[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_7028982
_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         'C35 H38 N2 P Ru, F6 P'
_chemical_formula_sum            'C35 H38 F6 N2 P2 Ru'
_chemical_formula_weight         763.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-20
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                89.425(3)
_cell_angle_beta                 88.941(3)
_cell_angle_gamma                85.4958(18)
_cell_formula_units_Z            4
_cell_length_a                   10.1826(2)
_cell_length_b                   15.1616(4)
_cell_length_c                   22.6072(12)
_cell_measurement_reflns_used    7822
_cell_measurement_temperature    109.95(10)
_cell_measurement_theta_max      25.9636
_cell_measurement_theta_min      2.9094
_cell_volume                     3478.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      109.95(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9930
_diffrn_measured_fraction_theta_max 0.9930
_diffrn_measurement_details
;
  1 omega  -87.00   13.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9152  -77.0000  -90.0000 100

  2 omega  -18.00    9.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9152  -99.0000 -180.0000 27

  3 omega  -20.00   55.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1652  -99.0000   60.0000 75

  4 omega  -65.00  -39.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9152 -178.0000 -120.0000 26

  5 omega   -1.00   56.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1652   57.0000  150.0000 57

  6 omega  -51.00   31.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1652  -57.0000 -180.0000 82

  7 omega   44.00   87.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1652   57.0000  -30.0000 43
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0300220000
_diffrn_orient_matrix_UB_12      0.0370309000
_diffrn_orient_matrix_UB_13      -0.0154108000
_diffrn_orient_matrix_UB_21      -0.0559088000
_diffrn_orient_matrix_UB_22      -0.0238028000
_diffrn_orient_matrix_UB_23      -0.0050902000
_diffrn_orient_matrix_UB_31      -0.0292707000
_diffrn_orient_matrix_UB_32      0.0162638000
_diffrn_orient_matrix_UB_33      0.0268589000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25827
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.1528
_exptl_crystal_size_mid          0.0964
_exptl_crystal_size_min          0.0749
_refine_diff_density_max         3.871
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         13625
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+38.3842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.1912
_reflns_number_gt                10463
_reflns_number_total             13625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52984c.txt
_cod_data_source_block           Complex[10iPr*]PF6
_cod_database_code               7028982
_chemical_oxdiff_formula         'C35 H38 F6 N2 P2 Ru'
_chemical_oxdiff_usercomment     'Sally CpstarRuPPh3Py2 PF6'
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F2A-F3A \\sim F3A-F4A \\sim F4A-F5A \\sim F5A-F2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F5A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(F2A) = Uanis(F4A)
Uanis(F3A) = Uanis(F5A)
Uanis(F3) = Uanis(F5)
Uanis(F2) = Uanis(F4)
4. Others
 Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C46(H46), C47(H47),
 C48(H48), C49(H49), C50(H50), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67),
 C68(H68), C69(H69), C70(H70)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C17(H17A,H17B,H17C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C52(H52A,H52B,
 H52C)
;