Unexpected Cyclopentadienyl/Alkoxo Ligand Exchange in Titano- and Zirconocene. New Opportunities
Piotr Sobota; Józef Utko; Łukasz John; Lucjan B. Jerzykiewicz; Anna Drág-Jarzábek; Inorganic Chemistry 47 (2008) 7939–7941; doi:10.1021/ic8009749

data_4306057
_publ_section_title
;
Unexpected Cyclopentadienyl/Alkoxo Ligand Exchange in Titano- and
Zirconocene. New Opportunities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7939
_journal_page_last               7941
_journal_paper_doi               10.1021/ic8009749
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         '2(C34 H65 Ca4 Cl6 O16 Zr2), 3(C H2 Cl2)'
_chemical_formula_sum            'C71 H136 Ca8 Cl18 O32 Zr4'
_chemical_formula_weight         2825.42
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.19(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.259(7)
_cell_length_b                   17.216(5)
_cell_length_c                   23.455(6)
_cell_measurement_reflns_used    2531
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     11769(6)
_computing_cell_refinement
;
CrysAlis RED. Version 1.171.31 Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD. Version 1.171.31 (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED. Version 1.171.31 (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
' DIAMOND. Version 3.1e. (Brandenburg, K.  2007)'
_computing_publication_material
;
SHELXTL. Version 6.14 (Bruker, 2003)
Platon Version 1.081 (Spek, A. L. 2005)
;
_computing_structure_refinement  'SHELXTL. Version 6.14 (Bruker, 2003)'
_computing_structure_solution    'SHELXTL. Version 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Kuma KM-4 CCD kappa-axis diffractometer'
_diffrn_measurement_method       \w
_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  0.1334
_diffrn_reflns_av_sigmaI/netI    0.2356
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49331
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis CCD. Version 1.171.31 (Oxford Diffraction Ltd., 2006)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S.
Comput. Phys. Commun. (1998). 111, 243.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             5776
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         14064
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.1720
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0383P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                7562
_reflns_number_total             14064
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8009749_si_002_2.cif
_cod_data_source_block           CCDC677967
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        11769(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C71 H136 Ca8 Cl18 O32 Zr4 '
_cod_database_code               4306057