#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/19/7011911.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_7011911
loop_
_publ_author_name
'Gibson, Vernon C.'
'Long, Nicholas J.'
'White, Andrew J. P.'
'Williams, Charlotte K.'
'Williams, David J.'
'Fontani, Marco'
'Zanello, Piero'
_publ_section_title
;
 Synthesis, characterisation and catalytic activity of metal complexes
 of neutral, unsymmetrical P/S ferrocenediyl ligands
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3280
_journal_paper_doi               10.1039/b205653d
_journal_year                    2002
_chemical_formula_sum            'C27 H21 Fe O4 P S W'
_chemical_formula_weight         712.17
_chemical_name_systematic
; 
? 
;
_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           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.596(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5019(15)
_cell_length_b                   17.863(2)
_cell_length_c                   12.4460(14)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      4.68
_cell_volume                     2544.9(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4609
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        99.97
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.263
_exptl_absorpt_correction_T_max  0.7758
_exptl_absorpt_correction_T_min  0.3622
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Rhombs
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_description       Orange
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.074
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_obs          0.0323
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0314P)²+3.4332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0788
_refine_ls_wR_factor_obs         0.0714
_reflns_number_observed          3683
_reflns_number_total             4375
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b205653d.txt
_cod_data_source_block           NL0106
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+3.4332P] 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^)+(0.0314P)^2^+3.4332P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2545.0(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C27 H21 O4 P S Fe W'
_cod_database_code               7011911
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_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
_atom_site_disorder_group
W W 0.20491(2) 0.365209(13) 0.65168(2) 0.03143(10) Uani 1 d . .
Fe Fe 0.10281(7) 0.14985(4) 0.50661(6) 0.0287(2) Uani 1 d . .
S S 0.00017(13) 0.31441(8) 0.59604(11) 0.0330(3) Uani 1 d . .
P P 0.25972(12) 0.31267(8) 0.47400(11) 0.0266(3) Uani 1 d . .
C1 C -0.0067(5) 0.2163(3) 0.5836(5) 0.0332(12) Uani 1 d . .
C2 C -0.0701(5) 0.1781(4) 0.4954(5) 0.0387(14) Uani 1 d . .
H2A H -0.1126(5) 0.2001(4) 0.4363(5) 0.046 Uiso 1 calc R .
C3 C -0.0562(6) 0.1011(4) 0.5147(6) 0.047(2) Uani 1 d . .
H3A H -0.0875(6) 0.0632(4) 0.4696(6) 0.056 Uiso 1 calc R .
C4 C 0.0135(6) 0.0902(4) 0.6145(6) 0.049(2) Uani 1 d . .
H4A H 0.0344(6) 0.0445(4) 0.6465(6) 0.058 Uiso 1 calc R .
C5 C 0.0446(6) 0.1611(4) 0.6555(5) 0.0389(13) Uani 1 d . .
H5A H 0.0912(6) 0.1706(4) 0.7194(5) 0.047 Uiso 1 calc R .
C6 C 0.2343(4) 0.2130(3) 0.4524(4) 0.0279(11) Uani 1 d . .
C7 C 0.1684(5) 0.1777(4) 0.3638(5) 0.0345(12) Uani 1 d . .
H7A H 0.1285(5) 0.2018(4) 0.3051(5) 0.041 Uiso 1 calc R .
C8 C 0.1744(6) 0.0987(4) 0.3809(5) 0.0394(13) Uani 1 d . .
H8A H 0.1381(6) 0.0626(4) 0.3354(5) 0.047 Uiso 1 calc R .
C9 C 0.2441(5) 0.0847(3) 0.4775(6) 0.0394(13) Uani 1 d . .
H9A H 0.2636(5) 0.0378(3) 0.5061(6) 0.047 Uiso 1 calc R .
C10 C 0.2803(5) 0.1554(3) 0.5246(5) 0.0350(12) Uani 1 d . .
