#------------------------------------------------------------------------------
#$Date: 2016-02-20 01:53:41 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176768 $
#$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
loop_
_publ_author_name
'Palacios, Elías'
'Burriel, Ramón'
'Ferloni, Paolo'
_publ_section_title
;
 The phases of [(CH₃)₄N](ClO₄) at low temperature
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              625
_journal_page_last               633
_journal_paper_doi               10.1107/S0108768103019013
_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
;
_space_group_IT_number           129
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2a'
_symmetry_space_group_name_H-M   'P 4/n m m :2'
_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       'ω--2θ 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/[σ²(Fo²)+(0.0430P)²+0.1615P] where P=(Fo²+2Fc²)/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)
_cod_data_source_file            bs0018.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               2103958
_cod_database_fobs_code          2103958
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_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_
_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_
_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
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
