 
data_nt0246_LeiHu_LH59
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_systematic         '9-hydroxy-10-phosphatriptycene'
_chemical_name_common             '9-hydroxy-10-phosphatriptycene'
_chemical_melting_point           ?
_chemical_formula_moiety          'C19 H13 O P' 
_chemical_formula_sum             'C19 H13 O P' 
_chemical_formula_weight          288.26

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'
 'O'  'O'   0.0492   0.0322
 '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       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_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'
 '-x, -y, -z'
 
_cell_length_a                    7.2966(4)
_cell_length_b                    8.2064(4)
_cell_length_c                    13.0501(7)
_cell_angle_alpha                 82.694(4)
_cell_angle_beta                  80.962(4)
_cell_angle_gamma                 69.948(5)
_cell_volume                      722.67(7)
_cell_formula_units_Z             2
_cell_measurement_temperature     295(2)
_cell_measurement_reflns_used     3430
_cell_measurement_theta_min       5.7330
_cell_measurement_theta_max       67.0640
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.325          
_exptl_crystal_F_000              300
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.150
_exptl_crystal_size_mid           0.110
_exptl_crystal_size_min           0.031
_exptl_absorpt_coefficient_mu     1.633
_shelx_estimated_absorpt_T_min    0.792
_shelx_estimated_absorpt_T_max    0.951
_exptl_absorpt_correction_T_min   0.844
_exptl_absorpt_correction_T_max   0.957
_exptl_absorpt_correction_type    analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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.
;
_exptl_absorpt_special_details    ?
_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  10.3712
_diffrn_reflns_number             5760
_diffrn_reflns_av_unetI/netI      0.0236
_diffrn_reflns_av_R_equivalents   0.0206
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.440
_diffrn_reflns_theta_max          67.123
_diffrn_reflns_theta_full         67.123
_diffrn_measured_fraction_theta_max   0.988
_diffrn_measured_fraction_theta_full  0.988
_diffrn_reflns_Laue_measured_fraction_max    0.988
_diffrn_reflns_Laue_measured_fraction_full   0.988
_diffrn_reflns_point_group_measured_fraction_max   0.988
_diffrn_reflns_point_group_measured_fraction_full  0.988
_reflns_number_total              2557
_reflns_number_gt                 2283
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction         'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL-2018/1 (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)+(0.0503P)²+0.2511P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    dual
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          2557
_refine_ls_number_parameters      193
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0416
_refine_ls_R_factor_gt            0.0365
_refine_ls_wR_factor_ref          0.1044
_refine_ls_wR_factor_gt           0.1000
_refine_ls_goodness_of_fit_ref    1.052
_refine_ls_restrained_S_all       1.052
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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 0.48919(7) -0.01878(6) 0.77639(4) 0.04190(17) Uani 1 1 d . . . . .
O1 O -0.0996(2) 0.0785(2) 0.70866(13) 0.0563(4) Uani 1 1 d . . . . .
H1 H -0.154(4) 0.025(4) 0.750(2) 0.084 Uiso 1 1 d . U . . .
C1 C 0.2001(3) 0.1286(2) 0.64579(15) 0.0407(4) Uani 1 1 d . . . . .
C2 C 0.3950(3) 0.1053(2) 0.65721(14) 0.0391(4) Uani 1 1 d . . . . .
C3 C 0.5063(3) 0.1790(3) 0.58225(15) 0.0449(4) Uani 1 1 d . . . . .
H3 H 0.636648 0.161885 0.589194 0.054 Uiso 1 1 calc R U . . .
C4 C 0.4226(3) 0.2785(3) 0.49688(16) 0.0529(5) Uani 1 1 d . . . . .
H4 H 0.496235 0.329719 0.446970 0.064 Uiso 1 1 calc R U . . .
C5 C 0.2305(3) 0.3016(3) 0.48594(17) 0.0559(5) Uani 1 1 d . . . . .
H5 H 0.175315 0.368260 0.428397 0.067 Uiso 1 1 calc R U . . .
C6 C 0.1179(3) 0.2263(3) 0.55983(16) 0.0501(5) Uani 1 1 d . . . . .
H6 H -0.011359 0.241557 0.551544 0.060 Uiso 1 1 calc R U . . .
C7 C 0.0899(3) 0.1192(2) 0.83486(15) 0.0424(4) Uani 1 1 d . . . . .
C8 C 0.2733(3) 0.0997(2) 0.86300(15) 0.0419(4) Uani 1 1 d . . . . .
C9 C 0.2865(3) 0.1710(3) 0.95120(16) 0.0513(5) Uani 1 1 d . . . . .
H9 H 0.409002 0.159513 0.969149 0.062 Uiso 1 1 calc R U . . .
C10 C 0.1170(4) 0.2594(3) 1.01255(18) 0.0611(6) Uani 1 1 d . . . . .
H10 H 0.125666 0.307165 1.071804 0.073 Uiso 1 1 calc R U . . .
C11 C -0.0636(4) 0.2765(3) 0.98593(18) 0.0633(6) Uani 1 1 d . . . . .
H11 H -0.176979 0.334861 1.027792 0.076 Uiso 1 1 calc R U . . .
C12 C -0.0787(3) 0.2078(3) 0.89733(17) 0.0531(5) Uani 1 1 d . . . . .
H12 H -0.201802 0.220905 0.879613 0.064 Uiso 1 1 calc R U . . .
C13 C 0.2058(3) -0.1519(2) 0.74250(14) 0.0418(4) Uani 1 1 d . . . . .
C14 C 0.3978(3) -0.1984(2) 0.76715(14) 0.0415(4) Uani 1 1 d . . . . .
C15 C 0.5108(3) -0.3720(3) 0.77868(16) 0.0499(5) Uani 1 1 d . . . . .
H15 H 0.637958 -0.403257 0.795906 0.060 Uiso 1 1 calc R U . . .
C16 C 0.4341(4) -0.4993(3) 0.76448(18) 0.0590(6) Uani 1 1 d . . . . .
H16 H 0.509564 -0.616175 0.772895 0.071 Uiso 1 1 calc R U . . .
C17 C 0.2477(4) -0.4538(3) 0.73815(18) 0.0589(6) Uani 1 1 d . . . . .
H17 H 0.198092 -0.539940 0.727728 0.071 Uiso 1 1 calc R U . . .
C18 C 0.1322(3) -0.2805(3) 0.72687(16) 0.0501(5) Uani 1 1 d . . . . .
H18 H 0.005769 -0.250580 0.708872 0.060 Uiso 1 1 calc R U . . .
C19 C 0.0877(3) 0.0433(2) 0.73343(15) 0.0437(4) Uani 1 1 d . . . . .
 
 
_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 C8 1.8371(19) . ?
P1 C14 1.8376(18) . ?
P1 C2 1.8388(19) . ?
O1 C19 1.378(2) . ?
O1 H1 0.79(3) . ?
C1 C6 1.383(3) . ?
C1 C2 1.398(3) . ?
C1 C19 1.538(3) . ?
C2 C3 1.385(3) . ?
C3 C4 1.386(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C12 1.389(3) . ?
C7 C8 1.394(3) . ?
C7 C19 1.537(3) . ?
C8 C9 1.386(3) . ?
C9 C10 1.385(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.372(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.384(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.387(3) . ?
C13 C14 1.398(3) . ?
C13 C19 1.536(3) . ?
C14 C15 1.382(3) . ?
C15 C16 1.387(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.369(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.384(3) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
 
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
C8 P1 C14 94.43(8) . . ?
C8 P1 C2 94.20(8) . . ?
C14 P1 C2 94.90(8) . . ?
C19 O1 H1 109(2) . . ?
C6 C1 C2 119.94(17) . . ?
C6 C1 C19 123.70(17) . . ?
C2 C1 C19 116.35(16) . . ?
C3 C2 C1 120.08(17) . . ?
C3 C2 P1 122.84(14) . . ?
C1 C2 P1 117.05(13) . . ?
C2 C3 C4 119.76(18) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.03(18) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.83(19) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 119.35(18) . . ?
C1 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C12 C7 C8 119.17(19) . . ?
C12 C7 C19 123.75(18) . . ?
C8 C7 C19 117.07(16) . . ?
C9 C8 C7 120.24(18) . . ?
C9 C8 P1 123.17(15) . . ?
C7 C8 P1 116.58(14) . . ?
C10 C9 C8 119.9(2) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C11 C10 C9 120.0(2) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.6(2) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 120.1(2) . . ?
C11 C12 H12 120.0 . . ?
C7 C12 H12 120.0 . . ?
C18 C13 C14 119.57(17) . . ?
C18 C13 C19 123.48(17) . . ?
C14 C13 C19 116.94(16) . . ?
C15 C14 C13 119.94(17) . . ?
C15 C14 P1 123.51(15) . . ?
C13 C14 P1 116.49(13) . . ?
C14 C15 C16 119.8(2) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 120.3(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.61(19) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C17 C18 C13 119.8(2) . . ?
C17 C18 H18 120.1 . . ?
C13 C18 H18 120.1 . . ?
O1 C19 C13 113.42(15) . . ?
O1 C19 C7 112.86(16) . . ?
C13 C19 C7 108.05(15) . . ?
O1 C19 C1 108.22(16) . . ?
C13 C19 C1 106.96(15) . . ?
C7 C19 C1 106.98(14) . . ?
 
_refine_diff_density_max    0.313
_refine_diff_density_min   -0.215
_refine_diff_density_rms    0.038



# start Validation Reply Form
_vrf_PLAT911_nt0246_LeiHu_LH59
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=  0.598         31 Report  
RESPONSE: These reflections are missing in the highest and lowest resolution 
shells because of the instrument geometry limitation. 
;
# end Validation Reply Form

 
data_nt0261_LeiHu_LH70
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_systematic         '9-thionobenzoate-10-phosphatriptycene'
_chemical_name_common             '9-thionobenzoate-10-phosphatriptycene'
_chemical_melting_point           ?
_chemical_formula_moiety          'C26 H17 O2 P S' 
_chemical_formula_sum             'C26 H17 O2 P S' 
_chemical_formula_weight          424.42