H10A H 0.3254(5) 0.1625(3) 0.5900(5) 0.042 Uiso 1 calc R .
C11 C -0.0967(7) 0.3301(5) 0.6999(6) 0.056(2) Uani 1 d . .
H11A H -0.1007(7) 0.3827(5) 0.7146(6) 0.083 Uiso 1 calc R .
H11B H -0.0674(7) 0.3041(5) 0.7645(6) 0.083 Uiso 1 calc R .
H11C H -0.1733(7) 0.3118(5) 0.6757(6) 0.083 Uiso 1 calc R .
C12 C 0.0780(3) 0.3811(3) 0.3456(3) 0.043(2) Uani 1 d G .
H12A H 0.0384(3) 0.3785(3) 0.4072(3) 0.051 Uiso 1 calc R .
C13 C 0.0240(3) 0.4127(3) 0.2516(3) 0.052(2) Uani 1 d G .
H13A H -0.0517(3) 0.4312(4) 0.2503(5) 0.063 Uiso 1 calc R .
C14 C 0.0831(4) 0.4167(3) 0.1595(3) 0.051(2) Uani 1 d G .
H14A H 0.0469(5) 0.4378(4) 0.0966(3) 0.061 Uiso 1 calc R .
C15 C 0.1962(4) 0.3890(3) 0.1614(3) 0.052(2) Uani 1 d G .
H15A H 0.2357(5) 0.3916(4) 0.0998(3) 0.062 Uiso 1 calc R .
C16 C 0.2502(3) 0.3574(3) 0.2554(3) 0.0430(14) Uani 1 d G .
H16A H 0.3259(3) 0.3389(4) 0.2567(4) 0.052 Uiso 1 calc R .
C17 C 0.1911(3) 0.3534(2) 0.3475(2) 0.0305(11) Uani 1 d G .
C18 C 0.4949(3) 0.2630(2) 0.4769(4) 0.048(2) Uani 1 d G .
H18A H 0.4664(3) 0.2152(2) 0.4874(4) 0.057 Uiso 1 calc R .
C19 C 0.6144(3) 0.2746(2) 0.4769(5) 0.060(2) Uani 1 d G .
H19A H 0.6658(4) 0.2345(3) 0.4874(7) 0.072 Uiso 1 calc R .
C20 C 0.6571(3) 0.3462(3) 0.4613(4) 0.048(2) Uani 1 d G .
H20A H 0.7370(3) 0.3540(3) 0.4613(6) 0.058 Uiso 1 calc R .
C21 C 0.5803(4) 0.4062(2) 0.4456(4) 0.053(2) Uani 1 d G .
H21A H 0.6088(5) 0.4541(2) 0.4352(6) 0.064 Uiso 1 calc R .
C22 C 0.4608(3) 0.3946(2) 0.4456(4) 0.046(2) Uani 1 d G .
H22A H 0.4094(4) 0.4347(2) 0.4352(6) 0.055 Uiso 1 calc R .
C23 C 0.4181(2) 0.3230(2) 0.4613(4) 0.0336(12) Uani 1 d G .
C24 C 0.3595(6) 0.4086(4) 0.6878(5) 0.0442(15) Uani 1 d . .
O24 O 0.4520(5) 0.4339(4) 0.7100(5) 0.075(2) Uani 1 d . .
C25 C 0.1608(7) 0.4033(4) 0.7921(5) 0.048(2) Uani 1 d . .
O25 O 0.1384(7) 0.4246(4) 0.8739(5) 0.079(2) Uani 1 d . .
C26 C 0.1555(5) 0.4646(3) 0.5787(6) 0.0386(13) Uani 1 d . .
O26 O 0.1357(5) 0.5205(3) 0.5408(6) 0.064(2) Uani 1 d . .
C27 C 0.2715(6) 0.2730(4) 0.7268(5) 0.0413(14) Uani 1 d . .
