#------------------------------------------------------------------------------
#$Date: 2018-08-12 04:57:49 +0300 (Sun, 12 Aug 2018) $
#$Revision: 209607 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/05/7030519.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7030519
loop_
_publ_author_name
'Broomfield, Lewis M.'
'Wright, Joseph A.'
'Bochmann, Manfred'
_publ_section_title
;
 Synthesis, structures and reactivity of 2-phosphorylmethyl-1H-pyrrolato
 complexes of titanium, yttrium and zinc
;
_journal_coden_ASTM              DTARAF
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              8269
_journal_page_last               8279
_journal_paper_doi               10.1039/b908394d
_journal_year                    2009
_chemical_formula_moiety         'C46 H58 N4 O2 P2 Ti, 2.5(C6 H6)'
_chemical_formula_structural     '[3-(t-Bu)-Pyr-P(O)Ph2]2Ti(NMe2)2.(2.5PhH)'
_chemical_formula_sum            'C61 H73 N4 O2 P2 Ti'
_chemical_formula_weight         1004.07
_chemical_name_common            'Compound 5c'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                108.236(9)
_cell_angle_beta                 95.852(9)
_cell_angle_gamma                107.144(9)
_cell_formula_units_Z            2
_cell_length_a                   12.1366(13)
_cell_length_b                   16.2331(17)
_cell_length_c                   16.3753(17)
_cell_measurement_reflns_used    4523
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      33.9468
_cell_measurement_theta_min      3.3565
_cell_volume                     2860.2(6)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen et al., 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1019
_diffrn_reflns_av_sigmaI/netI    0.2230
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29354
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         9990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.1815
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1165P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2274
_reflns_number_gt                3928
_reflns_number_total             9990
_reflns_threshold_expression     I>2σ(I)
_cod_duplicate_entry             7002382
_cod_data_source_file            b908394d.txt
_cod_data_source_block           5c
_cod_database_code               7030519
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ti1 Ti 0.60092(9) 0.27374(7) 0.13806(6) 0.0330(3) Uani 1 1 d .
C1 C 0.7536(5) 0.4248(4) 0.0313(3) 0.0358(14) Uani 1 1 d .
H1A H 0.7067 0.4618 0.0557 0.043 Uiso 1 1 calc R
H1B H 0.8012 0.4547 -0.0024 0.043 Uiso 1 1 calc R
C2 C 0.6735(4) 0.3302(4) -0.0281(4) 0.0290(13) Uani 1 1 d .
C3 C 0.5495(5) 0.1879(4) -0.0678(4) 0.0370(14) Uani 1 1 d .
H3 H 0.4981 0.1337 -0.0657 0.044 Uiso 1 1 calc R
C4 C 0.5772(5) 0.1989(4) -0.1450(4) 0.0334(14) Uani 1 1 d .
C5 C 0.6591(5) 0.2909(4) -0.1171(4) 0.0354(14) Uani 1 1 d .
H5 H 0.6963 0.3191 -0.1532 0.042 Uiso 1 1 calc R
C6 C 0.5335(6) 0.1303(4) -0.2375(4) 0.0458(16) Uani 1 1 d .
C7 C 0.4415(6) 0.0422(4) -0.2431(4) 0.0562(18) Uani 1 1 d .
H7A H 0.3729 0.0548 -0.2264 0.084 Uiso 1 1 calc R
H7B H 0.4724 0.0170 -0.2042 0.084 Uiso 1 1 calc R
H7C H 0.4203 -0.0014 -0.3024 0.084 Uiso 1 1 calc R
C8 C 0.4770(10) 0.1709(5) -0.2960(5) 0.117(4) Uani 1 1 d .
H8A H 0.4438 0.1250 -0.3540 0.176 Uiso 1 1 calc R
H8B H 0.5360 0.2235 -0.2993 0.176 Uiso 1 1 calc R
H8C H 0.4159 0.1895 -0.2714 0.176 Uiso 1 1 calc R
C9 C 0.6332(7) 0.1047(6) -0.2732(6) 0.119(4) Uani 1 1 d .
H9A H 0.6791 0.0926 -0.2300 0.178 Uiso 1 1 calc R
H9B H 0.6825 0.1548 -0.2868 0.178 Uiso 1 1 calc R
H9C H 0.6016 0.0504 -0.3257 0.178 Uiso 1 1 calc R
C10 C 0.9454(4) 0.5315(4) 0.1885(4) 0.0348(14) Uani 1 1 d .
C11 C 0.9703(5) 0.5545(4) 0.2784(4) 0.0375(14) Uani 1 1 d .
H11 H 0.9384 0.5097 0.3019 0.045 Uiso 1 1 calc R
C12 C 1.0407(5) 0.6411(5) 0.3340(4) 0.0492(17) Uani 1 1 d .
H12 H 1.0568 0.6548 0.3945 0.059 Uiso 1 1 calc R
C13 C 1.0881(5) 0.7088(4) 0.2994(5) 0.0515(17) Uani 1 1 d .
