#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:55:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179269 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/89/4318970.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_4318970
loop_
_publ_author_name
'Yahong Li'
'Angie Turnas'
'James T. Ciszewski'
'Aaron L. Odom'
_publ_section_title
;
 Group-4 η1-Pyrrolyl Complexes Incorporating
 N,N-Di(pyrrolyl-α-methyl)-N-methylamine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6298
_journal_page_last               6306
_journal_paper_doi               10.1021/ic0259484
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C17 H30 N4 Si Ti'
_chemical_formula_weight         366.44
_chemical_name_common            Ti(CH2SiMe3)(NMe2)(dpma)
_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                 129.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.646(11)
_cell_length_b                   8.568(3)
_cell_length_c                   20.885(9)
_cell_measurement_temperature    293(2)
_cell_volume                     3944(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0825
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8668
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.9024
_exptl_absorpt_correction_T_min  0.8139
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpipid
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0473
_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)+(0.0694P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                1974
_reflns_number_total             2844
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0259484_5.cif
_cod_data_source_block           alo7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318970
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti 0.11971(3) 0.34378(8) 0.19708(4) 0.0217(3) Uani 1 1 d . . .
Si Si 0.17724(5) 0.47027(14) 0.38974(7) 0.0271(3) Uani 1 1 d . . .
N1 N 0.14344(13) 0.2226(4) 0.13946(18) 0.0231(8) Uani 1 1 d . . .
N2 N 0.05679(13) 0.5121(4) 0.14503(18) 0.0237(8) Uani 1 1 d . . .
N3 N 0.15495(13) 0.5336(4) 0.15553(18) 0.0215(8) Uani 1 1 d . . .
N4 N 0.07334(14) 0.1858(4) 0.19510(19) 0.0248(8) Uani 1 1 d . . .
C1 C 0.19087(16) 0.3715(4) 0.3239(2) 0.0252(10) Uani 1 1 d . . .
H1A H 0.2068 0.2684 0.3472 0.030 Uiso 1 1 calc R . .
H1B H 0.2227 0.4286 0.3300 0.030 Uiso 1 1 calc R . .
C2 C 0.11837(19) 0.3618(5) 0.3854(3) 0.0397(12) Uani 1 1 d . . .
H2A H 0.1315 0.2563 0.4035 0.060 Uiso 1 1 calc R . .
H2B H 0.0807 0.3618 0.3293 0.060 Uiso 1 1 calc R . .
H2C H 0.1127 0.4120 0.4212 0.060 Uiso 1 1 calc R . .
C3 C 0.15122(19) 0.6754(5) 0.3545(2) 0.0359(11) Uani 1 1 d . . .
H3A H 0.1815 0.7320 0.3575 0.054 Uiso 1 1 calc R . .
H3B H 0.1449 0.7245 0.3898 0.054 Uiso 1 1 calc R . .
H3C H 0.1139 0.6752 0.2981 0.054 Uiso 1 1 calc R . .
C4 C 0.24764(18) 0.4752(5) 0.5019(2) 0.0328(11) Uani 1 1 d . . .
H4A H 0.2791 0.5301 0.5070 0.049 Uiso 1 1 calc R . .
H4B H 0.2607 0.3704 0.5220 0.049 Uiso 1 1 calc R . .
H4C H 0.2391 0.5275 0.5341 0.049 Uiso 1 1 calc R . .
C11 C 0.12973(17) 0.0718(5) 0.1077(2) 0.0299(11) Uani 1 1 d . . .
H11A H 0.1110 -0.0037 0.1165 0.036 Uiso 1 1 calc R . .
C12 C 0.14776(18) 0.0509(5) 0.0615(2) 0.0332(11) Uani 1 1 d . . .
H12A H 0.1436 -0.0396 0.0337 0.040 Uiso 1 1 calc R . .
C13 C 0.17407(18) 0.1929(5) 0.0640(2) 0.0312(11) Uani 1 1 d . . .
H13A H 0.1906 0.2137 0.0384 0.037 Uiso 1 1 calc R . .
C14 C 0.17046(16) 0.2928(5) 0.1111(2) 0.0249(10) Uani 1 1 d . . .
C21 C 0.01312(17) 0.5609(5) 0.1504(2) 0.0298(10) Uani 1 1 d . . .
H21A H 0.0045 0.5109 0.1813 0.036 Uiso 1 1 calc R . .
C22 C -0.01525(17) 0.6917(5) 0.1043(3) 0.0330(11) Uani 1 1 d . . .
H22A H -0.0457 0.7466 0.0985 0.040 Uiso 1 1 calc R . .
C23 C 0.01066(17) 0.7283(5) 0.0665(2) 0.0319(11) Uani 1 1 d . . .
H23A H 0.0002 0.8114 0.0309 0.038 Uiso 1 1 calc R . .
C24 C 0.05375(17) 0.6184(5) 0.0924(2) 0.0259(10) Uani 1 1 d . . .
C31 C 0.19283(17) 0.4560(5) 0.1399(2) 0.0287(10) Uani 1 1 d . . .
