#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:24:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179842 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/38/7013835.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_7013835
loop_
_publ_author_name
'Weber, Lothar'
'Pumpenmeier, Lars'
'Stammler, Hans-Georg'
'Neumann, Beate'
_publ_section_title
;
 Synthesis, structure and reactivity of ferrio-chloro-phosphanes,
 -arsanes and -stibanes [(CO)2(eta5-C5Me5)FePn(Cl)R] (Pn = P, As, Sb);
 R = tetramethylcyclopentadienyl, 2,7-di-tert-butylfluorenyl,
 2,7-di-tert-butyl-9-trimethylsilylfluorenyl) as precursor to novel
 metallo-phosphaalkenes, -arsaalkenes, and -stibaalkenes.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              659
_journal_page_last               667
_journal_paper_doi               10.1039/b315221a
_journal_year                    2004
_chemical_formula_moiety         'C21 H28 As Cl Fe O2'
_chemical_formula_sum            'C21 H28 As Cl Fe O2'
_chemical_formula_weight         478.65
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 102.9860(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5320(2)
_cell_length_b                   13.3380(3)
_cell_length_c                   19.0760(4)
_cell_measurement_reflns_used    5063
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2115.33(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'KappaCCD '
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.064
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59514
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    2.404
_exptl_absorpt_correction_T_max  0.9100
_exptl_absorpt_correction_T_min  0.5325
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0294
_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)+(0.0436P)²+0.3558P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                4384
_reflns_number_total             4850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b315221a.txt
_cod_data_source_block           compound2b
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7013835
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'
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
As1 As 0.26867(5) 0.91959(2) 0.126269(15) 0.02327(10) Uani 0.9385(14) 1 d P A 1
As1B As 0.1858(8) 0.8851(4) 0.1195(3) 0.0264(16) Uiso 0.0615(14) 1 d P A 2
Fe1 Fe 0.31451(5) 0.79596(3) 0.217527(19) 0.02273(10) Uani 1 1 d . . .
Cl1 Cl 0.00397(10) 0.95637(6) 0.10622(4) 0.03685(19) Uani 0.9385(14) 1 d P A 1
Cl1B Cl 0.3408(16) 1.0239(9) 0.1291(7) 0.041(3) Uiso 0.0615(14) 1 d P A 2
O1 O 0.0888(3) 0.64703(19) 0.14282(12) 0.0484(6) Uani 1 1 d . . .
O2 O 0.6114(3) 0.72858(17) 0.18290(11) 0.0389(5) Uani 1 1 d . . .
C1 C 0.2636(4) 0.9100(2) 0.28869(14) 0.0276(6) Uani 1 1 d . A .
C2 C 0.1736(3) 0.8217(2) 0.29332(13) 0.0283(6) Uani 1 1 d . A .
C3 C 0.2863(4) 0.7410(2) 0.31757(14) 0.0291(6) Uani 1 1 d . A .
C4 C 0.4435(4) 0.7793(2) 0.32540(13) 0.0268(6) Uani 1 1 d . A .
C5 C 0.4300(4) 0.8844(2) 0.30625(14) 0.0273(6) Uani 1 1 d . A .
C6 C 0.1970(4) 1.0139(2) 0.27644(16) 0.0376(7) Uani 1 1 d . . .
H6A H 0.1903 1.0437 0.3226 0.056 Uiso 1 1 calc R A .
H6B H 0.0894 1.0112 0.2447 0.056 Uiso 1 1 calc R . .
H6C H 0.2677 1.0547 0.2540 0.056 Uiso 1 1 calc R . .
C7 C -0.0059(4) 0.8142(3) 0.28298(17) 0.0402(7) Uani 1 1 d . . .
H7A H -0.0363 0.8308 0.3282 0.060 Uiso 1 1 calc R A .
H7B H -0.0406 0.7458 0.2686 0.060 Uiso 1 1 calc R . .
H7C H -0.0577 0.8613 0.2454 0.060 Uiso 1 1 calc R . .
C8 C 0.2451(4) 0.6361(2) 0.33557(16) 0.0388(8) Uani 1 1 d . . .
H8A H 0.2402 0.6327 0.3864 0.058 Uiso 1 1 calc R A .
H8B H 0.3277 0.5898 0.3267 0.058 Uiso 1 1 calc R . .
H8C H 0.1404 0.6173 0.3054 0.058 Uiso 1 1 calc R . .
C9 C 0.5974(4) 0.7230(2) 0.35429(15) 0.0366(7) Uani 1 1 d . . .
H9A H 0.6273 0.7297 0.4068 0.055 Uiso 1 1 calc R A .
H9B H 0.6832 0.7506 0.3334 0.055 Uiso 1 1 calc R . .
