The preparation of [M2Cp2(CO)4(μ-η2-PE)] (E = As or Sb), the first complexes with naked heterodiatomic Group 15 ligands, and of their adducts with W(CO)5
Davies, John E.; Mays, Martin J.; Raithby, Paul R.; Shields, Gregory P.; Tompkin, Peter K.; Woods, Anthony D.; Journal of the Chemical Society, Dalton Transactions  (2000) 1925–; doi:10.1039/b001409p

data_7009492
_publ_section_title
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 The preparation of [M2Cp2(CO)4(\m-\h2-PE)] (E&#x2005;=&#x2005;As or
 Sb), the first complexes with naked heterodiatomic Group 15 ligands,
 and of their adducts with W(CO)5
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1925
_journal_paper_doi               10.1039/b001409p
_journal_year                    2000
_chemical_formula_sum            'C24 H10 As Mo2 O14 P W2'
_chemical_formula_weight         1187.79
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 110.220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.677(5)
_cell_length_b                   10.799(5)
_cell_length_c                   16.916(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      25
_cell_volume                     3202(2)
_computing_cell_refinement       'Rigaku software'
_computing_data_collection       'Rigaku software'
_computing_data_reduction        TeXsan
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR 92'
_diffrn_ambient_temperature      290(2)
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       'omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Normal focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3014
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.57
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.066
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   psiscans
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.464
_exptl_crystal_description       Block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.999
_refine_ls_goodness_of_fit_obs   1.054
_refine_ls_hydrogen_treatment    'riding atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_restrained_S_obs      1.054
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_obs          0.0409
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0820
_refine_ls_wR_factor_obs         0.0702
_reflns_number_observed          2046
_reflns_number_total             3014
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001409p.txt
_cod_data_source_block           15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0181P)^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^)+(0.0181P)^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 
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_cod_original_cell_volume        3201.6(20)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009492