#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:23:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180137 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/34/7103465.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_7103465
loop_
_publ_author_name
'Selby, Jonathan D'
'Schulten, Christian'
'Schwarz, Andrew D'
'Stasch, Andreas'
'Clot, Eric'
'Jones, Cameron'
'Mountford, Philip'
_publ_section_title
;
 Cycloaddition reactions of transition metal hydrazides with alkynes
 and heteroalkynes: coupling of Ti=NNPh2 with PhCCMe, PhCCH, MeCN and
 tBuCP.
;
_journal_issue                   41
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5101
_journal_page_last               5103
_journal_paper_doi               10.1039/b813911c
_journal_year                    2008
_chemical_formula_sum            'C27 H29 N2 P Ti'
_chemical_formula_weight         460.39
_chemical_name_systematic
;
Cp2Ti{N(NPh2)PCtBu}
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.654(3)
_cell_length_b                   9.4448(19)
_cell_length_c                   16.641(3)
_cell_measurement_temperature    123(2)
_cell_volume                     2303.1(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9086
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0388
_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)+(0.0491P)²+1.2132P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                3892
_reflns_number_total             4906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813911c.txt
_cod_data_source_block           Compound_7
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7103465
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'
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 0.27106(2) 0.18615(4) -0.00085(2) 0.01766(11) Uani 1 1 d . . .
P1 P 0.30465(3) 0.24674(5) 0.16544(3) 0.02014(13) Uani 1 1 d . . .
N1 N 0.21731(10) 0.15564(16) 0.08894(11) 0.0197(4) Uani 1 1 d . . .
C1 C 0.36252(13) 0.3007(2) 0.10320(13) 0.0203(4) Uani 1 1 d . . .
N2 N 0.15298(11) 0.08464(16) 0.11492(12) 0.0228(4) Uani 1 1 d . . .
C2 C 0.44484(14) 0.3997(2) 0.13470(15) 0.0293(5) Uani 1 1 d . . .
C3 C 0.4929(2) 0.3916(4) 0.23184(17) 0.0604(9) Uani 1 1 d . . .
H3A H 0.4501 0.4182 0.2603 0.091 Uiso 1 1 calc R . .
H3B H 0.5449 0.4568 0.2494 0.091 Uiso 1 1 calc R . .
H3C H 0.5145 0.2948 0.2482 0.091 Uiso 1 1 calc R . .
C4 C 0.51357(15) 0.3617(3) 0.09119(19) 0.0426(6) Uani 1 1 d . . .
H4A H 0.5370 0.2659 0.1082 0.064 Uiso 1 1 calc R . .
H4B H 0.5643 0.4293 0.1089 0.064 Uiso 1 1 calc R . .
H4C H 0.4833 0.3657 0.0287 0.064 Uiso 1 1 calc R . .
C5 C 0.41369(16) 0.5533(2) 0.11099(18) 0.0403(6) Uani 1 1 d . . .
H5A H 0.3828 0.5608 0.0487 0.060 Uiso 1 1 calc R . .
H5B H 0.4669 0.6161 0.1292 0.060 Uiso 1 1 calc R . .
H5C H 0.3715 0.5810 0.1399 0.060 Uiso 1 1 calc R . .
C6 C 0.16854(12) -0.06226(19) 0.13540(13) 0.0198(4) Uani 1 1 d . . .
C7 C 0.11783(13) -0.1624(2) 0.07723(14) 0.0224(4) Uani 1 1 d . . .
H7 H 0.0733 -0.1334 0.0244 0.027 Uiso 1 1 calc R . .
C8 C 0.13256(14) -0.3055(2) 0.09659(15) 0.0253(5) Uani 1 1 d . . .
H8 H 0.0975 -0.3744 0.0571 0.030 Uiso 1 1 calc R . .
C9 C 0.19771(13) -0.3481(2) 0.17283(14) 0.0245(5) Uani 1 1 d . . .
H9 H 0.2078 -0.4461 0.1855 0.029 Uiso 1 1 calc R . .
C10 C 0.24875(14) -0.2477(2) 0.23121(14) 0.0259(5) Uani 1 1 d . . .
