#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/61/2006186.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_2006186 loop_ _publ_author_name 'Nightingale, David J.' 'Cronin, Leroy' 'Clark, James H.' _publ_contact_author ; Prof James H Clark Department of Chemistry University of York Heslington York YO1 5DD UK ; _publ_section_title ; Methylhexamethylenetetramine Fluoride Tetrahydrate, MeHMTAF.4H~2~O ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 789 _journal_page_last 791 _journal_paper_doi 10.1107/S0108270197000541 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac 'C7 H15 N4 + , F - , 4H2 O' _chemical_formula_sum 'C7 H23 F N4 O4' _chemical_formula_weight 246.29 _chemical_name_systematic ' methylhexamethylenetetramine fluoride tetrahydrate' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.52(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.854(4) _cell_length_b 6.352(4) _cell_length_c 19.372(6) _cell_measurement_reflns_used 20 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 8.81 _cell_measurement_theta_min 4.63 _cell_volume 1212.5(10) _computing_cell_refinement TEXSAN _computing_data_collection 'TEXSAN (Molecular Structure Corporation, 1992)' _computing_data_reduction TEXSAN _computing_molecular_graphics TEXSAN _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device AFC6S _diffrn_measurement_method \w--2\q _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 0.2597 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 1848 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.94 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_meas ? _exptl_crystal_description needle _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.28 _refine_diff_density_min -0.21 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 0.993 _refine_ls_goodness_of_fit_obs 1.301 _refine_ls_hydrogen_treatment 'H atoms: riding model' _refine_ls_matrix_type full _refine_ls_number_parameters 152 _refine_ls_number_reflns 1848 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.993 _refine_ls_restrained_S_obs 1.301 _refine_ls_R_factor_all 0.2852 _refine_ls_R_factor_obs .0828 _refine_ls_shift/esd_max -0.16 _refine_ls_shift/esd_mean 0.024 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0961P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.2541 _refine_ls_wR_factor_obs .1769 _reflns_number_observed 616 _reflns_number_total 1848 _reflns_observed_criterion >2sigma(I) _cod_data_source_file bm1129.cif _cod_data_source_block shelxl _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0961P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0961P)^2^] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1212.4(9) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2006186 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 N1 .040(4) .042(4) .041(4) .003(4) .008(3) -.001(4) N2 .044(5) .050(5) .058(5) .005(4) -.004(4) .001(4) N3 .042(4) .054(5) .048(5) -.003(4) .002(3) -.005(4) N4 .047(5) .042(5) .031(4) -.004(4) .009(3) -.001(4) C1 .043(5) .045(5) .038(5) .008(5) -.003(4) .009(5) C2 .062(7) .064(7) .042(5) -.006(6) .001(5) .008(5) C3 .047(6) .051(6) .056(6) -.008(5) .000(5) -.005(5) C4 .059(7) .032(6) .062(6) -.002(5) .005(5) -.003(5) C5 .051(6) .052(6) .039(5) -.009(5) .001(4) .010(5) C6 .031(5) .055(6) .053(6) -.003(5) -.006(4) -.014(5) C7 .066(6) .091(8) .053(6) .001(6) .005(5) -.018(6) O4 .084(5) .105(5) .071(4) .001(4) -.015(3) -.005(4) F1 .103(5) .081(4) .140(5) -.009(4) -.020(4) -.001(4) O1 .079(5) .082(5) .080(4) .005(4) .013(3) -.004(4) O3 .115(6) .080(5) .077(4) .011(4) -.003(4) .001(4) O2 .090(5) .092(5) .108(6) -.011(5) .006(4) .010(5) 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol N1 .2521(6) .4113(10) .6152(3) .041(2) Uani d . 1 . N N2 .1994(7) .0881(11) .5528(4) .051(2) Uani d . 1 . N N3 .3857(7) .3108(11) .5155(3) .048(2) Uani d . 1 . N N4 .1539(6) .4293(11) .4995(3) .040(2) Uani d . 1 . N C1 .1561(8) .5266(13) .5660(4) .042(2) Uani d . 1 . C H1A .058(4) .5260(13) .5864(10) .051 Uiso calc R 1 . H H1B .1871(14) .683(7) .5612(4) .051 Uiso calc R 1 . H C2 .2908(8) .4262(15) .4712(4) .056(3) Uani d . 1 . C H2A .3192(19) .554(8) .4663(6) .067 Uiso calc R 1 . H H2B .2884(8) .368(4) .431(3) .067 Uiso calc R 1 . H C3 .1084(9) .2115(13) .5083(4) .051(3) Uani d . 1 . C H3A .1024(10) .144(4) .463(2) .062 Uiso calc R 1 . H H3B .017(5) .2118(13) .5283(10) .062 Uiso calc R 1 . H C4 .3368(9) .0938(13) .5231(4) .051(3) Uani d . 1 . C H4A .402(3) .012(4) .5544(15) .061 Uiso calc R 1 . H H4B .3352(8) .022(4) .476(2) .061 Uiso calc R 1 . H C5 .2031(8) .1851(13) .6204(4) .047(2) Uani d . 1 . C H5A .271(3) .097(4) .6542(17) .057 Uiso calc R 1 . H H5B .102(5) .1821(13) .6426(12) .057 Uiso calc R 1 . H C6 .3924(7) .4070(14) .5827(4) .047(2) Uani d . 1 . C H6A .431(2) .567(7) .5782(4) .056 Uiso calc R 1 . H H6B .462(3) .319(4) .6156(16) .056 Uiso calc R 1 . H C7 .2563(8) .5138(16) .6842(4) .070(3) Uani d . 1 . C H7A .2912(8) .6542(16) .6798(4) .105 Uiso calc R 1 . H H7B .3140(8) .4341(16) .7147(4) .105 Uiso calc R 1 . H H7C .1663(8) .5191(16) .7028(4) .105 Uiso calc R 1 . H O4 .5368(6) -.0803(11) .6640(3) .087(2) Uani d . 1 . O F1 .1320(6) .5523(9) .2890(3) .108(2) Uani d . 1 . F O1 .0280(6) .1771(10) .3160(3) .080(2) Uani d . 1 . O O3 .2104(7) -.1117(10) .3627(3) .091(2) Uani d . 1 . O O2 .6086(6) .5413(11) .7218(3) .097(2) Uani d . 1 . O 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' F F 0.0171 0.0103 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C7 N1 C5 111.1(7) no C7 N1 C1 111.3(6) no C5 N1 C1 107.5(6) no C7 N1 C6 111.1(6) no C5 N1 C6 107.5(6) no C1 N1 C6 108.2(6) no C5 N2 C3 108.4(7) no C5 N2 C4 109.1(6) no C3 N2 C4 108.4(7) no C6 N3 C2 110.0(6) no C6 N3 C4 108.6(7) no C2 N3 C4 108.7(7) no C1 N4 C2 109.8(6) no C1 N4 C3 107.8(6) no C2 N4 C3 108.4(7) no N4 C1 N1 111.1(6) no N4 C2 N3 112.0(6) no N4 C3 N2 112.8(7) no N3 C4 N2 111.4(7) no N2 C5 N1 110.4(6) no N3 C6 N1 110.3(6) 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 N1 C7 . 1.488(9) no N1 C5 . 1.520(9) no N1 C1 . 1.523(8) no N1 C6 . 1.525(9) no N2 C5 . 1.447(9) no N2 C3 . 1.466(9) no N2 C4 . 1.476(9) no N3 C6 . 1.440(9) no N3 C2 . 1.461(9) no N3 C4 . 1.468(10) no N4 C1 . 1.429(8) no N4 C2 . 1.460(9) no N4 C3 . 1.465(9) no