# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_nt0284_LeiHu_73B
_database_code_depnum_ccdc_archive 'CCDC 2313762'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        '9-phosphatriptycene oxide hemihydrate'
_chemical_name_common            '9-phosphatriptycene oxide hemihydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C19 H13 O P), H2 O'
_chemical_formula_sum            'C38 H28 O3 P2'
_chemical_formula_weight         594.54

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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   16.51047(10)
_cell_length_b                   16.41081(10)
_cell_length_c                   23.08005(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6253.54(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    16846
_cell_measurement_theta_min      3.3020
_cell_measurement_theta_max      67.0790

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_F_000             2480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.549
_shelx_estimated_absorpt_T_min   0.549
_shelx_estimated_absorpt_T_max   0.812
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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 10.3712
_diffrn_reflns_number            28008
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.830
_diffrn_reflns_theta_max         67.114
_diffrn_reflns_theta_full        67.114
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5550
_reflns_number_gt                5212
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0572P)²+0.6349P] 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         5550
_refine_ls_number_parameters     980
_refine_ls_number_restraints     1047
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0967
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.040
_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
O2A O 0.5939(4) 0.2631(3) 0.6343(3) 0.161(3) Uani 0.451(3) 1 d . U P A 1
H21 H 0.629186 0.279190 0.608307 0.241 Uiso 0.451(3) 1 d R U P A 1
H22 H 0.567160 0.307472 0.643433 0.241 Uiso 0.451(3) 1 d R U P A 1
O2B O 0.6285(6) 0.2946(5) 0.6553(4) 0.171(3) Uani 0.409(3) 1 d . U P B 2
H23 H 0.593439 0.334726 0.655725 0.256 Uiso 0.409(3) 1 d R U P B 2
H24 H 0.661225 0.306205 0.626640 0.256 Uiso 0.409(3) 1 d R U P B 2
O2C O 0.5988(11) 0.3578(9) 0.6058(8) 0.180(4) Uani 0.140(3) 1 d . U P C 3
H25 H 0.580228 0.335859 0.640474 0.270 Uiso 0.140(3) 1 d R U P C 3
H26 H 0.599587 0.315674 0.582524 0.270 Uiso 0.140(3) 1 d R U P C 3
P1B P 0.75630(9) 0.27101(9) 0.49779(6) 0.0539(3) Uani 0.581(3) 1 d D U P D 1
O1B O 0.68829(16) 0.29957(19) 0.53336(12) 0.0880(7) Uani 0.581(3) 1 d D . P D 1
C1B C 0.8569(4) 0.3114(4) 0.5115(3) 0.0540(11) Uani 0.581(3) 1 d D U P D 1
C2B C 0.8774(4) 0.3680(3) 0.5534(2) 0.0731(12) Uani 0.581(3) 1 d D U P D 1
H2B H 0.838283 0.388116 0.578623 0.088 Uiso 0.581(3) 1 calc R U P D 1
C3B C 0.9565(5) 0.3941(6) 0.5575(4) 0.092(2) Uani 0.581(3) 1 d D U P D 1
H3B H 0.970705 0.433293 0.584777 0.110 Uiso 0.581(3) 1 calc R U P D 1
C4B C 1.0142(3) 0.3626(4) 0.5215(3) 0.0951(16) Uani 0.581(3) 1 d D U P D 1
H4B H 1.067583 0.379821 0.525199 0.114 Uiso 0.581(3) 1 calc R U P D 1
C5B C 0.9948(3) 0.3051(4) 0.4793(3) 0.0790(14) Uani 0.581(3) 1 d D U P D 1
H5B H 1.034516 0.284918 0.454534 0.095 Uiso 0.581(3) 1 calc R U P D 1
C6B C 0.9155(4) 0.2786(6) 0.4747(4) 0.0541(13) Uani 0.581(3) 1 d D U P D 1
C7B C 0.8865(6) 0.2170(6) 0.4315(4) 0.0604(19) Uani 0.581(3) 1 d D U P D 1
H7B H 0.932046 0.197685 0.408022 0.072 Uiso 0.581(3) 1 calc R U P D 1
C8B C 0.8217(5) 0.2542(7) 0.3926(3) 0.0482(13) Uani 0.581(3) 1 d D U P D 1
C9B C 0.8284(4) 0.2625(5) 0.3333(2) 0.0604(11) Uani 0.581(3) 1 d D . P D 1
H9B H 0.874184 0.243335 0.314213 0.072 Uiso 0.581(3) 1 calc R U P D 1
C10B C 0.7673(4) 0.2989(6) 0.3026(2) 0.0750(14) Uani 0.581(3) 1 d D . P D 1
H10B H 0.771220 0.302429 0.262466 0.090 Uiso 0.581(3) 1 calc R U P D 1
C11B C 0.7007(5) 0.3301(7) 0.3298(3) 0.081(2) Uani 0.581(3) 1 d D U P D 1
H11B H 0.661123 0.356350 0.308094 0.097 Uiso 0.581(3) 1 calc R U P D 1
C12B C 0.6913(3) 0.3232(5) 0.3893(3) 0.0717(13) Uani 0.581(3) 1 d D . P D 1
H12B H 0.645126 0.342723 0.407803 0.086 Uiso 0.581(3) 1 calc R U P D 1
C13B C 0.7533(4) 0.2860(4) 0.4203(2) 0.0499(9) Uani 0.581(3) 1 d D U P D 1
C14B C 0.8483(7) 0.1461(4) 0.4635(5) 0.0596(19) Uani 0.581(3) 1 d D U P D 1
C15B C 0.8794(4) 0.0677(4) 0.4608(4) 0.085(2) Uani 0.581(3) 1 d D U P D 1
H15B H 0.922433 0.055442 0.436212 0.102 Uiso 0.581(3) 1 calc R U P D 1
C16B C 0.8449(6) 0.0074(4) 0.4956(4) 0.101(3) Uani 0.581(3) 1 d D U P D 1
H16B H 0.866109 -0.045091 0.496021 0.121 Uiso 0.581(3) 1 calc R U P D 1
C17B C 0.7794(5) 0.0269(4) 0.5292(3) 0.105(3) Uani 0.581(3) 1 d D U P D 1
H17B H 0.755388 -0.013477 0.551594 0.126 Uiso 0.581(3) 1 calc R U P D 1
C18B C 0.7481(5) 0.1048(4) 0.5308(3) 0.0898(18) Uani 0.581(3) 1 d D U P D 1
H18B H 0.703820 0.116245 0.554371 0.108 Uiso 0.581(3) 1 calc R U P D 1
C19B C 0.7816(5) 0.1650(4) 0.4979(4) 0.0559(15) Uani 0.581(3) 1 d D U P D 1
P1C P 0.75037(15) 0.24061(18) 0.50957(11) 0.0650(6) Uani 0.353(3) 1 d D . P E 2
O1C O 0.6811(3) 0.2489(5) 0.5489(2) 0.1139(18) Uani 0.353(3) 1 d D . P E 2
C1C C 0.8377(7) 0.2990(6) 0.5257(4) 0.067(2) Uani 0.353(3) 1 d D . P E 2
C2C C 0.8473(9) 0.3535(7) 0.5720(4) 0.104(4) Uani 0.353(3) 1 d D . P E 2
H2C H 0.805422 0.361658 0.598392 0.124 Uiso 0.353(3) 1 calc R U P E 2
C3C C 0.9194(10) 0.3946(9) 0.5779(6) 0.121(5) Uani 0.353(3) 1 d D . P E 2
H3C H 0.926567 0.430876 0.608467 0.145 Uiso 0.353(3) 1 calc R U P E 2
C4C C 0.9789(12) 0.3826(13) 0.5400(9) 0.120(5) Uani 0.353(3) 1 d D . P E 2
H4C H 1.026667 0.412027 0.544436 0.145 Uiso 0.353(3) 1 calc R U P E 2
C5C C 0.9730(7) 0.3277(9) 0.4938(6) 0.093(3) Uani 0.353(3) 1 d D . P E 2
