#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/53/7015351.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_7015351
loop_
_publ_author_name
'Dureen, Meghan A.'
'Brown, Christopher C.'
'Morton, Jason G. M.'
'Stephan, Douglas W.'
_publ_section_title
;
 Titanium "constrained geometry" complexes with pendant arene groups.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2861
_journal_page_last               2867
_journal_paper_doi               10.1039/c0dt01530j
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C23 H29 N Si'
_chemical_formula_weight         347.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.91(3)
_cell_angle_beta                 82.78(3)
_cell_angle_gamma                64.73(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3969(19)
_cell_length_b                   10.297(2)
_cell_length_c                   12.440(3)
_cell_measurement_reflns_used    5043
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     1015.0(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10726
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colour
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0600
_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)+(0.1026P)²+0.2068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1891
_reflns_number_gt                3144
_reflns_number_total             4542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01530j.txt
_cod_data_source_block           (C5Me4HSiMe2N(H)C6H4Ph)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        1015.0(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7015351
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.27301(7) 0.06069(7) 0.29135(5) 0.0338(2) Uani 1 1 d . . .
N1 N 0.1094(2) 0.05776(19) 0.24379(17) 0.0344(4) Uani 1 1 d . . .
H1A H 0.1112 -0.0340 0.2630 0.041 Uiso 1 1 calc R . .
C1 C -0.0243(2) 0.1753(2) 0.18061(19) 0.0294(5) Uani 1 1 d . . .
C2 C -0.1391(2) 0.1457(2) 0.14173(18) 0.0287(5) Uani 1 1 d . . .
C7 C -0.1257(2) -0.0130(2) 0.17095(19) 0.0286(5) Uani 1 1 d . . .
C12 C -0.1237(2) -0.0709(2) 0.0852(2) 0.0323(5) Uani 1 1 d . . .
H12A H -0.1311 -0.0082 0.0066 0.039 Uiso 1 1 calc R . .
C6 C -0.0462(2) 0.3277(2) 0.1497(2) 0.0328(5) Uani 1 1 d . . .
H6A H 0.0285 0.3499 0.1763 0.039 Uiso 1 1 calc R . .
C5 C -0.1733(3) 0.4462(2) 0.0819(2) 0.0354(5) Uani 1 1 d . . .
H5A H -0.1856 0.5485 0.0629 0.043 Uiso 1 1 calc R . .
C3 C -0.2651(2) 0.2682(2) 0.0716(2) 0.0351(5) Uani 1 1 d . . .
H3A H -0.3406 0.2482 0.0439 0.042 Uiso 1 1 calc R . .
C13 C 0.4046(3) -0.1499(2) 0.3585(2) 0.0352(5) Uani 1 1 d . . .
H13A H 0.5109 -0.1629 0.3782 0.042 Uiso 1 1 calc R . .
C11 C -0.1110(3) -0.2184(3) 0.1126(2) 0.0391(6) Uani 1 1 d . . .
H11A H -0.1074 -0.2564 0.0527 0.047 Uiso 1 1 calc R . .
C4 C -0.2836(3) 0.4174(2) 0.0410(2) 0.0389(6) Uani 1 1 d . . .
H4A H -0.3702 0.4989 -0.0071 0.047 Uiso 1 1 calc R . .
C17 C 0.4199(2) -0.2332(3) 0.2770(2) 0.0380(5) Uani 1 1 d . . .
C10 C -0.1035(3) -0.3105(2) 0.2261(2) 0.0381(5) Uani 1 1 d . . .
H10A H -0.0950 -0.4115 0.2445 0.046 Uiso 1 1 calc R . .
C8 C -0.1161(3) -0.1083(2) 0.2857(2) 0.0358(5) Uani 1 1 d . . .
H8A H -0.1147 -0.0726 0.3460 0.043 Uiso 1 1 calc R . .
C16 C 0.3592(3) -0.3374(3) 0.3256(2) 0.0424(6) Uani 1 1 d . . .
C9 C -0.1085(3) -0.2543(3) 0.3127(2) 0.0398(5) Uani 1 1 d . . .
H9A H -0.1067 -0.3158 0.3911 0.048 Uiso 1 1 calc R . .
C14 C 0.3371(3) -0.2310(3) 0.4637(2) 0.0396(6) Uani 1 1 d . . .
C15 C 0.3089(3) -0.3368(3) 0.4417(2) 0.0427(6) Uani 1 1 d . . .
C22 C 0.3738(3) 0.1573(3) 0.1729(3) 0.0553(7) Uani 1 1 d . . .
H22A H 0.3038 0.2657 0.1392 0.083 Uiso 1 1 calc R . .
H22B H 0.4005 0.1096 0.1135 0.083 Uiso 1 1 calc R . .
H22C H 0.4704 0.1474 0.2037 0.083 Uiso 1 1 calc R . .
C21 C 0.4857(3) -0.1967(3) 0.1592(2) 0.0517(7) Uani 1 1 d . . .
H21A H 0.4846 -0.2657 0.1222 0.078 Uiso 1 1 calc R . .
