#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/36/2003678.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_2003678 loop_ _publ_author_name 'Thu\'ery, P.' 'Keller, N.' 'Lance, M.' 'Vigner, J.-D.' 'Nierlich, M.' _publ_section_title ; (H~4~-Hexaaza-18-crown-6)^4+^.4CF~3~SO~3~^{-^} and its Hydrated Form ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1407 _journal_page_last 1411 _journal_paper_doi 10.1107/S0108270194014241 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C12 H34 N6 , 4C F3 S O3' _chemical_formula_sum 'C16 H34 F12 N6 O12 S4' _chemical_formula_weight 858.72 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 104.58(5) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.919(4) _cell_length_b 14.128(3) _cell_length_c 14.079(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 243 _cell_measurement_theta_max 12 _cell_measurement_theta_min 8 _cell_volume 1716.9(12) _computing_cell_refinement 'Enraf-Nonius CAD-4 software' _computing_data_collection 'Enraf-Nonius CAD-4 software' _computing_data_reduction 'MolEN (Fair, 1990)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement MolEN _computing_structure_solution 'MULTAN11/82 (Main et al., 1982)' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 2473 _diffrn_reflns_theta_max 22 _diffrn_standards_decay_% insignificant _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.386 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.661 _exptl_crystal_description irregular _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.61 _refine_diff_density_min -0.44 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 2.09 _refine_ls_number_parameters 181 _refine_ls_number_reflns 1409 _refine_ls_R_factor_obs 0.058 _refine_ls_shift/esd_max 0.00 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme unit _refine_ls_wR_factor_obs 0.060 _reflns_number_observed 1409 _reflns_number_total 2102 _reflns_observed_criterion I>3\s(I) _cod_data_source_file ka1089.cif _cod_data_source_block I _cod_original_cell_volume 1717.0(10) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2003678 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,1/2+z -x,-y,-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_B_iso_or_equiv S(1) 0.7349(2) 0.3766(1) 0.0562(1) 2.66(4) S(2) 0.8084(2) 0.3770(1) 0.6749(1) 2.86(4) F(11) 0.8439(6) 0.2094(3) 0.0350(4) 5.7(1) F(12) 0.5994(6) 0.2201(4) -0.0137(5) 7.2(2) F(13) 0.7456(8) 0.2792(4) -0.0977(3) 8.5(2) F(21) 0.6957(9) 0.5243(4) 0.5710(4) 10.8(2) F(22) 0.9265(9) 0.4837(6) 0.5690(6) 20.9(2) F(23) 0.732(1) 0.4043(6) 0.4906(4) 19.3(3) O(11) 0.7087(8) 0.3507(4) 0.1481(4) 6.8(2) O(12) 0.8796(6) 0.4174(4) 0.0582(5) 6.0(2) O(13) 0.6033(7) 0.4280(4) -0.0012(5) 5.6(2) O(21) 0.8995(6) 0.2986(4) 0.6556(4) 4.0(1) O(22) 0.6543(6) 0.3554(5) 0.6759(5) 5.8(2) O(23) 0.8843(8) 0.4349(5) 0.7561(5) 7.0(2) N(1) 1.0145(6) 0.0177(4) 0.2928(4) 2.6(1) N(2) 0.7489(6) 0.1043(4) 0.3354(4) 2.6(1) N(3) 0.8023(6) 0.1313(4) 0.5462(4) 2.4(1) C(1) 0.8686(8) 0.0363(5) 0.2151(5) 3.1(1) C(2) 0.7920(8) 0.1229(6) 0.2431(3) 3.3(1) C(3) 