H9C H 0.5819 0.6519 0.3415 0.055 Uiso 1 1 calc R . .
C10 C 0.5669(4) 0.9565(2) 0.31030(17) 0.0377(7) Uani 1 1 d . . .
H10A H 0.5953 0.9863 0.3585 0.057 Uiso 1 1 calc R A .
H10B H 0.5346 1.0096 0.2744 0.057 Uiso 1 1 calc R . .
H10C H 0.6601 0.9207 0.3006 0.057 Uiso 1 1 calc R . .
C11 C 0.1789(4) 0.7073(2) 0.16787(14) 0.0324(7) Uani 1 1 d . A .
C12 C 0.4894(4) 0.7559(2) 0.19147(14) 0.0273(6) Uani 1 1 d . A .
C13 C 0.2606(3) 0.8581(2) 0.02814(14) 0.0267(6) Uani 1 1 d . . .
H13A H 0.2351 0.9116 -0.0094 0.032 Uiso 1 1 calc R A 1
C14 C 0.1536(4) 0.7702(2) 0.00511(14) 0.0283(6) Uani 1 1 d . A .
C15 C 0.2472(3) 0.6897(2) 0.00057(13) 0.0257(6) Uani 1 1 d . . .
C16 C 0.4169(3) 0.7193(2) 0.01770(13) 0.0260(6) Uani 1 1 d . A .
C17 C 0.4271(3) 0.8192(2) 0.03162(14) 0.0260(6) Uani 1 1 d . A .
C18 C -0.0281(4) 0.7736(2) -0.01290(17) 0.0375(7) Uani 1 1 d . . .
H18A H -0.0707 0.7065 -0.0269 0.056 Uiso 1 1 calc R A .
H18B H -0.0655 0.8203 -0.0528 0.056 Uiso 1 1 calc R . .
H18C H -0.0660 0.7961 0.0293 0.056 Uiso 1 1 calc R . .
C19 C 0.1930(4) 0.5833(2) -0.01892(16) 0.0344(6) Uani 1 1 d . A .
H19A H 0.0754 0.5798 -0.0280 0.052 Uiso 1 1 calc R . .
H19B H 0.2401 0.5384 0.0209 0.052 Uiso 1 1 calc R . .
H19C H 0.2282 0.5629 -0.0623 0.052 Uiso 1 1 calc R . .
C20 C 0.5518(4) 0.6463(2) 0.01929(15) 0.0313(6) Uani 1 1 d . . .
H20A H 0.6549 0.6819 0.0317 0.047 Uiso 1 1 calc R A .
H20B H 0.5394 0.6151 -0.0282 0.047 Uiso 1 1 calc R . .
H20C H 0.5491 0.5944 0.0553 0.047 Uiso 1 1 calc R . .
C21 C 0.5767(4) 0.8823(2) 0.04956(16) 0.0327(6) Uani 1 1 d . . .
H21A H 0.6706 0.8407 0.0482 0.049 Uiso 1 1 calc R A .
H21B H 0.5883 0.9109 0.0978 0.049 Uiso 1 1 calc R . .
H21C H 0.5686 0.9367 0.0143 0.049 Uiso 1 1 calc R . .
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 As1 Cl1 96.09(8) . . ?
C13 As1 Fe1 111.26(8) . . ?
Cl1 As1 Fe1 105.65(3) . . ?
C13 As1B Cl1B 85.6(4) . . ?
C13 As1B Fe1 115.3(2) . . ?
Cl1B As1B Fe1 101.3(4) . . ?
C12 Fe1 C11 98.02(13) . . ?
C12 Fe1 C2 153.53(12) . . ?
C11 Fe1 C2 94.06(12) . . ?
C12 Fe1 C3 115.28(12) . . ?
C11 Fe1 C3 93.35(12) . . ?
C2 Fe1 C3 40.18(11) . . ?
C12 Fe1 C5 97.08(12) . . ?
C11 Fe1 C5 158.46(12) . . ?
C2 Fe1 C5 66.12(11) . . ?
C3 Fe1 C5 66.24(11) . . ?
C12 Fe1 C4 87.36(12) . . ?
C11 Fe1 C4 125.75(12) . . ?
C2 Fe1 C4 66.54(11) . . ?
C3 Fe1 C4 39.05(11) . . ?
C5 Fe1 C4 39.98(10) . . ?
C12 Fe1 C1 134.34(12) . . ?
C11 Fe1 C1 127.60(13) . . ?
C2 Fe1 C1 39.01(11) . . ?
C3 Fe1 C1 66.02(10) . . ?
C5 Fe1 C1 39.04(11) . . ?
C4 Fe1 C1 66.07(10) . . ?
C12 Fe1 As1B 102.11(17) . . ?
C11 Fe1 As1B 76.9(2) . . ?