H5C H 1.016621 0.317873 0.469277 0.111 Uiso 0.353(3) 1 calc R U P E 2
C6C C 0.8992(7) 0.2887(9) 0.4860(6) 0.064(3) Uani 0.353(3) 1 d D . P E 2
C7C C 0.8828(9) 0.2321(8) 0.4352(6) 0.061(3) Uani 0.353(3) 1 d D . P E 2
H7C H 0.930069 0.228848 0.409577 0.073 Uiso 0.353(3) 1 calc R U P E 2
C8C C 0.8084(8) 0.2653(11) 0.4025(5) 0.057(3) Uani 0.353(3) 1 d D . P E 2
C9C C 0.8073(7) 0.2791(9) 0.3439(5) 0.079(3) Uani 0.353(3) 1 d D . P E 2
H9C H 0.852574 0.266779 0.321644 0.094 Uiso 0.353(3) 1 calc R U P E 2
C10C C 0.7385(7) 0.3115(8) 0.3177(5) 0.087(4) Uani 0.353(3) 1 d D . P E 2
H10C H 0.738080 0.323119 0.278285 0.105 Uiso 0.353(3) 1 calc R U P E 2
C11C C 0.6725(7) 0.3255(9) 0.3505(5) 0.092(4) Uani 0.353(3) 1 d D . P E 2
H11C H 0.627217 0.349503 0.333593 0.111 Uiso 0.353(3) 1 calc R U P E 2
C12C C 0.6702(7) 0.3052(11) 0.4090(5) 0.091(4) Uani 0.353(3) 1 d D . P E 2
H12C H 0.622615 0.312176 0.430041 0.109 Uiso 0.353(3) 1 calc R U P E 2
C13C C 0.7393(7) 0.2742(10) 0.4364(4) 0.064(3) Uani 0.353(3) 1 d D . P E 2
C14C C 0.8619(10) 0.1488(7) 0.4600(8) 0.050(2) Uani 0.353(3) 1 d D . P E 2
C15C C 0.9056(7) 0.0774(7) 0.4516(7) 0.071(2) Uani 0.353(3) 1 d D . P E 2
H15C H 0.951125 0.077833 0.427863 0.085 Uiso 0.353(3) 1 calc R U P E 2
C16C C 0.8824(7) 0.0062(6) 0.4781(6) 0.087(2) Uani 0.353(3) 1 d D . P E 2
H16C H 0.912890 -0.040660 0.472007 0.104 Uiso 0.353(3) 1 calc R U P E 2
C17C C 0.8144(8) 0.0022(8) 0.5139(7) 0.085(3) Uani 0.353(3) 1 d D . P E 2
H17C H 0.798359 -0.047179 0.530108 0.101 Uiso 0.353(3) 1 calc R U P E 2
C18C C 0.7711(5) 0.0728(5) 0.5250(3) 0.0689(18) Uani 0.353(3) 1 d D . P E 2
H18C H 0.726516 0.072773 0.549619 0.083 Uiso 0.353(3) 1 calc R U P E 2
C19C C 0.7969(6) 0.1428(5) 0.4982(5) 0.0486(16) Uani 0.353(3) 1 d D . P E 2
P1E P 0.8899(12) 0.2151(15) 0.4209(9) 0.067(3) Uani 0.0664(17) 1 d D U P F 3
O1E O 0.9499(14) 0.195(2) 0.3759(10) 0.152(10) Uani 0.0664(17) 1 d D . P F 3
C1E C 0.906(2) 0.293(3) 0.4743(17) 0.054(4) Uani 0.0664(17) 1 d D U P F 3
C2E C 0.980(3) 0.331(4) 0.486(3) 0.079(4) Uani 0.0664(17) 1 d D U P F 3
H2E H 1.024183 0.321208 0.462074 0.095 Uiso 0.0664(17) 1 calc R U P F 3
C3E C 0.986(3) 0.382(5) 0.533(3) 0.096(4) Uani 0.0664(17) 1 d D U P F 3
H3E H 1.035217 0.407425 0.540903 0.115 Uiso 0.0664(17) 1 calc R U P F 3
C4E C 0.922(3) 0.396(4) 0.567(3) 0.090(4) Uani 0.0664(17) 1 d D U P F 3
H4E H 0.926668 0.431390 0.597877 0.108 Uiso 0.0664(17) 1 calc R U P F 3
C5E C 0.848(3) 0.358(3) 0.5568(19) 0.073(4) Uani 0.0664(17) 1 d D U P F 3
H5E H 0.804867 0.366011 0.582373 0.088 Uiso 0.0664(17) 1 calc R U P F 3
C6E C 0.838(2) 0.308(3) 0.5088(16) 0.055(4) Uani 0.0664(17) 1 d D U P F 3
C7E C 0.7627(19) 0.257(2) 0.4990(13) 0.055(3) Uani 0.0664(17) 1 d D U P F 3
H7E H 0.719393 0.271514 0.526227 0.066 Uiso 0.0664(17) 1 calc R U P F 3
C8E C 0.7353(18) 0.267(4) 0.4360(13) 0.052(4) Uani 0.0664(17) 1 d D U P F 3
C9E C 0.660(2) 0.297(4) 0.4205(18) 0.077(12) Uani 0.0664(17) 1 d D . P F 3
H9E H 0.619062 0.300238 0.447752 0.092 Uiso 0.0664(17) 1 calc R U P F 3
C10E C 0.648(2) 0.322(4) 0.3641(19) 0.071(7) Uani 0.0664(17) 1 d D . P F 3
H10E H 0.596765 0.340807 0.353023 0.085 Uiso 0.0664(17) 1 calc R U P F 3
C11E C 0.708(2) 0.319(5) 0.325(2) 0.079(4) Uani 0.0664(17) 1 d D U P F 3
H11E H 0.699408 0.339369 0.287626 0.095 Uiso 0.0664(17) 1 calc R U P F 3
C12E C 0.784(2) 0.287(3) 0.3386(14) 0.067(9) Uani 0.0664(17) 1 d D . P F 3
H12E H 0.824742 0.284899 0.311156 0.081 Uiso 0.0664(17) 1 calc R U P F 3
C13E C 0.7963(15) 0.258(3) 0.3950(12) 0.048(4) Uani 0.0664(17) 1 d D U P F 3
C14E C 0.788(3) 0.168(2) 0.5050(19) 0.055(4) Uani 0.0664(17) 1 d D U P F 3
C15E C 0.736(3) 0.114(3) 0.533(2) 0.088(4) Uani 0.0664(17) 1 d D U P F 3
H15E H 0.695562 0.133035 0.557232 0.106 Uiso 0.0664(17) 1 calc R U P F 3
C16E C 0.745(3) 0.031(3) 0.524(2) 0.103(5) Uani 0.0664(17) 1 d D U P F 3
H16E H 0.710082 -0.005858 0.542196 0.124 Uiso 0.0664(17) 1 calc R U P F 3
C17E C 0.807(3) 0.003(2) 0.4890(19) 0.101(5) Uani 0.0664(17) 1 d D U P F 3
H17E H 0.814220 -0.052519 0.484565 0.121 Uiso 0.0664(17) 1 calc R U P F 3
C18E C 0.858(4) 0.0563(18) 0.460(3) 0.083(4) Uani 0.0664(17) 1 d D U P F 3
H18E H 0.897978 0.036483 0.435803 0.099 Uiso 0.0664(17) 1 calc R U P F 3
C19E C 0.848(3) 0.1387(17) 0.4678(19) 0.060(4) Uani 0.0664(17) 1 d D U P F 3
P1A P 0.49183(3) 0.45020(3) 0.72767(2) 0.05670(17) Uani 0.8730(17) 1 d D U P G
1
O1A O 0.49121(8) 0.37676(8) 0.69041(6) 0.0880(4) Uani 0.8730(17) 1 d D . P G 1
C1A C 0.5569(2) 0.45263(19) 0.78846(15) 0.0519(6) Uani 0.8730(17) 1 d D U P G 1
C2A C 0.60958(17) 0.39134(17) 0.80518(14) 0.0694(7) Uani 0.8730(17) 1 d D U P G
1
H2A H 0.611073 0.342385 0.784909 0.083 Uiso 0.8730(17) 1 calc R U P G 1
C3A C 0.6597(2) 0.40343(18) 0.85195(14) 0.0794(8) Uani 0.8730(17) 1 d D U P G 1
H3A H 0.695898 0.362820 0.862826 0.095 Uiso 0.8730(17) 1 calc R U P G 1
C4A C 0.6567(2) 0.4746(2) 0.88262(14) 0.0760(9) Uani 0.8730(17) 1 d D U P G 1
H4A H 0.691254 0.482301 0.913971 0.091 Uiso 0.8730(17) 1 calc R U P G 1
C5A C 0.6021(2) 0.5358(2) 0.86719(13) 0.0623(7) Uani 0.8730(17) 1 d D U P G 1
H5A H 0.599351 0.583470 0.888895 0.075 Uiso 0.8730(17) 1 calc R U P G 1
C6A C 0.5521(2) 0.5256(2) 0.81950(14) 0.0486(7) Uani 0.8730(17) 1 d D U P G 1
C7A C 0.4943(3) 0.5887(2) 0.7983(2) 0.0553(8) Uani 0.8730(17) 1 d D U P G 1
H7A H 0.495384 0.636817 0.823446 0.066 Uiso 0.8730(17) 1 calc R U P G 1
C8A C 0.40760(16) 0.55145(15) 0.79604(14) 0.0545(5) Uani 0.8730(17) 1 d D U P G
1
C9A C 0.34128(15) 0.58282(16) 0.82410(12) 0.0734(5) Uani 0.8730(17) 1 d D . P G
1
H9A H 0.345702 0.630597 0.845545 0.088 Uiso 0.8730(17) 1 calc R U P G 1
C10A C 0.26769(14) 0.54265(19) 0.82018(10) 0.0937(7) Uani 0.8730(17) 1 d D . P
G 1
H10A H 0.222651 0.564141 0.838948 0.112 Uiso 0.8730(17) 1 calc R U P G 1
