#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:50:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179866 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/62/7016273.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_7016273
loop_
_publ_author_name
'Xu, Xiaofeng'
'Sun, Hongjian'
'Shi, Yujie'
'Jia, Jiong'
'Li, Xiaoyan'
_publ_section_title
;
 Imine-assisted C-F bond activation by electron-rich iron complexes
 supported by trimethylphosphine.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7866
_journal_page_last               7872
_journal_paper_doi               10.1039/c1dt10843c
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C32 H30 F8 Fe N2 P2'
_chemical_formula_sum            'C32 H30 F8 Fe N2 P2'
_chemical_formula_weight         712.37
_chemical_name_systematic
;
?
;
_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                90.243(2)
_cell_angle_beta                 91.242(2)
_cell_angle_gamma                106.088(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6956(14)
_cell_length_b                   9.9219(14)
_cell_length_c                   16.955(2)
_cell_measurement_reflns_used    2234
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.46
_cell_volume                     1566.7(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      273(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8955
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.9679
_exptl_absorpt_correction_T_min  0.8272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_meas      1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0481
_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)+(0.0497P)²+0.5320P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                4079
_reflns_number_total             6679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10843c.txt
_cod_data_source_block           test
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7016273
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.74823(5) 0.76875(5) 0.25718(3) 0.03233(15) Uani 1 1 d . . .
P2 P 0.93573(10) 0.92066(10) 0.32895(5) 0.0383(2) Uani 1 1 d . . .
P3 P 0.84055(11) 0.76350(11) 0.13261(5) 0.0453(3) Uani 1 1 d . . .
F8 F 0.7129(2) 0.5998(2) 0.44067(12) 0.0530(6) Uani 1 1 d . . .
F7 F 0.4345(2) 0.7552(2) 0.14399(13) 0.0626(6) Uani 1 1 d . . .
N2 N 0.8020(3) 0.5902(3) 0.28483(16) 0.0374(7) Uani 1 1 d . . .
N1 N 0.6641(3) 0.9306(3) 0.23641(16) 0.0383(7) Uani 1 1 d . . .
F6 F 0.3743(2) 0.9525(2) 0.41004(14) 0.0646(7) Uani 1 1 d . . .
F5 F 0.5488(3) 0.6325(3) 0.55616(13) 0.0662(7) Uani 1 1 d . . .
F4 F 0.2221(2) 0.5306(3) 0.11110(14) 0.0707(7) Uani 1 1 d . . .
F3 F 0.4519(3) 0.2421(2) 0.24829(15) 0.0693(7) Uani 1 1 d . . .
C32 C 0.5725(4) 0.6259(4) 0.21484(19) 0.0370(8) Uani 1 1 d . . .
F2 F 0.2223(3) 0.2727(2) 0.16147(15) 0.0745(7) Uani 1 1 d . . .
C31 C 0.6397(3) 0.7644(3) 0.35732(19) 0.0359(8) Uani 1 1 d . . .
C30 C 0.9379(4) 0.4797(4) 0.3771(2) 0.0485(9) Uani 1 1 d . . .
H30A H 0.8528 0.4300 0.4000 0.058 Uiso 1 1 calc R . .
F1 F 0.3706(3) 0.7993(3) 0.54337(14) 0.0722(7) Uani 1 1 d . . .
C29 C 0.6306(4) 0.6906(4) 0.4270(2) 0.0389(8) Uani 1 1 d . . .
C28 C 0.9353(4) 0.5714(4) 0.3156(2) 0.0414(9) Uani 1 1 d . . .
C27 C 0.5694(4) 0.9438(4) 0.2877(2) 0.0434(9) Uani 1 1 d . . .
H27A H 0.5170 1.0087 0.2806 0.052 Uiso 1 1 calc R . .
C26 C 0.5459(4) 0.7033(4) 0.4888(2) 0.0454(9) Uani 1 1 d . . .
C25 C 0.9915(4) 0.8588(4) 0.4225(2) 0.0495(10) Uani 1 1 d . . .
H25A H 1.0691 0.9309 0.4459 0.074 Uiso 1 1 calc R . .
