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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/91/1519119.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_1519119
loop_
_publ_author_name
'Baker, Paul K.'
'Hursthouse, Michael B.'
_publ_section_title
;
 C24H20AsI2NO3W
;
_journal_name_full               'Crystal Structure Report Archive'
_journal_page_first              1184
_journal_year                    1992
_chemical_formula_moiety         'C24 H20 As I2 N O3 W'
_chemical_formula_sum            'C24 H20 As I2 N O3 W'
_chemical_formula_weight         882.98
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 105.335(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.465(3)
_cell_length_b                   11.129(2)
_cell_length_c                   20.950(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2577.9(9)
_computing_cell_refinement       REFINE
_computing_data_collection       'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_data_reduction        'ABSURD (Karaulov, 1992)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution
'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_sigmaI/netI    0.1358
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9636
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    8.175
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            unk
_exptl_crystal_density_diffrn    2.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unk
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.200
_refine_diff_density_min         -5.987
_refine_diff_density_rms         0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                3840
_reflns_number_total             4428
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            eCrystal-1184.cif
_cod_data_source_block           92src179
_cod_depositor_comments
;
Citation :
Baker, Paul K. and Hursthouse, Michael B. (1992) 
University of Southampton, Crystal Structure Report Archive. 
(doi:10.5258/ecrystals/1184)
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1519119
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
W1 W 0.46727(3) 0.23778(3) 0.130286(19) 0.01198(14) Uani 1 1 d . . .
I1 I 0.34567(6) 0.02275(6) 0.15138(3) 0.02063(19) Uani 1 1 d . . .
I2 I 0.67604(6) 0.15437(8) 0.22701(4) 0.0331(2) Uani 1 1 d . . .
As1 As 0.24445(8) 0.31171(8) 0.07506(5) 0.0108(2) Uani 1 1 d . . .
O1 O 0.5863(7) 0.0496(8) 0.0557(4) 0.034(2) Uani 1 1 d . . .
O2 O 0.4543(7) 0.3449(8) -0.0093(4) 0.033(2) Uani 1 1 d . . .
O3 O 0.6444(9) 0.4586(10) 0.1542(6) 0.060(3) Uani 1 1 d . . .
C1 C 0.2017(9) 0.1269(9) -0.0258(5) 0.019(2) Uani 1 1 d . . .
H1 H 0.2797 0.1020 -0.0045 0.023 Uiso 1 1 calc R . .
C2 C 0.1345(10) 0.0650(10) -0.0809(5) 0.025(2) Uani 1 1 d . . .
H2 H 0.1676 -0.0019 -0.0962 0.030 Uiso 1 1 calc R . .
C3 C 0.0193(9) 0.1020(10) -0.1129(5) 0.020(2) Uani 1 1 d . . .
H3 H -0.0248 0.0604 -0.1500 0.024 Uiso 1 1 calc R . .
C4 C -0.0310(9) 0.2005(11) -0.0903(6) 0.027(3) Uani 1 1 d . . .
H4 H -0.1090 0.2253 -0.1119 0.033 Uiso 1 1 calc R . .
C5 C 0.0371(9) 0.2638(10) -0.0338(6) 0.022(2) Uani 1 1 d . . .
H5 H 0.0040 0.3302 -0.0181 0.026 Uiso 1 1 calc R . .
C6 C 0.1517(8) 0.2264(9) -0.0026(5) 0.014(2) Uani 1 1 d . . .
C7 C 0.0714(9) 0.2191(9) 0.1404(5) 0.019(2) Uani 1 1 d . . .
H7 H 0.0892 0.1463 0.1233 0.023 Uiso 1 1 calc R . .
C8 C -0.0124(9) 0.2220(11) 0.1774(6) 0.025(2) Uani 1 1 d . . .
H8 H -0.0511 0.1522 0.1851 0.031 Uiso 1 1 calc R . .
C9 C -0.0378(10) 0.3323(12) 0.2030(6) 0.031(3) Uani 1 1 d . . .
H9 H -0.0937 0.3359 0.2280 0.038 Uiso 1 1 calc R . .
C10 C 0.0193(10) 0.4350(12) 0.1913(6) 0.034(3) Uani 1 1 d . . .
H10 H 0.0024 0.5077 0.2089 0.040 Uiso 1 1 calc R . .
