#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/17/4311774.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_4311774
loop_
_publ_author_name
'Shih-Hsien Hsu'
'Jr-Chiuan Chang'
'Chun-Liang Lai'
'Ching-Han Hu'
'Hon Man Lee'
'Gene-Hsiang Lee'
'Shie-Ming Peng'
'Jui-Hsien Huang'
_publ_section_title
;
 Terminal Titanium-Ligand Multiple Bonds. Cleavages of CO and CS Double
 Bonds with Ti Imido Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6786
_journal_page_last               6792
_journal_paper_doi               10.1021/ic049474f
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C21 H34 N2'
_chemical_formula_weight         314.50
_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                103.271(2)
_cell_angle_beta                 97.482(2)
_cell_angle_gamma                109.561(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1758(6)
_cell_length_b                   10.8200(7)
_cell_length_c                   11.9514(8)
_cell_measurement_reflns_used    1913
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.66
_cell_measurement_theta_min      2.42
_cell_volume                     1060.12(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART ApexCCD area detector'
_diffrn_measurement_method       '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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14143
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  0.9876
_exptl_absorpt_correction_T_min  0.9842
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.985
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.149
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1153P)²+0.1759P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2453
_reflns_number_gt                2834
_reflns_number_total             4854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049474fsi20040424_121107.cif
_cod_data_source_block           ic10318
_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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4311774
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
N1 N 0.3322(2) 0.29272(17) 0.20796(14) 0.0504(5) Uani 1 1 d . . .
N2 N 0.3676(2) 0.2111(2) -0.01398(16) 0.0672(6) Uani 1 1 d . . .
H2A H 0.3143 0.2044 0.0399 0.081 Uiso 1 1 calc R . .
C1 C 0.6163(3) 0.3442(4) -0.0605(3) 0.0959(10) Uani 1 1 d . . .
H1A H 0.5626 0.3615 -0.1262 0.144 Uiso 1 1 calc R . .
H1B H 0.6444 0.2667 -0.0885 0.144 Uiso 1 1 calc R . .
H1C H 0.7106 0.4234 -0.0199 0.144 Uiso 1 1 calc R . .
C2 C 0.5083(3) 0.3148(3) 0.0228(2) 0.0619(6) Uani 1 1 d . . .
C3 C 0.5575(3) 0.3965(3) 0.1368(2) 0.0640(6) Uani 1 1 d . . .
H3A H 0.6579 0.4658 0.1574 0.077 Uiso 1 1 calc R . .
C4 C 0.4716(3) 0.3870(2) 0.22778(19) 0.0567(6) Uani 1 1 d . . .
C5 C 0.5507(4) 0.4940(3) 0.3466(2) 0.0961(10) Uani 1 1 d . . .
H5A H 0.4711 0.5043 0.3885 0.144 Uiso 1 1 calc R . .
H5B H 0.6100 0.5801 0.3350 0.144 Uiso 1 1 calc R . .
H5C H 0.6212 0.4654 0.3914 0.144 Uiso 1 1 calc R . .
C6 C 0.2419(2) 0.2814(2) 0.29583(16) 0.0485(5) Uani 1 1 d . . .
C7 C 0.1396(3) 0.3523(2) 0.30921(19) 0.0563(6) Uani 1 1 d . . .
C8 C 0.0434(3) 0.3293(3) 0.3893(2) 0.0736(7) Uani 1 1 d . . .
H8A H -0.0248 0.3759 0.3999 0.088 Uiso 1 1 calc R . .
C9 C 0.0470(3) 0.2393(3) 0.4526(2) 0.0785(8) Uani 1 1 d . . .
H9A H -0.0180 0.2257 0.5058 0.094 Uiso 1 1 calc R . .
C10 C 0.1459(3) 0.1697(3) 0.4377(2) 0.0706(7) Uani 1 1 d . . .
H10A H 0.1472 0.1088 0.4811 0.085 Uiso 1 1 calc R . .
C11 C 0.2444(3) 0.1878(2) 0.35940(18) 0.0563(6) Uani 1 1 d . . .
C12 C 0.1302(3) 0.4465(3) 0.2342(2) 0.0723(7) Uani 1 1 d . . .
H12A H 0.2351 0.4841 0.2172 0.087 Uiso 1 1 calc R . .
C13 C 0.0139(5) 0.3657(4) 0.1177(3) 0.1154(13) Uani 1 1 d . . .
H13A H 0.0443 0.2934 0.0785 0.173 Uiso 1 1 calc R . .
H13B H 0.0139 0.4253 0.0694 0.173 Uiso 1 1 calc R . .
H13C H -0.0905 0.3270 0.1312 0.173 Uiso 1 1 calc R . .
C14 C 0.0906(6) 0.5671(4) 0.2943(4) 0.1320(15) Uani 1 1 d . . .
H14A H 0.0986 0.6273 0.2456 0.198 Uiso 1 1 calc R . .
H14B H 0.1638 0.6160 0.3693 0.198 Uiso 1 1 calc R . .
H14C H -0.0156 0.5341 0.3060 0.198 Uiso 1 1 calc R . .