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'
 'O'  'O'   0.0492   0.0322
 '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'
 'S'  'S'   0.3331   0.5567
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    25.0052(2)
_cell_length_b                    8.40856(8)
_cell_length_c                    20.01476(18)
_cell_angle_alpha                 90
_cell_angle_beta                  94.2309(8)
_cell_angle_gamma                 90
_cell_volume                      4196.79(7)
_cell_formula_units_Z             8
_cell_measurement_temperature     295(2)
_cell_measurement_reflns_used     14682
_cell_measurement_theta_min       3.5380
_cell_measurement_theta_max       67.0740
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.343          
_exptl_crystal_F_000              1760
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.490
_exptl_crystal_size_mid           0.190
_exptl_crystal_size_min           0.120
_exptl_absorpt_coefficient_mu     2.251
_shelx_estimated_absorpt_T_min    0.405
_shelx_estimated_absorpt_T_max    0.774
_exptl_absorpt_correction_T_min   0.541
_exptl_absorpt_correction_T_max   0.800
_exptl_absorpt_correction_type    analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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.
;
_exptl_absorpt_special_details    ?
_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             22983
_diffrn_reflns_av_unetI/netI      0.0173
_diffrn_reflns_av_R_equivalents   0.0188
_diffrn_reflns_limit_h_min        -29
_diffrn_reflns_limit_h_max        29
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          3.545
_diffrn_reflns_theta_max          67.136
_diffrn_reflns_theta_full         67.136
_diffrn_measured_fraction_theta_max   0.987
_diffrn_measured_fraction_theta_full  0.987
_diffrn_reflns_Laue_measured_fraction_max    0.987
_diffrn_reflns_Laue_measured_fraction_full   0.987
_diffrn_reflns_point_group_measured_fraction_max   0.987
_diffrn_reflns_point_group_measured_fraction_full  0.987
_reflns_number_total              7384
_reflns_number_gt                 7032
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction         'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution     'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2018/1 (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)+(0.0381P)²+1.7781P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    dual
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          7384
_refine_ls_number_parameters      541
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0382
_refine_ls_R_factor_gt            0.0366
_refine_ls_wR_factor_ref          0.0948
_refine_ls_wR_factor_gt           0.0937
_refine_ls_goodness_of_fit_ref    1.104
_refine_ls_restrained_S_all       1.104
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
S1B S 0.48595(2) 0.43750(8) 0.28506(3) 0.06911(18) Uani 1 1 d . . . . .
P1B P 0.73951(2) 0.56965(6) 0.19180(2) 0.04056(12) Uani 1 1 d . . . . .
O1B O 0.57007(4) 0.51435(15) 0.22567(6) 0.0402(3) Uani 1 1 d . . . . .
O2B O 0.58830(4) 0.38905(15) 0.32185(6) 0.0427(3) Uani 1 1 d . . . . .
C1B C 0.65420(6) 0.3673(2) 0.20926(8) 0.0360(3) Uani 1 1 d . . . . .
C2B C 0.70908(7) 0.3725(2) 0.19894(8) 0.0383(4) Uani 1 1 d . . . . .
C3B C 0.73712(8) 0.2333(2) 0.19034(9) 0.0455(4) Uani 1 1 d . . . . .
H3B H 0.773658 0.237084 0.184528 0.055 Uiso 1 1 calc R U . . .
C4B C 0.71096(9) 0.0883(2) 0.19035(11) 0.0561(5) Uani 1 1 d . . . . .
H4B H 0.729963 -0.005612 0.185515 0.067 Uiso 1 1 calc R U . . .
C5B C 0.65643(9) 0.0837(2) 0.19758(11) 0.0560(5) Uani 1 1 d . . . . .
H5B H 0.638637 -0.013513 0.196326 0.067 Uiso 1 1 calc R U . . .
C6B C 0.62798(8) 0.2227(2) 0.20669(9) 0.0449(4) Uani 1 1 d . . . . .
H6B H 0.591239 0.218440 0.211070 0.054 Uiso 1 1 calc R U . . .
C7B C 0.63170(6) 0.62039(19) 0.15195(8) 0.0352(3) Uani 1 1 d . . . . .
C8B C 0.68427(7) 0.6470(2) 0.13461(8) 0.0388(4) Uani 1 1 d . . . . .
C9B C 0.69279(8) 0.7333(2) 0.07753(9) 0.0483(4) Uani 1 1 d . . . . .
H9B H 0.727524 0.750828 0.065505 0.058 Uiso 1 1 calc R U . . .
C10B C 0.64949(9) 0.7935(3) 0.03826(10) 0.0539(5) Uani 1 1 d . . . . .
H10B H 0.655191 0.852753 0.000204 0.065 Uiso 1 1 calc R U . . .
C11B C 0.59815(8) 0.7656(2) 0.05549(9) 0.0495(4) Uani 1 1 d . . . . .
H11B H 0.569300 0.805565 0.028634 0.059 Uiso 1 1 calc R U . . .
C12B C 0.58870(7) 0.6787(2) 0.11247(8) 0.0405(4) Uani 1 1 d . . . . .
H12B H 0.553833 0.660243 0.123788 0.049 Uiso 1 1 calc R U . . .
C13B C 0.65645(7) 0.63160(19) 0.27215(8) 0.0361(3) Uani 1 1 d . . . . .
C14B C 0.71134(7) 0.6511(2) 0.26658(8) 0.0386(4) Uani 1 1 d . . . . .
C15B C 0.74171(8) 0.7407(2) 0.31395(10) 0.0498(4) Uani 1 1 d . . . . .
H15B H 0.778574 0.749639 0.311364 0.060 Uiso 1 1 calc R U . . .
C16B C 0.71723(10) 0.8163(3) 0.36475(11) 0.0598(5) Uani 1 1 d . . . . .
H16B H 0.737605 0.873866 0.397107 0.072 Uiso 1 1 calc R U . . .
C17B C 0.66248(10) 0.8059(2) 0.36723(10) 0.0568(5) Uani 1 1 d . . . . .
H17B H 0.645821 0.861188 0.400176 0.068 Uiso 1 1 calc R U . . .
C18B C 0.63163(8) 0.7137(2) 0.32110(9) 0.0445(4) Uani 1 1 d . . . . .
H18B H 0.594663 0.707544 0.323226 0.053 Uiso 1 1 calc R U . . .
C19B C 0.62722(6) 0.5289(2) 0.21747(8) 0.0342(3) Uani 1 1 d . . . . .
C20B C 0.55014(7) 0.4459(2) 0.27853(9) 0.0401(4) Uani 1 1 d . . . . .
C21B C 0.57407(7) 0.3138(2) 0.38121(9) 0.0412(4) Uani 1 1 d . . . . .
C22B C 0.56711(8) 0.1532(2) 0.38150(11) 0.0523(5) Uani 1 1 d . . . . .
H22B H 0.568028 0.093881 0.342387 0.063 Uiso 1 1 calc R U . . .
C23B C 0.55861(9) 0.0812(3) 0.44213(13) 0.0639(6) Uani 1 1 d . . . . .
H23B H 0.553516 -0.028254 0.443709 0.077 Uiso 1 1 calc R U . . .
C24B C 0.55761(10) 0.1685(3) 0.49961(12) 0.0708(7) Uani 1 1 d . . . . .
H24B H 0.552350 0.118450 0.540038 0.085 Uiso 1 1 calc R U . . .
C25B C 0.56434(13) 0.3289(3) 0.49749(12) 0.0822(8) Uani 1 1 d . . . . .
H25B H 0.563468 0.388581 0.536511 0.099 Uiso 1 1 calc R U . . .
C26B C 0.57244(11) 0.4031(3) 0.43771(11) 0.0672(6) Uani 1 1 d . . . . .
H26B H 0.576731 0.512895 0.436000 0.081 Uiso 1 1 calc R U . . .
S1A S 0.88525(2) 0.43354(6) 0.23393(2) 0.05101(13) Uani 1 1 d . . . . .
P1A P 0.83792(2) 0.44274(6) 0.56532(2) 0.04539(13) Uani 1 1 d . . . . .
O1A O 0.87515(5) 0.50721(14) 0.35735(6) 0.0406(3) Uani 1 1 d . . . . .
O2A O 0.88323(5) 0.24804(14) 0.34066(6) 0.0444(3) Uani 1 1 d . . . . .
C1A C 0.90930(7) 0.3922(2) 0.46777(9) 0.0400(4) Uani 1 1 d . . . . .
C2A C 0.90009(7) 0.3640(2) 0.53491(9) 0.0439(4) Uani 1 1 d . . . . .
C3A C 0.93902(9) 0.2882(3) 0.57674(11) 0.0575(5) Uani 1 1 d . . . . .
H3A H 0.932821 0.268303 0.621218 0.069 Uiso 1 1 calc R U . . .
C4A C 0.98686(9) 0.2426(3) 0.55225(13) 0.0670(6) Uani 1 1 d . . . . .
H4A H 1.012266 0.187982 0.579689 0.080 Uiso 1 1 calc R U . . .
C5A C 0.99696(8) 0.2779(3) 0.48745(13) 0.0625(6) Uani 1 1 d . . . . .
H5A H 1.029835 0.250647 0.471771 0.075 Uiso 1 1 calc R U . . .
C6A C 0.95867(7) 0.3537(2) 0.44509(10) 0.0482(4) Uani 1 1 d . . . . .
H6A H 0.966136 0.378688 0.401478 0.058 Uiso 1 1 calc R U . . .
C7A C 0.85843(6) 0.6419(2) 0.45871(8) 0.0378(4) Uani 1 1 d . . . . .
C8A C 0.84623(7) 0.6393(2) 0.52590(9) 0.0414(4) Uani 1 1 d . . . . .
C9A C 0.84200(8) 0.7812(2) 0.55996(10) 0.0495(4) Uani 1 1 d . . . . .
H9A H 0.833960 0.780456 0.604589 0.059 Uiso 1 1 calc R U . . .
C10A C 0.84967(9) 0.9245(2) 0.52794(11) 0.0565(5) Uani 1 1 d . . . . .
H10A H 0.846693 1.019647 0.551059 0.068 Uiso 1 1 calc R U . . .
C11A C 0.86171(9) 0.9262(2) 0.46185(11) 0.0538(5) Uani 1 1 d . . . . .
H11A H 0.866812 1.022699 0.440487 0.065 Uiso 1 1 calc R U . . .
C12A C 0.86627(7) 0.7845(2) 0.42694(9) 0.0433(4) Uani 1 1 d . . . . .
H12A H 0.874561 0.785900 0.382409 0.052 Uiso 1 1 calc R U . . .
C13A C 0.80980(7) 0.3916(2) 0.43048(9) 0.0388(4) Uani 1 1 d . . . . .
C14A C 0.79416(7) 0.3649(2) 0.49519(9) 0.0431(4) Uani 1 1 d . . . . .
C15A C 0.74583(8) 0.2893(3) 0.50421(10) 0.0543(5) Uani 1 1 d . . . . .
H15A H 0.735647 0.270097 0.547233 0.065 Uiso 1 1 calc R U . . .
C16A C 0.71283(8) 0.2427(3) 0.44919(11) 0.0606(5) Uani 1 1 d . . . . .
H16A H 0.680804 0.190205 0.455232 0.073 Uiso 1 1 calc R U . . .
C17A C 0.72739(8) 0.2739(3) 0.38547(11) 0.0557(5) Uani 1 1 d . . . . .
H17A H 0.704765 0.244229 0.348609 0.067 Uiso 1 1 calc R U . . .
C18A C 0.77557(7) 0.3491(2) 0.37590(9) 0.0449(4) Uani 1 1 d . . . . .
H18A H 0.784897 0.371148 0.332733 0.054 Uiso 1 1 calc R U . . .
C19A C 0.86370(7) 0.4772(2) 0.42653(8) 0.0370(4) Uani 1 1 d . . . . .
C20A C 0.88147(7) 0.3924(2) 0.31287(9) 0.0385(4) Uani 1 1 d . . . . .
C21A C 0.89616(7) 0.1167(2) 0.30093(9) 0.0423(4) Uani 1 1 d . . . . .
C22A C 0.94889(9) 0.0819(3) 0.29479(15) 0.0709(7) Uani 1 1 d . . . . .
H22A H 0.975860 0.146393 0.314494 0.085 Uiso 1 1 calc R U . . .
C23A C 0.96116(10) -0.0509(3) 0.25870(17) 0.0877(9) Uani 1 1 d . . . . .
H23A H 0.996820 -0.075606 0.253167 0.105 Uiso 1 1 calc R U . . .
C24A C 0.92135(10) -0.1468(3) 0.23096(14) 0.0705(7) Uani 1 1 d . . . . .
H24A H 0.929972 -0.236510 0.206769 0.085 Uiso 1 1 calc R U . . .
C25A C 0.86890(9) -0.1109(3) 0.23876(10) 0.0564(5) Uani 1 1 d . . . . .
H25A H 0.841904 -0.176747 0.220021 0.068 Uiso 1 1 calc R U . . .
C26A C 0.85572(8) 0.0222(2) 0.27423(9) 0.0458(4) Uani 1 1 d . . . . .
H26A H 0.820083 0.047052 0.279824 0.055 Uiso 1 1 calc R U . . .
 
 
_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
S1B C20B 1.6215(17) . ?
P1B C14B 1.8331(18) . ?
P1B C2B 1.8341(18) . ?
P1B C8B 1.8462(17) . ?
O1B C20B 1.333(2) . ?
O1B C19B 1.4556(18) . ?
O2B C20B 1.330(2) . ?
O2B C21B 1.415(2) . ?
C1B C6B 1.381(2) . ?
C1B C2B 1.404(2) . ?
C1B C19B 1.532(2) . ?
C2B C3B 1.382(3) . ?
C3B C4B 1.384(3) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.382(3) . ?
C4B H4B 0.9300 . ?
C5B C6B 1.387(3) . ?
C5B H5B 0.9300 . ?
C6B H6B 0.9300 . ?
C7B C12B 1.377(2) . ?
C7B C8B 1.402(2) . ?
C7B C19B 1.531(2) . ?
C8B C9B 1.383(2) . ?
C9B C10B 1.386(3) . ?
C9B H9B 0.9300 . ?
C10B C11B 1.374(3) . ?
C10B H10B 0.9300 . ?
C11B C12B 1.389(3) . ?
C11B H11B 0.9300 . ?
C12B H12B 0.9300 . ?
C13B C18B 1.383(2) . ?
C13B C14B 1.395(2) . ?
C13B C19B 1.536(2) . ?
C14B C15B 1.392(3) . ?
C15B C16B 1.380(3) . ?
C15B H15B 0.9300 . ?
C16B C17B 1.376(3) . ?
C16B H16B 0.9300 . ?
C17B C18B 1.394(3) . ?
C17B H17B 0.9300 . ?
C18B H18B 0.9300 . ?
C21B C26B 1.361(3) . ?
C21B C22B 1.362(3) . ?
C22B C23B 1.387(3) . ?
C22B H22B 0.9300 . ?
C23B C24B 1.367(4) . ?
C23B H23B 0.9300 . ?
C24B C25B 1.360(4) . ?
C24B H24B 0.9300 . ?
C25B C26B 1.378(3) . ?
C25B H25B 0.9300 . ?
C26B H26B 0.9300 . ?
S1A C20A 1.6269(17) . ?
P1A C2A 1.834(2) . ?
P1A C14A 1.8354(18) . ?
P1A C8A 1.8501(19) . ?
O1A C20A 1.331(2) . ?
O1A C19A 1.4565(19) . ?
O2A C20A 1.334(2) . ?
O2A C21A 1.413(2) . ?
C1A C6A 1.385(3) . ?
C1A C2A 1.400(3) . ?
C1A C19A 1.534(2) . ?
C2A C3A 1.391(3) . ?
C3A C4A 1.380(3) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.372(3) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.386(3) . ?
C5A H5A 0.9300 . ?
C6A H6A 0.9300 . ?
C7A C12A 1.378(2) . ?
C7A C8A 1.401(2) . ?
C7A C19A 1.537(2) . ?
C8A C9A 1.382(3) . ?
C9A C10A 1.384(3) . ?
C9A H9A 0.9300 . ?
C10A C11A 1.378(3) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.391(3) . ?
C11A H11A 0.9300 . ?
C12A H12A 0.9300 . ?
C13A C18A 1.384(2) . ?
C13A C14A 1.398(2) . ?
C13A C19A 1.535(2) . ?
C14A C15A 1.389(3) . ?
C15A C16A 1.383(3) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.377(3) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.387(3) . ?
C17A H17A 0.9300 . ?
C18A H18A 0.9300 . ?
C21A C26A 1.363(3) . ?
C21A C22A 1.365(3) . ?
C22A C23A 1.377(3) . ?
C22A H22A 0.9300 . ?
C23A C24A 1.367(4) . ?
C23A H23A 0.9300 . ?
C24A C25A 1.366(3) . ?
C24A H24A 0.9300 . ?
C25A C26A 1.379(3) . ?
C25A H25A 0.9300 . ?
C26A H26A 0.9300 . ?
 
