#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/56/2005676.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2005676 loop_ _publ_author_name 'Thu\'ery, P.' 'Nierlich, M.' 'Lamare, V.' 'Dozol, J.-F.' 'Asfari, Z.' 'Vicens, J.' _publ_section_title ; Caesium Iodide Complex of 1,3-Calix[4]-bis-crown-6 ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2729 _journal_page_last 2731 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Cs2 I2 (C40 H60 O12)] , 2C2 H3 N' _chemical_formula_moiety 'C48 H60 Cs2 I2 O12, N2 C4 H6' _chemical_formula_sum 'C52 H66 Cs2 I2 N2 O12' _chemical_formula_weight 1430.73 _chemical_name_systematic ;[13,16,19,22,25,28,42,45,48,51,54,57-dodecaoxahexacyclo[28.28.1.1^11,40^.- 0^5,58^.0^7,12^.0^29,34^.0^36,41^]hexaconta-1(58),2,4,7,9,11,29,31,33,36,38,40- dodecaene](diiodo)dicaesium ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90. _cell_angle_beta 97.39(3) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 18.150(9) _cell_length_b 17.990(9) _cell_length_c 17.365(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 295 _cell_measurement_theta_max 12 _cell_measurement_theta_min 8 _cell_volume 5623(4) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material MolEN _computing_structure_refinement MolEN _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 295 _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source X-ray_tube _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.01 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 2858 _diffrn_reflns_theta_max 20 _diffrn_reflns_theta_min 1 _diffrn_standards_decay_% 'not significant' _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.429 _exptl_absorpt_correction_T_max 0.38 _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_type '\y scans (North, Phillips & Mathews, 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _refine_diff_density_max 0.43 _refine_diff_density_min -0.58 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.791 _refine_ls_goodness_of_fit_obs 1.879 _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 317 _refine_ls_number_reflns 2281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.032 _refine_ls_R_factor_obs 0.025 _refine_ls_shift/esd_max 0.01 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/[\s^2^(F)]' _refine_ls_wR_factor_all 0.040 _refine_ls_wR_factor_obs 0.038 _reflns_number_observed 2281 _reflns_number_total 2625 _reflns_observed_criterion I>3\s(I) _[local]_cod_data_source_file pa1233.cif _[local]_cod_data_source_block TOZ _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_original_cell_volume 5623(7) _cod_database_code 2005676 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2+y,z -x,-y,-z 1/2-x,1/2-y,-z -x,y,1/2-z 1/2-x,1/2+y,1/2-z x,-y,1/2+z 1/2+x,1/2-y,1/2+z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_type_symbol Cs .48414(2) .27674(2) .04312(2) 