O27 O 0.3178(6) 0.2248(3) 0.7754(5) 0.063(2) 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'
S S 0.1246 0.1234 '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'
W W -0.8490 6.8722 '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
C24 W C25 88.1(3) . . ?
C24 W C27 85.4(3) . . ?
C25 W C27 89.4(3) . . ?
C24 W C26 88.0(3) . . ?
C25 W C26 90.6(3) . . ?
C27 W C26 173.4(3) . . ?
C24 W P 92.8(2) . . ?
C25 W P 178.3(2) . . ?
C27 W P 89.2(2) . . ?
C26 W P 90.9(2) . . ?
C24 W S 176.6(2) . . ?
C25 W S 93.0(2) . . ?
C27 W S 97.7(2) . . ?
C26 W S 88.8(2) . . ?
P W S 86.17(5) . . ?
C10 Fe C3 155.8(3) . . ?
C10 Fe C1 125.4(2) . . ?
C3 Fe C1 68.0(3) . . ?
C10 Fe C5 108.1(3) . . ?
C3 Fe C5 67.8(3) . . ?
C1 Fe C5 40.8(2) . . ?
C10 Fe C2 162.8(3) . . ?
C3 Fe C2 40.2(3) . . ?
C1 Fe C2 41.1(2) . . ?
C5 Fe C2 68.6(3) . . ?
C10 Fe C8 68.4(3) . . ?
C3 Fe C8 106.1(3) . . ?
C1 Fe C8 158.5(3) . . ?
C5 Fe C8 158.1(3) . . ?
C2 Fe C8 121.2(3) . . ?
C10 Fe C6 41.0(2) . . ?
C3 Fe C6 160.9(3) . . ?
C1 Fe C6 110.1(2) . . ?
C5 Fe C6 124.2(2) . . ?
C2 Fe C6 125.8(2) . . ?
C8 Fe C6 68.3(2) . . ?
C10 Fe C7 68.6(2) . . ?
C3 Fe C7 123.5(3) . . ?
C1 Fe C7 124.1(3) . . ?
C5 Fe C7 160.2(3) . . ?
C2 Fe C7 108.5(3) . . ?
C8 Fe C7 40.6(2) . . ?
C6 Fe C7 40.5(2) . . ?
C10 Fe C9 41.1(2) . . ?
C3 Fe C9 119.7(3) . . ?
C1 Fe C9 161.2(3) . . ?
C5 Fe C9 123.4(3) . . ?
C2 Fe C9 155.1(3) . . ?
C8 Fe C9 39.8(3) . . ?
C6 Fe C9 68.5(2) . . ?
C7 Fe C9 67.8(3) . . ?
C10 Fe C4 120.8(3) . . ?
C3 Fe C4 40.6(3) . . ?
C1 Fe C4 68.0(3) . . ?
C5 Fe C4 39.8(3) . . ?
C2 Fe C4 68.2(3) . . ?
C8 Fe C4 121.9(3) . . ?
C6 Fe C4 157.9(3) . . ?
C7 Fe C4 159.0(3) . . ?
C9 Fe C4 105.9(3) . . ?
C1 S C11 101.0(3) . . ?
C1 S W 114.2(2) . . ?
C11 S W 111.5(3) . . ?
C6 P C17 102.2(2) . . ?
C6 P C23 103.3(2) . . ?
C17 P C23 103.3(2) . . ?
C6 P W 116.1(2) . . ?
C17 P W 118.47(13) . . ?
C23 P W 111.5(2) . . ?
C5 C1 C2 107.6(6) . . ?
C5 C1 S 128.5(5) . . ?
C2 C1 S 123.9(5) . . ?
C5 C1 Fe 69.8(4) . . ?
C2 C1 Fe 69.7(4) . . ?
S C1 Fe 126.6(3) . . ?
C3 C2 C1 107.1(6) . . ?
C3 C2 Fe 69.6(4) . . ?
C1 C2 Fe 69.2(3) . . ?
