#------------------------------------------------------------------------------ #$Date: 2017-10-13 01:08:28 +0100 (Fri, 13 Oct 2017) $ #$Revision: 201955 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/53/2005308.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_2005308 loop_ _publ_author_name 'Kaplan, R. W.' 'Turnbull, M. M.' _publ_contact_author 'Mark M. Turnbull' _publ_section_title ; 2,2,6,6-Tetramethylpiperidinium Chloride ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2049 _journal_page_last 2051 _journal_paper_doi 10.1107/S0108270196001679 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac 'C9 H20 N + , Cl -' _chemical_formula_sum 'C9 H20 Cl N' _chemical_formula_weight 177.71 _chemical_name_systematic ; 2,2,6,6-Tetramethylpiperidinium chloride ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _audit_creation_method SHELXL _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.754(2) _cell_length_b 8.910(1) _cell_length_c 12.992(2) _cell_measurement_reflns_used 28 _cell_measurement_temperature 158(2) _cell_measurement_theta_max 12.48 _cell_measurement_theta_min 4.84 _cell_volume 1013.4(3) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Fait, 1991)' _computing_data_reduction 'SHELXTL (Sheldrick, 1985)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 158(2) _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 3804 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_min 2.77 _diffrn_standards_decay_% 3.20 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.321 _exptl_absorpt_correction_T_max 0.3799 _exptl_absorpt_correction_T_min 0.3592 _exptl_absorpt_correction_type '\y scans (SHELXTL; Sheldrick, 1985)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.165 _exptl_crystal_description small_prism _exptl_crystal_F_000 392 _exptl_crystal_size_max .4 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .15 _refine_diff_density_max .257 _refine_diff_density_min -.206 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack 0.08(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 0.819 _refine_ls_goodness_of_fit_obs 0.889 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 106 _refine_ls_number_reflns 1790 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.819 _refine_ls_restrained_S_obs 0.889 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_obs 0.0405 _refine_ls_shift/esd_max -0.005 _refine_ls_shift/esd_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0343P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0845 _refine_ls_wR_factor_obs 0.0804 _reflns_number_observed 1394 _reflns_number_total 1790 _reflns_observed_criterion >2sigma(I) _cod_data_source_file ta1077.cif _cod_data_source_block rwk74 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0343P)^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^)+(0.0343P)^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 1013.3(3) _cod_database_code 2005308 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' 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 Cl 0.0279(4) 0.0202(3) 0.0366(4) -0.0011(4) -0.0021(4) 0.0026(4) N1 0.0188(12) 0.0151(12) 0.0232(13) 0.0019(11) 0.0010(11) 0.0026(10) C2 0.023(2) 0.0221(15) 0.020(2) 0.0017(13) -0.0001(12) -0.0058(13) C3 0.026(2) 0.0191(14) 0.034(2) -0.0001(12) 0.002(2) -0.009(2) C4 0.025(2) 0.0210(15) 0.043(2) -0.0002(14) 0.005(2) 0.0058(14) C5 0.026(2) 0.027(2) 0.025(2) 0.0017(14) 0.0061(13) 0.0075(15) C6 0.029(2) 0.023(2) 0.018(2) -0.0030(13) 0.0041(13) 0.0037(14) C7 0.029(2) 0.036(2) 0.028(2) 0.0009(15) -0.0041(15) 0.003(2) C8 0.038(2) 0.027(2) 0.031(2) 0.0035(15) 0.005(2) 0.0017(15) C9 0.029(2) 0.027(2) 0.033(2) 0.0019(14) 0.011(2) 0.002(2) C10 0.039(2) 0.030(2) 0.025(2) -0.0038(15) 0.000(2) -0.0021(15) loop_ _atom_site_label _atom_site_occupancy _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_type_symbol Cl 1 .17837(8) .33654(8) .29046(6) .0282(2) Uani d . Cl N1 1 .1617(3) -0.3194(3) .2327(2) .0190(5) Uani d . N H1A 1 .159(3) -0.419(3) .247(2) .023 Uiso d . H H1B 1 .060(3) -0.294(3) .224(2) .023 Uiso d . H C2 1 .2266(3) -0.2289(3) .3212(2) .0217(7) Uani d . C C3 1 .2281(3) -.0645(3) .2877(3) .0263(8) Uani d . C H3A 1 .1216(3) -.0275(3) .2836(3) .032 Uiso calc R H H3B 1 .2820(3) -.0043(3) .3405(3) .032 Uiso calc R H C4 1 .3057(4) -.0411(3) .1839(2) .0297(8) Uani d . C H4A 1 .3015(4) .0665(3) .1650(2) .036 Uiso calc R H H4B 1 .4145(4) -.0709(3) .1888(2) .036 Uiso calc R H C5 1 .2272(3) -0.1338(3) .1015(2) .0259(7) Uani d . C H5A 1 .2796(3) -0.1167(3) .0350(2) .031 Uiso calc R H H5B 1 .1205(3) -.0985(3) .0942(2) .031 Uiso calc R H C6 1 .2258(3) -0.3021(3) .1242(2) .0230(7) Uani d . C C7 1 .3834(4) -0.2848(4) .3519(2) .0309(8) Uani d . C H7A 1 .4550(4) -0.2687(4) .2950(2) .046 Uiso calc R H H7B 1 .3780(4) -0.3921(4) .3678(2) .046 Uiso calc R H H7C 1 .4186(4) -0.2297(4) .4127(2) .046 Uiso calc R H C8 1 .1162(4) -0.2539(4) .4101(2) .0321(8) Uani d . C H8A 1 .0145(4) -0.2177(4) .3907(2) .048 Uiso calc R H H8B 1 .1521(4) -0.1989(4) .4708(2) .048 Uiso calc R H H8C 1 .1110(4) -0.3613(4) .4261(2) .048 Uiso calc R H C9 1 .3831(3) -0.3753(3) .1154(2) .0297(8) Uani d . C H9A 1 .4553(3) -0.3230(3) .1606(2) .045 Uiso calc R H H9B 1 .4188(3) -0.3690(3) .0440(2) .045 Uiso calc R H H9C 1 .3761(3) -0.4809(3) .1360(2) .045 Uiso calc R H C10 1 .1157(4) -0.3827(4) .0543(2) .0313(8) Uani d . C H10A 1 .0146(4) -0.3361(4) .0596(2) .047 Uiso calc R H H10B 1 .1090(4) -0.4884(4) .0747(2) .047 Uiso calc R H H10C 1 .1519(4) -0.3760(4) -.0170(2) .047 Uiso calc R H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 '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 C2 N1 C6 120.6(2) y C7 C2 N1 111.4(2) y C7 C2 C8 109.1(2) y N1 C2 C8 105.1(2) y C7 C2 C3 112.5(3) y N1 C2 C3 107.3(2) y C8 C2 C3 111.2(3) y C4 C3 C2 112.7(2) y C5 C4 C3 110.4(2) y C4 C5 C6 113.7(3) y C10 C6 N1 105.9(2) y C10 C6 C9 109.2(2) y N1 C6 C9 110.9(2) y C10 C6 C5 110.9(3) y N1 C6 C5 106.3(2) y C9 C6 C5 113.4(2) y loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N1 C2 1.515(4) y N1 C6 1.525(4) y C2 C7 1.513(4) y C2 C8 1.523(4) y C2 C3 1.528(4) y C3 C4 1.525(4) y C4 C5 1.516(4) y C5 C6 1.528(4) y C6 C10 1.506(4) y C6 C9 1.528(4) y loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 107545