#------------------------------------------------------------------------------
#$Date: 2016-02-05 01:48:17 +0200 (Fri, 05 Feb 2016) $
#$Revision: 176060 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/71/7037123.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_7037123
loop_
_publ_author_name
'Pritzwald-Stegmann, Julian Rodger Frederic'
'Lönnecke, Peter'
'Hey-Hawkins, Evamarie'
_publ_section_title
;
 Hydrophosphination reactions with transition metal ferrocenylphosphine
 complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2208
_journal_page_last               2217
_journal_paper_doi               10.1039/c5dt03374h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C15 H11 Fe O5 P W'
_chemical_formula_weight         541.91
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2015-08-22T20:04:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-08-22 deposited with the CCDC.
2015-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.01670(10)
_cell_length_b                   12.98960(10)
_cell_length_c                   20.8330(2)
_cell_measurement_reflns_used    33748
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      37.4586
_cell_measurement_theta_min      2.9274
_cell_volume                     3251.87(5)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_publication_material
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 1999, 32, 837-838.
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
;
 SHELXS-97
 Program for Crystal Structure Analysis (Release 97-2)
 G. M. Sheldrick, Institüt für Anorganische Chemie der Universität,
 Tammanstrasse 4, D-3400 Göttingen, Germany, 1998.
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.025521
_diffrn_orient_matrix_UB_12      -0.0463224
_diffrn_orient_matrix_UB_13      -0.010394
_diffrn_orient_matrix_UB_21      0.0210954
_diffrn_orient_matrix_UB_22      -0.0081716
_diffrn_orient_matrix_UB_23      0.0313917
_diffrn_orient_matrix_UB_31      -0.048866
_diffrn_orient_matrix_UB_32      -0.027725
_diffrn_orient_matrix_UB_33      0.0081165
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            100043
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.317
_diffrn_reflns_theta_min         3.026
_exptl_absorpt_coefficient_mu    8.08
_exptl_absorpt_correction_T_max  0.553
_exptl_absorpt_correction_T_min  0.19
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.214
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.544
_refine_diff_density_min         -1.58
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         7875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.039
_refine_ls_R_factor_gt           0.032
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0112P)²+10.8417P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0629
_reflns_Friedel_coverage         0
_reflns_number_gt                6883
_reflns_number_total             7875
