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_4335186
_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         'C18 H18 Cl2 N4 Ru, 3(C H2 Cl2)'
_chemical_formula_sum            'C21 H24 Cl8 N4 Ru'
_chemical_formula_weight         717.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.5352(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.54332(10)
_cell_length_b                   24.0817(3)
_cell_length_c                   13.86264(17)
_cell_measurement_reflns_used    19760
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.7726
_cell_measurement_theta_min      2.7947
_cell_volume                     2833.53(6)
_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
_diffrn_detector_area_resol_mean 15.9863
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34942
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         32.85
_diffrn_reflns_theta_min         2.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.734
_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            Red
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       plates
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.780
_refine_diff_density_min         -1.505
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         9620
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0359
_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/[\s^2^(Fo^2^)+(0.0193P)^2^+3.7898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                7886
_reflns_number_total             9620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4005196_si_002_5.cif
_cod_data_source_block           '[RuCl2(TPA)]'
_cod_original_cell_volume        2833.54(6)
_cod_database_code               4335186