H25B H 1.0227 0.7765 0.4132 0.074 Uiso 1 1 calc R . .
H25C H 0.9120 0.8366 0.4575 0.074 Uiso 1 1 calc R . .
C24 C 0.4500(4) 0.6313(4) 0.1722(2) 0.0430(9) Uani 1 1 d . . .
C23 C 0.6985(4) 0.4745(4) 0.2750(2) 0.0439(9) Uani 1 1 d . . .
H23A H 0.7089 0.3882 0.2910 0.053 Uiso 1 1 calc R . .
C22 C 0.3358(4) 0.3845(4) 0.1787(2) 0.0500(10) Uani 1 1 d . . .
C21 C 0.6891(4) 1.0312(4) 0.1734(2) 0.0442(9) Uani 1 1 d . . .
C20 C 0.5497(4) 0.8551(4) 0.3547(2) 0.0384(8) Uani 1 1 d . . .
C19 C 0.8897(5) 1.0762(4) 0.3669(2) 0.0563(11) Uani 1 1 d . . .
H19A H 0.9705 1.1347 0.3959 0.084 Uiso 1 1 calc R . .
H19B H 0.8094 1.0472 0.4011 0.084 Uiso 1 1 calc R . .
H19C H 0.8651 1.1278 0.3236 0.084 Uiso 1 1 calc R . .
C18 C 1.0631(4) 0.6444(4) 0.2823(2) 0.0502(10) Uani 1 1 d . . .
H18A H 1.0621 0.7052 0.2408 0.060 Uiso 1 1 calc R . .
C17 C 0.4575(4) 0.7906(4) 0.4834(2) 0.0465(9) Uani 1 1 d . . .
C16 C 0.4512(4) 0.3712(4) 0.2219(2) 0.0475(9) Uani 1 1 d . . .
C15 C 0.5761(5) 1.0544(4) 0.1288(2) 0.0548(11) Uani 1 1 d . . .
H15A H 0.4818 1.0048 0.1386 0.066 Uiso 1 1 calc R . .
C14 C 0.4594(4) 0.8652(4) 0.4162(2) 0.0469(9) Uani 1 1 d . . .
C13 C 0.3365(4) 0.5160(4) 0.1538(2) 0.0474(9) Uani 1 1 d . . .
C12 C 0.5680(4) 0.4871(4) 0.2384(2) 0.0406(8) Uani 1 1 d . . .
C11 C 1.0682(5) 0.4628(5) 0.4038(3) 0.0639(12) Uani 1 1 d . . .
H11A H 1.0703 0.4017 0.4450 0.077 Uiso 1 1 calc R . .
C10 C 1.1146(4) 1.0070(4) 0.2915(2) 0.0555(10) Uani 1 1 d . . .
H10A H 1.1721 1.0642 0.3326 0.083 Uiso 1 1 calc R . .
H10B H 1.1055 1.0647 0.2475 0.083 Uiso 1 1 calc R . .
H10C H 1.1597 0.9372 0.2750 0.083 Uiso 1 1 calc R . .
C9 C 0.7323(5) 0.7946(5) 0.0479(2) 0.0648(12) Uani 1 1 d . . .
H9A H 0.7818 0.7896 0.0000 0.097 Uiso 1 1 calc R . .
H9B H 0.7172 0.8858 0.0529 0.097 Uiso 1 1 calc R . .
H9C H 0.6412 0.7245 0.0464 0.097 Uiso 1 1 calc R . .
C8 C 0.8285(5) 1.1097(4) 0.1590(2) 0.0525(10) Uani 1 1 d . . .
H8A H 0.9044 1.0960 0.1894 0.063 Uiso 1 1 calc R . .
C7 C 0.8536(5) 0.5903(4) 0.1031(2) 0.0658(12) Uani 1 1 d . . .
H7A H 0.8923 0.5950 0.0512 0.099 Uiso 1 1 calc R . .
H7B H 0.7599 0.5247 0.1028 0.099 Uiso 1 1 calc R . .
