#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:35:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179337 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/34/4323492.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_4323492
loop_
_publ_author_name
'Claire J. Carmalt'
'Alan H. Cowley'
'Robert D. Culp'
'Richard A. Jones'
'Yang-Ming Sun'
'Bill Fitts'
'Sandra Whaley'
'Herbert W. Roesky'
_publ_section_title
;
 Monomeric Titanium(IV) Azides as a New Route to Titanium Nitride
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3108
_journal_page_last               3112
_journal_paper_doi               10.1021/ic9614834
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C16 H26 N8 Ti'
_chemical_formula_weight         378.35
_chemical_name_common            '[Ti(NMe2)3(N3)(bipy)]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 108.390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.682(2)
_cell_length_b                   8.8140(10)
_cell_length_c                   15.1280(10)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      8.27
_cell_measurement_theta_min      4.53
_cell_volume                     1984.2(4)
_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      178(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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_sigmaI/netI    0.1611
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3685
_diffrn_reflns_theta_max         23.74
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        1.46
_diffrn_standards_interval_count 96
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.96553
_exptl_absorpt_correction_T_min  0.57577
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.178
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.178
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_obs          0.0671
_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)+(0.0167P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0977
_refine_ls_wR_factor_obs         0.0753
_reflns_number_observed          1159
_reflns_number_total             2242
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9614834_1.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.0000P] 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^)+(0.0167P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323492
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ti1 Ti 0.77124(7) 0.01202(14) 0.80399(10) 0.0263(5) Uani 1 d . .
N1 N 0.6440(3) 0.1211(6) 0.7845(4) 0.031(2) Uani 1 d . .
N2 N 0.5874(4) 0.1706(6) 0.7180(5) 0.034(2) Uani 1 d . .
N3 N 0.5319(4) 0.2234(7) 0.6553(5) 0.048(2) Uani 1 d . .
N4 N 0.8749(3) -0.0973(6) 0.7949(4) 0.033(2) Uani 1 d . .
N5 N 0.8327(3) 0.2046(6) 0.8328(4) 0.038(2) Uani 1 d . .
N6 N 0.7712(3) -0.0754(6) 0.9205(4) 0.026(2) Uani 1 d . .
N7 N 0.6753(3) -0.1743(6) 0.7233(5) 0.023(2) Uani 1 d . .
N8 N 0.7314(4) 0.0587(6) 0.6469(4) 0.027(2) Uani 1 d . .
C1 C 0.9407(4) -0.0392(8) 0.7542(5) 0.059(3) Uani 1 d . .
H1A H 0.9383(18) 0.0719(8) 0.7529(24) 0.066(6) Uiso 1 calc R .
H1B H 0.9273(15) -0.0779(34) 0.6905(11) 0.066(6) Uiso 1 calc R .
H1C H 1.0009(5) -0.0724(36) 0.7916(16) 0.066(6) Uiso 1 calc R .
C2 C 0.8851(4) -0.2604(8) 0.8049(5) 0.059(3) Uani 1 d . .
H2A H 0.8459(21) -0.2991(10) 0.8390(24) 0.066(6) Uiso 1 calc R .
H2B H 0.9477(8) -0.2849(8) 0.8395(25) 0.066(6) Uiso 1 calc R .
H2C H 0.8686(25) -0.3075(9) 0.7432(6) 0.066(6) Uiso 1 calc R .
C3 C 0.9184(4) 0.2210(8) 0.9059(5) 0.061(3) Uani 1 d . .
H3A H 0.9621(8) 0.2677(39) 0.8801(8) 0.066(6) Uiso 1 calc R .
H3B H 0.9402(12) 0.1208(9) 0.9313(18) 0.066(6) Uiso 1 calc R .
H3C H 0.9107(7) 0.2854(35) 0.9556(13) 0.066(6) Uiso 1 calc R .
C4 C 0.7976(4) 0.3543(7) 0.8021(5) 0.053(3) Uani 1 d . .
H4A H 0.7376(12) 0.3449(7) 0.7563(19) 0.066(6) Uiso 1 calc R .
H4B H 0.8376(14) 0.4061(17) 0.7736(23) 0.066(6) Uiso 1 calc R .
H4C H 0.7936(22) 0.4131(16) 0.8557(6) 0.066(6) Uiso 1 calc R .
C5 C 0.8502(4) -0.1191(9) 0.9966(5) 0.068(3) Uani 1 d . .
H5A H 0.9026(7) -0.1218(44) 0.9745(8) 0.066(6) Uiso 1 calc R .
H5B H 0.8408(11) -0.2198(21) 1.0194(19) 0.066(6) Uiso 1 calc R .
H5C H 0.8606(16) -0.0451(26) 1.0473(12) 0.066(6) Uiso 1 calc R .
C6 C 0.6937(4) -0.0987(7) 0.9527(5) 0.042(2) Uani 1 d . .
H6A H 0.6928(15) -0.2041(13) 0.9729(25) 0.066(6) Uiso 1 calc R .
H6B H 0.6384(4) -0.0772(42) 0.9017(9) 0.066(6) Uiso 1 calc R .
H6C H 0.6978(14) -0.0304(31) 1.0050(18) 0.066(6) Uiso 1 calc R .
C7 C 0.6537(4) -0.2971(8) 0.7626(5) 0.029(2) Uani 1 d . .
H7 H 0.6846(4) -0.3147(8) 0.8267(5) 0.047(8) Uiso 1 calc R .
