#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:28:44 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180264 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/50/7115066.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7115066
loop_
_publ_author_name
'Kirkham, Matthew S.'
'Mahon, Mary F.'
'Whittlesey, Michael K.'
_publ_section_title
;
 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]−
;
_journal_issue                   9
_journal_name_full               'Chemical Communications'
_journal_page_first              813
_journal_paper_doi               10.1039/b009862k
_journal_year                    2001
_chemical_formula_sum            'C12 H33 F3 P4 Ru'
_chemical_formula_weight         459.33
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 106.061(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0705(11)
_cell_length_b                   17.621(2)
_cell_length_c                   12.7949(15)
_cell_measurement_temperature    133(2)
_cell_volume                     1965.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5399
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  0.9195
_exptl_absorpt_correction_T_min  0.8947
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         4105
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0452P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                3938
_reflns_number_total             4105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009862k.txt
_cod_data_source_block           sam
_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 'Monoclinic' changed to 'monoclinic'
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      Cc
_cod_database_code               7115066
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ru1 Ru 0.89812(3) 0.415926(15) -0.04838(2) 0.01986(8) Uani 1 1 d .
P1 P 1.03437(13) 0.31431(7) -0.09001(10) 0.0322(3) Uani 1 1 d .
P2 P 0.85285(13) 0.33732(6) 0.07785(10) 0.0288(2) Uani 1 1 d .
P3 P 1.10290(11) 0.47976(6) 0.05028(9) 0.0233(2) Uani 1 1 d .
P4 P 0.76081(11) 0.52085(6) -0.01542(9) 0.0230(2) Uani 1 1 d .
F1 F 0.6972(3) 0.36594(16) -0.1601(2) 0.0402(7) Uani 1 1 d .
F2 F 0.9161(3) 0.48004(14) -0.1828(2) 0.0328(6) Uani 1 1 d .
F3 F 0.4453(4) 0.3912(2) -0.2477(4) 0.0634(10) Uani 1 1 d .
H3 H 0.549(13) 0.370(6) -0.198(8) 0.14(4) Uiso 1 1 d .
C1 C 1.0548(8) 0.2430(3) 0.0154(4) 0.0526(15) Uani 1 1 d .
H1A H 1.0748 0.1927 -0.0126 0.063 Uiso 1 1 calc R
H1B H 1.1422 0.2559 0.0786 0.063 Uiso 1 1 calc R
C2 C 0.9075(8) 0.2405(3) 0.0494(5) 0.0520(15) Uani 1 1 d .
H2A H 0.9224 0.2087 0.1153 0.062 Uiso 1 1 calc R
H2B H 0.8246 0.2176 -0.0094 0.062 Uiso 1 1 calc R
C3 C 0.9353(7) 0.2670(3) -0.2160(4) 0.0449(13) Uani 1 1 d .
H3A H 0.9877 0.2193 -0.2222 0.067 Uiso 1 1 calc R
H3B H 0.9356 0.2999 -0.2778 0.067 Uiso 1 1 calc R
H3C H 0.8292 0.2564 -0.2162 0.067 Uiso 1 1 calc R
C4 C 1.2297(6) 0.3191(4) -0.1018(6) 0.0618(18) Uani 1 1 d .
H4A H 1.2992 0.3350 -0.0321 0.093 Uiso 1 1 calc R
H4B H 1.2344 0.3558 -0.1583 0.093 Uiso 1 1 calc R
H4C H 1.2607 0.2689 -0.1213 0.093 Uiso 1 1 calc R
C5 C 0.6507(7) 0.3218(4) 0.0712(6) 0.0594(17) Uani 1 1 d .
H5A H 0.6420 0.2782 0.1166 0.089 Uiso 1 1 calc R
H5B H 0.5924 0.3119 -0.0042 0.089 Uiso 1 1 calc R
H5C H 0.6097 0.3671 0.0977 0.089 Uiso 1 1 calc R
C6 C 0.9396(6) 0.3461(3) 0.2234(4) 0.0393(11) Uani 1 1 d .
H6A H 0.9247 0.3978 0.2466 0.059 Uiso 1 1 calc R
H6B H 1.0496 0.3352 0.2401 0.059 Uiso 1 1 calc R
H6C H 0.8913 0.3099 0.2619 0.059 Uiso 1 1 calc R
C7 C 1.0420(5) 0.5659(2) 0.1091(4) 0.0301(9) Uani 1 1 d .
