 
data_nt0469_LH_Trip_CPh3
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         
'9-phosphatriptycene triphenylcarbenium tetrafluoroborate complex'
_chemical_name_common             
'9-phosphatriptycene triphenylcarbenium tetrafluoroborate complex'
_chemical_melting_point           ?
_chemical_formula_moiety          'C38 H28 P 1+, B F4 1-'
_chemical_formula_sum             'C38 H28 B F4 P' 
_chemical_formula_weight          602.39

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'   0.0090   0.0039
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0727   0.0534
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.2955   0.4335
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            167
_space_group_name_H-M_alt         'R -3 c :H'
_space_group_name_Hall            '-R 3 2"c'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z+1/2'
 'x-y, -y, -z+1/2'
 '-x, -x+y, -z+1/2'
 'x+2/3, y+1/3, z+1/3'
 '-y+2/3, x-y+1/3, z+1/3'
 '-x+y+2/3, -x+1/3, z+1/3'
 'y+2/3, x+1/3, -z+5/6'
 'x-y+2/3, -y+1/3, -z+5/6'
 '-x+2/3, -x+y+1/3, -z+5/6'
 'x+1/3, y+2/3, z+2/3'
 '-y+1/3, x-y+2/3, z+2/3'
 '-x+y+1/3, -x+2/3, z+2/3'
 'y+1/3, x+2/3, -z+7/6'
 'x-y+1/3, -y+2/3, -z+7/6'
 '-x+1/3, -x+y+2/3, -z+7/6'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z-1/2'
 '-x+y, y, z-1/2'
 'x, x-y, z-1/2'
 '-x+2/3, -y+1/3, -z+1/3'
 'y+2/3, -x+y+1/3, -z+1/3'
 'x-y+2/3, x+1/3, -z+1/3'
 '-y+2/3, -x+1/3, z-1/6'
 '-x+y+2/3, y+1/3, z-1/6'
 'x+2/3, x-y+1/3, z-1/6'
 '-x+1/3, -y+2/3, -z+2/3'
 'y+1/3, -x+y+2/3, -z+2/3'
 'x-y+1/3, x+2/3, -z+2/3'
 '-y+1/3, -x+2/3, z+1/6'
 '-x+y+1/3, y+2/3, z+1/6'
 'x+1/3, x-y+2/3, z+1/6'
 