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
C14B P1B C2B 95.02(8) . . ?
C14B P1B C8B 93.42(8) . . ?
C2B P1B C8B 94.08(8) . . ?
C20B O1B C19B 123.61(13) . . ?
C20B O2B C21B 119.71(13) . . ?
C6B C1B C2B 119.25(16) . . ?
C6B C1B C19B 125.03(15) . . ?
C2B C1B C19B 115.55(14) . . ?
C3B C2B C1B 120.18(16) . . ?
C3B C2B P1B 122.60(13) . . ?
C1B C2B P1B 117.09(13) . . ?
C2B C3B C4B 120.15(17) . . ?
C2B C3B H3B 119.9 . . ?
C4B C3B H3B 119.9 . . ?
C5B C4B C3B 119.63(18) . . ?
C5B C4B H4B 120.2 . . ?
C3B C4B H4B 120.2 . . ?
C4B C5B C6B 120.64(18) . . ?
C4B C5B H5B 119.7 . . ?
C6B C5B H5B 119.7 . . ?
C1B C6B C5B 120.02(17) . . ?
C1B C6B H6B 120.0 . . ?
C5B C6B H6B 120.0 . . ?
C12B C7B C8B 120.51(15) . . ?
C12B C7B C19B 124.55(15) . . ?
C8B C7B C19B 114.92(14) . . ?
C9B C8B C7B 119.52(16) . . ?
C9B C8B P1B 122.90(13) . . ?
C7B C8B P1B 117.55(12) . . ?
C8B C9B C10B 119.90(17) . . ?
C8B C9B H9B 120.0 . . ?
C10B C9B H9B 120.0 . . ?
C11B C10B C9B 120.05(17) . . ?
C11B C10B H10B 120.0 . . ?
C9B C10B H10B 120.0 . . ?
C10B C11B C12B 120.96(17) . . ?
C10B C11B H11B 119.5 . . ?
C12B C11B H11B 119.5 . . ?
C7B C12B C11B 119.06(17) . . ?
C7B C12B H12B 120.5 . . ?
C11B C12B H12B 120.5 . . ?
C18B C13B C14B 119.58(16) . . ?
C18B C13B C19B 124.81(15) . . ?
C14B C13B C19B 115.36(14) . . ?
C15B C14B C13B 119.98(17) . . ?
C15B C14B P1B 122.36(14) . . ?
C13B C14B P1B 117.45(12) . . ?
C16B C15B C14B 120.12(19) . . ?
C16B C15B H15B 119.9 . . ?
C14B C15B H15B 119.9 . . ?
C17B C16B C15B 119.60(19) . . ?
C17B C16B H16B 120.2 . . ?
C15B C16B H16B 120.2 . . ?
C16B C17B C18B 120.97(19) . . ?
C16B C17B H17B 119.5 . . ?
C18B C17B H17B 119.5 . . ?
C13B C18B C17B 119.46(18) . . ?
C13B C18B H18B 120.3 . . ?
C17B C18B H18B 120.3 . . ?
O1B C19B C7B 105.86(12) . . ?
O1B C19B C1B 112.40(13) . . ?
C7B C19B C1B 107.05(13) . . ?
O1B C19B C13B 112.74(13) . . ?
C7B C19B C13B 105.49(13) . . ?
C1B C19B C13B 112.64(13) . . ?
O2B C20B O1B 112.36(14) . . ?
O2B C20B S1B 126.77(13) . . ?
O1B C20B S1B 120.86(13) . . ?
C26B C21B C22B 122.16(18) . . ?
C26B C21B O2B 118.42(17) . . ?
C22B C21B O2B 119.17(17) . . ?
C21B C22B C23B 117.7(2) . . ?
C21B C22B H22B 121.2 . . ?
C23B C22B H22B 121.2 . . ?
C24B C23B C22B 121.0(2) . . ?
C24B C23B H23B 119.5 . . ?
C22B C23B H23B 119.5 . . ?
C25B C24B C23B 119.8(2) . . ?
C25B C24B H24B 120.1 . . ?
C23B C24B H24B 120.1 . . ?
C24B C25B C26B 120.2(2) . . ?
C24B C25B H25B 119.9 . . ?
C26B C25B H25B 119.9 . . ?
C21B C26B C25B 119.1(2) . . ?
C21B C26B H26B 120.4 . . ?
C25B C26B H26B 120.4 . . ?
C2A P1A C14A 95.14(8) . . ?
C2A P1A C8A 93.22(8) . . ?
C14A P1A C8A 94.12(8) . . ?
C20A O1A C19A 123.49(13) . . ?
C20A O2A C21A 118.59(13) . . ?
C6A C1A C2A 119.27(17) . . ?
C6A C1A C19A 125.29(16) . . ?
C2A C1A C19A 115.26(15) . . ?
C3A C2A C1A 119.85(18) . . ?
C3A C2A P1A 122.57(16) . . ?
C1A C2A P1A 117.44(13) . . ?
C4A C3A C2A 120.0(2) . . ?
C4A C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C5A C4A C3A 120.0(2) . . ?
C5A C4A H4A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C4A C5A C6A 120.7(2) . . ?
C4A C5A H5A 119.6 . . ?
C6A C5A H5A 119.6 . . ?
C1A C6A C5A 119.9(2) . . ?
C1A C6A H6A 120.0 . . ?
C5A C6A H6A 120.0 . . ?
C12A C7A C8A 120.30(16) . . ?
C12A C7A C19A 124.82(15) . . ?
C8A C7A C19A 114.85(15) . . ?
C9A C8A C7A 119.38(17) . . ?
C9A C8A P1A 123.09(14) . . ?
C7A C8A P1A 117.53(13) . . ?
C8A C9A C10A 120.30(17) . . ?
C8A C9A H9A 119.8 . . ?
C10A C9A H9A 119.8 . . ?
C11A C10A C9A 120.07(18) . . ?
C11A C10A H10A 120.0 . . ?
C9A C10A H10A 120.0 . . ?
C10A C11A C12A 120.32(18) . . ?
C10A C11A H11A 119.8 . . ?
C12A C11A H11A 119.8 . . ?
C7A C12A C11A 119.63(17) . . ?
C7A C12A H12A 120.2 . . ?
C11A C12A H12A 120.2 . . ?
C18A C13A C14A 119.41(16) . . ?
C18A C13A C19A 125.06(16) . . ?
C14A C13A C19A 115.42(15) . . ?
C15A C14A C13A 119.93(17) . . ?
C15A C14A P1A 122.62(14) . . ?
C13A C14A P1A 117.37(13) . . ?
C16A C15A C14A 120.00(19) . . ?
C16A C15A H15A 120.0 . . ?
C14A C15A H15A 120.0 . . ?
C17A C16A C15A 120.02(19) . . ?
C17A C16A H16A 120.0 . . ?
C15A C16A H16A 120.0 . . ?
C16A C17A C18A 120.44(18) . . ?
C16A C17A H17A 119.8 . . ?
C18A C17A H17A 119.8 . . ?
C13A C18A C17A 120.11(17) . . ?
C13A C18A H18A 119.9 . . ?
C17A C18A H18A 119.9 . . ?
O1A C19A C1A 113.69(13) . . ?
O1A C19A C13A 111.40(13) . . ?
C1A C19A C13A 111.97(14) . . ?
O1A C19A C7A 105.75(13) . . ?
C1A C19A C7A 106.12(13) . . ?
C13A C19A C7A 107.36(13) . . ?
O1A C20A O2A 112.52(14) . . ?
O1A C20A S1A 120.90(13) . . ?
O2A C20A S1A 126.57(13) . . ?
C26A C21A C22A 122.25(18) . . ?
C26A C21A O2A 118.82(16) . . ?
C22A C21A O2A 118.74(17) . . ?
C21A C22A C23A 118.4(2) . . ?
C21A C22A H22A 120.8 . . ?
C23A C22A H22A 120.8 . . ?
C24A C23A C22A 120.5(2) . . ?
C24A C23A H23A 119.7 . . ?
C22A C23A H23A 119.7 . . ?
C25A C24A C23A 120.0(2) . . ?
C25A C24A H24A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
C24A C25A C26A 120.4(2) . . ?
C24A C25A H25A 119.8 . . ?
C26A C25A H25A 119.8 . . ?
C21A C26A C25A 118.44(18) . . ?
C21A C26A H26A 120.8 . . ?
C25A C26A H26A 120.8 . . ?
 
_refine_diff_density_max    0.333
_refine_diff_density_min   -0.419
_refine_diff_density_rms    0.034




# start Validation Reply Form
_vrf_PLAT241_nt0261_LeiHu_LH70
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C23A Check 
RESPONSE: This arom is part of the wobbling benzene group.
;
_vrf_PLAT331_nt0261_LeiHu_LH70
;
PROBLEM: Small Average Phenyl C-C Dist C21A     -C26A           1.37 Ang.  
RESPONSE: The average ring distance is smaller due to large thermal motion
of the wobbling benzene group.
;
_vrf_PLAT911_nt0261_LeiHu_LH70
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.598         95 Report
RESPONSE: 12 reflections were missing because of overflow, the rest was missing 
because of instrument geometry limitations.
;
_vrf_PLAT913_nt0261_LeiHu_LH70
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....         12 Note  
RESPONSE: These reflections were missing because of overflow.
;
# end Validation Reply Form

 
data_nt0523_Lei_P-trip
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         '10H-5,10-[1,2]benzenoacridophosphine'
_chemical_name_common             '9-phosphatriptycene'
_chemical_melting_point           ?
_chemical_formula_moiety          'C19 H13 P'
_chemical_formula_sum             'C19 H13 P' 
_chemical_formula_weight          272.26

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'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            9
_space_group_name_H-M_alt         'C c'
_space_group_name_Hall            'C -2yc'
 
_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'
 'x, -y, z+1/2'
 'x+1/2, y+1/2, z'
 'x+1/2, -y+1/2, z+1/2'
 
_cell_length_a                    15.0310(5)
_cell_length_b                    8.2009(2)
_cell_length_c                    13.1609(4)
_cell_angle_alpha                 90
_cell_angle_beta                  120.422(4)
_cell_angle_gamma                 90
_cell_volume                      1398.95(9)
_cell_formula_units_Z             4
_cell_measurement_temperature     295(2)
_cell_measurement_reflns_used     9083
_cell_measurement_theta_min       2.9500
_cell_measurement_theta_max       32.5290
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.293          
_exptl_crystal_F_000              568
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.790
_exptl_crystal_size_mid           0.600
_exptl_crystal_size_min           0.100
_exptl_absorpt_coefficient_mu     0.182
_shelx_estimated_absorpt_T_min    0.870
_shelx_estimated_absorpt_T_max    0.982
_exptl_absorpt_correction_T_min   0.327
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_correction_type    gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.16b (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature       295(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_monochromator   'graphite'                       
_diffrn_measurement_device_type   
;
Oxford Diffraction Xcalibur, Ruby, Gemini Ultra
; 
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  10.3712
_diffrn_reflns_number             19008
_diffrn_reflns_av_unetI/netI      0.0177
_diffrn_reflns_av_R_equivalents   0.0247
_diffrn_reflns_limit_h_min        -22
_diffrn_reflns_limit_h_max        22
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          2.939
_diffrn_reflns_theta_max          32.724
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.964
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.964
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.933
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              4808
_reflns_number_gt                 4319
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.933
_reflns_Friedel_fraction_max      0.901
_reflns_Friedel_fraction_full     0.999
 