H31A H 0.2348 0.4544 0.1905 0.034 Uiso 1 1 calc R . .
H31B H 0.1905 0.5127 0.0978 0.034 Uiso 1 1 calc R . .
C32 C 0.09658(16) 0.5887(5) 0.0759(2) 0.0240(10) Uani 1 1 d . . .
H32A H 0.1031 0.6837 0.0573 0.029 Uiso 1 1 calc R . .
H32B H 0.0801 0.5099 0.0330 0.029 Uiso 1 1 calc R . .
C33 C 0.18757(17) 0.6691(4) 0.2108(2) 0.0299(10) Uani 1 1 d . . .
H33A H 0.1992 0.7379 0.1869 0.045 Uiso 1 1 calc R . .
H33B H 0.2231 0.6339 0.2642 0.045 Uiso 1 1 calc R . .
H33C H 0.1615 0.7238 0.2172 0.045 Uiso 1 1 calc R . .
C41 C 0.1005(2) 0.0497(5) 0.2504(3) 0.0490(13) Uani 1 1 d . . .
H41A H 0.0689 -0.0169 0.2388 0.073 Uiso 1 1 calc R . .
H41B H 0.1256 0.0838 0.3073 0.073 Uiso 1 1 calc R . .
H41C H 0.1247 -0.0070 0.2414 0.073 Uiso 1 1 calc R . .
C42 C 0.00814(18) 0.1632(5) 0.1329(3) 0.0429(12) Uani 1 1 d . . .
H42A H -0.0035 0.0726 0.1468 0.064 Uiso 1 1 calc R . .
H42B H -0.0027 0.1489 0.0793 0.064 Uiso 1 1 calc R . .
H42C H -0.0124 0.2532 0.1316 0.064 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'
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
N4 Ti N2 97.38(14) . . ?
N4 Ti N1 96.86(13) . . ?
N2 Ti N1 125.39(13) . . ?
N4 Ti C1 102.37(15) . . ?
N2 Ti C1 114.78(15) . . ?
N1 Ti C1 112.98(14) . . ?
N4 Ti N3 162.54(12) . . ?
N2 Ti N3 75.60(12) . . ?
N1 Ti N3 75.37(12) . . ?
C1 Ti N3 95.07(13) . . ?
C1 Si C3 110.92(19) . . ?
C1 Si C2 110.27(19) . . ?
C3 Si C2 109.1(2) . . ?
C1 Si C4 111.60(19) . . ?
C3 Si C4 108.12(19) . . ?
C2 Si C4 106.7(2) . . ?
C14 N1 C11 105.4(3) . . ?
C14 N1 Ti 122.0(3) . . ?
C11 N1 Ti 131.8(3) . . ?
C24 N2 C21 105.2(3) . . ?
C24 N2 Ti 118.9(2) . . ?
C21 N2 Ti 135.9(3) . . ?
C33 N3 C31 109.9(3) . . ?
C33 N3 C32 108.8(3) . . ?
C31 N3 C32 110.7(3) . . ?
C33 N3 Ti 117.5(2) . . ?
C31 N3 Ti 108.6(2) . . ?
C32 N3 Ti 101.0(2) . . ?
C42 N4 C41 109.3(3) . . ?
C42 N4 Ti 127.1(3) . . ?
C41 N4 Ti 123.0(3) . . ?
Si C1 Ti 119.76(19) . . ?
C12 C11 N1 109.9(4) . . ?
C11 C12 C13 107.1(4) . . ?
C14 C13 C12 106.5(4) . . ?
C13 C14 N1 111.1(4) . . ?
C13 C14 C31 132.1(4) . . ?
N1 C14 C31 116.8(3) . . ?
C22 C21 N2 110.7(4) . . ?
C21 C22 C23 106.7(4) . . ?
C24 C23 C22 106.8(4) . . ?
C23 C24 N2 110.6(4) . . ?
C23 C24 C32 134.1(4) . . ?
N2 C24 C32 115.3(3) . . ?
N3 C31 C14 108.9(3) . . ?
C24 C32 N3 107.3(3) . . ?
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
Ti N4 1.878(3) . ?
Ti N2 2.002(3) . ?
Ti N1 2.008(3) . ?
Ti C1 2.081(4) . ?
Ti N3 2.353(3) . ?
Si C1 1.856(4) . ?
Si C3 1.867(4) . ?
Si C2 1.876(4) . ?
Si C4 1.877(4) . ?
N1 C14 1.377(5) . ?
N1 C11 1.389(5) . ?
N2 C24 1.386(5) . ?
N2 C21 1.389(5) . ?
N3 C33 1.475(4) . ?
N3 C31 1.476(5) . ?
N3 C32 1.494(5) . ?
N4 C42 1.454(5) . ?
N4 C41 1.468(5) . ?
C11 C12 1.365(5) . ?
C12 C13 1.415(6) . ?
C13 C14 1.357(5) . ?
C14 C31 1.495(5) . ?
C21 C22 1.357(5) . ?
C22 C23 1.422(5) . ?
C23 C24 1.360(5) . ?
C24 C32 1.494(5) . ?