_cell_length_a                    13.4876(2)
_cell_length_b                    13.4876(2)
_cell_length_c                    57.4638(16)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      9053.0(4)
_cell_formula_units_Z             12
_cell_measurement_temperature     295(2)
_cell_measurement_reflns_used     6752
_cell_measurement_theta_min       4.0660
_cell_measurement_theta_max       66.9570
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.326          
_exptl_crystal_F_000              3744
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.280
_exptl_crystal_size_mid           0.190
_exptl_crystal_size_min           0.073
_exptl_absorpt_coefficient_mu     1.239
_shelx_estimated_absorpt_T_min    0.723
_shelx_estimated_absorpt_T_max    0.915
_exptl_absorpt_correction_T_min   0.802
_exptl_absorpt_correction_T_max   0.917
_exptl_absorpt_correction_type    analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.16b (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       295(2)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source                    'fine-focus sealed tube'
_diffrn_radiation_monochromator   'multilayer mirror'                       
_diffrn_measurement_device_type   
;
Oxford Diffraction Xcalibur, Ruby, Gemini Ultra
; 
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  5.1856
_diffrn_reflns_number             24564
_diffrn_reflns_av_unetI/netI      0.0133
_diffrn_reflns_av_R_equivalents   0.0368
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -68
_diffrn_reflns_limit_l_max        61
_diffrn_reflns_theta_min          4.086
_diffrn_reflns_theta_max          66.922
_diffrn_reflns_theta_full         66.922
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              1799
_reflns_number_gt                 1529
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement        'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_reduction         'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_structure_solution     'SHELXT 2015 (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1415P)²+7.6459P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    dual
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          1799
_refine_ls_number_parameters      133
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0717
_refine_ls_R_factor_gt            0.0648
_refine_ls_wR_factor_ref          0.2122
_refine_ls_wR_factor_gt           0.2026
_refine_ls_goodness_of_fit_ref    1.079
_refine_ls_restrained_S_all       1.079
_refine_ls_shift/su_max           0.018
_refine_ls_shift/su_mean          0.003
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
P1 P 0.666667 0.333333 0.24610(2) 0.0522(4) Uani 1 3 d S T P . .
C1 C 0.7043(2) 0.4671(2) 0.23151(5) 0.0580(6) Uani 1 1 d . . . . .
C2 C 0.7373(2) 0.5745(2) 0.24066(5) 0.0669(7) Uani 1 1 d . . . . .
H2 H 0.743084 0.586206 0.256672 0.080 Uiso 1 1 calc R U . . .
C3 C 0.7614(3) 0.6642(2) 0.22553(6) 0.0783(9) Uani 1 1 d . . . . .
H3 H 0.784057 0.736527 0.231502 0.094 Uiso 1 1 calc R U . . .
C4 C 0.7523(3) 0.6474(3) 0.20191(7) 0.0832(9) Uani 1 1 d . . . . .
H4 H 0.767269 0.708150 0.192098 0.100 Uiso 1 1 calc R U . . .
C5 C 0.7211(3) 0.5417(3) 0.19246(5) 0.0730(8) Uani 1 1 d . . . . .
H5 H 0.716022 0.531307 0.176416 0.088 Uiso 1 1 calc R U . . .
C6 C 0.6975(2) 0.4507(2) 0.20728(5) 0.0627(7) Uani 1 1 d . . . . .
C7 C 0.666667 0.333333 0.19808(9) 0.0629(11) Uani 1 3 d S T P . .
H7 H 0.666667 0.333333 0.181025 0.075 Uiso 1 3 calc R U P . .
C8 C 0.666667 0.333333 0.27888(8) 0.0530(10) Uani 1 3 d S T P . .
C9 C 0.5499(2) 0.3161(2) 0.28696(4) 0.0554(6) Uani 1 1 d . . . . .
C10 C 0.5066(2) 0.3825(3) 0.27774(5) 0.0676(7) Uani 1 1 d . . . . .
H10 H 0.548466 0.437835 0.266600 0.081 Uiso 1 1 calc R U . . .
C11 C 0.4023(3) 0.3668(3) 0.28497(6) 0.0816(9) Uani 1 1 d . . . . .
H11 H 0.373779 0.410767 0.278531 0.098 Uiso 1 1 calc R U . . .
C12 C 0.3404(3) 0.2865(3) 0.30163(7) 0.0878(10) Uani 1 1 d . . . . .
H12 H 0.269690 0.275434 0.306387 0.105 Uiso 1 1 calc R U . . .
C13 C 0.3831(3) 0.2228(3) 0.31122(6) 0.0787(9) Uani 1 1 d . . . . .
H13 H 0.341829 0.169302 0.322703 0.094 Uiso 1 1 calc R U . . .
C14 C 0.4872(2) 0.2375(2) 0.30397(5) 0.0649(7) Uani 1 1 d . . . . .
H14 H 0.515385 0.193722 0.310652 0.078 Uiso 1 1 calc R U . . .
F1 F 0.8999(3) 0.9217(4) 0.19077(10) 0.1943(18) Uani 1 1 d . . . . .
F2 F 1.000000 1.000000 0.22181(14) 0.400(11) Uani 1 3 d S T P . .
B1 B 1.000000 1.000000 0.20061(19) 0.106(3) Uani 1 3 d S T P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
P1 C1 1.816(3) . ?
P1 C1 1.816(3) 3_665 ?
P1 C1 1.816(3) 2_655 ?
P1 C8 1.884(5) . ?
C1 C2 1.389(4) . ?
C1 C6 1.405(4) . ?
C2 C3 1.390(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.372(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.380(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.517(3) . ?
C7 H7 0.9800 . ?
C8 C9 1.544(3) 2_655 ?
C8 C9 1.544(3) 3_665 ?
C8 C9 1.544(3) . ?
C9 C14 1.378(4) . ?
C9 C10 1.395(4) . ?
C10 C11 1.377(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.372(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.366(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.381(4) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
F1 B1 1.353(6) . ?
F2 B1 1.218(14) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C1 P1 C1 100.39(11) . 3_665 ?
C1 P1 C1 100.39(11) . 2_655 ?
C1 P1 C1 100.39(11) 3_665 2_655 ?
C1 P1 C8 117.49(9) . . ?
C1 P1 C8 117.49(9) 3_665 . ?
C1 P1 C8 117.49(9) 2_655 . ?
C2 C1 C6 120.1(2) . . ?
C2 C1 P1 130.2(2) . . ?
C6 C1 P1 109.71(19) . . ?
C1 C2 C3 119.0(3) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 121.0(3) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 119.1(3) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C1 119.9(3) . . ?
C5 C6 C7 121.9(3) . . ?
C1 C6 C7 118.1(3) . . ?
C6 C7 C6 108.5(2) 3_665 . ?
C6 C7 C6 108.5(2) 3_665 2_655 ?
C6 C7 C6 108.5(2) . 2_655 ?
C6 C7 H7 110.4 3_665 . ?
C6 C7 H7 110.4 . . ?
C6 C7 H7 110.4 2_655 . ?
C9 C8 C9 111.36(17) 2_655 3_665 ?
C9 C8 C9 111.36(17) 2_655 . ?
C9 C8 C9 111.36(17) 3_665 . ?
C9 C8 P1 107.51(18) 2_655 . ?
C9 C8 P1 107.51(18) 3_665 . ?
C9 C8 P1 107.51(18) . . ?
C14 C9 C10 118.0(2) . . ?
C14 C9 C8 121.1(2) . . ?
C10 C9 C8 120.8(2) . . ?
C11 C10 C9 120.7(3) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 C10 120.2(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C11 119.8(3) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 120.4(3) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C9 C14 C13 120.9(3) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
F2 B1 F1 114.7(5) . 3_675 ?
F2 B1 F1 114.7(5) . . ?
F1 B1 F1 103.8(5) 3_675 . ?
F2 B1 F1 114.7(5) . 2_765 ?
F1 B1 F1 103.8(5) 3_675 2_765 ?
F1 B1 F1 103.8(5) . 2_765 ?
 
_refine_diff_density_max    0.562
_refine_diff_density_min   -0.416
_refine_diff_density_rms    0.064



# start Validation Reply Form
_vrf_PLAT260_nt0469_LH_Trip_CPh3
;
PROBLEM: Large Average Ueq of Residue Including        F1      0.233 Check 
RESPONSE: Large thermal motion of the BH4- anion.
;
_vrf_PLAT340_nt0469_LH_Trip_CPh3
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00425 Ang.  
RESPONSE: Large thermal motion.
;
# end Validation Reply Form