C2 C3 C4 109.2(6) . . ?
C2 C3 Fe 70.2(4) . . ?
C4 C3 Fe 70.7(4) . . ?
C5 C4 C3 107.2(6) . . ?
C5 C4 Fe 69.2(4) . . ?
C3 C4 Fe 68.6(4) . . ?
C4 C5 C1 108.8(6) . . ?
C4 C5 Fe 71.0(4) . . ?
C1 C5 Fe 69.5(3) . . ?
C7 C6 C10 107.7(5) . . ?
C7 C6 P 127.9(5) . . ?
C10 C6 P 124.5(4) . . ?
C7 C6 Fe 70.0(3) . . ?
C10 C6 Fe 68.8(3) . . ?
P C6 Fe 127.0(3) . . ?
C6 C7 C8 108.0(6) . . ?
C6 C7 Fe 69.5(3) . . ?
C8 C7 Fe 69.5(3) . . ?
C9 C8 C7 108.6(5) . . ?
C9 C8 Fe 70.3(4) . . ?
C7 C8 Fe 69.9(3) . . ?
C8 C9 C10 108.2(5) . . ?
C8 C9 Fe 69.8(4) . . ?
C10 C9 Fe 68.5(3) . . ?
C6 C10 C9 107.5(5) . . ?
C6 C10 Fe 70.2(3) . . ?
C9 C10 Fe 70.4(3) . . ?
C13 C12 C17 120.0 . . ?
C12 C13 C14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C17 120.0 . . ?
C16 C17 C12 120.0 . . ?
C16 C17 P 121.5(2) . . ?
C12 C17 P 118.5(2) . . ?
C19 C18 C23 120.0 . . ?
C20 C19 C18 120.0 . . ?
C19 C20 C21 120.0 . . ?
C22 C21 C20 120.0 . . ?
C21 C22 C23 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 P 117.9(2) . . ?
C18 C23 P 121.9(2) . . ?
O24 C24 W 179.4(6) . . ?
O25 C25 W 178.2(7) . . ?
O26 C26 W 175.5(6) . . ?
O27 C27 W 173.2(6) . . ?
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
W C24 1.952(7) . ?
W C25 1.986(6) . ?
W C27 2.008(7) . ?
W C26 2.050(7) . ?
W P 2.5378(14) . ?
W S 2.555(2) . ?
Fe C10 2.034(6) . ?
Fe C3 2.037(6) . ?
Fe C1 2.037(6) . ?
Fe C5 2.041(6) . ?
Fe C2 2.044(6) . ?
Fe C8 2.053(6) . ?
Fe C6 2.053(5) . ?
Fe C7 2.059(6) . ?
Fe C9 2.059(6) . ?
Fe C4 2.065(6) . ?
S C1 1.760(6) . ?
S C11 1.809(6) . ?
P C6 1.820(6) . ?
P C17 1.841(3) . ?
P C23 1.853(3) . ?
C1 C5 1.421(9) . ?
C1 C2 1.431(9) . ?
C2 C3 1.402(10) . ?
C3 C4 1.424(11) . ?
C4 C5 1.399(10) . ?
C6 C7 1.424(8) . ?
C6 C10 1.433(8) . ?
C7 C8 1.427(9) . ?
C8 C9 1.401(10) . ?
C9 C10 1.437(8) . ?
C12 C13 1.39 . ?
C12 C17 1.39 . ?
C13 C14 1.39 . ?
C14 C15 1.39 . ?
C15 C16 1.39 . ?
C16 C17 1.39 . ?
C18 C19 1.39 . ?
C18 C23 1.39 . ?
C19 C20 1.39 . ?
C20 C21 1.39 . ?
C21 C22 1.39 . ?
C22 C23 1.39 . ?
C24 O24 1.164(9) . ?
C25 O25 1.140(9) . ?
C26 O26 1.118(8) . ?
C27 O27 1.153(9) . ?
