Thermal Isomerization of the Buchwald Seven-Membered Zirconacyclocumulene and Its Interaction with Acetylenes. Synthesis and Structures of Novel Seven-Membered Zirconacyclocumulene Complexes
Burlakov, Vladimir V.; Bogdanov, Vyacheslav S.; Arndt, Perdita; Baumann, Wolfgang; Spannenberg, Anke; Lyssenko, Konstantin A.; Ananyev, Ivan V.; Rosenthal, Uwe; Shur, Vladimir B.; Organometallics 34 (2015) 2471–; doi:10.1021/om501205s

data_4085351
_publ_section_title
;
 Thermal Isomerization of the Buchwald Seven-Membered Zirconacyclocumulene
 and Its Interaction with Acetylenes. Synthesis and Structures of Novel
 Seven-Membered Zirconacyclocumulene Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2471
_journal_paper_doi               10.1021/om501205s
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C20 H38 Si4'
_chemical_formula_weight         390.86
_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                90.062(2)
_cell_angle_beta                 94.187(2)
_cell_angle_gamma                96.880(2)
_cell_formula_units_Z            2
_cell_length_a                   6.5912(2)
_cell_length_b                   13.0722(4)
_cell_length_c                   15.5139(4)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.89
_cell_measurement_theta_min      2.63
_cell_volume                     1323.47(7)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32856
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.981
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         5784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0521P)^2^+0.4013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                4638
_reflns_number_total             5784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501205s_si_002.cif
_cod_data_source_block           compound_9
_cod_depositor_comments
'Adding full bibliography for 4085350--4085354.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085351