#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:27:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179378 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/75/4327573.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4327573
loop_
_publ_author_name
'Joel T. Mague'
'Jamin L. Krinsky'
_publ_section_title
;
 Synthetic and Structural Studies of the Coordination Behavior of
 2-Pyridylbis(diphenylphosphino)methane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1962
_journal_page_last               1971
_journal_paper_doi               10.1021/ic001266+
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '(C O)3 (((C6 H5)2 P)2 C H (C5 H4 N)) Fe'
_chemical_formula_sum            'C33 H25 Fe N O3 P2'
_chemical_formula_weight         601.33
_chemical_name_systematic
; 
 Tricarbonyl(2-pyridylbis(diphenylphosphino)methane)iron(0)
;
_space_group_IT_number           1
_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                114.054(14)
_cell_angle_beta                 93.112(11)
_cell_angle_gamma                104.440(14)
_cell_formula_units_Z            1
_cell_length_a                   9.2281(12)
_cell_length_b                   9.3040(19)
_cell_length_c                   9.4420(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.91
_cell_measurement_theta_min      15.22
_cell_volume                     705.7(2)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1987)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1997)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'θ/2θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2668
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.8565
_exptl_absorpt_correction_T_min  0.6958
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ψ scans (North, et al., 1968)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       Plate
_exptl_crystal_F_000             310
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         2668
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0310
_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/[σ²(Fo²)+(0.0528P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                2351
_reflns_number_total             2668
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0012662B_07.cif
_cod_data_source_block           7
_cod_database_code               4327573
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe Fe 0.74567(5) 0.55624(5) 0.13983(5) 0.02773(17) Uani 1 1 d .
P1 P 0.49733(12) 0.50525(12) 0.13973(11) 0.0262(2) Uani 1 1 d .
P2 P 0.64270(12) 0.54472(12) -0.08260(11) 0.0253(2) Uani 1 1 d .
O1 O 0.8011(7) 0.4105(9) 0.3500(8) 0.107(2) Uani 1 1 d .
O2 O 0.9992(5) 0.4588(8) 0.0013(5) 0.0905(18) Uani 1 1 d .
O3 O 0.8762(6) 0.9081(5) 0.3357(6) 0.0805(15) Uani 1 1 d .
N N 0.2575(5) 0.5760(5) -0.1853(5) 0.0433(10) Uani 1 1 d .
C1 C 0.7762(7) 0.4673(9) 0.2676(7) 0.0592(17) Uani 1 1 d .
C2 C 0.8980(6) 0.4968(8) 0.0547(6) 0.0496(14) Uani 1 1 d .
C3 C 0.8201(6) 0.7715(7) 0.2587(6) 0.0458(12) Uani 1 1 d .
C4 C 0.4234(5) 0.6380(5) 0.3013(5) 0.0300(9) Uani 1 1 d .
C5 C 0.4843(6) 0.6758(5) 0.4539(5) 0.0373(10) Uani 1 1 d .
H5 H 0.5649 0.6388 0.4722 0.041 Uiso 1 1 calc R
C6 C 0.4250(7) 0.7686(7) 0.5790(6) 0.0521(14) Uani 1 1 d .
H6 H 0.4662 0.7942 0.6816 0.057 Uiso 1 1 calc R
C7 C 0.3059(7) 0.8228(7) 0.5523(7) 0.0561(15) Uani 1 1 d .
H7 H 0.2657 0.8839 0.6368 0.062 Uiso 1 1 calc R
C8 C 0.2461(7) 0.7880(8) 0.4034(7) 0.0570(15) Uani 1 1 d .
H8 H 0.1657 0.8261 0.3869 0.063 Uiso 1 1 calc R
C9 C 0.3037(6) 0.6961(7) 0.2753(6) 0.0437(12) Uani 1 1 d .
H9 H 0.2630 0.6735 0.1735 0.048 Uiso 1 1 calc R
C10 C 0.3786(5) 0.2999(5) 0.1034(5) 0.0326(9) Uani 1 1 d .
C11 C 0.2429(6) 0.2746(6) 0.1587(6) 0.0442(12) Uani 1 1 d .
H11 H 0.2066 0.3635 0.2115 0.049 Uiso 1 1 calc R
C12 C 0.1612(6) 0.1190(7) 0.1361(8) 0.0573(15) Uani 1 1 d .
H12 H 0.0706 0.1035 0.1743 0.063 Uiso 1 1 calc R
C13 C 0.2133(7) -0.0137(7) 0.0571(7) 0.0569(15) Uani 1 1 d .
