#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100118.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_1100118 loop_ _publ_author_name 'E. Goreshnik' 'M. Leblanc' 'V. Maisonneuve' _publ_contact_author_address ; Laboratoire des Fluorures - UMR 6010 CNRS, Facult\'e des Sciences, Universit\'e du Maine, Avenue Olivier Messiaen, 72085 LE MANS Cedex 9, FRANCE ; _publ_contact_author_email vincent.maisonneuve@univ-lemans.fr _publ_contact_author_fax '(33) 2 43 83 35 06' _publ_contact_author_name 'Vincent Maisonneuve' _publ_contact_author_phone '(33) 2 43 83 35 61' _publ_section_title ; 1,4,8,11-Tetraazacyclodecane-1,4,8,11-tetraium bis(aquapentafluoroaluminate) dihydrate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m1059 _journal_page_last m1061 _journal_paper_category EM _journal_paper_doi 10.1107/S1600536803023699 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '(C10 H28 N4) [Al F5 (H2 O)]2, 2H2 O' _chemical_formula_moiety 'C10 H28 N4 1+, 2Al F5 H2 O 2-, 2H2 O' _chemical_formula_sum 'C10 H36 Al2 F10 N4 O4' _chemical_formula_weight 520.3675 _chemical_name_common ? _chemical_name_systematic ; 1,4,8,11-Tetraazacyclodecane-1,4,8,11-tetraium bis(aquapentafluoroaluminate) dihydrate ; _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_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 97.141(8) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.4930(8) _cell_length_b 8.9320(10) _cell_length_c 13.434(2) _cell_measurement_reflns_used 32 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 10 _cell_measurement_theta_min 2.5 _cell_volume 1011.2(2) _computing_cell_refinement 'STADI4 (Stoe & Cie, 1998)' _computing_data_collection 'STADI4 (Stoe & Cie, 1998)' _computing_data_reduction 'X-RED (Stoe & Cie, 1998)' _computing_molecular_graphics ; DIAMOND (Brandenburg, 2001), ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 Farrugia, 1997) ; _computing_publication_material 'enCIFer (CCDC, 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Siemens AED2' _diffrn_measurement_method 2\q/\w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0919 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2955 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 2.69 _diffrn_standards_decay_% 15 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.261 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description parallelepiped _exptl_crystal_F_000 544 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_special_details ; ? ; _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. ; _refine_diff_density_max 0.453 _refine_diff_density_min -0.468 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 148 _refine_ls_number_reflns 2955 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.1639 _refine_ls_R_factor_gt 0.0632 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.517P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1198 _refine_ls_wR_factor_ref 0.1508 _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. ; _reflns_number_gt 1591 _reflns_number_total 2955 _reflns_threshold_expression I>2\s(I) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1100118 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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Al 0.34962(11) 0.21382(12) 0.06661(8) 0.0178(2) Uani d . 