#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:04:07 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179912 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/07/7020730.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_7020730
loop_
_publ_author_name
'Xu, Xiaofeng'
'Jia, Jiong'
'Sun, Hongjian'
'Liu, Yuxia'
'Xu, Wengang'
'Shi, Yujie'
'Zhang, Dongju'
'Li, Xiaoyan'
_publ_section_title
;
 Selective activation of C--F and C--H bonds with iron complexes, the
 relevant mechanism study by DFT calculations and study on the chemical
 properties of hydrido iron complex
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              3417
_journal_paper_doi               10.1039/c2dt31795h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C22 H35 F2 Fe I N P3'
_chemical_formula_weight         627.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.492(7)
_cell_length_b                   12.097(6)
_cell_length_c                   34.022(17)
_cell_measurement_reflns_used    1070
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.43
_cell_measurement_theta_min      2.34
_cell_volume                     5553(5)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.1621
_diffrn_reflns_av_sigmaI/netI    0.1821
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            17416
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    1.851
_exptl_absorpt_correction_T_max  0.8660
_exptl_absorpt_correction_T_min  0.7687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.842
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.1667
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0666P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                1452
_reflns_number_total             3628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31795h.txt
_cod_data_source_block           d:\tmp\h_sun\9\sun9
_cod_original_sg_symbol_H-M      cmca
_cod_database_code               7020730
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x, -y, -z'
'-x, y+1/2, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x, y, z'
'x, -y-1/2, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y, z-1/2'
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 1.0000 0.32244(12) 0.14983(4) 0.0330(4) Uani 1 2 d S . .
I1 I 1.0000 0.54728(6) 0.16505(2) 0.0466(3) Uani 1 2 d S . .
P1 P 0.83258(17) 0.33763(17) 0.14729(7) 0.0448(6) Uani 1 1 d . . .
P2 P 1.0000 0.2643(2) 0.21226(9) 0.0434(8) Uani 1 2 d S . .
N1 N 1.0000 0.3582(7) 0.0941(3) 0.036(2) Uani 1 2 d S . .
H1 H 1.0000 0.4263 0.0869 0.043 Uiso 1 2 calc SR . .
C1 C 1.0000 0.1732(8) 0.1265(3) 0.041(3) Uani 1 2 d S . .
C2 C 1.0000 0.0677(9) 0.1426(4) 0.050(3) Uani 1 2 d S . .
H2 H 1.0000 0.0605 0.1698 0.060 Uiso 1 2 calc SR . .
C3 C 1.0000 -0.0283(9) 0.1196(5) 0.065(4) Uani 1 2 d S . .
H3 H 1.0000 -0.0972 0.1317 0.078 Uiso 1 2 calc SR . .
C4 C 1.0000 -0.0219(12) 0.0792(5) 0.070(4) Uani 1 2 d S . .
H4 H 1.0000 -0.0860 0.0641 0.084 Uiso 1 2 calc SR . .
C5 C 1.0000 0.0774(10) 0.0619(4) 0.074(5) Uani 1 2 d S . .
H5 H 1.0000 0.0822 0.0346 0.089 Uiso 1 2 calc SR . .
C6 C 1.0000 0.1735(10) 0.0843(3) 0.047(3) Uani 1 2 d S . .
C7 C 1.0000 0.2817(10) 0.0678(4) 0.045(3) Uani 1 2 d S . .
C8 C 0.7627(7) 0.2114(7) 0.1360(3) 0.085(4) Uani 1 1 d . . .
H8A H 0.7771 0.1560 0.1554 0.128 Uiso 1 1 calc R . .
H8B H 0.7816 0.1847 0.1105 0.128 Uiso 1 1 calc R . .
H8C H 0.6931 0.2274 0.1362 0.128 Uiso 1 1 calc R . .
C9 C 0.7863(6) 0.4203(7) 0.1061(2) 0.061(3) Uani 1 1 d . . .
H9A H 0.7159 0.4296 0.1086 0.091 Uiso 1 1 calc R . .
H9B H 0.8008 0.3832 0.0818 0.091 Uiso 1 1 calc R . .
H9C H 0.8179 0.4914 0.1063 0.091 Uiso 1 1 calc R . .
C10 C 0.7618(7) 0.4003(7) 0.1873(3) 0.069(3) Uani 1 1 d . . .
H10A H 0.7887 0.4718 0.1932 0.103 Uiso 1 1 calc R . .
H10B H 0.7656 0.3540 0.2102 0.103 Uiso 1 1 calc R . .
H10C H 0.6938 0.4080 0.1794 0.103 Uiso 1 1 calc R . .
C11 C 0.8958(6) 0.1759(7) 0.2295(3) 0.059(3) Uani 1 1 d . . .
H11A H 0.9121 0.1445 0.2546 0.088 Uiso 1 1 calc R . .