C11A C 0.25993(18) 0.4713(3) 0.78893(13) 0.1063(10) Uani 0.8730(17) 1 d D U P G
1
H11A H 0.210570 0.444018 0.787896 0.128 Uiso 0.8730(17) 1 calc R U P G 1
C12A C 0.32552(16) 0.44073(18) 0.75935(10) 0.0879(7) Uani 0.8730(17) 1 d D . P
G 1
H12A H 0.320315 0.393704 0.737177 0.105 Uiso 0.8730(17) 1 calc R U P G 1
C13A C 0.39926(12) 0.48032(14) 0.76278(10) 0.0577(5) Uani 0.8730(17) 1 d D U P
G 1
C14A C 0.5140(3) 0.61208(19) 0.73596(15) 0.0558(6) Uani 0.8730(17) 1 d D U P G
1
C15A C 0.5288(3) 0.6907(2) 0.71758(14) 0.0759(7) Uani 0.8730(17) 1 d D U P G 1
H15A H 0.525724 0.734157 0.743342 0.091 Uiso 0.8730(17) 1 calc R U P G 1
C16A C 0.5487(3) 0.7036(2) 0.65961(16) 0.0975(10) Uani 0.8730(17) 1 d D U P G 1
H16A H 0.557875 0.756499 0.646734 0.117 Uiso 0.8730(17) 1 calc R U P G 1
C17A C 0.5549(3) 0.6405(2) 0.62117(16) 0.0946(11) Uani 0.8730(17) 1 d D U P G 1
H17A H 0.569571 0.650835 0.582961 0.113 Uiso 0.8730(17) 1 calc R U P G 1
C18A C 0.5397(3) 0.5617(2) 0.63860(14) 0.0767(9) Uani 0.8730(17) 1 d D U P G 1
H18A H 0.543775 0.518691 0.612527 0.092 Uiso 0.8730(17) 1 calc R U P G 1
C19A C 0.5182(2) 0.54780(15) 0.69607(12) 0.0549(6) Uani 0.8730(17) 1 d D U P G
1
P1D P 0.4796(7) 0.6006(6) 0.8032(4) 0.081(2) Uani 0.1270(17) 1 d D U P G 2
O1D O 0.4712(13) 0.6743(9) 0.8415(7) 0.189(9) Uani 0.1270(17) 1 d D . P G 2
C1D C 0.5550(16) 0.5340(14) 0.8299(10) 0.044(3) Uani 0.1270(17) 1 d D U P G 2
C2D C 0.5929(14) 0.5516(14) 0.8803(8) 0.057(4) Uani 0.1270(17) 1 d D U P G 2
H2D H 0.582109 0.598835 0.901133 0.069 Uiso 0.1270(17) 1 calc R U P G 2
C3D C 0.6474(15) 0.4958(14) 0.8981(8) 0.069(4) Uani 0.1270(17) 1 d D U P G 2
H3D H 0.677152 0.505653 0.931615 0.083 Uiso 0.1270(17) 1 calc R U P G 2
C4D C 0.6599(18) 0.4263(15) 0.8686(10) 0.079(4) Uani 0.1270(17) 1 d D U P G 2
H4D H 0.692612 0.386670 0.885355 0.095 Uiso 0.1270(17) 1 calc R U P G 2
C5D C 0.6271(13) 0.4106(11) 0.8153(10) 0.067(4) Uani 0.1270(17) 1 d D U P G 2
H5D H 0.643011 0.366482 0.792757 0.081 Uiso 0.1270(17) 1 calc R U P G 2
C6D C 0.5666(15) 0.4672(14) 0.7970(10) 0.047(3) Uani 0.1270(17) 1 d D U P G 2
C7D C 0.5208(7) 0.4516(8) 0.7416(5) 0.056(3) Uani 0.1270(17) 1 d D U P G 2
H7D H 0.535291 0.400523 0.722179 0.067 Uiso 0.1270(17) 1 calc R U P G 2
C8D C 0.4248(7) 0.4605(9) 0.7567(7) 0.061(3) Uani 0.1270(17) 1 d D U P G 2
C9D C 0.3609(10) 0.4034(12) 0.7535(9) 0.112(5) Uani 0.1270(17) 1 d D . P G 2
H9D H 0.368989 0.354853 0.733529 0.134 Uiso 0.1270(17) 1 calc R U P G 2
C10D C 0.2866(12) 0.4178(16) 0.7794(10) 0.139(8) Uani 0.1270(17) 1 d D . P G 2
H10D H 0.247931 0.376630 0.777460 0.167 Uiso 0.1270(17) 1 calc R U P G 2
C11D C 0.2657(13) 0.4881(18) 0.8078(13) 0.114(5) Uani 0.1270(17) 1 d D U P G 2
H11D H 0.212906 0.497226 0.820164 0.137 Uiso 0.1270(17) 1 calc R U P G 2
C12D C 0.3243(10) 0.5435(13) 0.8170(10) 0.097(5) Uani 0.1270(17) 1 d D . P G 2
H12D H 0.315289 0.589926 0.839191 0.116 Uiso 0.1270(17) 1 calc R U P G 2
C13D C 0.4012(10) 0.5274(11) 0.7908(11) 0.061(3) Uani 0.1270(17) 1 d D U P G 2
C14D C 0.5231(17) 0.5276(11) 0.7017(8) 0.060(3) Uani 0.1270(17) 1 d D U P G 2
C15D C 0.540(2) 0.5374(16) 0.6433(10) 0.074(4) Uani 0.1270(17) 1 d D U P G 2
H15D H 0.541427 0.490415 0.620753 0.089 Uiso 0.1270(17) 1 calc R U P G 2
C16D C 0.555(2) 0.6101(14) 0.6154(12) 0.085(4) Uani 0.1270(17) 1 d D U P G 2
H16D H 0.563722 0.610351 0.575647 0.102 Uiso 0.1270(17) 1 calc R U P G 2
C17D C 0.557(3) 0.6810(15) 0.6452(11) 0.095(5) Uani 0.1270(17) 1 d D U P G 2
H17D H 0.571899 0.729475 0.627225 0.114 Uiso 0.1270(17) 1 calc R U P G 2
C18D C 0.536(3) 0.6792(14) 0.7026(10) 0.080(4) Uani 0.1270(17) 1 d D U P G 2
H18D H 0.532053 0.727461 0.723456 0.096 Uiso 0.1270(17) 1 calc R U P G 2
C19D C 0.521(2) 0.6038(13) 0.7299(9) 0.058(4) Uani 0.1270(17) 1 d D U P G 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
O2A H21 0.8761 . ?
O2A H22 0.8769 . ?
O2B H23 0.8773 . ?
O2B H24 0.8759 . ?
O2C H25 0.9304 . ?
O2C H26 0.8756 . ?
P1B O1B 1.468(3) . ?
P1B C19B 1.789(5) . ?
P1B C13B 1.806(4) . ?
P1B C1B 1.817(5) . ?
C1B C2B 1.384(6) . ?
C1B C6B 1.394(6) . ?
C2B C3B 1.378(9) . ?
C2B H2B 0.9300 . ?
C3B C4B 1.366(8) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.393(7) . ?
C4B H4B 0.9300 . ?
C5B C6B 1.384(7) . ?
C5B H5B 0.9300 . ?
C6B C7B 1.499(9) . ?
C7B C14B 1.514(9) . ?
C7B C8B 1.525(9) . ?
C7B H7B 0.9800 . ?
C8B C9B 1.380(6) . ?
C8B C13B 1.399(6) . ?
C9B C10B 1.370(7) . ?
C9B H9B 0.9300 . ?
C10B C11B 1.365(7) . ?
C10B H10B 0.9300 . ?
C11B C12B 1.387(7) . ?
C11B H11B 0.9300 . ?
C12B C13B 1.390(6) . ?
C12B H12B 0.9300 . ?
C14B C15B 1.388(7) . ?
C14B C19B 1.393(7) . ?
C15B C16B 1.396(8) . ?
C15B H15B 0.9300 . ?
C16B C17B 1.368(10) . ?
C16B H16B 0.9300 . ?
C17B C18B 1.379(8) . ?
C17B H17B 0.9300 . ?
C18B C19B 1.363(7) . ?
C18B H18B 0.9300 . ?
P1C O1C 1.466(5) . ?
P1C C1C 1.771(9) . ?
P1C C13C 1.786(9) . ?
P1C C19C 1.799(8) . ?
C1C C6C 1.377(10) . ?
C1C C2C 1.402(10) . ?
C2C C3C 1.376(12) . ?
C2C H2C 0.9300 . ?
C3C C4C 1.331(15) . ?
C3C H3C 0.9300 . ?
C4C C5C 1.400(14) . ?
C4C H4C 0.9300 . ?
C5C C6C 1.389(11) . ?
C5C H5C 0.9300 . ?
C6C C7C 1.520(12) . ?
C7C C14C 1.523(12) . ?
C7C C8C 1.541(12) . ?
C7C H7C 0.9800 . ?
C8C C9C 1.371(11) . ?
C8C C13C 1.391(10) . ?
C9C C10C 1.393(11) . ?
C9C H9C 0.9300 . ?
C10C C11C 1.346(12) . ?
C10C H10C 0.9300 . ?
C11C C12C 1.393(11) . ?
C11C H11C 0.9300 . ?
C12C C13C 1.400(10) . ?
C12C H12C 0.9300 . ?
C14C C15C 1.390(11) . ?
C14C C19C 1.393(11) . ?
C15C C16C 1.373(12) . ?
C15C H15C 0.9300 . ?
C16C C17C 1.397(14) . ?
C16C H16C 0.9300 . ?
C17C C18C 1.385(14) . ?
C17C H17C 0.9300 . ?
C18C C19C 1.372(10) . ?
C18C H18C 0.9300 . ?
P1E O1E 1.470(15) . ?
P1E C1E 1.796(16) . ?
P1E C19E 1.797(16) . ?
P1E C13E 1.801(16) . ?
C1E C2E 1.395(17) . ?
