Reactions of trifluoromethyl-phosphine and -arsine with a ruthenium carbonyl cluster: synthesis, characterization and reactivity of cluster derivatives capped by trifluoromethyl-phosphinidene and -arsinidene moieties
Ang, How Ghee; Ang, Siau Gek; Du, Shaowu; Sow, Boon Hwa; Wu, Xintao; Journal of the Chemical Society, Dalton Transactions  (1999) 2799–; doi:10.1039/a902598g

data_7027433
_publ_contact_author
;
Ang How Ghee
Department of Chemistry, National University of Singapore, Kent Ridge,
Singapore 119260
;
_publ_section_title
;
 Reactions of trifluoromethyl-phosphine and -arsine with a ruthenium
 carbonyl cluster: synthesis, characterization and reactivity of cluster
 derivatives capped by trifluoromethyl-phosphinidene and -arsinidene
 moieties
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2799
_journal_paper_doi               10.1039/a902598g
_journal_year                    1999
_chemical_formula_sum            'C14 H2 As F3 O13 Ru4'
_chemical_formula_weight         914.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.3431(2)
_cell_length_b                   15.46710(10)
_cell_length_c                   18.0049(2)
_cell_measurement_temperature    293(2)
_cell_volume                     4829.77(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
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_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    3.896
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.515
_exptl_crystal_description       'Rectangular block'
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_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00098(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_goodness_of_fit_obs   1.130
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6243
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.130
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_refine_ls_R_factor_obs          0.0252
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0094P)^2^+5.2140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0498
_refine_ls_wR_factor_obs         0.0448
_reflns_number_observed          5124
_reflns_number_total             6243
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902598gsup1.cif
_cod_data_source_block           Cpd7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0094P)^2^+5.2140P] 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^)+(0.0094P)^2^+5.2140P] 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      Pbca
_cod_database_code               7027433