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_7009493
_publ_section_title
;
 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            'C19 H10 Mo2 O9 P Sb W'
_chemical_formula_weight         910.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                97.85(3)
_cell_angle_beta                 96.34(2)
_cell_angle_gamma                118.86(2)
_cell_formula_units_Z            4
_cell_length_a                   15.974(5)
_cell_length_b                   16.236(8)
_cell_length_c                   10.623(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_volume                     2340.4(16)
_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      150(2)
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8554
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        -1.5
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.203
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'v dark'
_exptl_crystal_density_diffrn    2.585
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.907
_refine_diff_density_min         -2.340
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.092
_refine_ls_goodness_of_fit_obs   1.111
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.111
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_obs          0.0350
_refine_ls_shift/esd_max         0.204
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+11.5801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0922
_refine_ls_wR_factor_obs         0.0896
_reflns_number_observed          7556
_reflns_number_total             8232
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001409p.txt
_cod_data_source_block           13
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psiscan' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+11.5801P] 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^)+(0.0465P)^2^+11.5801P] 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        2340.4(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009493