_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 (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)+(0.0449P)²+0.0442P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Flack x determined using 1900 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.08(2)
_chemical_absolute_configuration  .
_refine_ls_number_reflns          4808
_refine_ls_number_parameters      362
_refine_ls_number_restraints      818
_refine_ls_R_factor_all           0.0335
_refine_ls_R_factor_gt            0.0283
_refine_ls_wR_factor_ref          0.0768
_refine_ls_wR_factor_gt           0.0731
_refine_ls_goodness_of_fit_ref    1.015
_refine_ls_restrained_S_all       0.969
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
P1A P 0.54007(5) 0.24183(5) 0.39543(6) 0.03882(17) Uani 0.796(3) 1 d D U P A 1
C19A C 0.47188(19) 0.2356(3) 0.5647(2) 0.0432(5) Uani 0.796(3) 1 d D U P A 1
H19A H 0.449043 0.233957 0.622478 0.052 Uiso 0.796(3) 1 calc R U P A 1
C1A C 0.5166(5) 0.4296(5) 0.4548(5) 0.0392(7) Uani 0.796(3) 1 d D U P A 1
C2A C 0.5302(8) 0.5856(5) 0.4235(8) 0.0517(10) Uani 0.796(3) 1 d D U P A 1
H2A H 0.552325 0.599531 0.369609 0.062 Uiso 0.796(3) 1 calc R U P A 1
C3A C 0.5104(6) 0.7213(6) 0.4731(6) 0.0640(14) Uani 0.796(3) 1 d D U P A 1
H3A H 0.518643 0.825698 0.451470 0.077 Uiso 0.796(3) 1 calc R U P A 1
C4A C 0.4791(5) 0.7016(6) 0.5534(5) 0.0630(11) Uani 0.796(3) 1 d D U P A 1
H4A H 0.466880 0.792707 0.586640 0.076 Uiso 0.796(3) 1 calc R U P A 1
C5A C 0.4655(5) 0.5472(5) 0.5856(5) 0.0523(8) Uani 0.796(3) 1 d D U P A 1
H5A H 0.444413 0.535051 0.640470 0.063 Uiso 0.796(3) 1 calc R U P A 1
C6A C 0.4833(4) 0.4091(5) 0.5360(5) 0.0427(9) Uani 0.796(3) 1 d D U P A 1
C7A C 0.4169(3) 0.1446(6) 0.3632(4) 0.0375(6) Uani 0.796(3) 1 d D U P A 1
C8A C 0.3523(4) 0.0648(9) 0.2593(5) 0.0499(11) Uani 0.796(3) 1 d D U P A 1
H8A H 0.367874 0.061670 0.199416 0.060 Uiso 0.796(3) 1 calc R U P A 1
C9A C 0.2638(5) -0.0110(11) 0.2441(6) 0.0612(15) Uani 0.796(3) 1 d D U P A 1
H9A H 0.219581 -0.063539 0.173546 0.073 Uiso 0.796(3) 1 calc R U P A 1
C10A C 0.2414(6) -0.0086(11) 0.3330(5) 0.0622(13) Uani 0.796(3) 1 d D U P A 1
H10A H 0.182987 -0.062408 0.322994 0.075 Uiso 0.796(3) 1 calc R U P A 1
C11A C 0.3045(4) 0.0727(7) 0.4371(4) 0.0520(8) Uani 0.796(3) 1 d D U P A 1
H11A H 0.287073 0.077044 0.495524 0.062 Uiso 0.796(3) 1 calc R U P A 1
C12A C 0.3945(4) 0.1486(7) 0.4546(4) 0.0419(9) Uani 0.796(3) 1 d D U P A 1
C13A C 0.6156(4) 0.1420(8) 0.5407(4) 0.0388(7) Uani 0.796(3) 1 d D U P A 1
C14A C 0.7075(5) 0.0612(13) 0.5768(6) 0.0537(12) Uani 0.796(3) 1 d D U P A 1
H14A H 0.736147 0.057501 0.528615 0.064 Uiso 0.796(3) 1 calc R U P A 1
C15A C 0.7569(6) -0.0153(14) 0.6875(6) 0.0641(17) Uani 0.796(3) 1 d D U P A 1
H15A H 0.817870 -0.072501 0.711919 0.077 Uiso 0.796(3) 1 calc R U P A 1
C16A C 0.7163(6) -0.0065(15) 0.7595(7) 0.0670(17) Uani 0.796(3) 1 d D U P A 1
H16A H 0.749643 -0.057985 0.832478 0.080 Uiso 0.796(3) 1 calc R U P A 1
C17A C 0.6262(6) 0.0781(13) 0.7248(7) 0.0559(13) Uani 0.796(3) 1 d D U P A 1
H17A H 0.600998 0.087980 0.776089 0.067 Uiso 0.796(3) 1 calc R U P A 1
C18A C 0.5726(4) 0.1488(7) 0.6134(4) 0.0427(10) Uani 0.796(3) 1 d D U P A 1
P1B P 0.4581(2) 0.2411(3) 0.6006(3) 0.0473(8) Uani 0.204(3) 1 d D U P A 2
C19B C 0.5276(9) 0.2398(12) 0.4350(10) 0.059(2) Uani 0.204(3) 1 d D U P A 2
H19B H 0.551970 0.240531 0.378621 0.071 Uiso 0.204(3) 1 calc R U P A 2
C1B C 0.4827(18) 0.4311(16) 0.5440(17) 0.043(4) Uani 0.204(3) 1 d D U P A 2
C2B C 0.468(3) 0.5874(18) 0.572(2) 0.063(4) Uani 0.204(3) 1 d D U P A 2
H2B H 0.443520 0.602259 0.623397 0.075 Uiso 0.204(3) 1 calc R U P A 2
C3B C 0.488(2) 0.720(2) 0.524(2) 0.059(4) Uani 0.204(3) 1 d D U P A 2
H3B H 0.477502 0.823432 0.545362 0.071 Uiso 0.204(3) 1 calc R U P A 2
C4B C 0.523(2) 0.704(2) 0.447(2) 0.058(4) Uani 0.204(3) 1 d D U P A 2
H4B H 0.537222 0.795945 0.416266 0.070 Uiso 0.204(3) 1 calc R U P A 2
C5B C 0.536(3) 0.550(2) 0.415(3) 0.056(4) Uani 0.204(3) 1 d D U P A 2
H5B H 0.559901 0.538192 0.363069 0.067 Uiso 0.204(3) 1 calc R U P A 2
C6B C 0.514(2) 0.4114(19) 0.461(2) 0.054(4) Uani 0.204(3) 1 d D U P A 2
C7B C 0.3813(15) 0.147(3) 0.4503(15) 0.045(4) Uani 0.204(3) 1 d D U P A 2
C8B C 0.2914(18) 0.066(4) 0.4123(19) 0.068(5) Uani 0.204(3) 1 d D U P A 2
H8B H 0.263496 0.059090 0.461084 0.081 Uiso 0.204(3) 1 calc R U P A 2
C9B C 0.242(2) -0.004(5) 0.305(2) 0.058(5) Uani 0.204(3) 1 d D U P A 2
H9B H 0.178467 -0.054819 0.279911 0.069 Uiso 0.204(3) 1 calc R U P A 2
C10B C 0.282(2) -0.003(5) 0.234(2) 0.056(4) Uani 0.204(3) 1 d D U P A 2
H10B H 0.249635 -0.057570 0.161643 0.067 Uiso 0.204(3) 1 calc R U P A 2
C11B C 0.3743(18) 0.081(4) 0.2700(19) 0.050(3) Uani 0.204(3) 1 d D U P A 2
H11B H 0.399644 0.091465 0.218818 0.060 Uiso 0.204(3) 1 calc R U P A 2
C12B C 0.4285(15) 0.151(3) 0.3815(16) 0.053(4) Uani 0.204(3) 1 d D U P A 2
C13B C 0.5828(14) 0.145(2) 0.6316(15) 0.036(3) Uani 0.204(3) 1 d D U P A 2
C14B C 0.642(2) 0.055(5) 0.731(3) 0.046(3) Uani 0.204(3) 1 d D U P A 2
H14B H 0.620104 0.039795 0.785015 0.055 Uiso 0.204(3) 1 calc R U P A 2
C15B C 0.733(2) -0.013(4) 0.750(2) 0.050(4) Uani 0.204(3) 1 d D U P A 2
H15B H 0.777547 -0.062306 0.822421 0.060 Uiso 0.204(3) 1 calc R U P A 2
C16B C 0.758(2) -0.008(5) 0.663(3) 0.054(4) Uani 0.204(3) 1 d D U P A 2
H16B H 0.817926 -0.056660 0.673921 0.065 Uiso 0.204(3) 1 calc R U P A 2
C17B C 0.692(2) 0.070(6) 0.559(2) 0.058(5) Uani 0.204(3) 1 d D U P A 2
H17B H 0.706180 0.066583 0.497631 0.069 Uiso 0.204(3) 1 calc R U P A 2
C18B C 0.6037(16) 0.154(3) 0.5414(18) 0.050(4) Uani 0.204(3) 1 d D U P A 2
 
 
_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
P1A C1A 1.840(3) . ?
P1A C13A 1.848(4) . ?
P1A C7A 1.857(3) . ?
C19A C18A 1.492(5) . ?
C19A C12A 1.501(5) . ?
C19A C6A 1.504(5) . ?
C19A H19A 0.9800 . ?
C1A C2A 1.391(5) . ?
C1A C6A 1.400(5) . ?
C2A C3A 1.397(6) . ?
C2A H2A 0.9300 . ?
C3A C4A 1.366(6) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.383(5) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.398(5) . ?
C5A H5A 0.9300 . ?
C7A C8A 1.377(5) . ?
C7A C12A 1.404(5) . ?
C8A C9A 1.388(6) . ?
C8A H8A 0.9300 . ?
C9A C10A 1.371(7) . ?
C9A H9A 0.9300 . ?
C10A C11A 1.380(6) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.399(5) . ?
C11A H11A 0.9300 . ?
C13A C14A 1.382(6) . ?
C13A C18A 1.401(5) . ?
C14A C15A 1.404(7) . ?
C14A H14A 0.9300 . ?
C15A C16A 1.365(7) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.377(7) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.392(7) . ?
C17A H17A 0.9300 . ?
P1B C1B 1.843(12) . ?
P1B C7B 1.878(14) . ?
P1B C13B 1.878(13) . ?
C19B C18B 1.466(17) . ?
C19B C12B 1.478(16) . ?
C19B C6B 1.486(16) . ?
C19B H19B 0.9800 . ?
C1B C2B 1.382(18) . ?
C1B C6B 1.401(17) . ?
C2B C3B 1.357(17) . ?
C2B H2B 0.9300 . ?
C3B C4B 1.371(17) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.374(18) . ?
C4B H4B 0.9300 . ?
C5B C6B 1.403(19) . ?
C5B H5B 0.9300 . ?
C7B C8B 1.354(19) . ?
C7B C12B 1.404(17) . ?
C8B C9B 1.35(2) . ?
C8B H8B 0.9300 . ?
C9B C10B 1.360(18) . ?
C9B H9B 0.9300 . ?
C10B C11B 1.396(19) . ?
C10B H10B 0.9300 . ?
C11B C12B 1.391(18) . ?
C11B H11B 0.9300 . ?
C13B C14B 1.363(19) . ?
C13B C18B 1.374(17) . ?
C14B C15B 1.38(2) . ?
C14B H14B 0.9300 . ?
C15B C16B 1.382(19) . ?
C15B H15B 0.9300 . ?
C16B C17B 1.37(2) . ?
C16B H16B 0.9300 . ?
C17B C18B 1.41(2) . ?
C17B H17B 0.9300 . ?
 