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt03374h2.cif
_cod_data_source_block           x1578fin_compound_1c
_cod_depositor_comments
'Adding full bibliography for 7037122--7037129.cif.'
_cod_database_code               7037123
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
W1 W 0.22749(2) 0.63614(2) 0.97303(2) 0.01907(3) Uani 1 1 d
Fe1 Fe 0.13190(3) 0.71972(3) 0.74266(2) 0.01792(7) Uani 1 1 d
P1 P 0.10077(6) 0.58895(6) 0.88181(4) 0.01983(12) Uani 1 1 d
O1 O 0.1536(3) 0.4317(3) 1.04521(16) 0.0554(9) Uani 1 1 d
O2 O 0.4323(2) 0.5113(2) 0.91521(16) 0.0436(7) Uani 1 1 d
O3 O 0.3850(2) 0.6943(2) 1.08849(12) 0.0360(6) Uani 1 1 d
O4 O 0.0381(3) 0.7699(3) 1.03924(15) 0.0535(9) Uani 1 1 d
O5 O 0.3005(3) 0.8408(2) 0.90128(14) 0.0381(6) Uani 1 1 d
C1 C 0.1468(2) 0.5935(2) 0.79963(14) 0.0191(4) Uani 1 1 d
C2 C 0.0801(3) 0.5700(2) 0.74460(15) 0.0228(5) Uani 1 1 d
C3 C 0.1456(3) 0.5873(2) 0.68871(15) 0.0262(6) Uani 1 1 d
C4 C 0.2529(3) 0.6217(2) 0.70849(15) 0.0242(5) Uani 1 1 d
C5 C 0.2547(2) 0.6257(2) 0.77671(14) 0.0202(5) Uani 1 1 d
C6 C 0.0798(3) 0.8413(2) 0.79804(16) 0.0242(5) Uani 1 1 d
C7 C -0.0051(3) 0.8117(2) 0.75511(19) 0.0287(6) Uani 1 1 d
C8 C 0.0363(4) 0.8217(3) 0.69218(18) 0.0356(8) Uani 1 1 d
C9 C 0.1473(4) 0.8573(3) 0.69590(18) 0.0344(8) Uani 1 1 d
C10 C 0.1744(3) 0.8698(2) 0.76163(18) 0.0282(6) Uani 1 1 d
C11 C 0.1785(3) 0.5053(3) 1.01954(16) 0.0319(7) Uani 1 1 d
C12 C 0.3574(3) 0.5548(2) 0.93419(15) 0.0254(5) Uani 1 1 d
C13 C 0.3282(3) 0.6730(3) 1.04657(15) 0.0255(5) Uani 1 1 d
C14 C 0.1033(3) 0.7198(3) 1.01505(16) 0.0314(7) Uani 1 1 d
C15 C 0.2742(3) 0.7664(2) 0.92592(14) 0.0248(5) Uani 1 1 d
H1P1 H 0.056(3) 0.498(3) 0.8873(17) 0.020(9) Uiso 1 1 d
H2 H 0.007(4) 0.552(3) 0.745(2) 0.032(11) Uiso 1 1 d
H2P1 H 0.006(4) 0.631(3) 0.881(2) 0.035(12) Uiso 1 1 d
H3 H 0.121(3) 0.580(3) 0.6456(18) 0.021(9) Uiso 1 1 d
H4 H 0.312(4) 0.642(3) 0.680(2) 0.034(11) Uiso 1 1 d
H5 H 0.317(3) 0.651(3) 0.8032(18) 0.021(9) Uiso 1 1 d
H6 H 0.070(4) 0.841(3) 0.842(2) 0.031(11) Uiso 1 1 d
H7 H -0.069(4) 0.790(3) 0.767(2) 0.037(12) Uiso 1 1 d
H8 H 0.002(4) 0.807(4) 0.661(2) 0.039(13) Uiso 1 1 d
H9 H 0.185(4) 0.866(3) 0.663(2) 0.033(11) Uiso 1 1 d
H10 H 0.239(4) 0.889(3) 0.777(2) 0.034(12) Uiso 1 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -0.849 6.8722 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 -29 0.0329
1 0 29 0.042
9 -16 -1 0.1308
-11 14 2 0.0921
-16 -6 1 0.1104
15 9 1 0.1008
17 2 -4 0.1163
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C13 W1 C15 90.19(13)
C13 W1 C14 89.22(13)
C15 W1 C14 88.03(14)
C13 W1 C11 90.60(14)
C15 W1 C11 179.15(14)
C14 W1 C11 91.66(15)
C13 W1 C12 88.01(13)
C15 W1 C12 91.62(13)
C14 W1 C12 177.21(13)
C11 W1 C12 88.73(14)
C13 W1 P1 179.48(10)
C15 W1 P1 90.30(9)
C14 W1 P1 90.64(10)
C11 W1 P1 88.91(11)
C12 W1 P1 92.13(9)
C1 Fe1 C2 41.14(11)
C1 Fe1 C5 41.49(11)
C2 Fe1 C5 69.13(12)
