiso 1 1 calc R . .
H22B H -0.2475 0.8434 0.1320 0.201 Uiso 1 1 calc R . .
H22C H -0.2294 0.8914 0.0573 0.201 Uiso 1 1 calc R . .
C23 C -0.2490(6) 0.6758(6) 0.0931(5) 0.129(3) Uiso 1 1 d D . .
H23A H -0.2758 0.6280 0.1130 0.193 Uiso 1 1 calc R . .
H23B H -0.2676 0.6716 0.0321 0.193 Uiso 1 1 calc R . .
H23C H -0.2794 0.7257 0.1058 0.193 Uiso 1 1 calc R . .
C24 C -0.0776(11) 0.6202(8) 0.2036(7) 0.203(5) Uiso 1 1 d D . .
H24A H -0.1271 0.5803 0.2094 0.305 Uiso 1 1 calc R . .
H24B H -0.0441 0.6494 0.2571 0.305 Uiso 1 1 calc R . .
H24C H -0.0246 0.5917 0.1891 0.305 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0380(4) 0.0356(4) 0.0477(4) -0.0001(2) 0.0156(3) 0.0002(2)
P1 0.0416(5) 0.0443(6) 0.0585(6) 0.0007(4) 0.0151(4) -0.0057(4)
P2 0.0376(5) 0.0506(6) 0.0555(6) 0.0037(4) 0.0168(4) 0.0025(4)
N1 0.0457(17) 0.0489(18) 0.065(2) -0.0037(14) 0.0216(15) -0.0070(13)
N2 0.058(2) 0.058(2) 0.091(3) 0.0216(19) 0.0081(19) -0.0101(17)
N3 0.0427(17) 0.062(2) 0.0517(18) -0.0011(14) 0.0150(14) 0.0003(14)
N4 0.061(2) 0.098(3) 0.112(4) 0.031(3) 0.023(2) -0.004(2)
N5 0.072(2) 0.0465(18) 0.073(2) -0.0109(16) 0.0306(18) 0.0047(16)
N6 0.062(2) 0.059(2) 0.061(2) 0.0156(16) 0.0222(16) 0.0081(16)
C1 0.045(2) 0.076(3) 0.088(3) 0.005(2) 0.026(2) -0.002(2)
C2 0.066(3) 0.076(3) 0.136(5) 0.010(3) 0.041(3) 0.018(3)
C3 0.046(3) 0.106(4) 0.131(5) 0.009(4) 0.026(3) -0.010(3)
C4 0.094(4) 0.136(6) 0.112(5) -0.001(4) 0.062(4) 0.004(4)
C5 0.084(3) 0.074(3) 0.068(3) -0.018(2) 0.023(2) -0.018(3)
C6 0.121(5) 0.123(6) 0.114(5) -0.038(4) 0.063(4) 0.005(4)
C7 0.134(6) 0.133(6) 0.063(3) 0.008(4) 0.016(3) -0.012(5)
C8 0.159(7) 0.108(5) 0.115(5) -0.051(4) 0.048(5) -0.064(5)
C9 0.084(4) 0.081(4) 0.119(5) 0.031(3) -0.010(3) -0.008(3)
C10 0.100(5) 0.075(4) 0.150(6) 0.040(4) 0.018(4) -0.025(3)
C11 0.116(5) 0.099(4) 0.091(4) -0.019(3) 0.058(4) 0.011(3)
C12 0.096(4) 0.049(3) 0.112(4) -0.017(3) 0.030(3) -0.002(2)
C13 0.073(3) 0.078(3) 0.095(4) 0.032(3) 0.023(3) 0.017(3)
C14 0.105(4) 0.113(4) 0.062(3) 0.019(3) 0.042(3) 0.018(3)
C15 0.056(2) 0.091(3) 0.055(2) 0.004(2) 0.0126(19) 0.003(2)
C16 0.120(6) 0.356(17) 0.079(5) 0.054(7) 0.019(4) -0.091(8)
C17 0.236(13) 0.184(10) 0.114(7) -0.055(7) 0.004(7) 0.089(10)
C18 0.077(4) 0.179(8) 0.082(4) 0.027(4) -0.005(3) 0.004(4)
C19 0.067(3) 0.068(3) 0.100(4) -0.002(3) 0.034(3) 0.015(2)
C20 0.310(19) 0.225(14) 0.152(9) -0.053(9) 0.063(11) 0.134(13)
C21 0.140(8) 0.103(7) 0.39(2) -0.095(10) 0.090(11) -0.018(6)
C22 0.101(5) 0.107(5) 0.204(9) 0.008(5) 0.068(6) 0.046(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N1 1.852(3) . ?
