#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:31:56 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178655 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/66/4076642.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_4076642
loop_
_publ_author_name
'Jenny, Titus A.'
'Huber, Vroni'
'Ma, Liqian'
'Raemy, Jacques'
'Zeller, David'
'Stoeckli-Evans, Helen'
_publ_section_title
;
 Synthesis, X-ray Structure, and Reactivity of Phosphine-Substituted Iron
 Carbonyl Complexes Containingσ-Alkyl−π-Allyl Ligands
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2504
_journal_paper_doi               10.1021/om010781s
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C17 H34 Fe O7 P2'
_chemical_formula_weight         468.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8370(10)
_cell_length_b                   14.4150(10)
_cell_length_c                   17.0720(10)
_cell_measurement_temperature    193(2)
_cell_volume                     2174.7(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_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    0.0184
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2195
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.874
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.53
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.0042(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.083
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_obs          0.0318
_refine_ls_shift/esd_max         -0.445
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0463P)²+2.1946P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0852
_refine_ls_wR_factor_obs         0.0828
_reflns_number_observed          2110
_reflns_number_total             2195
_reflns_observed_criterion       2sigma(I)
_cod_data_source_file            om010781s.cif
_cod_data_source_block           compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+2.1946P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+2.1946P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4076642
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.53738(6) 0.51026(4) 0.90542(3) 0.0174(2) Uani 1 d .
C1 C 0.6111(5) 0.6278(3) 0.8365(3) 0.0227(9) Uani 1 d .
H1 H 0.6153(5) 0.6187(3) 0.7785(3) 0.027 Uiso 1 calc R
C2 C 0.4668(5) 0.6412(3) 0.8694(3) 0.0245(9) Uani 1 d .
C3 C 0.4610(5) 0.6437(3) 0.9521(2) 0.0240(8) Uani 1 d .
H3 H 0.3586(5) 0.6455(3) 0.9769(2) 0.029 Uiso 1 calc R
C4 C 0.5896(5) 0.6846(3) 0.9975(3) 0.0261(9) Uani 1 d .
H4A H 0.5831(5) 0.6653(3) 1.0530(3) 0.031 Uiso 1 calc R
H4B H 0.5846(5) 0.7532(3) 0.9953(3) 0.031 Uiso 1 calc R
C5 C 0.7377(5) 0.6512(3) 0.9622(2) 0.0238(9) Uani 1 d .
H5 H 0.8264(5) 0.6775(3) 0.9910(2) 0.029 Uiso 1 calc R
C6 C 0.7464(5) 0.6743(3) 0.8740(3) 0.0239(9) Uani 1 d .
C7 C 0.7317(5) 0.5459(3) 0.9706(2) 0.0219(9) Uani 1 d .
H7A H 0.7210(5) 0.5273(3) 1.0261(2) 0.026 Uiso 1 calc R
H7B H 0.8235(5) 0.5165(3) 0.9484(2) 0.026 Uiso 1 calc R
C8 C 0.3256(5) 0.6539(4) 0.8212(3) 0.0368(12) Uani 1 d .
H8A H 0.3108(23) 0.7200(4) 0.8102(18) 0.055 Uiso 1 calc R
H8B H 0.2382(8) 0.6300(23) 0.8503(9) 0.055 Uiso 1 calc R
H8C H 0.3358(17) 0.6199(20) 0.7718(10) 0.055 Uiso 1 calc R
C9 C 0.8942(5) 0.6401(3) 0.8378(3) 0.0320(10) Uani 1 d .
H9A H 0.9799(5) 0.6706(17) 0.8635(13) 0.048 Uiso 1 calc R
H9B H 0.8953(17) 0.6548(20) 0.7817(5) 0.048 Uiso 1 calc R
H9C H 0.9024(18) 0.5728(5) 0.8448(17) 0.048 Uiso 1 calc R
C10 C 0.7365(5) 0.7800(3) 0.8583(3) 0.0319(10) Uani 1 d .
H10A H 0.8261(19) 0.8107(4) 0.8800(17) 0.048 Uiso 1 calc R
H10B H 0.6453(20) 0.8050(5) 0.8833(16) 0.048 Uiso 1 calc R
H10C H 0.7317(36) 0.7911(3) 0.8017(3) 0.048 Uiso 1 calc R
P1 P 0.45940(13) 0.44300(7) 1.01016(6) 0.0212(2) Uani 1 d .
O1 O 0.4667(4) 0.5071(2) 1.0866(2) 0.0315(7) Uani 1 d .
C11 C 0.4177(7) 0.4748(3) 1.1625(3) 0.0435(13) Uani 1 d .