H13 H 1.1355 0.7682 0.3365 0.062 Uiso 1 1 calc R
C14 C 1.0641(5) 0.6868(4) 0.2100(5) 0.0496(17) Uani 1 1 d .
H14 H 1.0966 0.7319 0.1871 0.060 Uiso 1 1 calc R
C15 C 0.9942(5) 0.6009(4) 0.1536(4) 0.0405(15) Uani 1 1 d .
H15 H 0.9786 0.5878 0.0932 0.049 Uiso 1 1 calc R
C16 C 0.9352(5) 0.3533(4) 0.0679(3) 0.0345(14) Uani 1 1 d .
C17 C 0.8807(6) 0.2599(4) 0.0186(4) 0.0479(16) Uani 1 1 d .
H17 H 0.7997 0.2321 0.0110 0.057 Uiso 1 1 calc R
C18 C 0.9478(6) 0.2071(5) -0.0200(4) 0.0533(18) Uani 1 1 d .
H18 H 0.9107 0.1446 -0.0534 0.064 Uiso 1 1 calc R
C19 C 1.0678(7) 0.2471(6) -0.0088(4) 0.064(2) Uani 1 1 d .
H19 H 1.1116 0.2117 -0.0343 0.076 Uiso 1 1 calc R
C20 C 1.1230(6) 0.3400(5) 0.0404(5) 0.0595(19) Uani 1 1 d .
H20 H 1.2040 0.3673 0.0474 0.071 Uiso 1 1 calc R
C21 C 1.0577(5) 0.3926(4) 0.0793(4) 0.0444(16) Uani 1 1 d .
H21 H 1.0958 0.4548 0.1134 0.053 Uiso 1 1 calc R
C22 C 0.6554(5) 0.4905(4) 0.3158(3) 0.0353(14) Uani 1 1 d .
H22A H 0.7354 0.5026 0.3064 0.042 Uiso 1 1 calc R
H22B H 0.6545 0.5428 0.3644 0.042 Uiso 1 1 calc R
C23 C 0.6161(5) 0.4046(4) 0.3369(3) 0.0311(13) Uani 1 1 d .
C24 C 0.5617(5) 0.2573(4) 0.3179(4) 0.0431(16) Uani 1 1 d .
H24 H 0.5447 0.1939 0.2924 0.052 Uiso 1 1 calc R
C25 C 0.5482(5) 0.2998(4) 0.3997(4) 0.0448(16) Uani 1 1 d .
C26 C 0.5825(5) 0.3947(4) 0.4120(4) 0.0435(16) Uani 1 1 d .
H26 H 0.5824 0.4419 0.4619 0.052 Uiso 1 1 calc R
C27 C 0.5102(7) 0.2558(5) 0.4664(4) 0.063(2) Uani 1 1 d .
C28 C 0.4514(8) 0.3094(5) 0.5285(5) 0.089(3) Uani 1 1 d .
H28A H 0.5044 0.3719 0.5584 0.133 Uiso 1 1 calc R
H28B H 0.4311 0.2811 0.5709 0.133 Uiso 1 1 calc R
H28C H 0.3811 0.3095 0.4959 0.133 Uiso 1 1 calc R
C29 C 0.4314(9) 0.1569(5) 0.4230(5) 0.102(3) Uani 1 1 d .
H29A H 0.4119 0.1311 0.4671 0.153 Uiso 1 1 calc R
H29B H 0.4715 0.1228 0.3858 0.153 Uiso 1 1 calc R
H29C H 0.3605 0.1534 0.3882 0.153 Uiso 1 1 calc R
C30 C 0.6254(8) 0.2607(7) 0.5237(6) 0.107(3) Uani 1 1 d .
H30A H 0.6792 0.3233 0.5478 0.160 Uiso 1 1 calc R
H30B H 0.6617 0.2220 0.4877 0.160 Uiso 1 1 calc R
H30C H 0.6056 0.2396 0.5708 0.160 Uiso 1 1 calc R
C31 C 0.6117(5) 0.5741(4) 0.1890(4) 0.0334(14) Uani 1 1 d .
C32 C 0.5483(5) 0.5781(4) 0.1148(4) 0.0407(15) Uani 1 1 d .
H32 H 0.4776 0.5307 0.0835 0.049 Uiso 1 1 calc R
C33 C 0.5900(5) 0.6522(4) 0.0875(4) 0.0415(15) Uani 1 1 d .
H33 H 0.5470 0.6546 0.0385 0.050 Uiso 1 1 calc R
C34 C 0.6963(6) 0.7228(4) 0.1335(4) 0.0518(17) Uani 1 1 d .
H34 H 0.7246 0.7727 0.1157 0.062 Uiso 1 1 calc R
C35 C 0.7594(6) 0.7181(4) 0.2058(4) 0.0525(18) Uani 1 1 d .
H35 H 0.8309 0.7649 0.2361 0.063 Uiso 1 1 calc R
C36 C 0.7183(5) 0.6452(4) 0.2341(4) 0.0460(16) Uani 1 1 d .
