#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:30:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179114 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/76/4307677.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_4307677
loop_
_publ_author_name
'Shaun P. Green'
'Cameron Jones'
'Guoxia Jin'
'Andreas Stasch'
_publ_section_title
;
Base-Stabilized Amidodiarsenes: Synthesis, Structure, and Theoretical
Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8
_journal_page_last               10
_journal_paper_doi               10.1021/ic062163f
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C37 H56 I2 N3 Sb'
_chemical_formula_weight         918.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.643(4)
_cell_length_b                   18.352(4)
_cell_length_c                   21.162(4)
_cell_measurement_temperature    150(2)
_cell_volume                     7629(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa 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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17571
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    2.370
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.478
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         9172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0324
_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)+(0.0170P)²+12.8103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                7250
_reflns_number_total             9172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062163fsi20061114_083116.cif
_cod_data_source_block           compound3b
_cod_database_code               4307677
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, 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
I1 I 0.073990(10) 0.300070(12) 0.076613(11) 0.03342(6) Uani 1 1 d . . .
Sb1 Sb 0.215479(10) 0.307377(10) 0.116444(9) 0.02385(5) Uani 1 1 d . . .
N1 N 0.30804(11) 0.37377(12) 0.13657(11) 0.0196(5) Uani 1 1 d . . .
C1 C 0.28800(14) 0.42894(14) 0.09881(12) 0.0178(5) Uani 1 1 d . . .
I2 I 0.168538(13) 0.32961(2) 0.237019(11) 0.06144(10) Uani 1 1 d . . .
N2 N 0.22436(11) 0.41271(12) 0.07577(11) 0.0188(5) Uani 1 1 d . . .
C2 C 0.37632(14) 0.34652(15) 0.14428(14) 0.0224(6) Uani 1 1 d . . .
N3 N 0.32397(12) 0.49073(12) 0.08717(10) 0.0204(5) Uani 1 1 d . . .
C3 C 0.40137(16) 0.33518(16) 0.20602(14) 0.0279(7) Uani 1 1 d . . .
C4 C 0.46634(18) 0.3057(2) 0.21304(17) 0.0416(9) Uani 1 1 d . . .
H4 H 0.4841 0.2991 0.2544 0.050 Uiso 1 1 calc R . .
C5 C 0.50529(18) 0.2858(2) 0.16222(19) 0.0458(9) Uani 1 1 d . . .
H5 H 0.5497 0.2667 0.1684 0.055 Uiso 1 1 calc R . .
C6 C 0.47934(16) 0.29384(19) 0.10193(17) 0.0371(8) Uani 1 1 d . . .
H6 H 0.5058 0.2783 0.0668 0.045 Uiso 1 1 calc R . .
C7 C 0.41535(15) 0.32417(16) 0.09148(14) 0.0251(6) Uani 1 1 d . . .
C8 C 0.35953(17) 0.34953(17) 0.26460(14) 0.0317(7) Uani 1 1 d . . .
H8 H 0.3172 0.3760 0.2517 0.038 Uiso 1 1 calc R . .
C9 C 0.3968(2) 0.3960(2) 0.31385(17) 0.0536(11) Uani 1 1 d . . .
H9A H 0.4354 0.3685 0.3309 0.080 Uiso 1 1 calc R . .
H9B H 0.3654 0.4083 0.3482 0.080 Uiso 1 1 calc R . .
H9C H 0.4133 0.4408 0.2940 0.080 Uiso 1 1 calc R . .
C10 C 0.3385(2) 0.2767(2) 0.29505(19) 0.0532(10) Uani 1 1 d . . .
H10A H 0.3142 0.2470 0.2639 0.080 Uiso 1 1 calc R . .
H10B H 0.3087 0.2862 0.3313 0.080 Uiso 1 1 calc R . .
H10C H 0.3793 0.2507 0.3093 0.080 Uiso 1 1 calc R . .
C11 C 0.38938(15) 0.32539(16) 0.02395(14) 0.0264(6) Uani 1 1 d . . .
H11 H 0.3494 0.3590 0.0219 0.032 Uiso 1 1 calc R . .
C12 C 0.44277(17) 0.35189(19) -0.02335(16) 0.0374(8) Uani 1 1 d . . .
H12A H 0.4641 0.3965 -0.0074 0.056 Uiso 1 1 calc R . .