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
C1A P1A C13A 94.6(2) . . ?
C1A P1A C7A 94.2(2) . . ?
C13A P1A C7A 93.7(2) . . ?
C18A C19A C12A 108.0(4) . . ?
C18A C19A C6A 109.8(3) . . ?
C12A C19A C6A 109.8(3) . . ?
C18A C19A H19A 109.7 . . ?
C12A C19A H19A 109.7 . . ?
C6A C19A H19A 109.7 . . ?
C2A C1A C6A 120.0(4) . . ?
C2A C1A P1A 123.7(3) . . ?
C6A C1A P1A 116.3(3) . . ?
C1A C2A C3A 119.8(5) . . ?
C1A C2A H2A 120.1 . . ?
C3A C2A H2A 120.1 . . ?
C4A C3A C2A 120.4(4) . . ?
C4A C3A H3A 119.8 . . ?
C2A C3A H3A 119.8 . . ?
C3A C4A C5A 120.5(4) . . ?
C3A C4A H4A 119.8 . . ?
C5A C4A H4A 119.8 . . ?
C4A C5A C6A 120.4(4) . . ?
C4A C5A H5A 119.8 . . ?
C6A C5A H5A 119.8 . . ?
C5A C6A C1A 119.0(4) . . ?
C5A C6A C19A 125.1(4) . . ?
C1A C6A C19A 115.8(4) . . ?
C8A C7A C12A 120.5(4) . . ?
C8A C7A P1A 123.5(3) . . ?
C12A C7A P1A 116.0(3) . . ?
C7A C8A C9A 119.9(5) . . ?
C7A C8A H8A 120.0 . . ?
C9A C8A H8A 120.0 . . ?
C10A C9A C8A 120.1(5) . . ?
C10A C9A H9A 119.9 . . ?
C8A C9A H9A 119.9 . . ?
C9A C10A C11A 120.8(5) . . ?
C9A C10A H10A 119.6 . . ?
C11A C10A H10A 119.6 . . ?
C10A C11A C12A 120.0(5) . . ?
C10A C11A H11A 120.0 . . ?
C12A C11A H11A 120.0 . . ?
C11A C12A C7A 118.7(4) . . ?
C11A C12A C19A 125.6(4) . . ?
C7A C12A C19A 115.7(4) . . ?
C14A C13A C18A 120.7(4) . . ?
C14A C13A P1A 123.5(4) . . ?
C18A C13A P1A 115.8(4) . . ?
C13A C14A C15A 118.8(5) . . ?
C13A C14A H14A 120.6 . . ?
C15A C14A H14A 120.6 . . ?
C16A C15A C14A 120.6(6) . . ?
C16A C15A H15A 119.7 . . ?
C14A C15A H15A 119.7 . . ?
C15A C16A C17A 120.5(6) . . ?
C15A C16A H16A 119.8 . . ?
C17A C16A H16A 119.8 . . ?
C16A C17A C18A 120.4(6) . . ?
C16A C17A H17A 119.8 . . ?
C18A C17A H17A 119.8 . . ?
C17A C18A C13A 118.8(5) . . ?
C17A C18A C19A 124.9(5) . . ?
C13A C18A C19A 116.4(4) . . ?
C1B P1B C7B 93.6(8) . . ?
C1B P1B C13B 93.5(8) . . ?
C7B P1B C13B 94.0(8) . . ?
C18B C19B C12B 109.1(14) . . ?
C18B C19B C6B 111.8(14) . . ?
C12B C19B C6B 110.6(14) . . ?
C18B C19B H19B 108.4 . . ?
C12B C19B H19B 108.4 . . ?
C6B C19B H19B 108.4 . . ?
C2B C1B C6B 118.4(13) . . ?
C2B C1B P1B 125.9(12) . . ?
C6B C1B P1B 115.7(12) . . ?
C3B C2B C1B 121.3(16) . . ?
C3B C2B H2B 119.3 . . ?
C1B C2B H2B 119.3 . . ?
C2B C3B C4B 121.5(17) . . ?
C2B C3B H3B 119.2 . . ?
C4B C3B H3B 119.2 . . ?
C3B C4B C5B 118.6(17) . . ?
C3B C4B H4B 120.7 . . ?
C5B C4B H4B 120.7 . . ?
C4B C5B C6B 121.1(17) . . ?
C4B C5B H5B 119.5 . . ?
C6B C5B H5B 119.5 . . ?
C1B C6B C5B 119.0(14) . . ?
C1B C6B C19B 115.3(14) . . ?
C5B C6B C19B 125.6(15) . . ?
C8B C7B C12B 120.5(14) . . ?
C8B C7B P1B 123.8(13) . . ?
C12B C7B P1B 115.4(12) . . ?
C9B C8B C7B 121.3(17) . . ?
C9B C8B H8B 119.4 . . ?
C7B C8B H8B 119.4 . . ?
C8B C9B C10B 121(2) . . ?
C8B C9B H9B 119.4 . . ?
C10B C9B H9B 119.4 . . ?
C9B C10B C11B 118.7(19) . . ?
C9B C10B H10B 120.7 . . ?
C11B C10B H10B 120.7 . . ?
C12B C11B C10B 121.0(16) . . ?
C12B C11B H11B 119.5 . . ?
C10B C11B H11B 119.5 . . ?
C11B C12B C7B 117.1(15) . . ?
C11B C12B C19B 128.0(15) . . ?
C7B C12B C19B 114.8(13) . . ?
C14B C13B C18B 122.2(15) . . ?
C14B C13B P1B 121.8(13) . . ?
C18B C13B P1B 115.5(12) . . ?
C13B C14B C15B 120.1(17) . . ?
C13B C14B H14B 120.0 . . ?
C15B C14B H14B 120.0 . . ?
C14B C15B C16B 119.5(19) . . ?
C14B C15B H15B 120.2 . . ?
C16B C15B H15B 120.2 . . ?
C17B C16B C15B 119.0(18) . . ?
C17B C16B H16B 120.5 . . ?
C15B C16B H16B 120.5 . . ?
C16B C17B C18B 122.1(18) . . ?
C16B C17B H17B 119.0 . . ?
C18B C17B H17B 119.0 . . ?
C13B C18B C17B 116.4(16) . . ?
C13B C18B C19B 116.2(14) . . ?
C17B C18B C19B 127.3(16) . . ?
 
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
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C13A P1A C1A C2A 132.9(8) . . . . ?
C7A P1A C1A C2A -133.0(7) . . . . ?
C13A P1A C1A C6A -47.1(6) . . . . ?
C7A P1A C1A C6A 47.0(6) . . . . ?
C6A C1A C2A C3A 0.0(13) . . . . ?
P1A C1A C2A C3A 180.0(6) . . . . ?
C1A C2A C3A C4A 0.8(13) . . . . ?
C2A C3A C4A C5A -0.7(11) . . . . ?
C3A C4A C5A C6A -0.2(10) . . . . ?
C4A C5A C6A C1A 1.0(10) . . . . ?
C4A C5A C6A C19A 179.5(5) . . . . ?
C2A C1A C6A C5A -0.8(11) . . . . ?
P1A C1A C6A C5A 179.1(5) . . . . ?
C2A C1A C6A C19A -179.5(6) . . . . ?
P1A C1A C6A C19A 0.4(8) . . . . ?
C18A C19A C6A C5A -119.9(6) . . . . ?
C12A C19A C6A C5A 121.5(6) . . . . ?
C18A C19A C6A C1A 58.7(6) . . . . ?
C12A C19A C6A C1A -59.9(6) . . . . ?
C1A P1A C7A C8A 135.0(6) . . . . ?
C13A P1A C7A C8A -130.1(6) . . . . ?
C1A P1A C7A C12A -48.3(5) . . . . ?
C13A P1A C7A C12A 46.6(5) . . . . ?
C12A C7A C8A C9A 0.6(11) . . . . ?
P1A C7A C8A C9A 177.1(6) . . . . ?
C7A C8A C9A C10A -0.9(13) . . . . ?
C8A C9A C10A C11A 1.9(14) . . . . ?
C9A C10A C11A C12A -2.5(13) . . . . ?
C10A C11A C12A C7A 2.1(10) . . . . ?
C10A C11A C12A C19A -177.6(7) . . . . ?
C8A C7A C12A C11A -1.2(10) . . . . ?
P1A C7A C12A C11A -178.0(5) . . . . ?
C8A C7A C12A C19A 178.6(6) . . . . ?
P1A C7A C12A C19A 1.8(7) . . . . ?
C18A C19A C12A C11A 118.2(6) . . . . ?
C6A C19A C12A C11A -122.1(6) . . . . ?
C18A C19A C12A C7A -61.6(6) . . . . ?
C6A C19A C12A C7A 58.1(6) . . . . ?
C1A P1A C13A C14A -134.6(8) . . . . ?
C7A P1A C13A C14A 130.8(8) . . . . ?
C1A P1A C13A C18A 47.0(6) . . . . ?
C7A P1A C13A C18A -47.5(6) . . . . ?
C18A C13A C14A C15A 0.5(14) . . . . ?
P1A C13A C14A C15A -177.8(8) . . . . ?
C13A C14A C15A C16A -1.7(17) . . . . ?
C14A C15A C16A C17A -0.2(18) . . . . ?
C15A C16A C17A C18A 3.2(18) . . . . ?
C16A C17A C18A C13A -4.4(15) . . . . ?
C16A C17A C18A C19A 176.8(9) . . . . ?
C14A C13A C18A C17A 2.5(13) . . . . ?
P1A C13A C18A C17A -179.1(7) . . . . ?
C14A C13A C18A C19A -178.5(7) . . . . ?
P1A C13A C18A C19A -0.1(8) . . . . ?
C12A C19A C18A C17A -120.3(8) . . . . ?
C6A C19A C18A C17A 120.0(8) . . . . ?
C12A C19A C18A C13A 60.8(6) . . . . ?
C6A C19A C18A C13A -58.9(7) . . . . ?
C7B P1B C1B C2B 131(3) . . . . ?
C13B P1B C1B C2B -135(3) . . . . ?
C7B P1B C1B C6B -46(2) . . . . ?
C13B P1B C1B C6B 49(2) . . . . ?
C6B C1B C2B C3B -3(5) . . . . ?
P1B C1B C2B C3B -180(2) . . . . ?
C1B C2B C3B C4B 1(5) . . . . ?
C2B C3B C4B C5B 1(5) . . . . ?
C3B C4B C5B C6B 0(5) . . . . ?
C2B C1B C6B C5B 5(5) . . . . ?
P1B C1B C6B C5B -179(3) . . . . ?
C2B C1B C6B C19B -180(2) . . . . ?
P1B C1B C6B C19B -3(3) . . . . ?
C4B C5B C6B C1B -3(5) . . . . ?
C4B C5B C6B C19B -178(3) . . . . ?
C18B C19B C6B C1B -58(3) . . . . ?
C12B C19B C6B C1B 64(3) . . . . ?
C18B C19B C6B C5B 117(3) . . . . ?
C12B C19B C6B C5B -121(3) . . . . ?
C1B P1B C7B C8B -136(3) . . . . ?
C13B P1B C7B C8B 130(3) . . . . ?
C1B P1B C7B C12B 50(2) . . . . ?
C13B P1B C7B C12B -43(2) . . . . ?
C12B C7B C8B C9B -4(5) . . . . ?
P1B C7B C8B C9B -177(3) . . . . ?
C7B C8B C9B C10B 3(6) . . . . ?
C8B C9B C10B C11B -4(6) . . . . ?
C9B C10B C11B C12B 6(5) . . . . ?
C10B C11B C12B C7B -7(5) . . . . ?
C10B C11B C12B C19B 178(3) . . . . ?
C8B C7B C12B C11B 6(4) . . . . ?
P1B C7B C12B C11B 180(2) . . . . ?
C8B C7B C12B C19B -178(2) . . . . ?
P1B C7B C12B C19B -5(3) . . . . ?
C18B C19B C12B C11B -119(3) . . . . ?
C6B C19B C12B C11B 117(3) . . . . ?
C18B C19B C12B C7B 65(2) . . . . ?
C6B C19B C12B C7B -58(2) . . . . ?
C1B P1B C13B C14B 140(3) . . . . ?
C7B P1B C13B C14B -127(3) . . . . ?
C1B P1B C13B C18B -48(2) . . . . ?
C7B P1B C13B C18B 45(2) . . . . ?
C18B C13B C14B C15B 9(5) . . . . ?
P1B C13B C14B C15B -180(3) . . . . ?
C13B C14B C15B C16B -8(6) . . . . ?
C14B C15B C16B C17B 2(6) . . . . ?
C15B C16B C17B C18B 4(7) . . . . ?
C14B C13B C18B C17B -2(5) . . . . ?
P1B C13B C18B C17B -174(3) . . . . ?
C14B C13B C18B C19B 173(3) . . . . ?
P1B C13B C18B C19B 2(3) . . . . ?
C16B C17B C18B C13B -4(6) . . . . ?
C16B C17B C18B C19B -180(4) . . . . ?
C12B C19B C18B C13B -64(3) . . . . ?
C6B C19B C18B C13B 59(3) . . . . ?
C12B C19B C18B C17B 112(4) . . . . ?
C6B C19B C18B C17B -126(4) . . . . ?
 