C1E C6E 1.398(16) . ?
C2E C3E 1.377(19) . ?
C2E H2E 0.9300 . ?
C3E C4E 1.340(19) . ?
C3E H3E 0.9300 . ?
C4E C5E 1.389(19) . ?
C4E H4E 0.9300 . ?
C5E C6E 1.389(17) . ?
C5E H5E 0.9300 . ?
C6E C7E 1.510(18) . ?
C7E C14E 1.528(18) . ?
C7E C8E 1.530(18) . ?
C7E H7E 0.9800 . ?
C8E C9E 1.378(17) . ?
C8E C13E 1.390(16) . ?
C9E C10E 1.384(18) . ?
C9E H9E 0.9300 . ?
C10E C11E 1.353(19) . ?
C10E H10E 0.9300 . ?
C11E C12E 1.388(18) . ?
C11E H11E 0.9300 . ?
C12E C13E 1.401(17) . ?
C12E H12E 0.9300 . ?
C14E C15E 1.394(17) . ?
C14E C19E 1.397(16) . ?
C15E C16E 1.381(19) . ?
C15E H15E 0.9300 . ?
C16E C17E 1.381(19) . ?
C16E H16E 0.9300 . ?
C17E C18E 1.38(2) . ?
C17E H17E 0.9300 . ?
C18E C19E 1.373(17) . ?
C18E H18E 0.9300 . ?
P1A O1A 1.4807(13) . ?
P1A C1A 1.767(3) . ?
P1A C13A 1.799(2) . ?
P1A C19A 1.813(2) . ?
C1A C2A 1.385(3) . ?
C1A C6A 1.397(3) . ?
C2A C3A 1.374(4) . ?
C2A H2A 0.9300 . ?
C3A C4A 1.367(4) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.395(4) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.387(3) . ?
C5A H5A 0.9300 . ?
C6A C7A 1.492(5) . ?
C7A C14A 1.524(5) . ?
C7A C8A 1.557(4) . ?
C7A H7A 0.9800 . ?
C8A C9A 1.372(3) . ?
C8A C13A 1.404(3) . ?
C9A C10A 1.385(3) . ?
C9A H9A 0.9300 . ?
C10A C11A 1.382(4) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.375(4) . ?
C11A H11A 0.9300 . ?
C12A C13A 1.382(3) . ?
C12A H12A 0.9300 . ?
C14A C15A 1.380(3) . ?
C14A C19A 1.402(3) . ?
C15A C16A 1.393(4) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.368(4) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.377(4) . ?
C17A H17A 0.9300 . ?
C18A C19A 1.392(3) . ?
C18A H18A 0.9300 . ?
P1D O1D 1.505(13) . ?
P1D C1D 1.767(17) . ?
P1D C13D 1.790(15) . ?
P1D C19D 1.827(16) . ?
C1D C6D 1.348(16) . ?
C1D C2D 1.351(17) . ?
C2D C3D 1.349(18) . ?
C2D H2D 0.9300 . ?
C3D C4D 1.344(17) . ?
C3D H3D 0.9300 . ?
C4D C5D 1.368(18) . ?
C4D H4D 0.9300 . ?
C5D C6D 1.428(18) . ?
C5D H5D 0.9300 . ?
C6D C7D 1.506(15) . ?
C7D C14D 1.551(16) . ?
C7D C8D 1.630(14) . ?
C7D H7D 0.9800 . ?
C8D C13D 1.405(14) . ?
C8D C9D 1.413(16) . ?
C9D C10D 1.386(17) . ?
C9D H9D 0.9300 . ?
C10D C11D 1.37(2) . ?
C10D H10D 0.9300 . ?
C11D C12D 1.344(18) . ?
C11D H11D 0.9300 . ?
C12D C13D 1.431(16) . ?
C12D H12D 0.9300 . ?
C14D C15D 1.386(18) . ?
C14D C19D 1.410(16) . ?
C15D C16D 1.377(18) . ?
C15D H15D 0.9300 . ?
C16D C17D 1.352(18) . ?
C16D H16D 0.9300 . ?
C17D C18D 1.368(19) . ?
C17D H17D 0.9300 . ?
C18D C19D 1.411(19) . ?
C18D H18D 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
H21 O2A H22 104.5 . . ?
H23 O2B H24 104.5 . . ?
H25 O2C H26 103.1 . . ?
O1B P1B C19B 119.2(2) . . ?
O1B P1B C13B 119.3(2) . . ?
C19B P1B C13B 98.1(4) . . ?
O1B P1B C1B 119.1(3) . . ?
C19B P1B C1B 98.1(4) . . ?
C13B P1B C1B 98.5(3) . . ?
C2B C1B C6B 121.0(5) . . ?
C2B C1B P1B 126.2(5) . . ?
C6B C1B P1B 112.8(5) . . ?
C3B C2B C1B 119.2(5) . . ?
C3B C2B H2B 120.4 . . ?
C1B C2B H2B 120.4 . . ?
C4B C3B C2B 120.1(7) . . ?
C4B C3B H3B 120.0 . . ?
C2B C3B H3B 120.0 . . ?
C3B C4B C5B 121.5(6) . . ?
C3B C4B H4B 119.3 . . ?
C5B C4B H4B 119.3 . . ?
C6B C5B C4B 118.9(5) . . ?
C6B C5B H5B 120.6 . . ?
C4B C5B H5B 120.6 . . ?
C5B C6B C1B 119.3(6) . . ?
C5B C6B C7B 124.4(6) . . ?
C1B C6B C7B 116.3(6) . . ?
C6B C7B C14B 109.1(8) . . ?
C6B C7B C8B 110.2(8) . . ?
C14B C7B C8B 107.6(8) . . ?
C6B C7B H7B 109.9 . . ?
C14B C7B H7B 109.9 . . ?
C8B C7B H7B 109.9 . . ?
C9B C8B C13B 118.8(5) . . ?
C9B C8B C7B 124.6(6) . . ?
C13B C8B C7B 116.5(6) . . ?
C10B C9B C8B 119.8(5) . . ?
C10B C9B H9B 120.1 . . ?
C8B C9B H9B 120.1 . . ?
C11B C10B C9B 121.2(5) . . ?
C11B C10B H10B 119.4 . . ?
C9B C10B H10B 119.4 . . ?
C10B C11B C12B 121.1(6) . . ?
C10B C11B H11B 119.5 . . ?
C12B C11B H11B 119.5 . . ?
C11B C12B C13B 117.5(5) . . ?
C11B C12B H12B 121.2 . . ?
C13B C12B H12B 121.2 . . ?
C12B C13B C8B 121.6(5) . . ?
C12B C13B P1B 126.1(4) . . ?
C8B C13B P1B 112.3(4) . . ?
C15B C14B C19B 121.6(6) . . ?
C15B C14B C7B 122.5(7) . . ?
C19B C14B C7B 115.9(6) . . ?
C14B C15B C16B 118.7(6) . . ?
C14B C15B H15B 120.7 . . ?
C16B C15B H15B 120.7 . . ?
C17B C16B C15B 118.9(6) . . ?
C17B C16B H16B 120.6 . . ?
C15B C16B H16B 120.6 . . ?
C16B C17B C18B 121.9(6) . . ?
C16B C17B H17B 119.0 . . ?
C18B C17B H17B 119.0 . . ?
C19B C18B C17B 120.2(6) . . ?
C19B C18B H18B 119.9 . . ?
C17B C18B H18B 119.9 . . ?
C18B C19B C14B 118.6(5) . . ?
C18B C19B P1B 127.6(5) . . ?
C14B C19B P1B 113.6(4) . . ?
O1C P1C C1C 117.0(4) . . ?
O1C P1C C13C 118.5(4) . . ?
C1C P1C C13C 96.6(6) . . ?
O1C P1C C19C 120.4(4) . . ?
C1C P1C C19C 99.6(5) . . ?
C13C P1C C19C 100.4(6) . . ?
C6C C1C C2C 120.2(9) . . ?
C6C C1C P1C 113.1(6) . . ?
C2C C1C P1C 126.6(8) . . ?
C3C C2C C1C 119.0(10) . . ?
C3C C2C H2C 120.5 . . ?
C1C C2C H2C 120.5 . . ?
C4C C3C C2C 120.1(11) . . ?
C4C C3C H3C 119.9 . . ?
C2C C3C H3C 119.9 . . ?
C3C C4C C5C 123.0(13) . . ?
C3C C4C H4C 118.5 . . ?
C5C C4C H4C 118.5 . . ?
C6C C5C C4C 117.2(10) . . ?
C6C C5C H5C 121.4 . . ?
C4C C5C H5C 121.4 . . ?
C1C C6C C5C 120.3(9) . . ?
C1C C6C C7C 117.3(9) . . ?
C5C C6C C7C 122.5(11) . . ?
C6C C7C C14C 107.4(11) . . ?
C6C C7C C8C 107.7(10) . . ?
C14C C7C C8C 108.7(12) . . ?
C6C C7C H7C 111.0 . . ?
C14C C7C H7C 111.0 . . ?
C8C C7C H7C 111.0 . . ?
C9C C8C C13C 121.7(9) . . ?
C9C C8C C7C 123.5(10) . . ?
C13C C8C C7C 114.6(9) . . ?
C8C C9C C10C 120.2(9) . . ?
C8C C9C H9C 119.9 . . ?
C10C C9C H9C 119.9 . . ?
