# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
_publ_contact_author_name 'Piskunov, Alexandr'
_publ_contact_author_email pial@iomc.ras.ru
_publ_section_title
;
Synthesis and Molecular Structure of Indium complexes based
on 3,6-di-tert-butyl-o-benzoquinone. Looking
for indium(I) o-semiquinolate
;
loop_
_publ_author_name
A.Piskunov
A.Maleeva
G.Fukin
E.Baranov
A.Bogomyakov
;
V.Cherkasov
;
G.Abakumov
# Attachment '- Complex_1.cif'
data_insqm
_database_code_depnum_ccdc_archive 'CCDC 780469'
#TrackingRef '- Complex_1.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C42 H60 In O6'
_chemical_formula_weight 775.72
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'
In In -0.7276 1.3100 '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)/n
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 11.3435(4)
_cell_length_b 10.0725(4)
_cell_length_c 36.4349(14)
_cell_angle_alpha 90.00
_cell_angle_beta 90.2650(10)
_cell_angle_gamma 90.00
_cell_volume 4162.9(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 900
_cell_measurement_theta_min 2
_cell_measurement_theta_max 30
_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.44
_exptl_crystal_size_min 0.33
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.238
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1636
_exptl_absorpt_coefficient_mu 0.610
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7710
_exptl_absorpt_correction_T_max 0.8241
_exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 34581
_diffrn_reflns_av_R_equivalents 0.0293
_diffrn_reflns_av_sigmaI/netI 0.0239
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -44
_diffrn_reflns_limit_l_max 44
_diffrn_reflns_theta_min 2.63
_diffrn_reflns_theta_max 26.00
_reflns_number_total 8117
_reflns_number_gt 7169
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SHELXTL'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0308P)^2^+3.1580P] where P=(Fo^2^+2Fc^2^)/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 8117
_refine_ls_number_parameters 460
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0371
_refine_ls_R_factor_gt 0.0306
_refine_ls_wR_factor_ref 0.0696
_refine_ls_wR_factor_gt 0.0675
_refine_ls_goodness_of_fit_ref 1.071
_refine_ls_restrained_S_all 1.071
_refine_ls_shift/su_max 0.001
_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
In1 In 0.372349(10) 0.570371(12) 0.123490(3) 0.01680(3) Uani 1 1 d . . .
O1 O 0.51088(10) 0.60409(12) 0.08491(3) 0.0206(3) Uani 1 1 d . . .
O2 O 0.29776(10) 0.70738(12) 0.08418(3) 0.0200(3) Uani 1 1 d . . .
O3 O 0.50984(10) 0.59987(12) 0.16346(3) 0.0204(3) Uani 1 1 d . . .
O4 O 0.28655(10) 0.66527(12) 0.16953(3) 0.0199(3) Uani 1 1 d . . .
O5 O 0.42821(10) 0.36422(12) 0.12384(3) 0.0211(3) Uani 1 1 d . . .
O6 O 0.21307(10) 0.45733(12) 0.11781(3) 0.0216(3) Uani 1 1 d . . .
C1 C 0.48430(15) 0.67780(17) 0.05745(5) 0.0182(4) Uani 1 1 d . . .
C2 C 0.36451(15) 0.73359(17) 0.05659(5) 0.0187(4) Uani 1 1 d . . .
C3 C 0.32643(15) 0.81235(17) 0.02592(5) 0.0207(4) Uani 1 1 d . . .
C4 C 0.41002(16) 0.83799(19) -0.00008(5) 0.0250(4) Uani 1 1 d . . .
H4A H 0.3889 0.8938 -0.0201 0.030 Uiso 1 1 calc R . .
C5 C 0.52698(16) 0.78603(19) 0.00100(5) 0.0245(4) Uani 1 1 d . . .
H5A H 0.5796 0.8093 -0.0182 0.029 Uiso 1 1 calc R . .
C6 C 0.56684(15) 0.70418(18) 0.02837(5) 0.0200(4) Uani 1 1 d . . .
C7 C 0.19907(16) 0.86253(19) 0.02314(5) 0.0240(4) Uani 1 1 d . . .
C8 C 0.17566(18) 0.9610(2) 0.05442(5) 0.0299(5) Uani 1 1 d . . .
H8A H 0.1840 0.9154 0.0781 0.045 Uiso 1 1 calc R . .
H8B H 0.0955 0.9964 0.0521 0.045 Uiso 1 1 calc R . .
H8C H 0.2325 1.0341 0.0531 0.045 Uiso 1 1 calc R . .
C9 C 0.11103(16) 0.7469(2) 0.02572(6) 0.0305(5) Uani 1 1 d . . .
H9A H 0.1210 0.7018 0.0494 0.046 Uiso 1 1 calc R . .
H9B H 0.1256 0.6839 0.0057 0.046 Uiso 1 1 calc R . .
H9C H 0.0305 0.7813 0.0237 0.046 Uiso 1 1 calc R . .
C10 C 0.17803(18) 0.9336(2) -0.01372(5) 0.0332(5) Uani 1 1 d . . .
H10A H 0.2325 1.0086 -0.0159 0.050 Uiso 1 1 calc R . .
H10B H 0.0967 0.9661 -0.0148 0.050 Uiso 1 1 calc R . .
H10C H 0.1915 0.8712 -0.0339 0.050 Uiso 1 1 calc R . .
C11 C 0.68894(15) 0.63923(19) 0.02905(5) 0.0234(4) Uani 1 1 d . . .
C12 C 0.75826(17) 0.6706(2) -0.00584(6) 0.0340(5) Uani 1 1 d . . .
H12A H 0.7137 0.6399 -0.0273 0.051 Uiso 1 1 calc R . .
H12B H 0.8347 0.6254 -0.0049 0.051 Uiso 1 1 calc R . .
H12C H 0.7707 0.7667 -0.0076 0.051 Uiso 1 1 calc R . .
C13 C 0.75979(16) 0.6898(2) 0.06243(5) 0.0300(5) Uani 1 1 d . . .
H13A H 0.7174 0.6682 0.0850 0.045 Uiso 1 1 calc R . .
H13B H 0.7696 0.7863 0.0606 0.045 Uiso 1 1 calc R . .
H13C H 0.8374 0.6472 0.0629 0.045 Uiso 1 1 calc R . .
C14 C 0.67528(17) 0.4880(2) 0.03120(6) 0.0299(5) Uani 1 1 d . . .
H14A H 0.6292 0.4567 0.0101 0.045 Uiso 1 1 calc R . .
H14B H 0.6346 0.4643 0.0539 0.045 Uiso 1 1 calc R . .
H14C H 0.7533 0.4464 0.0309 0.045 Uiso 1 1 calc R . .
C15 C 0.47673(15) 0.64207(16) 0.19490(5) 0.0174(4) Uani 1 1 d . . .
C16 C 0.35143(14) 0.68086(17) 0.19834(5) 0.0179(4) Uani 1 1 d . . .
C17 C 0.30796(15) 0.73117(17) 0.23240(5) 0.0190(4) Uani 1 1 d . . .
C18 C 0.38832(16) 0.74032(18) 0.26049(5) 0.0229(4) Uani 1 1 d . . .
H18A H 0.3625 0.7748 0.2834 0.027 Uiso 1 1 calc R . .
C19 C 0.50845(15) 0.70084(18) 0.25724(5) 0.0230(4) Uani 1 1 d . . .
H19A H 0.5585 0.7102 0.2781 0.028 Uiso 1 1 calc R . .
C20 C 0.55541(15) 0.65030(17) 0.22582(5) 0.0188(4) Uani 1 1 d . . .
C21 C 0.17716(15) 0.76641(18) 0.23731(5) 0.0216(4) Uani 1 1 d . . .
C22 C 0.10337(16) 0.6392(2) 0.23305(5) 0.0276(4) Uani 1 1 d . . .
H22A H 0.1277 0.5744 0.2517 0.041 Uiso 1 1 calc R . .
H22B H 0.1157 0.6017 0.2085 0.041 Uiso 1 1 calc R . .
H22C H 0.0197 0.6604 0.2362 0.041 Uiso 1 1 calc R . .
C23 C 0.13673(17) 0.8691(2) 0.20862(5) 0.0282(4) Uani 1 1 d . . .
H23A H 0.1439 0.8309 0.1840 0.042 Uiso 1 1 calc R . .
H23B H 0.1862 0.9486 0.2105 0.042 Uiso 1 1 calc R . .
H23C H 0.0543 0.8930 0.2131 0.042 Uiso 1 1 calc R . .
C24 C 0.15430(16) 0.8252(2) 0.27545(5) 0.0270(4) Uani 1 1 d . . .
H24A H 0.1777 0.7608 0.2943 0.040 Uiso 1 1 calc R . .
H24B H 0.0702 0.8454 0.2780 0.040 Uiso 1 1 calc R . .
H24C H 0.2004 0.9068 0.2785 0.040 Uiso 1 1 calc R . .
C25 C 0.68341(15) 0.60344(18) 0.22227(5) 0.0220(4) Uani 1 1 d . . .
C26 C 0.74571(16) 0.6040(2) 0.25971(5) 0.0282(4) Uani 1 1 d . . .
H26A H 0.7020 0.5478 0.2769 0.042 Uiso 1 1 calc R . .
H26B H 0.7490 0.6950 0.2692 0.042 Uiso 1 1 calc R . .
H26C H 0.8260 0.5695 0.2570 0.042 Uiso 1 1 calc R . .
C27 C 0.74996(16) 0.6956(2) 0.19585(5) 0.0289(5) Uani 1 1 d . . .
H27A H 0.7479 0.7867 0.2053 0.043 Uiso 1 1 calc R . .
H27B H 0.7124 0.6925 0.1716 0.043 Uiso 1 1 calc R . .
H27C H 0.8320 0.6662 0.1939 0.043 Uiso 1 1 calc R . .
C28 C 0.68760(16) 0.45969(18) 0.20798(6) 0.0267(4) Uani 1 1 d . . .
H28A H 0.6431 0.4019 0.2246 0.040 Uiso 1 1 calc R . .
H28B H 0.7697 0.4298 0.2069 0.040 Uiso 1 1 calc R . .
H28C H 0.6526 0.4559 0.1834 0.040 Uiso 1 1 calc R . .
C29 C 0.34556(14) 0.28004(17) 0.12708(4) 0.0176(4) Uani 1 1 d . . .
C30 C 0.22285(15) 0.33202(18) 0.12389(4) 0.0187(4) Uani 1 1 d . . .
C31 C 0.12313(15) 0.24620(18) 0.12744(5) 0.0210(4) Uani 1 1 d . . .
C32 C 0.14802(16) 0.11695(19) 0.13583(5) 0.0234(4) Uani 1 1 d . . .
H32A H 0.0840 0.0581 0.1400 0.028 Uiso 1 1 calc R . .
C33 C 0.26513(15) 0.06553(18) 0.13868(5) 0.0214(4) Uani 1 1 d . . .
H33A H 0.2749 -0.0257 0.1446 0.026 Uiso 1 1 calc R . .
C34 C 0.36381(15) 0.14072(17) 0.13336(5) 0.0192(4) Uani 1 1 d . . .
C35 C -0.00147(15) 0.2998(2) 0.12089(5) 0.0253(4) Uani 1 1 d . . .
C36 C -0.01058(17) 0.3491(2) 0.08095(5) 0.0306(5) Uani 1 1 d . . .
H36A H 0.0468 0.4204 0.0770 0.046 Uiso 1 1 calc R . .
H36B H -0.0903 0.3829 0.0763 0.046 Uiso 1 1 calc R . .
H36C H 0.0059 0.2755 0.0642 0.046 Uiso 1 1 calc R . .
C37 C -0.02983(16) 0.4144(2) 0.14734(5) 0.0298(5) Uani 1 1 d . . .
H37A H 0.0261 0.4871 0.1435 0.045 Uiso 1 1 calc R . .
H37B H -0.0235 0.3828 0.1727 0.045 Uiso 1 1 calc R . .
H37C H -0.1102 0.4461 0.1427 0.045 Uiso 1 1 calc R . .
