Rapid Inversion at Phosphorus in the [η4-(C6H11)3SnP7W(CO)3]2- and [(en)(CO)3W(η1,η4-P7)M(CO)3]3- Ions Where M = Cr, W
Scott Charles; Janet A. Danis; James C. Fettinger; Bryan W. Eichhorn; Inorganic Chemistry 36 (1997) 3772–3778; doi:10.1021/ic961177q

data_4323517
_publ_section_title
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 Rapid Inversion at Phosphorus in the [\h4-(C6H11)3SnP7W(CO)3]2- and
 [(en)(CO)3W(\h1,\h4-P7)M(CO)3]3- Ions Where M = Cr, W
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3772
_journal_page_last               3778
_journal_paper_doi               10.1021/ic961177q
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C57 H105 K2 N4 O15 P7 Sn W'
_chemical_formula_weight         1683.98
_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                97.374(10)
_cell_angle_beta                 93.273(13)
_cell_angle_gamma                111.217(9)
_cell_formula_units_Z            2
_cell_length_a                   12.247(2)
_cell_length_b                   15.1909(14)
_cell_length_c                   21.292(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      19.04
_cell_measurement_theta_min      17.54
_cell_volume                     3639.1(9)
_computing_cell_refinement       'Enraf-Nonius EXPRESS'
_computing_data_collection       'Enraf-Nonius EXPRESS'
_computing_data_reduction        'Harms, XCAD4; 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      153(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega:2theta 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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0918
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9811
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        20
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.251
_exptl_absorpt_correction_T_max  0.9355
_exptl_absorpt_correction_T_min  0.5300
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       plate
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.485
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.140
_refine_ls_goodness_of_fit_obs   1.264
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         9502
_refine_ls_number_restraints     565
_refine_ls_restrained_S_all      1.184
_refine_ls_restrained_S_obs      1.312
_refine_ls_R_factor_all          0.1533
_refine_ls_R_factor_obs          0.1050
_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^)+(0.0483P)^2^+78.8481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2269
_refine_ls_wR_factor_obs         0.2021
_reflns_number_observed          6377
_reflns_number_total             9502
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961177q_2.cif
_cod_data_source_block           '[cy3SnP7W(CO)3][K-crypt]2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+78.8481P] 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^)+(0.0483P)^2^+78.8481P] 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        3639.2(8)
_cod_database_code               4323517