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_4077678
_publ_section_title
;
 Water-Soluble Tungsten Hydrides:&#x00A0; Synthesis, Structures, and
 Reactions of (C5H4CO2H)(CO)3WH and Related Complexes
;
_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        CH2Cl2/ET2O
_chemical_formula_moiety         '(C16 H36 N 1+), (C9 H5 O5 W 1-) '
_chemical_formula_structural     '[N (C4H9)4] [W (C5 H4 C O2 H) (C O)3)]'
_chemical_formula_sum            'C25 H41 N O5 W'
_chemical_formula_weight         619.44
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                99.18(2)
_cell_angle_beta                 105.12(2)
_cell_angle_gamma                102.030(10)
_cell_formula_units_Z            2
_cell_length_a                   9.775(2)
_cell_length_b                   11.127(2)
_cell_length_c                   13.440(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      15
_cell_volume                     1344.3(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    'SHELX-76 (Sheldrick, 1976)'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7815
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        '15% decay corrected'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.329
_exptl_absorpt_correction_T_max  .673
_exptl_absorpt_correction_T_min  .534
_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            yellow-brown
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_exptl_crystal_size_max          .66
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_refine_ls_hydrogen_treatment    'xyz refined on anion with a common U'
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_refine_ls_number_reflns         7813
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_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_obs          0.0361
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_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.4428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0915
_refine_ls_wR_factor_obs         0.0797
_reflns_number_observed          5472
_reflns_number_total             7815
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om990778x.cif
_cod_data_source_block           wcocpacc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.4428P] 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^)+(0.0451P)^2^+0.4428P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1344.3(4)
_cod_original_sg_symbol_H-M      P_-1
_cod_database_code               4077678