#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/60/2226035.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2226035
loop_
_publ_author_name
'Xu, Guoqiang'
'Li, Xiaoyan'
_publ_section_title
;
 {1,3-Bis[(diphenylphosphanyl-κP)oxy]propane}dicarbonyliron(0)
;
_journal_coeditor_code           ZS2034
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m544
_journal_paper_doi               10.1107/S1600536810013759
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Fe (C27 H26 O2 P2) (C O)2]'
_chemical_formula_moiety         'C29 H26 Fe O4 P2'
_chemical_formula_sum            'C29 H26 Fe O4 P2'
_chemical_formula_weight         556.29
_chemical_melting_point          385
_chemical_name_systematic
;
{1,3-Bis[(diphenylphosphanyl-κP)oxy]propane}dicarbonyliron(0)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.14(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.589(3)
_cell_length_b                   15.191(3)
_cell_length_c                   14.384(3)
_cell_measurement_reflns_used    17176
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.79
_cell_measurement_theta_min      1.90
_cell_volume                     2642.4(11)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω 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  0.0803
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17176
_diffrn_reflns_theta_full        26.79
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         1.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.8990
_exptl_absorpt_correction_T_min  0.8283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0487
_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)+(0.0350P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                3864
_reflns_number_total             5590
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            zs2034.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2226035
_cod_database_fobs_code          2226035
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.86496(4) 0.14441(3) 0.60132(3) 0.01955(11) Uani d . 1 . .
P P1 0.80915(7) 0.11051(5) 0.72478(5) 0.02269(17) Uani d . 1 . .
P P2 0.94395(6) 0.26876(5) 0.59809(5) 0.02229(17) Uani d . 1 . .
C C1 0.6609(3) 0.1013(2) 0.7101(2) 0.0233(6) Uani d . 1 . .
C C2 0.5887(3) 0.0808(2) 0.6205(2) 0.0310(7) Uani d . 1 . .
H H2 0.6157 0.0750 0.5669 0.037 Uiso calc R 1 . .
C C3 0.4769(3) 0.0689(3) 0.6105(2) 0.0363(8) Uani d . 1 . .
H H3 0.4296 0.0545 0.5503 0.044 Uiso calc R 1 . .
C C4 0.4353(3) 0.0783(2) 0.6893(2) 0.0337(8) Uani d . 1 . .
H H4 0.3603 0.0702 0.6825 0.040 Uiso calc R 1 . .
C C5 0.5061(3) 0.0997(2) 0.7781(2) 0.0314(7) Uani d . 1 . .
H H5 0.4782 0.1069 0.8311 0.038 Uiso calc R 1 . .
C C6 0.6177(3) 0.1107(2) 0.7895(2) 0.0281(7) Uani d . 1 . .
H H6 0.6645 0.1245 0.8501 0.034 Uiso calc R 1 . .
C C7 0.8558(3) 0.0063(2) 0.7873(2) 0.0262(7) Uani d . 1 . .
C C8 0.8773(3) -0.0665(2) 0.7358(2) 0.0310(7) Uani d . 1 . .
H H8 0.8735 -0.0605 0.6706 0.037 Uiso calc R 1 . .
C C9 0.9041(3) -0.1472(2) 0.7806(2) 0.0361(8) Uani d . 1 . .
H H9 0.9192 -0.1949 0.7458 0.043 Uiso calc R 1 . .
C C10 0.9086(3) -0.1566(2) 0.8773(2) 0.0356(8) Uani d . 1 . .
H H10 0.9250 -0.2112 0.9071 0.043 Uiso calc R 1 . .
C C11 0.8887(3) -0.0852(2) 0.9300(2) 0.0342(8) Uani d . 1 . .
H H11 0.8927 -0.0916 0.9952 0.041 Uiso calc R 1 . .
C C12 0.8629(3) -0.0040(2) 0.8852(2) 0.0290(7) Uani d . 1 . .
H H12 0.8502 0.0440 0.9208 0.035 Uiso calc R 1 . .
