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_4103890
_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            'C34 H33 B F10 Si2 Zr'
_chemical_formula_weight         789.81
_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   'at B1 from difmap, others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.946(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0841(3)
_cell_length_b                   15.8190(5)
_cell_length_c                   11.5732(4)
_cell_measurement_reflns_used    3269
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41
_cell_volume                     1783.70(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12284
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.9734
_exptl_absorpt_correction_T_min  0.8765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.482
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4394
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+1.4024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                3035
_reflns_number_total             4394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8084302_si_004.cif
_cod_data_source_block           erk4560
_cod_original_cell_volume        1783.7(1)
_cod_database_code               4103890