 
data_92src179
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_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
 
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'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
_symmetry_space_group_name_hall   '-P 2ybc'
 
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'
 
_cell_length_a                    11.465(3)
_cell_length_b                    11.129(2)
_cell_length_c                    20.950(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  105.335(5)
_cell_angle_gamma                 90.00
_cell_volume                      2577.9(9)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        unk
_exptl_crystal_colour             unk
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.2
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.275
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1632
_exptl_absorpt_coefficient_mu     8.175
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
 'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_standards_number         'None'
_diffrn_standards_interval_count 'N/A'
_diffrn_standards_interval_time  'N/A'
_diffrn_standards_decay_%        'N/A'
_diffrn_reflns_number             9636
_diffrn_reflns_av_R_equivalents   0.0815
_diffrn_reflns_av_sigmaI/netI     0.1358
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -24
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          2.96
_diffrn_reflns_theta_max          25.02
_reflns_number_total              4428
_reflns_number_gt                 3840
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        REFINE
_computing_data_reduction         'ABSURD (Karaulov, 1992)'
_computing_structure_solution     'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material   SHELXL97
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4428
_refine_ls_number_parameters      294
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0523
_refine_ls_R_factor_gt            0.0474
_refine_ls_wR_factor_ref          0.1284
_refine_ls_wR_factor_gt           0.1241
_refine_ls_goodness_of_fit_ref    0.824
_refine_ls_restrained_S_all       0.824
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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 . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
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
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 . ?
 
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
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 . . ?
 
_diffrn_measured_fraction_theta_max    0.973
_diffrn_reflns_theta_full              25.02
_diffrn_measured_fraction_theta_full   0.973
_refine_diff_density_max    2.200
_refine_diff_density_min   -5.987
_refine_diff_density_rms    0.335