C C14 0.9435(3) 0.2174(2) 0.8523(2) 0.0280(7) Uani d . 1 . .
H H14A 0.9913 0.1969 0.8143 0.034 Uiso calc R 1 . .
H H14B 0.9749 0.1985 0.9188 0.034 Uiso calc R 1 . .
C C15 0.9355(3) 0.3167(2) 0.8480(2) 0.0276(7) Uani d . 1 . .
H H15A 0.8859 0.3362 0.8847 0.033 Uiso calc R 1 . .
H H15B 1.0079 0.3416 0.8779 0.033 Uiso calc R 1 . .
C C16 0.8941(3) 0.3508(2) 0.7457(2) 0.0267(6) Uani d . 1 . .
H H16A 0.8238 0.3236 0.7135 0.032 Uiso calc R 1 . .
H H16B 0.8834 0.4140 0.7464 0.032 Uiso calc R 1 . .
C C18 0.8717(2) 0.3468(2) 0.5048(2) 0.0246(6) Uani d . 1 . .
C C19 0.8872(3) 0.4367(2) 0.5213(2) 0.0295(7) Uani d . 1 . .
H H19 0.9362 0.4564 0.5785 0.035 Uiso calc R 1 . .
C C20 0.8308(3) 0.4973(2) 0.4537(2) 0.0347(8) Uani d . 1 . .
H H20 0.8409 0.5572 0.4662 0.042 Uiso calc R 1 . .
C C21 0.7590(3) 0.4685(2) 0.3673(2) 0.0350(8) Uani d . 1 . .
H H21 0.7213 0.5090 0.3215 0.042 Uiso calc R 1 . .
C C22 0.7440(3) 0.3796(3) 0.3498(2) 0.0352(8) Uani d . 1 . .
H H22 0.6965 0.3602 0.2918 0.042 Uiso calc R 1 . .
C C23 0.7994(3) 0.3186(2) 0.4183(2) 0.0294(7) Uani d . 1 . .
H H23 0.7881 0.2587 0.4062 0.035 Uiso calc R 1 . .
C C24 1.0822(3) 0.2664(2) 0.5825(2) 0.0241(6) Uani d . 1 . .
C C25 1.1746(3) 0.2932(2) 0.6554(2) 0.0309(7) Uani d . 1 . .
H H25 1.1658 0.3147 0.7134 0.037 Uiso calc R 1 . .
C C26 1.2795(3) 0.2883(3) 0.6426(3) 0.0376(8) Uani d . 1 . .
H H26 1.3408 0.3058 0.6920 0.045 Uiso calc R 1 . .
C C27 1.2931(3) 0.2572(3) 0.5554(3) 0.0401(9) Uani d . 1 . .
H H27 1.3632 0.2545 0.5460 0.048 Uiso calc R 1 . .
C C28 1.2025(3) 0.2307(3) 0.4837(2) 0.0412(9) Uani d . 1 . .
H H28 1.2115 0.2097 0.4256 0.049 Uiso calc R 1 . .
C C29 1.0982(3) 0.2345(3) 0.4964(2) 0.0365(8) Uani d . 1 . .
H H29 1.0377 0.2156 0.4471 0.044 Uiso calc R 1 . .
C C30 0.7896(3) 0.1023(2) 0.4877(2) 0.0328(8) Uani d . 1 . .
C C31 0.9862(3) 0.0802(2) 0.6249(2) 0.0351(8) Uani d . 1 . .
O O1 0.7392(2) 0.0776(2) 0.41268(18) 0.0520(7) Uani d . 1 . .
O O2 1.0661(2) 0.0395(2) 0.6391(2) 0.0513(7) Uani d . 1 . .
O O3 0.83459(18) 0.18051(15) 0.81476(13) 0.0262(5) Uani d . 1 . .
O O4 0.97462(18) 0.33011(14) 0.69448(14) 0.0261(5) Uani d . 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'
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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C31 Fe1 C30 . . 101.01(16) ?
