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_4085353
_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            'C36 H38 Si2 Zr'
_chemical_formula_weight         618.06
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 106.7800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6414(8)
_cell_length_b                   11.7600(7)
_cell_length_c                   20.4613(11)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.21
_cell_volume                     3142.7(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33595
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.020
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+1.9110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6067
_reflns_number_total             7228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501205s_si_002.cif
_cod_data_source_block           complex_12
_cod_depositor_comments
'Adding full bibliography for 4085350--4085354.cif.'
_cod_database_code               4085353
_shelxl_version_number           2014-3
_shelx_res_checksum              3699
_shelx_hkl_checksum              41132