Tri(pyridylmethyl)phosphine: The Elusive Congener of TPA Shows Surprisingly Different Coordination Behavior
Christopher J. Whiteoak; James D. Nobbs; Evgeny Kiryushchenkov; Sandro Pagano; Andrew J.P. White; George J.P. Britovsek; Inorganic Chemistry 52 (2013) 7000–7009; doi:10.1021/ic4005196

data_4335188
_publ_section_title
;
 Tri(pyridylmethyl)phosphine: The Elusive Congener of TPA Shows
 Surprisingly Different Coordination Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7000
_journal_page_last               7009
_journal_paper_doi               10.1021/ic4005196
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'C24 H27 N6 P Ru, 2(F6 Sb), 0.5(C4 H10 O), 0.5(C2 H3 N)'
_chemical_formula_sum            'C27 H33.5 F12 N6.5 O0.5 P Ru Sb2'
_chemical_formula_weight         1060.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.078(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.7301(3)
_cell_length_b                   37.0357(11)
_cell_length_c                   20.8357(10)
_cell_measurement_reflns_used    16256
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.3118
_cell_measurement_theta_min      2.1562
_cell_volume                     8125.8(5)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45251
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         72.46
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.579
_exptl_absorpt_correction_T_max  0.414
_exptl_absorpt_correction_T_min  0.079
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) 
(compiled Feb 27 2009,15:38:38) 
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            Colourless
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       tablets
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.652
_refine_diff_density_min         -2.345
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.00023(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   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1032
_refine_ls_number_reflns         15859
_refine_ls_number_restraints     1393
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+17.6486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2200
_refine_ls_wR_factor_ref         0.2349
_reflns_number_gt                11889
_reflns_number_total             15859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4005196_si_002_7.cif
_cod_data_source_block           '[Ru(MeCN)3(TPP)](SbF6)2'
_cod_original_formula_sum        'C27 H33.50 F12 N6.50 O0.50 P Ru Sb2'
_cod_database_code               4335188