H36 H 0.7618 0.6435 0.2833 0.055 Uiso 1 1 calc R
C37 C 0.4152(5) 0.4672(4) 0.2450(4) 0.0371(14) Uani 1 1 d .
C38 C 0.3523(5) 0.3886(5) 0.2602(4) 0.0535(18) Uani 1 1 d .
H38 H 0.3819 0.3408 0.2544 0.064 Uiso 1 1 calc R
C39 C 0.2448(6) 0.3828(5) 0.2842(4) 0.0614(19) Uani 1 1 d .
H39 H 0.2026 0.3309 0.2952 0.074 Uiso 1 1 calc R
C40 C 0.1997(6) 0.4528(6) 0.2919(4) 0.065(2) Uani 1 1 d .
H40 H 0.1278 0.4482 0.3087 0.078 Uiso 1 1 calc R
C41 C 0.2608(6) 0.5298(5) 0.2746(4) 0.0538(18) Uani 1 1 d .
H41 H 0.2290 0.5761 0.2782 0.065 Uiso 1 1 calc R
C42 C 0.3690(5) 0.5381(4) 0.2521(3) 0.0398(15) Uani 1 1 d .
H42 H 0.4110 0.5905 0.2417 0.048 Uiso 1 1 calc R
C43 C 0.3948(5) 0.1042(4) 0.1211(4) 0.0425(15) Uani 1 1 d .
H43A H 0.3513 0.1160 0.1666 0.064 Uiso 1 1 calc R
H43B H 0.4581 0.0860 0.1404 0.064 Uiso 1 1 calc R
H43C H 0.3432 0.0557 0.0690 0.064 Uiso 1 1 calc R
C44 C 0.3454(5) 0.2059(4) 0.0585(4) 0.0455(16) Uani 1 1 d .
H44A H 0.3085 0.1566 0.0028 0.068 Uiso 1 1 calc R
H44B H 0.3754 0.2633 0.0495 0.068 Uiso 1 1 calc R
H44C H 0.2886 0.2093 0.0950 0.068 Uiso 1 1 calc R
C45 C 0.7769(5) 0.2094(4) 0.2152(4) 0.0515(17) Uani 1 1 d .
H45A H 0.7616 0.1637 0.2422 0.077 Uiso 1 1 calc R
H45B H 0.7901 0.2690 0.2587 0.077 Uiso 1 1 calc R
H45C H 0.8457 0.2109 0.1907 0.077 Uiso 1 1 calc R
C46 C 0.6527(5) 0.0966(4) 0.0767(4) 0.0422(15) Uani 1 1 d .
H46A H 0.7208 0.0980 0.0514 0.063 Uiso 1 1 calc R
H46B H 0.5858 0.0831 0.0318 0.063 Uiso 1 1 calc R
H46C H 0.6369 0.0496 0.1022 0.063 Uiso 1 1 calc R
N1 N 0.6076(4) 0.2676(3) 0.0060(3) 0.0310(11) Uani 1 1 d .
N2 N 0.6037(4) 0.3189(3) 0.2765(3) 0.0380(12) Uani 1 1 d .
N3 N 0.4431(4) 0.1880(3) 0.1019(3) 0.0344(11) Uani 1 1 d .
N4 N 0.6746(4) 0.1862(3) 0.1448(3) 0.0347(11) Uani 1 1 d .
O1 O 0.7753(3) 0.3748(2) 0.1737(2) 0.0336(9) Uani 1 1 d .
O2 O 0.5491(3) 0.3891(2) 0.1446(2) 0.0324(9) Uani 1 1 d .
P1 P 0.84824(13) 0.41858(10) 0.11903(10) 0.0341(4) Uani 1 1 d .
P2 P 0.55776(13) 0.47510(10) 0.21866(10) 0.0331(4) Uani 1 1 d .
C47 C 0.0083(8) 0.5870(6) 0.5514(5) 0.077(2) Uani 1 1 d .
H47 H 0.0123 0.6459 0.5860 0.092 Uiso 1 1 calc R
C48 C 0.1093(7) 0.5662(6) 0.5481(5) 0.067(2) Uani 1 1 d .
H48 H 0.1824 0.6098 0.5800 0.080 Uiso 1 1 calc R
C49 C -0.0991(7) 0.5219(7) 0.5044(5) 0.074(2) Uani 1 1 d .