Ti1 N3 1.856(3) . ?
Ti1 N5 1.925(3) . ?
Ti1 N6 1.929(3) . ?
P1 N1 1.545(3) . ?
P1 N2 1.687(4) . ?
P1 C5 1.856(5) . ?
P1 C1 1.883(5) . ?
P2 N3 1.541(3) . ?
P2 N4 1.769(4) . ?
P2 C19 1.786(5) . ?
P2 C15 1.818(5) . ?
N2 C9 1.433(6) . ?
N2 C10 1.456(6) . ?
N4 C24 1.439(8) . ?
N4 C23 1.469(7) . ?
N5 C12 1.445(6) . ?
N5 C11 1.450(6) . ?
N6 C14 1.430(6) . ?
N6 C13 1.435(6) . ?
C1 C2 1.507(7) . ?
C1 C3 1.519(7) . ?
C1 C4 1.544(8) . ?
C5 C8 1.532(8) . ?
C5 C7 1.542(9) . ?
C5 C6 1.558(8) . ?
C15 C16 1.505(9) . ?
C15 C18 1.524(7) . ?
C15 C17 1.530(10) . ?
C19 C21 1.437(12) . ?
C19 C22 1.486(8) . ?
C19 C20 1.519(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ti1 N3 113.49(15) . . ?
N1 Ti1 N5 107.13(16) . . ?
N3 Ti1 N5 112.50(16) . . ?
N1 Ti1 N6 112.66(16) . . ?
N3 Ti1 N6 106.32(15) . . ?
N5 Ti1 N6 104.47(16) . . ?
N1 P1 N2 110.37(19) . . ?
N1 P1 C5 111.7(2) . . ?
N2 P1 C5 105.5(2) . . ?
N1 P1 C1 109.6(2) . . ?
N2 P1 C1 106.6(2) . . ?
C5 P1 C1 113.0(2) . . ?
N3 P2 N4 110.5(2) . . ?
N3 P2 C19 109.9(2) . . ?
N4 P2 C19 107.1(3) . . ?
N3 P2 C15 111.16(19) . . ?
N4 P2 C15 108.5(2) . . ?
C19 P2 C15 109.5(3) . . ?
P1 N1 Ti1 162.6(2) . . ?
C9 N2 C10 113.7(4) . . ?
C9 N2 P1 120.3(3) . . ?
C10 N2 P1 126.0(4) . . ?
P2 N3 Ti1 162.8(2) . . ?
C24 N4 C23 120.8(8) . . ?
C24 N4 P2 116.2(7) . . ?
C23 N4 P2 122.8(5) . . ?
C12 N5 C11 111.1(4) . . ?
C12 N5 Ti1 121.2(3) . . ?
C11 N5 Ti1 126.9(3) . . ?
C14 N6 C13 110.3(4) . . ?
C14 N6 Ti1 126.7(3) . . ?
C13 N6 Ti1 122.3(3) . . ?
C2 C1 C3 108.7(5) . . ?
C2 C1 C4 106.2(5) . . ?
C3 C1 C4 109.7(5) . . ?
C2 C1 P1 107.7(3) . . ?
C3 C1 P1 116.8(4) . . ?
C4 C1 P1 107.3(4) . . ?
C8 C5 C7 110.4(5) . . ?
C8 C5 C6 108.6(6) . . ?
C7 C5 C6 107.7(6) . . ?
C8 C5 P1 116.2(4) . . ?
C7 C5 P1 109.6(4) . . ?
C6 C5 P1 103.7(4) . . ?
C16 C15 C18 108.8(6) . . ?
C16 C15 C17 102.3(9) . . ?
C18 C15 C17 105.2(6) . . ?
C16 C15 P2 110.5(4) . . ?
