#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/84/4308482.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_4308482
loop_
_publ_author_name
'Claire J. Carmalt'
'Anne C. Newport'
'Shane A. O'Neill'
'Ivan P. Parkin'
'Andrew J. P. White'
'David J. Williams'
_publ_section_title
;
Synthesis of Titanium(IV) Guanidinate Complexes and the Formation of
Titanium Carbonitride via Low-Pressure Chemical Vapor Deposition
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              615
_journal_page_last               619
_journal_paper_doi               10.1021/ic049013u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C17 H44 Cl N5 Si2 Ti'
_chemical_formula_weight         458.10
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.81(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.139(3)
_cell_length_b                   14.614(3)
_cell_length_c                   18.034(4)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      24.64
_cell_measurement_theta_min      2.11
_cell_volume                     2633.1(11)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0877
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4050
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         3.92
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.634
_exptl_absorpt_correction_T_max  0.7426
_exptl_absorpt_correction_T_min  0.3041
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       'prismatic needles'
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.090
_refine_ls_goodness_of_fit_obs   1.190
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_restrained_S_obs      1.190
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_obs          0.0753
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0792P)²+7.7467P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2196
_refine_ls_wR_factor_obs         0.1790
_reflns_number_observed          2451
_reflns_number_total             3811
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic049013usi20041111_015420_1.cif
_cod_data_source_block           Compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+7.7467P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+7.7467P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2633.0(10)
_cod_original_formula_sum        'C17 H44 N5 Si2 Cl Ti'
_cod_database_code               4308482
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ti Ti 0.02235(12) 0.77014(9) 0.23971(7) 0.0250(3) Uani 1 d . .
Cl Cl 0.1050(2) 0.7928(2) 0.36835(11) 0.0495(6) Uani 1 d . .
N1 N 0.0464(6) 0.7684(4) 0.1260(3) 0.0296(13) Uani 1 d . .
N2 N 0.2169(6) 0.7493(4) 0.2169(3) 0.0276(14) Uani 1 d . .
C3 C 0.1759(7) 0.7516(4) 0.1419(4) 0.0231(15) Uani 1 d . .
N4 N 0.2607(6) 0.7391(4) 0.0879(3) 0.0284(13) Uani 1 d . .
C5 C -0.0332(8) 0.7602(6) 0.0512(4) 0.039(2) Uani 1 d . .
H5A H 0.0289(8) 0.7603(6) 0.0137(4) 0.047 Uiso 1 calc R .
C6 C -0.1291(9) 0.8408(7) 0.0338(5) 0.054(2) Uani 1 d . .
H6A H -0.0783(9) 0.8982(7) 0.0395(5) 0.081 Uiso 1 calc R .
H6B H -0.1934(9) 0.8404(7) 0.0687(5) 0.081 Uiso 1 calc R .
H6C H -0.1773(9) 0.8357(7) -0.0180(5) 0.081 Uiso 1 calc R .
C7 C -0.1133(11) 0.6718(7) 0.0421(5) 0.061(3) Uani 1 d . .
H7A H -0.0524(11) 0.6196(7) 0.0532(5) 0.091 Uiso 1 calc R .
H7B H -0.1615(11) 0.6670(7) -0.0097(5) 0.091 Uiso 1 calc R .
H7C H -0.1776(11) 0.6717(7) 0.0770(5) 0.091 Uiso 1 calc R .
C8 C 0.3572(7) 0.7440(5) 0.2513(4) 0.033(2) Uani 1 d . .
H8A H 0.4104(7) 0.7257(5) 0.2118(4) 0.039 Uiso 1 calc R .
C9 C 0.4091(9) 0.8359(7) 0.2839(6) 0.057(2) Uani 1 d . .
H9A H 0.3966(9) 0.8823(7) 0.2441(6) 0.085 Uiso 1 calc R .
H9B H 0.5045(9) 0.8307(7) 0.3049(6) 0.085 Uiso 1 calc R .
H9C H 0.3596(9) 0.8539(7) 0.3238(6) 0.085 Uiso 1 calc R .
C10 C 0.3766(9) 0.6714(7) 0.3133(5) 0.051(2) Uani 1 d . .
H10A H 0.3431(9) 0.6123(7) 0.2922(5) 0.076 Uiso 1 calc R .
H10B H 0.3270(9) 0.6892(7) 0.3532(5) 0.076 Uiso 1 calc R .
H10C H 0.4720(9) 0.6660(7) 0.3344(5) 0.076 Uiso 1 calc R .