C8 C 0.5895(4) -0.4000(8) 0.7162(6) 0.034(2) Uani 1 d . .
H8 H 0.5758(4) -0.4850(8) 0.7479(6) 0.047(8) Uiso 1 calc R .
C9 C 0.5452(4) -0.3775(8) 0.6227(6) 0.038(2) Uani 1 d . .
H9 H 0.5013(4) -0.4477(8) 0.5882(6) 0.047(8) Uiso 1 calc R .
C10 C 0.5662(4) -0.2520(8) 0.5810(5) 0.030(2) Uani 1 d . .
H10 H 0.5353(4) -0.2327(8) 0.5171(5) 0.047(8) Uiso 1 calc R .
C11 C 0.6278(4) 0.0124(8) 0.4941(6) 0.035(2) Uani 1 d . .
H11 H 0.5791(4) -0.0445(8) 0.4547(6) 0.047(8) Uiso 1 calc R .
C12 C 0.6641(5) 0.1303(9) 0.4589(6) 0.046(3) Uani 1 d . .
H12 H 0.6401(5) 0.1572(9) 0.3950(6) 0.047(8) Uiso 1 calc R .
C13 C 0.7356(5) 0.2095(8) 0.5171(7) 0.046(3) Uani 1 d . .
H13 H 0.7630(5) 0.2894(8) 0.4937(7) 0.047(8) Uiso 1 calc R .
C14 C 0.7666(5) 0.1707(8) 0.6096(6) 0.033(2) Uani 1 d . .
H14 H 0.8157(5) 0.2263(8) 0.6493(6) 0.047(8) Uiso 1 calc R .
C15 C 0.6322(5) -0.1522(8) 0.6313(6) 0.022(2) Uani 1 d . .
C16 C 0.6634(4) -0.0229(8) 0.5884(6) 0.029(2) Uani 1 d . .
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'
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
N6 Ti1 N4 96.3(2) . . ?
N6 Ti1 N5 106.8(2) . . ?
N4 Ti1 N5 94.8(2) . . ?
N6 Ti1 N1 92.1(2) . . ?
N4 Ti1 N1 168.2(3) . . ?
N5 Ti1 N1 90.8(2) . . ?
N6 Ti1 N8 160.3(2) . . ?
N4 Ti1 N8 88.6(2) . . ?
N5 Ti1 N8 91.7(2) . . ?
N1 Ti1 N8 80.8(2) . . ?
N6 Ti1 N7 90.6(2) . . ?
N4 Ti1 N7 91.7(2) . . ?
N5 Ti1 N7 160.5(3) . . ?
N1 Ti1 N7 79.8(2) . . ?
N8 Ti1 N7 70.1(2) . . ?
N2 N1 Ti1 133.7(5) . . ?
N3 N2 N1 177.5(8) . . ?
C2 N4 C1 108.9(6) . . ?
C2 N4 Ti1 123.7(5) . . ?
C1 N4 Ti1 125.5(4) . . ?
C4 N5 C3 108.7(5) . . ?
C4 N5 Ti1 127.9(4) . . ?
C3 N5 Ti1 122.3(4) . . ?
C5 N6 C6 106.9(6) . . ?
C5 N6 Ti1 125.9(4) . . ?
C6 N6 Ti1 127.1(4) . . ?
C7 N7 C15 117.5(6) . . ?
C7 N7 Ti1 124.1(5) . . ?
C15 N7 Ti1 118.2(5) . . ?
C14 N8 C16 117.4(7) . . ?
C14 N8 Ti1 123.7(6) . . ?
C16 N8 Ti1 118.7(5) . . ?
N7 C7 C8 124.0(7) . . ?
C7 C8 C9 118.7(7) . . ?
C10 C9 C8 118.3(7) . . ?
C9 C10 C15 120.5(8) . . ?
C12 C11 C16 119.1(7) . . ?
C11 C12 C13 119.3(8) . . ?
C14 C13 C12 118.7(8) . . ?
N8 C14 C13 123.6(7) . . ?
N7 C15 C10 121.0(7) . . ?
N7 C15 C16 115.9(7) . . ?
C10 C15 C16 123.0(8) . . ?
N8 C16 C11 121.8(7) . . ?
N8 C16 C15 115.2(8) . . ?
C11 C16 C15 122.9(8) . . ?
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
Ti1 N6 1.924(6) . ?
Ti1 N4 1.932(5) . ?
Ti1 N5 1.933(5) . ?
Ti1 N1 2.150(5) . ?
Ti1 N8 2.296(6) . ?
Ti1 N7 2.300(6) . ?
N1 N2 1.194(7) . ?
N2 N3 1.163(7) . ?
N4 C2 1.449(8) . ?
N4 C1 1.452(7) . ?
N5 C4 1.448(7) . ?
N5 C3 1.453(7) . ?
N6 C5 1.452(7) . ?
N6 C6 1.459(7) . ?
N7 C7 1.329(7) . ?
N7 C15 1.356(8) . ?
N8 C14 1.339(8) . ?
N8 C16 1.358(7) . ?
C7 C8 1.372(8) . ?
C8 C9 1.379(8) . ?
C9 C10 1.364(8) . ?
C10 C15 1.388(8) . ?
C11 C12 1.371(9) . ?
C11 C16 1.394(8) . ?
C12 C13 1.378(9) . ?
C13 C14 1.372(9) . ?
C15 C16 1.469(8) . ?