H11A H 0.3286(27) 0.5101(19) 1.1791(10) 0.065 Uiso 1 calc R
H11B H 0.4994(17) 0.4835(24) 1.2006(5) 0.065 Uiso 1 calc R
H11C H 0.3918(41) 0.4088(8) 1.1593(6) 0.065 Uiso 1 calc R
O2 O 0.5261(4) 0.3454(2) 1.0407(2) 0.0325(7) Uani 1 d .
C12 C 0.6840(6) 0.3322(4) 1.0526(3) 0.0436(13) Uani 1 d .
H12A H 0.7052(8) 0.2658(4) 1.0587(22) 0.065 Uiso 1 calc R
H12B H 0.7158(10) 0.3654(22) 1.0999(13) 0.065 Uiso 1 calc R
H12C H 0.7397(6) 0.3562(24) 1.0073(11) 0.065 Uiso 1 calc R
O3 O 0.2880(3) 0.4032(2) 1.0126(2) 0.0300(7) Uani 1 d .
C13 C 0.1621(5) 0.4653(4) 1.0044(3) 0.0416(12) Uani 1 d .
H13A H 0.1486(27) 0.5003(19) 1.0532(9) 0.062 Uiso 1 calc R
H13B H 0.0703(10) 0.4296(4) 0.9933(22) 0.062 Uiso 1 calc R
H13C H 0.1816(20) 0.5086(17) 0.9613(15) 0.062 Uiso 1 calc R
P2 P 0.66949(13) 0.41361(8) 0.83813(7) 0.0241(3) Uani 1 d .
O4 O 0.8357(4) 0.3887(2) 0.8655(2) 0.0413(9) Uani 1 d .
C14 C 0.9318(6) 0.3251(4) 0.8220(4) 0.0463(14) Uani 1 d .
H14A H 0.9192(34) 0.2621(6) 0.8427(16) 0.069 Uiso 1 calc R
H14B H 1.0378(7) 0.3441(16) 0.8274(19) 0.069 Uiso 1 calc R
H14C H 0.9032(30) 0.3261(20) 0.7665(5) 0.069 Uiso 1 calc R
O5 O 0.5985(4) 0.3163(2) 0.8130(2) 0.0438(9) Uani 1 d .
C15 C 0.5354(7) 0.2526(3) 0.8687(3) 0.0467(13) Uani 1 d .
H15A H 0.6144(13) 0.2329(21) 0.9055(14) 0.070 Uiso 1 calc R
H15B H 0.4953(41) 0.1983(13) 0.8412(4) 0.070 Uiso 1 calc R
H15C H 0.4536(31) 0.2832(10) 0.8976(16) 0.070 Uiso 1 calc R
O6 O 0.7150(4) 0.4450(3) 0.7493(2) 0.0430(9) Uani 1 d .
C16 C 0.6030(7) 0.4514(4) 0.6904(3) 0.0450(13) Uani 1 d .
H16A H 0.5684(30) 0.3890(4) 0.6763(15) 0.067 Uiso 1 calc R
H16B H 0.6457(14) 0.4819(23) 0.6441(8) 0.067 Uiso 1 calc R
H16C H 0.5173(19) 0.4877(22) 0.7100(8) 0.067 Uiso 1 calc R
O7 O 0.2800(4) 0.4326(3) 0.8216(2) 0.0368(8) Uani 1 d .
C17 C 0.3801(5) 0.4664(3) 0.8541(2) 0.0243(9) Uani 1 d .
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'
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
C17 Fe1 C2 86.7(2)
C17 Fe1 C7 173.0(2)
C2 Fe1 C7 100.3(2)
C17 Fe1 P1 89.92(14)
C2 Fe1 P1 124.02(13)
C7 Fe1 P1 86.11(12)
C17 Fe1 P2 85.98(14)
C2 Fe1 P2 126.33(13)
C7 Fe1 P2 89.85(12)
P1 Fe1 P2 109.06(5)
C17 Fe1 C1 104.4(2)
C2 Fe1 C1 38.6(2)
C7 Fe1 C1 81.4(2)
P1 Fe1 C1 154.58(12)
P2 Fe1 C1 93.05(12)
C17 Fe1 C3 104.7(2)