C2 Fe1 As1B 103.54(15) . . ?
C3 Fe1 As1B 142.38(17) . . ?
C5 Fe1 As1B 114.67(17) . . ?
C4 Fe1 As1B 154.45(16) . . ?
C1 Fe1 As1B 91.17(15) . . ?
C12 Fe1 As1 90.82(9) . . ?
C11 Fe1 As1 95.25(9) . . ?
C2 Fe1 As1 111.48(8) . . ?
C3 Fe1 As1 151.03(8) . . ?
C5 Fe1 As1 99.80(8) . . ?
C4 Fe1 As1 138.82(8) . . ?
C1 Fe1 As1 87.01(7) . . ?
As1B Fe1 As1 20.46(18) . . ?
C2 C1 C5 108.1(2) . . ?
C2 C1 C6 125.9(3) . . ?
C5 C1 C6 125.6(3) . . ?
C2 C1 Fe1 68.93(15) . . ?
C5 C1 Fe1 69.30(15) . . ?
C6 C1 Fe1 132.93(19) . . ?
C1 C2 C3 107.9(2) . . ?
C1 C2 C7 126.6(3) . . ?
C3 C2 C7 125.2(3) . . ?
C1 C2 Fe1 72.06(15) . . ?
C3 C2 Fe1 69.98(15) . . ?
C7 C2 Fe1 128.4(2) . . ?
C4 C3 C2 108.2(2) . . ?
C4 C3 C8 125.4(3) . . ?
C2 C3 C8 126.4(3) . . ?
C4 C3 Fe1 70.78(15) . . ?
C2 C3 Fe1 69.84(14) . . ?
C8 C3 Fe1 127.69(19) . . ?
C3 C4 C5 107.7(2) . . ?
C3 C4 C9 126.0(3) . . ?
C5 C4 C9 126.1(3) . . ?
C3 C4 Fe1 70.17(16) . . ?
C5 C4 Fe1 70.01(15) . . ?
C9 C4 Fe1 128.94(19) . . ?
C1 C5 C4 108.1(2) . . ?
C1 C5 C10 125.5(3) . . ?
C4 C5 C10 126.2(3) . . ?
C1 C5 Fe1 71.66(15) . . ?
C4 C5 Fe1 70.01(15) . . ?
C10 C5 Fe1 127.97(19) . . ?
O1 C11 Fe1 172.7(2) . . ?
O2 C12 Fe1 172.0(2) . . ?
C14 C13 C17 104.6(2) . . ?
C14 C13 As1B 95.9(3) . . ?
C17 C13 As1B 120.2(2) . . ?
C14 C13 As1 118.77(18) . . ?
C17 C13 As1 105.27(17) . . ?
As1B C13 As1 23.6(2) . . ?
C15 C14 C13 108.2(2) . . ?
C15 C14 C18 126.8(3) . . ?
C13 C14 C18 125.0(3) . . ?
C14 C15 C16 109.8(2) . . ?
C14 C15 C19 127.4(3) . . ?
C16 C15 C19 122.7(2) . . ?
C17 C16 C15 109.0(2) . . ?
C17 C16 C20 128.1(3) . . ?
C15 C16 C20 122.9(2) . . ?
C16 C17 C13 108.2(2) . . ?
C16 C17 C21 127.5(3) . . ?
C13 C17 C21 124.3(2) . . ?
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
As1 C13 2.031(3) . ?
As1 Cl1 2.2581(9) . ?
As1 Fe1 2.3658(4) . ?
As1B C13 2.019(6) . ?
As1B Cl1B 2.259(15) . ?
As1B Fe1 2.279(5) . ?
Fe1 C12 1.758(3) . ?
Fe1 C11 1.772(3) . ?
Fe1 C2 2.106(3) . ?
Fe1 C3 2.108(3) . ?
Fe1 C5 2.116(3) . ?
Fe1 C4 2.116(3) . ?
Fe1 C1 2.147(3) . ?
O1 C11 1.141(4) . ?
O2 C12 1.149(3) . ?
C1 C2 1.421(4) . ?
C1 C5 1.425(4) . ?
C1 C6 1.495(4) . ?
C2 C3 1.448(4) . ?
C2 C7 1.502(4) . ?
C3 C4 1.412(4) . ?
C3 C8 1.501(4) . ?
C4 C5 1.447(4) . ?
C4 C9 1.506(4) . ?
C5 C10 1.502(4) . ?
C13 C14 1.490(4) . ?
C13 C17 1.500(4) . ?
C14 C15 1.354(4) . ?
C14 C18 1.511(4) . ?
C15 C16 1.465(4) . ?
C15 C19 1.512(4) . ?
C16 C17 1.357(4) . ?
C16 C20 1.502(4) . ?
C17 C21 1.503(4) . ?