H7C H 0.9156 0.5601 0.1398 0.099 Uiso 1 1 calc R . .
C6 C 1.1939(5) 0.5353(5) 0.3702(3) 0.0727(14) Uani 1 1 d . . .
H6A H 1.2805 0.5218 0.3879 0.087 Uiso 1 1 calc R . .
C5 C 1.0174(5) 0.8711(5) 0.1014(2) 0.0665(12) Uani 1 1 d . . .
H5A H 1.0311 0.8500 0.0473 0.100 Uiso 1 1 calc R . .
H5B H 1.0912 0.8509 0.1340 0.100 Uiso 1 1 calc R . .
H5C H 1.0220 0.9687 0.1067 0.100 Uiso 1 1 calc R . .
C4 C 0.7447(6) 1.2287(5) 0.0545(3) 0.0709(14) Uani 1 1 d . . .
H4A H 0.7634 1.2938 0.0140 0.085 Uiso 1 1 calc R . .
C3 C 1.1924(4) 0.6275(5) 0.3104(3) 0.0615(12) Uani 1 1 d . . .
H3A H 1.2782 0.6787 0.2888 0.074 Uiso 1 1 calc R . .
C2 C 0.6070(6) 1.1535(5) 0.0690(2) 0.0676(13) Uani 1 1 d . . .
H2A H 0.5321 1.1686 0.0383 0.081 Uiso 1 1 calc R . .
C1 C 0.8547(5) 1.2075(5) 0.1001(2) 0.0666(12) Uani 1 1 d . . .
H1A H 0.9485 1.2600 0.0912 0.080 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'
F F 0.0171 0.0103 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C32 Fe1 C31 86.34(13) . . ?
C32 Fe1 N1 93.09(12) . . ?
C31 Fe1 N1 80.67(13) . . ?
C32 Fe1 N2 80.44(13) . . ?
C31 Fe1 N2 92.54(12) . . ?
N1 Fe1 N2 170.95(12) . . ?
C32 Fe1 P3 86.12(10) . . ?
C31 Fe1 P3 171.61(10) . . ?
N1 Fe1 P3 96.08(9) . . ?
N2 Fe1 P3 89.82(8) . . ?
C32 Fe1 P2 169.48(10) . . ?
C31 Fe1 P2 83.87(10) . . ?
N1 Fe1 P2 89.14(8) . . ?
N2 Fe1 P2 96.11(8) . . ?
P3 Fe1 P2 103.88(4) . . ?
C25 P2 C10 98.34(18) . . ?
C25 P2 C19 98.13(17) . . ?
C10 P2 C19 98.95(19) . . ?
C25 P2 Fe1 117.83(13) . . ?
C10 P2 Fe1 125.67(13) . . ?
C19 P2 Fe1 113.11(13) . . ?
C7 P3 C9 98.1(2) . . ?
C7 P3 C5 99.5(2) . . ?
C9 P3 C5 98.5(2) . . ?
C7 P3 Fe1 113.49(15) . . ?
C9 P3 Fe1 117.54(14) . . ?
C5 P3 Fe1 125.12(14) . . ?
C23 N2 C28 114.9(3) . . ?
C23 N2 Fe1 114.9(2) . . ?
C28 N2 Fe1 130.2(2) . . ?
C27 N1 C21 115.1(3) . . ?
C27 N1 Fe1 114.4(2) . . ?
C21 N1 Fe1 130.4(2) . . ?
C24 C32 C12 112.5(3) . . ?
C24 C32 Fe1 135.1(3) . . ?
C12 C32 Fe1 112.3(2) . . ?
C29 C31 C20 113.2(3) . . ?
C29 C31 Fe1 134.5(3) . . ?
C20 C31 Fe1 112.3(2) . . ?
C11 C30 C28 119.5(4) . . ?
C26 C29 F8 114.1(3) . . ?
C26 C29 C31 124.7(3) . . ?
F8 C29 C31 121.2(3) . . ?
C18 C28 C30 119.3(3) . . ?
C18 C28 N2 119.3(3) . . ?
C30 C28 N2 121.4(3) . . ?