C11C C10C C9C 118.8(9) . . ?
C11C C10C H10C 120.6 . . ?
C9C C10C H10C 120.6 . . ?
C10C C11C C12C 121.7(9) . . ?
C10C C11C H11C 119.1 . . ?
C12C C11C H11C 119.1 . . ?
C11C C12C C13C 120.2(10) . . ?
C11C C12C H12C 119.9 . . ?
C13C C12C H12C 119.9 . . ?
C8C C13C C12C 117.0(9) . . ?
C8C C13C P1C 114.6(7) . . ?
C12C C13C P1C 128.4(8) . . ?
C15C C14C C19C 115.4(9) . . ?
C15C C14C C7C 125.9(10) . . ?
C19C C14C C7C 118.5(10) . . ?
C16C C15C C14C 120.7(8) . . ?
C16C C15C H15C 119.7 . . ?
C14C C15C H15C 119.7 . . ?
C15C C16C C17C 121.9(10) . . ?
C15C C16C H16C 119.0 . . ?
C17C C16C H16C 119.0 . . ?
C18C C17C C16C 119.0(10) . . ?
C18C C17C H17C 120.5 . . ?
C16C C17C H17C 120.5 . . ?
C19C C18C C17C 117.2(8) . . ?
C19C C18C H18C 121.4 . . ?
C17C C18C H18C 121.4 . . ?
C18C C19C C14C 125.7(8) . . ?
C18C C19C P1C 123.3(7) . . ?
C14C C19C P1C 111.0(7) . . ?
O1E P1E C1E 122.9(17) . . ?
O1E P1E C19E 122.1(17) . . ?
C1E P1E C19E 98.0(15) . . ?
O1E P1E C13E 115.5(16) . . ?
C1E P1E C13E 94.2(15) . . ?
C19E P1E C13E 98.2(15) . . ?
C2E C1E C6E 121.1(19) . . ?
C2E C1E P1E 125(2) . . ?
C6E C1E P1E 113.5(16) . . ?
C3E C2E C1E 119(2) . . ?
C3E C2E H2E 120.4 . . ?
C1E C2E H2E 120.4 . . ?
C4E C3E C2E 120(3) . . ?
C4E C3E H3E 120.0 . . ?
C2E C3E H3E 120.0 . . ?
C3E C4E C5E 122(3) . . ?
C3E C4E H4E 119.1 . . ?
C5E C4E H4E 119.1 . . ?
C6E C5E C4E 120(2) . . ?
C6E C5E H5E 120.0 . . ?
C4E C5E H5E 120.0 . . ?
C5E C6E C1E 117.5(19) . . ?
C5E C6E C7E 123(2) . . ?
C1E C6E C7E 118.5(18) . . ?
C6E C7E C14E 107(2) . . ?
C6E C7E C8E 109(2) . . ?
C14E C7E C8E 105(2) . . ?
C6E C7E H7E 111.7 . . ?
C14E C7E H7E 111.7 . . ?
C8E C7E H7E 111.7 . . ?
C9E C8E C13E 120.6(19) . . ?
C9E C8E C7E 123(2) . . ?
C13E C8E C7E 115.0(19) . . ?
C8E C9E C10E 119(2) . . ?
C8E C9E H9E 120.4 . . ?
C10E C9E H9E 120.4 . . ?
C11E C10E C9E 121(2) . . ?
C11E C10E H10E 119.7 . . ?
C9E C10E H10E 119.7 . . ?
C10E C11E C12E 121(2) . . ?
C10E C11E H11E 119.3 . . ?
C12E C11E H11E 119.3 . . ?
C11E C12E C13E 119(2) . . ?
C11E C12E H12E 120.7 . . ?
C13E C12E H12E 120.7 . . ?
C8E C13E C12E 119.3(18) . . ?
C8E C13E P1E 115.8(16) . . ?
C12E C13E P1E 124.7(18) . . ?
C15E C14E C19E 120(2) . . ?
C15E C14E C7E 119(2) . . ?
C19E C14E C7E 117.9(19) . . ?
C16E C15E C14E 120(2) . . ?
C16E C15E H15E 120.0 . . ?
C14E C15E H15E 120.0 . . ?
C15E C16E C17E 119(2) . . ?
C15E C16E H16E 120.5 . . ?
C17E C16E H16E 120.5 . . ?
C16E C17E C18E 122(2) . . ?
C16E C17E H17E 119.1 . . ?
C18E C17E H17E 119.1 . . ?
C19E C18E C17E 119(2) . . ?
C19E C18E H18E 120.5 . . ?
C17E C18E H18E 120.5 . . ?
C18E C19E C14E 120(2) . . ?
C18E C19E P1E 124(2) . . ?
C14E C19E P1E 113.8(16) . . ?
O1A P1A C1A 118.93(11) . . ?
O1A P1A C13A 118.64(9) . . ?
C1A P1A C13A 98.77(13) . . ?
O1A P1A C19A 119.14(12) . . ?
C1A P1A C19A 98.84(16) . . ?
C13A P1A C19A 98.20(13) . . ?
C2A C1A C6A 121.0(3) . . ?
C2A C1A P1A 125.9(2) . . ?
C6A C1A P1A 113.1(2) . . ?
C3A C2A C1A 119.5(2) . . ?
C3A C2A H2A 120.3 . . ?
C1A C2A H2A 120.3 . . ?
C4A C3A C2A 120.6(3) . . ?
C4A C3A H3A 119.7 . . ?
C2A C3A H3A 119.7 . . ?
C3A C4A C5A 120.4(3) . . ?
C3A C4A H4A 119.8 . . ?
C5A C4A H4A 119.8 . . ?
C6A C5A C4A 120.0(3) . . ?
C6A C5A H5A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C5A C6A C1A 118.5(3) . . ?
C5A C6A C7A 123.9(3) . . ?
C1A C6A C7A 117.6(3) . . ?
C6A C7A C14A 110.4(3) . . ?
C6A C7A C8A 109.0(3) . . ?
C14A C7A C8A 105.3(3) . . ?
C6A C7A H7A 110.7 . . ?
C14A C7A H7A 110.7 . . ?
C8A C7A H7A 110.7 . . ?
C9A C8A C13A 119.5(2) . . ?
C9A C8A C7A 124.8(2) . . ?
C13A C8A C7A 115.8(2) . . ?
C8A C9A C10A 119.4(2) . . ?
C8A C9A H9A 120.3 . . ?
C10A C9A H9A 120.3 . . ?
C11A C10A C9A 121.3(2) . . ?
C11A C10A H10A 119.4 . . ?
C9A C10A H10A 119.4 . . ?
C12A C11A C10A 119.7(3) . . ?
C12A C11A H11A 120.2 . . ?
C10A C11A H11A 120.2 . . ?
C11A C12A C13A 119.6(2) . . ?
C11A C12A H12A 120.2 . . ?
C13A C12A H12A 120.2 . . ?
C12A C13A C8A 120.6(2) . . ?
C12A C13A P1A 126.40(18) . . ?
C8A C13A P1A 113.04(18) . . ?
C15A C14A C19A 119.5(3) . . ?
C15A C14A C7A 124.3(3) . . ?
C19A C14A C7A 116.2(3) . . ?
C14A C15A C16A 118.6(3) . . ?
C14A C15A H15A 120.7 . . ?
C16A C15A H15A 120.7 . . ?
C17A C16A C15A 121.7(3) . . ?
C17A C16A H16A 119.2 . . ?
C15A C16A H16A 119.2 . . ?
C16A C17A C18A 120.5(3) . . ?
C16A C17A H17A 119.7 . . ?
C18A C17A H17A 119.7 . . ?
C17A C18A C19A 118.6(3) . . ?
C17A C18A H18A 120.7 . . ?
C19A C18A H18A 120.7 . . ?
C18A C19A C14A 121.0(2) . . ?
C18A C19A P1A 126.1(2) . . ?
C14A C19A P1A 112.9(2) . . ?
O1D P1D C1D 111.0(10) . . ?
O1D P1D C13D 124.6(12) . . ?
C1D P1D C13D 98.6(12) . . ?
O1D P1D C19D 123.7(12) . . ?
C1D P1D C19D 94.3(13) . . ?
C13D P1D C19D 98.2(12) . . ?
C6D C1D C2D 126.4(17) . . ?
C6D C1D P1D 114.0(14) . . ?
C2D C1D P1D 119.6(15) . . ?
C3D C2D C1D 115.3(16) . . ?
C3D C2D H2D 122.4 . . ?
C1D C2D H2D 122.4 . . ?
C4D C3D C2D 122(2) . . ?
C4D C3D H3D 119.2 . . ?
C2D C3D H3D 119.2 . . ?
C3D C4D C5D 124(2) . . ?
C3D C4D H4D 118.2 . . ?
C5D C4D H4D 118.2 . . ?
C4D C5D C6D 114.9(17) . . ?
C4D C5D H5D 122.5 . . ?
C6D C5D H5D 122.5 . . ?
C1D C6D C5D 117.4(15) . . ?
C1D C6D C7D 123.1(16) . . ?
C5D C6D C7D 119.5(15) . . ?
C6D C7D C14D 110.8(15) . . ?
C6D C7D C8D 106.9(13) . . ?
C14D C7D C8D 94.5(13) . . ?
C6D C7D H7D 114.3 . . ?
C14D C7D H7D 114.3 . . ?
