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_4077680
_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_formula_moiety         '(C13 H18 O2 N3 P1 W)'
_chemical_formula_sum            'C13 H18 N3 O2 P W'
_chemical_formula_weight         463.12
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.76(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.920(3)
_cell_length_b                   6.642(2)
_cell_length_c                   18.845(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.9
_cell_measurement_theta_min      16.4
_cell_volume                     1428.6(7)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf-Noius CAD$'
_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    0.0313
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4143
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        >1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.202
_exptl_absorpt_correction_T_max  1.292
_exptl_absorpt_correction_T_min  .514
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Parkin, S., Moezzi, B., and Hope, H.,  J. Appl. Cryst., 1995, 28, 53-56.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          .47
_exptl_crystal_size_mid          .38
_exptl_crystal_size_min          .20
_refine_diff_density_max         2.436
_refine_diff_density_min         -2.619
_refine_diff_density_rms         0.320
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.329
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.329
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0343P)^2^+46.1207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                3332
_reflns_number_total             4143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990778x.cif
_cod_data_source_block           mxabs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        1428.6(5)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4077680