Monomeric Titanium(IV) Azides as a New Route to Titanium Nitride
Claire J. Carmalt; Alan H. Cowley; Robert D. Culp; Richard A. Jones; Yang-Ming Sun; Bill Fitts; Sandra Whaley; Herbert W. Roesky; Inorganic Chemistry 36 (1997) 3108–3112; doi:10.1021/ic9614834

data_4323493
_publ_section_title
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 Monomeric Titanium(IV) Azides as a New Route to Titanium Nitride
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_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            'C14 H22 N10 Ti'
_chemical_formula_weight         378.32
_chemical_name_common            '[Ti(NMe2)2(N3)2(py)2]'
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1200(10)
_cell_length_b                   15.899(3)
_cell_length_c                   16.946(4)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      12.1
_cell_measurement_theta_min      11.4
_cell_volume                     1918.3(6)
_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       '\w 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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            1507
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        1.56
_diffrn_standards_interval_count 96
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.8752
_exptl_absorpt_correction_T_min  0.8002
_exptl_absorpt_correction_type   'Face-Centered Index'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       'triangular prism'
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_coef       0.0040(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.097
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.325
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_obs          0.0418
_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/[\s^2^(Fo^2^)+(0.0537P)^2^+1.5283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1269
_refine_ls_wR_factor_obs         0.1015
_reflns_number_observed          1284
_reflns_number_total             1458
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9614834_2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+1.5283P] 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^)+(0.0537P)^2^+1.5283P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323493