C2 Fe1 C3 38.6(2)
C7 Fe1 C3 81.1(2)
P1 Fe1 C3 89.70(11)
P2 Fe1 C3 158.64(12)
C1 Fe1 C3 66.6(2)
C2 C1 C6 119.1(4)
C2 C1 Fe1 67.5(2)
C6 C1 Fe1 110.8(3)
C1 C2 C3 115.8(4)
C1 C2 C8 123.3(4)
C3 C2 C8 120.8(5)
C1 C2 Fe1 73.9(3)
C3 C2 Fe1 74.9(2)
C8 C2 Fe1 121.3(3)
C2 C3 C4 120.0(4)
C2 C3 Fe1 66.6(2)
C4 C3 Fe1 107.5(3)
C3 C4 C5 108.9(3)
C4 C5 C7 104.4(4)
C4 C5 C6 111.2(4)
C7 C5 C6 108.0(3)
C1 C6 C9 111.2(3)
C1 C6 C5 106.1(3)
C9 C6 C5 111.6(4)
C1 C6 C10 108.5(4)
C9 C6 C10 107.2(4)
C5 C6 C10 112.2(3)
C5 C7 Fe1 102.8(3)
O1 P1 O2 103.1(2)
O1 P1 O3 102.8(2)
O2 P1 O3 91.4(2)
O1 P1 Fe1 113.89(12)
O2 P1 Fe1 123.08(13)
O3 P1 Fe1 118.73(12)
C11 O1 P1 122.2(3)
C12 O2 P1 121.4(3)
C13 O3 P1 120.1(3)
O4 P2 O5 104.2(2)
O4 P2 O6 96.2(2)
O5 P2 O6 95.2(2)
O4 P2 Fe1 119.51(14)
O5 P2 Fe1 119.99(14)
O6 P2 Fe1 116.78(14)
C14 O4 P2 122.3(3)
C15 O5 P2 122.5(3)
C16 O6 P2 120.4(3)
O7 C17 Fe1 176.1(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe1 C17 1.761(4)
Fe1 C2 2.080(4)
Fe1 C7 2.109(4)
Fe1 P1 2.1476(12)
Fe1 P2 2.1503(12)
Fe1 C1 2.163(4)
Fe1 C3 2.188(4)
C1 C2 1.406(6)
C1 C6 1.514(6)
C2 C3 1.413(6)
C2 C8 1.506(6)
C3 C4 1.496(6)
C4 C5 1.519(6)
C5 C7 1.525(6)
C5 C6 1.543(6)
C6 C9 1.527(6)
C6 C10 1.550(6)
P1 O1 1.600(3)
P1 O2 1.612(3)
P1 O3 1.620(3)
O1 C11 1.444(5)
O2 C12 1.423(6)
O3 C13 1.435(6)
P2 O4 1.583(4)
P2 O5 1.596(3)
P2 O6 1.633(4)
O4 C14 1.455(6)
O5 C15 1.434(6)
O6 C16 1.414(6)
O7 C17 1.152(5)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C17 Fe1 C1 C2 65.4(3)
C2 Fe1 C1 C2 0.000(2)
C7 Fe1 C1 C2 -118.6(3)
P1 Fe1 C1 C2 -57.0(4)
P2 Fe1 C1 C2 152.0(2)
C3 Fe1 C1 C2 -34.6(3)
C17 Fe1 C1 C6 179.4(3)
C2 Fe1 C1 C6 113.9(4)
C7 Fe1 C1 C6 -4.6(3)
P1 Fe1 C1 C6 56.9(4)
P2 Fe1 C1 C6 -94.0(3)
C3 Fe1 C1 C6 79.3(3)
C6 C1 C2 C3 -38.3(6)
Fe1 C1 C2 C3 63.8(3)
C6 C1 C2 C8 140.7(4)
Fe1 C1 C2 C8 -117.2(4)
C6 C1 C2 Fe1 -102.1(4)
Fe1 C1 C2 Fe1 0.000(1)
C17 Fe1 C2 C1 -118.1(3)
C7 Fe1 C2 C1 62.0(3)
P1 Fe1 C2 C1 154.2(2)
P2 Fe1 C2 C1 -35.5(3)
C1 Fe1 C2 C1 0.000(2)
C3 Fe1 C2 C1 123.2(4)
C17 Fe1 C2 C3 118.7(3)
C7 Fe1 C2 C3 -61.3(3)
P1 Fe1 C2 C3 31.0(3)
P2 Fe1 C2 C3 -158.8(2)
C1 Fe1 C2 C3 -123.2(4)
C3 Fe1 C2 C3 0.000(4)
C17 Fe1 C2 C8 1.5(4)
C7 Fe1 C2 C8 -178.5(4)
P1 Fe1 C2 C8 -86.2(4)
P2 Fe1 C2 C8 84.0(4)
C1 Fe1 C2 C8 119.6(5)
C3 Fe1 C2 C8 -117.2(5)
