#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:01:52 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178799 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/53/4105309.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_4105309
loop_
_publ_author_name
'Heather A. Spinney'
'Nicholas A. Piro'
'Christopher C. Cummins'
_publ_section_title
;
 Triple-Bond Reactivity of an AsP Complex Intermediate: Synthesis Stemming
 from Molecular Arsenic, As4
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16233
_journal_page_last               16243
_journal_paper_doi               10.1021/ja906550h
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C17 H16 As O5 P W'
_chemical_formula_weight         590.04
_chemical_name_common            'AsPW(CO)5 Cyclohexadiene Trap'
_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                 109.567(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8402(16)
_cell_length_b                   9.0940(10)
_cell_length_c                   15.3767(17)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.68
_cell_measurement_theta_min      2.64
_cell_volume                     1823.6(4)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_data_collection       'APEX2 3.0 (Bruker-AXS, 2008)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi 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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47759
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    8.247
_exptl_absorpt_correction_T_max  0.6832
_exptl_absorpt_correction_T_min  0.1911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.149
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.929
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0155
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0136P)²+1.8718P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0351
_refine_ls_wR_factor_ref         0.0362
_reflns_number_gt                4974
_reflns_number_total             5327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906550h_si_001_3.cif
_cod_data_source_block           07161
_cod_database_code               4105309
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
W1 W 0.851619(6) 0.737412(8) 0.864877(5) 0.01419(3) Uani 1 1 d .
C1 C 0.92548(18) 0.9308(2) 0.88664(14) 0.0228(4) Uani 1 1 d .
O1 O 0.96844(15) 1.04011(18) 0.89821(11) 0.0343(4) Uani 1 1 d .
C2 C 0.93151(15) 0.6731(2) 0.99640(14) 0.0168(4) Uani 1 1 d .
O2 O 0.97270(12) 0.63795(16) 1.07103(10) 0.0224(3) Uani 1 1 d .
C3 C 0.74238(16) 0.8141(2) 0.91453(14) 0.0187(4) Uani 1 1 d .
O3 O 0.68182(13) 0.85641(18) 0.94400(12) 0.0291(3) Uani 1 1 d .
C4 C 0.76040(17) 0.8035(2) 0.73684(14) 0.0202(4) Uani 1 1 d .
O4 O 0.70615(13) 0.84242(18) 0.66684(11) 0.0289(4) Uani 1 1 d .
C5 C 0.96432(17) 0.6596(2) 0.81748(14) 0.0210(4) Uani 1 1 d .
O5 O 1.02914(13) 0.6206(2) 0.79328(12) 0.0328(4) Uani 1 1 d .
As1 As 0.590200(15) 0.48498(2) 0.776248(13) 0.01605(4) Uani 1 1 d .
P1 P 0.76644(4) 0.48621(5) 0.83649(3) 0.01216(8) Uani 1 1 d .
C11 C 0.79729(15) 0.3698(2) 0.74739(13) 0.0155(3) Uani 1 1 d .
H11 H 0.8733 0.3568 0.7659 0.019 Uiso 1 1 calc R
C12 C 0.75796(16) 0.4521(2) 0.65404(13) 0.0187(4) Uani 1 1 d .
H12A H 0.7843 0.5542 0.6629 0.022 Uiso 1 1 calc R
H12B H 0.7854 0.4034 0.6096 0.022 Uiso 1 1 calc R
C13 C 0.63987(16) 0.4558(2) 0.61313(14) 0.0208(4) Uani 1 1 d .
H13A H 0.6181 0.4224 0.5482 0.025 Uiso 1 1 calc R
H13B H 0.6160 0.5584 0.6136 0.025 Uiso 1 1 calc R
C14 C 0.58880(16) 0.3572(2) 0.66762(13) 0.0193(4) Uani 1 1 d .
H14 H 0.5163 0.3360 0.6286 0.023 Uiso 1 1 calc R
C15 C 0.64554(17) 0.2175(2) 0.69519(13) 0.0193(4) Uani 1 1 d .
H15 H 0.6103 0.1260 0.6847 0.023 Uiso 1 1 calc R
C16 C 0.74702(16) 0.2225(2) 0.73498(13) 0.0174(4) Uani 1 1 d .
H16 H 0.7860 0.1353 0.7548 0.021 Uiso 1 1 calc R
C21 C 0.78453(14) 0.3748(2) 0.94432(12) 0.0140(3) Uani 1 1 d .