C8D C7D H7D 114.3 . . ?
C13D C8D C9D 109.9(13) . . ?
C13D C8D C7D 117.3(12) . . ?
C9D C8D C7D 131.0(13) . . ?
C10D C9D C8D 121.7(18) . . ?
C10D C9D H9D 119.1 . . ?
C8D C9D H9D 119.1 . . ?
C11D C10D C9D 124.9(19) . . ?
C11D C10D H10D 117.6 . . ?
C9D C10D H10D 117.6 . . ?
C12D C11D C10D 117.7(19) . . ?
C12D C11D H11D 121.2 . . ?
C10D C11D H11D 121.2 . . ?
C11D C12D C13D 116.5(17) . . ?
C11D C12D H12D 121.8 . . ?
C13D C12D H12D 121.8 . . ?
C8D C13D C12D 128.8(14) . . ?
C8D C13D P1D 114.4(11) . . ?
C12D C13D P1D 116.7(13) . . ?
C15D C14D C19D 110.6(16) . . ?
C15D C14D C7D 132.5(17) . . ?
C19D C14D C7D 116.0(15) . . ?
C16D C15D C14D 126(2) . . ?
C16D C15D H15D 116.9 . . ?
C14D C15D H15D 116.9 . . ?
C17D C16D C15D 121(2) . . ?
C17D C16D H16D 119.5 . . ?
C15D C16D H16D 119.5 . . ?
C16D C17D C18D 118(2) . . ?
C16D C17D H17D 121.1 . . ?
C18D C17D H17D 121.1 . . ?
C17D C18D C19D 119.8(18) . . ?
C17D C18D H18D 120.1 . . ?
C19D C18D H18D 120.1 . . ?
C14D C19D C18D 124.5(16) . . ?
C14D C19D P1D 114.3(15) . . ?
C18D C19D P1D 120.4(15) . . ?

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
O1B P1B C1B C2B 0.3(8) . . . . ?
C19B P1B C1B C2B -129.7(7) . . . . ?
C13B P1B C1B C2B 130.8(7) . . . . ?
O1B P1B C1B C6B 179.7(6) . . . . ?
C19B P1B C1B C6B 49.7(7) . . . . ?
C13B P1B C1B C6B -49.8(7) . . . . ?
C6B C1B C2B C3B 2.2(12) . . . . ?
P1B C1B C2B C3B -178.4(7) . . . . ?
C1B C2B C3B C4B -1.9(14) . . . . ?
C2B C3B C4B C5B 1.4(15) . . . . ?
C3B C4B C5B C6B -1.2(13) . . . . ?
C4B C5B C6B C1B 1.5(14) . . . . ?
C4B C5B C6B C7B -179.8(9) . . . . ?
C2B C1B C6B C5B -2.0(14) . . . . ?
P1B C1B C6B C5B 178.5(7) . . . . ?
C2B C1B C6B C7B 179.1(7) . . . . ?
P1B C1B C6B C7B -0.3(11) . . . . ?
C5B C6B C7B C14B 122.0(10) . . . . ?
C1B C6B C7B C14B -59.2(11) . . . . ?
C5B C6B C7B C8B -120.0(11) . . . . ?
C1B C6B C7B C8B 58.8(11) . . . . ?
C6B C7B C8B C9B 118.8(11) . . . . ?
C14B C7B C8B C9B -122.3(11) . . . . ?
C6B C7B C8B C13B -57.5(11) . . . . ?
C14B C7B C8B C13B 61.5(11) . . . . ?
C13B C8B C9B C10B -2.1(15) . . . . ?
C7B C8B C9B C10B -178.3(9) . . . . ?
C8B C9B C10B C11B 2.4(16) . . . . ?
C9B C10B C11B C12B -2.5(18) . . . . ?
C10B C11B C12B C13B 2.2(15) . . . . ?
C11B C12B C13B C8B -2.0(12) . . . . ?
C11B C12B C13B P1B 179.0(7) . . . . ?
C9B C8B C13B C12B 2.0(14) . . . . ?
C7B C8B C13B C12B 178.5(8) . . . . ?
C9B C8B C13B P1B -179.0(8) . . . . ?
C7B C8B C13B P1B -2.5(11) . . . . ?
O1B P1B C13B C12B 0.1(7) . . . . ?
C19B P1B C13B C12B 130.3(7) . . . . ?
C1B P1B C13B C12B -130.3(7) . . . . ?
O1B P1B C13B C8B -178.9(6) . . . . ?
C19B P1B C13B C8B -48.8(7) . . . . ?
C1B P1B C13B C8B 50.7(7) . . . . ?
C6B C7B C14B C15B -117.0(12) . . . . ?
C8B C7B C14B C15B 123.4(12) . . . . ?
C6B C7B C14B C19B 60.4(13) . . . . ?
C8B C7B C14B C19B -59.2(12) . . . . ?
C19B C14B C15B C16B -3.0(17) . . . . ?
C7B C14B C15B C16B 174.3(10) . . . . ?
C14B C15B C16B C17B 2.9(14) . . . . ?
C15B C16B C17B C18B -1.8(13) . . . . ?
C16B C17B C18B C19B 0.7(12) . . . . ?
C17B C18B C19B C14B -0.6(13) . . . . ?
C17B C18B C19B P1B -174.4(8) . . . . ?
C15B C14B C19B C18B 1.8(17) . . . . ?
C7B C14B C19B C18B -175.6(9) . . . . ?
C15B C14B C19B P1B 176.5(10) . . . . ?
C7B C14B C19B P1B -0.9(14) . . . . ?
O1B P1B C19B C18B -4.5(10) . . . . ?
C13B P1B C19B C18B -134.8(8) . . . . ?
C1B P1B C19B C18B 125.4(8) . . . . ?
O1B P1B C19B C14B -178.7(8) . . . . ?
C13B P1B C19B C14B 51.1(9) . . . . ?
C1B P1B C19B C14B -48.7(9) . . . . ?
O1C P1C C1C C6C -178.9(9) . . . . ?
C13C P1C C1C C6C -52.1(11) . . . . ?
C19C P1C C1C C6C 49.7(11) . . . . ?
O1C P1C C1C C2C -0.9(12) . . . . ?
C13C P1C C1C C2C 125.9(11) . . . . ?
C19C P1C C1C C2C -132.4(11) . . . . ?
C6C C1C C2C C3C -1.6(18) . . . . ?
P1C C1C C2C C3C -179.4(10) . . . . ?
C1C C2C C3C C4C 0(2) . . . . ?
C2C C3C C4C C5C -1(3) . . . . ?
C3C C4C C5C C6C 4(3) . . . . ?
C2C C1C C6C C5C 4(2) . . . . ?
P1C C1C C6C C5C -177.4(12) . . . . ?
C2C C1C C6C C7C -176.8(11) . . . . ?
P1C C1C C6C C7C 1.3(17) . . . . ?
C4C C5C C6C C1C -6(2) . . . . ?
C4C C5C C6C C7C 175.7(16) . . . . ?
C1C C6C C7C C14C -58.5(16) . . . . ?
C5C C6C C7C C14C 120.3(17) . . . . ?
C1C C6C C7C C8C 58.4(16) . . . . ?
C5C C6C C7C C8C -122.9(16) . . . . ?
C6C C7C C8C C9C 128.6(17) . . . . ?
C14C C7C C8C C9C -115.4(18) . . . . ?
C6C C7C C8C C13C -56.5(17) . . . . ?
C14C C7C C8C C13C 59.5(17) . . . . ?
C13C C8C C9C C10C 7(3) . . . . ?
C7C C8C C9C C10C -178.1(14) . . . . ?
C8C C9C C10C C11C -3(2) . . . . ?
C9C C10C C11C C12C -3(2) . . . . ?
C10C C11C C12C C13C 4(2) . . . . ?
C9C C8C C13C C12C -6(2) . . . . ?
C7C C8C C13C C12C 179.2(13) . . . . ?
C9C C8C C13C P1C 172.2(14) . . . . ?
C7C C8C C13C P1C -3(2) . . . . ?
C11C C12C C13C C8C 0(2) . . . . ?
C11C C12C C13C P1C -177.6(14) . . . . ?
O1C P1C C13C C8C 178.9(11) . . . . ?
C1C P1C C13C C8C 53.2(14) . . . . ?
C19C P1C C13C C8C -47.9(14) . . . . ?
O1C P1C C13C C12C -3.3(17) . . . . ?
C1C P1C C13C C12C -129.1(15) . . . . ?
C19C P1C C13C C12C 129.9(14) . . . . ?
C6C C7C C14C C15C -117(2) . . . . ?
C8C C7C C14C C15C 127(2) . . . . ?
C6C C7C C14C C19C 57(2) . . . . ?
C8C C7C C14C C19C -59(2) . . . . ?
C19C C14C C15C C16C 3(3) . . . . ?
C7C C14C C15C C16C 177.5(16) . . . . ?
C14C C15C C16C C17C 0(3) . . . . ?
C15C C16C C17C C18C -3(3) . . . . ?
C16C C17C C18C C19C 2(2) . . . . ?
C17C C18C C19C C14C 1(2) . . . . ?
C17C C18C C19C P1C -177.7(11) . . . . ?
C15C C14C C19C C18C -4(3) . . . . ?
C7C C14C C19C C18C -178.8(13) . . . . ?
C15C C14C C19C P1C 175.5(14) . . . . ?
