#------------------------------------------------------------------------------
#$Date: 2017-10-13 08:28:26 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201972 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/19/2101914.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_2101914
loop_
_publ_author_name
'Lloyd, M. A.'
'Brock, C. P.'
_publ_section_title
;
 [MPh₄][BPh₄], M = P, As and Sb
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              773
_journal_page_last               779
_journal_paper_doi               10.1107/S0108768197005077
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         '(C24 H20 P+), (C24H20B-)'
_chemical_formula_sum            'C48 H40 B P'
_chemical_formula_weight         658.63
_chemical_name_systematic
;
tetraphenylphosphonium tetraphenylborate
;
_chemical_temperature_decomposition 548(5)
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   15.7960(10)
_cell_length_b                   15.7960(10)
_cell_length_c                   14.1980(10)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      13.1
_cell_volume                     3542.6(4)
_computing_cell_refinement       'CAD4 (ENRAF-Nonius, 1989)'
_computing_data_collection       'CAD4 (ENRAF-Nonius, 1989)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_measurement_device       'ENRAF-Nonius CAD4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0098
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2274
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        <0.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'initially colorless (see text)'
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_meas      ?
_exptl_crystal_description
;
See Fig. 1
;
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.23
_refine_ls_abs_structure_details '0.1(2) (Flack, 1977)'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.21
_refine_ls_goodness_of_fit_obs   1.214
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_obs          0.050
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1172P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.172
_refine_ls_wR_factor_obs         0.1567
_reflns_number_observed          1889
_reflns_number_total             2264
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cr0521.cif
_cod_data_source_block           PPh8B
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as 'd. 275(5)_C'. The value 'd. 275(5)_C' was changed to '548(5)' -
it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as 'd. 275(5)_C'. The value 'd. 275(5)_C' was changed to '548(5)' -
it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3542.3(4)
_cod_database_code               2101914
_cod_database_fobs_code          2101914
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
P1 0.0000 0.0000 0.0000 0.0353(10) Uani d S 1 P
C1 0.0710(2) 0.0570(2) 0.0744(2) 0.0346(13) Uani d G 1 C
C2 0.0919(2) 0.1410(2) 0.0571(2) 0.0430(14) Uani d G 1 C
C3 0.1502(2) 0.1822(2) 0.1144(2) 0.057(2) Uani d G 1 C
C4 0.1876(2) 0.1392(3) 0.1890(2) 0.056(2) Uani d G 1 C
C5 0.1668(2) 0.0552(3) 0.2063(2) 0.055(2) Uani d G 1 C
C6 0.1085(2) 0.0141(2) 0.1490(3) 0.047(2) Uani d G 1 C
P2 0.0000 0.5000 0.2500 0.0350(9) Uani d S 1 P
C7 0.0711(2) 0.4430(2) 0.3254(2) 0.045(2) Uani d G 1 C
C8 0.0879(3) 0.3575(2) 0.3114(2) 0.0475(15) Uani d G 1 C
C9 0.1434(3) 0.3152(2) 0.3710(3) 0.054(2) Uani d G 1 C