C38 C -0.09469(16) 0.1908(2) 0.12610(6) 0.0346(5) Uani 1 1 d . . .
H38A H -0.0780 0.1167 0.1095 0.052 Uiso 1 1 calc R . .
H38B H -0.1730 0.2269 0.1206 0.052 Uiso 1 1 calc R . .
H38C H -0.0925 0.1593 0.1515 0.052 Uiso 1 1 calc R . .
C39 C 0.48925(15) 0.08215(17) 0.13345(5) 0.0198(4) Uani 1 1 d . . .
C40 C 0.54268(17) 0.1015(2) 0.09521(5) 0.0274(4) Uani 1 1 d . . .
H40A H 0.5444 0.1964 0.0893 0.041 Uiso 1 1 calc R . .
H40B H 0.4946 0.0544 0.0770 0.041 Uiso 1 1 calc R . .
H40C H 0.6232 0.0661 0.0950 0.041 Uiso 1 1 calc R . .
C41 C 0.56688(16) 0.15018(19) 0.16253(5) 0.0251(4) Uani 1 1 d . . .
H41A H 0.5321 0.1374 0.1869 0.038 Uiso 1 1 calc R . .
H41B H 0.5720 0.2453 0.1572 0.038 Uiso 1 1 calc R . .
H41C H 0.6460 0.1112 0.1621 0.038 Uiso 1 1 calc R . .
C42 C 0.48787(17) -0.06680(18) 0.14201(6) 0.0283(4) Uani 1 1 d . . .
H42A H 0.4550 -0.0811 0.1665 0.042 Uiso 1 1 calc R . .
H42B H 0.5685 -0.1016 0.1412 0.042 Uiso 1 1 calc R . .
H42C H 0.4392 -0.1130 0.1238 0.042 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
In1 0.01812(6) 0.01740(6) 0.01488(6) 0.00117(5) 0.00000(4) 0.00036(5)
O1 0.0201(6) 0.0236(6) 0.0182(6) 0.0040(5) 0.0010(5) 0.0019(5)
O2 0.0201(6) 0.0229(6) 0.0170(6) 0.0020(5) 0.0018(5) 0.0025(5)
O3 0.0180(5) 0.0254(6) 0.0178(6) -0.0020(5) 0.0000(5) 0.0008(5)
O4 0.0185(6) 0.0260(6) 0.0153(6) 0.0002(5) -0.0014(5) 0.0026(5)
O5 0.0186(6) 0.0191(6) 0.0257(6) 0.0015(5) 0.0004(5) 0.0003(5)
O6 0.0199(6) 0.0210(6) 0.0239(6) 0.0013(5) -0.0021(5) 0.0005(5)
C1 0.0221(8) 0.0160(8) 0.0164(8) -0.0011(6) -0.0028(6) -0.0012(7)
C2 0.0224(8) 0.0177(8) 0.0160(8) -0.0024(7) 0.0004(7) -0.0014(7)
C3 0.0266(9) 0.0189(9) 0.0166(8) -0.0018(7) -0.0026(7) 0.0028(7)
C4 0.0312(9) 0.0246(9) 0.0191(9) 0.0033(7) -0.0026(7) 0.0028(8)
C5 0.0280(9) 0.0257(9) 0.0199(8) 0.0032(8) 0.0029(7) -0.0031(8)
C6 0.0226(8) 0.0204(9) 0.0170(8) -0.0023(7) 0.0007(7) -0.0022(7)
C7 0.0244(9) 0.0285(10) 0.0192(9) -0.0007(7) -0.0031(7) 0.0073(8)
C8 0.0359(10) 0.0299(10) 0.0237(9) -0.0011(8) -0.0028(8) 0.0131(8)
C9 0.0232(9) 0.0387(12) 0.0296(10) -0.0041(8) -0.0036(8) 0.0050(8)
C10 0.0338(10) 0.0413(12) 0.0243(9) 0.0036(9) -0.0047(8) 0.0132(9)
C11 0.0197(8) 0.0281(10) 0.0224(9) 0.0017(8) 0.0034(7) -0.0012(7)
C12 0.0266(9) 0.0451(12) 0.0302(10) 0.0046(9) 0.0083(8) 0.0032(9)
C13 0.0232(9) 0.0375(11) 0.0294(10) 0.0010(9) -0.0020(8) -0.0029(8)
C14 0.0266(9) 0.0298(10) 0.0335(10) -0.0020(9) 0.0032(8) 0.0059(8)
C15 0.0214(8) 0.0140(8) 0.0169(8) 0.0011(6) 0.0011(6) -0.0009(7)
C16 0.0208(8) 0.0157(8) 0.0171(8) 0.0029(7) 0.0008(6) -0.0007(7)
C17 0.0222(8) 0.0159(8) 0.0188(8) 0.0017(7) 0.0039(7) 0.0003(7)
C18 0.0286(9) 0.0227(9) 0.0173(8) -0.0029(7) 0.0017(7) 0.0008(7)
C19 0.0251(9) 0.0229(9) 0.0210(9) -0.0020(7) -0.0059(7) -0.0010(8)
C20 0.0201(8) 0.0157(8) 0.0205(8) -0.0002(7) -0.0023(7) -0.0029(7)
C21 0.0208(8) 0.0225(9) 0.0217(9) 0.0016(7) 0.0029(7) 0.0028(7)
C22 0.0207(8) 0.0308(10) 0.0312(10) -0.0003(8) 0.0044(8) -0.0026(8)
C23 0.0275(9) 0.0311(10) 0.0262(10) 0.0043(8) 0.0045(8) 0.0089(8)
C24 0.0259(9) 0.0301(10) 0.0250(9) -0.0003(8) 0.0061(7) 0.0045(8)
C25 0.0168(8) 0.0234(9) 0.0256(9) -0.0010(7) -0.0022(7) -0.0011(7)
C26 0.0222(9) 0.0332(10) 0.0292(10) -0.0035(8) -0.0073(8) 0.0003(8)
C27 0.0210(9) 0.0332(11) 0.0325(10) 0.0029(9) -0.0005(8) -0.0026(8)
C28 0.0209(8) 0.0249(10) 0.0342(10) -0.0051(8) -0.0033(8) 0.0035(7)
C29 0.0224(8) 0.0174(8) 0.0131(8) -0.0007(7) 0.0012(6) -0.0011(7)
C30 0.0214(8) 0.0248(9) 0.0100(7) 0.0004(7) -0.0008(6) -0.0005(7)
C31 0.0215(8) 0.0281(10) 0.0134(8) -0.0006(7) -0.0003(7) -0.0018(7)
C32 0.0234(9) 0.0272(9) 0.0197(8) -0.0002(7) 0.0001(7) -0.0072(8)
C33 0.0255(8) 0.0192(8) 0.0196(8) 0.0021(7) -0.0005(7) -0.0018(7)
C34 0.0233(8) 0.0193(9) 0.0151(8) -0.0002(7) -0.0001(7) 0.0005(7)
C35 0.0193(8) 0.0328(10) 0.0239(9) 0.0020(8) -0.0009(7) -0.0016(8)
C36 0.0233(9) 0.0423(12) 0.0262(10) 0.0026(9) -0.0066(8) -0.0011(9)
C37 0.0219(9) 0.0367(11) 0.0307(10) 0.0002(9) 0.0025(8) 0.0031(8)
C38 0.0212(9) 0.0419(12) 0.0406(12) 0.0054(10) -0.0014(8) -0.0051(9)
C39 0.0226(8) 0.0158(8) 0.0210(8) 0.0010(7) -0.0005(7) 0.0006(7)
C40 0.0292(9) 0.0300(10) 0.0231(9) 0.0014(8) 0.0025(8) 0.0058(8)
C41 0.0256(9) 0.0259(10) 0.0238(9) -0.0026(8) -0.0056(7) 0.0032(8)
C42 0.0301(9) 0.0197(9) 0.0351(10) 0.0041(8) -0.0017(8) 0.0026(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds 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
In1 O1 2.1403(12) . ?
In1 O6 2.1448(12) . ?
In1 O3 2.1497(12) . ?
In1 O2 2.1589(12) . ?
In1 O4 2.1656(12) . ?
In1 O5 2.1710(12) . ?
O1 C1 1.281(2) . ?
O2 C2 1.289(2) . ?
O3 C15 1.280(2) . ?
O4 C16 1.289(2) . ?
O5 C29 1.270(2) . ?
O6 C30 1.286(2) . ?
C1 C6 1.442(2) . ?
C1 C2 1.471(2) . ?
C2 C3 1.435(2) . ?
C3 C4 1.368(3) . ?
C3 C7 1.534(2) . ?
C4 C5 1.427(3) . ?
C5 C6 1.369(3) . ?
C6 C11 1.532(2) . ?
C7 C8 1.535(3) . ?
C7 C9 1.537(3) . ?
C7 C10 1.539(3) . ?
C11 C12 1.531(3) . ?
C11 C14 1.533(3) . ?
C11 C13 1.541(3) . ?
C15 C20 1.436(2) . ?
C15 C16 1.480(2) . ?
C16 C17 1.430(2) . ?
C17 C18 1.371(2) . ?
C17 C21 1.537(2) . ?
C18 C19 1.425(3) . ?
C19 C20 1.364(2) . ?
C20 C25 1.533(2) . ?
C21 C24 1.533(3) . ?
C21 C22 1.538(3) . ?
C21 C23 1.539(3) . ?
C25 C26 1.533(2) . ?
C25 C27 1.537(3) . ?
C25 C28 1.539(3) . ?
C29 C34 1.437(2) . ?
C29 C30 1.491(2) . ?
C30 C31 1.430(2) . ?
C31 C32 1.366(3) . ?
C31 C35 1.531(2) . ?
C32 C33 1.429(3) . ?
C33 C34 1.366(2) . ?
C34 C39 1.540(2) . ?
C35 C38 1.536(3) . ?
C35 C37 1.538(3) . ?
C35 C36 1.541(3) . ?
C39 C42 1.532(2) . ?
C39 C40 1.534(2) . ?
C39 C41 1.536(2) . ?
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
O1 In1 O6 129.92(5) . . ?
O1 In1 O3 83.71(4) . . ?
O6 In1 O3 138.33(5) . . ?
O1 In1 O2 75.50(4) . . ?
O6 In1 O2 87.02(4) . . ?
O3 In1 O2 129.94(5) . . ?
O1 In1 O4 140.59(5) . . ?
O6 In1 O4 85.85(5) . . ?
O3 In1 O4 75.02(4) . . ?
O2 In1 O4 93.18(4) . . ?
O1 In1 O5 86.59(5) . . ?
O6 In1 O5 74.84(4) . . ?
O3 In1 O5 85.26(5) . . ?
O2 In1 O5 136.79(5) . . ?
O4 In1 O5 123.35(5) . . ?
C1 O1 In1 115.73(10) . . ?
C2 O2 In1 114.74(10) . . ?
C15 O3 In1 115.93(10) . . ?
C16 O4 In1 115.32(10) . . ?
C29 O5 In1 115.06(11) . . ?
C30 O6 In1 115.62(10) . . ?
O1 C1 C6 121.98(15) . . ?
O1 C1 C2 116.89(15) . . ?
C6 C1 C2 121.13(15) . . ?
O2 C2 C3 123.01(15) . . ?
O2 C2 C1 116.83(15) . . ?
C3 C2 C1 120.16(15) . . ?
C4 C3 C2 115.88(16) . . ?
C4 C3 C7 123.22(16) . . ?
C2 C3 C7 120.90(15) . . ?
C3 C4 C5 123.99(17) . . ?
C6 C5 C4 123.02(17) . . ?
C5 C6 C1 115.65(16) . . ?
C5 C6 C11 124.36(16) . . ?
C1 C6 C11 119.97(15) . . ?
C3 C7 C8 109.27(15) . . ?
C3 C7 C9 111.00(15) . . ?
C8 C7 C9 109.23(16) . . ?
C3 C7 C10 110.67(15) . . ?