1 . . Al F1 0.3863(2) 0.3257(3) 0.17890(16) 0.0324(5) Uani d . 1 . . F F2 0.4504(2) 0.3417(3) -0.00278(17) 0.0329(5) Uani d . 1 . . F F3 0.2390(2) 0.0843(3) 0.13107(16) 0.0335(5) Uani d . 1 . . F F4 0.5146(2) 0.1058(2) 0.09959(16) 0.0319(5) Uani d . 1 . . F F5 0.1823(2) 0.3229(2) 0.03060(15) 0.0232(5) Uani d . 1 . . F O1 0.3038(3) 0.0969(3) -0.0546(2) 0.0302(6) Uani d D 1 . . O H1WA 0.357(4) 0.027(3) -0.073(3) 0.036 Uiso d D 1 . . H H1WB 0.212(2) 0.088(4) -0.081(3) 0.036 Uiso d D 1 . . H O2 0.0375(3) 0.0195(4) 0.8369(3) 0.0479(9) Uani d D 1 . . O H2WA -0.031(4) 0.000(6) 0.873(3) 0.058 Uiso d D 1 . . H H2WB 0.007(5) 0.068(5) 0.787(2) 0.058 Uiso d D 1 . . H N1 0.2341(3) 0.0972(3) 0.5466(2) 0.0219(6) Uani d . 1 . . N H1A 0.2650 0.0067 0.5270 0.026 Uiso calc R 1 . . H H1B 0.1275 0.1003 0.5344 0.026 Uiso calc R 1 . . H N2 0.3241(3) 0.0578(3) 0.3272(2) 0.0219(6) Uani d . 1 . . N H2A 0.2853 -0.0263 0.3520 0.026 Uiso calc R 1 . . H H2B 0.2937 0.0588 0.2606 0.026 Uiso calc R 1 . . H C1 0.2989(4) 0.2118(4) 0.4837(3) 0.0246(7) Uani d . 1 . . C H1C 0.4138 0.2108 0.4974 0.029 Uiso calc R 1 . . H H1D 0.2626 0.3096 0.5023 0.029 Uiso calc R 1 . . H C2 0.5509(4) -0.0952(4) 0.3105(3) 0.0253(8) Uani d . 1 . . C H2C 0.4945 -0.1761 0.3387 0.030 Uiso calc R 1 . . H H2D 0.5308 -0.1022 0.2380 0.030 Uiso calc R 1 . . H C3 0.2799(4) 0.1101(5) 0.6576(3) 0.0290(8) Uani d . 1 . . C H3A 0.2450 0.2067 0.6796 0.035 Uiso calc R 1 . . H H3B 0.2243 0.0335 0.6907 0.035 Uiso calc R 1 . . H C4 0.2521(4) 0.1894(4) 0.3728(3) 0.0273(8) Uani d . 1 . . C H4A 0.1376 0.1796 0.3607 0.033 Uiso calc R 1 . . H H4B 0.2806 0.2789 0.3382 0.033 Uiso calc R 1 . . H C5 0.4908(4) 0.0525(4) 0.3441(3) 0.0266(8) Uani d . 1 . . C H5A 0.5259 0.0665 0.4150 0.032 Uiso calc R 1 . . H H5B 0.5345 0.1330 0.3076 0.032 Uiso calc R 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Al 0.0138(4) 0.0195(5) 0.0198(5) 0.0021(4) 0.0013(3) 0.0001(4) F1 0.0273(11) 0.0366(14) 0.0310(12) 0.0051(9) -0.0049(9) -0.0142(10) F2 0.0170(10) 0.0407(13) 0.0409(13) -0.0052(9) 0.0037(9) 0.0106(11) F3 0.0255(10) 0.0455(14) 0.0289(11) -0.0104(10) 0.0015(9) 0.0126(10) F4 0.0223(10) 0.0353(13) 0.0357(12) 0.0139(9) -0.0058(9) -0.0045(10) F5 0.0142(9) 0.0267(11) 0.0283(11) 0.0042(8) 0.0011(7) 0.0015(9) O1 0.0199(12) 0.0372(17) 0.0317(14) 0.0080(11) -0.0040(11) -0.0127(12) O2 0.0246(15) 0.070(2) 0.0464(19) -0.0048(15) -0.0067(13) 0.0148(18) N1 0.0132(12) 0.0292(17) 0.0235(14) 0.0025(11) 0.0028(11) -0.0016(13) N2 0.0187(13) 0.0255(16) 0.0209(14) -0.0051(12) 0.0001(11) -0.0006(12) C1 0.0233(16) 0.0219(18) 0.0287(18) -0.0017(15) 