C7C C14C C19C P1C 0(2) . . . . ?
O1C P1C C19C C18C -0.3(13) . . . . ?
C1C P1C C19C C18C 129.0(10) . . . . ?
C13C P1C C19C C18C -132.4(11) . . . . ?
O1C P1C C19C C14C -179.3(12) . . . . ?
C1C P1C C19C C14C -50.0(13) . . . . ?
C13C P1C C19C C14C 48.6(14) . . . . ?
O1E P1E C1E C2E -13(5) . . . . ?
C19E P1E C1E C2E 124(4) . . . . ?
C13E P1E C1E C2E -137(4) . . . . ?
O1E P1E C1E C6E 173(3) . . . . ?
C19E P1E C1E C6E -50(3) . . . . ?
C13E P1E C1E C6E 49(3) . . . . ?
C6E C1E C2E C3E 1(3) . . . . ?
P1E C1E C2E C3E -172(4) . . . . ?
C1E C2E C3E C4E 0(3) . . . . ?
C2E C3E C4E C5E 1(6) . . . . ?
C3E C4E C5E C6E -4(8) . . . . ?
C4E C5E C6E C1E 5(7) . . . . ?
C4E C5E C6E C7E 173(5) . . . . ?
C2E C1E C6E C5E -4(5) . . . . ?
P1E C1E C6E C5E 170(4) . . . . ?
C2E C1E C6E C7E -172(4) . . . . ?
P1E C1E C6E C7E 2(5) . . . . ?
C5E C6E C7E C14E -112(5) . . . . ?
C1E C6E C7E C14E 56(4) . . . . ?
C5E C6E C7E C8E 134(4) . . . . ?
C1E C6E C7E C8E -58(4) . . . . ?
C6E C7E C8E C9E -120(4) . . . . ?
C14E C7E C8E C9E 125(3) . . . . ?
C6E C7E C8E C13E 48(4) . . . . ?
C14E C7E C8E C13E -67(4) . . . . ?
C13E C8E C9E C10E -3(3) . . . . ?
C7E C8E C9E C10E 164(5) . . . . ?
C8E C9E C10E C11E -2(3) . . . . ?
C9E C10E C11E C12E 4(7) . . . . ?
C10E C11E C12E C13E -1(8) . . . . ?
C9E C8E C13E C12E 6(5) . . . . ?
C7E C8E C13E C12E -162(4) . . . . ?
C9E C8E C13E P1E -178(3) . . . . ?
C7E C8E C13E P1E 14(5) . . . . ?
C11E C12E C13E C8E -4(7) . . . . ?
C11E C12E C13E P1E -180(5) . . . . ?
O1E P1E C13E C8E 172(3) . . . . ?
C1E P1E C13E C8E -59(3) . . . . ?
C19E P1E C13E C8E 40(3) . . . . ?
O1E P1E C13E C12E -12(5) . . . . ?
C1E P1E C13E C12E 117(4) . . . . ?
C19E P1E C13E C12E -144(4) . . . . ?
C6E C7E C14E C15E 141(3) . . . . ?
C8E C7E C14E C15E -103(3) . . . . ?
C6E C7E C14E C19E -59(4) . . . . ?
C8E C7E C14E C19E 57(4) . . . . ?
C19E C14E C15E C16E 1(3) . . . . ?
C7E C14E C15E C16E 161(4) . . . . ?
C14E C15E C16E C17E 1(3) . . . . ?
C15E C16E C17E C18E -3(5) . . . . ?
C16E C17E C18E C19E 2(7) . . . . ?
C17E C18E C19E C14E 1(7) . . . . ?
C17E C18E C19E P1E -163(4) . . . . ?
C15E C14E C19E C18E -2(5) . . . . ?
C7E C14E C19E C18E -162(5) . . . . ?
C15E C14E C19E P1E 164(3) . . . . ?
C7E C14E C19E P1E 3(5) . . . . ?
O1E P1E C19E C18E -11(5) . . . . ?
C1E P1E C19E C18E -148(5) . . . . ?
C13E P1E C19E C18E 116(5) . . . . ?
O1E P1E C19E C14E -176(3) . . . . ?
C1E P1E C19E C14E 47(4) . . . . ?
C13E P1E C19E C14E -49(4) . . . . ?
O1A P1A C1A C2A 0.6(4) . . . . ?
C13A P1A C1A C2A 130.4(3) . . . . ?
C19A P1A C1A C2A -129.8(4) . . . . ?
O1A P1A C1A C6A 179.4(2) . . . . ?
C13A P1A C1A C6A -50.9(3) . . . . ?
C19A P1A C1A C6A 48.9(3) . . . . ?
C6A C1A C2A C3A -2.0(6) . . . . ?
P1A C1A C2A C3A 176.7(3) . . . . ?
C1A C2A C3A C4A 1.3(5) . . . . ?
C2A C3A C4A C5A 0.6(5) . . . . ?
C3A C4A C5A C6A -1.8(4) . . . . ?
C4A C5A C6A C1A 1.1(4) . . . . ?
C4A C5A C6A C7A -177.5(4) . . . . ?
C2A C1A C6A C5A 0.8(5) . . . . ?
P1A C1A C6A C5A -178.1(3) . . . . ?
C2A C1A C6A C7A 179.5(4) . . . . ?
P1A C1A C6A C7A 0.6(5) . . . . ?
C5A C6A C7A C14A 120.7(4) . . . . ?
C1A C6A C7A C14A -57.9(5) . . . . ?
C5A C6A C7A C8A -124.1(3) . . . . ?
C1A C6A C7A C8A 57.3(5) . . . . ?
C6A C7A C8A C9A 123.7(4) . . . . ?
C14A C7A C8A C9A -117.9(4) . . . . ?
C6A C7A C8A C13A -55.9(4) . . . . ?
C14A C7A C8A C13A 62.5(4) . . . . ?
C13A C8A C9A C10A 1.5(5) . . . . ?
C7A C8A C9A C10A -178.1(3) . . . . ?
C8A C9A C10A C11A 0.5(4) . . . . ?
C9A C10A C11A C12A -2.3(5) . . . . ?
C10A C11A C12A C13A 2.1(5) . . . . ?
C11A C12A C13A C8A -0.2(4) . . . . ?
C11A C12A C13A P1A 179.9(3) . . . . ?
C9A C8A C13A C12A -1.7(4) . . . . ?
C7A C8A C13A C12A 177.9(3) . . . . ?
C9A C8A C13A P1A 178.3(2) . . . . ?
C7A C8A C13A P1A -2.1(4) . . . . ?
O1A P1A C13A C12A 0.9(3) . . . . ?
C1A P1A C13A C12A -129.0(3) . . . . ?
C19A P1A C13A C12A 130.7(3) . . . . ?
O1A P1A C13A C8A -179.05(19) . . . . ?
C1A P1A C13A C8A 51.0(2) . . . . ?
C19A P1A C13A C8A -49.3(2) . . . . ?
C6A C7A C14A C15A -124.6(5) . . . . ?
C8A C7A C14A C15A 117.9(5) . . . . ?
C6A C7A C14A C19A 54.1(5) . . . . ?
C8A C7A C14A C19A -63.4(5) . . . . ?
C19A C14A C15A C16A -0.7(8) . . . . ?
C7A C14A C15A C16A 178.0(5) . . . . ?
C14A C15A C16A C17A -1.1(8) . . . . ?
C15A C16A C17A C18A 1.6(7) . . . . ?
C16A C17A C18A C19A -0.2(5) . . . . ?
C17A C18A C19A C14A -1.6(4) . . . . ?
C17A C18A C19A P1A 177.5(3) . . . . ?
C15A C14A C19A C18A 2.1(6) . . . . ?
C7A C14A C19A C18A -176.7(4) . . . . ?
C15A C14A C19A P1A -177.1(4) . . . . ?
C7A C14A C19A P1A 4.1(5) . . . . ?
O1A P1A C19A C18A -0.9(4) . . . . ?
C1A P1A C19A C18A 129.4(3) . . . . ?
C13A P1A C19A C18A -130.3(3) . . . . ?
O1A P1A C19A C14A 178.2(3) . . . . ?
C1A P1A C19A C14A -51.4(3) . . . . ?
C13A P1A C19A C14A 48.8(3) . . . . ?
O1D P1D C1D C6D -179(2) . . . . ?
C13D P1D C1D C6D 49(2) . . . . ?
C19D P1D C1D C6D -50(2) . . . . ?
O1D P1D C1D C2D 3(2) . . . . ?
C13D P1D C1D C2D -129.1(19) . . . . ?
C19D P1D C1D C2D 132(2) . . . . ?
C6D C1D C2D C3D 0(3) . . . . ?
P1D C1D C2D C3D 178(2) . . . . ?
C1D C2D C3D C4D -3(2) . . . . ?
C2D C3D C4D C5D 9(4) . . . . ?
C3D C4D C5D C6D -11(4) . . . . ?
C2D C1D C6D C5D -3(4) . . . . ?
P1D C1D C6D C5D 179(2) . . . . ?
C2D C1D C6D C7D 179(2) . . . . ?
P1D C1D C6D C7D 1(4) . . . . ?
C4D C5D C6D C1D 8(4) . . . . ?
C4D C5D C6D C7D -174(2) . . . . ?
C1D C6D C7D C14D 49(3) . . . . ?
C5D C6D C7D C14D -129(2) . . . . ?