_refine_diff_density_max    0.116
_refine_diff_density_min   -0.158
_refine_diff_density_rms    0.027



# start Validation Reply Form
_vrf_PLAT089_nt0523_Lei_P-trip
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       6.87 Note  
RESPONSE: Whole molecule positional disorder.
;
# end Validation Reply Form

 
data_nt0424_LH-p-trip-CH3_100K
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         '9-methylphosphatriptcene iodide'
_chemical_name_common             '9-methylphosphatriptcene iodide'
_chemical_melting_point           ?
_chemical_formula_moiety          'C20 H16 P 1+, I 1-'
_chemical_formula_sum             'C20 H16 I P' 
_chemical_formula_weight          414.20

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'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'I'  'I'  -0.4742   1.8119
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            60
_space_group_name_H-M_alt         'P b c n'
_space_group_name_Hall            '-P 2n 2ab'
 
_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'
 '-x+1/2, -y+1/2, z+1/2'
 '-x, y, -z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, y-1/2, -z-1/2'
 'x, -y, z-1/2'
 '-x-1/2, y-1/2, z'
 
_cell_length_a                    20.6313(3)
_cell_length_b                    11.37299(17)
_cell_length_c                    15.5505(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      3648.76(10)
_cell_formula_units_Z             8
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     11198
_cell_measurement_theta_min       2.3730
_cell_measurement_theta_max       32.5580
 
_exptl_crystal_description        prism
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.508          
_exptl_crystal_F_000              1632
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.430
_exptl_crystal_size_mid           0.240
_exptl_crystal_size_min           0.190
_exptl_absorpt_coefficient_mu     1.837
_shelx_estimated_absorpt_T_min    0.505
_shelx_estimated_absorpt_T_max    0.722
_exptl_absorpt_correction_T_min   0.515
_exptl_absorpt_correction_T_max   0.742
_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       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_monochromator   'graphite'                       
_diffrn_measurement_device_type   
;
Oxford Diffraction Xcalibur, Ruby, Gemini Ultra
; 
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  10.3712
_diffrn_reflns_number             18728
_diffrn_reflns_av_unetI/netI      0.0188
_diffrn_reflns_av_R_equivalents   0.0240
_diffrn_reflns_limit_h_min        -26
_diffrn_reflns_limit_h_max        21
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          2.428
_diffrn_reflns_theta_max          27.103
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              4027
_reflns_number_gt                 3753
_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 (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)+(0.0284P)²+38.9900P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          4027
_refine_ls_number_parameters      231
_refine_ls_number_restraints      13
_refine_ls_R_factor_all           0.0766
_refine_ls_R_factor_gt            0.0732
_refine_ls_wR_factor_ref          0.1645
_refine_ls_wR_factor_gt           0.1630
_refine_ls_goodness_of_fit_ref    1.229
_refine_ls_restrained_S_all       1.228
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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 0.31770(7) 0.43902(13) 0.26546(9) 0.0188(3) Uani 1 1 d . . . . .
C1 C 0.2886(3) 0.5372(5) 0.3480(4) 0.0220(12) Uani 1 1 d . . . . .
C2 C 0.2270(3) 0.5409(6) 0.3845(4) 0.0287(13) Uani 1 1 d . . . . .
H2 H 0.194272 0.487056 0.367254 0.034 Uiso 1 1 calc R U . . .
C3 C 0.2147(3) 0.6260(6) 0.4471(4) 0.0335(15) Uani 1 1 d . . . . .
H3 H 0.173129 0.629746 0.473401 0.040 Uiso 1 1 calc R U . . .
C4 C 0.2623(3) 0.7047(6) 0.4712(4) 0.0340(15) Uani 1 1 d . . . . .
H4 H 0.253002 0.762084 0.513891 0.041 Uiso 1 1 calc R U . . .
C5 C 0.3240(3) 0.7012(6) 0.4338(4) 0.0287(13) Uani 1 1 d . . . . .
H5 H 0.356285 0.756020 0.450726 0.034 Uiso 1 1 calc R U . . .
C6 C 0.3374(3) 0.6171(5) 0.3720(4) 0.0236(12) Uani 1 1 d . . . . .
C7 C 0.4031(3) 0.6059(5) 0.3266(4) 0.0215(12) Uani 1 1 d . . . . .
H7 H 0.434181 0.666263 0.348504 0.026 Uiso 1 1 calc R U . . .
C8 C 0.3501(3) 0.5413(5) 0.1892(4) 0.0209(11) Uani 1 1 d . . . . .
C9 C 0.3373(3) 0.5468(5) 0.1011(4) 0.0225(12) Uani 1 1 d . . . . .
H9 H 0.308707 0.492381 0.074575 0.027 Uiso 1 1 calc R U . . .
C10 C 0.3676(3) 0.6341(6) 0.0534(4) 0.0276(13) Uani 1 1 d . . . . .
H10 H 0.361282 0.637098 -0.007053 0.033 Uiso 1 1 calc R U . . .
C11 C 0.4069(3) 0.7166(6) 0.0926(4) 0.0294(14) Uani 1 1 d . . . . .
H11 H 0.425734 0.777672 0.059255 0.035 Uiso 1 1 calc R U . . .
C12 C 0.4193(3) 0.7109(5) 0.1816(4) 0.0270(13) Uani 1 1 d . . . . .
H12 H 0.446352 0.767782 0.208281 0.032 Uiso 1 1 calc R U . . .
C13 C 0.3917(3) 0.6217(5) 0.2297(4) 0.0202(11) Uani 1 1 d . . . . .
C14 C 0.3910(3) 0.3876(5) 0.3137(3) 0.0199(11) Uani 1 1 d . . . . .
C15 C 0.4105(3) 0.2706(5) 0.3241(4) 0.0233(12) Uani 1 1 d . . . . .
H15 H 0.384002 0.207537 0.304942 0.028 Uiso 1 1 calc R U . . .
C16 C 0.4701(3) 0.2494(6) 0.3635(4) 0.0286(13) Uani 1 1 d . . . . .
H16 H 0.485033 0.170899 0.369797 0.034 Uiso 1 1 calc R U . . .
C17 C 0.5079(3) 0.3421(6) 0.3937(4) 0.0288(13) Uani 1 1 d . . . . .
H17 H 0.547742 0.325919 0.421949 0.035 Uiso 1 1 calc R U . . .
C18 C 0.4880(3) 0.4576(5) 0.3830(4) 0.0244(12) Uani 1 1 d . . . . .
H18 H 0.514298 0.520216 0.403466 0.029 Uiso 1 1 calc R U . . .
C19 C 0.4293(3) 0.4816(5) 0.3423(4) 0.0201(11) Uani 1 1 d . . . . .
C20 C 0.2622(3) 0.3305(5) 0.2291(4) 0.0281(13) Uani 1 1 d . . . . .
H20A H 0.283883 0.278388 0.187961 0.042 Uiso 1 1 calc R U . . .
H20B H 0.225280 0.368825 0.201037 0.042 Uiso 1 1 calc R U . . .
H20C H 0.246768 0.284313 0.278224 0.042 Uiso 1 1 calc R U . . .
I1 I 0.35323(3) 0.93358(4) 0.63211(4) 0.03828(19) Uani 0.834(2) 1 d . . P A 1
I1B I 0.4491(7) 0.9508(11) 0.2947(7) 0.117(5) Uani 0.087(2) 1 d . . P B 2
I1C I 0.4473(12) 0.967(3) 0.4690(13) 0.074(8) Uani 0.035(2) 1 d . U P C 3
I1D I 0.4583(8) 0.8895(19) 0.4563(12) 0.066(6) Uani 0.045(2) 1 d . U P D 4
 
 
_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 C20 1.776(6) . ?
P1 C14 1.786(6) . ?
P1 C8 1.791(6) . ?
P1 C1 1.804(6) . ?
C1 C2 1.393(8) . ?
C1 C6 1.406(8) . ?
C2 C3 1.396(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.400(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.533(8) . ?
C7 C19 1.533(8) . ?
C7 C13 1.535(8) . ?
C7 H7 1.0000 . ?
C8 C9 1.397(8) . ?
C8 C13 1.402(8) . ?
C9 C10 1.387(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.408(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(8) . ?
C12 H12 0.9500 . ?
C14 C15 1.399(8) . ?
C14 C19 1.403(8) . ?
C15 C16 1.394(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.393(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.393(8) . ?
C18 H18 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

 
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
C20 P1 C14 116.9(3) . . ?
C20 P1 C8 118.8(3) . . ?
C14 P1 C8 100.0(3) . . ?
C20 P1 C1 116.3(3) . . ?
C14 P1 C1 100.7(3) . . ?
C8 P1 C1 101.1(3) . . ?
C2 C1 C6 121.8(6) . . ?
C2 C1 P1 127.7(5) . . ?
C6 C1 P1 110.5(4) . . ?
C1 C2 C3 118.1(6) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 120.6(6) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 121.0(6) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 119.4(6) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 119.1(6) . . ?
C5 C6 C7 123.7(6) . . ?
C1 C6 C7 117.2(5) . . ?
C19 C7 C6 108.4(5) . . ?
C19 C7 C13 108.6(5) . . ?
C6 C7 C13 107.9(5) . . ?
C19 C7 H7 110.6 . . ?
C6 C7 H7 110.6 . . ?
C13 C7 H7 110.6 . . ?
C9 C8 C13 121.8(5) . . ?
C9 C8 P1 127.4(5) . . ?
C13 C8 P1 110.8(4) . . ?
C10 C9 C8 118.1(6) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 H9 120.9 . . ?
C11 C10 C9 120.9(6) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 120.6(6) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 119.4(6) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C8 119.1(5) . . ?
C12 C13 C7 123.6(5) . . ?
C8 C13 C7 117.3(5) . . ?
C15 C14 C19 121.7(5) . . ?
C15 C14 P1 127.2(5) . . ?
C19 C14 P1 111.1(4) . . ?
C16 C15 C14 118.0(6) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C17 C16 C15 120.8(6) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C18 C17 C16 120.7(6) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 119.8(6) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C18 C19 C14 119.0(5) . . ?
C18 C19 C7 124.1(5) . . ?
C14 C19 C7 116.9(5) . . ?
P1 C20 H20A 109.5 . . ?
P1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
P1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
 
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
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C20 P1 C1 C2 -2.6(6) . . . . ?
C14 P1 C1 C2 -129.9(5) . . . . ?
C8 P1 C1 C2 127.5(5) . . . . ?
C20 P1 C1 C6 179.0(4) . . . . ?
C14 P1 C1 C6 51.7(5) . . . . ?
C8 P1 C1 C6 -50.9(5) . . . . ?
C6 C1 C2 C3 -0.8(9) . . . . ?
P1 C1 C2 C3 -179.1(5) . . . . ?
C1 C2 C3 C4 0.7(9) . . . . ?
C2 C3 C4 C5 -0.1(10) . . . . ?
C3 C4 C5 C6 -0.3(9) . . . . ?
C4 C5 C6 C1 0.2(9) . . . . ?
C4 C5 C6 C7 179.6(5) . . . . ?
C2 C1 C6 C5 0.4(9) . . . . ?
P1 C1 C6 C5 178.9(4) . . . . ?
C2 C1 C6 C7 -179.1(5) . . . . ?
P1 C1 C6 C7 -0.5(6) . . . . ?
C5 C6 C7 C19 122.3(6) . . . . ?
C1 C6 C7 C19 -58.2(6) . . . . ?
C5 C6 C7 C13 -120.3(6) . . . . ?
C1 C6 C7 C13 59.2(7) . . . . ?
C20 P1 C8 C9 -0.5(6) . . . . ?
C14 P1 C8 C9 127.9(5) . . . . ?
C1 P1 C8 C9 -129.0(5) . . . . ?
C20 P1 C8 C13 178.6(4) . . . . ?
C14 P1 C8 C13 -53.0(4) . . . . ?
C1 P1 C8 C13 50.1(5) . . . . ?
C13 C8 C9 C10 0.7(8) . . . . ?
P1 C8 C9 C10 179.7(4) . . . . ?
C8 C9 C10 C11 -3.0(9) . . . . ?
C9 C10 C11 C12 2.7(9) . . . . ?
C10 C11 C12 C13 0.0(9) . . . . ?
C11 C12 C13 C8 -2.2(8) . . . . ?
C11 C12 C13 C7 178.7(5) . . . . ?
C9 C8 C13 C12 1.9(8) . . . . ?
P1 C8 C13 C12 -177.3(4) . . . . ?
C9 C8 C13 C7 -179.0(5) . . . . ?
P1 C8 C13 C7 1.9(6) . . . . ?
C19 C7 C13 C12 -123.9(6) . . . . ?
C6 C7 C13 C12 118.8(6) . . . . ?
C19 C7 C13 C8 56.9(6) . . . . ?
C6 C7 C13 C8 -60.3(7) . . . . ?
C20 P1 C14 C15 1.8(6) . . . . ?
C8 P1 C14 C15 -127.8(5) . . . . ?
C1 P1 C14 C15 128.7(5) . . . . ?
C20 P1 C14 C19 -177.8(4) . . . . ?
C8 P1 C14 C19 52.5(4) . . . . ?
C1 P1 C14 C19 -50.9(5) . . . . ?
C19 C14 C15 C16 -0.6(8) . . . . ?
P1 C14 C15 C16 179.8(4) . . . . ?
C14 C15 C16 C17 1.9(9) . . . . ?
C15 C16 C17 C18 -1.9(10) . . . . ?
C16 C17 C18 C19 0.5(9) . . . . ?
C17 C18 C19 C14 0.8(9) . . . . ?
C17 C18 C19 C7 -179.5(5) . . . . ?
C15 C14 C19 C18 -0.7(8) . . . . ?
P1 C14 C19 C18 178.9(4) . . . . ?
C15 C14 C19 C7 179.5(5) . . . . ?
P1 C14 C19 C7 -0.9(6) . . . . ?
C6 C7 C19 C18 -120.4(6) . . . . ?
C13 C7 C19 C18 122.7(6) . . . . ?
C6 C7 C19 C14 59.4(6) . . . . ?
C13 C7 C19 C14 -57.6(6) . . . . ?
 
