Group 4 Dimethylmetallocenes: Improved Synthesis and Reactivity Studies
Davide Balboni; Isabella Camurati; Giansiro Prini; Luigi Resconi; Simona Galli; Pierluigi Mercandelli; Angelo Sironi; Inorganic Chemistry 40 (2001) 6588–6597; doi:10.1021/ic010018q

data_4320684
_publ_section_title
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 Group 4 Dimethylmetallocenes: Improved Synthesis and Reactivity Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6588
_journal_page_last               6597
_journal_paper_doi               10.1021/ic010018q
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C36 H24 F10 O2 Zr'
_chemical_formula_sum            'C36 H24 F10 O2 Zr'
_chemical_formula_weight         769.77
_chemical_melting_point          ?
_chemical_name_systematic
;
 rac-[ethylenebis(4,7-dimethyl-\h^5^-1-indenyl)]
 bis(pentafluorophenoxo)zirconium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 114.52(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.301(4)
_cell_length_b                   15.289(6)
_cell_length_c                   14.334(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     3050.8(19)
_computing_structure_refinement
;
 Sheldrick, G. M. SHELX97: program for crystal structure refinement;
 University of G\"ottingen: G\"ottingen, 1996.
;
_computing_structure_solution
;
 SIR96: Altomare, A.; Cascarano, G.; Giacovazzo, C.; Guagliardi, A.;
 Burla, M. C.; Polidori, C.; Camalli, M. J. Appl. Crystallogr. 1994, 27, 435.
;
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.600
_diffrn_measured_fraction_theta_max 0.600
_diffrn_measurement_details
;
 scan range: (0.80 + 0.35tan\q)\% 
 maximum time per reflection: 50 s
 required \s(I)/I: 0.01
;
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5544
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9460
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 Psi-scan of 3 reflections having \c values near 90\% .
 North, A. C. T.; Phillips, D. C.; Mathews, F. S.
 Acta Crystallogr. 1968, A24, 351.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         3211
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.034P)^2^+1.09P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                3211
_reflns_number_total             5341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic010018q_2.cif
_cod_data_source_block           compound-m6c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_cell_volume        3050.8(18)
_cod_database_code               4320684