Synthesis and structural characterization of an azatitanacyclobutene: the key intermediate in the catalytic anti-Markovnikov addition of primary amines to [small alpha]-alkynes.
Ward, Benjamin D; Maisse-Francois, Aline; Mountford, Philip; Gade, Lutz H; Chemical communications (Cambridge, England)  (2004) 704–705; doi:10.1039/b316383k

data_7102540
_publ_section_title
;
 Synthesis and structural characterization of an azatitanacyclobutene:
 the key intermediate in the catalytic anti-Markovnikov addition of
 primary amines to [small alpha]-alkynes.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              704
_journal_page_last               705
_journal_paper_doi               10.1039/b316383k
_journal_year                    2004
_chemical_formula_moiety         'C36 H54 N4 Si2 Ti'
_chemical_formula_sum            'C36 H54 N4 Si2 Ti'
_chemical_formula_weight         646.93
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 104.045(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9150(2)
_cell_length_b                   20.6148(4)
_cell_length_c                   18.9685(5)
_cell_measurement_reflns_used    11205
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.4
_cell_volume                     3761.2(1)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
11205 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  30. mm.
Scan angle =  1.6 deg 1 scans of   60 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    8.80 Omega =    0.00 Kappa =    0.00  121 frames
Set 2 Theta =   -6.90 Kappa = -166.00 Phi   =    0.00   30 frames
Friedel pairs were averaged. Internal R = 0.05
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11205
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.14
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.187
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4494
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.117
_refine_ls_R_factor_gt           0.054
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.189
_refine_ls_wR_factor_ref         0.071
_reflns_number_gt                4494
_reflns_number_total             11205
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b316383k.txt
_cod_data_source_block           st1475
_cod_database_code               7102540