C8 C7 C10 108.71(16) . . ?
C9 C7 C10 107.91(15) . . ?
C12 C11 C6 111.47(15) . . ?
C12 C11 C14 107.46(16) . . ?
C6 C11 C14 109.48(15) . . ?
C12 C11 C13 108.59(15) . . ?
C6 C11 C13 109.86(15) . . ?
C14 C11 C13 109.93(16) . . ?
O3 C15 C20 122.50(15) . . ?
O3 C15 C16 116.70(14) . . ?
C20 C15 C16 120.79(15) . . ?
O4 C16 C17 123.50(15) . . ?
O4 C16 C15 116.36(14) . . ?
C17 C16 C15 120.14(15) . . ?
C18 C17 C16 116.17(15) . . ?
C18 C17 C21 122.44(16) . . ?
C16 C17 C21 121.32(15) . . ?
C17 C18 C19 123.51(16) . . ?
C20 C19 C18 123.47(16) . . ?
C19 C20 C15 115.87(15) . . ?
C19 C20 C25 124.05(15) . . ?
C15 C20 C25 120.09(15) . . ?
C24 C21 C17 111.23(14) . . ?
C24 C21 C22 108.60(15) . . ?
C17 C21 C22 108.73(14) . . ?
C24 C21 C23 107.77(15) . . ?
C17 C21 C23 111.15(14) . . ?
C22 C21 C23 109.31(15) . . ?
C20 C25 C26 110.89(15) . . ?
C20 C25 C27 109.58(15) . . ?
C26 C25 C27 109.22(15) . . ?
C20 C25 C28 110.42(14) . . ?
C26 C25 C28 106.81(15) . . ?
C27 C25 C28 109.87(15) . . ?
O5 C29 C34 124.13(15) . . ?
O5 C29 C30 116.59(15) . . ?
C34 C29 C30 119.29(15) . . ?
O6 C30 C31 122.76(15) . . ?
O6 C30 C29 115.96(15) . . ?
C31 C30 C29 121.28(16) . . ?
C32 C31 C30 115.68(16) . . ?
C32 C31 C35 124.09(16) . . ?
C30 C31 C35 120.20(16) . . ?
C31 C32 C33 123.54(17) . . ?
C34 C33 C32 123.42(17) . . ?
C33 C34 C29 116.52(16) . . ?
C33 C34 C39 123.02(16) . . ?
C29 C34 C39 120.46(15) . . ?
C31 C35 C38 111.37(16) . . ?
C31 C35 C37 111.25(15) . . ?
C38 C35 C37 108.21(15) . . ?
C31 C35 C36 108.59(15) . . ?
C38 C35 C36 107.68(15) . . ?
C37 C35 C36 109.66(16) . . ?
C42 C39 C40 108.28(15) . . ?
C42 C39 C41 107.62(15) . . ?
C40 C39 C41 110.00(15) . . ?
C42 C39 C34 111.41(14) . . ?
C40 C39 C34 108.56(14) . . ?
C41 C39 C34 110.93(14) . . ?
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full 26.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max 0.720
_refine_diff_density_min -0.263
_refine_diff_density_rms 0.063
_publ_section_references
;
Bruker (2000) SAINTPlus Data Reduction and Correction Program v. 6.02a, Bruker
AXS, Madison, Wisconsin, USA.
Bruker (2000) SMART. Bruker Molecular Analysis Research Tool,
v. 5.625 Bruker AXS, Madison, Wisconsin, USA.
Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector
Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA.
Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software
Suite, Bruker AXS, Madison, Wisconsin, USA.
;
# Attachment '- Complex_2.cif'
data_insqdpm
_database_code_depnum_ccdc_archive 'CCDC 780470'
#TrackingRef '- Complex_2.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C52 H64 In N2 O4'
_chemical_formula_weight 895.87
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'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M P2(1)2(1)2(1)
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 11.0275(5)
_cell_length_b 18.7637(8)
_cell_length_c 23.0694(10)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 4773.4(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 900
_cell_measurement_theta_min 2
_cell_measurement_theta_max 30
_exptl_crystal_description prism
_exptl_crystal_colour green
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.247
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1884
_exptl_absorpt_coefficient_mu 0.539
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8337
_exptl_absorpt_correction_T_max 0.9235
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 31166
_diffrn_reflns_av_R_equivalents 0.0391
_diffrn_reflns_av_sigmaI/netI 0.0453
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 2.05
_diffrn_reflns_theta_max 27.00
_reflns_number_total 10394
_reflns_number_gt 9294
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SHELXTL'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0361P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.574(15)
_refine_ls_number_reflns 10394
_refine_ls_number_parameters 547
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0428
_refine_ls_R_factor_gt 0.0347
_refine_ls_wR_factor_ref 0.0739
_refine_ls_wR_factor_gt 0.0712
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_restrained_S_all 1.038
_refine_ls_shift/su_max 0.002
_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
In1 In 0.593190(14) 0.737028(9) 0.243947(7) 0.02338(5) Uani 1 1 d . . .
O1 O 0.69859(16) 0.80559(9) 0.29345(8) 0.0274(4) Uani 1 1 d . . .
O2 O 0.70431(17) 0.66302(10) 0.28397(9) 0.0285(4) Uani 1 1 d . . .
O3 O 0.60107(19) 0.81087(9) 0.17105(7) 0.0269(4) Uani 1 1 d . . .
O4 O 0.60916(19) 0.67104(9) 0.16576(8) 0.0285(4) Uani 1 1 d . . .
N1 N 0.4288(2) 0.80254(12) 0.27132(10) 0.0282(5) Uani 1 1 d . . .
N2 N 0.43369(19) 0.66327(11) 0.26180(11) 0.0281(5) Uani 1 1 d . . .
C1 C 0.7829(2) 0.76999(16) 0.32460(11) 0.0254(6) Uani 1 1 d . . .
C2 C 0.7856(2) 0.69450(15) 0.31952(12) 0.0255(6) Uani 1 1 d . . .
C3 C 0.8714(2) 0.65396(15) 0.35041(12) 0.0259(6) Uani 1 1 d . . .
C4 C 0.9512(3) 0.69095(17) 0.38628(13) 0.0329(7) Uani 1 1 d . . .
H4A H 1.0104 0.6650 0.4075 0.039 Uiso 1 1 calc R . .
C5 C 0.9468(2) 0.76402(17) 0.39199(12) 0.0318(6) Uani 1 1 d . . .
H5A H 1.0027 0.7868 0.4173 0.038 Uiso 1 1 calc R . .
C6 C 0.8634(2) 0.80557(15) 0.36199(13) 0.0277(7) Uani 1 1 d . . .
C7 C 0.8738(2) 0.57212(15) 0.34357(13) 0.0311(7) Uani 1 1 d . . .
C8 C 0.8959(3) 0.55178(16) 0.27980(13) 0.0378(7) Uani 1 1 d . . .
H8A H 0.9017 0.4998 0.2764 0.057 Uiso 1 1 calc R . .
H8B H 0.9717 0.5735 0.2664 0.057 Uiso 1 1 calc R . .
H8C H 0.8285 0.5690 0.2560 0.057 Uiso 1 1 calc R . .
C9 C 0.7532(3) 0.53997(17) 0.36386(15) 0.0393(8) Uani 1 1 d . . .
H9A H 0.7561 0.4880 0.3597 0.059 Uiso 1 1 calc R . .
H9B H 0.6869 0.5591 0.3402 0.059 Uiso 1 1 calc R . .
H9C H 0.7396 0.5523 0.4046 0.059 Uiso 1 1 calc R . .
C10 C 0.9742(3) 0.53853(17) 0.38054(15) 0.0412(8) Uani 1 1 d . . .
H10A H 0.9771 0.4871 0.3733 0.062 Uiso 1 1 calc R . .
H10B H 0.9573 0.5471 0.4217 0.062 Uiso 1 1 calc R . .
H10C H 1.0524 0.5599 0.3703 0.062 Uiso 1 1 calc R . .
C11 C 0.8575(3) 0.88721(16) 0.36875(14) 0.0320(7) Uani 1 1 d . . .
C12 C 0.8785(3) 0.92325(16) 0.30924(14) 0.0390(8) Uani 1 1 d . . .
H12A H 0.9562 0.9073 0.2932 0.059 Uiso 1 1 calc R . .
H12B H 0.8799 0.9751 0.3142 0.059 Uiso 1 1 calc R . .
H12C H 0.8128 0.9102 0.2827 0.059 Uiso 1 1 calc R . .
C13 C 0.9532(3) 0.91558(17) 0.41076(14) 0.0392(8) Uani 1 1 d . . .
H13A H 0.9404 0.8945 0.4491 0.059 Uiso 1 1 calc R . .
H13B H 0.9463 0.9675 0.4134 0.059 Uiso 1 1 calc R . .
H13C H 1.0341 0.9029 0.3966 0.059 Uiso 1 1 calc R . .
C14 C 0.7325(3) 0.90976(19) 0.39246(15) 0.0420(8) Uani 1 1 d . . .
H14A H 0.7200 0.8884 0.4308 0.063 Uiso 1 1 calc R . .
H14B H 0.6688 0.8934 0.3660 0.063 Uiso 1 1 calc R . .
H14C H 0.7292 0.9618 0.3957 0.063 Uiso 1 1 calc R . .
C15 C 0.6175(2) 0.78298(15) 0.12076(12) 0.0262(6) Uani 1 1 d . . .
C16 C 0.6219(2) 0.70493(15) 0.11786(12) 0.0276(6) Uani 1 1 d . . .
C17 C 0.6426(3) 0.66914(17) 0.06377(14) 0.0358(7) Uani 1 1 d . . .
C18 C 0.6513(4) 0.71271(19) 0.01649(15) 0.0525(10) Uani 1 1 d . . .
H18A H 0.6628 0.6913 -0.0204 0.063 Uiso 1 1 calc R . .
C19 C 0.6444(3) 0.78777(18) 0.01942(15) 0.0502(9) Uani 1 1 d . . .
H19A H 0.6498 0.8138 -0.0158 0.060 Uiso 1 1 calc R . .
C20 C 0.6304(3) 0.82526(16) 0.06948(13) 0.0346(7) Uani 1 1 d . . .
C21 C 0.6543(3) 0.58788(17) 0.06172(14) 0.0420(8) Uani 1 1 d . . .
C22 C 0.6777(5) 0.5629(2) -0.00118(15) 0.0706(14) Uani 1 1 d . . .
H22A H 0.6081 0.5756 -0.0255 0.106 Uiso 1 1 calc R . .
H22B H 0.6890 0.5111 -0.0017 0.106 Uiso 1 1 calc R . .
H22C H 0.7508 0.5862 -0.0162 0.106 Uiso 1 1 calc R . .
C23 C 0.5372(3) 0.55279(19) 0.08218(16) 0.0507(9) Uani 1 1 d . . .
H23A H 0.5203 0.5672 0.1222 0.076 Uiso 1 1 calc R . .
H23B H 0.5458 0.5009 0.0804 0.076 Uiso 1 1 calc R . .
H23C H 0.4700 0.5678 0.0571 0.076 Uiso 1 1 calc R . .
C24 C 0.7607(3) 0.56349(19) 0.09981(16) 0.0501(10) Uani 1 1 d . . .
H24A H 0.7455 0.5773 0.1401 0.075 Uiso 1 1 calc R . .
H24B H 0.8357 0.5860 0.0862 0.075 Uiso 1 1 calc R . .
H24C H 0.7689 0.5116 0.0974 0.075 Uiso 1 1 calc R . .
C25 C 0.6315(3) 0.90645(17) 0.07279(14) 0.0405(8) Uani 1 1 d . . .
C26 C 0.6457(4) 0.9400(2) 0.01167(16) 0.0664(13) Uani 1 1 d . . .
H26A H 0.5777 0.9252 -0.0129 0.100 Uiso 1 1 calc R . .
H26B H 0.7220 0.9239 -0.0057 0.100 Uiso 1 1 calc R . .
H26C H 0.6462 0.9921 0.0150 0.100 Uiso 1 1 calc R . .