_refine_diff_density_max    2.588
_refine_diff_density_min   -2.064
_refine_diff_density_rms    0.138



# start Validation Reply Form
_vrf_PLAT260_nt0424_LH-p-trip-CH3_100K
;
PROBLEM: Large Average Ueq of Residue Including       I1B      0.117 Check 
RESPONSE: Minor component of disordered I-.
;
_vrf_PLAT342_nt0424_LH-p-trip-CH3_100K
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00871 Ang.  
RESPONSE: Iodine is disordered, modelled with positions.
;
_vrf_PLAT971_nt0424_LH-p-trip-CH3_100K
;
PROBLEM: Check Calcd Resid. Dens.  0.71A   From I1              2.37 eA-3  
RESPONSE: Truncation error peak.
;
_vrf_PLAT972_nt0424_LH-p-trip-CH3_100K
;
PROBLEM: Check Calcd Resid. Dens.  0.72A   From I1             -1.80 eA-3  
RESPONSE: Truncation error peak.
;
_vrf_PLAT978_nt0424_LH-p-trip-CH3_100K
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: Heavy atom in the structure (iodine).
;
# end Validation Reply Form

 
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

 
data_nt0433_LHG09
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         
'9-phosphatriptycene tris(pentafluorophenyl)borane complex'
_chemical_name_common             
'9-phosphatriptycene tris(pentafluorophenyl)borane complex'
_chemical_melting_point           ?
_chemical_formula_moiety          'C37 H13 B F15 P, 0.711(C H2 Cl2)'
_chemical_formula_sum             'C37.71 H14.42 B Cl1.42 F15 P' 
_chemical_formula_weight          844.71

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'
 'Cl'  'Cl'   0.3639   0.7018
 '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'
 'F'  'F'   0.0727   0.0534
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    15.2134(2)
_cell_length_b                    13.99260(17)
_cell_length_c                    16.96049(17)
_cell_angle_alpha                 90
_cell_angle_beta                  98.3027(12)
_cell_angle_gamma                 90
_cell_volume                      3572.61(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     295(2)
_cell_measurement_reflns_used     7215
_cell_measurement_theta_min       4.1040
_cell_measurement_theta_max       66.8670
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.570          
_exptl_crystal_F_000              1680
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.490
_exptl_crystal_size_mid           0.047
_exptl_crystal_size_min           0.021
_exptl_absorpt_coefficient_mu     2.651
_shelx_estimated_absorpt_T_min    0.357
_shelx_estimated_absorpt_T_max    0.946
_exptl_absorpt_correction_T_min   0.552
_exptl_absorpt_correction_T_max   0.946
_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             19970
_diffrn_reflns_av_unetI/netI      0.0271
_diffrn_reflns_av_R_equivalents   0.0320
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          2.935
_diffrn_reflns_theta_max          67.065
_diffrn_reflns_theta_full         67.065
_diffrn_measured_fraction_theta_max   0.992
_diffrn_measured_fraction_theta_full  0.992
_diffrn_reflns_Laue_measured_fraction_max    0.992
_diffrn_reflns_Laue_measured_fraction_full   0.992
_diffrn_reflns_point_group_measured_fraction_max   0.992
_diffrn_reflns_point_group_measured_fraction_full  0.992
_reflns_number_total              6330
_reflns_number_gt                 5013
_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 (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)+(0.0690P)²+0.6037P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          6330
_refine_ls_number_parameters      599
_refine_ls_number_restraints      96
_refine_ls_R_factor_all           0.0562
_refine_ls_R_factor_gt            0.0429
_refine_ls_wR_factor_ref          0.1243
_refine_ls_wR_factor_gt           0.1133
_refine_ls_goodness_of_fit_ref    1.033
_refine_ls_restrained_S_all       1.063
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
C38A C 0.156(4) 0.766(5) 0.6393(17) 0.368(16) Uani 0.238(6) 1 d D U P A 1
H38A H 0.168858 0.830488 0.657798 0.442 Uiso 0.238(6) 1 calc R U P A 1
H38B H 0.094667 0.752108 0.643153 0.442 Uiso 0.238(6) 1 calc R U P A 1
Cl1A Cl 0.2226(5) 0.6882(7) 0.7002(7) 0.221(5) Uani 0.238(6) 1 d D U P A 1
Cl2A Cl 0.1727(19) 0.757(2) 0.5403(12) 0.431(15) Uani 0.238(6) 1 d D U P A 1
C38B C 0.1501(16) 0.765(6) 0.9187(19) 0.257(16) Uani 0.112(6) 1 d D U P B 2
H38C H 0.110334 0.711039 0.920135 0.309 Uiso 0.112(6) 1 calc R U P B 2
H38D H 0.114447 0.820637 0.901520 0.309 Uiso 0.112(6) 1 calc R U P B 2
Cl1B Cl 0.2061(18) 0.785(2) 1.0131(15) 0.236(11) Uani 0.112(6) 1 d D U P B 2
Cl2B Cl 0.2218(17) 0.7422(14) 0.8513(14) 0.205(9) Uani 0.112(6) 1 d D U P B 2
C38C C 0.287(3) 0.784(5) 0.860(2) 0.266(16) Uani 0.134(5) 1 d D U P C 3
H38E H 0.346027 0.757134 0.870939 0.319 Uiso 0.134(5) 1 calc R U P C 3
H38F H 0.290932 0.843796 0.831767 0.319 Uiso 0.134(5) 1 calc R U P C 3
Cl1C Cl 0.2502(9) 0.8083(10) 0.9494(12) 0.190(7) Uani 0.134(5) 1 d D U P C 3
Cl2C Cl 0.2192(12) 0.7066(15) 0.8002(13) 0.204(7) Uani 0.134(5) 1 d D U P C 3
C38D C 0.199(6) 0.698(2) 0.699(2) 0.384(18) Uani 0.227(7) 1 d D U P D 4
H38G H 0.261082 0.678087 0.707923 0.460 Uiso 0.227(7) 1 calc R U P D 4
H38H H 0.164496 0.645485 0.673596 0.460 Uiso 0.227(7) 1 calc R U P D 4
Cl1D Cl 0.1650(16) 0.7223(17) 0.7896(12) 0.368(13) Uani 0.227(7) 1 d D U P D 4
Cl2D Cl 0.1885(8) 0.7953(12) 0.6363(9) 0.284(8) Uani 0.227(7) 1 d D U P D 4
P1 P 0.34534(3) 0.29047(4) 0.73330(3) 0.04471(14) Uani 1 1 d . . . . .
F1 F 0.29789(10) 0.47433(10) 0.79946(8) 0.0721(4) Uani 1 1 d . . . . .
F2 F 0.28258(12) 0.55568(12) 0.93853(9) 0.0876(5) Uani 1 1 d . . . . .
F3 F 0.16631(13) 0.48535(14) 1.03091(8) 0.0946(5) Uani 1 1 d . . . . .
F4 F 0.06487(12) 0.33128(15) 0.97914(9) 0.0973(5) Uani 1 1 d . . . . .
F5 F 0.07713(10) 0.25053(11) 0.84159(9) 0.0760(4) Uani 1 1 d . . . . .
F6 F 0.03375(10) 0.25202(13) 0.63413(10) 0.0866(5) Uani 1 1 d . . . . .
F7 F -0.03515(12) 0.07898(16) 0.61835(13) 0.1115(6) Uani 1 1 d . . . . .
F8 F 0.04879(14) -0.07159(14) 0.69535(15) 0.1191(7) Uani 1 1 d . . . . .
F9 F 0.20544(13) -0.04322(12) 0.79302(13) 0.1022(6) Uani 1 1 d . . . . .
F10 F 0.27751(9) 0.12954(10) 0.80809(8) 0.0671(4) Uani 1 1 d . . . . .
F11 F 0.09649(12) 0.48836(14) 0.72000(9) 0.0952(6) Uani 1 1 d . . . . .
F12 F 0.05148(18) 0.59248(16) 0.59213(12) 0.1306(9) Uani 1 1 d . . . . .
F13 F 0.10187(18) 0.54243(16) 0.45045(11) 0.1277(8) Uani 1 1 d . . . . .
F14 F 0.19722(14) 0.37945(14) 0.44126(8) 0.0974(6) Uani 1 1 d . . . . .
F15 F 0.24241(10) 0.27196(10) 0.56905(8) 0.0710(4) Uani 1 1 d . . . . .
C1 C 0.41439(14) 0.28321(14) 0.83106(12) 0.0487(5) Uani 1 1 d . . . . .
C2 C 0.38544(16) 0.27773(16) 0.90515(12) 0.0560(5) Uani 1 1 d . . . . .
H2 H 0.325046 0.276863 0.908849 0.067 Uiso 1 1 calc R U . . .
C3 C 0.44775(19) 0.27358(18) 0.97340(14) 0.0665(6) Uani 1 1 d . . . . .
H3 H 0.428883 0.269659 1.023071 0.080 Uiso 1 1 calc R U . . .
C4 C 0.53697(19) 0.27521(19) 0.96832(14) 0.0690(7) Uani 1 1 d . . . . .
H4 H 0.577996 0.274673 1.014631 0.083 Uiso 1 1 calc R U . . .
C5 C 0.56632(17) 0.27763(17) 0.89493(14) 0.0622(6) Uani 1 1 d . . . . .
H5 H 0.626843 0.277664 0.891770 0.075 Uiso 1 1 calc R U . . .
C6 C 0.50470(15) 0.28003(15) 0.82576(13) 0.0522(5) Uani 1 1 d . . . . .
C7 C 0.39398(14) 0.18795(14) 0.68775(11) 0.0470(4) Uani 1 1 d . . . . .
C8 C 0.34946(16) 0.11296(15) 0.64597(12) 0.0530(5) Uani 1 1 d . . . . .
H8 H 0.287698 0.111753 0.637196 0.064 Uiso 1 1 calc R U . . .
C9 C 0.39756(18) 0.03988(16) 0.61740(13) 0.0617(6) Uani 1 1 d . . . . .
H9 H 0.367835 -0.010844 0.589897 0.074 Uiso 1 1 calc R U . . .
C10 C 0.48867(18) 0.04169(17) 0.62932(14) 0.0652(6) Uani 1 1 d . . . . .
H10 H 0.520419 -0.007927 0.610266 0.078 Uiso 1 1 calc R U . . .
C11 C 0.53342(16) 0.11731(17) 0.66969(13) 0.0601(6) Uani 1 1 d . . . . .
H11 H 0.595181 0.118811 0.677067 0.072 Uiso 1 1 calc R U . . .
C12 C 0.48645(14) 0.19069(15) 0.69911(12) 0.0509(5) Uani 1 1 d . . . . .
C13 C 0.40686(14) 0.38412(15) 0.68888(12) 0.0503(5) Uani 1 1 d . . . . .
C14 C 0.37308(17) 0.46521(16) 0.64843(13) 0.0585(5) Uani 1 1 d . . . . .
H14 H 0.312733 0.478903 0.643782 0.070 Uiso 1 1 calc R U . . .
C15 C 0.4293(2) 0.52557(18) 0.61507(16) 0.0736(7) Uani 1 1 d . . . . .
H15 H 0.406135 0.578856 0.586521 0.088 Uiso 1 1 calc R U . . .
C16 C 0.5186(2) 0.5080(2) 0.62350(17) 0.0799(8) Uani 1 1 d . . . . .
H16 H 0.555664 0.549513 0.600920 0.096 Uiso 1 1 calc R U . . .
C17 C 0.55408(18) 0.4291(2) 0.66523(16) 0.0710(7) Uani 1 1 d . . . . .
H17 H 0.614960 0.417953 0.671532 0.085 Uiso 1 1 calc R U . . .
C18 C 0.49822(15) 0.36603(16) 0.69794(13) 0.0545(5) Uani 1 1 d . . . . .
C19 C 0.53161(15) 0.27662(16) 0.74283(13) 0.0550(5) Uani 1 1 d . . . . .
H19 H 0.596300 0.271576 0.746212 0.066 Uiso 1 1 calc R U . . .
C20 C 0.19252(14) 0.35515(16) 0.81437(12) 0.0518(5) Uani 1 1 d . . . . .
C21 C 0.23947(15) 0.43541(16) 0.84321(13) 0.0552(5) Uani 1 1 d . . . . .
C22 C 0.23299(17) 0.47923(18) 0.91479(14) 0.0631(6) Uani 1 1 d . . . . .
C23 C 0.17474(18) 0.4435(2) 0.96127(13) 0.0675(7) Uani 1 1 d . . . . .
C24 C 0.12397(17) 0.3661(2) 0.93520(14) 0.0670(7) Uani 1 1 d . . . . .
C25 C 0.13258(15) 0.32411(18) 0.86322(13) 0.0575(5) Uani 1 1 d . . . . .
C26 C 0.16273(14) 0.19955(17) 0.71881(12) 0.0546(5) Uani 1 1 d . . . . .
C27 C 0.08120(16) 0.1809(2) 0.67276(15) 0.0663(6) Uani 1 1 d . . . . .
C28 C 0.04295(18) 0.0915(2) 0.66482(17) 0.0779(8) Uani 1 1 d . . . . .
C29 C 0.0847(2) 0.0158(2) 0.70394(19) 0.0815(8) Uani 1 1 d . . . . .
C30 C 0.16365(19) 0.02983(19) 0.75275(17) 0.0728(7) Uani 1 1 d . . . . .
C31 C 0.19964(15) 0.12040(18) 0.75911(13) 0.0588(6) Uani 1 1 d . . . . .
C32 C 0.17461(14) 0.37452(17) 0.65232(12) 0.0544(5) Uani 1 1 d . . . . .
C33 C 0.12487(18) 0.4575(2) 0.65293(14) 0.0679(6) Uani 1 1 d . . . . .
C34 C 0.1001(2) 0.5135(2) 0.58693(18) 0.0874(9) Uani 1 1 d . . . . .
C35 C 0.1248(2) 0.4882(2) 0.51494(16) 0.0863(9) Uani 1 1 d . . . . .
C36 C 0.17206(19) 0.4061(2) 0.51058(14) 0.0723(7) Uani 1 1 d . . . . .
C37 C 0.19440(15) 0.35168(17) 0.57760(13) 0.0578(5) Uani 1 1 d . . . . .
B1 B 0.20586(16) 0.30642(18) 0.72925(14) 0.0509(5) Uani 1 1 d . . . . .
 
