Synthesis of Titanium(IV) Guanidinate Complexes and the Formation of Titanium Carbonitride via Low-Pressure Chemical Vapor Deposition
Claire J. Carmalt; Anne C. Newport; Shane A. O'Neill; Ivan P. Parkin; Andrew J. P. White; David J. Williams; Inorganic Chemistry 44 (2005) 615–619; doi:10.1021/ic049013u

data_4308483
_publ_section_title
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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            'C23 H52.6 Cl2 N6 Si2 Ti'
_chemical_formula_weight         588.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 99.694(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9348(6)
_cell_length_b                   13.1922(12)
_cell_length_c                   13.9804(8)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      10.64
_cell_volume                     1624.3(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      183(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4/RA'
_diffrn_measurement_method       '\w 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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3030
_diffrn_reflns_theta_full        63.97
_diffrn_reflns_theta_max         63.97
_diffrn_reflns_theta_min         3.21
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.612
_exptl_absorpt_correction_T_max  0.4084
_exptl_absorpt_correction_T_min  0.2666
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             633
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(10)
_refine_ls_extinction_coef       0.0013(2)
_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_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         2907
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.4336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                2724
_reflns_number_total             2907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049013usi20041111_015420_2.cif
_cod_data_source_block           Compound_2/3
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_formula_sum        'C23 H52.60 Cl2 N6 Si2 Ti'
_cod_database_code               4308483