C27 C 0.7402(4) 0.93039(19) 0.10935(17) 0.0484(10) Uani 1 1 d . . .
H27A H 0.7314 0.9123 0.1490 0.073 Uiso 1 1 calc R . .
H27B H 0.7437 0.9826 0.1101 0.073 Uiso 1 1 calc R . .
H27C H 0.8151 0.9116 0.0923 0.073 Uiso 1 1 calc R . .
C28 C 0.5131(3) 0.93441(19) 0.09916(17) 0.0529(10) Uani 1 1 d . . .
H28A H 0.5031 0.9149 0.1383 0.079 Uiso 1 1 calc R . .
H28B H 0.4446 0.9196 0.0749 0.079 Uiso 1 1 calc R . .
H28C H 0.5159 0.9866 0.1011 0.079 Uiso 1 1 calc R . .
C29 C 0.4366(3) 0.87370(16) 0.27562(15) 0.0395(8) Uani 1 1 d . . .
H29A H 0.5108 0.8965 0.2659 0.047 Uiso 1 1 calc R . .
C30 C 0.3404(3) 0.91471(18) 0.29374(16) 0.0464(9) Uani 1 1 d . . .
H30A H 0.3474 0.9651 0.2965 0.056 Uiso 1 1 calc R . .
C31 C 0.2338(3) 0.88069(18) 0.30780(15) 0.0430(8) Uani 1 1 d . . .
H31A H 0.1657 0.9078 0.3201 0.052 Uiso 1 1 calc R . .
C32 C 0.2252(3) 0.80822(18) 0.30424(13) 0.0370(8) Uani 1 1 d . . .
H32A H 0.1520 0.7846 0.3144 0.044 Uiso 1 1 calc R . .
C33 C 0.3255(2) 0.76944(16) 0.28543(11) 0.0267(6) Uani 1 1 d . . .
C34 C 0.3266(2) 0.69122(15) 0.27841(12) 0.0261(6) Uani 1 1 d . . .
C35 C 0.2274(3) 0.64678(17) 0.28791(13) 0.0343(7) Uani 1 1 d . . .
H35A H 0.1517 0.6663 0.2995 0.041 Uiso 1 1 calc R . .
C36 C 0.2398(3) 0.57437(17) 0.28046(14) 0.0389(8) Uani 1 1 d . . .
H36A H 0.1728 0.5436 0.2869 0.047 Uiso 1 1 calc R . .
C37 C 0.3502(3) 0.54674(16) 0.26358(15) 0.0403(8) Uani 1 1 d . . .
H37A H 0.3604 0.4969 0.2582 0.048 Uiso 1 1 calc R . .
C38 C 0.4451(2) 0.59300(13) 0.25477(14) 0.0335(6) Uani 1 1 d . . .
H38A H 0.5215 0.5743 0.2433 0.040 Uiso 1 1 calc R . .
C1S C 0.4523(3) 0.7876(2) 0.43522(17) 0.0605(11) Uani 1 1 d . . .
H1SA H 0.4898 0.8332 0.4363 0.073 Uiso 1 1 calc R . .
C2S C 0.5150(4) 0.7321(3) 0.41350(18) 0.0811(15) Uani 1 1 d . . .
H2SA H 0.5952 0.7390 0.3995 0.097 Uiso 1 1 calc R . .
C3S C 0.4636(6) 0.6658(3) 0.41149(19) 0.0853(18) Uani 1 1 d . . .
H3SA H 0.5080 0.6263 0.3969 0.102 Uiso 1 1 calc R . .
C4S C 0.3471(5) 0.6573(2) 0.43086(19) 0.0721(14) Uani 1 1 d . . .
H4SA H 0.3096 0.6117 0.4289 0.087 Uiso 1 1 calc R . .
C5S C 0.2836(3) 0.71461(19) 0.45332(15) 0.0472(9) Uani 1 1 d . . .
H5SA H 0.2032 0.7081 0.4671 0.057 Uiso 1 1 calc R . .
C6S C 0.3359(3) 0.78057(17) 0.45587(13) 0.0397(8) Uani 1 1 d . . .
C7S C 0.2695(4) 0.8426(2) 0.48139(19) 0.0744(13) Uani 1 1 d . . .
H7SA H 0.1821 0.8335 0.4802 0.112 Uiso 1 1 calc R . .
H7SB H 0.2879 0.8857 0.4590 0.112 Uiso 1 1 calc R . .
H7SC H 0.2951 0.8494 0.5217 0.112 Uiso 1 1 calc R . .
C8S C 0.1345(4) 0.7948(3) 0.15647(17) 0.0731(13) Uani 1 1 d U . .
H8SA H 0.1091 0.8422 0.1640 0.088 Uiso 1 1 calc R . .
C9S C 0.2540(5) 0.7809(3) 0.1389(2) 0.0874(15) Uani 1 1 d U . .
H9SA H 0.3098 0.8191 0.1344 0.105 Uiso 1 1 calc R . .
C10S C 0.2895(4) 0.7135(4) 0.1283(2) 0.094(2) Uani 1 1 d . . .
H10D H 0.3703 0.7048 0.1159 0.113 Uiso 1 1 calc R . .
C11S C 0.2142(5) 0.6589(3) 0.13482(18) 0.0836(17) Uani 1 1 d . . .
H11A H 0.2417 0.6116 0.1281 0.100 Uiso 1 1 calc R . .
C12S C 0.0951(4) 0.6712(2) 0.15141(15) 0.0609(10) Uani 1 1 d . . .
H12D H 0.0408 0.6321 0.1550 0.073 Uiso 1 1 calc R . .
C13S C 0.0543(3) 0.7392(2) 0.16278(14) 0.0547(10) Uani 1 1 d . . .
C14S C -0.0741(4) 0.7510(3) 0.1815(2) 0.1020(19) Uani 1 1 d . . .
H14D H -0.0785 0.7936 0.2060 0.153 Uiso 1 1 calc R . .
H14E H -0.1023 0.7095 0.2035 0.153 Uiso 1 1 calc R . .
H14F H -0.1255 0.7575 0.1473 0.153 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
In1 0.02043(8) 0.02703(9) 0.02268(9) 0.00027(7) 0.00121(8) 0.00133(7)
O1 0.0272(11) 0.0278(11) 0.0271(11) -0.0015(8) -0.0044(9) 0.0034(8)
O2 0.0270(11) 0.0281(11) 0.0305(11) -0.0010(8) -0.0059(9) 0.0044(8)
O3 0.0296(10) 0.0295(10) 0.0215(10) -0.0003(7) 0.0030(10) 0.0006(9)
O4 0.0350(12) 0.0288(10) 0.0218(10) 0.0005(8) 0.0031(10) 0.0004(9)
N1 0.0257(13) 0.0308(13) 0.0279(13) -0.0007(9) 0.0034(10) 0.0021(9)
N2 0.0251(12) 0.0332(13) 0.0258(12) 0.0035(10) 0.0025(10) 0.0003(9)
C1 0.0200(12) 0.0353(17) 0.0208(13) -0.0007(13) 0.0031(10) 0.0024(13)
C2 0.0230(14) 0.0314(17) 0.0220(15) 0.0016(11) 0.0037(12) 0.0004(12)
C3 0.0200(14) 0.0331(16) 0.0246(15) 0.0046(12) 0.0029(11) 0.0006(11)
C4 0.0262(15) 0.046(2) 0.0270(16) 0.0089(14) -0.0006(12) 0.0047(13)
C5 0.0250(13) 0.0430(16) 0.0273(14) -0.0011(15) -0.0011(11) -0.0032(14)
C6 0.0252(14) 0.0315(17) 0.0263(16) 0.0005(12) 0.0031(12) -0.0041(12)
C7 0.0261(15) 0.0346(17) 0.0326(17) 0.0067(13) 0.0022(12) 0.0046(12)
C8 0.0370(17) 0.0338(16) 0.0427(17) -0.0044(13) 0.0019(16) 0.0063(15)
C9 0.0362(18) 0.0379(19) 0.044(2) 0.0104(15) -0.0009(15) 0.0002(14)
C10 0.0390(18) 0.0386(18) 0.046(2) 0.0072(15) -0.0030(16) 0.0078(15)
C11 0.0311(16) 0.0326(17) 0.0324(17) -0.0045(13) 0.0008(13) -0.0033(13)
C12 0.041(2) 0.0358(17) 0.0401(19) 0.0056(14) -0.0040(15) -0.0085(14)
C13 0.0413(18) 0.0397(19) 0.0366(18) -0.0043(14) -0.0020(14) -0.0081(14)
C14 0.0372(19) 0.040(2) 0.049(2) -0.0120(16) 0.0040(16) -0.0020(16)
C15 0.0201(15) 0.0320(16) 0.0264(15) 0.0014(11) -0.0025(11) -0.0015(11)
C16 0.0252(16) 0.0327(15) 0.0249(15) 0.0000(12) -0.0001(12) -0.0013(11)
C17 0.0461(19) 0.0377(19) 0.0236(17) -0.0045(13) 0.0031(14) -0.0044(14)
C18 0.090(3) 0.045(2) 0.0222(17) -0.0082(14) 0.0078(17) -0.0067(19)
C19 0.084(3) 0.0395(19) 0.0268(18) 0.0078(14) 0.0012(17) -0.0049(18)
C20 0.0416(19) 0.0368(18) 0.0255(17) -0.0002(13) -0.0015(13) -0.0034(13)
C21 0.060(2) 0.0381(19) 0.0280(18) -0.0067(14) 0.0094(16) -0.0003(16)
C22 0.125(4) 0.045(2) 0.042(2) -0.0146(19) 0.017(3) -0.005(2)
C23 0.065(2) 0.040(2) 0.046(2) -0.0078(16) -0.0023(19) -0.0144(18)
C24 0.056(2) 0.042(2) 0.052(2) -0.0069(17) 0.0120(19) 0.0067(17)
C25 0.058(2) 0.0338(18) 0.0294(17) 0.0081(13) -0.0005(15) -0.0013(15)
C26 0.121(4) 0.038(2) 0.040(2) 0.0123(17) -0.003(2) -0.006(2)
C27 0.050(2) 0.038(2) 0.056(2) -0.0008(17) -0.0015(18) -0.0097(17)
C28 0.057(2) 0.040(2) 0.062(3) 0.0118(18) -0.006(2) 0.0113(18)
C29 0.0304(17) 0.0371(18) 0.051(2) 0.0026(14) 0.0063(14) 0.0008(12)
C30 0.047(2) 0.0334(18) 0.059(2) -0.0026(17) 0.0104(18) 0.0080(15)
C31 0.0349(18) 0.051(2) 0.043(2) -0.0035(16) 0.0095(16) 0.0164(15)
C32 0.0268(16) 0.055(2) 0.0292(17) -0.0068(15) 0.0035(14) 0.0046(14)
C33 0.0231(13) 0.0381(16) 0.0189(13) 0.0012(13) 0.0001(10) 0.0021(12)
C34 0.0231(14) 0.0386(17) 0.0165(13) 0.0019(11) -0.0007(11) 0.0009(11)
C35 0.0261(16) 0.048(2) 0.0291(17) 0.0018(14) 0.0024(13) -0.0017(13)
C36 0.0344(17) 0.0422(19) 0.0401(18) 0.0003(15) 0.0059(15) -0.0109(14)
C37 0.0373(16) 0.0341(16) 0.050(2) -0.0028(15) 0.0038(16) -0.0057(12)
C38 0.0310(14) 0.0312(15) 0.0383(17) -0.0014(15) 0.0036(14) 0.0002(10)
C1S 0.053(2) 0.076(3) 0.052(2) 0.019(2) -0.0048(19) -0.018(2)
C2S 0.059(3) 0.141(5) 0.043(2) 0.020(3) 0.014(2) 0.029(3)
C3S 0.119(5) 0.097(4) 0.040(3) -0.019(3) -0.016(3) 0.067(4)
C4S 0.111(4) 0.048(3) 0.057(3) 0.002(2) -0.037(3) 0.005(3)
C5S 0.046(2) 0.054(2) 0.041(2) 0.0081(16) -0.0091(16) -0.0086(17)
C6S 0.0459(19) 0.043(2) 0.0297(18) -0.0008(14) -0.0095(15) 0.0027(15)
C7S 0.088(3) 0.065(3) 0.069(3) -0.018(2) -0.028(3) 0.021(3)
C8S 0.085(3) 0.097(3) 0.037(2) 0.014(2) -0.017(2) -0.026(3)
C9S 0.086(3) 0.127(4) 0.049(3) 0.024(3) -0.023(2) -0.053(3)
C10S 0.044(3) 0.192(7) 0.047(3) 0.017(4) -0.009(2) -0.004(4)
C11S 0.081(4) 0.136(5) 0.034(2) -0.004(3) -0.017(2) 0.047(3)
C12S 0.067(3) 0.080(3) 0.0349(19) 0.0095(17) -0.019(2) -0.005(3)
C13S 0.0432(19) 0.087(3) 0.0342(17) 0.011(2) 0.0013(14) 0.008(2)
C14S 0.061(3) 0.175(6) 0.070(3) 0.006(3) 0.017(2) 0.027(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds 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
In1 O2 2.0694(18) . ?
