C‒F bond activation of perfluoroalkenes by ruthenium phosphine hydride complexes: X-ray crystal structures of cis-Ru(dmpe)2F(F‥HF) and [Ru(dcpe)2H]+[(CF3)2CC(O)CF2CF3]−
Kirkham, Matthew S.; Mahon, Mary F.; Whittlesey, Michael K.; Chemical Communications  (2001) 813–; doi:10.1039/b009862k

data_7115067
_publ_section_title
;
 C--F bond activation of perfluoroalkenes by ruthenium phosphine hydride
 complexes: X-ray crystal structures of cis-Ru(dmpe)2F(F&#x2025;HF) and
 [Ru(dcpe)2H]+[(CF3)2C&#xE006;C(O)CF2CF3]&#x2212;
;
_journal_issue                   9
_journal_name_full               'Chemical Communications'
_journal_page_first              813
_journal_paper_doi               10.1039/b009862k
_journal_year                    2001
_chemical_formula_sum            'C70 H109 F11 O P4 Ru'
_chemical_formula_weight         1400.52
_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-97
_cell_angle_alpha                106.140(2)
_cell_angle_beta                 93.171(2)
_cell_angle_gamma                93.832(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3863(3)
_cell_length_b                   13.6610(4)
_cell_length_c                   21.9070(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     3542.23(17)
_computing_data_reduction
;
Denzo and Scalepack (otwinowski & Minor, 1997
;
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       KappaCCD
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33863
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         23.82
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.9720
_exptl_absorpt_correction_T_min  0.9450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.629
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0099(13)
_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   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         10742
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+5.6715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1613
_reflns_number_gt                8993
_reflns_number_total             10742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009862k.txt
_cod_data_source_block           k00mkw1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'multiscan'
changed to 'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115067