[Ru(η(5)-C5H5)(η(6)-C10H8)]PF6 as a catalyst precursor for the one-pot direct C-H alkenylation of nitrogen heterocycles.
Lynam, Jason M.; Milner, Lucy M.; Mistry, Neetisha S.; Slattery, John M.; Warrington, Sally R.; Whitwood, Adrian C.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 4565–4572; doi:10.1039/c3dt52984c

data_7028981
_publ_section_title
;
 [Ru(\h(5)-C5H5)(\h(6)-C10H8)]PF6 as a catalyst precursor for the one-pot
 direct C-H alkenylation of nitrogen heterocycles.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4565
_journal_page_last               4572
_journal_paper_doi               10.1039/c3dt52984c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         '6(C21 H34 N2 P Ru), 2(C5 H12 P0.5), 7(F6 P)'
_chemical_formula_sum            'C136 H228 F42 N12 P14 Ru6'
_chemical_formula_weight         3869.36
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-P 3*'
_space_group_name_H-M_alt        'R -3: R'
_atom_sites_solution_primary     direct
_audit_creation_date             2013-01-22
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                105.795
_cell_angle_beta                 105.795
_cell_angle_gamma                105.795
_cell_formula_units_Z            1
_cell_length_a                   16.9556(10)
_cell_length_b                   16.9556(10)
_cell_length_c                   16.9556(10)
_cell_measurement_reflns_used    4648
_cell_measurement_temperature    163.0
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.52
_cell_volume                     4185.9(4)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      163.0
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43426
_diffrn_reflns_theta_full        28.2868
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.51
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.754930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0878 before and 0.0427 after correction.
The Ratio of minimum to maximum transmission is 0.7549.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.5349
_exptl_crystal_description       needle
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.3813
_refine_diff_density_min         -1.4734
_refine_diff_density_rms         0.1706
_refine_ls_d_res_high            0.7499
_refine_ls_d_res_low             13.5231
_refine_ls_goodness_of_fit_ref   1.0410
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6932
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0408
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+5.8614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -22
_reflns_limit_k_max              22
_reflns_limit_k_min              -8
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                5073
_reflns_number_total             6932
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c3dt52984c.txt
_cod_data_source_block           Complex[10iPr]PF6[MePiPr3]PF6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_source_target' value 'MO' changed to 'Mo' according to
/usr/data/users/saulius/automatic-downloads/current/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_database_code               7028981
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H3 of C3, H9 of C9, H8 of C8, H7 of C7, H4 of C4, H10 of C10, H2 of C2, H16
  of C16, H19 of C19, H6 of C6, H1 of C1, H13 of C13, H5 of C5, H22 of C22
 At 1.5 times of:
  {H14a,H14b,H14c} of C14, {H18a,H18b,H18c} of C18, {H17a,H17b,H17c} of C17,
  {H15a,H15b,H15c} of C15, {H12a,H12b,H12c} of C12, {H20a,H20b,H20c} of C20,
  {H21a,H21b,H21c} of C21, {H25a,H25b,H25c} of C25, {H23a,H23b,H23c} of C23,
  {H24a,H24b,H24c} of C24
2. Restrained distances
 C24-C22 = C22-C23
 1.53 with sigma of 0.01
 C22-P4
 1.8 with sigma of 0.005
3. Others
 Fixed Sof: P4(0.166667) C22(0.5) H22(0.5) C23(0.5) H23a(0.5) H23b(0.5)
 H23c(0.5) C24(0.5) H24a(0.5) H24b(0.5) H24c(0.5) C25(0.166667) H25a(0.16667)
 H25b(0.16667) H25c(0.16667)
 Fixed Uiso: C22(0.1) C23(0.1) C24(0.1) C25(0.1)
4.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C1(H1), C13(H13), C2(H2), C3(H3), C4(H4), C5(H5), C22(H22)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C9(H9), C8(H8), C7(H7)
4.c Idealised Me refined with everything fixed:
 C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c)
4.d Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C12(H12a,H12b,H12c), C20(H20a,H20b,H20c), C14(H14a,H14b,
 H14c), C18(H18a,H18b,H18c), C17(H17a,H17b,H17c), C15(H15a,H15b,H15c)
;