H13 H 0.1579 -0.1188 0.0416 0.063 Uiso 1 1 calc R
C14 C 0.3472(7) 0.0098(6) 0.0015(6) 0.0519(14) Uani 1 1 d .
H14 H 0.3816 -0.0800 -0.0534 0.057 Uiso 1 1 calc R
C15 C 0.4312(6) 0.1658(6) 0.0264(5) 0.0401(11) Uani 1 1 d .
H15 H 0.5236 0.1810 -0.0087 0.044 Uiso 1 1 calc R
C16 C 0.6100(5) 0.3675(5) -0.2724(5) 0.0304(9) Uani 1 1 d .
C17 C 0.6718(6) 0.2421(5) -0.2887(5) 0.0365(10) Uani 1 1 d .
H17 H 0.7252 0.2447 -0.2008 0.040 Uiso 1 1 calc R
C18 C 0.6548(7) 0.1127(6) -0.4350(6) 0.0501(13) Uani 1 1 d .
H18 H 0.6993 0.0301 -0.4463 0.055 Uiso 1 1 calc R
C19 C 0.5727(7) 0.1067(7) -0.5623(6) 0.0516(14) Uani 1 1 d .
H19 H 0.5608 0.0190 -0.6605 0.057 Uiso 1 1 calc R
C20 C 0.5070(6) 0.2274(7) -0.5484(6) 0.0488(13) Uani 1 1 d .
H20 H 0.4493 0.2203 -0.6362 0.054 Uiso 1 1 calc R
C21 C 0.5268(6) 0.3590(6) -0.4045(5) 0.0379(10) Uani 1 1 d .
H21 H 0.4846 0.4427 -0.3953 0.042 Uiso 1 1 calc R
C22 C 0.7213(5) 0.7192(5) -0.1277(5) 0.0321(9) Uani 1 1 d .
C23 C 0.7145(6) 0.8749(6) -0.0293(6) 0.0404(11) Uani 1 1 d .
H23 H 0.6618 0.8888 0.0542 0.044 Uiso 1 1 calc R
C24 C 0.7851(7) 1.0092(7) -0.0543(8) 0.0548(14) Uani 1 1 d .
H24 H 0.7790 1.1129 0.0121 0.060 Uiso 1 1 calc R
C25 C 0.8643(6) 0.9919(7) -0.1758(8) 0.0553(15) Uani 1 1 d .
H25 H 0.9124 1.0833 -0.1916 0.061 Uiso 1 1 calc R
C26 C 0.8721(6) 0.8393(8) -0.2734(7) 0.0544(14) Uani 1 1 d .
H26 H 0.9262 0.8278 -0.3557 0.060 Uiso 1 1 calc R
C27 C 0.8011(6) 0.7010(7) -0.2525(6) 0.0425(11) Uani 1 1 d .
H27 H 0.8065 0.5976 -0.3207 0.047 Uiso 1 1 calc R
C28 C 0.4539(5) 0.5542(5) -0.0275(5) 0.0242(9) Uani 1 1 d .
H28 H 0.4613 0.6717 0.0209 0.027 Uiso 1 1 calc R
C29 C 0.3115(5) 0.4717(5) -0.1513(4) 0.0272(9) Uani 1 1 d .
C30 C 0.2483(6) 0.3018(6) -0.2317(5) 0.0375(11) Uani 1 1 d .
H30 H 0.2885 0.2318 -0.2054 0.041 Uiso 1 1 calc R
C31 C 0.1250(6) 0.2389(7) -0.3512(6) 0.0512(14) Uani 1 1 d .
H31 H 0.0799 0.1257 -0.4064 0.056 Uiso 1 1 calc R
C32 C 0.0698(6) 0.3462(8) -0.3873(7) 0.0592(16) Uani 1 1 d .
H32 H -0.0129 0.3072 -0.4677 0.065 Uiso 1 1 calc R
C33 C 0.1380(7) 0.5092(8) -0.3039(7) 0.0587(15) Uani 1 1 d .
H33 H 0.1000 0.5806 -0.3300 0.065 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C2 Fe C1 87.5(3) y
C2 Fe C3 104.9(3) y
C1 Fe C3 104.4(3) y
C2 Fe P2 91.06(18) y
C1 Fe P2 152.7(2) y
C3 Fe P2 102.26(18) y
C2 Fe P1 149.7(2) y
C1 Fe P1 94.5(2) y
C3 Fe P1 103.83(17) y
P2 Fe P1 73.55(4) y
C4 P1 C10 101.8(2) ?
C4 P1 C28 105.14(19) ?
C10 P1 C28 111.03(19) ?
