<i>cyclo</i>-Tri-μ-oxido-tris{[(η^5^,η^5^)-1,2-bis(cyclopentadienyl)-1,1,2,2-tetramethyldisilane]zirconium(IV)}: a trimeric disila-bridged oxidozirconocene
Arnold, Thomas; Braunschweig, Holger; Gruss, Katrin; Acta Crystallographica Section E 67 (2011) m391–; doi:10.1107/S1600536811007094

data_2229849
_publ_section_title
;
 <i>cyclo</i>-Tri-\m-oxido-tris{[(\h^5^,\h^5^)-1,2-bis(cyclopentadienyl)-1,1,2,2-tetramethyldisilane]zirconium(IV)}:
 a trimeric disila-bridged oxidozirconocene
;
_journal_coeditor_code           SU2258
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m391
_journal_paper_doi               10.1107/S1600536811007094
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Zr3 (C14 H20 Si2)3 O3]'
_chemical_formula_moiety         'C42 H60 O3 Si6 Zr3'
_chemical_formula_sum            'C42 H60 O3 Si6 Zr3'
_chemical_formula_weight         1055.10
_chemical_name_systematic
<i>cyclo</i>-Tri-\m-oxido-tris{[(\h^5^,\h^5^)-1,2-bis(cyclopentadienyl)-1,1,2,2-tetramethyldisilane]zirconium(IV)}
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.7830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5399(7)
_cell_length_b                   26.667(2)
_cell_length_c                   20.9072(18)
_cell_measurement_reflns_used    7751
_cell_measurement_temperature    174(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.48
_cell_volume                     4737.0(7)
_computing_cell_refinement       'SAINT-Plus-NT (Bruker, 2007)'
_computing_data_collection       'SMART-NT (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus-NT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      174(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            126251
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.56029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         11796
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+3.3311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                10301
_reflns_number_total             11796
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2258.cif
_cod_data_source_block           I
_cod_original_cell_volume        4737.1(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2229849
_cod_database_fobs_code          2229849