C18 C15 P2 119.2(4) . . ?
C17 C15 P2 109.3(5) . . ?
C21 C19 C22 109.8(7) . . ?
C21 C19 C20 88.9(9) . . ?
C22 C19 C20 107.1(7) . . ?
C21 C19 P2 113.3(5) . . ?
C22 C19 P2 122.2(5) . . ?
C20 C19 P2 110.3(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.583
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.096

#===end

data_[tBu2(Me2N)PN]2TiMe2
_database_code_depnum_ccdc_archive 'CCDC 702184'
_audit_creation_method           SHELXL-97
_chemical_formula_sum            'C22 H54 N4 P2 Ti'
_chemical_formula_weight         484.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.8460(17)
_cell_length_b                   16.457(2)
_cell_length_c                   15.107(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.2010(10)
_cell_angle_gamma                90.00
_cell_volume                     3066.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      25.0
_exptl_crystal_description       blocks
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7417
_exptl_absorpt_correction_T_max  0.8573
_diffrn_measurement_device_type  'Bruker SMART system'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_number            29063
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5393
_reflns_number_gt                4378
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1909P)^2^+0.8288P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5393
_refine_ls_number_parameters     247
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0855
_refine_ls_wR_factor_ref         0.2842
_refine_ls_wR_factor_gt          0.2651
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.47651(6) 0.20941(4) 0.18928(5) 0.0529(3) Uani 1 1 d . . .
P1 P 0.67083(9) 0.07110(7) 0.27588(8) 0.0618(4) Uani 1 1 d . . .
P2 P 0.35457(9) 0.30713(7) 0.32902(8) 0.0611(4) Uani 1 1 d D . .
N1 N 0.5796(3) 0.1352(2) 0.2436(3) 0.0708(10) Uani 1 1 d . . .
N2 N 0.4094(3) 0.2625(3) 0.2640(3) 0.0708(10) Uani 1 1 d . . .
N3 N 0.6486(5) 0.0136(4) 0.3610(4) 0.115(2) Uani 1 1 d . . .
N4 N 0.4434(4) 0.3163(5) 0.4388(3) 0.121(2) Uani 1 1 d D . .
C1 C 0.5467(6) 0.2946(4) 0.1191(4) 0.0927(17) Uani 1 1 d . . .
H1A H 0.6031 0.3237 0.1627 0.139 Uiso 1 1 calc R . .
H1B H 0.4922 0.3322 0.0866 0.139 Uiso 1 1 calc R . .
H1C H 0.5768 0.2668 0.0760 0.139 Uiso 1 1 calc R . .
C2 C 0.3565(4) 0.1525(3) 0.0834(4) 0.0814(14) Uani 1 1 d . . .
H2A H 0.3204 0.1117 0.1095 0.122 Uiso 1 1 calc R . .
H2B H 0.3896 0.1275 0.0406 0.122 Uiso 1 1 calc R . .
H2C H 0.3047 0.1922 0.0518 0.122 Uiso 1 1 calc R . .
C3 C 0.8020(4) 0.1231(4) 0.3192(5) 0.0952(19) Uani 1 1 d . . .
C4 C 0.7860(9) 0.1810(8) 0.3973(9) 0.211(7) Uani 1 1 d . . .
H4A H 0.8521 0.2101 0.4242 0.317 Uiso 1 1 calc R . .
H4B H 0.7673 0.1493 0.4439 0.317 Uiso 1 1 calc R . .
H4C H 0.7289 0.2190 0.3714 0.317 Uiso 1 1 calc R . .
C5 C 0.9000(6) 0.0704(7) 0.3683(8) 0.168(4) Uani 1 1 d . . .
H5A H 0.9630 0.1042 0.3890 0.251 Uiso 1 1 calc R . .
H5B H 0.9124 0.0303 0.3262 0.251 Uiso 1 1 calc R . .
H5C H 0.8856 0.0439 0.4202 0.251 Uiso 1 1 calc R . .
C6 C 0.8263(8) 0.1765(8) 0.2462(8) 0.185(5) Uani 1 1 d . . .
H6A H 0.8950 0.2027 0.2709 0.277 Uiso 1 1 calc R . .