In1 O1 2.0761(18) . ?
In1 O3 2.1806(17) . ?
In1 O4 2.1948(18) . ?
In1 N2 2.276(2) . ?
In1 N1 2.279(2) . ?
O1 C1 1.352(3) . ?
O2 C2 1.351(3) . ?
O3 C15 1.285(3) . ?
O4 C16 1.283(3) . ?
N1 C33 1.338(3) . ?
N1 C29 1.342(4) . ?
N2 C38 1.335(3) . ?
N2 C34 1.347(3) . ?
C1 C6 1.406(4) . ?
C1 C2 1.422(4) . ?
C2 C3 1.407(4) . ?
C3 C4 1.393(4) . ?
C3 C7 1.544(4) . ?
C4 C5 1.378(4) . ?
C5 C6 1.390(4) . ?
C6 C11 1.541(4) . ?
C7 C9 1.533(4) . ?
C7 C10 1.533(4) . ?
C7 C8 1.539(4) . ?
C11 C13 1.528(4) . ?
C11 C14 1.542(4) . ?
C11 C12 1.548(4) . ?
C15 C20 1.431(4) . ?
C15 C16 1.467(4) . ?
C16 C17 1.435(4) . ?
C17 C18 1.367(5) . ?
C17 C21 1.531(4) . ?
C18 C19 1.412(5) . ?
C19 C20 1.361(5) . ?
C20 C25 1.525(4) . ?
C21 C23 1.524(5) . ?
C21 C24 1.536(5) . ?
C21 C22 1.547(4) . ?
C25 C28 1.533(5) . ?
C25 C27 1.533(5) . ?
C25 C26 1.552(5) . ?
C29 C30 1.375(4) . ?
C30 C31 1.377(5) . ?
C31 C32 1.366(5) . ?
C32 C33 1.393(4) . ?
C33 C34 1.477(4) . ?
C34 C35 1.393(4) . ?
C35 C36 1.376(4) . ?
C36 C37 1.379(4) . ?
C37 C38 1.375(4) . ?
C1S C2S 1.347(6) . ?
C1S C6S 1.376(5) . ?
C2S C3S 1.368(7) . ?
C3S C4S 1.369(7) . ?
C4S C5S 1.384(6) . ?
C5S C6S 1.366(5) . ?
C6S C7S 1.496(5) . ?
C8S C13S 1.374(6) . ?
C8S C9S 1.403(7) . ?
C9S C10S 1.347(8) . ?
C10S C11S 1.328(7) . ?
C11S C12S 1.388(6) . ?
C12S C13S 1.379(5) . ?
C13S C14S 1.497(5) . ?
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
O2 In1 O1 80.73(7) . . ?
O2 In1 O3 138.32(8) . . ?
O1 In1 O3 90.47(7) . . ?
O2 In1 O4 86.59(7) . . ?
O1 In1 O4 139.17(7) . . ?
O3 In1 O4 73.83(6) . . ?
O2 In1 N2 88.21(8) . . ?
O1 In1 N2 135.24(8) . . ?
O3 In1 N2 123.83(8) . . ?
O4 In1 N2 82.40(8) . . ?
O2 In1 N1 135.17(8) . . ?
O1 In1 N1 87.63(8) . . ?
O3 In1 N1 84.42(8) . . ?
O4 In1 N1 126.56(8) . . ?
N2 In1 N1 70.32(7) . . ?
C1 O1 In1 111.80(16) . . ?
C2 O2 In1 111.74(16) . . ?
C15 O3 In1 116.30(17) . . ?
C16 O4 In1 115.92(17) . . ?
C33 N1 C29 119.9(2) . . ?
C33 N1 In1 119.63(18) . . ?
C29 N1 In1 120.41(18) . . ?
C38 N2 C34 120.1(2) . . ?
C38 N2 In1 120.39(16) . . ?
C34 N2 In1 119.47(17) . . ?
O1 C1 C6 121.7(3) . . ?
O1 C1 C2 117.6(2) . . ?
C6 C1 C2 120.7(3) . . ?
O2 C2 C3 121.1(2) . . ?
O2 C2 C1 118.2(2) . . ?
C3 C2 C1 120.7(3) . . ?
C4 C3 C2 117.1(3) . . ?
C4 C3 C7 123.0(2) . . ?
C2 C3 C7 119.8(2) . . ?
C5 C4 C3 122.0(3) . . ?
C4 C5 C6 122.2(3) . . ?
C5 C6 C1 117.2(3) . . ?
C5 C6 C11 122.4(3) . . ?
C1 C6 C11 120.5(3) . . ?
C9 C7 C10 107.1(2) . . ?
C9 C7 C8 109.4(3) . . ?
C10 C7 C8 108.4(2) . . ?
C9 C7 C3 110.2(2) . . ?
C10 C7 C3 111.4(2) . . ?
C8 C7 C3 110.3(2) . . ?
C13 C11 C6 112.4(3) . . ?
C13 C11 C14 107.3(3) . . ?
C6 C11 C14 110.3(2) . . ?
C13 C11 C12 107.9(2) . . ?
C6 C11 C12 109.8(2) . . ?
C14 C11 C12 109.2(3) . . ?
O3 C15 C20 122.3(3) . . ?
O3 C15 C16 116.9(3) . . ?
C20 C15 C16 120.8(3) . . ?
O4 C16 C17 122.3(3) . . ?
O4 C16 C15 116.9(3) . . ?
C17 C16 C15 120.8(3) . . ?
C18 C17 C16 115.2(3) . . ?
C18 C17 C21 124.4(3) . . ?
C16 C17 C21 120.4(3) . . ?
C17 C18 C19 123.7(3) . . ?
C20 C19 C18 124.2(3) . . ?
C19 C20 C15 115.2(3) . . ?
C19 C20 C25 123.9(3) . . ?
C15 C20 C25 120.9(3) . . ?
C23 C21 C17 110.4(3) . . ?
C23 C21 C24 110.0(3) . . ?
C17 C21 C24 110.1(3) . . ?
C23 C21 C22 107.5(3) . . ?
C17 C21 C22 110.2(3) . . ?
C24 C21 C22 108.6(3) . . ?
C20 C25 C28 110.8(3) . . ?
C20 C25 C27 109.0(3) . . ?
C28 C25 C27 110.3(3) . . ?
C20 C25 C26 111.1(3) . . ?
C28 C25 C26 107.9(3) . . ?
C27 C25 C26 107.6(3) . . ?
N1 C29 C30 122.0(3) . . ?
C29 C30 C31 118.1(3) . . ?
C32 C31 C30 120.4(3) . . ?
C31 C32 C33 118.9(3) . . ?
N1 C33 C32 120.6(3) . . ?
N1 C33 C34 115.3(2) . . ?
C32 C33 C34 124.1(3) . . ?
N2 C34 C35 120.0(3) . . ?
N2 C34 C33 115.2(2) . . ?
C35 C34 C33 124.8(3) . . ?
C36 C35 C34 119.6(3) . . ?
C35 C36 C37 119.6(3) . . ?
C38 C37 C36 118.5(3) . . ?
N2 C38 C37 122.3(3) . . ?
C2S C1S C6S 122.2(4) . . ?
C1S C2S C3S 120.2(4) . . ?
C2S C3S C4S 119.0(4) . . ?
C3S C4S C5S 120.3(4) . . ?
C6S C5S C4S 120.5(4) . . ?
C5S C6S C1S 117.8(3) . . ?
C5S C6S C7S 121.0(3) . . ?
C1S C6S C7S 121.2(4) . . ?
C13S C8S C9S 119.7(5) . . ?
C10S C9S C8S 119.9(5) . . ?
C11S C10S C9S 121.5(5) . . ?
C10S C11S C12S 119.7(5) . . ?
C13S C12S C11S 121.0(4) . . ?
C8S C13S C12S 118.2(4) . . ?
C8S C13S C14S 121.8(5) . . ?
C12S C13S C14S 120.0(4) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 27.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 1.066
_refine_diff_density_min -0.282
_refine_diff_density_rms 0.063
_publ_section_references
;
Bruker (2000) SAINTPlus Data Reduction and Correction Program v. 6.02a, Bruker
AXS, Madison, Wisconsin, USA.
Bruker (2000) SMART. Bruker Molecular Analysis Research Tool,
v. 5.625 Bruker AXS, Madison, Wisconsin, USA.
Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector
Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA.
Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software
Suite, Bruker AXS, Madison, Wisconsin, USA.
;
# Attachment '- Complex_3.cif'
data_incat1m
_database_code_depnum_ccdc_archive 'CCDC 780471'
#TrackingRef '- Complex_3.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C42 H76 In K N2 O8'
_chemical_formula_weight 890.97
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M C2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 17.0349(5)
_cell_length_b 17.2131(5)
_cell_length_c 16.1378(5)
_cell_angle_alpha 90.00
_cell_angle_beta 98.1120(10)
_cell_angle_gamma 90.00
_cell_volume 4684.6(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 900
_cell_measurement_theta_min 2
_cell_measurement_theta_max 29
_exptl_crystal_description stick
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.263
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1896
_exptl_absorpt_coefficient_mu 0.641
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7612
_exptl_absorpt_correction_T_max 0.9387
_exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 22340
_diffrn_reflns_av_R_equivalents 0.0177
_diffrn_reflns_av_sigmaI/netI 0.0159
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 2.37
_diffrn_reflns_theta_max 27.50
_reflns_number_total 5381
_reflns_number_gt 5044
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SHELXTL'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0335P)^2^+2.5314P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary patt
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_ls_hydrogen_treatment refall
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5381
_refine_ls_number_parameters 397
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0247
_refine_ls_R_factor_gt 0.0224
_refine_ls_wR_factor_ref 0.0561
_refine_ls_wR_factor_gt 0.0550
_refine_ls_goodness_of_fit_ref 1.052
_refine_ls_restrained_S_all 1.052
_refine_ls_shift/su_max 0.001
_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
In1 In 0.5000 -0.107197(5) -0.2500 0.01909(3) Uani 1 2 d S . .
K1 K 0.5000 -0.312849(18) -0.2500 0.02521(7) Uani 1 2 d S . .
O1 O 0.39304(5) -0.10930(4) -0.19810(5) 0.02212(16) Uani 1 1 d . . .
O2 O 0.52802(4) -0.18559(4) -0.14729(4) 0.02316(16) Uani 1 1 d . . .
C1 C 0.39969(6) -0.14509(6) -0.12323(6) 0.0211(2) Uani 1 1 d . . .
C2 C 0.47256(6) -0.18462(6) -0.09499(6) 0.0210(2) Uani 1 1 d . . .
C3 C 0.48567(7) -0.21865(6) -0.01437(6) 0.0226(2) Uani 1 1 d . . .
C4 C 0.42215(7) -0.21769(6) 0.03166(7) 0.0251(2) Uani 1 1 d . . .