Si11 Si 0.2913(2) 0.6254(2) 0.06203(12) 0.0372(5) Uani 1 d . .
C12 C 0.2315(12) 0.5452(6) 0.1277(6) 0.064(3) Uani 1 d . .
H12A H 0.1354(12) 0.5543(6) 0.1264(6) 0.096 Uiso 1 calc R .
H12B H 0.2796(12) 0.5563(6) 0.1788(6) 0.096 Uiso 1 calc R .
H12C H 0.2477(12) 0.4822(6) 0.1128(6) 0.096 Uiso 1 calc R .
C13 C 0.2003(13) 0.5988(8) -0.0354(5) 0.070(3) Uani 1 d . .
H13A H 0.2304(13) 0.6407(8) -0.0716(5) 0.105 Uiso 1 calc R .
H13B H 0.1038(13) 0.6062(8) -0.0371(5) 0.105 Uiso 1 calc R .
H13C H 0.2193(13) 0.5356(8) -0.0485(5) 0.105 Uiso 1 calc R .
C14 C 0.4728(11) 0.6099(8) 0.0632(7) 0.074(3) Uani 1 d . .
H14A H 0.5030(11) 0.6530(8) 0.0280(7) 0.111 Uiso 1 calc R .
H14B H 0.4898(11) 0.5471(8) 0.0481(7) 0.111 Uiso 1 calc R .
H14C H 0.5218(11) 0.6212(8) 0.1140(7) 0.111 Uiso 1 calc R .
Si15 Si 0.3259(2) 0.8369(2) 0.05057(13) 0.0379(5) Uani 1 d . .
C16 C 0.2962(13) 0.8330(9) -0.0531(6) 0.075(3) Uani 1 d . .
H16A H 0.3389(13) 0.7784(9) -0.0698(6) 0.113 Uiso 1 calc R .
H16B H 0.3343(13) 0.8878(9) -0.0726(6) 0.113 Uiso 1 calc R .
H16C H 0.1997(13) 0.8308(9) -0.0719(6) 0.113 Uiso 1 calc R .
C17 C 0.5087(9) 0.8484(8) 0.0827(7) 0.068(3) Uani 1 d . .
H17A H 0.5544(9) 0.7946(8) 0.0668(7) 0.102 Uiso 1 calc R .
H17B H 0.5274(9) 0.8531(8) 0.1377(7) 0.102 Uiso 1 calc R .
H17C H 0.5410(9) 0.9036(8) 0.0607(7) 0.102 Uiso 1 calc R .
C18 C 0.2458(10) 0.9394(6) 0.0820(6) 0.058(3) Uani 1 d . .
H18A H 0.2615(10) 0.9414(6) 0.1371(6) 0.087 Uiso 1 calc R .
H18B H 0.1493(10) 0.9371(6) 0.0631(6) 0.087 Uiso 1 calc R .
H18C H 0.2838(10) 0.9942(6) 0.0624(6) 0.087 Uiso 1 calc R .
N19 N -0.0927(6) 0.8726(4) 0.2304(4) 0.0362(15) Uani 1 d . .
C20 C -0.0626(11) 0.9593(6) 0.1988(6) 0.058(2) Uani 1 d . .
H20A H -0.1440(11) 0.9843(6) 0.1684(6) 0.087 Uiso 1 d R .
H20B H 0.0057(11) 0.9505(6) 0.1670(6) 0.087 Uiso 1 d R .
H20C H -0.0291(11) 1.0021(6) 0.2396(6) 0.087 Uiso 1 d R .
C21 C -0.1918(10) 0.8828(6) 0.2787(6) 0.054(2) Uani 1 d . .
H21A H -0.2037(10) 0.8243(6) 0.3032(6) 0.081 Uiso 1 d R .
H21B H -0.2771(10) 0.9019(6) 0.2485(6) 0.081 Uiso 1 d R .
H21C H -0.1618(10) 0.9293(6) 0.3170(6) 0.081 Uiso 1 d R .
N22 N -0.0818(7) 0.6666(5) 0.2456(4) 0.038(2) Uani 1 d . .
C23 C -0.2260(9) 0.6554(7) 0.2265(6) 0.053(2) Uani 1 d . .
H23A H -0.2668(9) 0.7132(7) 0.2070(6) 0.080 Uiso 1 d R .
H23B H -0.2618(9) 0.6376(7) 0.2716(6) 0.080 Uiso 1 d R .