H10 H 0.2936 -0.2771 0.2837 0.031 Uiso 1 1 calc R . .
C11 C 0.23398(13) -0.1044(2) 0.21257(14) 0.0228(4) Uani 1 1 d . . .
H11 H 0.2685 -0.0355 0.2524 0.027 Uiso 1 1 calc R . .
C12 C 0.08612(12) 0.15931(19) 0.13430(13) 0.0182(4) Uani 1 1 d . . .
C13 C 0.02625(12) 0.0880(2) 0.16656(13) 0.0205(4) Uani 1 1 d . . .
H13 H 0.0323 -0.0112 0.1764 0.025 Uiso 1 1 calc R . .
C14 C -0.04174(13) 0.1621(2) 0.18415(14) 0.0234(4) Uani 1 1 d . . .
H14 H -0.0815 0.1127 0.2063 0.028 Uiso 1 1 calc R . .
C15 C -0.05286(13) 0.3068(2) 0.17000(14) 0.0246(4) Uani 1 1 d . . .
H15 H -0.1003 0.3563 0.1811 0.030 Uiso 1 1 calc R . .
C16 C 0.00700(13) 0.3774(2) 0.13923(14) 0.0235(4) Uani 1 1 d . . .
H16 H 0.0007 0.4767 0.1300 0.028 Uiso 1 1 calc R . .
C17 C 0.07586(13) 0.30615(19) 0.12173(13) 0.0194(4) Uani 1 1 d . . .
H17 H 0.1163 0.3570 0.1011 0.023 Uiso 1 1 calc R . .
C18 C 0.29646(17) 0.0099(3) -0.09531(16) 0.0368(6) Uani 1 1 d . . .
H18 H 0.2648 0.0154 -0.1555 0.044 Uiso 1 1 calc R . .
C19 C 0.26720(15) -0.0627(2) -0.03669(16) 0.0318(5) Uani 1 1 d . . .
H19 H 0.2114 -0.1132 -0.0498 0.038 Uiso 1 1 calc R . .
C20 C 0.33441(14) -0.0482(2) 0.04503(15) 0.0269(5) Uani 1 1 d . . .
H20 H 0.3328 -0.0889 0.0967 0.032 Uiso 1 1 calc R . .
C21 C 0.40426(14) 0.0365(2) 0.03717(15) 0.0297(5) Uani 1 1 d . . .
H21 H 0.4581 0.0644 0.0826 0.036 Uiso 1 1 calc R . .
C22 C 0.38091(16) 0.0734(2) -0.04982(17) 0.0359(6) Uani 1 1 d . . .
H22 H 0.4159 0.1308 -0.0736 0.043 Uiso 1 1 calc R . .
C23 C 0.14851(14) 0.2347(2) -0.13252(14) 0.0281(5) Uani 1 1 d . . .
H23 H 0.1151 0.1572 -0.1650 0.034 Uiso 1 1 calc R . .
C24 C 0.12896(14) 0.3075(2) -0.06720(15) 0.0272(5) Uani 1 1 d . . .
H24 H 0.0791 0.2893 -0.0487 0.033 Uiso 1 1 calc R . .
C25 C 0.19628(14) 0.4118(2) -0.03421(14) 0.0266(5) Uani 1 1 d . . .
H25 H 0.2005 0.4755 0.0112 0.032 Uiso 1 1 calc R . .
C26 C 0.25624(15) 0.4054(2) -0.08025(14) 0.0278(5) Uani 1 1 d . . .
H26 H 0.3080 0.4642 -0.0715 0.033 Uiso 1 1 calc R . .
C27 C 0.22647(15) 0.2975(2) -0.14093(14) 0.0288(5) Uani 1 1 d . . .
H27 H 0.2541 0.2709 -0.1811 0.035 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'
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
_geom_angle_publ_flag
N1 Ti1 C1 78.54(7) . . ?
N1 Ti1 C23 107.61(8) . . ?
C1 Ti1 C23 138.14(8) . . ?
N1 Ti1 C22 137.68(8) . . ?
C1 Ti1 C22 98.38(8) . . ?
C23 Ti1 C22 102.33(9) . . ?
N1 Ti1 C24 81.09(7) . . ?