C1 C2 C3 C4 34.2(6)
C8 C2 C3 C4 -144.8(4)
Fe1 C2 C3 C4 97.4(4)
C1 C2 C3 Fe1 -63.2(3)
C8 C2 C3 Fe1 117.8(4)
Fe1 C2 C3 Fe1 0.000(2)
C17 Fe1 C3 C2 -64.9(3)
C2 Fe1 C3 C2 0.000(4)
C7 Fe1 C3 C2 119.2(3)
P1 Fe1 C3 C2 -154.7(3)
P2 Fe1 C3 C2 53.3(5)
C1 Fe1 C3 C2 34.7(3)
C17 Fe1 C3 C4 179.4(3)
C2 Fe1 C3 C4 -115.8(4)
C7 Fe1 C3 C4 3.4(3)
P1 Fe1 C3 C4 89.5(3)
P2 Fe1 C3 C4 -62.5(5)
C1 Fe1 C3 C4 -81.1(3)
C2 C3 C4 C5 -43.2(5)
Fe1 C3 C4 C5 29.4(4)
C3 C4 C5 C7 -60.5(4)
C3 C4 C5 C6 55.6(4)
C2 C1 C6 C9 171.5(4)
Fe1 C1 C6 C9 96.4(4)
C2 C1 C6 C5 50.0(5)
Fe1 C1 C6 C5 -25.1(4)
C2 C1 C6 C10 -70.8(5)
Fe1 C1 C6 C10 -145.9(3)
C4 C5 C6 C1 -58.2(4)
C7 C5 C6 C1 55.7(4)
C4 C5 C6 C9 -179.4(3)
C7 C5 C6 C9 -65.5(5)
C4 C5 C6 C10 60.2(5)
C7 C5 C6 C10 174.1(4)
C4 C5 C7 Fe1 60.2(3)
C6 C5 C7 Fe1 -58.2(4)
C17 Fe1 C7 C5 179.7(13)
C2 Fe1 C7 C5 -0.8(3)
P1 Fe1 C7 C5 -124.7(3)
P2 Fe1 C7 C5 126.2(3)
C1 Fe1 C7 C5 33.1(3)
C3 Fe1 C7 C5 -34.4(3)
C17 Fe1 P1 O1 -134.9(2)
C2 Fe1 P1 O1 -49.0(2)
C7 Fe1 P1 O1 50.9(2)
P2 Fe1 P1 O1 139.35(15)
C1 Fe1 P1 O1 -9.8(3)
C3 Fe1 P1 O1 -30.2(2)
C17 Fe1 P1 O2 99.4(2)
C2 Fe1 P1 O2 -174.7(2)
C7 Fe1 P1 O2 -74.9(2)
P2 Fe1 P1 O2 13.6(2)
C1 Fe1 P1 O2 -135.5(3)
C3 Fe1 P1 O2 -155.9(2)
C17 Fe1 P1 O3 -13.6(2)
C2 Fe1 P1 O3 72.3(2)
C7 Fe1 P1 O3 172.2(2)
P2 Fe1 P1 O3 -99.35(14)
C1 Fe1 P1 O3 111.5(3)
C3 Fe1 P1 O3 91.1(2)
O2 P1 O1 C11 -45.0(4)
O3 P1 O1 C11 49.5(4)
Fe1 P1 O1 C11 179.3(3)
O1 P1 O2 C12 -76.3(4)
O3 P1 O2 C12 -179.8(4)
Fe1 P1 O2 C12 54.0(4)
O1 P1 O3 C13 64.6(4)
O2 P1 O3 C13 168.4(4)
Fe1 P1 O3 C13 -62.1(4)
C17 Fe1 P2 O4 -163.6(2)
C2 Fe1 P2 O4 113.5(2)
C7 Fe1 P2 O4 10.7(2)
P1 Fe1 P2 O4 -75.1(2)
C1 Fe1 P2 O4 92.2(2)
C3 Fe1 P2 O4 75.1(4)
C17 Fe1 P2 O5 -32.9(2)
C2 Fe1 P2 O5 -115.8(2)
C7 Fe1 P2 O5 141.4(2)
P1 Fe1 P2 O5 55.6(2)
C1 Fe1 P2 O5 -137.1(2)
C3 Fe1 P2 O5 -154.2(4)
C17 Fe1 P2 O6 81.2(2)
C2 Fe1 P2 O6 -1.7(2)
C7 Fe1 P2 O6 -104.5(2)
P1 Fe1 P2 O6 169.7(2)
C1 Fe1 P2 O6 -23.0(2)
C3 Fe1 P2 O6 -40.1(4)
O5 P2 O4 C14 43.6(4)
O6 P2 O4 C14 -53.4(4)
Fe1 P2 O4 C14 -179.0(3)
O4 P2 O5 C15 82.1(4)
O6 P2 O5 C15 179.9(4)
Fe1 P2 O5 C15 -55.0(5)
O4 P2 O6 C16 163.0(4)
O5 P2 O6 C16 58.0(4)
Fe1 P2 O6 C16 -69.4(4)
C2 Fe1 C17 O7 175.7(54)
C7 Fe1 C17 O7 -4.7(64)
P1 Fe1 C17 O7 -60.2(54)
P2 Fe1 C17 O7 48.9(54)
C1 Fe1 C17 O7 141.1(53)
C3 Fe1 C17 O7 -149.9(53)