H4 H 0.4279(8) -0.2408(8) 0.0842(9) 0.029(3) Uiso 1 1 d . . .
C5 C 0.35048(7) -0.18172(6) 0.00323(7) 0.0252(2) Uani 1 1 d . . .
H5 H 0.3089(8) -0.1826(8) 0.0369(8) 0.025(3) Uiso 1 1 d . . .
C6 C 0.33800(6) -0.14245(6) -0.07355(6) 0.0222(2) Uani 1 1 d . . .
C7 C 0.56636(7) -0.25368(6) 0.02166(7) 0.0268(2) Uani 1 1 d . . .
C8 C 0.63230(8) -0.19353(8) 0.01853(8) 0.0354(3) Uani 1 1 d . . .
H8A H 0.6824(10) -0.2142(9) 0.0403(10) 0.042(4) Uiso 1 1 d . . .
H8B H 0.6240(9) -0.1501(9) 0.0523(10) 0.042(4) Uiso 1 1 d . . .
H8C H 0.6334(9) -0.1758(9) -0.0383(10) 0.038(4) Uiso 1 1 d . . .
C9 C 0.56891(8) -0.27806(8) 0.11357(7) 0.0350(3) Uani 1 1 d . . .
H9A H 0.5300(9) -0.3178(9) 0.1216(9) 0.040(4) Uiso 1 1 d . . .
H9B H 0.6196(10) -0.2974(9) 0.1344(10) 0.040(4) Uiso 1 1 d . . .
H9C H 0.5550(9) -0.2323(9) 0.1511(10) 0.042(4) Uiso 1 1 d . . .
C10 C 0.58386(9) -0.32627(8) -0.02779(8) 0.0387(3) Uani 1 1 d . . .
H10A H 0.6335(10) -0.3512(10) -0.0044(10) 0.047(4) Uiso 1 1 d . . .
H10B H 0.5867(9) -0.3133(9) -0.0838(10) 0.041(4) Uiso 1 1 d . . .
H10C H 0.5444(9) -0.3661(10) -0.0274(10) 0.044(4) Uiso 1 1 d . . .
C11 C 0.26129(7) -0.09660(6) -0.10147(7) 0.0246(2) Uani 1 1 d . . .
C12 C 0.20437(7) -0.10039(7) -0.03602(8) 0.0299(3) Uani 1 1 d . . .
H12A H 0.1866(9) -0.1517(9) -0.0267(9) 0.036(4) Uiso 1 1 d . . .
H12B H 0.2279(8) -0.0789(9) 0.0162(9) 0.035(4) Uiso 1 1 d . . .
H12C H 0.1582(9) -0.0715(9) -0.0549(9) 0.041(4) Uiso 1 1 d . . .
C13 C 0.28103(7) -0.01047(7) -0.11310(7) 0.0286(2) Uani 1 1 d . . .
H13A H 0.3061(9) 0.0128(9) -0.0591(9) 0.040(4) Uiso 1 1 d . . .
H13B H 0.3158(8) -0.0038(8) -0.1527(8) 0.031(3) Uiso 1 1 d . . .
H13C H 0.2354(8) 0.0195(8) -0.1290(9) 0.033(4) Uiso 1 1 d . . .
C14 C 0.21687(7) -0.12925(8) -0.18369(7) 0.0313(3) Uani 1 1 d . . .
H14A H 0.1683(10) -0.1010(8) -0.1988(10) 0.039(4) Uiso 1 1 d . . .
H14B H 0.2012(9) -0.1824(9) -0.1766(10) 0.043(4) Uiso 1 1 d . . .
H14C H 0.2488(8) -0.1266(8) -0.2275(9) 0.034(4) Uiso 1 1 d . . .
O1S O 0.45998(5) -0.43671(5) -0.16171(6) 0.0353(2) Uani 1 1 d . . .
O2S O 0.34246(5) -0.35610(5) -0.26097(5) 0.0341(2) Uani 1 1 d . . .
C1S C 0.51017(11) -0.50106(8) -0.13839(10) 0.0480(4) Uani 1 1 d . . .
H1SA H 0.4917(10) -0.5468(10) -0.1736(10) 0.054(5) Uiso 1 1 d . . .
H1SB H 0.5098(10) -0.5134(10) -0.0809(11) 0.055(5) Uiso 1 1 d . . .
H1SC H 0.5647(12) -0.4858(12) -0.1458(12) 0.072(6) Uiso 1 1 d . . .
C2S C 0.37926(9) -0.45155(9) -0.15753(9) 0.0436(3) Uani 1 1 d . . .
H2SA H 0.3615(10) -0.4910(11) -0.1975(11) 0.058(5) Uiso 1 1 d . . .
H2SB H 0.3734(11) -0.4705(11) -0.1040(12) 0.064(5) Uiso 1 1 d . . .
C3S C 0.33419(8) -0.37813(9) -0.17779(9) 0.0413(3) Uani 1 1 d . . .
H3SA H 0.2788(11) -0.3868(9) -0.1747(11) 0.052(5) Uiso 1 1 d . . .
H3SB H 0.3548(9) -0.3365(9) -0.1410(10) 0.041(4) Uiso 1 1 d . . .
C4S C 0.29730(9) -0.28834(10) -0.28603(11) 0.0490(4) Uani 1 1 d . . .
H4SA H 0.2430(11) -0.2952(10) -0.2828(11) 0.056(5) Uiso 1 1 d . . .
H4SB H 0.3036(12) -0.2774(11) -0.3419(13) 0.065(6) Uiso 1 1 d . . .
H4SC H 0.3125(11) -0.2434(12) -0.2499(12) 0.066(6) Uiso 1 1 d . . .
N1S N 0.55713(5) 0.00006(5) -0.17253(5) 0.02366(19) Uani 1 1 d . . .
C5S C 0.64337(7) -0.01064(7) -0.14820(7) 0.0297(3) Uani 1 1 d . . .
H5SA H 0.6672(8) 0.0342(8) -0.1156(8) 0.030(3) Uiso 1 1 d . . .
H5SB H 0.6671(8) -0.0159(8) -0.1982(9) 0.032(3) Uiso 1 1 d . . .
H5SC H 0.6530(8) -0.0567(9) -0.1150(9) 0.036(4) Uiso 1 1 d . . .
C6S C 0.52079(7) 0.00969(7) -0.09462(7) 0.0263(2) Uani 1 1 d . . .
H6SA H 0.4666(8) 0.0155(7) -0.1079(8) 0.022(3) Uiso 1 1 d . . .
H6SB H 0.5434(7) 0.0539(8) -0.0636(8) 0.025(3) Uiso 1 1 d . . .
H6SC H 0.5331(7) -0.0357(8) -0.0614(8) 0.024(3) Uiso 1 1 d . . .
C7S C 0.54189(7) 0.06931(6) -0.22683(7) 0.0287(2) Uani 1 1 d . . .
H7SA H 0.5525(9) 0.1166(8) -0.1933(9) 0.031(4) Uiso 1 1 d . . .
H7SB H 0.5789(8) 0.0673(8) -0.2654(8) 0.028(3) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
In1 0.02561(5) 0.01862(5) 0.01330(4) 0.000 0.00360(3) 0.000
K1 0.02627(15) 0.01939(14) 0.03071(16) 0.000 0.00663(12) 0.000
O1 0.0254(3) 0.0259(4) 0.0150(3) 0.0041(3) 0.0028(3) -0.0002(3)
O2 0.0287(4) 0.0237(3) 0.0176(3) 0.0024(3) 0.0048(3) 0.0028(3)
C1 0.0279(5) 0.0199(4) 0.0152(4) 0.0000(4) 0.0025(4) -0.0058(4)
C2 0.0288(5) 0.0174(4) 0.0167(4) -0.0010(4) 0.0027(4) -0.0038(4)
C3 0.0317(5) 0.0175(4) 0.0175(5) 0.0001(4) -0.0002(4) -0.0047(4)
C4 0.0375(6) 0.0210(5) 0.0167(5) 0.0023(4) 0.0041(4) -0.0066(4)
C5 0.0323(5) 0.0247(5) 0.0200(5) 0.0000(4) 0.0082(4) -0.0078(4)
C6 0.0259(5) 0.0217(5) 0.0188(4) -0.0003(4) 0.0031(4) -0.0056(4)
C7 0.0358(6) 0.0239(5) 0.0192(5) 0.0033(4) -0.0011(4) -0.0004(4)
C8 0.0313(6) 0.0385(6) 0.0340(6) 0.0097(5) -0.0036(5) -0.0031(5)
C9 0.0445(7) 0.0371(6) 0.0215(5) 0.0084(5) -0.0018(5) 0.0010(5)
C10 0.0548(8) 0.0315(6) 0.0277(6) 0.0002(5) -0.0019(5) 0.0124(6)
C11 0.0250(5) 0.0291(5) 0.0202(5) 0.0005(4) 0.0045(4) -0.0038(4)
C12 0.0274(5) 0.0367(6) 0.0265(5) 0.0004(5) 0.0074(4) -0.0043(5)
C13 0.0304(5) 0.0283(5) 0.0281(5) 0.0025(4) 0.0081(4) 0.0001(4)
C14 0.0280(5) 0.0402(6) 0.0249(5) -0.0030(5) 0.0005(4) -0.0024(5)
O1S 0.0398(4) 0.0248(4) 0.0431(5) 0.0046(3) 0.0122(4) 0.0001(3)
O2S 0.0311(4) 0.0435(5) 0.0283(4) -0.0042(4) 0.0062(3) -0.0032(4)
C1S 0.0736(10) 0.0314(6) 0.0415(7) 0.0095(6) 0.0173(7) 0.0143(7)
C2S 0.0506(7) 0.0452(7) 0.0387(7) 0.0026(6) 0.0194(6) -0.0152(6)
C3S 0.0336(6) 0.0590(8) 0.0342(6) -0.0012(6) 0.0152(5) -0.0031(6)
C4S 0.0344(7) 0.0639(10) 0.0470(8) 0.0007(7) -0.0003(6) 0.0085(7)
N1S 0.0318(5) 0.0238(4) 0.0164(4) -0.0016(3) 0.0069(3) -0.0037(4)
C5S 0.0313(5) 0.0359(6) 0.0223(5) -0.0062(5) 0.0052(4) -0.0081(5)
C6S 0.0362(6) 0.0260(5) 0.0183(5) -0.0051(4) 0.0099(4) -0.0063(4)
C7S 0.0445(6) 0.0219(5) 0.0218(5) -0.0017(4) 0.0112(5) -0.0068(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds 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
In1 O1 2.1103(8) 2_654 ?
In1 O1 2.1103(8) . ?
In1 O2 2.1384(7) 2_654 ?
In1 O2 2.1384(7) . ?
In1 N1S 2.3611(9) 2_654 ?
In1 N1S 2.3612(9) . ?
In1 K1 3.5399(3) . ?
K1 O1S 2.7046(9) 2_654 ?
K1 O1S 2.7046(9) . ?
K1 O2 2.7477(8) 2_654 ?
K1 O2 2.7478(8) . ?
K1 O2S 2.7665(9) . ?
K1 O2S 2.7665(9) 2_654 ?
K1 C3S 3.3952(14) 2_654 ?
K1 C3S 3.3952(14) . ?
K1 C2 3.4174(10) 2_654 ?
K1 C2 3.4174(10) . ?
K1 C4S 3.4457(15) . ?
K1 C4S 3.4457(15) 2_654 ?
O1 C1 1.3468(12) . ?
O2 C2 1.3530(13) . ?
C1 C6 1.4095(15) . ?
C1 C2 1.4324(15) . ?
C2 C3 1.4154(14) . ?
C3 C4 1.3965(16) . ?
C3 C7 1.5380(16) . ?
C4 C5 1.3879(16) . ?
C5 C6 1.4011(15) . ?
C6 C11 1.5387(15) . ?
C7 C8 1.5337(17) . ?
C7 C10 1.5344(17) . ?
C7 C9 1.5362(16) . ?
C11 C12 1.5326(16) . ?