C11 C 0.1024(9) 0.4312(10) 0.1535(5) 0.024(2) Uani 1 1 d . . .
H11 H 0.1399 0.5012 0.1449 0.029 Uiso 1 1 calc R . .
C12 C 0.1286(8) 0.3214(9) 0.1287(5) 0.0121(19) Uani 1 1 d . . .
C13 C 0.2039(9) 0.5165(10) -0.0170(5) 0.022(2) Uani 1 1 d . . .
H13 H 0.1642 0.4630 -0.0496 0.026 Uiso 1 1 calc R . .
C14 C 0.2168(10) 0.6393(11) -0.0319(6) 0.033(3) Uani 1 1 d . . .
H14 H 0.1866 0.6660 -0.0751 0.039 Uiso 1 1 calc R . .
C15 C 0.2729(11) 0.7195(11) 0.0162(7) 0.032(3) Uani 1 1 d . . .
H15 H 0.2770 0.8004 0.0060 0.038 Uiso 1 1 calc R . .
C16 C 0.3241(10) 0.6784(10) 0.0809(6) 0.026(3) Uani 1 1 d . . .
H16 H 0.3643 0.7317 0.1136 0.032 Uiso 1 1 calc R . .
C17 C 0.3146(9) 0.5587(9) 0.0959(6) 0.021(2) Uani 1 1 d . . .
H17 H 0.3501 0.5311 0.1385 0.025 Uiso 1 1 calc R . .
C18 C 0.2522(8) 0.4789(9) 0.0476(5) 0.016(2) Uani 1 1 d . . .
N1 N 0.4106(7) 0.3022(8) 0.2148(4) 0.0189(19) Uani 1 1 d . . .
C19 C 0.4590(8) 0.3055(9) 0.0414(5) 0.017(2) Uani 1 1 d . . .
C20 C 0.5435(9) 0.1180(10) 0.0823(5) 0.024(2) Uani 1 1 d . . .
C21 C 0.5771(11) 0.3797(12) 0.1447(6) 0.034(3) Uani 1 1 d . . .
C22 C 0.3854(10) 0.3111(11) 0.2634(6) 0.030(3) Uani 1 1 d . . .
C23 C 0.3486(15) 0.310(2) 0.3248(8) 0.077(7) Uani 1 1 d . . .
H23A H 0.4192 0.2950 0.3612 0.092 Uiso 1 1 calc R . .
H23B H 0.3185 0.3896 0.3315 0.092 Uiso 1 1 calc R . .
C24 C 0.256(2) 0.2223(15) 0.3270(9) 0.074(6) Uani 1 1 d . . .
H24A H 0.2377 0.2271 0.3690 0.111 Uiso 1 1 calc R . .
H24B H 0.2859 0.1433 0.3214 0.111 Uiso 1 1 calc R . .
H24C H 0.1849 0.2383 0.2921 0.111 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'
N N 0.0061 0.0033 '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'
I I -0.4742 1.8119 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C21 W1 C19 73.3(5) . .
C21 W1 C20 105.2(5) . .
C19 W1 C20 72.6(4) . .
C21 W1 N1 85.8(4) . .
C19 W1 N1 133.7(4) . .
C20 W1 N1 153.7(4) . .
C21 W1 As1 108.6(4) . .
C19 W1 As1 70.8(3) . .
C20 W1 As1 119.1(3) . .
N1 W1 As1 77.9(2) . .
C21 W1 I2 76.8(4) . .
C19 W1 I2 127.7(3) . .
C20 W1 I2 75.2(3) . .
N1 W1 I2 84.5(2) . .
As1 W1 I2 160.97(3) . .
C21 W1 I1 162.4(4) . .
C19 W1 I1 123.9(3) . .
C20 W1 I1 79.4(3) . .
N1 W1 I1 83.5(2) . .
As1 W1 I1 82.76(3) . .
I2 W1 I1 88.26(3) . .
C6 As1 C12 101.7(4) . .
C6 As1 C18 106.1(4) . .
C12 As1 C18 101.9(4) . .
C6 As1 W1 117.8(3) . .
C12 As1 W1 119.4(3) . .
C18 As1 W1 108.1(3) . .
C6 C1 C2 119.7(9) . .
C6 C1 H1 120.2 . .
