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_7009495
_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 O9 P2 W3'
_chemical_formula_weight         995.76
_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                 106.510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.255(3)
_cell_length_b                   8.095(4)
_cell_length_c                   31.957(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     4776(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       AFC5R
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            4356
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        1%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    14.597
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   'empirical (10 psi scans) '
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.770
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.192
_refine_diff_density_min         -1.417
_refine_diff_density_rms         0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.141
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_obs          0.0444
_refine_ls_shift/esd_max         0.185
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2240
_refine_ls_wR_factor_obs         0.0891
_reflns_number_observed          2666
_reflns_number_total             4223
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001409p.txt
_cod_data_source_block           17
_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 2.4.1 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^)+(0.0319P)^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^)+(0.0319P)^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 
;
_cod_original_cell_volume        4775.7(25)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009495