#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:53:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179429 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/26/4332692.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332692
loop_
_publ_author_name
'Han, Hua'
'Elsmaili, Mona'
'Johnson, Samuel A.'
_publ_section_title
;
 Diligating Tripodal Amido-Phosphine Ligands:  the Effect of a
 Proximal Antipodal Early Transition Metal on Phosphine Donor Ability in a
 Building Block for Heterometallic Complexes
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7435
_journal_page_last               7445
_journal_paper_doi               10.1021/ic060692d
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C23 H27 N4 P Ti'
_chemical_formula_weight         438.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9600(8)
_cell_length_b                   14.4825(9)
_cell_length_c                   12.8136(8)
_cell_measurement_temperature    173(2)
_cell_volume                     2219.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21270
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_correction_T_min  0.8709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BRUKER 2001'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0584P)²+0.5684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                4491
_reflns_number_total             5102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060692dsup2.cif
_cod_data_source_block           sj1c
_cod_database_code               4332692
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'
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
C1 C 0.91992(12) 0.36743(9) 0.64434(11) 0.0334(3) Uani 1 1 d .
H1A H 0.8928 0.4129 0.6962 0.040 Uiso 1 1 calc R
H1B H 0.9973 0.3851 0.6257 0.040 Uiso 1 1 calc R
C2 C 0.77861(11) 0.20680(10) 0.70376(10) 0.0314(3) Uani 1 1 d .
H2A H 0.7793 0.1436 0.7333 0.038 Uiso 1 1 calc R
H2B H 0.7327 0.2454 0.7508 0.038 Uiso 1 1 calc R
C3 C 0.99732(11) 0.17976(10) 0.60991(10) 0.0327(3) Uani 1 1 d .
H3A H 1.0778 0.1957 0.6119 0.039 Uiso 1 1 calc R
H3B H 0.9904 0.1143 0.6313 0.039 Uiso 1 1 calc R
C4 C 0.80743(12) 0.46303(9) 0.52721(10) 0.0327(3) Uani 1 1 d .
C5 C 0.70173(14) 0.47031(12) 0.48180(13) 0.0459(4) Uani 1 1 d .
H5 H 0.6605 0.4159 0.4662 0.055 Uiso 1 1 calc R
C6 C 0.65610(18) 0.55613(15) 0.45914(16) 0.0656(5) Uani 1 1 d .
H6 H 0.5844 0.5601 0.4274 0.079 Uiso 1 1 calc R
C7 C 0.7145(2) 0.63580(13) 0.48248(16) 0.0681(6) Uani 1 1 d .
H7 H 0.6828 0.6945 0.4676 0.082 Uiso 1 1 calc R
C8 C 0.81904(19) 0.62972(12) 0.52757(14) 0.0562(5) Uani 1 1 d .
H8 H 0.8592 0.6845 0.5437 0.067 Uiso 1 1 calc R
C9 C 0.86591(14) 0.54458(10) 0.54948(12) 0.0405(3) Uani 1 1 d .
H9 H 0.9383 0.5413 0.5799 0.049 Uiso 1 1 calc R
C10 C 0.61479(10) 0.16206(9) 0.59974(10) 0.0288(3) Uani 1 1 d .
C11 C 0.54359(11) 0.17966(10) 0.51479(11) 0.0332(3) Uani 1 1 d .
H11 H 0.5660 0.2225 0.4627 0.040 Uiso 1 1 calc R
C12 C 0.44147(12) 0.13572(10) 0.50565(12) 0.0370(3) Uani 1 1 d .
H12 H 0.3955 0.1476 0.4467 0.044 Uiso 1 1 calc R
C13 C 0.40562(12) 0.07478(11) 0.58134(13) 0.0412(3) Uani 1 1 d .
H13 H 0.3359 0.0440 0.5744 0.049 Uiso 1 1 calc R
C14 C 0.47261(13) 0.05922(11) 0.66729(13) 0.0433(3) Uani 1 1 d .
H14 H 0.4479 0.0183 0.7204 0.052 Uiso 1 1 calc R
C15 C 0.57567(12) 0.10252(10) 0.67740(11) 0.0358(3) Uani 1 1 d .
H15 H 0.6200 0.0916 0.7377 0.043 Uiso 1 1 calc R
C16 C 1.02503(10) 0.14224(9) 0.42736(10) 0.0291(3) Uani 1 1 d .
C17 C 1.01335(12) 0.16493(10) 0.32129(11) 0.0343(3) Uani 1 1 d .
H17 H 0.9618 0.2115 0.3011 0.041 Uiso 1 1 calc R
C18 C 1.07600(12) 0.12028(11) 0.24567(11) 0.0377(3) Uani 1 1 d .
H18 H 1.0656 0.1356 0.1742 0.045 Uiso 1 1 calc R
C19 C 1.15355(13) 0.05363(10) 0.27315(12) 0.0402(3) Uani 1 1 d .
H19 H 1.1957 0.0227 0.2211 0.048 Uiso 1 1 calc R
C20 C 1.16874(13) 0.03276(11) 0.37755(13) 0.0418(3) Uani 1 1 d .
