Pentacarbonyl-2κ^5^<i>C</i>-chlorido-1κ<i>Cl</i>-bis[1(η^5^)-cyclopentadienyl][μ-oxido(phenyl)methylene-1:2κ^2^<i>O</i>:<i>C</i>]hafnium(IV)tungsten(0)
Esterhuysen, Catharine; Nel, I. B. Jacques; Cronje, Stephanie; Acta Crystallographica Section E 64 (2008) m1150–; doi:10.1107/S1600536808025245

data_2219445
_publ_section_title
Pentacarbonyl-2\k^5^<i>C</i>-chlorido-1\k<i>Cl</i>-bis[1(\h^5^)-cyclopentadienyl][\m-oxido(phenyl)methylene-1:2\k^2^<i>O</i>:<i>C</i>]hafnium(IV)tungsten(0)
_journal_coeditor_code           TK2291
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1150
_journal_paper_doi               10.1107/S1600536808025245
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Hf W (C5 H5)2 (C7 H5 O) Cl (C O)5]'
_chemical_formula_moiety         'C22 H15 Cl Hf O6 W'
_chemical_formula_sum            'C22 H15 Cl Hf O6 W'
_chemical_formula_weight         773.13
_chemical_name_systematic
;
Pentacarbonyl-2\k^5^<i>C</i>-chlorido-1\k<i>Cl</i>-bis[1(\h^5^)-
cyclopentadienyl][\m-oxido(phenyl)methylene-
1:2\k^2^<i>O</i>:<i>C</i>]hafnium(IV)tungsten(0)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 96.1520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5422(2)
_cell_length_b                   12.5546(3)
_cell_length_c                   21.0237(7)
_cell_measurement_reflns_used    12410
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.9
_cell_volume                     2241.68(11)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'X-SEED (Barbour, 2001; Atwood & Barbour, 2003)'
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans to fill Ewald sphere'
_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  0.049
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12410
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    9.910
_exptl_absorpt_correction_T_max  0.089
_exptl_absorpt_correction_T_min  0.056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.61
_refine_diff_density_min         -1.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.074
_refine_ls_wR_factor_ref         0.079
_reflns_number_gt                4234
_reflns_number_total             5106
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2291.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2219445
_cod_database_fobs_code          2219445