Reaction of Titanacyclobutene‒Silacyclobutene Fused-Ring Complexes with Nitriles via Formal Insertion of the C‒N Triple Bond of Nitrile into the Silacyclobutene Ring
Zhao, Jing; Zhang, Shaoguang; Zhang, Wen-Xiong; Xi, Zhenfeng; Organometallics 33 (2014) 8–; doi:10.1021/om401065c

data_4082236
_publ_section_title
;
 Reaction of Titanacyclobutene--Silacyclobutene Fused-Ring Complexes with
 Nitriles via Formal Insertion of the C--N Triple Bond of Nitrile into the
 Silacyclobutene Ring
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              8
_journal_paper_doi               10.1021/om401065c
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C35 H31 N Si Ti'
_chemical_formula_sum            'C35 H31 N Si Ti'
_chemical_formula_weight         541.60
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-29
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.916(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9762(8)
_cell_length_b                   11.2754(4)
_cell_length_c                   17.1936(9)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    99.98(11)
_cell_measurement_theta_max      30.2688
_cell_measurement_theta_min      2.9009
_cell_volume                     2785.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      99.98(11)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9822
_diffrn_measurement_details
;
  1 omega    1.00   86.00   1.0000    2.6000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   77.0000  120.0000 85

  2 omega  -65.00   47.00   1.0000    2.6000
omega____ theta____ kappa____ phi______ frames
    -       13.6191  -77.0000   30.0000 112

  3 omega    2.00   39.00   1.0000    2.6000
omega____ theta____ kappa____ phi______ frames
    -       13.6191  -38.0000 -120.0000 37

  4 omega   34.00  100.00   1.0000    2.6000
omega____ theta____ kappa____ phi______ frames
    -       13.6191 -178.0000   30.0000 66

  5 omega    1.00   29.00   1.0000    2.6000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   38.0000  -90.0000 28

  6 omega   47.00   89.00   1.0000    2.6000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   38.0000  -90.0000 42

  7 omega  -18.00   20.00   1.0000    2.6000
omega____ theta____ kappa____ phi______ frames
    -      -14.4003  -85.0000  163.0000 38
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0196563000
_diffrn_orient_matrix_UB_12      0.0079482000
_diffrn_orient_matrix_UB_13      -0.0295126000
_diffrn_orient_matrix_UB_21      0.0399582000
_diffrn_orient_matrix_UB_22      -0.0323793000
_diffrn_orient_matrix_UB_23      0.0279351000
_diffrn_orient_matrix_UB_31      -0.0213186000
_diffrn_orient_matrix_UB_32      -0.0532970000
_diffrn_orient_matrix_UB_33      -0.0213227000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23411
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.91
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0435P)^2^+1.4439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                4198
_reflns_number_total             4911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401065c_si_002.cif
_cod_data_source_block           zhaoj
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-18343/cifs/4082236.cif.
;
_cod_original_cell_volume        2785.8(2)
_cod_database_code               4082236
_chemical_oxdiff_formula         C35H40NTiSi
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42