H49 H -0.1667 0.5376 0.5079 0.089 Uiso 1 1 calc R
C50 C 1.0487(10) 0.0067(9) 0.2649(6) 0.290(12) Uani 1 1 d G
H50 H 1.0811 -0.0036 0.3131 0.349 Uiso 1 1 calc R
C51 C 1.1220(6) 0.0534(9) 0.2217(7) 0.264(11) Uani 1 1 d G
H51 H 1.2035 0.0742 0.2410 0.317 Uiso 1 1 calc R
C52 C 1.0735(7) 0.0688(6) 0.1497(7) 0.188(6) Uani 1 1 d G
H52 H 1.1226 0.1000 0.1208 0.225 Uiso 1 1 calc R
C53 C 0.9517(7) 0.0377(6) 0.1208(5) 0.126(4) Uani 1 1 d G
H53 H 0.9193 0.0480 0.0726 0.152 Uiso 1 1 calc R
C54 C 0.8784(5) -0.0090(5) 0.1640(6) 0.100(3) Uani 1 1 d G
H54 H 0.7969 -0.0298 0.1447 0.120 Uiso 1 1 calc R
C55 C 0.9268(9) -0.0244(6) 0.2361(6) 0.191(6) Uani 1 1 d G
H55 H 0.8778 -0.0556 0.2650 0.229 Uiso 1 1 calc R
C56 C 0.8888(12) 0.0598(7) 0.5443(8) 0.330(11) Uiso 1 1 d G
H56 H 0.8477 0.0185 0.5686 0.396 Uiso 1 1 calc R
C57 C 1.0108(12) 0.1005(8) 0.5709(6) 0.263(8) Uiso 1 1 d G
H57 H 1.0515 0.0865 0.6130 0.315 Uiso 1 1 calc R
C58 C 1.0722(7) 0.1622(7) 0.5347(7) 0.161(5) Uiso 1 1 d G
H58 H 1.1539 0.1894 0.5525 0.194 Uiso 1 1 calc R
C59 C 1.0115(10) 0.1831(6) 0.4718(7) 0.289(9) Uiso 1 1 d G
H59 H 1.0525 0.2244 0.4475 0.346 Uiso 1 1 calc R
C60 C 0.8894(10) 0.1424(8) 0.4451(6) 0.173(5) Uiso 1 1 d G
H60 H 0.8488 0.1564 0.4030 0.207 Uiso 1 1 calc R
C61 C 0.8281(7) 0.0807(7) 0.4814(8) 0.218(6) Uiso 1 1 d G
H61 H 0.7464 0.0535 0.4636 0.261 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 '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'
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
N3 Ti1 N4 95.88(19) . .
N3 Ti1 O2 94.11(16) . .
N4 Ti1 O2 169.56(17) . .
N3 Ti1 N1 91.92(17) . .
N4 Ti1 N1 100.20(18) . .
O2 Ti1 N1 82.44(14) . .
N3 Ti1 N2 96.07(18) . .
N4 Ti1 N2 92.30(18) . .
O2 Ti1 N2 83.63(15) . .
N1 Ti1 N2 164.40(17) . .
N3 Ti1 O1 176.36(16) . .
N4 Ti1 O1 87.13(16) . .
O2 Ti1 O1 83.00(13) . .
N1 Ti1 O1 85.53(15) . .
N2 Ti1 O1 85.83(15) . .
C2 C1 P1 110.7(3) . .
C2 C1 H1A 109.5 . .
P1 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
P1 C1 H1B 109.5 . .
H1A C1 H1B 108.1 . .
C5 C2 N1 111.2(5) . .
C5 C2 C1 127.7(5) . .
N1 C2 C1 121.0(5) . .
C4 C3 N1 112.2(5) . .
C4 C3 H3 123.9 . .
N1 C3 H3 123.9 . .
C3 C4 C5 104.6(5) . .
C3 C4 C6 128.7(5) . .
C5 C4 C6 126.7(5) . .
C2 C5 C4 108.0(5) . .
C2 C5 H5 126.0 . .
C4 C5 H5 126.0 . .
C4 C6 C7 112.1(5) . .
C4 C6 C9 110.6(5) . .
C7 C6 C9 106.9(6) . .
C4 C6 C8 109.8(5) . .
C7 C6 C8 107.3(6) . .
C9 C6 C8 110.0(7) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 C15 118.4(5) . .
C11 C10 P1 120.0(4) . .
C15 C10 P1 121.5(4) . .
C12 C11 C10 121.8(6) . .
C12 C11 H11 119.1 . .
C10 C11 H11 119.1 . .
C11 C12 C13 119.4(6) . .
C11 C12 H12 120.3 . .
C13 C12 H12 120.3 . .
C14 C13 C12 119.3(6) . .
C14 C13 H13 120.4 . .
C12 C13 H13 120.4 . .
C15 C14 C13 122.1(6) . .
C15 C14 H14 119.0 . .
C13 C14 H14 119.0 . .
C14 C15 C10 119.0(6) . .
C14 C15 H15 120.5 . .
C10 C15 H15 120.5 . .
C17 C16 C21 118.5(5) . .
C17 C16 P1 119.3(4) . .
C21 C16 P1 122.2(5) . .
C16 C17 C18 120.1(6) . .
C16 C17 H17 120.0 . .
C18 C17 H17 120.0 . .
C19 C18 C17 120.6(6) . .
C19 C18 H18 119.7 . .
C17 C18 H18 119.7 . .
C18 C19 C20 119.9(6) . .
