 
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