Chelating versus bridging behaviour and NMR fluxionality of dppf in the nido clusters [M3Se2(CO)7(dppf )] [M = Fe or Ru, dppf = Fe(η5-C5H4PPh2)2]. Crystal structure of the chelated ruthenium derivative †
Cauzzi, Daniele; Graiff, Claudia; Massera, Chiara; Predieri, Giovanni; Tiripicchio, Antonio; Acquotti, Domenico; Journal of the Chemical Society, Dalton Transactions  (1999) 3515–; doi:10.1039/a904866i

data_7027615
_publ_section_title
;
 Chelating versus bridging behaviour and NMR fluxionality of dppf in the
 nido clusters [M3Se2(CO)7(dppf&#x200A;)] [M&#x2005;=&#x2005;Fe or Ru,
 dppf&#x2005;=&#x2005;Fe(\h5-C5H4PPh2)2]. Crystal structure of the
 chelated ruthenium derivative&#x200A;&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3515
_journal_paper_doi               10.1039/a904866i
_journal_year                    1999
_chemical_formula_moiety         'C41H28O7P2FeRu3Se2 .CH2Cl2'
_chemical_formula_sum            'C42 H30 Cl2 Fe O7 P2 Ru3 Se2'
_chemical_formula_weight         1296.52
_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                79.77(2)
_cell_angle_beta                 84.24(3)
_cell_angle_gamma                72.31(2)
_cell_formula_units_Z            2
_cell_length_a                   9.201(2)
_cell_length_b                   12.020(3)
_cell_length_c                   21.405(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.84
_cell_measurement_theta_min      11.06
_cell_volume                     2216.8(9)
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Philips PW 1100'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1656
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10683
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    3.206
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8196
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.561
_refine_ls_goodness_of_fit_obs   0.680
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         10679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.619
_refine_ls_restrained_S_obs      0.680
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         0.174
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0944P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1449
_refine_ls_wR_factor_obs         0.1012
_reflns_number_observed          4549
_reflns_number_total             10683
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904866isup1.cif
_cod_data_source_block           g13f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0944P)^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^)+( 0.0944P)^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_database_code               7027615