C31 Fe1 P2 . . 96.31(12) ?
C30 Fe1 P2 . . 115.62(12) ?
C31 Fe1 P1 . . 99.98(12) ?
C30 Fe1 P1 . . 117.64(11) ?
P2 Fe1 P1 . . 119.37(4) ?
O3 P1 C1 . . 96.34(13) ?
O3 P1 C7 . . 101.98(13) ?
C1 P1 C7 . . 99.68(14) ?
O3 P1 Fe1 . . 117.47(9) ?
C1 P1 Fe1 . . 118.84(10) ?
C7 P1 Fe1 . . 118.60(11) ?
O4 P2 C24 . . 96.22(13) ?
O4 P2 C18 . . 101.85(13) ?
C24 P2 C18 . . 102.69(14) ?
O4 P2 Fe1 . . 119.27(9) ?
C24 P2 Fe1 . . 116.88(11) ?
C18 P2 Fe1 . . 116.62(11) ?
C2 C1 C6 . . 118.4(3) ?
C2 C1 P1 . . 120.6(2) ?
C6 C1 P1 . . 120.9(2) ?
C3 C2 C1 . . 120.6(3) ?
C3 C2 H2 . . 119.7 ?
C1 C2 H2 . . 119.7 ?
C4 C3 C2 . . 120.4(3) ?
C4 C3 H3 . . 119.8 ?
C2 C3 H3 . . 119.8 ?
C5 C4 C3 . . 119.3(3) ?
C5 C4 H4 . . 120.4 ?
C3 C4 H4 . . 120.4 ?
C6 C5 C4 . . 121.0(3) ?
C6 C5 H5 . . 119.5 ?
C4 C5 H5 . . 119.5 ?
C5 C6 C1 . . 120.3(3) ?
C5 C6 H6 . . 119.9 ?
C1 C6 H6 . . 119.9 ?
C12 C7 C8 . . 118.5(3) ?
C12 C7 P1 . . 120.9(3) ?
C8 C7 P1 . . 120.4(2) ?
C9 C8 C7 . . 120.9(3) ?
C9 C8 H8 . . 119.6 ?
C7 C8 H8 . . 119.6 ?
C8 C9 C10 . . 119.8(3) ?
C8 C9 H9 . . 120.1 ?
C10 C9 H9 . . 120.1 ?
C9 C10 C11 . . 120.3(3) ?
C9 C10 H10 . . 119.8 ?
C11 C10 H10 . . 119.8 ?
C10 C11 C12 . . 119.8(3) ?
C10 C11 H11 . . 120.1 ?
C12 C11 H11 . . 120.1 ?
C11 C12 C7 . . 120.6(3) ?
C11 C12 H12 . . 119.7 ?
C7 C12 H12 . . 119.7 ?
O3 C14 C15 . . 109.1(3) ?
O3 C14 H14A . . 109.9 ?
C15 C14 H14A . . 109.9 ?
O3 C14 H14B . . 109.9 ?
C15 C14 H14B . . 109.9 ?
H14A C14 H14B . . 108.3 ?
C16 C15 C14 . . 112.6(2) ?
C16 C15 H15A . . 109.1 ?
C14 C15 H15A . . 109.1 ?
C16 C15 H15B . . 109.1 ?
C14 C15 H15B . . 109.1 ?
H15A C15 H15B . . 107.8 ?
O4 C16 C15 . . 108.8(2) ?
O4 C16 H16A . . 109.9 ?
C15 C16 H16A . . 109.9 ?
O4 C16 H16B . . 109.9 ?
C15 C16 H16B . . 109.9 ?
H16A C16 H16B . . 108.3 ?
C23 C18 C19 . . 118.8(3) ?
C23 C18 P2 . . 121.6(3) ?
C19 C18 P2 . . 119.6(2) ?
C20 C19 C18 . . 120.9(3) ?
C20 C19 H19 . . 119.6 ?