H12B H 0.4208 0.3620 -0.0640 0.056 Uiso 1 1 calc R . .
H12C H 0.4776 0.3142 -0.0290 0.056 Uiso 1 1 calc R . .
C13 C 0.3660(2) 0.2494(2) 0.00397(17) 0.0453(9) Uani 1 1 d . . .
H13A H 0.4046 0.2156 0.0057 0.068 Uiso 1 1 calc R . .
H13B H 0.3481 0.2513 -0.0393 0.068 Uiso 1 1 calc R . .
H13C H 0.3301 0.2325 0.0327 0.068 Uiso 1 1 calc R . .
C14 C 0.17535(14) 0.45784(15) 0.04427(14) 0.0236(6) Uani 1 1 d . . .
C15 C 0.13959(15) 0.51254(17) 0.07661(17) 0.0323(7) Uani 1 1 d . . .
C16 C 0.09271(18) 0.55414(19) 0.0419(2) 0.0465(10) Uani 1 1 d . . .
H16 H 0.0688 0.5923 0.0626 0.056 Uiso 1 1 calc R . .
C17 C 0.08039(18) 0.5414(2) -0.0209(2) 0.0505(11) Uani 1 1 d . . .
H17 H 0.0493 0.5713 -0.0435 0.061 Uiso 1 1 calc R . .
C18 C 0.11311(18) 0.48535(18) -0.05082(18) 0.0414(9) Uani 1 1 d . . .
H18 H 0.1034 0.4760 -0.0940 0.050 Uiso 1 1 calc R . .
C19 C 0.16021(16) 0.44175(16) -0.01968(15) 0.0301(7) Uani 1 1 d . . .
C20 C 0.14412(18) 0.52390(19) 0.14740(18) 0.0417(9) Uani 1 1 d . . .
H20 H 0.1838 0.4954 0.1638 0.050 Uiso 1 1 calc R . .
C21 C 0.1532(2) 0.6040(2) 0.1672(2) 0.0567(11) Uani 1 1 d . . .
H21A H 0.1935 0.6243 0.1462 0.085 Uiso 1 1 calc R . .
H21B H 0.1591 0.6069 0.2131 0.085 Uiso 1 1 calc R . .
H21C H 0.1129 0.6320 0.1547 0.085 Uiso 1 1 calc R . .
C22 C 0.0786(2) 0.4938(2) 0.1781(2) 0.0629(13) Uani 1 1 d . . .
H22A H 0.0399 0.5246 0.1664 0.094 Uiso 1 1 calc R . .
H22B H 0.0837 0.4936 0.2241 0.094 Uiso 1 1 calc R . .
H22C H 0.0706 0.4439 0.1632 0.094 Uiso 1 1 calc R . .
C23 C 0.1916(2) 0.37780(19) -0.05507(17) 0.0450(10) Uani 1 1 d . . .
H23 H 0.2107 0.3435 -0.0229 0.054 Uiso 1 1 calc R . .
C24 C 0.2485(2) 0.3997(2) -0.0978(2) 0.0656(13) Uani 1 1 d . . .
H24A H 0.2322 0.4364 -0.1279 0.098 Uiso 1 1 calc R . .
H24B H 0.2648 0.3569 -0.1210 0.098 Uiso 1 1 calc R . .
H24C H 0.2858 0.4201 -0.0727 0.098 Uiso 1 1 calc R . .
C25 C 0.1385(3) 0.3356(2) -0.09387(18) 0.0637(14) Uani 1 1 d . . .
H25A H 0.1216 0.3666 -0.1281 0.095 Uiso 1 1 calc R . .
H25B H 0.1006 0.3215 -0.0664 0.095 Uiso 1 1 calc R . .
H25C H 0.1596 0.2918 -0.1118 0.095 Uiso 1 1 calc R . .
C26 C 0.37101(15) 0.51696(16) 0.13842(14) 0.0260(6) Uani 1 1 d . . .
H26 H 0.3746 0.4748 0.1681 0.031 Uiso 1 1 calc R . .
C27 C 0.3403(2) 0.5770(3) 0.1776(2) 0.0633(13) Uani 1 1 d . . .
H27A H 0.2954 0.5610 0.1935 0.076 Uiso 1 1 calc R . .
H27B H 0.3331 0.6204 0.1506 0.076 Uiso 1 1 calc R . .
