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_2103958
_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 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       '\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)
_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