Pentacarbonyl-2κ<i>^5^C-</i>chlorido-1κ<i>Cl-</i>bis[1(η^5^)-cyclopentadienyl][μ~2~-oxido(methyl)methylene-1:2κ^2^<i>O</i>:<i>C</i>]tungsten(0)zirconium(IV)
Esterhuysen, Catharine; Neveling, Arno; Luruli, Nyambeni; Kruger, Gert J.; Cronje, Stephanie; Acta Crystallographica Section E 64 (2008) m1252–; doi:10.1107/S1600536808028006

data_2219675
_publ_section_title
Pentacarbonyl-2\k<i>^5^C-</i>chlorido-1\k<i>Cl-</i>bis[1(\h^5^)-cyclopentadienyl][\m~2~-oxido(methyl)methylene-1:2\k^2^<i>O</i>:<i>C</i>]tungsten(0)zirconium(IV)
_journal_coeditor_code           OM2260
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1252
_journal_paper_doi               10.1107/S1600536808028006
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Zr W (C5 H5)2 (C2 H3 O) Cl (C O)5]'
_chemical_formula_moiety         'C17 H13 Cl O6 W Zr'
_chemical_formula_sum            'C17 H13 Cl O6 W Zr'
_chemical_formula_weight         623.79
_chemical_name_systematic
;
Pentacarbonyl-2\k<i>^5^C-</i>chlorido-1\k<i>Cl-</i>bis[1(\h^5^)-\
cyclopentadienyl][\m~2~-oxido(methyl)methylene-1:2\k^2^<i>O</i>:<i>C</i>]\
tungsten(IV)zirconium(0)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.3794(8)
_cell_length_b                   12.3852(7)
_cell_length_c                   7.2404(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      2
_cell_volume                     2006.85(16)
_computing_cell_refinement       'PWPC (Gomm, 1998)'
_computing_data_collection       'PWPC (Gomm, 1998)'
_computing_data_reduction        'XTAL3.4 (Hall <i>et al.</i>,  1995)'
_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      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Philips PW1100 diffractometer'
_diffrn_measurement_method       '\w/2\q 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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2070
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.407
_exptl_absorpt_correction_T_max  0.2580
_exptl_absorpt_correction_T_min  0.2193
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.145
_refine_diff_density_min         -1.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0530P)^2^+1.7971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                1521
_reflns_number_total             1851
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2260.cif
_cod_data_source_block           I
_cod_database_code               2219675
_cod_database_fobs_code          2219675