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_4082235
_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         'C37 H35 N Si Ti'
_chemical_formula_sum            'C37 H35 N Si Ti'
_chemical_formula_weight         569.65
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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     iterative
_audit_creation_date             2013-10-11
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.069(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2052(3)
_cell_length_b                   17.3311(5)
_cell_length_c                   17.0297(6)
_cell_measurement_reflns_used    6452
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.9020
_cell_measurement_theta_min      3.7230
_cell_volume                     2974.35(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.9919
_diffrn_measured_fraction_theta_max 0.8327
_diffrn_measurement_details
;
  1 omega  -75.00   96.00   1.0000   13.8600
omega____ theta____ kappa____ phi______ frames
    -       10.7017    0.0000    0.0000 171
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0258797000
_diffrn_orient_matrix_UB_12      -0.0258699000
_diffrn_orient_matrix_UB_13      0.0259712000
_diffrn_orient_matrix_UB_21      0.0622730000
_diffrn_orient_matrix_UB_22      -0.0189832000
_diffrn_orient_matrix_UB_23      0.0078280000
_diffrn_orient_matrix_UB_31      0.0201607000
_diffrn_orient_matrix_UB_32      0.0254162000
_diffrn_orient_matrix_UB_33      0.0322820000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11341
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.100
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+2.0176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4460
_reflns_number_total             5222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om401065c_si_002.cif
_cod_data_source_block           zj46
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-18343/cifs/4082235.cif.
;
_cod_original_cell_volume        2974.35(17)
_cod_database_code               4082235
_chemical_oxdiff_formula         'C26 H17 N1 Si1 Ti1'
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37)
2.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C27(H27A,H27B,H27C)
;
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.932
_shelxl_version_number           2013-3