Synthesis and structure of air-stable Lewis acidic binuclear complex of zirconocene pentafluorophenylsulfonate and its catalytic application in the allylation of carbonyl compounds with tetraallyltin.
Qiu, Renhua; Xu, Xinhua; Li, Yinhui; Zhang, Guoping; Shao, Lingling; An, Delie; Yin, Shuangfeng; Chemical communications (Cambridge, England) 34 (2009) 1679–1681; doi:10.1039/b821366f

data_7104282
_publ_section_title
;
 Synthesis and structure of air-stable Lewis acidic binuclear complex
 of zirconocene pentafluorophenylsulfonate and its catalytic
 application in the allylation of carbonyl compounds with
 tetraallyltin.
;
_journal_issue                   13
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1679
_journal_page_last               1681
_journal_paper_doi               10.1039/b821366f
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'ZrCp2,OH, H2O, OSO2C6F5'
_chemical_formula_sum            'C34 H36 F20 O26 S4 Zr2'
_chemical_formula_weight         1551.31
_chemical_name_common            (Zr2Cp2(/n2-OH)2(H2O)6(OSO2C6F5)4(H2O)6)
_chemical_name_systematic        '[Zr2Cp2(/n2-OH)2(H2O)6(OSO2C6F5)4(H2O)6]'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4274(9)
_cell_length_b                   12.0826(7)
_cell_length_c                   29.1463(17)
_cell_measurement_reflns_used    9214
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.783
_cell_measurement_theta_min      4.504
_cell_volume                     5433.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            30851
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6919
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.491
_exptl_crystal_size_mid          0.405
_exptl_crystal_size_min          0.227
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.00096(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         6169
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0743P)^2^+0.7773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                4815
_reflns_number_total             6169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b821366f.txt
_cod_data_source_block           cd27276
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7104282