0.6985(8) 0.1895(5) 0.3771(5) 3.1(1) C(4) 0.6586(8) 0.1645(5) 0.4724(5) 3.0(1) C(5) 0.7660(8) 0.0928(5) 0.6373(5) 2.9(1) C(6) 0.9121(8) 0.0752(5) 0.7179(5) 2.9(1) C(10) 0.7281(8) 0.2662(6) -0.0108(5) 3.3(2) C(20) 0.788(1) 0.4507(7) 0.5697(7) 9.0(3) H1 0.988 0.019 0.361 6.0 H2 1.094 0.072 0.290 6.0 H3 0.879 0.189 0.565 6.0 H4 0.855 0.078 0.514 6.0 H11 0.801 -0.016 0.210 6.0 H12 0.892 0.047 0.154 6.0 H21 0.862 0.175 0.251 6.0 H22 0.701 0.137 0.193 6.0 H31 0.609 0.214 0.332 6.0 H32 0.778 0.236 0.389 6.0 H41 0.618 0.219 0.497 6.0 H42 0.583 0.115 0.461 6.0 H51 0.712 0.035 0.622 6.0 H52 0.703 0.137 0.660 6.0 H61 0.885 0.076 0.779 6.0 H62 0.984 0.125 0.717 6.0 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C(6) N(1) C(1) 3_756 . 113.8(5) yes C(1) C(2) N(2) . . 108.9(6) yes N(2) C(3) C(4) . . 109.2(6) yes C(4) N(3) C(5) . . 111.9(5) yes C(5) C(6) N(1) . 3_756 112.6(6) yes N(1) C(1) C(2) . . 108.7(6) yes C(2) N(2) C(3) . . 112.6(6) yes C(3) C(4) N(3) . . 109.6(6) yes N(3) C(5) C(6) . . 111.6(6) yes O(13) N(1) O(22) 2_555 2_554 110.6(3) yes O(11) S(1) O(12) . . 116.6(5) no O(11) S(1) O(13) . . 110.0(4) no O(11) S(1) C(10) . . 105.0(6) no O(12) S(1) O(13) . . 114.7(4) no O(12) S(1) C(10) . . 105.9(4) no O(13) S(1) C(10) . . 103.0(4) no O(21) S(2) O(22) . . 115.6(4) no O(21) S(2) O(23) . . 114.5(4) no O(21) S(2) C(20) . . 103.6(9) no O(22) S(2) O(23) . . 112.5(4) no O(22) S(2) C(20) . . 103.9(4) no O(23) S(2) C(20) . . 105.0(9) no S(1) C(10) F(11) . . 110.1(9) no S(1) C(10) F(12) . . 110.9(9) no S(1) C(10) F(13) . . 112.0(7) no F(11) C(10) F(12) . . 106.3(9) no F(11) C(10) F(13) . . 106.0(10) no F(12) C(10) F(13) . . 111.0(10) no S(2) C20 F(21) . . 112.(3) no S(2) C20 F(22) . . 108.(2) no S(2) C20 F(23) . . 111.0(10) no F(21) C20 F(22) . . 108.0(10) no F(21) C20 F(23) . . 108.(2) no F(22) C20 F(23) . . 110.(3) no 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 N(1) C(1) . 1.497(9) yes N(2) C(2) . 1.468(9) yes N(3) C(4) . 1.507(9) yes C(1) C(2) . 1.500(10) yes C(5) C(6) . 1.520(10) yes N(1) C(6) 3_756 1.490(10) yes N(2) C(3) . 1.460(9) yes N(3) C(5) . 1.501(9) yes C(3) C(4) . 1.510(10) yes N(1) O(22) 2_554 2.920(10) yes N(3) O(21) . 2.830(10) yes N(1) O(13) 2_555 2.910(10) yes S(1) O(11) . 1.420(6) no S(1) O(12) . 1.408(6) no S(1) O(13) . 1.443(6) no S(1) C(10) . 1.820(10) no S(2) O(21) . 1.441(5) no S(2) O(22) . 1.411(6) no S(2) O(23) . 1.430(7) no S(2) C(20) . 1.78(4) no F(11) C(10) . 1.340(10) no F(12) C(10) . 1.311(8) no F(13) C(10) . 1.29(2) no F(21) C(20) . 1.33(2) no F(22) C(20) . 1.32(2) no F(23) C(20) . 1.28(4) no 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_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C(6) N(1) C(1) C(2) 3_756 . . 170.4(6) yes C(1) C(2) N(2) C(3) . . . 169.9(6) yes N(2) C(3) C(4) N(3) . . . 64.4(7) yes C(4) N(3) C(5) C(6) . . . -170.2(5) yes C(5) C(6) N(1) C(1) 3_756 3_756 . -179.0(5) yes N(1) C(1) C(2) N(2) . . . -62.8(7) yes C(2) N(2) C(3) C(4) . . . -179.2(6) yes C(3) C(4) N(3) C(5) . . . -172.2(6) yes N(3) C(5) C(6) N(1) . . 3_756 -83.0(5) yes