Structures of amino(triphenyl)phosphonium bromide and amino(triphenyl)phosphonium hexachloroantimonate
Pohl, E.; Gosink, H. J.; Herbst-Irmer, R.; Noltemeyer, M.; Roesky, H. W.; Sheldrick, G. M.; Acta Crystallographica Section C 49 (1993) 1280–1283; doi:10.1107/S0108270192013180

data_2001500
_publ_section_title
;
 Structures of amino(triphenyl)phosphonium bromide and
 amino(triphenyl)phosphonium hexachloroantimonate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1280
_journal_page_last               1283
_journal_paper_doi               10.1107/S0108270192013180
_journal_volume                  49
_journal_year                    1993
_chemical_formula_sum            'C18 H17 Cl6 N P Sb'
_chemical_formula_weight         612.75
_chemical_name_systematic
;
Aminotriphenylphosphonium hexachloroantimonate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.3940(10)
_cell_length_b                   16.7120(10)
_cell_length_c                   20.177(2)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293.0(10)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     4853.5(7)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 19??)'
_computing_publication_material  SHELXL-92
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1992)'
_computing_structure_solution    'SHELXS-92 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.0(10)
_diffrn_measurement_device       'Stoe-Siemens AED four-circle-diffractometer'
_diffrn_measurement_method       'Profile data from 2\q/\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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6622
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.868
_exptl_absorpt_correction_T_max  0.233
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       Block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.348
_refine_ls_extinction_coef       0.00046(4)
_refine_ls_extinction_method     SHELXL-92
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.079
_refine_ls_hydrogen_treatment
;  Coordinates of H atoms attached to N refined with distance restraints;
   those of C-H H atoms not refined
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         6320
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.079
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_obs          '0.0302 for F > 4\s(F)'
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w=1/[s^2^(Fo^2^) + (0.0225P)^2^ + 5.7476P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.0667
_refine_ls_wR_factor_obs         '0.0625 for F > 4\s(F)'
_reflns_number_observed          5329
_reflns_number_total             6320
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            sh1034.cif
_cod_data_source_block           dada
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C18 H17 Cl6 N1 P1 Sb1'
_cod_database_code               2001500