C18 C19 H19 120.1 . .
C20 C19 H19 120.1 . .
C19 C20 C21 120.0(6) . .
C19 C20 H20 120.0 . .
C21 C20 H20 120.0 . .
C20 C21 C16 120.9(6) . .
C20 C21 H21 119.5 . .
C16 C21 H21 119.5 . .
C23 C22 P2 108.8(4) . .
C23 C22 H22A 109.9 . .
P2 C22 H22A 109.9 . .
C23 C22 H22B 109.9 . .
P2 C22 H22B 109.9 . .
H22A C22 H22B 108.3 . .
C26 C23 N2 109.7(5) . .
C26 C23 C22 128.6(5) . .
N2 C23 C22 121.7(5) . .
C25 C24 N2 112.4(5) . .
C25 C24 H24 123.8 . .
N2 C24 H24 123.8 . .
C24 C25 C26 105.4(5) . .
C24 C25 C27 127.5(6) . .
C26 C25 C27 127.0(5) . .
C23 C26 C25 107.8(5) . .
C23 C26 H26 126.1 . .
C25 C26 H26 126.1 . .
C29 C27 C28 110.3(7) . .
C29 C27 C25 112.0(5) . .
C28 C27 C25 111.7(6) . .
C29 C27 C30 109.0(7) . .
C28 C27 C30 106.6(6) . .
C25 C27 C30 107.1(6) . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C27 C29 H29A 109.5 . .
C27 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C27 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C27 C30 H30A 109.5 . .
C27 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
C27 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C36 C31 C32 118.8(5) . .
C36 C31 P2 122.2(4) . .
C32 C31 P2 118.9(4) . .
C33 C32 C31 120.6(5) . .
C33 C32 H32 119.7 . .
C31 C32 H32 119.7 . .
C32 C33 C34 119.9(5) . .
C32 C33 H33 120.0 . .
C34 C33 H33 120.0 . .
C35 C34 C33 119.4(6) . .
C35 C34 H34 120.3 . .
C33 C34 H34 120.3 . .
C34 C35 C36 121.2(6) . .
C34 C35 H35 119.4 . .
C36 C35 H35 119.4 . .
C35 C36 C31 120.1(6) . .
C35 C36 H36 120.0 . .
C31 C36 H36 120.0 . .
C38 C37 C42 120.2(5) . .
C38 C37 P2 117.9(4) . .
C42 C37 P2 121.9(5) . .
C39 C38 C37 118.9(6) . .
C39 C38 H38 120.6 . .
C37 C38 H38 120.6 . .
C40 C39 C38 120.9(6) . .
C40 C39 H39 119.5 . .
C38 C39 H39 119.5 . .
C39 C40 C41 120.2(6) . .
C39 C40 H40 119.9 . .
C41 C40 H40 119.9 . .
C42 C41 C40 120.1(6) . .
C42 C41 H41 120.0 . .
C40 C41 H41 120.0 . .
C41 C42 C37 119.7(6) . .
C41 C42 H42 120.2 . .
C37 C42 H42 120.2 . .
N3 C43 H43A 109.5 . .
N3 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
N3 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
N3 C44 H44A 109.5 . .
N3 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
N3 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
N4 C45 H45A 109.5 . .
N4 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
N4 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
N4 C46 H46A 109.5 . .
N4 C46 H46B 109.5 . .
H46A C46 H46B 109.5 . .
N4 C46 H46C 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
C3 N1 C2 104.0(4) . .
C3 N1 Ti1 123.2(3) . .
C2 N1 Ti1 132.4(4) . .
C24 N2 C23 104.7(4) . .
C24 N2 Ti1 122.1(4) . .
C23 N2 Ti1 131.5(3) . .
C43 N3 C44 108.6(4) . .
C43 N3 Ti1 128.5(4) . .
C44 N3 Ti1 122.4(3) . .
C46 N4 C45 111.1(4) . .
C46 N4 Ti1 126.0(4) . .
C45 N4 Ti1 122.2(3) . .
P1 O1 Ti1 130.7(2) . .
P2 O2 Ti1 133.6(2) . .
O1 P1 C10 108.8(2) . .
O1 P1 C1 110.1(2) . .
C10 P1 C1 110.5(2) . .
O1 P1 C16 112.7(2) . .
C10 P1 C16 108.5(3) . .
C1 P1 C16 106.2(2) . .
O2 P2 C31 110.3(2) . .
O2 P2 C22 110.8(2) . .
C31 P2 C22 108.6(3) . .
O2 P2 C37 110.5(2) . .
C31 P2 C37 109.1(3) . .
C22 P2 C37 107.5(3) . .
C48 C47 C49 120.7(8) . .
C48 C47 H47 119.7 . .
C49 C47 H47 119.7 . .
C47 C48 C49 117.6(8) . 2_566
C47 C48 H48 121.2 . .
C49 C48 H48 121.2 2_566 .
C47 C49 C48 121.7(8) . 2_566
C47 C49 H49 119.2 . .
