#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:49:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178669 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/80/4078049.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_4078049
loop_
_publ_author_name
'Aharonovich, Sinai'
'Botoshansky, Mark'
'Balazs, Yael S.'
'Eisen, Moris S.'
_publ_section_title
;
 Elucidation of Substituent Effects in the Polymerization of Propylene
 Promoted by Titanium Amidinates
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3435
_journal_paper_doi               10.1021/om300068w
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C30 H54 Cl2 N4 Si4 Ti'
_chemical_formula_sum            'C30 H54 Cl2 N4 Si4 Ti'
_chemical_formula_weight         701.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 128.7431(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.4890(5)
_cell_length_b                   8.8040(3)
_cell_length_c                   20.1850(5)
_cell_measurement_reflns_used    8400
_cell_measurement_temperature    230.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     3948.7(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius (1997), KappaCCD Collect Program'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics
;
Molecular Structure Corporation (1999). 
ORTEP. TEXRAY Structure Analysis Package. 
MSC, 3200 Research Forest Drive, The 
Woodlands,TX 77381, USA.
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland 
"maXus": a computer program for the solution and refinement of crystal 
structures from diffraction data University of Glasgow, Scotland, UK, 
Nonius BV, Delft, The Netherlands and MacScience Co. Ltd.,
Yokohama, Japan (1998)
;
_diffrn_ambient_temperature      230.0(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6025
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.8650
_exptl_absorpt_correction_T_min  0.8182
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0517P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                2485
_reflns_number_total             3499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300068w_si_002.cif
_cod_data_source_block           tipetam
_cod_original_cell_volume        3948.73(18)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4078049
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ti1 Ti 0.0000 0.95579(5) 0.2500 0.03903(15) Uani 1 2 d S
Si1 Si 0.15420(3) 1.01852(7) 0.42201(4) 0.04888(17) Uani 1 1 d .
Si2 Si -0.04248(3) 0.66292(7) 0.32910(4) 0.04713(17) Uani 1 1 d .
Cl1 Cl 0.03315(3) 1.12971(7) 0.20320(4) 0.06550(19) Uani 1 1 d .
N1 N 0.08587(7) 0.91696(17) 0.36259(10) 0.0399(4) Uani 1 1 d .
N2 N 0.00546(7) 0.78519(17) 0.32650(10) 0.0394(4) Uani 1 1 d .
C1 C 0.21464(10) 0.9333(3) 0.52704(15) 0.0658(7) Uani 1 1 d .
H1A H 0.2230 0.8311 0.5190 0.079(8) Uiso 1 1 calc R
H1B H 0.2017 0.9298 0.5614 0.094(9) Uiso 1 1 calc R
H1C H 0.2508 0.9946 0.5555 0.088(8) Uiso 1 1 calc R
C2 C 0.13942(13) 1.2139(3) 0.4389(2) 0.0828(9) Uani 1 1 d .
H2A H 0.1078 1.2596 0.3845 0.092(9) Uiso 1 1 calc R
H2B H 0.1758 1.2741 0.4672 0.103(10) Uiso 1 1 calc R
H2C H 0.1269 1.2104 0.4738 0.098(11) Uiso 1 1 calc R
C3 C 0.18354(12) 1.0177(4) 0.36189(17) 0.0813(9) Uani 1 1 d .
H3A H 0.1536 1.0605 0.3059 0.141(14) Uiso 1 1 calc R
H3B H 0.1924 0.9142 0.3564 0.149(16) Uiso 1 1 calc R
H3C H 0.2200 1.0781 0.3920 0.105(10) Uiso 1 1 calc R
C4 C 0.06250(9) 0.8220(2) 0.38739(12) 0.0375(4) Uani 1 1 d .
C5 C 0.09683(8) 0.7686(2) 0.47688(11) 0.0388(4) Uani 1 1 d .
C6 C 0.13400(10) 0.6429(2) 0.50672(13) 0.0493(5) Uani 1 1 d .
H6 H 0.1384 0.5896 0.4705 0.056(6) Uiso 1 1 calc R
C7 C 0.16488(10) 0.5953(3) 0.58992(13) 0.0518(5) Uani 1 1 d .
H7 H 0.1895 0.5087 0.6093 0.062(7) Uiso 1 1 calc R
C8 C 0.15998(10) 0.6736(2) 0.64491(13) 0.0473(5) Uani 1 1 d .
C9 C 0.12216(10) 0.7979(2) 0.61405(13) 0.0513(5) Uani 1 1 d .
H9 H 0.1178 0.8514 0.6502 0.073(7) Uiso 1 1 calc R
C10 C 0.09062(10) 0.8451(2) 0.53086(13) 0.0487(5) Uani 1 1 d .
H10 H 0.0648 0.9295 0.5109 0.054(6) Uiso 1 1 calc R
C11 C 0.19715(11) 0.6276(3) 0.73716(13) 0.0608(6) Uani 1 1 d .
H11A H 0.1793 0.6712 0.7615 0.101(10) Uiso 1 1 calc R
H11B H 0.1963 0.5167 0.7408 0.073(7) Uiso 1 1 calc R
C12 C 0.26107(14) 0.6792(5) 0.78796(17) 0.1020(11) Uani 1 1 d .
H12A H 0.2832 0.6478 0.8466 0.089(8) Uiso 1 1 calc R
H12B H 0.2622 0.7891 0.7853 0.151(16) Uiso 1 1 calc R
H12C H 0.2792 0.6343 0.7649 0.159(18) Uiso 1 1 calc R
C13 C -0.07840(13) 0.7710(3) 0.3652(2) 0.0794(8) Uani 1 1 d .
