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_4085350
_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_moiety
'2(C30 H46 Si4 Zr), 0.5(C30 H46 Si4 Zr), 0.5(C30 H46 Si4 Zr)'
_chemical_formula_sum            'C30 H46 Si4 Zr'
_chemical_formula_weight         608.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.149(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.014(3)
_cell_length_b                   23.494(5)
_cell_length_c                   20.568(4)
_cell_measurement_reflns_used    973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     6644(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector''
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1615
_diffrn_reflns_av_sigmaI/netI    0.1667
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57448
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2562
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         14796
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1641
_refine_ls_R_factor_gt           0.0759
_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^)+(0.0372P)^2^+9.9135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                7797
_reflns_number_total             14796
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om501205s_si_002.cif
_cod_data_source_block           complex_8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4085350--4085354.cif.
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4085350