H6B H 0.7706 0.2169 0.2272 0.277 Uiso 1 1 calc R . .
H6C H 0.8286 0.1439 0.1941 0.277 Uiso 1 1 calc R . .
C7 C 0.6691(4) 0.0016(3) 0.1790(4) 0.0747(13) Uani 1 1 d . . .
C8 C 0.5625(7) -0.0456(5) 0.1570(6) 0.126(3) Uani 1 1 d . . .
H8A H 0.5592 -0.0824 0.1070 0.189 Uiso 1 1 calc R . .
H8B H 0.5028 -0.0082 0.1397 0.189 Uiso 1 1 calc R . .
H8C H 0.5586 -0.0757 0.2104 0.189 Uiso 1 1 calc R . .
C9 C 0.6539(7) 0.0507(5) 0.0896(5) 0.118(2) Uani 1 1 d . . .
H9A H 0.6533 0.0143 0.0397 0.177 Uiso 1 1 calc R . .
H9B H 0.7124 0.0886 0.0972 0.177 Uiso 1 1 calc R . .
H9C H 0.5864 0.0796 0.0761 0.177 Uiso 1 1 calc R . .
C10 C 0.7638(7) -0.0580(6) 0.1930(6) 0.144(4) Uani 1 1 d . . .
H10A H 0.7543 -0.0907 0.1386 0.216 Uiso 1 1 calc R . .
H10B H 0.7661 -0.0925 0.2447 0.216 Uiso 1 1 calc R . .
H10C H 0.8306 -0.0283 0.2044 0.216 Uiso 1 1 calc R . .
C11 C 0.5563(10) 0.0250(8) 0.3926(8) 0.188(5) Uani 1 1 d . . .
H11A H 0.5576 -0.0131 0.4411 0.283 Uiso 1 1 calc R . .
H11B H 0.4921 0.0164 0.3426 0.283 Uiso 1 1 calc R . .
H11C H 0.5562 0.0793 0.4156 0.283 Uiso 1 1 calc R . .
C12 C 0.7116(10) -0.0583(7) 0.4018(7) 0.188(5) Uani 1 1 d . . .
H12A H 0.6824 -0.0806 0.4485 0.282 Uiso 1 1 calc R . .
H12B H 0.7858 -0.0430 0.4288 0.282 Uiso 1 1 calc R . .
H12C H 0.7078 -0.0983 0.3547 0.282 Uiso 1 1 calc R . .
C13 C 0.2355(5) 0.2509(4) 0.3359(4) 0.0879(16) Uani 1 1 d . . .
C14 C 0.1630(10) 0.2382(13) 0.2441(8) 0.248(9) Uani 1 1 d . . .
H14A H 0.1001 0.2088 0.2486 0.372 Uiso 1 1 calc R . .
H14B H 0.1998 0.2075 0.2079 0.372 Uiso 1 1 calc R . .
H14C H 0.1412 0.2898 0.2153 0.372 Uiso 1 1 calc R . .
C15 C 0.1723(8) 0.2800(6) 0.4018(8) 0.164(5) Uani 1 1 d . . .
H15A H 0.1117 0.2446 0.3974 0.246 Uiso 1 1 calc R . .
H15B H 0.1468 0.3343 0.3858 0.246 Uiso 1 1 calc R . .
H15C H 0.2189 0.2793 0.4638 0.246 Uiso 1 1 calc R . .
C16 C 0.2593(13) 0.1656(7) 0.3486(13) 0.225(7) Uani 1 1 d . . .
H16A H 0.1955 0.1369 0.3522 0.338 Uiso 1 1 calc R . .
H16B H 0.3160 0.1575 0.4047 0.338 Uiso 1 1 calc R . .
H16C H 0.2823 0.1453 0.2975 0.338 Uiso 1 1 calc R . .
C17 C 0.3169(6) 0.4067(3) 0.2845(5) 0.105(2) Uani 1 1 d D . .
C18 C 0.2548(9) 0.4618(5) 0.3308(8) 0.180(5) Uani 1 1 d D . .
H18A H 0.2416 0.5127 0.2986 0.271 Uiso 1 1 calc R . .
