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_4308482
_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       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
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_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
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_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'
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_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
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_refine_ls_number_reflns         3359
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_refine_ls_restrained_S_obs      1.190
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_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^)+(0.0792P)^2^+7.7467P] where P=(Fo^2^+2Fc^2^)/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