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

data_4306422
_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         'C30 H70 N12 O11 Ti4'
_chemical_formula_sum            'C30 H70 N12 O11 Ti4'
_chemical_formula_weight         966.58
_chemical_name_common            'Ti Cluster'
_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                 91.892(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4138(15)
_cell_length_b                   14.9548(18)
_cell_length_c                   13.2278(16)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      2.59
_cell_volume                     2454.3(5)
_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_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            46025
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.7902
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Twinabs v. 2007/5 (Bruker, 2007)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.24(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         9157
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0654P)^2^+1.1345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                8932
_reflns_number_total             9157
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic8012415_si_002_1.cif
_cod_data_source_block           bt1171t
_cod_database_code               4306422