C15 C 0.3517(3) 0.1086(3) 0.3425(2) 0.0740(7) Uani 1 1 d . . .
H15A H 0.3913 0.1207 0.2718 0.089 Uiso 1 1 calc R . .
C16 C 0.4944(5) 0.1637(5) 0.4442(4) 0.1490(18) Uani 1 1 d . . .
H16A H 0.5639 0.1160 0.4269 0.224 Uiso 1 1 calc R . .
H16B H 0.4601 0.1502 0.5145 0.224 Uiso 1 1 calc R . .
H16C H 0.5498 0.2598 0.4557 0.224 Uiso 1 1 calc R . .
C17 C 0.2669(5) -0.0425(4) 0.3215(5) 0.1433(17) Uani 1 1 d . . .
H17A H 0.3418 -0.0867 0.3162 0.215 Uiso 1 1 calc R . .
H17B H 0.1874 -0.0798 0.2491 0.215 Uiso 1 1 calc R . .
H17C H 0.2173 -0.0577 0.3856 0.215 Uiso 1 1 calc R . .
C18 C 0.2853(4) 0.1069(3) -0.1261(2) 0.0859(9) Uani 1 1 d . . .
C19 C 0.1262(4) 0.0218(4) -0.1083(3) 0.1163(14) Uani 1 1 d . . .
H19A H 0.0667 0.0787 -0.0898 0.174 Uiso 1 1 calc R . .
H19B H 0.1427 -0.0158 -0.0446 0.174 Uiso 1 1 calc R . .
H19C H 0.0685 -0.0514 -0.1793 0.174 Uiso 1 1 calc R . .
C20 C 0.3730(7) 0.0098(6) -0.1554(6) 0.208(3) Uani 1 1 d . . .
H20A H 0.4623 0.0526 -0.1860 0.312 Uiso 1 1 calc R . .
H20B H 0.3023 -0.0738 -0.2133 0.312 Uiso 1 1 calc R . .
H20C H 0.4093 -0.0101 -0.0851 0.312 Uiso 1 1 calc R . .
C21 C 0.2584(8) 0.1671(6) -0.2230(4) 0.215(3) Uani 1 1 d . . .
H21A H 0.2268 0.2425 -0.1947 0.322 Uiso 1 1 calc R . .
H21B H 0.1763 0.0985 -0.2873 0.322 Uiso 1 1 calc R . .
H21C H 0.3547 0.1991 -0.2497 0.322 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'
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
C4 N1 C6 122.58(17) . . ?
C2 N2 C18 133.4(2) . . ?
N2 C2 C3 120.7(2) . . ?
N2 C2 C1 120.7(2) . . ?
C3 C2 C1 118.6(2) . . ?
C2 C3 C4 127.0(2) . . ?
N1 C4 C3 120.9(2) . . ?
N1 C4 C5 122.3(2) . . ?
C3 C4 C5 116.7(2) . . ?
C7 C6 C11 120.76(19) . . ?
C7 C6 N1 119.84(19) . . ?
C11 C6 N1 119.06(19) . . ?
C8 C7 C6 118.0(2) . . ?
C8 C7 C12 121.6(2) . . ?
C6 C7 C12 120.34(19) . . ?
C9 C8 C7 121.4(2) . . ?
C10 C9 C8 120.0(2) . . ?
C9 C10 C11 121.5(2) . . ?
C10 C11 C6 118.4(2) . . ?
C10 C11 C15 120.9(2) . . ?
C6 C11 C15 120.7(2) . . ?
C13 C12 C14 110.4(3) . . ?
C13 C12 C7 110.3(2) . . ?
C14 C12 C7 114.2(3) . . ?
C17 C15 C16 109.8(3) . . ?
C17 C15 C11 113.1(3) . . ?
C16 C15 C11 112.1(2) . . ?
N2 C18 C21 112.4(3) . . ?
N2 C18 C19 106.0(2) . . ?
C21 C18 C19 109.0(3) . . ?
N2 C18 C20 110.4(3) . . ?
C21 C18 C20 112.2(5) . . ?
C19 C18 C20 106.5(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
N1 C4 1.292(3) . ?
N1 C6 1.422(2) . ?
N2 C2 1.332(3) . ?
N2 C18 1.452(3) . ?
C1 C2 1.505(3) . ?
C2 C3 1.364(3) . ?
C3 C4 1.426(3) . ?
C4 C5 1.516(3) . ?
C6 C7 1.401(3) . ?
C6 C11 1.403(3) . ?
C7 C8 1.392(3) . ?
C7 C12 1.519(3) . ?
C8 C9 1.370(4) . ?
C9 C10 1.364(4) . ?
C10 C11 1.384(3) . ?
C11 C15 1.510(3) . ?
C12 C13 1.507(4) . ?
C12 C14 1.518(4) . ?
C15 C17 1.500(4) . ?
C15 C16 1.509(4) . ?
C18 C21 1.485(5) . ?
C18 C19 1.515(4) . ?
C18 C20 1.530(6) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660894