0.0040(14) -0.0006(16) C2 0.0234(16) 0.029(2) 0.0237(17) 0.0001(15) 0.0022(13) -0.0027(15) C3 0.0238(17) 0.037(2) 0.0271(18) 0.0045(16) 0.0072(14) -0.0025(17) C4 0.0204(16) 0.031(2) 0.0304(19) 0.0053(15) 0.0028(14) 0.0061(16) C5 0.0179(16) 0.029(2) 0.0316(19) -0.0007(14) -0.0042(14) -0.0005(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0560 0.0520 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0140 0.0100 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 F4 Al F5 . . 178.87(12) ? F4 Al F2 . . 93.80(11) ? F5 Al F2 . . 85.63(11) ? F4 Al F3 . . 88.40(12) ? F5 Al F3 . . 92.12(11) ? F2 Al F3 . . 176.81(12) ? F4 Al F1 . . 92.57(11) ? F5 Al F1 . . 88.43(11) ? F2 Al F1 . . 92.20(12) ? F3 Al F1 . . 90.00(12) ? F4 Al O1 . . 89.21(11) ? F5 Al O1 . . 89.79(11) ? F2 Al O1 . . 87.99(13) ? F3 Al O1 . . 89.74(12) ? F1 Al O1 . . 178.19(12) ? Al O1 H1WA . . 127(3) ? Al O1 H1WB . . 120(3) ? H1WA O1 H1WB . . 109(3) ? H2WA O2 H2WB . . 115(3) ? C1 N1 C3 . . 116.6(3) ? C1 N1 H1A . . 108.1 ? C3 N1 H1A . . 108.1 ? C1 N1 H1B . . 108.1 ? C3 N1 H1B . . 108.1 ? H1A N1 H1B . . 107.3 ? C5 N2 C4 . . 114.6(3) ? C5 N2 H2A . . 108.6 ? C4 N2 H2A . . 108.6 ? C5 N2 H2B . . 108.6 ? C4 N2 H2B . . 108.6 ? H2A N2 H2B . . 107.6 ? N1 C1 C4 . . 113.8(3) ? N1 C1 H1C . . 108.8 ? C4 C1 H1C . . 108.8 ? N1 C1 H1D . . 108.8 ? C4 C1 H1D . . 108.8 ? H1C C1 H1D . . 107.7 ? C3 C2 C5 3_656 . 110.6(3) ? C3 C2 H2C 3_656 . 109.5 ? C5 C2 H2C . . 109.5 ? C3 C2 H2D 3_656 . 109.5 ? C5 C2 H2D . . 109.5 ? H2C C2 H2D . . 108.1 ? C2 C3 N1 3_656 . 114.3(3) ? C2 C3 H3A 3_656 . 108.7 ? N1 C3 H3A . . 108.7 ? C2 C3 H3B 3_656 . 108.7 ? N1 C3 H3B . . 108.7 ? H3A C3 H3B . . 107.6 ? N2 C4 C1 . . 116.1(3) ? N2 C4 H4A . . 108.3 ? C1 C4 H4A . . 108.3 ? N2 C4 H4B . . 108.3 ? C1 C4 H4B . . 108.3 ? H4A C4 H4B . . 107.4 ? N2 C5 C2 . . 110.7(3) ? N2 C5 H5A . . 109.5 ? C2 C5 H5A . . 109.5 ? N2 C5 H5B . . 109.5 ? C2 C5 H5B . . 109.5 ? H5A C5 H5B . . 108.1 ? 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 Al F4 . 1.713(2) y Al F5 . 1.741(2) y Al F2 . 1.762(2) y Al F3 . 1.781(2) y Al F1 . 1.804(2) y Al O1 . 1.933(3) y O1 H1WA . 0.83(2) ? O1 H1WB . 0.82(2) ? O2 H2WA . 0.82(4) ? O2 H2WB . 0.81(2) ? N1 C1 . 1.478(4) y N1 C3 . 1.497(4) y N1 H1A . 0.9000 ? N1 H1B . 0.9000 ? N2 C5 . 1.407(4) y N2 C4 . 1.491(5) y N2 H2A . 0.9000 ? N2 H2B . 0.9000 ? C1 C4 . 1.506(5) y C1 H1C . 0.9700 ? C1 H1D . 0.9700 ? C2 C3 3_656 1.454(5) y C2 C5 . 1.503(5) y C2 H2C . 0.9700 ? C2 H2D . 0.9700 ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1 H1WA F4 3_655 0.83(2) 1.676(18) 2.501(3) 172(4) O1 H1WB O2 1_554 0.82(2) 1.84(2) 2.626(4) 161(4) O2 H2WA F3 3_556 0.82(4) 1.92(4) 2.610(4) 141(5) O2 H2WB F1 4_566 0.81(2) 1.92(2) 2.718(4) 166(4) N1 H1A F5 2_545 0.90 1.89 2.787(4) 173 N1 H1A F2 2_545 0.90 2.34 2.789(4) 111 N1 H1B F2 4_566 0.90 1.61 2.478(3) 161 N2 H2A F1 2_545 0.90 1.97 2.732(4) 141 N2 H2A F5 2_545 0.90 2.07 2.842(4) 144 N2 H2B F3 . 0.90 1.76 2.655(4) 173