H21B H 0.5942 -0.2096 0.1658 0.078 Uiso 1 1 calc R . .
H21C H 0.4214 -0.0908 0.1126 0.078 Uiso 1 1 calc R . .
C18 C 0.3069(4) -0.1965(3) 0.5735(2) 0.0611(8) Uani 1 1 d . . .
H18A H 0.2631 -0.2641 0.6292 0.092 Uiso 1 1 calc R . .
H18B H 0.2319 -0.0899 0.5581 0.092 Uiso 1 1 calc R . .
H18C H 0.4060 -0.2128 0.6052 0.092 Uiso 1 1 calc R . .
C20 C 0.3445(3) -0.4412(3) 0.2729(3) 0.0631(8) Uani 1 1 d . . .
H20A H 0.3859 -0.4219 0.1951 0.095 Uiso 1 1 calc R . .
H20B H 0.2333 -0.4217 0.2687 0.095 Uiso 1 1 calc R . .
H20C H 0.4044 -0.5477 0.3204 0.095 Uiso 1 1 calc R . .
C19 C 0.2428(3) -0.4435(3) 0.5221(3) 0.0620(8) Uani 1 1 d . . .
H19A H 0.2171 -0.4222 0.5946 0.093 Uiso 1 1 calc R . .
H19B H 0.3208 -0.5491 0.5377 0.093 Uiso 1 1 calc R . .
H19C H 0.1472 -0.4293 0.4869 0.093 Uiso 1 1 calc R . .
C23 C 0.2187(3) 0.1654(3) 0.3958(2) 0.0524(7) Uani 1 1 d . . .
H23A H 0.1506 0.2732 0.3566 0.079 Uiso 1 1 calc R . .
H23B H 0.3144 0.1578 0.4261 0.079 Uiso 1 1 calc R . .
H23C H 0.1626 0.1204 0.4595 0.079 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'
Si Si 0.0817 0.0704 '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 Si1 C22 113.10(12) . . ?
N1 Si1 C23 111.32(11) . . ?
C22 Si1 C23 106.10(14) . . ?
N1 Si1 C13 102.74(10) . . ?
C22 Si1 C13 110.75(12) . . ?
C23 Si1 C13 113.01(11) . . ?
C1 N1 Si1 131.04(14) . . ?
N1 C1 C6 120.35(19) . . ?
N1 C1 C2 121.57(18) . . ?
C6 C1 C2 118.04(19) . . ?
C3 C2 C1 118.82(19) . . ?
C3 C2 C7 119.47(18) . . ?
C1 C2 C7 121.69(19) . . ?
C12 C7 C8 117.74(19) . . ?
C12 C7 C2 121.2(2) . . ?
C8 C7 C2 121.0(2) . . ?
C11 C12 C7 121.1(2) . . ?
C5 C6 C1 121.6(2) . . ?
C6 C5 C4 120.50(19) . . ?
C4 C3 C2 122.2(2) . . ?
C14 C13 C17 103.10(19) . . ?
C14 C13 Si1 113.33(16) . . ?
C17 C13 Si1 110.41(15) . . ?
C10 C11 C12 120.6(2) . . ?
C3 C4 C5 118.8(2) . . ?
C16 C17 C21 127.2(2) . . ?
C16 C17 C13 108.9(2) . . ?
C21 C17 C13 123.9(2) . . ?
C11 C10 C9 119.3(2) . . ?
C9 C8 C7 120.9(2) . . ?
C17 C16 C15 109.5(2) . . ?
C17 C16 C20 126.9(3) . . ?
C15 C16 C20 123.6(2) . . ?
C10 C9 C8 120.3(2) . . ?
C15 C14 C18 126.6(2) . . ?
C15 C14 C13 108.9(2) . . ?
C18 C14 C13 124.5(2) . . ?
C14 C15 C16 109.4(2) . . ?
C14 C15 C19 126.8(3) . . ?
C16 C15 C19 123.7(2) . . ?
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
Si1 N1 1.7312(19) . ?
Si1 C22 1.859(3) . ?
Si1 C23 1.867(3) . ?
Si1 C13 1.896(2) . ?
N1 C1 1.388(3) . ?
C1 C6 1.401(3) . ?
C1 C2 1.418(3) . ?
C2 C3 1.395(3) . ?
C2 C7 1.492(3) . ?
C7 C12 1.391(3) . ?
C7 C8 1.399(3) . ?
C12 C11 1.386(3) . ?
C6 C5 1.377(3) . ?
C5 C4 1.387(3) . ?
C3 C4 1.380(3) . ?
C13 C14 1.506(3) . ?
C13 C17 1.507(3) . ?
C11 C10 1.379(3) . ?
C17 C16 1.345(3) . ?
C17 C21 1.499(4) . ?
C10 C9 1.383(3) . ?
C8 C9 1.389(3) . ?
C16 C15 1.463(4) . ?
C16 C20 1.499(4) . ?
C14 C15 1.347(3) . ?
C14 C18 1.497(4) . ?
C15 C19 1.493(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652811