N1 C27 C20 117.4(3) . . ?
F5 C26 C29 120.8(3) . . ?
F5 C26 C17 118.8(3) . . ?
C29 C26 C17 120.4(3) . . ?
F7 C24 C13 114.3(3) . . ?
F7 C24 C32 121.2(3) . . ?
C13 C24 C32 124.4(4) . . ?
N2 C23 C12 116.7(3) . . ?
F2 C22 C16 121.6(4) . . ?
F2 C22 C13 120.5(3) . . ?
C16 C22 C13 117.9(3) . . ?
C8 C21 C15 119.4(4) . . ?
C8 C21 N1 119.2(3) . . ?
C15 C21 N1 121.4(4) . . ?
C14 C20 C31 122.6(3) . . ?
C14 C20 C27 123.1(3) . . ?
C31 C20 C27 114.1(3) . . ?
C28 C18 C3 120.4(4) . . ?
F1 C17 C14 121.6(3) . . ?
F1 C17 C26 120.2(3) . . ?
C14 C17 C26 118.2(3) . . ?
F3 C16 C22 118.9(3) . . ?
F3 C16 C12 120.2(3) . . ?
C22 C16 C12 120.9(4) . . ?
C21 C15 C2 118.7(4) . . ?
F6 C14 C17 119.1(3) . . ?
F6 C14 C20 120.0(4) . . ?
C17 C14 C20 120.9(3) . . ?
F4 C13 C22 118.4(3) . . ?
F4 C13 C24 120.5(4) . . ?
C22 C13 C24 121.1(3) . . ?
C16 C12 C32 123.1(3) . . ?
C16 C12 C23 122.4(3) . . ?
C32 C12 C23 114.3(3) . . ?
C6 C11 C30 120.6(4) . . ?
C1 C8 C21 120.3(4) . . ?
C11 C6 C3 120.2(4) . . ?
C2 C4 C1 119.3(4) . . ?
C6 C3 C18 119.9(4) . . ?
C4 C2 C15 121.4(4) . . ?
C4 C1 C8 120.8(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C32 2.007(3) . ?
Fe1 C31 2.011(3) . ?
Fe1 N1 2.021(3) . ?
Fe1 N2 2.035(3) . ?
Fe1 P3 2.3175(11) . ?
Fe1 P2 2.3297(10) . ?
P2 C25 1.828(3) . ?
P2 C10 1.836(4) . ?
P2 C19 1.839(4) . ?
P3 C7 1.827(4) . ?
P3 C9 1.838(4) . ?
P3 C5 1.841(4) . ?
F8 C29 1.376(4) . ?
F7 C24 1.367(4) . ?
N2 C23 1.305(4) . ?
N2 C28 1.444(4) . ?
N1 C27 1.312(4) . ?
N1 C21 1.443(4) . ?
F6 C14 1.355(4) . ?
F5 C26 1.347(4) . ?
F4 C13 1.353(4) . ?
F3 C16 1.360(4) . ?
C32 C24 1.390(5) . ?
C32 C12 1.425(5) . ?
F2 C22 1.354(4) . ?
C31 C29 1.385(5) . ?
C31 C20 1.418(5) . ?
C30 C11 1.386(5) . ?
C30 C28 1.391(5) . ?
F1 C17 1.352(4) . ?
C29 C26 1.372(5) . ?
C28 C18 1.383(5) . ?
C27 C20 1.423(5) . ?
C26 C17 1.379(5) . ?
C24 C13 1.379(5) . ?
C23 C12 1.434(5) . ?
C22 C16 1.362(5) . ?
C22 C13 1.371(5) . ?
C21 C8 1.387(5) . ?
C21 C15 1.390(5) . ?
C20 C14 1.396(5) . ?
C18 C3 1.385(5) . ?
C17 C14 1.359(5) . ?
C16 C12 1.394(5) . ?
C15 C2 1.393(6) . ?
C11 C6 1.369(6) . ?
C8 C1 1.373(5) . ?
C6 C3 1.371(6) . ?
C4 C2 1.365(6) . ?
C4 C1 1.368(6) . ?
