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_4082237
_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         'C45 H35 N Si Ti, C4 H4 O'
_chemical_formula_sum            'C49 H43 N O Si Ti'
_chemical_formula_weight         737.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-11-21
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.915(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2653(6)
_cell_length_b                   19.3916(6)
_cell_length_c                   24.7760(8)
_cell_measurement_reflns_used    7532
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.1200
_cell_measurement_theta_min      3.3210
_cell_volume                     7551.3(5)
_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
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.9923
_diffrn_measured_fraction_theta_max 0.8206
_diffrn_measurement_details
;
  1 omega   35.00   99.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  178.0000  -90.0000 64

  2 omega  -60.00   36.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -57.0000   60.0000 96
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0389917000
_diffrn_orient_matrix_UB_12      0.0184292000
_diffrn_orient_matrix_UB_13      0.0071018000
_diffrn_orient_matrix_UB_21      -0.0054069000
_diffrn_orient_matrix_UB_22      0.0086510000
_diffrn_orient_matrix_UB_23      -0.0285048000
_diffrn_orient_matrix_UB_31      -0.0221227000
_diffrn_orient_matrix_UB_32      0.0303881000
_diffrn_orient_matrix_UB_33      0.0038191000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14417
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_min         3.275
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94514
_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
;
;
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7392
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+16.5480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6208
_reflns_number_total             7392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om401065c_si_002.cif
_cod_data_source_block           13sep06b
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-18343/cifs/4082237.cif.
;
_cod_original_cell_volume        7551.3(4)
_cod_database_code               4082237
_chemical_oxdiff_formula         'C46 H17 N1 Si1 Ti1'
_reflns_odcompleteness_completeness 99.23
_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
2. Restrained distances
 O1-C48
 1.48 with sigma of 0.01
 O1-C49
 1.48 with sigma of 0.01
 O1A-C48
 1.48 with sigma of 0.01
 O1A-C48
 1.48 with sigma of 0.01
3. Others
 Fixed Sof: O1(0.5) O1A(0.5)
4.a Ternary CH refined with riding coordinates:
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45)
4.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C47(H47A,H47B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35)
;
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.943
_shelxl_version_number           2013-3