C11 C13 1.5375(16) . ?
C11 C14 1.5381(16) . ?
O1S C2S 1.4095(17) . ?
O1S C1S 1.4172(17) . ?
O2S C3S 1.4209(16) . ?
O2S C4S 1.4241(18) . ?
C2S C3S 1.491(2) . ?
N1S C5S 1.4778(15) . ?
N1S C7S 1.4806(14) . ?
N1S C6S 1.4869(13) . ?
C7S C7S 1.515(2) 2_654 ?
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
O1 In1 O1 178.04(4) 2_654 . ?
O1 In1 O2 78.02(3) 2_654 2_654 ?
O1 In1 O2 100.72(3) . 2_654 ?
O1 In1 O2 100.72(3) 2_654 . ?
O1 In1 O2 78.02(3) . . ?
O2 In1 O2 101.75(4) 2_654 . ?
O1 In1 N1S 96.76(3) 2_654 2_654 ?
O1 In1 N1S 84.79(3) . 2_654 ?
O2 In1 N1S 93.02(3) 2_654 2_654 ?
O2 In1 N1S 159.08(3) . 2_654 ?
O1 In1 N1S 84.79(3) 2_654 . ?
O1 In1 N1S 96.76(3) . . ?
O2 In1 N1S 159.08(3) 2_654 . ?
O2 In1 N1S 93.02(3) . . ?
N1S In1 N1S 77.13(4) 2_654 . ?
O1 In1 K1 89.018(19) 2_654 . ?
O1 In1 K1 89.017(19) . . ?
O2 In1 K1 50.87(2) 2_654 . ?
O2 In1 K1 50.87(2) . . ?
N1S In1 K1 141.43(2) 2_654 . ?
N1S In1 K1 141.43(2) . . ?
O1S K1 O1S 75.94(4) 2_654 . ?
O1S K1 O2 110.24(2) 2_654 2_654 ?
O1S K1 O2 155.64(2) . 2_654 ?
O1S K1 O2 155.64(2) 2_654 . ?
O1S K1 O2 110.24(2) . . ?
O2 K1 O2 74.27(3) 2_654 . ?
O1S K1 O2S 93.93(3) 2_654 . ?
O1S K1 O2S 60.48(3) . . ?
O2 K1 O2S 95.25(2) 2_654 . ?
O2 K1 O2S 109.73(2) . . ?
O1S K1 O2S 60.48(3) 2_654 2_654 ?
O1S K1 O2S 93.93(3) . 2_654 ?
O2 K1 O2S 109.72(2) 2_654 2_654 ?
O2 K1 O2S 95.25(2) . 2_654 ?
O2S K1 O2S 148.78(4) . 2_654 ?
O1S K1 C3S 43.49(3) 2_654 2_654 ?
O1S K1 C3S 101.75(3) . 2_654 ?
O2 K1 C3S 97.99(3) 2_654 2_654 ?
O2 K1 C3S 112.88(3) . 2_654 ?
O2S K1 C3S 137.35(3) . 2_654 ?
O2S K1 C3S 24.00(3) 2_654 2_654 ?
O1S K1 C3S 101.75(3) 2_654 . ?
O1S K1 C3S 43.49(3) . . ?
O2 K1 C3S 112.88(3) 2_654 . ?
O2 K1 C3S 97.99(3) . . ?
O2S K1 C3S 24.00(3) . . ?
O2S K1 C3S 137.35(3) 2_654 . ?
C3S K1 C3S 141.35(5) 2_654 . ?
O1S K1 C2 93.03(3) 2_654 2_654 ?
O1S K1 C2 164.91(3) . 2_654 ?
O2 K1 C2 22.12(2) 2_654 2_654 ?
O2 K1 C2 84.06(2) . 2_654 ?
O2S K1 C2 111.02(3) . 2_654 ?
O2S K1 C2 89.37(3) 2_654 2_654 ?
C3S K1 C2 75.89(3) 2_654 2_654 ?
C3S K1 C2 132.17(3) . 2_654 ?
O1S K1 C2 164.91(3) 2_654 . ?
O1S K1 C2 93.03(3) . . ?
O2 K1 C2 84.06(2) 2_654 . ?
O2 K1 C2 22.12(2) . . ?
O2S K1 C2 89.37(3) . . ?
O2S K1 C2 111.01(3) 2_654 . ?
C3S K1 C2 132.17(3) 2_654 . ?
C3S K1 C2 75.89(3) . . ?
C2 K1 C2 99.53(3) 2_654 . ?
O1S K1 C4S 109.19(4) 2_654 . ?
O1S K1 C4S 82.20(4) . . ?
O2 K1 C4S 73.50(3) 2_654 . ?
O2 K1 C4S 95.10(3) . . ?
O2S K1 C4S 23.39(3) . . ?
O2S K1 C4S 169.65(4) 2_654 . ?
C3S K1 C4S 147.67(4) 2_654 . ?
C3S K1 C4S 40.18(4) . . ?
C2 K1 C4S 91.99(3) 2_654 . ?
C2 K1 C4S 78.88(3) . . ?
O1S K1 C4S 82.20(4) 2_654 2_654 ?
O1S K1 C4S 109.19(4) . 2_654 ?
O2 K1 C4S 95.10(3) 2_654 2_654 ?
O2 K1 C4S 73.50(3) . 2_654 ?
O2S K1 C4S 169.65(4) . 2_654 ?
O2S K1 C4S 23.39(3) 2_654 2_654 ?
C3S K1 C4S 40.19(4) 2_654 2_654 ?
C3S K1 C4S 147.67(4) . 2_654 ?
C2 K1 C4S 78.88(3) 2_654 2_654 ?
C2 K1 C4S 91.99(3) . 2_654 ?
C4S K1 C4S 165.93(6) . 2_654 ?
C1 O1 In1 113.32(6) . . ?
C2 O2 In1 112.12(6) . . ?
C2 O2 K1 108.00(6) . . ?
In1 O2 K1 91.99(3) . . ?
O1 C1 C6 121.36(9) . . ?
O1 C1 C2 117.53(9) . . ?
C6 C1 C2 121.10(9) . . ?
O2 C2 C3 122.33(9) . . ?
O2 C2 C1 117.23(9) . . ?
C3 C2 C1 120.42(10) . . ?
O2 C2 K1 49.88(5) . . ?
C3 C2 K1 112.67(6) . . ?
C1 C2 K1 106.01(6) . . ?
C4 C3 C2 116.77(10) . . ?
C4 C3 C7 121.45(9) . . ?
C2 C3 C7 121.77(10) . . ?
C5 C4 C3 122.74(10) . . ?
C4 C5 C6 121.62(10) . . ?
C5 C6 C1 117.08(10) . . ?
C5 C6 C11 121.54(10) . . ?
C1 C6 C11 121.37(9) . . ?
C8 C7 C10 109.62(11) . . ?
C8 C7 C9 107.17(10) . . ?
C10 C7 C9 107.37(10) . . ?
C8 C7 C3 110.03(9) . . ?
C10 C7 C3 110.58(9) . . ?
C9 C7 C3 111.97(10) . . ?
C12 C11 C13 107.20(9) . . ?
C12 C11 C14 107.27(9) . . ?
C13 C11 C14 109.67(9) . . ?
C12 C11 C6 111.72(9) . . ?
C13 C11 C6 109.81(9) . . ?
C14 C11 C6 111.06(9) . . ?
C2S O1S C1S 113.69(11) . . ?
C2S O1S K1 119.22(8) . . ?
C1S O1S K1 124.64(9) . . ?
C3S O2S C4S 111.42(11) . . ?
C3S O2S K1 103.65(7) . . ?
C4S O2S K1 106.15(8) . . ?
O1S C2S C3S 108.16(11) . . ?
O2S C3S C2S 108.46(11) . . ?
O2S C3S K1 52.35(6) . . ?
C2S C3S K1 85.88(8) . . ?
O2S C4S K1 50.46(6) . . ?
C5S N1S C7S 110.02(9) . . ?
C5S N1S C6S 107.83(8) . . ?
C7S N1S C6S 110.58(9) . . ?
C5S N1S In1 111.30(7) . . ?
C7S N1S In1 106.94(6) . . ?
C6S N1S In1 110.20(6) . . ?
N1S C7S C7S 111.50(8) . 2_654 ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.550
_refine_diff_density_min -0.380
_refine_diff_density_rms 0.067
_publ_section_references
;
Bruker (2000) SAINTPlus Data Reduction and Correction Program v. 6.02a, Bruker
AXS, Madison, Wisconsin, USA.
Bruker (2000) SMART. Bruker Molecular Analysis Research Tool,
v. 5.625 Bruker AXS, Madison, Wisconsin, USA.
Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector
Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA.
Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software
Suite, Bruker AXS, Madison, Wisconsin, USA.
;
# Attachment '- Complex_4.cif'
data_incat3m
_database_code_depnum_ccdc_archive 'CCDC 780472'
#TrackingRef '- Complex_4.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C36 H56 I2 In2 O6'
_chemical_formula_weight 1068.25
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'
In In -0.7276 1.3100 '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'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M Pbcn
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a 22.3131(9)
_cell_length_b 9.8806(4)
_cell_length_c 18.2309(8)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 4019.3(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used 900
_cell_measurement_theta_min 2
_cell_measurement_theta_max 30
_exptl_crystal_description prism
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.22
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.765
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2096
_exptl_absorpt_coefficient_mu 2.723
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.3942
_exptl_absorpt_correction_T_max 0.5857
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 22913
_diffrn_reflns_av_R_equivalents 0.0206
_diffrn_reflns_av_sigmaI/netI 0.0152
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 1.83
_diffrn_reflns_theta_max 26.00
_reflns_number_total 3945
_reflns_number_gt 3579
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SHELXTL'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0331P)^2^+2.6531P] where P=(Fo^2^+2Fc^2^)/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 3945
_refine_ls_number_parameters 215
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0256
_refine_ls_R_factor_gt 0.0225
_refine_ls_wR_factor_ref 0.0571
_refine_ls_wR_factor_gt 0.0557
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_restrained_S_all 1.054
_refine_ls_shift/su_max 0.002
_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
In1 In 0.5000 0.531562(17) 0.2500 0.01898(4) Uani 1 2 d S . .
I1 I 0.564986(6) 0.990954(17) 0.151699(9) 0.04789(5) Uani 1 1 d . . .
O1 O 0.45006(5) 0.70425(12) 0.19833(7) 0.0214(3) Uani 1 1 d . . .
C1 C 0.38928(8) 0.67687(17) 0.20951(9) 0.0209(4) Uani 1 1 d . . .
In2 In 0.5000 0.858722(18) 0.2500 0.02231(4) Uani 1 2 d S . .
C2 C 0.37646(8) 0.59086(17) 0.26951(9) 0.0203(4) Uani 1 1 d . . .
O2 O 0.42284(5) 0.54244(13) 0.30987(7) 0.0227(3) Uani 1 1 d . . .
C3 C 0.31708(8) 0.55220(18) 0.28525(9) 0.0214(4) Uani 1 1 d . . .
O3 O 0.46828(6) 0.38390(14) 0.16756(7) 0.0300(3) Uani 1 1 d . . .
C4 C 0.27332(8) 0.5990(2) 0.23736(10) 0.0259(4) Uani 1 1 d . . .
H4A H 0.2328 0.5742 0.2459 0.031 Uiso 1 1 calc R . .
C5 C 0.28648(8) 0.68070(19) 0.17743(11) 0.0263(4) Uani 1 1 d . . .
H5A H 0.2547 0.7086 0.1462 0.032 Uiso 1 1 calc R . .
C6 C 0.34475(8) 0.72329(18) 0.16138(9) 0.0219(4) Uani 1 1 d . . .
C7 C 0.30167(8) 0.46582(18) 0.35282(10) 0.0239(4) Uani 1 1 d . . .
C8 C 0.32234(9) 0.5412(2) 0.42192(11) 0.0303(4) Uani 1 1 d . . .
H8A H 0.3027 0.6298 0.4242 0.046 Uiso 1 1 calc R . .