C18 C19 H19 . . 119.6 ?
C19 C20 C21 . . 119.9(3) ?
C19 C20 H20 . . 120.0 ?
C21 C20 H20 . . 120.0 ?
C22 C21 C20 . . 119.6(3) ?
C22 C21 H21 . . 120.2 ?
C20 C21 H21 . . 120.2 ?
C21 C22 C23 . . 120.5(3) ?
C21 C22 H22 . . 119.7 ?
C23 C22 H22 . . 119.7 ?
C18 C23 C22 . . 120.2(3) ?
C18 C23 H23 . . 119.9 ?
C22 C23 H23 . . 119.9 ?
C25 C24 C29 . . 118.3(3) ?
C25 C24 P2 . . 122.0(2) ?
C29 C24 P2 . . 119.8(2) ?
C26 C25 C24 . . 120.7(3) ?
C26 C25 H25 . . 119.6 ?
C24 C25 H25 . . 119.6 ?
C25 C26 C27 . . 119.9(3) ?
C25 C26 H26 . . 120.1 ?
C27 C26 H26 . . 120.1 ?
C28 C27 C26 . . 119.5(3) ?
C28 C27 H27 . . 120.3 ?
C26 C27 H27 . . 120.3 ?
C27 C28 C29 . . 120.9(3) ?
C27 C28 H28 . . 119.5 ?
C29 C28 H28 . . 119.5 ?
C28 C29 C24 . . 120.7(3) ?
C28 C29 H29 . . 119.6 ?
C24 C29 H29 . . 119.6 ?
O1 C30 Fe1 . . 177.8(3) ?
O2 C31 Fe1 . . 178.6(3) ?
C14 O3 P1 . . 120.4(2) ?
C16 O4 P2 . . 121.75(19) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 C31 . 1.763(4) ?
Fe1 C30 . 1.765(3) ?
Fe1 P2 . 2.1414(10) ?
Fe1 P1 . 2.1462(10) ?
P1 O3 . 1.636(2) ?
P1 C1 . 1.824(3) ?
P1 C7 . 1.834(3) ?
P2 O4 . 1.625(2) ?
P2 C24 . 1.816(3) ?
P2 C18 . 1.832(3) ?
C1 C2 . 1.390(4) ?
C1 C6 . 1.402(4) ?
C2 C3 . 1.387(5) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.382(5) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.378(5) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.378(5) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C12 . 1.395(4) ?
C7 C8 . 1.399(5) ?
C8 C9 . 1.382(5) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.385(5) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.385(5) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.387(5) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C14 O3 . 1.440(4) ?
C14 C15 . 1.513(5) ?
C14 H14A . 0.9700 ?
C14 H14B . 0.9700 ?
C15 C16 . 1.509(4) ?
C15 H15A . 0.9700 ?
C15 H15B . 0.9700 ?
C16 O4 . 1.443(4) ?
C16 H16A . 0.9700 ?
C16 H16B . 0.9700 ?
C18 C23 . 1.389(4) ?
C18 C19 . 1.390(5) ?
C19 C20 . 1.382(5) ?
C19 H19 . 0.9300 ?
C20 C21 . 1.389(5) ?
C20 H20 . 0.9300 ?
C21 C22 . 1.377(5) ?
C21 H21 . 0.9300 ?
C22 C23 . 1.391(5) ?
C22 H22 . 0.9300 ?
C23 H23 . 0.9300 ?
C24 C25 . 1.394(4) ?
C24 C29 . 1.395(4) ?
C25 C26 . 1.386(5) ?
C25 H25 . 0.9300 ?
C26 C27 . 1.395(5) ?
C26 H26 . 0.9300 ?
C27 C28 . 1.369(5) ?
C27 H27 . 0.9300 ?
C28 C29 . 1.377(5) ?
C28 H28 . 0.9300 ?
C29 H29 . 0.9300 ?
C30 O1 . 1.152(4) ?
C31 O2 . 1.150(4) ?