C4 P1 Fe 121.05(15) ?
C10 P1 Fe 120.89(15) ?
C28 P1 Fe 95.76(14) ?
C4 P1 P2 134.36(14) ?
C10 P1 P2 119.59(14) ?
C28 P1 P2 44.48(14) ?
Fe P1 P2 52.99(3) ?
C16 P2 C22 103.0(2) ?
C16 P2 C28 107.4(2) ?
C22 P2 C28 107.83(19) ?
C16 P2 Fe 123.44(15) ?
C22 P2 Fe 117.51(14) ?
C28 P2 Fe 96.37(13) ?
C16 P2 P1 118.30(14) ?
C22 P2 P1 134.79(15) ?
C28 P2 P1 44.64(13) ?
Fe P2 P1 53.46(3) ?
C29 N C33 116.8(5) ?
O1 C1 Fe 177.7(6) ?
O2 C2 Fe 178.9(5) ?
O3 C3 Fe 175.8(5) ?
C5 C4 C9 119.5(4) ?
C5 C4 P1 118.4(3) ?
C9 C4 P1 122.0(3) ?
C4 C5 C6 120.0(5) ?
C7 C6 C5 120.1(5) ?
C8 C7 C6 120.5(5) ?
C7 C8 C9 120.8(5) ?
C8 C9 C4 119.1(5) ?
C11 C10 C15 118.7(4) ?
C11 C10 P1 122.5(4) ?
C15 C10 P1 118.6(4) ?
C12 C11 C10 120.6(5) ?
C13 C12 C11 120.2(5) ?
C14 C13 C12 119.7(5) ?
C13 C14 C15 120.4(5) ?
C14 C15 C10 120.3(5) ?
C17 C16 C21 119.0(4) ?
C17 C16 P2 120.5(3) ?
C21 C16 P2 120.5(3) ?
C16 C17 C18 120.3(5) ?
C19 C18 C17 119.6(5) ?
C18 C19 C20 121.2(5) ?
C19 C20 C21 119.7(5) ?
C20 C21 C16 120.1(5) ?
C23 C22 C27 118.9(4) ?
C23 C22 P2 120.1(3) ?
C27 C22 P2 120.7(3) ?
C24 C23 C22 120.5(5) ?
C25 C24 C23 120.7(5) ?
C26 C25 C24 119.4(5) ?
C25 C26 C27 121.4(5) ?
C26 C27 C22 119.1(5) ?
C29 C28 P2 120.9(3) ?
C29 C28 P1 126.7(3) ?
P2 C28 P1 90.89(19) ?
N C29 C30 122.5(4) ?
N C29 C28 113.9(4) ?
C30 C29 C28 123.4(4) ?
C31 C30 C29 118.7(5) ?
C32 C31 C30 118.9(5) ?
C33 C32 C31 118.6(5) ?
N C33 C32 124.5(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Fe C2 1.754(5) y
Fe C1 1.764(6) y
Fe C3 1.772(5) y
Fe P2 2.2077(11) y
Fe P1 2.2212(12) y
P1 C4 1.821(4) ?
P1 C10 1.830(4) ?
P1 C28 1.863(4) ?
P1 P2 2.6513(14) ?
P2 C16 1.818(4) ?
P2 C22 1.831(4) ?
P2 C28 1.858(4) ?
O1 C1 1.146(7) ?
O2 C2 1.150(7) ?
O3 C3 1.135(6) ?
N C29 1.331(6) ?
N C33 1.346(7) ?
C4 C5 1.384(6) ?
C4 C9 1.397(7) ?
C5 C6 1.384(7) ?
C6 C7 1.370(8) ?
C7 C8 1.357(9) ?
C8 C9 1.389(7) ?
C10 C11 1.385(7) ?
C10 C15 1.387(6) ?
C11 C12 1.377(7) ?
C12 C13 1.376(8) ?
C13 C14 1.371(9) ?
C14 C15 1.380(7) ?
C16 C17 1.381(6) ?
C16 C21 1.392(6) ?
C17 C18 1.381(6) ?
C18 C19 1.359(8) ?
C19 C20 1.369(8) ?
C20 C21 1.373(7) ?
C22 C23 1.386(6) ?
C22 C27 1.398(7) ?
C23 C24 1.375(7) ?
C24 C25 1.369(9) ?
C25 C26 1.364(9) ?
C26 C27 1.387(7) ?
C28 C29 1.510(6) ?
C29 C30 1.388(6) ?
C30 C31 1.379(7) ?
C31 C32 1.373(9) ?
C32 C33 1.346(9) ?
