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_7027616
_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         C33H24O7P2Ru3Se2
_chemical_formula_sum            'C33 H24 O7 P2 Ru3 Se2'
_chemical_formula_weight         1055.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.31(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.550(5)
_cell_length_b                   10.891(4)
_cell_length_c                   24.876(6)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.76
_cell_measurement_theta_min      11.13
_cell_volume                     3587(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Philips PW 1100'
_diffrn_measurement_method       '\q/2\q 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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.1637
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8840
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    3.411
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9026
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.419
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       0.0002(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.2953
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.250
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+4.6451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.2664
_reflns_number_gt                3277
_reflns_number_total             8658
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904866isup1.cif
_cod_data_source_block           gra5h
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+4.6451P] 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^)+(0.0947P)^2^+4.6451P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7027616