Five-Membered Zirconacycloallenoids: Synthesis and Characterization of Members of a Unique Class of Internally Metal-Stabilized Bent Allenoid Compounds
Juri Ugolotti; Gerald Kehr; Roland Fröhlich; Stefan Grimme; Gerhard Erker; Journal of the American Chemical Society 131 (2009) 1996–2007; doi:10.1021/ja8084302

data_4103889
_publ_section_title
;
 Five-Membered Zirconacycloallenoids: Synthesis and Characterization of
 Members of a Unique Class of Internally Metal-Stabilized Bent Allenoid
 Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1996
_journal_page_last               2007
_journal_paper_doi               10.1021/ja8084302
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C45 H57 B F10 Si2 Zr'
_chemical_formula_weight         946.12
_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                111.166(1)
_cell_angle_beta                 94.238(1)
_cell_angle_gamma                111.542(1)
_cell_formula_units_Z            2
_cell_length_a                   12.0655(1)
_cell_length_b                   14.5258(2)
_cell_length_c                   15.7909(3)
_cell_measurement_reflns_used    3351
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41
_cell_volume                     2331.55(7)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22053
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  0.9160
_exptl_absorpt_correction_T_min  0.8852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         11248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.7303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                8750
_reflns_number_total             11248
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8084302_si_003.cif
_cod_data_source_block           erk4538
_cod_original_cell_volume        2331.55(6)
_cod_database_code               4103889