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_4335184
_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         'C36 H42 Fe N12 P2, 2(C F3 O3 S), C H2 Cl2'
_chemical_formula_sum            'C39 H44 Cl2 F6 Fe N12 O6 P2 S2'
_chemical_formula_weight         1143.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.8540(17)
_cell_angle_beta                 97.9214(18)
_cell_angle_gamma                104.5567(18)
_cell_formula_units_Z            2
_cell_length_a                   13.1348(3)
_cell_length_b                   13.5183(3)
_cell_length_c                   14.2438(3)
_cell_measurement_reflns_used    14339
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.6962
_cell_measurement_theta_min      4.2391
_cell_volume                     2415.17(10)
_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 0.985
_diffrn_measured_fraction_theta_max 0.897
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24564
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         32.77
_diffrn_reflns_theta_min         4.25
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
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            Orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         16039
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0596
_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^)+(0.1174P)^2^+0.4560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1763
_reflns_number_gt                13459
_reflns_number_total             16039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4005196_si_002_3.cif
_cod_data_source_block           '[Fe(TPAMP)2](OTf)2'
_cod_database_code               4335184