C48 C49 H49 119.2 2_566 .
C51 C50 C55 120.0 . .
C51 C50 H50 120.0 . .
C55 C50 H50 120.0 . .
C52 C51 C50 120.0 . .
C52 C51 H51 120.0 . .
C50 C51 H51 120.0 . .
C51 C52 C53 120.0 . .
C51 C52 H52 120.0 . .
C53 C52 H52 120.0 . .
C54 C53 C52 120.0 . .
C54 C53 H53 120.0 . .
C52 C53 H53 120.0 . .
C53 C54 C55 120.0 . .
C53 C54 H54 120.0 . .
C55 C54 H54 120.0 . .
C54 C55 C50 120.0 . .
C54 C55 H55 120.0 . .
C50 C55 H55 120.0 . .
C57 C56 C61 120.0 . .
C57 C56 H56 120.0 . .
C61 C56 H56 120.0 . .
C56 C57 C58 120.0 . .
C56 C57 H57 120.0 . .
C58 C57 H57 120.0 . .
C57 C58 C59 120.0 . .
C57 C58 H58 120.0 . .
C59 C58 H58 120.0 . .
C60 C59 C58 120.0 . .
C60 C59 H59 120.0 . .
C58 C59 H59 120.0 . .
C59 C60 C61 120.0 . .
C59 C60 H60 120.0 . .
C61 C60 H60 120.0 . .
C60 C61 C56 120.0 . .
C60 C61 H61 120.0 . .
C56 C61 H61 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N3 1.907(4) .
Ti1 N4 1.913(4) .
Ti1 O2 2.120(3) .
Ti1 N1 2.144(4) .
Ti1 N2 2.146(5) .
Ti1 O1 2.148(3) .
C1 C2 1.497(7) .
C1 P1 1.794(5) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C5 1.365(7) .
C2 N1 1.397(6) .
C3 C4 1.392(7) .
C3 N1 1.393(6) .
C3 H3 0.9300 .
C4 C5 1.426(7) .
C4 C6 1.499(7) .
C5 H5 0.9300 .
C6 C7 1.502(8) .
C6 C9 1.506(9) .
C6 C8 1.532(9) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
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 C11 1.378(7) .
C10 C15 1.422(7) .
C10 P1 1.787(6) .
C11 C12 1.367(8) .
C11 H11 0.9300 .
C12 C13 1.394(8) .
C12 H12 0.9300 .
C13 C14 1.371(8) .
C13 H13 0.9300 .
C14 C15 1.361(8) .
C14 H14 0.9300 .
C15 H15 0.9300 .
C16 C17 1.387(7) .
C16 C21 1.401(8) .
C16 P1 1.795(6) .
C17 C18 1.404(8) .
C17 H17 0.9300 .
C18 C19 1.374(9) .
C18 H18 0.9300 .
C19 C20 1.380(9) .
C19 H19 0.9300 .
C20 C21 1.387(8) .
C20 H20 0.9300 .
C21 H21 0.9300 .
C22 C23 1.495(7) .
C22 P2 1.786(5) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 C26 1.376(7) .
C23 N2 1.385(6) .
C24 C25 1.353(8) .
C24 N2 1.384(6) .
C24 H24 0.9300 .
C25 C26 1.413(7) .
C25 C27 1.520(8) .
C26 H26 0.9300 .
C27 C29 1.496(9) .
C27 C28 1.503(10) .
C27 C30 1.570(10) .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C30 H30A 0.9600 .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
C31 C36 1.394(7) .
C31 C32 1.400(7) .
C31 P2 1.783(6) .
C32 C33 1.388(7) .
C32 H32 0.9300 .
C33 C34 1.391(8) .
C33 H33 0.9300 .
C34 C35 1.377(8) .
C34 H34 0.9300 .
C35 C36 1.382(7) .
C35 H35 0.9300 .
C36 H36 0.9300 .
C37 C38 1.391(8) .
C37 C42 1.402(7) .
C37 P2 1.803(6) .
C38 C39 1.386(8) .
C38 H38 0.9300 .
C39 C40 1.378(9) .
C39 H39 0.9300 .
C40 C41 1.382(9) .
C40 H40 0.9300 .
C41 C42 1.379(8) .
C41 H41 0.9300 .
C42 H42 0.9300 .
C43 N3 1.458(6) .
C43 H43A 0.9600 .
C43 H43B 0.9600 .
C43 H43C 0.9600 .
C44 N3 1.467(6) .
C44 H44A 0.9600 .
C44 H44B 0.9600 .
C44 H44C 0.9600 .
C45 N4 1.474(7) .
C45 H45A 0.9600 .
C45 H45B 0.9600 .
C45 H45C 0.9600 .
C46 N4 1.458(6) .
C46 H46A 0.9600 .
C46 H46B 0.9600 .
C46 H46C 0.9600 .
O1 P1 1.510(3) .
O2 P2 1.503(4) .
C47 C48 1.367(10) .