C1 Ti1 C24 112.55(8) . . ?
C23 Ti1 C24 34.17(8) . . ?
C22 Ti1 C24 135.73(9) . . ?
N1 Ti1 C25 90.09(7) . . ?
C1 Ti1 C25 82.51(8) . . ?
C23 Ti1 C25 56.64(7) . . ?
C22 Ti1 C25 131.75(8) . . ?
C24 Ti1 C25 34.06(7) . . ?
N1 Ti1 C21 105.96(8) . . ?
C1 Ti1 C21 79.12(8) . . ?
C23 Ti1 C21 133.83(8) . . ?
C22 Ti1 C21 34.02(8) . . ?
C24 Ti1 C21 167.67(8) . . ?
C25 Ti1 C21 152.50(8) . . ?
N1 Ti1 C18 127.04(8) . . ?
C1 Ti1 C18 131.76(8) . . ?
C23 Ti1 C18 78.39(8) . . ?
C22 Ti1 C18 33.96(8) . . ?
C24 Ti1 C18 111.58(9) . . ?
C25 Ti1 C18 129.76(8) . . ?
C21 Ti1 C18 56.09(8) . . ?
N1 Ti1 C19 93.69(8) . . ?
C1 Ti1 C19 130.51(8) . . ?
C23 Ti1 C19 91.02(8) . . ?
C22 Ti1 C19 56.17(8) . . ?
C24 Ti1 C19 114.32(8) . . ?
C25 Ti1 C19 146.85(8) . . ?
C21 Ti1 C19 55.94(8) . . ?
C18 Ti1 C19 33.52(8) . . ?
N1 Ti1 C26 123.52(7) . . ?
C1 Ti1 C26 85.22(8) . . ?
C23 Ti1 C26 56.31(7) . . ?
C22 Ti1 C26 97.86(8) . . ?
C24 Ti1 C26 56.31(7) . . ?
C25 Ti1 C26 33.90(7) . . ?
C21 Ti1 C26 123.49(8) . . ?
C18 Ti1 C26 103.89(8) . . ?
C19 Ti1 C26 134.92(8) . . ?
N1 Ti1 C27 137.27(7) . . ?
C1 Ti1 C27 116.61(8) . . ?
C23 Ti1 C27 33.95(8) . . ?
C22 Ti1 C27 82.19(8) . . ?
C24 Ti1 C27 56.19(8) . . ?
C25 Ti1 C27 56.00(8) . . ?
C21 Ti1 C27 115.86(8) . . ?
C18 Ti1 C27 74.40(8) . . ?
C19 Ti1 C27 102.15(8) . . ?
C26 Ti1 C27 33.42(7) . . ?
N1 Ti1 C20 82.26(7) . . ?
C1 Ti1 C20 97.16(8) . . ?
C23 Ti1 C20 124.57(8) . . ?
C22 Ti1 C20 56.01(8) . . ?
C24 Ti1 C20 141.99(7) . . ?
C25 Ti1 C20 172.24(8) . . ?
C21 Ti1 C20 33.51(7) . . ?
C18 Ti1 C20 55.65(8) . . ?
C19 Ti1 C20 33.58(8) . . ?
C26 Ti1 C20 153.86(8) . . ?
C27 Ti1 C20 130.02(8) . . ?
C1 P1 N1 98.93(9) . . ?
N2 N1 P1 118.59(14) . . ?
N2 N1 Ti1 147.94(14) . . ?
P1 N1 Ti1 92.70(7) . . ?
C2 C1 P1 123.21(16) . . ?
C2 C1 Ti1 147.16(16) . . ?
P1 C1 Ti1 89.60(8) . . ?
C12 N2 N1 120.72(15) . . ?
C12 N2 C6 121.07(16) . . ?
N1 N2 C6 117.28(15) . . ?
C3 C2 C1 112.01(18) . . ?
C3 C2 C4 108.8(2) . . ?
C1 C2 C4 109.97(19) . . ?
C3 C2 C5 108.2(2) . . ?
C1 C2 C5 109.66(17) . . ?
C4 C2 C5 108.11(19) . . ?
C7 C6 C11 120.34(17) . . ?
