#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/39/2103958.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_2103958 _space_group_IT_number 129 _symmetry_space_group_name_Hall '-P 4a 2a' _symmetry_space_group_name_H-M 'P 4/n m m :2' _[local]_cod_cif_authors_sg_H-M 'P 4/n m m' loop_ _publ_author_name 'Palacios, El\'ias' 'Burriel, Ram\'on' 'Ferloni, Paolo' _publ_section_title ; The phases of [(CH~3~)~4~N](ClO~4~) at low temperature ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 625 _journal_page_last 633 _journal_volume 59 _journal_year 2003 _chemical_formula_moiety 'C4 H12 N, Cl O4' _chemical_formula_sum 'C4 H12 Cl N O4' _chemical_formula_weight 173.60 _chemical_name_systematic ; tetramethylammonium perchlorate ; _symmetry_cell_setting tetragonal _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.2376(14) _cell_length_b 8.2376(14) _cell_length_c 5.8256(12) _cell_measurement_reflns_used 45 _cell_measurement_temperature 210.0(10) _cell_measurement_theta_max 30.4 _cell_measurement_theta_min 3.5 _cell_volume 395.31(13) _computing_cell_refinement FULLPROF _computing_data_collection 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 210(5) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w--2\q scan' _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 0.046 _diffrn_reflns_av_sigmaI/netI 0.1055 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 1534 _diffrn_reflns_theta_full 30.45 _diffrn_reflns_theta_max 30.45 _diffrn_reflns_theta_min 3.50 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.446 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 184 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.732 _refine_diff_density_min -0.6572 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.254 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 36 _refine_ls_number_reflns 376 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.255 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0567 _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^)+(0.0430P)^2^+0.1615P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1325 _refine_ls_wR_factor_ref 0.1358 _reflns_number_gt 331 _reflns_number_total 376 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file bs0018.cif _[local]_cod_data_source_block II loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z' '-y, -x, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z' '-x-1/2, y, z' '-y-1/2, -x-1/2, z' 'y, x, z' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_type_symbol N 0.7500 0.2500 0.5000 0.0253(7) Uani d S 1 N C 0.2500 0.6030(3) 0.3538(4) 0.0409(6) Uani d S 1 C H1 0.2500 0.5030 0.4520 0.050(10) Uiso d S 1 H H2 0.3490 0.6020 0.2560 0.053(6) Uiso d . 1 H Cl 0.2307(8) 0.2500 -0.0742(2) 0.0252(10) Uani d SPD 0.25 Cl O1 0.2500 0.2500 0.1644(6) 0.0532(11) Uani d SD 1 O O2 0.1453(11) 0.3892(5) -0.1398(7) 0.069(3) Uani d PD 0.25 O O3 0.3832(12) 0.2500 -0.1790(11) 0.143(10) Uani d SPD 0.25 O 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 N 0.0236(10) 0.0236(10) 0.0286(14) 0.000 0.000 0.000 C 0.0461(15) 0.0348(13) 0.0419(13) 0.000 0.000 -0.0123(10) Cl 0.012(5) 0.034(6) 0.0297(5) 0.000 0.0008(7) 0.000 O1 0.0613(18) 0.0613(18) 0.0370(19) 0.000 0.000 0.000 O2 0.085(8) 0.036(4) 0.088(4) 0.012(4) -0.050(5) 0.003(4) O3 0.105(13) 0.17(2) 0.151(13) 0.000 0.105(11) 0.000 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 C 4 1.481(2) yes N C 9_666 1.481(2) no N C 3_655 1.481(2) no N C 10_656 1.481(2) no C N 9_666 1.481(2) no Cl O1 . 1.399(3) yes Cl O2 . 1.398(3) yes Cl O3 . 1.397(3) yes 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 N C 4 9_666 109.31(11) yes C N C 4 3_655 109.8(2) yes C N C 9_666 3_655 109.31(11) no C N C 4 10_656 109.31(11) no C N C 9_666 10_656 109.8(2) no C N C 3_655 10_656 109.31(11) no O3 Cl O2 . 13_565 109.44(11) no O3 Cl O2 . . 109.44(11) no O2 Cl O2 13_565 . 110.2(4) no O3 Cl O1 . . 109.38(11) no O2 Cl O1 13_565 . 109.19(10) no O2 Cl O1 . . 109.19(10) no _cod_database_code 2103958