The phases of [(CH~3~)~4~N](ClO~4~) at low temperature
Palacios, Elías; Burriel, Ramón; Ferloni, Paolo; Acta Crystallographica Section B 59 (2003) 625–633; doi:10.1107/S0108768103019013

data_2103957
_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_paper_doi               10.1107/S0108768103019013
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'C4 H12N, Cl O4'
_chemical_formula_sum            'C4 H12 Cl N O4'
_chemical_formula_weight         173.60
_chemical_name_systematic
;
 Tetramethylammonium perchlorate
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            4
_cell_length_a                   11.714(3)
_cell_length_b                   11.784(3)
_cell_length_c                   5.8265(9)
_cell_measurement_reflns_used    55
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      1.7
_cell_volume                     804.3(3)
_computing_cell_refinement       FULLPROF
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(5)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens P4'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1729
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.269
_refine_diff_density_min         -1.386
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1389
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.873
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2334
_refine_ls_wR_factor_ref         0.2477
_reflns_number_gt                1210
_reflns_number_total             1389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bs0018.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2~1~ 2~1~ 2'
_cod_database_code               2103957
_cod_database_fobs_code          2103957