H11B H 0.8845 0.1177 0.2108 0.088 Uiso 1 1 calc R . .
H11C H 0.8369 0.2200 0.2319 0.088 Uiso 1 1 calc R . .
C12 C 1.0000 0.3673(11) 0.2514(3) 0.069(4) Uani 1 2 d S . .
H12A H 0.9350 0.3989 0.2538 0.104 Uiso 0.50 1 calc PR . .
H12B H 1.0468 0.4245 0.2452 0.104 Uiso 0.50 1 calc PR . .
H12C H 1.0182 0.3329 0.2758 0.104 Uiso 0.50 1 calc PR . .
C13 C 1.014(2) 0.3012(10) 0.0250(4) 0.049(5) Uiso 0.50 1 d P . .
C14 C 0.9402(19) 0.338(2) 0.0031(7) 0.086(8) Uiso 0.50 1 d P . -1
C15 C 0.936(2) 0.358(3) -0.0374(9) 0.119(12) Uiso 0.50 1 d P . -1
H15A H 0.8810 0.3804 -0.0517 0.142 Uiso 0.50 1 calc PR . -1
C16 C 1.0310(13) 0.3375(14) -0.0523(5) 0.054(6) Uiso 0.50 1 d P . -1
H16A H 1.0377 0.3477 -0.0793 0.065 Uiso 0.50 1 calc PR . -1
C17 C 1.112(2) 0.306(2) -0.0342(8) 0.105(9) Uiso 0.50 1 d P . -1
H17A H 1.1725 0.2983 -0.0467 0.126 Uiso 0.50 1 calc PR . -1
C18 C 1.098(2) 0.285(2) 0.0054(7) 0.080(7) Uiso 0.50 1 d P . -1
F1 F 0.8449(14) 0.3591(16) 0.0185(5) 0.162(7) Uiso 0.50 1 d P A -1
F2 F 1.1754(12) 0.2479(14) 0.0255(5) 0.139(5) Uiso 0.50 1 d P B -1
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'
I I -0.4742 1.8119 '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
N1 Fe1 C1 79.1(4)
N1 Fe1 P2 174.5(3)
C1 Fe1 P2 95.4(3)
N1 Fe1 P1 86.84(7)
C1 Fe1 P1 93.37(7)
P2 Fe1 P1 93.54(7)
N1 Fe1 I1 87.9(3)
C1 Fe1 I1 167.1(3)
P2 Fe1 I1 97.55(10)
P1 Fe1 I1 85.85(6)
C10 P1 C9 99.5(4)
C10 P1 C8 103.4(5)
C9 P1 C8 96.9(5)
C10 P1 Fe1 121.7(3)
C9 P1 Fe1 114.4(3)
C8 P1 Fe1 116.9(3)
C12 P2 C11 99.4(4)
C12 P2 Fe1 118.5(4)
C11 P2 Fe1 118.6(3)
C7 N1 Fe1 121.2(8)
C2 C1 C6 113.4(10)
C2 C1 Fe1 133.1(9)
C6 C1 Fe1 113.6(8)
C1 C2 C3 122.9(13)
C4 C3 C2 120.7(12)
C5 C4 C3 119.3(12)
C4 C5 C6 120.6(14)
C5 C6 C7 123.5(12)
C5 C6 C1 123.1(12)
C7 C6 C1 113.4(10)
N1 C7 C6 112.8(11)
N1 C7 C13 124.5(11)
C6 C7 C13 122.1(11)
C14 C13 C18 114.3(19)
C14 C13 C7 121(2)
C18 C13 C7 125(2)
C13 C14 C15 130(3)
C13 C14 F1 123(2)
C15 C14 F1 107(2)
C16 C15 C14 107(3)
C17 C16 C15 130(2)
C16 C17 C18 114(3)
F2 C18 C13 118(2)
F2 C18 C17 118(3)
C13 C18 C17 125(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe1 N1 1.945(9)
Fe1 C1 1.973(10)
Fe1 P2 2.238(3)
Fe1 P1 2.268(2)
Fe1 I1 2.769(2)
P1 C10 1.827(9)
P1 C9 1.831(8)
P1 C8 1.835(8)
P2 C12 1.824(13)
P2 C11 1.860(8)
N1 C7 1.287(13)
C1 C2 1.388(14)
C1 C6 1.436(14)
C2 C3 1.400(16)
C3 C4 1.376(19)
C4 C5 1.339(17)
C5 C6 1.389(14)
C6 C7 1.424(15)
C7 C13 1.487(16)
C13 C14 1.32(3)
C13 C18 1.34(4)
C14 C15 1.40(3)
C14 F1 1.41(3)
C15 C16 1.40(3)
C16 C17 1.31(3)
C17 C18 1.38(3)
C18 F2 1.32(3)