C7 C6 N2 119.22(18) . . ?
C11 C6 N2 120.44(17) . . ?
C6 C7 C8 119.61(19) . . ?
C9 C8 C7 120.38(19) . . ?
C8 C9 C10 120.05(18) . . ?
C11 C10 C9 119.90(19) . . ?
C6 C11 C10 119.72(18) . . ?
N2 C12 C17 121.51(17) . . ?
N2 C12 C13 120.21(17) . . ?
C17 C12 C13 118.28(17) . . ?
C14 C13 C12 120.20(18) . . ?
C15 C14 C13 121.36(19) . . ?
C16 C15 C14 118.40(18) . . ?
C17 C16 C15 121.39(18) . . ?
C16 C17 C12 120.35(18) . . ?
C19 C18 C22 108.1(2) . . ?
C19 C18 Ti1 73.38(13) . . ?
C22 C18 Ti1 72.21(13) . . ?
C18 C19 C20 108.1(2) . . ?
C18 C19 Ti1 73.10(13) . . ?
C20 C19 Ti1 73.82(12) . . ?
C21 C20 C19 108.0(2) . . ?
C21 C20 Ti1 72.30(12) . . ?
C19 C20 Ti1 72.60(12) . . ?
C20 C21 C22 108.0(2) . . ?
C20 C21 Ti1 74.19(11) . . ?
C22 C21 Ti1 72.38(12) . . ?
C18 C22 C21 107.7(2) . . ?
C18 C22 Ti1 73.83(12) . . ?
C21 C22 Ti1 73.60(12) . . ?
C27 C23 C24 107.6(2) . . ?
C27 C23 Ti1 74.22(12) . . ?
C24 C23 Ti1 73.06(12) . . ?
C25 C24 C23 107.90(19) . . ?
C25 C24 Ti1 73.07(12) . . ?
C23 C24 Ti1 72.77(12) . . ?
C24 C25 C26 108.0(2) . . ?
C24 C25 Ti1 72.87(12) . . ?
C26 C25 Ti1 73.91(12) . . ?
C27 C26 C25 108.01(19) . . ?
C27 C26 Ti1 73.38(12) . . ?
C25 C26 Ti1 72.19(12) . . ?
C26 C27 C23 108.5(2) . . ?
C26 C27 Ti1 73.20(13) . . ?
C23 C27 Ti1 71.83(12) . . ?
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 1.9770(17) . ?
Ti1 C1 2.115(2) . ?
Ti1 C23 2.395(2) . ?
Ti1 C22 2.396(2) . ?
Ti1 C24 2.398(2) . ?
Ti1 C25 2.401(2) . ?
Ti1 C21 2.412(2) . ?
Ti1 C18 2.417(2) . ?
Ti1 C19 2.420(2) . ?
Ti1 C26 2.423(2) . ?
Ti1 C27 2.425(2) . ?
Ti1 C20 2.436(2) . ?
P1 C1 1.677(2) . ?
P1 N1 1.7336(18) . ?
N1 N2 1.399(2) . ?
C1 C2 1.528(3) . ?
N2 C12 1.391(2) . ?
N2 C6 1.429(2) . ?
C2 C3 1.526(3) . ?
C2 C4 1.536(3) . ?
C2 C5 1.538(3) . ?
C6 C7 1.386(3) . ?
C6 C11 1.390(3) . ?
C7 C8 1.390(3) . ?
C8 C9 1.379(3) . ?
C9 C10 1.391(3) . ?
C10 C11 1.390(3) . ?
C12 C17 1.403(3) . ?
C12 C13 1.405(3) . ?
C13 C14 1.388(3) . ?
C14 C15 1.387(3) . ?
C15 C16 1.387(3) . ?
C16 C17 1.386(3) . ?
C18 C19 1.395(4) . ?
C18 C22 1.406(4) . ?
C19 C20 1.403(3) . ?
C20 C21 1.398(3) . ?
C21 C22 1.406(3) . ?
C23 C27 1.408(3) . ?
C23 C24 1.408(3) . ?
C24 C25 1.406(3) . ?
C25 C26 1.406(3) . ?
C26 C27 1.394(3) . ?