C47 C49 1.372(10) .
C47 H47 0.9300 .
C48 C49 1.379(10) 2_566
C48 H48 0.9300 .
C49 C48 1.379(10) 2_566
C49 H49 0.9300 .
C50 C51 1.3900 .
C50 C55 1.3900 .
C50 H50 0.9300 .
C51 C52 1.3900 .
C51 H51 0.9300 .
C52 C53 1.3900 .
C52 H52 0.9300 .
C53 C54 1.3900 .
C53 H53 0.9300 .
C54 C55 1.3900 .
C54 H54 0.9300 .
C55 H55 0.9300 .
C56 C57 1.3900 .
C56 C61 1.3900 .
C56 H56 0.9300 .
C57 C58 1.3900 .
C57 H57 0.9300 .
C58 C59 1.3900 .
C58 H58 0.9300 .
C59 C60 1.3900 .
C59 H59 0.9300 .
C60 C61 1.3900 .
C60 H60 0.9300 .
C61 H61 0.9300 .
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_4
P1 C1 C2 C5 -125.5(5) .
P1 C1 C2 N1 50.0(6) .
N1 C3 C4 C5 0.9(6) .
N1 C3 C4 C6 -179.9(5) .
N1 C2 C5 C4 2.0(6) .
C1 C2 C5 C4 177.9(5) .
C3 C4 C5 C2 -1.7(6) .
C6 C4 C5 C2 179.0(5) .
C3 C4 C6 C7 4.8(8) .
C5 C4 C6 C7 -176.2(5) .
C3 C4 C6 C9 -114.4(7) .
C5 C4 C6 C9 64.6(8) .
C3 C4 C6 C8 123.9(7) .
C5 C4 C6 C8 -57.0(8) .
C15 C10 C11 C12 -0.5(8) .
P1 C10 C11 C12 -177.5(4) .
C10 C11 C12 C13 0.5(9) .
C11 C12 C13 C14 -0.6(9) .
C12 C13 C14 C15 0.6(9) .
C13 C14 C15 C10 -0.6(9) .
C11 C10 C15 C14 0.5(8) .
P1 C10 C15 C14 177.5(4) .
C21 C16 C17 C18 -1.1(8) .
P1 C16 C17 C18 -178.3(4) .
C16 C17 C18 C19 0.5(9) .
C17 C18 C19 C20 -0.3(10) .
C18 C19 C20 C21 0.8(10) .
C19 C20 C21 C16 -1.5(9) .
C17 C16 C21 C20 1.6(8) .
P1 C16 C21 C20 178.7(4) .
P2 C22 C23 C26 -120.6(6) .
P2 C22 C23 N2 56.3(6) .
N2 C24 C25 C26 0.5(7) .
N2 C24 C25 C27 -176.6(6) .
N2 C23 C26 C25 0.4(6) .
C22 C23 C26 C25 177.5(5) .
C24 C25 C26 C23 -0.5(7) .
C27 C25 C26 C23 176.6(6) .
C24 C25 C27 C29 -29.0(10) .
C26 C25 C27 C29 154.4(7) .
C24 C25 C27 C28 -153.2(7) .
C26 C25 C27 C28 30.2(10) .
C24 C25 C27 C30 90.4(8) .
C26 C25 C27 C30 -86.1(8) .
C36 C31 C32 C33 -1.0(8) .
P2 C31 C32 C33 -177.3(4) .
C31 C32 C33 C34 0.7(8) .
C32 C33 C34 C35 0.2(9) .
C33 C34 C35 C36 -0.8(10) .
C34 C35 C36 C31 0.5(10) .
C32 C31 C36 C35 0.4(8) .
P2 C31 C36 C35 176.6(5) .
C42 C37 C38 C39 -1.3(9) .
P2 C37 C38 C39 177.3(5) .
C37 C38 C39 C40 0.8(10) .
C38 C39 C40 C41 0.7(11) .
C39 C40 C41 C42 -1.9(10) .
C40 C41 C42 C37 1.4(9) .
C38 C37 C42 C41 0.2(8) .
P2 C37 C42 C41 -178.3(4) .
C4 C3 N1 C2 0.3(6) .
C4 C3 N1 Ti1 -173.8(3) .
C5 C2 N1 C3 -1.4(6) .
C1 C2 N1 C3 -177.6(4) .
C5 C2 N1 Ti1 171.9(4) .
C1 C2 N1 Ti1 -4.2(7) .
N3 Ti1 N1 C3 -33.5(4) .
N4 Ti1 N1 C3 62.8(4) .
O2 Ti1 N1 C3 -127.4(4) .
N2 Ti1 N1 C3 -154.4(6) .
O1 Ti1 N1 C3 149.1(4) .
N3 Ti1 N1 C2 154.2(4) .
N4 Ti1 N1 C2 -109.5(4) .
O2 Ti1 N1 C2 60.3(4) .
N2 Ti1 N1 C2 33.3(9) .
O1 Ti1 N1 C2 -23.2(4) .