C2 C1 H1 120.2 . .
C3 C2 C1 120.4(10) . .
C3 C2 H2 119.8 . .
C1 C2 H2 119.8 . .
C4 C3 C2 120.3(9) . .
C4 C3 H3 119.8 . .
C2 C3 H3 119.8 . .
C3 C4 C5 119.5(9) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
C6 C5 C4 119.6(10) . .
C6 C5 H5 120.2 . .
C4 C5 H5 120.2 . .
C5 C6 C1 120.5(9) . .
C5 C6 As1 119.7(7) . .
C1 C6 As1 119.8(7) . .
C12 C7 C8 121.1(10) . .
C12 C7 H7 119.5 . .
C8 C7 H7 119.5 . .
C7 C8 C9 118.7(11) . .
C7 C8 H8 120.7 . .
C9 C8 H8 120.7 . .
C10 C9 C8 120.4(10) . .
C10 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C9 C10 C11 120.5(11) . .
C9 C10 H10 119.8 . .
C11 C10 H10 119.8 . .
C12 C11 C10 119.2(10) . .
C12 C11 H11 120.4 . .
C10 C11 H11 120.4 . .
C7 C12 C11 120.2(9) . .
C7 C12 As1 119.2(7) . .
C11 C12 As1 120.6(7) . .
C18 C13 C14 117.9(11) . .
C18 C13 H13 121.1 . .
C14 C13 H13 121.1 . .
C15 C14 C13 121.5(12) . .
C15 C14 H14 119.3 . .
C13 C14 H14 119.3 . .
C14 C15 C16 119.5(11) . .
C14 C15 H15 120.3 . .
C16 C15 H15 120.3 . .
C17 C16 C15 119.7(11) . .
C17 C16 H16 120.1 . .
C15 C16 H16 120.1 . .
C16 C17 C18 120.4(11) . .
C16 C17 H17 119.8 . .
C18 C17 H17 119.8 . .
C13 C18 C17 120.9(10) . .
C13 C18 As1 122.5(8) . .
C17 C18 As1 116.6(8) . .
C22 N1 W1 165.2(10) . .
O2 C19 W1 179.6(9) . .
O1 C20 W1 179.2(11) . .
O3 C21 W1 177.2(13) . .
N1 C22 C23 174.3(14) . .
C24 C23 C22 114.6(12) . .
C24 C23 H23A 108.6 . .
C22 C23 H23A 108.6 . .
C24 C23 H23B 108.6 . .
C22 C23 H23B 108.6 . .
H23A C23 H23B 107.6 . .
C23 C24 H24A 109.5 . .
C23 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C23 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C21 1.992(12) .
W1 C19 1.987(10) .
W1 C20 2.004(11) .
W1 N1 2.163(9) .
W1 As1 2.6416(11) .
W1 I2 2.8516(9) .
W1 I1 2.8621(8) .
As1 C6 1.941(9) .
As1 C12 1.956(9) .
As1 C18 1.957(10) .
O1 C20 1.129(13) .
O2 C19 1.137(12) .
O3 C21 1.151(14) .
C1 C6 1.392(14) .
C1 C2 1.390(14) .
C1 H1 0.9300 .
C2 C3 1.377(14) .
C2 H2 0.9300 .
C3 C4 1.380(15) .
C3 H3 0.9300 .
C4 C5 1.420(15) .
C4 H4 0.9300 .
C5 C6 1.368(14) .
C5 H5 0.9300 .
C7 C12 1.368(14) .
C7 C8 1.386(15) .
C7 H7 0.9300 .
C8 C9 1.400(17) .
C8 H8 0.9300 .
C9 C10 1.371(17) .
C9 H9 0.9300 .
C10 C11 1.392(15) .
C10 H10 0.9300 .
C11 C12 1.392(14) .
C11 H11 0.9300 .
C13 C18 1.385(14) .
C13 C14 1.418(16) .
C13 H13 0.9300 .
C14 C15 1.371(19) .
C14 H14 0.9300 .
C15 C16 1.405(18) .
C15 H15 0.9300 .
C16 C17 1.379(15) .
C16 H16 0.9300 .
C17 C18 1.393(14) .
C17 H17 0.9300 .
N1 C22 1.135(14) .
C22 C23 1.456(18) .
C23 C24 1.45(2) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