H7A H 1.0162 0.5532 0.1773 0.036 Uiso 1 1 calc R
H7B H 1.1258 0.6038 0.1258 0.036 Uiso 1 1 calc R
C8 C 0.9004(5) 0.5982(2) 0.0252(4) 0.0297(9) Uani 1 1 d .
H8A H 0.9294 0.6178 -0.0389 0.036 Uiso 1 1 calc R
H8B H 0.8557 0.6404 0.0575 0.036 Uiso 1 1 calc R
C9 C 1.2521(5) 0.4417(3) 0.1639(4) 0.0365(11) Uani 1 1 d .
H9A H 1.2964 0.3963 0.1404 0.055 Uiso 1 1 calc R
H9B H 1.2078 0.4284 0.2232 0.055 Uiso 1 1 calc R
H9C H 1.3324 0.4800 0.1894 0.055 Uiso 1 1 calc R
C10 C 1.2173(5) 0.5200(3) -0.0326(4) 0.0381(11) Uani 1 1 d .
H10A H 1.2908 0.5564 0.0108 0.057 Uiso 1 1 calc R
H10B H 1.1498 0.5458 -0.0956 0.057 Uiso 1 1 calc R
H10C H 1.2730 0.4793 -0.0576 0.057 Uiso 1 1 calc R
C11 C 0.6599(5) 0.5248(3) 0.0887(4) 0.0336(10) Uani 1 1 d .
H11A H 0.6112 0.5746 0.0869 0.050 Uiso 1 1 calc R
H11B H 0.7328 0.5168 0.1603 0.050 Uiso 1 1 calc R
H11C H 0.5812 0.4851 0.0751 0.050 Uiso 1 1 calc R
C12 C 0.6182(6) 0.5539(3) -0.1373(4) 0.0372(11) Uani 1 1 d .
H12A H 0.5339 0.5172 -0.1577 0.056 Uiso 1 1 calc R
H12B H 0.6660 0.5590 -0.1969 0.056 Uiso 1 1 calc R
H12C H 0.5782 0.6033 -0.1227 0.056 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
F2 Ru1 F1 85.44(11)
F2 Ru1 P3 87.19(8)
F1 Ru1 P3 172.33(9)
F2 Ru1 P2 171.63(8)
F1 Ru1 P2 86.33(9)
P3 Ru1 P2 101.09(4)
F2 Ru1 P1 93.45(8)
F1 Ru1 P1 86.51(8)
P3 Ru1 P1 96.07(4)
P2 Ru1 P1 84.51(5)
F2 Ru1 P4 83.57(8)
F1 Ru1 P4 92.74(8)
P3 Ru1 P4 84.32(4)
P2 Ru1 P4 98.37(4)
P1 Ru1 P4 176.98(5)
C1 P1 C3 105.4(3)
C1 P1 C4 101.0(3)
C3 P1 C4 101.6(3)
C1 P1 Ru1 108.38(18)
C3 P1 Ru1 113.20(17)
C4 P1 Ru1 125.2(2)
C6 P2 C5 101.8(3)
C6 P2 C2 102.5(3)
C5 P2 C2 100.0(3)
C6 P2 Ru1 124.76(17)
C5 P2 Ru1 115.9(2)
C2 P2 Ru1 108.43(19)
C9 P3 C10 101.0(2)
C9 P3 C7 102.6(2)
C10 P3 C7 101.6(2)
C9 P3 Ru1 125.71(17)
C10 P3 Ru1 112.64(16)
C7 P3 Ru1 110.35(14)
C11 P4 C12 103.5(2)
C11 P4 C8 102.3(2)
C12 P4 C8 106.0(2)
C11 P4 Ru1 124.51(15)
C12 P4 Ru1 112.73(15)
C8 P4 Ru1 106.20(14)
C2 C1 P1 108.5(4)
C1 C2 P2 109.7(4)
C8 C7 P3 107.8(3)
C7 C8 P4 107.5(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru1 F2 2.101(3)
Ru1 F1 2.168(3)
Ru1 P3 2.2386(10)
Ru1 P2 2.2499(12)
Ru1 P1 2.3199(11)
Ru1 P4 2.3319(10)
P1 C1 1.815(5)
P1 C3 1.817(5)
P1 C4 1.821(6)
P2 C6 1.817(5)
P2 C5 1.832(6)
P2 C2 1.841(5)
P3 C9 1.818(4)
P3 C10 1.820(5)
P3 C7 1.845(4)
P4 C11 1.814(5)
P4 C12 1.824(4)
P4 C8 1.835(4)
C1 C2 1.516(9)
C7 C8 1.537(6)
