Titanocene and Zirconocene Complexes with Diaminoacetylenes: Formation of Unusual Metallacycles and Fulvene Complexes
Àrias, Òscar; Petrov, Alex R.; Bannenberg, Thomas; Altenburger, Kai; Arndt, Perdita; Jones, Peter G.; Rosenthal, Uwe; Tamm, Matthias; Organometallics 33 (2014) 1774–; doi:10.1021/om500121p

data_4082848
_publ_section_title
;
 Titanocene and Zirconocene Complexes with Diaminoacetylenes: Formation of
 Unusual Metallacycles and Fulvene Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1774
_journal_paper_doi               10.1021/om500121p
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C30 H50 N2 Zr'
_chemical_formula_weight         529.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.487(5)
_cell_angle_beta                 110.835(6)
_cell_angle_gamma                114.542(6)
_cell_formula_units_Z            2
_cell_length_a                   10.2288(7)
_cell_length_b                   11.7739(7)
_cell_length_c                   14.2956(8)
_cell_measurement_reflns_used    41549
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6773
_cell_measurement_theta_min      3.3624
_cell_volume                     1438.78(19)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45336
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         75.82
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    3.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_exptl_crystal_colour            'green-orange dichroic'
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+0.9023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                5915
_reflns_number_total             5952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500121p_si_001.cif
_cod_data_source_block           oscar01
_cod_depositor_comments          'Adding full bibliography for 4082848.cif.'
_cod_original_cell_volume        1438.78(15)
_cod_database_code               4082848