 
_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
C38A Cl1A 1.717(10) . ?
C38A Cl2A 1.736(10) . ?
C38A H38A 0.9700 . ?
C38A H38B 0.9700 . ?
C38B Cl2B 1.721(10) . ?
C38B Cl1B 1.723(10) . ?
C38B H38C 0.9700 . ?
C38B H38D 0.9700 . ?
C38C Cl1C 1.718(10) . ?
C38C Cl2C 1.725(10) . ?
C38C H38E 0.9700 . ?
C38C H38F 0.9700 . ?
C38D Cl2D 1.721(10) . ?
C38D Cl1D 1.727(10) . ?
C38D H38G 0.9700 . ?
C38D H38H 0.9700 . ?
P1 C1 1.833(2) . ?
P1 C13 1.834(2) . ?
P1 C7 1.835(2) . ?
P1 B1 2.125(2) . ?
F1 C21 1.352(3) . ?
F2 C22 1.337(3) . ?
F3 C23 1.341(3) . ?
F4 C24 1.340(3) . ?
F5 C25 1.348(3) . ?
F6 C27 1.343(3) . ?
F7 C28 1.339(3) . ?
F8 C29 1.338(3) . ?
F9 C30 1.338(3) . ?
F10 C31 1.351(3) . ?
F11 C33 1.345(3) . ?
F12 C34 1.340(3) . ?
F13 C35 1.335(3) . ?
F14 C36 1.341(3) . ?
F15 C37 1.353(3) . ?
C1 C6 1.390(3) . ?
C1 C2 1.392(3) . ?
C2 C3 1.387(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.373(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(3) . ?
C5 H5 0.9300 . ?
C6 C19 1.521(3) . ?
C7 C8 1.387(3) . ?
C7 C12 1.393(3) . ?
C8 C9 1.385(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.372(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.384(3) . ?
C11 H11 0.9300 . ?
C12 C19 1.523(3) . ?
C13 C14 1.386(3) . ?
C13 C18 1.399(3) . ?
C14 C15 1.380(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.368(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.379(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.394(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.514(3) . ?
C19 H19 0.9800 . ?
C20 C21 1.382(3) . ?
C20 C25 1.387(3) . ?
C20 B1 1.636(3) . ?
C21 C22 1.376(3) . ?
C22 C23 1.363(4) . ?
C23 C24 1.367(4) . ?
C24 C25 1.378(3) . ?
C26 C31 1.378(3) . ?
C26 C27 1.392(3) . ?
C26 B1 1.632(3) . ?
C27 C28 1.378(4) . ?
C28 C29 1.358(5) . ?
C29 C30 1.371(4) . ?
C30 C31 1.378(4) . ?
C32 C37 1.382(3) . ?
C32 C33 1.386(3) . ?
C32 B1 1.630(3) . ?
C33 C34 1.374(4) . ?
C34 C35 1.374(4) . ?
C35 C36 1.364(4) . ?
C36 C37 1.369(3) . ?
 
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
Cl1A C38A Cl2A 112.7(9) . . ?
Cl1A C38A H38A 109.0 . . ?
Cl2A C38A H38A 109.0 . . ?
Cl1A C38A H38B 109.1 . . ?
Cl2A C38A H38B 109.1 . . ?
H38A C38A H38B 107.8 . . ?
Cl2B C38B Cl1B 111.8(9) . . ?
Cl2B C38B H38C 109.3 . . ?
Cl1B C38B H38C 109.3 . . ?
Cl2B C38B H38D 109.3 . . ?
Cl1B C38B H38D 109.3 . . ?
H38C C38B H38D 107.9 . . ?
Cl1C C38C Cl2C 113.7(10) . . ?
Cl1C C38C H38E 108.8 . . ?
Cl2C C38C H38E 108.8 . . ?
Cl1C C38C H38F 108.8 . . ?
Cl2C C38C H38F 108.8 . . ?
H38E C38C H38F 107.7 . . ?
Cl2D C38D Cl1D 112.3(10) . . ?
Cl2D C38D H38G 109.1 . . ?
Cl1D C38D H38G 109.1 . . ?
Cl2D C38D H38H 109.1 . . ?
Cl1D C38D H38H 109.1 . . ?
H38G C38D H38H 107.9 . . ?
C1 P1 C13 98.71(10) . . ?
C1 P1 C7 97.14(9) . . ?
C13 P1 C7 97.17(9) . . ?
C1 P1 B1 118.31(9) . . ?
C13 P1 B1 118.56(10) . . ?
C7 P1 B1 122.00(10) . . ?
C6 C1 C2 120.1(2) . . ?
C6 C1 P1 112.69(15) . . ?
C2 C1 P1 127.21(17) . . ?
C3 C2 C1 119.2(2) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C4 C3 C2 120.6(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 120.5(2) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 119.6(2) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 119.8(2) . . ?
C1 C6 C19 117.46(19) . . ?
C5 C6 C19 122.7(2) . . ?
C8 C7 C12 120.04(19) . . ?
C8 C7 P1 127.57(17) . . ?
C12 C7 P1 112.39(15) . . ?
C9 C8 C7 119.6(2) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C8 120.6(2) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.1(2) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 120.2(2) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C7 119.6(2) . . ?
C11 C12 C19 122.7(2) . . ?
C7 C12 C19 117.69(18) . . ?
C14 C13 C18 119.6(2) . . ?
C14 C13 P1 127.85(17) . . ?
C18 C13 P1 112.54(16) . . ?
C15 C14 C13 119.8(2) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 120.8(2) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 120.5(2) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C18 119.7(3) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C17 C18 C13 119.6(2) . . ?
C17 C18 C19 122.9(2) . . ?
C13 C18 C19 117.43(19) . . ?
C18 C19 C6 108.87(18) . . ?
C18 C19 C12 108.21(17) . . ?
C6 C19 C12 108.19(17) . . ?
C18 C19 H19 110.5 . . ?
C6 C19 H19 110.5 . . ?
C12 C19 H19 110.5 . . ?
C21 C20 C25 113.19(19) . . ?
C21 C20 B1 121.84(19) . . ?
C25 C20 B1 124.9(2) . . ?
F1 C21 C22 116.2(2) . . ?
F1 C21 C20 118.70(18) . . ?
C22 C21 C20 125.1(2) . . ?
F2 C22 C23 120.3(2) . . ?
F2 C22 C21 120.8(2) . . ?
C23 C22 C21 118.8(2) . . ?
F3 C23 C22 120.2(3) . . ?
F3 C23 C24 120.6(2) . . ?
C22 C23 C24 119.2(2) . . ?
F4 C24 C23 120.1(2) . . ?
F4 C24 C25 119.7(3) . . ?
C23 C24 C25 120.2(2) . . ?
F5 C25 C24 115.5(2) . . ?
F5 C25 C20 121.07(19) . . ?
C24 C25 C20 123.4(2) . . ?
C31 C26 C27 113.2(2) . . ?
C31 C26 B1 123.64(19) . . ?
C27 C26 B1 123.0(2) . . ?
F6 C27 C28 115.8(2) . . ?
F6 C27 C26 120.5(2) . . ?
C28 C27 C26 123.7(3) . . ?
F7 C28 C29 119.8(3) . . ?
F7 C28 C27 120.2(3) . . ?
C29 C28 C27 120.0(3) . . ?
F8 C29 C28 120.3(3) . . ?
F8 C29 C30 120.3(3) . . ?
C28 C29 C30 119.3(2) . . ?
F9 C30 C29 120.6(2) . . ?
F9 C30 C31 120.5(3) . . ?
C29 C30 C31 118.8(3) . . ?
F10 C31 C26 119.2(2) . . ?
F10 C31 C30 116.0(2) . . ?
C26 C31 C30 124.8(2) . . ?
C37 C32 C33 113.1(2) . . ?
C37 C32 B1 121.5(2) . . ?
C33 C32 B1 125.43(19) . . ?
F11 C33 C34 115.0(2) . . ?
F11 C33 C32 121.2(2) . . ?
C34 C33 C32 123.9(2) . . ?
F12 C34 C33 120.4(3) . . ?
F12 C34 C35 119.7(3) . . ?
C33 C34 C35 119.9(3) . . ?
F13 C35 C36 120.8(3) . . ?
F13 C35 C34 120.6(3) . . ?
C36 C35 C34 118.6(2) . . ?
F14 C36 C35 120.1(2) . . ?
F14 C36 C37 120.4(2) . . ?
C35 C36 C37 119.5(2) . . ?
F15 C37 C36 116.3(2) . . ?
F15 C37 C32 118.8(2) . . ?
C36 C37 C32 124.9(2) . . ?
C32 B1 C26 112.49(18) . . ?
C32 B1 C20 113.82(18) . . ?
C26 B1 C20 112.24(17) . . ?
C32 B1 P1 105.17(14) . . ?
C26 B1 P1 106.93(15) . . ?
C20 B1 P1 105.42(14) . . ?
 
_refine_diff_density_max    0.356
_refine_diff_density_min   -0.252
_refine_diff_density_rms    0.040



# start Validation Reply Form
_vrf_PLAT411_nt0433_LHG09
;
PROBLEM: Short Inter H...H Contact  H17      ..H38F     .       1.78 Ang.  
RESPONSE: Disordered dichloromethane molecule with small occupancy.
;
_vrf_PLAT260_nt0433_LHG09
;
PROBLEM: Large Average Ueq of Residue Including      Cl1A      0.340 Check 
RESPONSE: Disordered molecules of dichloromethane in the channels.
;
_vrf_PLAT077_nt0433_LHG09
;
PROBLEM: Unitcell Contains Non-integer Number of Atoms ..     Please Check 
RESPONSE: Disordered molecules of dichloromethane in the channels with total
occupancy 0.71. 
;
_vrf_PLAT911_nt0433_LHG09
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.597         48 Report
RESPONSE: 5 reflections are missing because of overflow, the rest is missing 
in the highest resolution shell because of the instrument geometry limitations.
;
# end Validation Reply Form