C25 C24 N2 C23 -0.3(7) .
C25 C24 N2 Ti1 -166.8(4) .
C26 C23 N2 C24 -0.1(6) .
C22 C23 N2 C24 -177.5(5) .
C26 C23 N2 Ti1 164.6(4) .
C22 C23 N2 Ti1 -12.8(7) .
N3 Ti1 N2 C24 45.7(4) .
N4 Ti1 N2 C24 -50.5(4) .
O2 Ti1 N2 C24 139.2(4) .
N1 Ti1 N2 C24 166.1(6) .
O1 Ti1 N2 C24 -137.4(4) .
N3 Ti1 N2 C23 -116.8(5) .
N4 Ti1 N2 C23 147.0(5) .
O2 Ti1 N2 C23 -23.3(5) .
N1 Ti1 N2 C23 3.6(9) .
O1 Ti1 N2 C23 60.1(5) .
N4 Ti1 N3 C43 29.0(5) .
O2 Ti1 N3 C43 -148.0(4) .
N1 Ti1 N3 C43 129.5(4) .
N2 Ti1 N3 C43 -63.9(5) .
N4 Ti1 N3 C44 -160.1(4) .
O2 Ti1 N3 C44 22.9(4) .
N1 Ti1 N3 C44 -59.6(4) .
N2 Ti1 N3 C44 106.9(4) .
N3 Ti1 N4 C46 49.9(4) .
O2 Ti1 N4 C46 -147.0(8) .
N1 Ti1 N4 C46 -43.1(4) .
N2 Ti1 N4 C46 146.2(4) .
O1 Ti1 N4 C46 -128.1(4) .
N3 Ti1 N4 C45 -141.0(4) .
O2 Ti1 N4 C45 22.2(12) .
N1 Ti1 N4 C45 126.0(4) .
N2 Ti1 N4 C45 -44.6(4) .
O1 Ti1 N4 C45 41.1(4) .
N4 Ti1 O1 P1 105.4(3) .
O2 Ti1 O1 P1 -78.0(3) .
N1 Ti1 O1 P1 4.9(3) .
N2 Ti1 O1 P1 -162.1(3) .
N3 Ti1 O2 P2 114.6(3) .
N4 Ti1 O2 P2 -48.6(11) .
N1 Ti1 O2 P2 -154.1(3) .
N2 Ti1 O2 P2 18.9(3) .
O1 Ti1 O2 P2 -67.7(3) .
Ti1 O1 P1 C10 151.2(3) .
Ti1 O1 P1 C1 29.9(4) .
Ti1 O1 P1 C16 -88.5(3) .
C11 C10 P1 O1 19.1(5) .
C15 C10 P1 O1 -157.8(4) .
C11 C10 P1 C1 140.1(4) .
C15 C10 P1 C1 -36.8(5) .
C11 C10 P1 C16 -103.8(4) .
C15 C10 P1 C16 79.2(5) .
C2 C1 P1 O1 -60.8(4) .
C2 C1 P1 C10 178.9(4) .
C2 C1 P1 C16 61.5(4) .
C17 C16 P1 O1 52.1(5) .
C21 C16 P1 O1 -124.9(4) .
C17 C16 P1 C10 172.7(4) .
C21 C16 P1 C10 -4.4(5) .
C17 C16 P1 C1 -68.5(5) .
C21 C16 P1 C1 114.4(5) .
Ti1 O2 P2 C31 133.6(3) .
Ti1 O2 P2 C22 13.3(4) .
Ti1 O2 P2 C37 -105.7(3) .
C36 C31 P2 O2 -117.1(5) .
C32 C31 P2 O2 59.1(5) .
C36 C31 P2 C22 4.5(5) .
C32 C31 P2 C22 -179.3(4) .
C36 C31 P2 C37 121.3(5) .
C32 C31 P2 C37 -62.5(5) .
C23 C22 P2 O2 -54.2(4) .
C23 C22 P2 C31 -175.5(4) .
C23 C22 P2 C37 66.5(4) .
C38 C37 P2 O2 51.4(5) .
C42 C37 P2 O2 -130.0(4) .
C38 C37 P2 C31 172.9(4) .
C42 C37 P2 C31 -8.5(6) .
C38 C37 P2 C22 -69.5(5) .
C42 C37 P2 C22 109.0(5) .
C49 C47 C48 C49 0.3(12) 2_566
C48 C47 C49 C48 -0.3(12) 2_566
C55 C50 C51 C52 0.0 .
C50 C51 C52 C53 0.0 .
C51 C52 C53 C54 0.0 .
C52 C53 C54 C55 0.0 .
C53 C54 C55 C50 0.0 .
C51 C50 C55 C54 0.0 .
C61 C56 C57 C58 0.0 .
C56 C57 C58 C59 0.0 .
C57 C58 C59 C60 0.0 .
C58 C59 C60 C61 0.0 .
C59 C60 C61 C56 0.0 .
C57 C56 C61 C60 0.0 .