H18B H 0.2962 0.4709 0.3934 0.271 Uiso 1 1 calc R . .
H18C H 0.1869 0.4369 0.3298 0.271 Uiso 1 1 calc R . .
C21 C 0.4174(9) 0.3604(6) 0.5148(6) 0.156(3) Uiso 1 1 d D . .
H21A H 0.4779 0.3574 0.5690 0.233 Uiso 1 1 calc R . .
H21B H 0.3549 0.3363 0.5273 0.233 Uiso 1 1 calc R . .
H21C H 0.4025 0.4163 0.4977 0.233 Uiso 1 1 calc R . .
C22 C 0.5239(12) 0.2538(9) 0.4667(11) 0.243(7) Uiso 1 1 d D . .
H22A H 0.5632 0.2616 0.5302 0.364 Uiso 1 1 calc R . .
H22B H 0.5731 0.2565 0.4293 0.364 Uiso 1 1 calc R . .
H22D H 0.4891 0.2016 0.4592 0.364 Uiso 1 1 calc R . .
C19 C 0.2623(13) 0.4025(8) 0.1812(6) 0.332(15) Uani 1 1 d D . .
H19A H 0.2421 0.4562 0.1579 0.499 Uiso 1 1 calc R . .
H19B H 0.1986 0.3691 0.1699 0.499 Uiso 1 1 calc R . .
H19C H 0.3116 0.3795 0.1506 0.499 Uiso 1 1 calc R . .
C20 C 0.4277(9) 0.4506(11) 0.2907(12) 0.303(10) Uiso 1 1 d D . .
H20A H 0.4138 0.5053 0.2685 0.454 Uiso 1 1 calc R . .
H20B H 0.4653 0.4219 0.2536 0.454 Uiso 1 1 calc R . .
H20C H 0.4713 0.4514 0.3536 0.454 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0552(5) 0.0561(5) 0.0474(5) -0.0055(3) 0.0147(3) 0.0057(3)
P1 0.0591(7) 0.0715(7) 0.0554(6) -0.0035(5) 0.0172(5) 0.0154(5)
P2 0.0575(7) 0.0637(7) 0.0644(7) -0.0128(5) 0.0207(5) 0.0070(5)
N1 0.067(2) 0.075(2) 0.067(2) -0.0071(18) 0.0144(18) 0.0173(18)
N2 0.075(2) 0.076(2) 0.065(2) -0.0080(19) 0.0270(19) 0.017(2)
N3 0.127(4) 0.131(5) 0.102(4) 0.041(3) 0.056(3) 0.047(4)
N4 0.097(4) 0.178(6) 0.082(3) -0.040(4) 0.018(3) 0.030(4)
C1 0.104(4) 0.090(4) 0.088(4) 0.011(3) 0.035(3) -0.017(3)
C2 0.073(3) 0.084(3) 0.076(3) -0.013(3) 0.002(2) -0.004(2)
C3 0.061(3) 0.106(4) 0.108(4) -0.033(4) 0.005(3) 0.005(3)
C4 0.146(8) 0.214(11) 0.225(13) -0.142(10) -0.029(8) 0.031(8)
C5 0.067(4) 0.189(9) 0.214(10) -0.054(8) -0.014(5) 0.040(5)
C6 0.117(7) 0.236(12) 0.186(10) 0.022(9) 0.019(7) -0.089(8)
C7 0.072(3) 0.076(3) 0.080(3) -0.011(2) 0.028(2) 0.014(2)
C8 0.113(5) 0.125(6) 0.141(6) -0.039(5) 0.037(5) -0.026(4)
C9 0.153(7) 0.125(6) 0.085(4) -0.014(4) 0.048(4) 0.002(5)
C10 0.121(6) 0.150(7) 0.144(7) -0.064(6) 0.007(5) 0.062(5)
C11 0.220(11) 0.216(11) 0.186(10) 0.064(9) 0.150(9) 0.039(9)
C12 0.232(12) 0.186(10) 0.154(8) 0.091(8) 0.069(8) 0.101(9)
C13 0.087(4) 0.092(4) 0.097(4) -0.024(3) 0.045(3) -0.019(3)
C14 0.150(10) 0.43(2) 0.156(10) -0.106(14) 0.031(8) -0.136(13)
C15 0.146(8) 0.186(9) 0.208(10) -0.066(8) 0.130(8) -0.058(7)
C16 0.246(15) 0.121(8) 0.36(2) 0.008(11) 0.169(16) -0.052(9)
C17 0.120(5) 0.070(3) 0.147(6) 0.010(4) 0.074(5) 0.033(3)
C18 0.231(11) 0.107(6) 0.249(12) 0.002(7) 0.140(10) 0.078(7)
C19 0.61(4) 0.252(17) 0.181(12) 0.117(12) 0.181(18) 0.28(2)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N1 1.820(4) . ?
