Reactions of Group 4 Metallocene Alkyne Complexes with Carbodiimides: Experimental and Theoretical Studies of the Structure and Bonding of Five-Membered Hetero-Metallacycloallenes
Katharina Kaleta; Martin Ruhmann; Oliver Theilmann; Torsten Beweries; Subhendu Roy; Perdita Arndt; Alexander Villinger; Eluvathingal D. Jemmis; Axel Schulz; Uwe Rosenthal; Journal of the American Chemical Society 133 (2011) 5463–5473; doi:10.1021/ja111479j

data_4105907
_publ_section_title
;
 Reactions of Group 4 Metallocene Alkyne Complexes with Carbodiimides:
 Experimental and Theoretical Studies of the Structure and Bonding of
 Five-Membered Hetero-Metallacycloallenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5463
_journal_page_last               5473
_journal_paper_doi               10.1021/ja111479j
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C50 H48 N4 Ti2'
_chemical_formula_sum            'C50 H48 N4 Ti2'
_chemical_formula_weight         800.72
_chemical_name_systematic
;
 ?
;
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 94.238(3)
_cell_angle_gamma                103.346(3)
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_cell_length_a                   8.1040(6)
_cell_length_b                   10.3858(7)
_cell_length_c                   12.3515(9)
_cell_measurement_reflns_used    2606
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      45.527
_cell_measurement_theta_min      8.387
_cell_volume                     1003.96(13)
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_collection       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and psi scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12735
_diffrn_reflns_theta_full        28.51
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         4.26
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.9784
_exptl_absorpt_correction_T_min  0.8138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0683P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                2644
_reflns_number_total             4905
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja111479j_si_004.cif
_cod_data_source_block           av_ot11
_cod_original_cell_volume        1003.96(12)
_cod_database_code               4105907