Facile Synthesis of Monoazidotitanium Isopropoxides
Sukesh Shekar; Brendan Twamley; Rudolf J. Wehmschulte; Inorganic Chemistry 47 (2008) 10804–10806; doi:10.1021/ic8012415

data_4306423
_publ_contact_author_address
;       Department of Chemistry
        Florida Institute of Technology
        150 West University Blvd.
        Melbourne, FL 32901
;
_publ_contact_author_email       rwehmsch@fit.edu
_publ_contact_author_fax         '321 674 8951'
_publ_contact_author_name        'Rudolf J. Wehmschulte'
_publ_contact_author_phone       '321 674 7659'
_publ_section_title
;
Facile Synthesis of Monoazidotitanium Isopropoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10804
_journal_page_last               10806
_journal_paper_doi               10.1021/ic8012415
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C36 H84 N12 O12 Ti4'
_chemical_formula_sum            'C36 H84 N12 O12 Ti4'
_chemical_formula_weight         1068.75
_chemical_name_common            '{N3 Ti (OiPr)3 }4'
_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                66.767(1)
_cell_angle_beta                 72.717(2)
_cell_angle_gamma                69.662(1)
_cell_formula_units_Z            1
_cell_length_a                   10.4433(9)
_cell_length_b                   11.9712(10)
_cell_length_c                   13.2598(11)
_cell_measurement_reflns_used    7962
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.33
_cell_volume                     1403.5(2)
_computing_cell_refinement       'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_data_collection       'SMART v. 5.632 (Bruker, 2006)'
_computing_data_reduction        'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_molecular_graphics    'XP, SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)'
_computing_structure_refinement  'XL, SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_structure_solution    'XS, SHELXTL  v. 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            20624
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.70
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.8830
_exptl_absorpt_correction_T_min  0.7428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2007/4 (Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.857
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5078
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+1.7846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                4124
_reflns_number_total             5078
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic8012415_si_002_2.cif
_cod_data_source_block           bt1182
_cod_database_code               4306423