Ti1 N2 1.822(4) . ?
Ti1 C1 2.107(5) . ?
Ti1 C2 2.107(5) . ?
P1 N1 1.551(4) . ?
P1 N3 1.684(5) . ?
P1 C3 1.841(6) . ?
P1 C7 1.852(5) . ?
P2 N2 1.546(4) . ?
P2 N4 1.738(5) . ?
P2 C17 1.786(6) . ?
P2 C13 1.815(6) . ?
N3 C11 1.409(10) . ?
N3 C12 1.468(10) . ?
N4 C22 1.435(9) . ?
N4 C21 1.474(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C6 1.508(12) . ?
C3 C5 1.538(10) . ?
C3 C4 1.574(11) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.528(9) . ?
C7 C10 1.532(8) . ?
C7 C9 1.538(9) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C16 1.440(13) . ?
C13 C14 1.453(12) . ?
C13 C15 1.526(9) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.503(6) . ?
C17 C19 1.524(8) . ?
C17 C20 1.576(8) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22D 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ti1 N2 116.90(18) . . ?
N1 Ti1 C1 108.3(2) . . ?
N2 Ti1 C1 109.6(2) . . ?
N1 Ti1 C2 109.3(2) . . ?
N2 Ti1 C2 108.1(2) . . ?
C1 Ti1 C2 103.9(2) . . ?
N1 P1 N3 110.3(2) . . ?
N1 P1 C3 109.4(3) . . ?
N3 P1 C3 108.9(3) . . ?
N1 P1 C7 109.3(2) . . ?
N3 P1 C7 106.8(3) . . ?
C3 P1 C7 112.1(3) . . ?
N2 P2 N4 110.7(2) . . ?
N2 P2 C17 108.7(3) . . ?
N4 P2 C17 108.5(4) . . ?
N2 P2 C13 109.6(2) . . ?
N4 P2 C13 109.2(3) . . ?
C17 P2 C13 110.2(3) . . ?
P1 N1 Ti1 171.5(3) . . ?
P2 N2 Ti1 178.8(3) . . ?
C11 N3 C12 112.5(7) . . ?
C11 N3 P1 121.5(6) . . ?
C12 N3 P1 125.6(6) . . ?
C22 N4 C21 115.2(9) . . ?
C22 N4 P2 116.4(8) . . ?
C21 N4 P2 123.7(5) . . ?
Ti1 C1 H1A 109.5 . . ?
Ti1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Ti1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Ti1 C2 H2A 109.5 . . ?
Ti1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Ti1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C6 C3 C5 111.9(8) . . ?
C6 C3 C4 107.0(9) . . ?
C5 C3 C4 103.9(7) . . ?
C6 C3 P1 111.5(5) . . ?
C5 C3 P1 117.0(6) . . ?
C4 C3 P1 104.5(6) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C10 109.5(6) . . ?
C8 C7 C9 100.9(6) . . ?
C10 C7 C9 111.0(6) . . ?
C8 C7 P1 107.3(4) . . ?
C10 C7 P1 116.9(4) . . ?
C9 C7 P1 109.9(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C16 C13 C14 92.4(11) . . ?
C16 C13 C15 110.5(8) . . ?
C14 C13 C15 110.6(8) . . ?
C16 C13 P2 110.7(7) . . ?
C14 C13 P2 110.2(6) . . ?
C15 C13 P2 119.2(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C19 110.6(6) . . ?
C18 C17 C20 106.5(6) . . ?
C19 C17 C20 103.4(7) . . ?
C18 C17 P2 120.1(5) . . ?