C28 C 0.3854(3) 0.5980(2) 0.2337(2) 0.0677(14) Uani 1 1 d . . .
H28A H 0.3667 0.6424 0.2539 0.081 Uiso 1 1 calc R . .
H28B H 0.3845 0.5583 0.2653 0.081 Uiso 1 1 calc R . .
C29 C 0.4582(3) 0.6122(2) 0.2140(2) 0.0654(14) Uani 1 1 d . . .
H29A H 0.4601 0.6573 0.1884 0.078 Uiso 1 1 calc R . .
H29B H 0.4865 0.6196 0.2521 0.078 Uiso 1 1 calc R . .
C30 C 0.4862(2) 0.5512(3) 0.1769(2) 0.0635(13) Uani 1 1 d . . .
H30A H 0.4897 0.5077 0.2044 0.076 Uiso 1 1 calc R . .
H30B H 0.5327 0.5640 0.1627 0.076 Uiso 1 1 calc R . .
C31 C 0.44298(18) 0.5324(2) 0.11934(18) 0.0497(10) Uani 1 1 d . . .
H31A H 0.4438 0.5736 0.0892 0.060 Uiso 1 1 calc R . .
H31B H 0.4623 0.4892 0.0979 0.060 Uiso 1 1 calc R . .
C32 C 0.31502(15) 0.53152(15) 0.02624(13) 0.0218(6) Uani 1 1 d . . .
H32 H 0.2771 0.5067 0.0032 0.026 Uiso 1 1 calc R . .
C33 C 0.2935(2) 0.61101(19) 0.03357(18) 0.0456(10) Uani 1 1 d . . .
H33A H 0.2521 0.6139 0.0601 0.055 Uiso 1 1 calc R . .
H33B H 0.3301 0.6388 0.0548 0.055 Uiso 1 1 calc R . .
C34 C 0.2791(2) 0.6441(2) -0.0310(2) 0.0628(13) Uani 1 1 d . . .
H34A H 0.2398 0.6188 -0.0502 0.075 Uiso 1 1 calc R . .
H34B H 0.2666 0.6960 -0.0256 0.075 Uiso 1 1 calc R . .
C35 C 0.33901(18) 0.63896(18) -0.07504(15) 0.0373(8) Uani 1 1 d . . .
H35A H 0.3259 0.6578 -0.1172 0.045 Uiso 1 1 calc R . .
H35B H 0.3766 0.6696 -0.0588 0.045 Uiso 1 1 calc R . .
C36 C 0.3631(2) 0.56174(19) -0.08130(16) 0.0484(10) Uani 1 1 d . . .
H36A H 0.4054 0.5606 -0.1067 0.058 Uiso 1 1 calc R . .
H36B H 0.3282 0.5328 -0.1039 0.058 Uiso 1 1 calc R . .
C37 C 0.37651(19) 0.5277(2) -0.01688(16) 0.0435(9) Uani 1 1 d . . .
H37A H 0.3897 0.4761 -0.0226 0.052 Uiso 1 1 calc R . .
H37B H 0.4151 0.5533 0.0034 0.052 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'
Sb Sb -0.5866 1.5461 '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'
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
N2 Sb1 N1 60.85(8) . . ?
N2 Sb1 I2 105.62(6) . . ?
N1 Sb1 I2 90.87(6) . . ?
N2 Sb1 I1 90.17(6) . . ?
N1 Sb1 I1 149.32(6) . . ?
I2 Sb1 I1 87.433(13) . . ?
C1 N1 C2 126.8(2) . . ?
C1 N1 Sb1 93.38(16) . . ?
C2 N1 Sb1 126.23(17) . . ?
N1 C1 N3 125.6(2) . . ?
N1 C1 N2 108.2(2) . . ?
N3 C1 N2 126.1(2) . . ?
C1 N2 C14 130.6(2) . . ?
C1 N2 Sb1 97.37(16) . . ?
C14 N2 Sb1 131.22(17) . . ?
C3 C2 C7 119.9(3) . . ?
C3 C2 N1 118.7(3) . . ?
C7 C2 N1 121.0(3) . . ?
C1 N3 C32 120.7(2) . . ?
C1 N3 C26 117.1(2) . . ?
C32 N3 C26 122.1(2) . . ?
C4 C3 C2 118.4(3) . . ?