3.769(8) Beq CS I .37970(2) .34614(2) -.14078(2) 4.705(9) Beq I O1 .5878(2) .3766(1) .1760(2) 2.67(6) Beq O O2 .6253(2) .3725(2) .0161(2) 4.05(7) Beq O O3 .6134(3) .2440(2) -.0828(2) 6.6(1) Beq O O4 .5070(2) .1238(2) -.0770(2) 7.5(1) Beq O O5 .3865(2) .1298(2) .0105(2) 4.57(8) Beq O O6 .3975(2) .1853(2) .1685(2) 2.87(6) Beq O N .6808(3) .0445(4) -.2136(4) 9.2(2) Beq N C1 .6090(3) .4388(3) .1306(3) 3.9(1) Beq C C2 .6611(3) .4166(3) .0759(3) 4.2(1) Beq C C3 .6701(3) .3575(3) -.0422(3) 5.3(1) Beq C C4 .6275(4) .3152(3) -.1072(3) 5.8(1) Beq C C5 .5796(5) .1987(4) -.1465(3) 13.0(2) Beq C C6 .5574(4) .1339(5) -.1298(4) 11.5(2) Beq C C7 .4360(3) .1081(4) -.1067(3) 6.2(1) Beq C C8 .3922(3) .0795(3) -.0499(3) 6.0(2) Beq C C9 .3453(3) .1033(3) .0676(3) 5.8(1) Beq C C10 .3320(3) .1584(3) .1233(3) 4.3(1) Beq C C11 .6026(2) .3873(2) .2559(2) 2.52(9) Beq C C12 .5623(2) .4401(2) .2927(3) 2.8(1) Beq C C13 .5848(3) .4524(3) .3717(3) 3.4(1) Beq C C14 .6419(3) .4115(3) .4121(3) 3.8(1) Beq C C15 .6775(3) .3570(2) .3755(3) 3.4(1) Beq C C16 .6580(2) .3428(2) .2958(3) 2.8(1) Beq C C17 .6994(2) .2847(3) .2562(3) 3.3(1) Beq C C18 .6521(2) .2233(2) .2146(3) 2.8(1) Beq C C19 .6041(2) .1791(2) .2517(2) 2.45(9) Beq C C20 .5565(2) .1275(2) .2113(3) 2.9(1) Beq C C21 .5627(3) .1156(3) .1333(3) 3.6(1) Beq C C22 .6146(3) .1549(3) .0970(3) 4.1(1) Beq C C23 .6568(3) .2091(3) .1374(3) 3.6(1) Beq C C24 .50 .0833(4) .25 3.7(2) Beq C C25 .50 .4845(3) .25 3.3(1) Beq C C26 .7118(3) .0093(3) -.2511(3) 4.9(1) Beq C C27 .7522(3) -.0368(3) -.2978(3) 4.4(1) Beq C H1 .632 .476 .165 6.0 ? H H2 .556 .459 .101 6.0 ? H H3 .681 .459 .054 6.0 ? H H4 .700 .388 .104 6.0 ? H H5 .711 .328 -.021 6.0 ? H H6 .688 .403 -.060 6.0 ? H H7 .582 .341 -.122 6.0 ? H H8 .655 .313 -.150 6.0 ? H H9 .610 .197 -.187 6.0 ? H H10 .534 .223 -.164 6.0 ? H H11 .539 .108 -.176 6.0 ? H H12 .602 .112 -.107 6.0 ? H H13 .436 .074 -.148 6.0 ? H H14 .413 .153 -.126 6.0 ? H H15 .344 .066 -.073 6.0 ? H H16 .417 .037 -.028 6.0 ? H H17 .373 .064 .095 6.0 ? H H18 .299 .084 .043 6.0 ? H H19 .308 .199 .095 6.0 ? H H20 .300 .139 .157 6.0 ? H H21 .560 .490 .398 6.0 ? H H22 .656 .422 .466 6.0 ? H H23 .716 .328 .404 6.0 ? H H24 .734 .262 .295 6.0 ? H H25 .726 .309 .219 6.0 ? H H26 .531 .081 .104 6.0 ? H H27 .621 .145 .044 6.0 ? H H28 .690 .238 .112 6.0 ? H H29 .474 .053 .211 6.0 ? H H30 .520 .515 .213 6.0 ? H H31 .757 -.086 -.278 6.0 ? H H32 .727 -.038 0.349 6.0 ? H H33 .800 -.016 -.298 6.0 ? H loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 4 1 -3 -3 7 -8 2 5 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag I Cs O1 . 126.73(5) yes I Cs O2 . 91.31(7) yes I Cs O3 . 79.99(9) yes I Cs O4 . 80.70(10) yes I Cs O5 . 85.14(7) yes I Cs O6 . 120.22(6) yes O1 Cs O2 . 53.93(8) yes O2 Cs O3 . 51.10(10) yes O3 Cs O4 . 49.40(10) yes O4 Cs O5 . 49.50(10) yes O5 Cs O6 . 53.23(8) yes C11 O1 C1 . 