H21 H 0.8595 0.3643 0.9791 0.017 Uiso 1 1 calc R
C22 C 0.73334(15) 0.4601(2) 1.00448(13) 0.0166(3) Uani 1 1 d .
H22A H 0.7571 0.4185 1.0676 0.020 Uiso 1 1 calc R
H22B H 0.7555 0.5641 1.0088 0.020 Uiso 1 1 calc R
C23 C 0.61531(16) 0.4539(2) 0.96575(14) 0.0209(4) Uani 1 1 d .
H23A H 0.5881 0.5548 0.9502 0.025 Uiso 1 1 calc R
H23B H 0.5893 0.4152 1.0139 0.025 Uiso 1 1 calc R
C24 C 0.57529(16) 0.3561(2) 0.87887(14) 0.0199(4) Uani 1 1 d .
H24 H 0.5012 0.3330 0.8663 0.024 Uiso 1 1 calc R
C25 C 0.63479(17) 0.2178(2) 0.89224(13) 0.0199(4) Uani 1 1 d .
H25 H 0.6010 0.1254 0.8783 0.024 Uiso 1 1 calc R
C26 C 0.73723(16) 0.2258(2) 0.92445(13) 0.0168(4) Uani 1 1 d .
H26 H 0.7783 0.1397 0.9343 0.020 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'
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'
As As 0.0499 2.0058 '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
C1 W1 C3 92.19(9)
C1 W1 C2 90.53(8)
C3 W1 C2 87.15(8)
C1 W1 C4 91.08(8)
C3 W1 C4 87.92(8)
C2 W1 C4 174.87(8)
C1 W1 C5 87.47(9)
C3 W1 C5 178.77(8)
C2 W1 C5 91.67(8)
C4 W1 C5 93.27(8)
C1 W1 P1 176.99(7)
C3 W1 P1 90.70(6)
C2 W1 P1 88.78(5)
C4 W1 P1 89.86(6)
C5 W1 P1 89.61(6)
O1 C1 W1 178.9(2)
O2 C2 W1 177.17(17)
O3 C3 W1 178.81(19)
O4 C4 W1 176.97(19)
O5 C5 W1 177.38(19)
C14 As1 C24 109.49(8)
C14 As1 P1 92.91(6)
C24 As1 P1 93.43(6)
C21 P1 C11 109.91(8)
C21 P1 As1 99.32(6)
C11 P1 As1 99.90(6)
C21 P1 W1 114.49(6)
C11 P1 W1 115.07(6)
As1 P1 W1 116.22(2)
C16 C11 C12 108.16(16)
C16 C11 P1 112.75(13)
C12 C11 P1 107.88(13)
C13 C12 C11 112.60(16)
C12 C13 C14 112.32(16)
C15 C14 C13 110.95(17)
C15 C14 As1 113.46(13)
C13 C14 As1 103.49(13)
C16 C15 C14 118.64(18)
C15 C16 C11 117.65(18)
C26 C21 C22 108.69(15)
C26 C21 P1 112.83(13)
C22 C21 P1 107.64(12)
C23 C22 C21 112.87(16)
C22 C23 C24 112.44(16)
C25 C24 C23 110.35(17)
C25 C24 As1 113.70(14)
C23 C24 As1 103.85(13)
C26 C25 C24 118.46(18)
C25 C26 C21 117.60(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 C1 2.005(2)
W1 C3 2.032(2)
W1 C2 2.039(2)
W1 C4 2.041(2)
W1 C5 2.056(2)
W1 P1 2.5405(5)
C1 O1 1.141(3)
C2 O2 1.143(2)
C3 O3 1.145(3)
C4 O4 1.143(3)
C5 O5 1.137(3)
As1 C14 2.029(2)
As1 C24 2.031(2)
As1 P1 2.3010(6)
P1 C21 1.8871(18)
P1 C11 1.8898(19)
C11 C16 1.493(3)
C11 C12 1.547(3)
C12 C13 1.543(3)
C13 C14 1.550(3)
C14 C15 1.479(3)
C15 C16 1.332(3)
C21 C26 1.491(3)
C21 C22 1.549(3)
C22 C23 1.541(3)
C23 C24 1.545(3)
C24 C25 1.480(3)
C25 C26 1.338(3)