C19 C17 P2 110.1(6) . . ?
C20 C17 P2 104.7(8) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C21 H21A 109.5 . . ?
N4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 H22A 109.5 . . ?
N4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N4 C22 H22D 109.5 . . ?
H22A C22 H22D 109.5 . . ?
H22B C22 H22D 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 P1 N1 Ti1 -150.9(19) . . . . ?
C3 P1 N1 Ti1 89(2) . . . . ?
C7 P1 N1 Ti1 -34(2) . . . . ?
N2 Ti1 N1 P1 -173.2(19) . . . . ?
C1 Ti1 N1 P1 -49(2) . . . . ?
C2 Ti1 N1 P1 64(2) . . . . ?
N4 P2 N2 Ti1 6(16) . . . . ?
C17 P2 N2 Ti1 125(16) . . . . ?
C13 P2 N2 Ti1 -114(16) . . . . ?
N1 Ti1 N2 P2 24(16) . . . . ?
C1 Ti1 N2 P2 -100(16) . . . . ?
C2 Ti1 N2 P2 148(16) . . . . ?
N1 P1 N3 C11 1.5(10) . . . . ?
C3 P1 N3 C11 121.6(9) . . . . ?
C7 P1 N3 C11 -117.2(9) . . . . ?
N1 P1 N3 C12 173.4(8) . . . . ?
C3 P1 N3 C12 -66.5(9) . . . . ?
C7 P1 N3 C12 54.7(9) . . . . ?
N2 P2 N4 C22 -29.4(10) . . . . ?
C17 P2 N4 C22 -148.5(9) . . . . ?
C13 P2 N4 C22 91.4(9) . . . . ?
N2 P2 N4 C21 176.1(7) . . . . ?
C17 P2 N4 C21 56.9(8) . . . . ?
C13 P2 N4 C21 -63.1(8) . . . . ?
N1 P1 C3 C6 -58.7(7) . . . . ?
N3 P1 C3 C6 -179.4(7) . . . . ?
C7 P1 C3 C6 62.6(7) . . . . ?
N1 P1 C3 C5 170.6(6) . . . . ?
N3 P1 C3 C5 50.0(7) . . . . ?
C7 P1 C3 C5 -68.0(7) . . . . ?
N1 P1 C3 C4 56.5(7) . . . . ?
N3 P1 C3 C4 -64.2(7) . . . . ?
C7 P1 C3 C4 177.8(7) . . . . ?
N1 P1 C7 C8 -65.5(5) . . . . ?
N3 P1 C7 C8 53.9(5) . . . . ?
C3 P1 C7 C8 173.1(5) . . . . ?
N1 P1 C7 C10 171.1(6) . . . . ?
N3 P1 C7 C10 -69.5(6) . . . . ?
C3 P1 C7 C10 49.7(7) . . . . ?
N1 P1 C7 C9 43.4(5) . . . . ?
N3 P1 C7 C9 162.8(5) . . . . ?
C3 P1 C7 C9 -78.0(5) . . . . ?
N2 P2 C13 C16 45.7(9) . . . . ?
N4 P2 C13 C16 -75.7(9) . . . . ?
C17 P2 C13 C16 165.2(9) . . . . ?
N2 P2 C13 C14 -55.1(10) . . . . ?
N4 P2 C13 C14 -176.5(10) . . . . ?
C17 P2 C13 C14 64.4(10) . . . . ?
N2 P2 C13 C15 175.5(7) . . . . ?
N4 P2 C13 C15 54.1(8) . . . . ?
C17 P2 C13 C15 -65.0(8) . . . . ?
N2 P2 C17 C18 175.8(6) . . . . ?
N4 P2 C17 C18 -63.8(7) . . . . ?
C13 P2 C17 C18 55.7(7) . . . . ?
N2 P2 C17 C19 45.7(7) . . . . ?
N4 P2 C17 C19 166.1(7) . . . . ?
C13 P2 C17 C19 -74.4(7) . . . . ?
N2 P2 C17 C20 -64.8(7) . . . . ?
N4 P2 C17 C20 55.6(7) . . . . ?
C13 P2 C17 C20 175.1(7) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.553
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.103
#===END