113.9(4) yes O1 C1 C2 . 112.2(4) yes C1 C2 O2 . 110.8(4) yes C2 O2 C3 . 112.8(4) yes O2 C3 C4 . 110.6(5) yes C3 C4 O3 . 109.9(6) yes C4 O3 C5 . 111.4(6) yes O3 C5 C6 . 117.0(9) yes C5 C6 O4 . 121.5(7) yes C6 O4 C7 . 116.9(6) yes O4 C7 C8 . 113.4(6) yes C7 C8 O5 . 112.5(6) yes C8 O5 C9 . 114.1(5) yes O5 C9 C10 . 113.3(5) yes C9 C10 O6 . 114.1(5) yes C10 O6 C19 5_655 113.5(4) yes O1 C11 C12 . 120.2(5) yes O1 C11 C16 . 116.7(4) yes C12 C11 C16 . 123.1(5) yes C11 C12 C13 . 116.8(5) yes C11 C12 C25 . 122.7(4) yes C12 C13 C14 . 121.2(5) yes C13 C12 C25 . 120.5(4) yes C13 C14 C15 . 120.7(5) yes C14 C15 C16 . 120.6(5) yes C15 C16 C11 . 117.3(5) yes C15 C16 C17 . 119.9(5) yes C11 C16 C17 . 122.8(5) yes C16 C17 C18 . 115.9(4) yes C17 C18 C19 . 122.7(5) yes C17 C18 C23 . 119.6(5) yes C19 C18 C23 . 117.7(5) yes C18 C19 C20 . 122.0(5) yes C19 C20 C21 . 118.1(5) yes C19 C20 C24 . 122.3(4) yes C21 C20 C24 . 119.6(5) yes C20 C21 C22 . 120.5(5) yes C21 C22 C23 . 119.6(5) yes C18 C23 C22 . 121.8(5) yes C12 C25 C12 5_655 115.6(6) yes C20 C24 C20 5_655 116.9(6) yes N C26 C27 . 178.7(8) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cs I . 3.7140(5) yes Cs O1 . 3.313(3) yes Cs O2 . 3.172(4) yes Cs O3 . 3.458(5) yes Cs O4 . 3.510(5) yes Cs O5 . 3.192(4) yes Cs O6 . 3.286(3) yes Cs C13 5_655 3.770(5) yes Cs C14 5_655 3.489(5) yes Cs C15 5_655 3.709(5) yes Cs C21 . 3.509(5) yes Cs C22 . 3.273(5) yes Cs C23 . 3.559(5) yes O1 C1 . 1.449(6) yes C1 C2 . 1.478(7) yes C2 O2 . 1.398(6) yes O2 C3 . 1.405(7) yes C3 C4 . 1.491(9) yes C4 O3 . 1.383(7) yes O3 C5 . 1.450(10) yes C5 C6 . 1.280(10) yes C6 O4 . 1.390(10) yes O4 C7 . 1.355(8) yes C7 C8 . 1.437(9) yes C8 O5 . 1.399(7) yes O5 C9 . 1.401(8) yes C9 C10 . 1.428(8) yes C10 O6 . 1.423(6) yes O6 C19 5_655 1.394(6) yes O1 C11 . 1.393(6) yes C11 C12 . 1.401(7) yes C11 C16 . 1.397(7) yes C12 C13 . 1.397(7) yes C12 C25 . 1.501(6) yes C13 C14 . 1.386(8) yes C14 C15 . 1.375(7) yes C15 C16 . 1.407(8) yes C16 C17 . 1.505(7) yes C17 C18 . 1.524(7) yes C18 C19 . 1.397(7) yes C18 C23 . 1.378(8) yes C19 C20 . 1.394(7) yes C20 C21 . 1.389(8) yes C20 C24 . 1.520(7) yes C21 C22 . 1.393(8) yes C22 C23 . 1.376(8) yes N C26 . 1.111(8) yes C26 C27 . 1.426(9) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C12 C11 O1 C1 . . 68.6(5) yes C16 C11 O1 C1 . . -112.0(4) yes C11 O1 C1 C2 . . 123.5(4) yes O1 C1 C2 O2 . . 69.8(5) yes C1 C2 O2 C3 . . 172.9(4) yes C2 O2 C3 C4 . . -175.8(4) yes O2 C3 C4 O3 . . -69.5(6) yes C3 C4 O3 C5 . . -173.4(6) yes C4 O3 C5 C6 . . -173.3(7) yes O3 C5 C6 O4 . . 56.0(10) yes C5 C6 O4 C7 . . 103.6(8) yes C6 O4 C7 C8 . . 164.6(6) yes O4 C7 C8 O5 . . 60.9(7) yes C7 C8 O5 C9 . . -179.0(5) yes C8 O5 C9 C10 . . -172.5(5) yes O5 C9 C10 O6 . . -63.7(6) yes C9 C10 O6 C19 . 5_655 -125.1(4) yes C10 O6 C19 C18 5_655 5_655 -69.2(5) yes C10 O6 C19 C20 5_655 5_655 110.7(4) yes