H23C H -0.2467(9) 0.6077(7) 0.1881(6) 0.080 Uiso 1 d R .
C24 C -0.0156(10) 0.5829(6) 0.2738(7) 0.061(3) Uani 1 d . .
H24A H 0.0813(10) 0.5931(6) 0.2850(7) 0.091 Uiso 1 d R .
H24B H -0.0355(10) 0.5348(6) 0.2357(7) 0.091 Uiso 1 d R .
H24C H -0.0477(10) 0.5641(6) 0.3197(7) 0.091 Uiso 1 d R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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
N22 Ti N19 107.6(3) . . ?
N22 Ti N2 117.0(3) . . ?
N19 Ti N2 133.1(3) . . ?
N22 Ti N1 101.9(3) . . ?
N19 Ti N1 95.4(3) . . ?
N2 Ti N1 62.6(2) . . ?
N22 Ti Cl 99.7(2) . . ?
N19 Ti Cl 95.0(2) . . ?
N2 Ti Cl 91.4(2) . . ?
N1 Ti Cl 151.8(2) . . ?
N22 Ti C3 111.8(2) . . ?
N19 Ti C3 117.5(2) . . ?
N2 Ti C3 31.7(2) . . ?
N1 Ti C3 30.9(2) . . ?
Cl Ti C3 122.6(2) . . ?
C3 N1 C5 124.1(6) . . ?
C3 N1 Ti 93.8(4) . . ?
C5 N1 Ti 140.0(5) . . ?
C3 N2 C8 122.8(6) . . ?
C3 N2 Ti 93.1(4) . . ?
C8 N2 Ti 143.7(4) . . ?
N1 C3 N2 110.4(6) . . ?
N1 C3 N4 125.0(6) . . ?
N2 C3 N4 124.6(6) . . ?
N1 C3 Ti 55.2(3) . . ?
N2 C3 Ti 55.2(3) . . ?
N4 C3 Ti 178.7(4) . . ?
C3 N4 Si15 118.1(4) . . ?
C3 N4 Si11 117.2(4) . . ?
Si15 N4 Si11 124.7(3) . . ?
N1 C5 C7 111.8(7) . . ?
N1 C5 C6 111.1(7) . . ?
C7 C5 C6 108.9(7) . . ?
N2 C8 C9 111.5(6) . . ?
N2 C8 C10 110.1(6) . . ?
C9 C8 C10 109.6(7) . . ?
N4 Si11 C12 109.7(4) . . ?
N4 Si11 C14 109.3(4) . . ?
C12 Si11 C14 110.5(6) . . ?
N4 Si11 C13 111.2(4) . . ?
C12 Si11 C13 107.8(5) . . ?
C14 Si11 C13 108.3(6) . . ?
N4 Si15 C18 109.3(3) . . ?
N4 Si15 C16 110.9(5) . . ?
C18 Si15 C16 109.5(5) . . ?
N4 Si15 C17 112.0(4) . . ?
C18 Si15 C17 107.5(5) . . ?
C16 Si15 C17 107.6(6) . . ?
C20 N19 C21 111.2(7) . . ?
C20 N19 Ti 124.3(6) . . ?
C21 N19 Ti 120.7(6) . . ?
C24 N22 C23 112.1(7) . . ?
C24 N22 Ti 118.3(6) . . ?
C23 N22 Ti 129.6(6) . . ?
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 N22 1.858(7) . ?
Ti N19 1.888(6) . ?
Ti N2 2.104(6) . ?
Ti N1 2.106(6) . ?
Ti Cl 2.352(2) . ?
Ti C3 2.558(7) . ?
N1 C3 1.319(9) . ?
N1 C5 1.455(9) . ?
N2 C3 1.346(9) . ?
N2 C8 1.454(9) . ?
C3 N4 1.416(9) . ?
N4 Si15 1.757(6) . ?
N4 Si11 1.768(6) . ?
C5 C7 1.521(13) . ?
C5 C6 1.526(12) . ?
C8 C9 1.524(12) . ?
C8 C10 1.531(11) . ?
Si11 C12 1.841(10) . ?
Si11 C14 1.851(11) . ?
Si11 C13 1.882(10) . ?
Si15 C18 1.838(9) . ?
Si15 C16 1.843(10) . ?
Si15 C17 1.853(10) . ?
N19 C20 1.443(11) . ?
N19 C21 1.445(10) . ?
N22 C24 1.446(12) . ?
N22 C23 1.453(11) . ?