C4 C3 C8 118.6(3) . . ?
C2 C3 C8 123.0(3) . . ?
C5 C4 C3 122.1(3) . . ?
C4 C5 C6 119.4(3) . . ?
C5 C6 C7 121.5(3) . . ?
C6 C7 C2 118.6(3) . . ?
C6 C7 C11 117.3(3) . . ?
C2 C7 C11 123.8(3) . . ?
C3 C8 C9 113.3(3) . . ?
C3 C8 C10 109.8(3) . . ?
C9 C8 C10 109.0(3) . . ?
C7 C11 C13 110.4(3) . . ?
C7 C11 C12 113.0(3) . . ?
C13 C11 C12 108.4(3) . . ?
C15 C14 C19 120.7(3) . . ?
C15 C14 N2 121.5(3) . . ?
C19 C14 N2 117.7(3) . . ?
C14 C15 C16 117.5(3) . . ?
C14 C15 C20 123.5(3) . . ?
C16 C15 C20 118.8(3) . . ?
C17 C16 C15 122.0(3) . . ?
C18 C17 C16 119.6(3) . . ?
C17 C18 C19 121.7(4) . . ?
C18 C19 C14 118.2(3) . . ?
C18 C19 C23 118.7(3) . . ?
C14 C19 C23 123.1(3) . . ?
C15 C20 C21 114.0(3) . . ?
C15 C20 C22 108.5(3) . . ?
C21 C20 C22 109.0(3) . . ?
C24 C23 C19 113.2(3) . . ?
C24 C23 C25 108.6(3) . . ?
C19 C23 C25 112.1(3) . . ?
C31 C26 N3 116.5(3) . . ?
C31 C26 C27 112.8(3) . . ?
N3 C26 C27 112.7(3) . . ?
C26 C27 C28 112.4(3) . . ?
C29 C28 C27 112.1(4) . . ?
C30 C29 C28 111.7(3) . . ?
C29 C30 C31 112.9(4) . . ?
C26 C31 C30 110.7(3) . . ?
N3 C32 C37 113.6(2) . . ?
N3 C32 C33 114.9(2) . . ?
C37 C32 C33 109.0(3) . . ?
C34 C33 C32 110.0(3) . . ?
C35 C34 C33 112.8(3) . . ?
C36 C35 C34 111.2(3) . . ?
C35 C36 C37 111.3(3) . . ?
C32 C37 C36 112.5(3) . . ?
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
I1 Sb1 2.9074(6) . ?
Sb1 N2 2.123(2) . ?
Sb1 N1 2.230(2) . ?
Sb1 I2 2.7436(6) . ?
N1 C1 1.349(3) . ?
N1 C2 1.441(4) . ?
C1 N3 1.359(3) . ?
C1 N2 1.374(3) . ?
N2 C14 1.434(3) . ?
C2 C3 1.411(4) . ?
C2 C7 1.416(4) . ?
N3 C32 1.501(3) . ?
N3 C26 1.504(3) . ?
C3 C4 1.394(5) . ?
C3 C8 1.511(4) . ?
C4 C5 1.369(5) . ?
C5 C6 1.382(5) . ?
C6 C7 1.392(4) . ?
C7 C11 1.517(4) . ?
C8 C9 1.532(5) . ?
C8 C10 1.540(5) . ?
C11 C13 1.528(4) . ?
C11 C12 1.529(4) . ?
C14 C15 1.403(4) . ?
C14 C19 1.417(4) . ?
C15 C16 1.404(5) . ?
C15 C20 1.515(5) . ?
C16 C17 1.370(6) . ?
C17 C18 1.369(5) . ?
C18 C19 1.389(4) . ?
C19 C23 1.523(5) . ?
C20 C21 1.540(5) . ?
C20 C22 1.544(5) . ?
C23 C24 1.493(6) . ?
C23 C25 1.536(5) . ?
C26 C31 1.497(4) . ?
C26 C27 1.505(5) . ?
C27 C28 1.529(5) . ?
C28 C29 1.512(7) . ?
C29 C30 1.473(6) . ?
C30 C31 1.524(5) . ?
C32 C37 1.515(4) . ?
C32 C33 1.527(4) . ?
C33 C34 1.521(5) . ?
C34 C35 1.504(5) . ?
C35 C36 1.500(5) . ?
C36 C37 1.522(5) . ?