H13A H -0.0995 0.8579 0.3283 0.115(12) Uiso 1 1 calc R
H13B H -0.0478 0.8057 0.4229 0.112(12) Uiso 1 1 calc R
H13C H -0.1067 0.7061 0.3632 0.123(11) Uiso 1 1 calc R
C14 C -0.00276(11) 0.4972(3) 0.39962(16) 0.0628(6) Uani 1 1 d .
H14A H 0.0261 0.5315 0.4579 0.090(9) Uiso 1 1 calc R
H14B H 0.0181 0.4431 0.3830 0.086(9) Uiso 1 1 calc R
H14C H -0.0317 0.4299 0.3949 0.093(9) Uiso 1 1 calc R
C15 C -0.09778(13) 0.5908(3) 0.21920(16) 0.0792(9) Uani 1 1 d .
H15A H -0.1194 0.6755 0.1807 0.112(11) Uiso 1 1 calc R
H15B H -0.1261 0.5237 0.2163 0.102(9) Uiso 1 1 calc R
H15C H -0.0769 0.5353 0.2031 0.127(13) 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
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N1 Ti1 N1 161.04(9) 2 .
N1 Ti1 N2 100.52(6) 2 .
N1 Ti1 N2 65.21(6) . .
N1 Ti1 N2 100.51(6) . 2
N2 Ti1 N2 88.06(8) . 2
N1 Ti1 Cl1 93.11(4) 2 2
N1 Ti1 Cl1 99.57(5) . 2
N2 Ti1 Cl1 92.01(4) . 2
N2 Ti1 Cl1 157.89(5) 2 2
N1 Ti1 Cl1 99.56(5) 2 .
N1 Ti1 Cl1 93.10(4) . .
N2 Ti1 Cl1 157.88(5) . .
Cl1 Ti1 Cl1 96.08(4) 2 .
N1 Si1 C2 108.35(11) . .
N1 Si1 C3 108.12(10) . .
C2 Si1 C3 111.79(16) . .
N1 Si1 C1 114.33(10) . .
C2 Si1 C1 108.65(13) . .
C3 Si1 C1 105.65(12) . .
N2 Si2 C13 109.10(10) . .
N2 Si2 C14 113.07(10) . .
C13 Si2 C14 109.04(13) . .
N2 Si2 C15 105.52(9) . .
C13 Si2 C15 112.50(15) . .
C14 Si2 C15 107.65(13) . .
C4 N1 Si1 130.94(14) . .
C4 N1 Ti1 89.49(11) . .
Si1 N1 Ti1 134.81(9) . .
C4 N2 Si2 130.10(13) . .
C4 N2 Ti1 89.45(11) . .
Si2 N2 Ti1 139.40(9) . .
Si1 C1 H1A 109.5 . .
Si1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Si1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Si1 C2 H2A 109.5 . .
Si1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Si1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
Si1 C3 H3A 109.5 . .
Si1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
Si1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N2 C4 N1 114.34(17) . .
N2 C4 C5 122.64(16) . .
N1 C4 C5 122.95(17) . .
C6 C5 C10 119.18(18) . .
C6 C5 C4 121.51(16) . .
C10 C5 C4 119.30(17) . .
C5 C6 C7 120.16(19) . .
C5 C6 H6 119.9 . .
C7 C6 H6 119.9 . .
C6 C7 C8 121.0(2) . .
C6 C7 H7 119.5 . .
C8 C7 H7 119.5 . .
C9 C8 C7 118.31(19) . .
C9 C8 C11 121.05(19) . .
C7 C8 C11 120.6(2) . .
C8 C9 C10 121.11(19) . .
C8 C9 H9 119.4 . .
C10 C9 H9 119.4 . .
C9 C10 C5 120.3(2) . .
C9 C10 H10 119.9 . .
C5 C10 H10 119.9 . .
C12 C11 C8 112.1(2) . .
C12 C11 H11A 109.2 . .
C8 C11 H11A 109.2 . .
C12 C11 H11B 109.2 . .
C8 C11 H11B 109.2 . .
H11A C11 H11B 107.9 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
Si2 C13 H13A 109.5 . .
Si2 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
Si2 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
Si2 C14 H14A 109.5 . .
Si2 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
Si2 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
Si2 C15 H15A 109.5 . .
Si2 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
Si2 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ti1 N1 2.0754(16)
Ti1 N2 2.0891(15)
Ti1 Cl1 2.2902(6)
Si1 N1 1.7622(16)
Si1 C2 1.853(3)
Si1 C3 1.855(2)
Si1 C1 1.858(2)
Si2 N2 1.7653(16)
Si2 C13 1.848(2)
Si2 C14 1.849(2)
Si2 C15 1.853(2)
N1 C4 1.345(2)
N2 C4 1.325(2)
C1 H1A 0.9700
C1 H1B 0.9700
C1 H1C 0.9700
C2 H2A 0.9700
C2 H2B 0.9700
C2 H2C 0.9700
C3 H3A 0.9700
C3 H3B 0.9700
C3 H3C 0.9700
C4 C5 1.493(3)
C5 C6 1.382(3)
C5 C10 1.383(3)
C6 C7 1.386(3)
C6 H6 0.9400
C7 C8 1.386(3)
C7 H7 0.9400
C8 C9 1.381(3)
C8 C11 1.512(3)
C9 C10 1.382(3)
C9 H9 0.9400
C10 H10 0.9400
C11 C12 1.496(4)
C11 H11A 0.9800
C11 H11B 0.9800
C12 H12A 0.9700
C12 H12B 0.9700
C12 H12C 0.9700
C13 H13A 0.9700
C13 H13B 0.9700
C13 H13C 0.9700
C14 H14A 0.9700
C14 H14B 0.9700
C14 H14C 0.9700
C15 H15A 0.9700
C15 H15B 0.9700
C15 H15C 0.9700