H8B H 0.3659 0.5536 0.4202 0.046 Uiso 1 1 calc R . .
H8C H 0.3117 0.4883 0.4655 0.046 Uiso 1 1 calc R . .
C9 C 0.23424(8) 0.4405(2) 0.35935(11) 0.0312(4) Uani 1 1 d . . .
H9A H 0.2132 0.5273 0.3635 0.047 Uiso 1 1 calc R . .
H9B H 0.2262 0.3858 0.4031 0.047 Uiso 1 1 calc R . .
H9C H 0.2201 0.3924 0.3157 0.047 Uiso 1 1 calc R . .
C10 C 0.33246(9) 0.3267(2) 0.34849(11) 0.0289(4) Uani 1 1 d . . .
H10A H 0.3186 0.2787 0.3046 0.043 Uiso 1 1 calc R . .
H10B H 0.3224 0.2736 0.3922 0.043 Uiso 1 1 calc R . .
H10C H 0.3760 0.3391 0.3459 0.043 Uiso 1 1 calc R . .
C11 C 0.35764(8) 0.81525(18) 0.09517(10) 0.0246(4) Uani 1 1 d . . .
C12 C 0.30129(9) 0.8409(2) 0.04924(11) 0.0345(5) Uani 1 1 d . . .
H12A H 0.3115 0.8977 0.0070 0.052 Uiso 1 1 calc R . .
H12B H 0.2712 0.8870 0.0793 0.052 Uiso 1 1 calc R . .
H12C H 0.2851 0.7543 0.0320 0.052 Uiso 1 1 calc R . .
C13 C 0.37959(10) 0.9538(2) 0.12201(12) 0.0333(5) Uani 1 1 d . . .
H13A H 0.3850 1.0143 0.0799 0.050 Uiso 1 1 calc R . .
H13B H 0.4179 0.9430 0.1477 0.050 Uiso 1 1 calc R . .
H13C H 0.3499 0.9926 0.1556 0.050 Uiso 1 1 calc R . .
C14 C 0.40521(9) 0.7514(2) 0.04452(10) 0.0320(5) Uani 1 1 d . . .
H14A H 0.4115 0.8100 0.0018 0.048 Uiso 1 1 calc R . .
H14B H 0.3914 0.6623 0.0281 0.048 Uiso 1 1 calc R . .
H14C H 0.4430 0.7415 0.0714 0.048 Uiso 1 1 calc R . .
C15 C 0.41115(10) 0.3115(2) 0.16937(12) 0.0349(5) Uani 1 1 d . . .
H15A H 0.3833 0.3533 0.2051 0.042 Uiso 1 1 calc R . .
H15B H 0.4172 0.2153 0.1827 0.042 Uiso 1 1 calc R . .
C16 C 0.38748(9) 0.3243(2) 0.09263(13) 0.0381(5) Uani 1 1 d . . .
H16A H 0.3679 0.4130 0.0847 0.046 Uiso 1 1 calc R . .
H16B H 0.3587 0.2510 0.0811 0.046 Uiso 1 1 calc R . .
C17 C 0.44476(10) 0.3112(2) 0.04725(12) 0.0395(5) Uani 1 1 d . . .
H17A H 0.4571 0.2154 0.0424 0.047 Uiso 1 1 calc R . .
H17B H 0.4395 0.3507 -0.0023 0.047 Uiso 1 1 calc R . .
C18 C 0.48961(9) 0.3911(3) 0.09184(11) 0.0367(5) Uani 1 1 d . . .
H18A H 0.5301 0.3510 0.0875 0.044 Uiso 1 1 calc R . .
H18B H 0.4912 0.4863 0.0749 0.044 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
In1 0.01472(8) 0.01910(9) 0.02311(8) 0.000 0.00024(6) 0.000
I1 0.03024(8) 0.05388(9) 0.05954(10) 0.02481(7) 0.00273(6) -0.01054(6)
O1 0.0167(5) 0.0216(6) 0.0260(6) 0.0007(5) 0.0008(5) -0.0006(5)
C1 0.0172(8) 0.0205(8) 0.0251(9) -0.0041(7) -0.0004(7) -0.0011(7)
In2 0.01714(8) 0.01873(9) 0.03104(9) 0.000 -0.00111(7) 0.000
C2 0.0178(8) 0.0187(8) 0.0243(8) -0.0029(7) -0.0013(6) 0.0019(7)
O2 0.0156(5) 0.0282(6) 0.0243(6) 0.0027(5) 0.0006(5) 0.0015(5)
C3 0.0198(8) 0.0202(8) 0.0243(8) -0.0016(7) 0.0007(7) 0.0005(7)
O3 0.0295(7) 0.0312(7) 0.0295(7) -0.0045(6) 0.0053(5) -0.0091(6)
C4 0.0160(8) 0.0289(10) 0.0327(9) -0.0026(8) -0.0003(7) -0.0004(7)
C5 0.0187(8) 0.0299(9) 0.0305(9) 0.0006(8) -0.0058(7) 0.0011(7)
C6 0.0205(8) 0.0220(8) 0.0232(8) -0.0009(7) -0.0014(7) 0.0003(7)
C7 0.0191(8) 0.0247(9) 0.0279(9) 0.0007(7) 0.0032(7) -0.0007(7)
C8 0.0285(10) 0.0341(10) 0.0284(9) -0.0016(8) 0.0031(8) -0.0016(8)
C9 0.0224(9) 0.0347(10) 0.0363(10) 0.0038(9) 0.0059(8) -0.0014(8)
C10 0.0289(10) 0.0255(9) 0.0324(10) 0.0031(8) 0.0031(8) 0.0001(8)
C11 0.0246(9) 0.0254(9) 0.0237(9) 0.0011(7) -0.0016(7) 0.0023(7)
C12 0.0302(10) 0.0412(11) 0.0322(10) 0.0084(9) -0.0064(8) 0.0022(9)
C13 0.0364(11) 0.0280(10) 0.0356(10) 0.0038(8) -0.0037(9) -0.0015(8)
C14 0.0340(10) 0.0372(11) 0.0249(9) 0.0034(8) 0.0025(8) 0.0045(9)
C15 0.0352(11) 0.0307(10) 0.0387(11) -0.0092(8) 0.0077(9) -0.0143(8)
C16 0.0264(10) 0.0344(11) 0.0535(13) 0.0018(10) -0.0042(9) -0.0020(9)
C17 0.0357(11) 0.0512(13) 0.0315(10) -0.0002(9) -0.0048(9) -0.0058(9)
C18 0.0344(11) 0.0476(12) 0.0282(10) -0.0058(9) 0.0053(8) -0.0076(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds 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
In1 O2 2.0413(12) . ?
In1 O2 2.0414(12) 3_655 ?
In1 O3 2.2109(13) . ?
In1 O3 2.2110(13) 3_655 ?
In1 O1 2.2450(12) 3_655 ?
In1 O1 2.2451(12) . ?
In1 In2 3.2325(3) . ?
I1 In2 2.64978(18) . ?
O1 C1 1.398(2) . ?
O1 In2 2.1115(12) . ?
C1 C6 1.403(2) . ?
C1 C2 1.414(2) . ?
In2 O1 2.1114(12) 3_655 ?
In2 I1 2.64975(18) 3_655 ?
C2 O2 1.357(2) . ?
C2 C3 1.408(2) . ?
C3 C4 1.389(3) . ?
C3 C7 1.538(2) . ?
O3 C18 1.462(2) . ?
O3 C15 1.462(2) . ?
C4 C5 1.390(3) . ?
C5 C6 1.398(3) . ?
C6 C11 1.538(2) . ?
C7 C9 1.530(3) . ?
C7 C8 1.534(3) . ?
C7 C10 1.539(3) . ?
C11 C12 1.532(3) . ?
C11 C13 1.534(3) . ?
C11 C14 1.542(3) . ?
C15 C16 1.501(3) . ?
C16 C17 1.528(3) . ?
C17 C18 1.512(3) . ?
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
O2 In1 O2 173.96(7) . 3_655 ?
O2 In1 O3 97.37(5) . . ?
O2 In1 O3 86.63(5) 3_655 . ?
O2 In1 O3 86.63(5) . 3_655 ?
O2 In1 O3 97.37(5) 3_655 3_655 ?
O3 In1 O3 97.42(7) . 3_655 ?
O2 In1 O1 98.87(5) . 3_655 ?
O2 In1 O1 76.45(5) 3_655 3_655 ?
O3 In1 O1 161.01(5) . 3_655 ?
O3 In1 O1 93.29(5) 3_655 3_655 ?
O2 In1 O1 76.45(5) . . ?
O2 In1 O1 98.87(5) 3_655 . ?
O3 In1 O1 93.29(5) . . ?
O3 In1 O1 161.01(5) 3_655 . ?
O1 In1 O1 81.07(6) 3_655 . ?
O2 In1 In2 86.98(4) . . ?
O2 In1 In2 86.98(4) 3_655 . ?
O3 In1 In2 131.29(4) . . ?
O3 In1 In2 131.29(4) 3_655 . ?
O1 In1 In2 40.53(3) 3_655 . ?
O1 In1 In2 40.53(3) . . ?
C1 O1 In2 125.94(10) . . ?
C1 O1 In1 105.86(9) . . ?
In2 O1 In1 95.76(5) . . ?
O1 C1 C6 122.19(15) . . ?
O1 C1 C2 115.17(14) . . ?
C6 C1 C2 122.48(16) . . ?
O1 In2 O1 87.42(6) 3_655 . ?
O1 In2 I1 110.09(3) 3_655 3_655 ?
O1 In2 I1 111.67(3) . 3_655 ?
O1 In2 I1 111.67(3) 3_655 . ?
O1 In2 I1 110.09(3) . . ?
I1 In2 I1 120.914(10) 3_655 . ?
O1 In2 In1 43.71(3) 3_655 . ?
O1 In2 In1 43.71(3) . . ?
I1 In2 In1 119.543(5) 3_655 . ?
I1 In2 In1 119.543(5) . . ?
O2 C2 C3 120.76(15) . . ?
O2 C2 C1 118.48(15) . . ?
C3 C2 C1 120.72(15) . . ?
C2 O2 In1 111.83(10) . . ?
C4 C3 C2 116.29(16) . . ?
C4 C3 C7 122.08(16) . . ?
C2 C3 C7 121.61(15) . . ?
C18 O3 C15 109.21(14) . . ?
C18 O3 In1 120.36(12) . . ?
C15 O3 In1 125.92(11) . . ?
C3 C4 C5 122.61(17) . . ?
C4 C5 C6 122.42(17) . . ?
C5 C6 C1 115.43(16) . . ?
C5 C6 C11 121.08(16) . . ?
C1 C6 C11 123.49(16) . . ?
C9 C7 C8 108.12(15) . . ?
C9 C7 C3 111.89(15) . . ?
C8 C7 C3 108.73(15) . . ?
C9 C7 C10 107.29(15) . . ?
C8 C7 C10 109.97(16) . . ?
C3 C7 C10 110.78(15) . . ?
C12 C11 C13 106.80(16) . . ?
C12 C11 C6 111.91(15) . . ?
C13 C11 C6 109.67(15) . . ?
C12 C11 C14 107.78(16) . . ?
C13 C11 C14 109.64(16) . . ?
C6 C11 C14 110.93(15) . . ?
O3 C15 C16 104.16(16) . . ?
C15 C16 C17 101.73(17) . . ?
C18 C17 C16 102.62(17) . . ?
O3 C18 C17 105.47(16) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 1.211
_refine_diff_density_min -0.423
_refine_diff_density_rms 0.088
_publ_section_references
;
Bruker (2000) SAINTPlus Data Reduction and Correction Program v. 6.02a, Bruker
AXS, Madison, Wisconsin, USA.
Bruker (2000) SMART. Bruker Molecular Analysis Research Tool,
v. 5.625 Bruker AXS, Madison, Wisconsin, USA.
Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector
Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA.
Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software
Suite, Bruker AXS, Madison, Wisconsin, USA.
;