C10 0.1822(2) 0.3584(3) 0.4446(2) 0.057(2) Uani d G 1 C
C11 0.1654(2) 0.4439(3) 0.4586(2) 0.055(2) Uani d G 1 C
C12 0.1098(2) 0.4862(2) 0.3990(3) 0.047(2) Uani d G 1 C
B1 0.0000 0.0000 0.5000 0.029(3) Uani d S 1 B
C13 0.0684(2) 0.0515(2) 0.5706(2) 0.0332(12) Uani d G 1 C
C14 0.0821(2) 0.1383(2) 0.5642(2) 0.0451(14) Uani d G 1 C
C15 0.1375(2) 0.1778(2) 0.6263(3) 0.059(2) Uani d G 1 C
C16 0.1791(2) 0.1307(3) 0.6947(2) 0.061(2) Uani d G 1 C
C17 0.1654(2) 0.0440(3) 0.7011(2) 0.058(2) Uani d G 1 C
C18 0.1100(2) 0.0044(2) 0.6391(3) 0.0458(12) Uani d G 1 C
B2 0.0000 0.5000 0.7500 0.033(4) Uani d S 1 B
C19 0.0666(2) 0.4455(2) 0.8220(2) 0.0371(13) Uani d G 1 C
C20 0.0817(2) 0.3594(2) 0.8114(2) 0.0458(15) Uani d G 1 C
C21 0.1393(3) 0.3187(2) 0.8701(3) 0.054(2) Uani d G 1 C
C22 0.1817(2) 0.3642(3) 0.9393(2) 0.055(2) Uani d G 1 C
C23 0.1666(2) 0.4504(3) 0.9499(2) 0.051(2) Uani d G 1 C
C24 0.1091(2) 0.4910(2) 0.8912(3) 0.0489(14) Uani d G 1 C
H2 0.0669(3) 0.1698(3) 0.0071(3) 0.052 Uiso calc R 1 H
H3 0.1642(4) 0.2384(2) 0.1028(4) 0.068 Uiso calc R 1 H
H4 0.2267(3) 0.1667(4) 0.2273(3) 0.067 Uiso calc R 1 H
H5 0.1918(3) 0.0264(4) 0.2562(3) 0.066 Uiso calc R 1 H
H6 0.0945(3) -0.0422(2) 0.1606(4) 0.056 Uiso calc R 1 H
H8 0.0619(4) 0.3287(3) 0.2622(3) 0.057 Uiso calc R 1 H
H9 0.1546(4) 0.2581(2) 0.3616(4) 0.065 Uiso calc R 1 H
H10 0.2193(3) 0.3301(4) 0.4845(4) 0.068 Uiso calc R 1 H
H11 0.1913(3) 0.4728(4) 0.5079(3) 0.066 Uiso calc R 1 H
H12 0.0986(4) 0.5433(2) 0.4084(4) 0.057 Uiso calc R 1 H
H14 0.0542(3) 0.1698(3) 0.5184(3) 0.054 Uiso calc R 1 H
H15 0.1466(3) 0.2359(2) 0.6220(4) 0.071 Uiso calc R 1 H
H16 0.2161(3) 0.1572(4) 0.7363(3) 0.073 Uiso calc R 1 H
H17 0.1933(3) 0.0124(4) 0.7469(3) 0.070 Uiso calc R 1 H
H18 0.1009(3) -0.0536(2) 0.6433(4) 0.055 Uiso calc R 1 H
H20 0.0533(3) 0.3289(3) 0.7651(3) 0.055 Uiso calc R 1 H
H21 0.1494(4) 0.2610(2) 0.8630(4) 0.064 Uiso calc R 1 H
H22 0.2202(3) 0.3370(4) 0.9786(4) 0.066 Uiso calc R 1 H
H23 0.1950(3) 0.4808(4) 0.9962(3) 0.061 Uiso calc R 1 H
H24 0.0989(4) 0.5487(2) 0.8983(4) 0.059 Uiso calc R 1 H
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_3
_geom_angle
_geom_angle_publ_flag
C1 P1 C1 2 107.4(2) yes
C1 P1 C1 3 110.50(11) yes
C2 C1 P1 . 121.8(2) yes
C4 C1 P1 . 177.1(3) yes
C7 P2 C7 2_565 106.7(2) yes
C7 P2 C7 8 110.88(13) yes
C8 C7 P2 . 121.4(2) yes
C10 C7 P2 . 178.6(2) yes
C13 B1 C13 2 106.9(2) yes
C13 B1 C13 3_556 110.76(12) yes
C14 C13 B1 . 122.5(2) yes
C16 C13 B1 . 177.0(2) yes
C19 B2 C19 2_565 106.1(2) yes
C19 B2 C19 7_456 111.18(13) yes
C20 C19 B2 . 122.5(2) yes
C22 C19 B2 . 176.8(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
P1 C1 1.784(3) yes
P2 C7 1.794(3) yes
B1 C13 1.684(3) yes
B2 C19 1.701(3) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
_geom_torsion_publ_flag
P1 P1 C1 C2 1_556 -135.4(3) no
P1 P1 C1 C3 1_556 -138.3(5) no
P1 P1 C1 C5 1_556 49.7(4) no
P1 P1 C1 C6 1_556 47.2(2) no
P2 P2 C7 C8 1_556 131.6(3) no
P2 P2 C7 C9 1_556 131.7(6) no
P2 P2 C7 C11 1_556 -48.7(4) no
P2 P2 C7 C12 1_556 -48.6(2) no
B1 B1 C13 C14 1_556 -124.7(2) no
B1 B1 C13 C15 1_556 -122.6(5) no
B1 B1 C13 C17 1_556 51.7(3) no
B1 B1 C13 C18 1_556 53.4(2) no
B2 B2 C19 C20 1_556 129.7(3) no
B2 B2 C19 C21 1_556 132.3(6) no
B2 B2 C19 C23 1_556 -54.9(4) no
B2 B2 C19 C24 1_556 -52.7(2) no
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 8006796