H20 H 1.2232 -0.0118 0.3972 0.050 Uiso 1 1 calc R
C21 C 1.10555(12) 0.07596(10) 0.45395(11) 0.0363(3) Uani 1 1 d .
H21 H 1.1170 0.0604 0.5252 0.044 Uiso 1 1 calc R
C22 C 0.74742(18) 0.31835(14) 0.28299(13) 0.0593(5) Uani 1 1 d .
H22A H 0.7875 0.2996 0.2198 0.089 Uiso 1 1 calc R
H22B H 0.7782 0.3768 0.3087 0.089 Uiso 1 1 calc R
H22C H 0.6679 0.3264 0.2668 0.089 Uiso 1 1 calc R
C23 C 0.72981(15) 0.15615(12) 0.32675(13) 0.0490(4) Uani 1 1 d .
H23A H 0.7748 0.1398 0.2656 0.074 Uiso 1 1 calc R
H23B H 0.6503 0.1550 0.3080 0.074 Uiso 1 1 calc R
H23C H 0.7438 0.1115 0.3828 0.074 Uiso 1 1 calc R
N1 N 0.85045(9) 0.37547(8) 0.55067(9) 0.0319(2) Uani 1 1 d .
N2 N 0.72129(9) 0.20262(8) 0.60236(8) 0.0295(2) Uani 1 1 d .
N3 N 0.95909(9) 0.18746(8) 0.50191(8) 0.0295(2) Uani 1 1 d .
N4 N 0.76017(10) 0.24806(8) 0.36209(9) 0.0338(3) Uani 1 1 d .
P1 P 0.92442(3) 0.25173(2) 0.70837(3) 0.03107(10) Uani 1 1 d .
Ti1 Ti 0.818355(19) 0.254265(15) 0.496985(17) 0.02556(9) Uani 1 1 d .
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
N1 C1 P1 116.61(9)
N2 C2 P1 118.56(9)
N3 C3 P1 117.03(9)
C5 C4 N1 119.36(13)
C5 C4 C9 118.23(14)
N1 C4 C9 122.41(13)
C6 C5 C4 120.71(17)
C7 C6 C5 120.30(19)
C8 C7 C6 119.66(17)
C7 C8 C9 120.58(18)
C8 C9 C4 120.52(17)
C15 C10 N2 123.09(12)
C15 C10 C11 117.42(12)
N2 C10 C11 119.48(12)
C12 C11 C10 121.13(13)
C13 C12 C11 120.69(14)
C14 C13 C12 119.00(14)
C13 C14 C15 121.00(14)
C14 C15 C10 120.66(13)
C21 C16 N3 122.78(12)
C21 C16 C17 117.56(12)
N3 C16 C17 119.65(12)
C18 C17 C16 120.94(13)
C19 C18 C17 120.69(13)
C20 C19 C18 119.05(13)
C19 C20 C21 120.88(14)
C20 C21 C16 120.83(13)
C4 N1 C1 117.12(11)
C4 N1 Ti1 132.54(9)
C1 N1 Ti1 109.48(8)
C10 N2 C2 117.44(11)
C10 N2 Ti1 133.75(9)
C2 N2 Ti1 108.78(8)
C16 N3 C3 115.73(10)
C16 N3 Ti1 134.33(9)
C3 N3 Ti1 109.80(8)
C22 N4 C23 113.65(13)
C22 N4 Ti1 130.95(11)
C23 N4 Ti1 115.22(10)
C3 P1 C2 102.89(6)
C3 P1 C1 102.64(6)
C2 P1 C1 105.86(6)
C3 P1 Ti1 65.80(4)
C2 P1 Ti1 65.13(4)
C1 P1 Ti1 65.09(4)
N4 Ti1 N1 116.71(5)
N4 Ti1 N2 113.91(5)
N1 Ti1 N2 102.89(5)
N4 Ti1 N3 109.17(5)
N1 Ti1 N3 105.69(5)
N2 Ti1 N3 107.81(5)
N4 Ti1 P1 175.30(4)
N1 Ti1 P1 66.61(3)
N2 Ti1 P1 67.47(3)
N3 Ti1 P1 66.29(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.4634(17)
C1 P1 1.8664(14)
C2 N2 1.4694(16)
C2 P1 1.8622(14)
C3 N3 1.4612(16)
C3 P1 1.8550(14)
C4 C5 1.395(2)
C4 N1 1.4011(17)
C4 C9 1.402(2)
C5 C6 1.388(2)
C6 C7 1.381(3)
C7 C8 1.380(3)
C8 C9 1.383(2)
C10 C15 1.3979(19)
C10 N2 1.4031(17)
C10 C11 1.4044(18)
C11 C12 1.382(2)
C12 C13 1.380(2)
C13 C14 1.379(2)
C14 C15 1.389(2)
C16 C21 1.4014(19)
C16 N3 1.4019(17)
C16 C17 1.4051(19)
C17 C18 1.386(2)
C18 C19 1.384(2)
C19 C20 1.383(2)
C20 C21 1.387(2)
C22 N4 1.444(2)
C23 N4 1.452(2)
N1 Ti1 1.9238(11)
N2 Ti1 1.9326(11)
N3 Ti1 1.9424(11)
N4 Ti1 1.8646(12)
P1 Ti1 2.9895(4)
