Water-Soluble Tungsten Hydrides: Synthesis, Structures, and Reactions of (C5H4CO2H)(CO)3WH and Related Complexes
Shafiq, Faisal; Szalda, David J.; Creutz, Carol; Bullock, R. Morris; Organometallics 19 (2000) 824–; doi:10.1021/om990778x

data_4077679
_publ_section_title
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 Water-Soluble Tungsten Hydrides:&#x00A0; Synthesis, Structures, and
 Reactions of (C5H4CO2H)(CO)3WH and Related Complexes
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_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              824
_journal_paper_doi               10.1021/om990778x
_journal_volume                  19
_journal_year                    2000
_chemical_compound_source        THF/hexanes
_chemical_formula_moiety         'C9 H6 O5 W'
_chemical_formula_structural     '[W (C5 H4 C O2 H)  H (C O)3)]'
_chemical_formula_sum            'C9 H6 O5 W'
_chemical_formula_weight         377.99
_chemical_name_systematic
;
  ?
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00(2)
_cell_angle_beta                 102.97(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   7.648(2)
_cell_length_b                   10.888(3)
_cell_length_c                   12.640(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      11
_cell_volume                     1025.7(5)
_computing_cell_refinement       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'XCAD4VAX (Sheldrick, 1993)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5983
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        <4.0%
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.259
_exptl_absorpt_correction_T_max  .546
_exptl_absorpt_correction_T_min  .221
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). ActaCryst. A24,
351-359
;
_exptl_crystal_colour            gold-brown
_exptl_crystal_density_diffrn    2.448
_exptl_crystal_description       pentagonal
_exptl_crystal_F_000             696
_exptl_crystal_size_max          .66
_exptl_crystal_size_mid          .47
_exptl_crystal_size_min          .30
_refine_diff_density_max         2.518
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.0034(4)
_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_all   0.988
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_hydrogen_treatment    'refine xyz with common isotropic U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_obs          0.0340
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0899
_refine_ls_wR_factor_obs         0.0744
_reflns_number_observed          1949
_reflns_number_total             2996
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om990778x.cif
_cod_data_source_block           wcohcpac
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4077679