C1 Fe1 C9 167.40(15)
C2 Fe1 C9 150.43(15)
C5 Fe1 C9 128.52(15)
C1 Fe1 C8 150.79(15)
C2 Fe1 C8 117.13(15)
C5 Fe1 C8 166.39(15)
C9 Fe1 C8 40.47(17)
C1 Fe1 C7 117.83(13)
C2 Fe1 C7 107.91(13)
C5 Fe1 C7 152.18(14)
C9 Fe1 C7 67.91(15)
C8 Fe1 C7 40.23(16)
C1 Fe1 C6 108.62(12)
C2 Fe1 C6 128.93(13)
C5 Fe1 C6 119.01(12)
C9 Fe1 C6 67.85(14)
C8 Fe1 C6 67.63(14)
C7 Fe1 C6 40.21(14)
C1 Fe1 C10 129.17(13)
C2 Fe1 C10 167.40(14)
C5 Fe1 C10 108.73(13)
C9 Fe1 C10 40.45(15)
C8 Fe1 C10 67.90(15)
C7 Fe1 C10 67.83(14)
C6 Fe1 C10 40.33(13)
C1 Fe1 C4 68.94(12)
C2 Fe1 C4 68.47(13)
C5 Fe1 C4 40.57(12)
C9 Fe1 C4 108.17(14)
C8 Fe1 C4 128.27(15)
C7 Fe1 C4 166.08(14)
C6 Fe1 C4 152.23(13)
C10 Fe1 C4 118.54(13)
C1 Fe1 C3 68.77(12)
C2 Fe1 C3 40.56(13)
C5 Fe1 C3 68.46(12)
C9 Fe1 C3 117.56(14)
C8 Fe1 C3 107.76(14)
C7 Fe1 C3 128.24(14)
C6 Fe1 C3 166.50(14)
C10 Fe1 C3 151.32(14)
C4 Fe1 C3 40.48(13)
C1 P1 W1 121.69(9)
C1 P1 H1P1 104.0(16)
W1 P1 H1P1 113.9(16)
C1 P1 H2P1 105(2)
W1 P1 H2P1 117(2)
H1P1 P1 H2P1 91(2)
C2 C1 C5 107.4(3)
C2 C1 P1 125.6(2)
C5 C1 P1 126.9(2)
C2 C1 Fe1 69.80(16)
C5 C1 Fe1 69.64(16)
P1 C1 Fe1 123.70(14)
C3 C2 C1 108.2(3)
C3 C2 Fe1 70.47(17)
C1 C2 Fe1 69.06(15)
C3 C2 H2 125(3)
C1 C2 H2 126(3)
Fe1 C2 H2 122(3)
C2 C3 C4 108.2(3)
C2 C3 Fe1 68.97(16)
C4 C3 Fe1 69.67(17)
C2 C3 H3 126(2)
C4 C3 H3 126(2)
Fe1 C3 H3 125(2)
C5 C4 C3 108.3(3)
C5 C4 Fe1 69.07(16)
C3 C4 Fe1 69.84(17)
C5 C4 H4 127(3)
C3 C4 H4 125(3)
Fe1 C4 H4 125(3)
C4 C5 C1 107.8(3)
C4 C5 Fe1 70.36(17)
C1 C5 Fe1 68.87(15)
C4 C5 H5 126(2)
C1 C5 H5 126(2)
Fe1 C5 H5 123(2)
C7 C6 C10 108.2(3)
C7 C6 Fe1 69.79(18)
C10 C6 Fe1 69.85(17)
C7 C6 H6 122(3)
C10 C6 H6 130(3)
Fe1 C6 H6 127(3)
C8 C7 C6 108.0(3)
C8 C7 Fe1 69.6(2)
C6 C7 Fe1 70.00(18)
C8 C7 H7 128(3)
C6 C7 H7 124(3)
Fe1 C7 H7 124(3)
C7 C8 C9 108.2(3)
C7 C8 Fe1 70.12(19)
C9 C8 Fe1 69.7(2)
C7 C8 H8 125(3)
C9 C8 H8 127(3)
Fe1 C8 H8 124(3)
C8 C9 C10 107.9(3)
C8 C9 Fe1 69.8(2)
C10 C9 Fe1 70.15(18)
C8 C9 H9 121(3)
C10 C9 H9 131(3)
Fe1 C9 H9 124(3)
C6 C10 C9 107.7(3)
C6 C10 Fe1 69.81(17)
C9 C10 Fe1 69.39(19)
C6 C10 H10 127(3)
C9 C10 H10 126(3)
Fe1 C10 H10 124(3)
O1 C11 W1 178.5(4)
O2 C12 W1 176.7(3)
O3 C13 W1 179.7(3)
O4 C14 W1 176.6(4)
O5 C15 W1 178.0(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 C13 2.010(3)
W1 C15 2.035(3)
W1 C14 2.043(3)
W1 C11 2.043(3)
W1 C12 2.051(3)
W1 P1 2.5112(8)
Fe1 C1 2.032(3)
Fe1 C2 2.042(3)
Fe1 C5 2.042(3)
Fe1 C9 2.044(3)
Fe1 C8 2.045(3)
Fe1 C7 2.051(3)
Fe1 C6 2.054(3)
Fe1 C10 2.054(3)
Fe1 C4 2.060(3)
Fe1 C3 2.062(3)
P1 C1 1.800(3)
P1 H1P1 1.30(4)
P1 H2P1 1.26(4)
O1 C11 1.136(4)
O2 C12 1.134(4)
O3 C13 1.143(4)
O4 C14 1.136(4)
O5 C15 1.139(4)
C1 C2 1.432(4)
C1 C5 1.443(4)
C2 C3 1.423(5)
C2 H2 0.90(4)
C3 C4 1.426(5)
C3 H3 0.95(4)
C4 C5 1.422(4)
C4 H4 0.96(4)
C5 H5 0.98(4)
C6 C7 1.411(5)
C6 C10 1.416(5)
C6 H6 0.93(4)
C7 C8 1.409(6)
C7 H7 0.85(5)
C8 C9 1.414(6)
C8 H8 0.80(5)
C9 C10 1.417(5)
C9 H9 0.83(5)
C10 H10 0.87(5)