C1D C6D C7D C8D -52(3) . . . . ?
C5D C6D C7D C8D 130(2) . . . . ?
C6D C7D C8D C13D 45(2) . . . . ?
C14D C7D C8D C13D -68.4(19) . . . . ?
C6D C7D C8D C9D -118.1(19) . . . . ?
C14D C7D C8D C9D 128.6(18) . . . . ?
C13D C8D C9D C10D 2.6(16) . . . . ?
C7D C8D C9D C10D 166.5(18) . . . . ?
C8D C9D C10D C11D 3(2) . . . . ?
C9D C10D C11D C12D -8(4) . . . . ?
C10D C11D C12D C13D 6(4) . . . . ?
C9D C8D C13D C12D -4(3) . . . . ?
C7D C8D C13D C12D -170(2) . . . . ?
C9D C8D C13D P1D 175.1(15) . . . . ?
C7D C8D C13D P1D 9(2) . . . . ?
C11D C12D C13D C8D -1(4) . . . . ?
C11D C12D C13D P1D -180(2) . . . . ?
O1D P1D C13D C8D -175.7(15) . . . . ?
C1D P1D C13D C8D -52.7(19) . . . . ?
C19D P1D C13D C8D 43(2) . . . . ?
O1D P1D C13D C12D 3(3) . . . . ?
C1D P1D C13D C12D 126(2) . . . . ?
C19D P1D C13D C12D -138(2) . . . . ?
C6D C7D C14D C15D 132(3) . . . . ?
C8D C7D C14D C15D -118(2) . . . . ?
C6D C7D C14D C19D -35(3) . . . . ?
C8D C7D C14D C19D 75(2) . . . . ?
C19D C14D C15D C16D 1(2) . . . . ?
C7D C14D C15D C16D -167(3) . . . . ?
C14D C15D C16D C17D 2(3) . . . . ?
C15D C16D C17D C18D -6(5) . . . . ?
C16D C17D C18D C19D 6(6) . . . . ?
C15D C14D C19D C18D -1(4) . . . . ?
C7D C14D C19D C18D 169(3) . . . . ?
C15D C14D C19D P1D 168(2) . . . . ?
C7D C14D C19D P1D -22(3) . . . . ?
C17D C18D C19D C14D -2(6) . . . . ?
C17D C18D C19D P1D -171(3) . . . . ?
O1D P1D C19D C14D -180(2) . . . . ?
C1D P1D C19D C14D 61(3) . . . . ?
C13D P1D C19D C14D -38(3) . . . . ?
O1D P1D C19D C18D -10(4) . . . . ?
C1D P1D C19D C18D -129(3) . . . . ?
C13D P1D C19D C18D 132(3) . . . . ?

_refine_diff_density_max         0.182
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.027




# start Validation Reply Form
_vrf_PLAT088_nt0284_LeiHu_73B    
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.66 Note  
RESPONSE: Whole structure is disordered.
;
_vrf_PLAT260_nt0284_LeiHu_73B    
;
PROBLEM: Large Average Ueq of Residue Including       O2A      0.161 Check 
RESPONSE: Disordered (over at least 3 positions) water molecule.

;
_vrf_PLAT911_nt0284_LeiHu_73B    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.598         27 Report
RESPONSE: These reflections are missing in the highest and lowest resolution
 shells because of the instrument geometry limitations.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1278_SMC103
_database_code_depnum_ccdc_archive 'CCDC 2313763'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        'phosphatriptycene sulfide'
_chemical_name_common            'phosphatriptycene sulfide'
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 P S'
_chemical_formula_sum            'C19 H13 P S'
_chemical_formula_weight         304.32

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'
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           15
_space_group_name_H-M_alt        'C 2/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'
'-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                   14.2480(3)
_cell_length_b                   13.5359(3)
_cell_length_c                   15.8127(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.7720(10)
_cell_angle_gamma                90
_cell_volume                     3049.35(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    9939
_cell_measurement_theta_min      4.5059
_cell_measurement_theta_max      66.7431

_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             1264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.045
_exptl_absorpt_coefficient_mu    2.772
_shelx_estimated_absorpt_T_min   0.715
_shelx_estimated_absorpt_T_max   0.885
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            22816
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.506
_diffrn_reflns_theta_max         66.738
_diffrn_reflns_theta_full        66.738
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2701
_reflns_number_gt                2431
_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/4 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0398P)²+2.6173P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2701
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0934
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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
S1 S 0.39274(4) 0.25784(4) 0.86991(4) 0.06357(18) Uani 1 1 d . . . . .
P1 P 0.33445(3) 0.37415(3) 0.82071(3) 0.04012(15) Uani 1 1 d . . . . .
C1 C 0.31706(12) 0.38028(13) 0.70738(10) 0.0417(4) Uani 1 1 d . . . . .
C2 C 0.34510(15) 0.30984(15) 0.64982(12) 0.0539(5) Uani 1 1 d . . . . .
H2 H 0.375731 0.252817 0.667940 0.065 Uiso 1 1 calc R U . . .
C3 C 0.32674(17) 0.3257(2) 0.56427(13) 0.0689(7) Uani 1 1 d . . . . .
H3 H 0.345189 0.278855 0.524773 0.083 Uiso 1 1 calc R U . . .
C4 C 0.28161(18) 0.4098(2) 0.53787(13) 0.0717(7) Uani 1 1 d . . . . .
H4 H 0.269276 0.419247 0.480534 0.086 Uiso 1 1 calc R U . . .
C5 C 0.25411(16) 0.48103(18) 0.59539(12) 0.0602(5) Uani 1 1 d . . . . .
H5 H 0.223746 0.537982 0.576739 0.072 Uiso 1 1 calc R U . . .
C6 C 0.27212(13) 0.46688(14) 0.68090(11) 0.0444(4) Uani 1 1 d . . . . .
C7 C 0.24638(13) 0.54104(13) 0.74929(12) 0.0450(4) Uani 1 1 d . . . . .
H7 H 0.215972 0.599335 0.724423 0.054 Uiso 1 1 calc R U . . .
C8 C 0.33595(12) 0.56997(13) 0.79728(11) 0.0429(4) Uani 1 1 d . . . . .
C9 C 0.36755(15) 0.66623(15) 0.80449(14) 0.0561(5) Uani 1 1 d . . . . .
H9 H 0.334216 0.717575 0.779081 0.067 Uiso 1 1 calc R U . . .
C10 C 0.44935(16) 0.68545(18) 0.84992(16) 0.0677(6) Uani 1 1 d . . . . .
H10 H 0.470790 0.750143 0.854605 0.081 Uiso 1 1 calc R U . . .
C11 C 0.49922(15) 0.61085(19) 0.88807(15) 0.0673(6) Uani 1 1 d . . . . .
H11 H 0.553793 0.625362 0.918509 0.081 Uiso 1 1 calc R U . . .
C12 C 0.46880(14) 0.51389(16) 0.88156(12) 0.0533(5) Uani 1 1 d . . . . .
H12 H 0.502628 0.463006 0.907119 0.064 Uiso 1 1 calc R U . . .
C13 C 0.38720(12) 0.49422(13) 0.83634(11) 0.0412(4) Uani 1 1 d . . . . .
C14 C 0.18148(12) 0.49013(13) 0.81184(11) 0.0433(4) Uani 1 1 d . . . . .
C15 C 0.09231(14) 0.52319(16) 0.83089(13) 0.0554(5) Uani 1 1 d . . . . .
H15 H 0.067472 0.578535 0.803868 0.067 Uiso 1 1 calc R U . . .
C16 C 0.04011(15) 0.4726(2) 0.89101(15) 0.0661(6) Uani 1 1 d . . . . .
H16 H -0.019874 0.494636 0.903857 0.079 Uiso 1 1 calc R U . . .
C17 C 0.07580(16) 0.39107(18) 0.93147(13) 0.0626(6) Uani 1 1 d . . . . .
H17 H 0.040342 0.358872 0.972010 0.075 Uiso 1 1 calc R U . . .
C18 C 0.16424(14) 0.35645(15) 0.91229(11) 0.0522(5) Uani 1 1 d . . . . .
H18 H 0.188260 0.300682 0.939253 0.063 Uiso 1 1 calc R U . . .
C19 C 0.21671(12) 0.40580(13) 0.85243(10) 0.0423(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
S1 P1 1.9380(7) . ?
P1 C13 1.8062(18) . ?
P1 C1 1.8077(17) . ?
P1 C19 1.8089(19) . ?
C1 C2 1.381(3) . ?
C1 C6 1.397(3) . ?
C2 C3 1.391(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.370(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.524(3) . ?
C7 C8 1.527(3) . ?
C7 C14 1.527(2) . ?
C7 H7 0.9800 . ?
C8 C9 1.383(3) . ?
C8 C13 1.398(3) . ?
C9 C10 1.386(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.370(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.385(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.383(3) . ?
C12 H12 0.9300 . ?
C14 C15 1.384(3) . ?
C14 C19 1.399(3) . ?
C15 C16 1.394(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.371(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.382(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.386(3) . ?
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
C13 P1 C1 98.37(8) . . ?
C13 P1 C19 97.74(8) . . ?
C1 P1 C19 98.56(8) . . ?
C13 P1 S1 120.05(6) . . ?
C1 P1 S1 119.18(6) . . ?
C19 P1 S1 118.36(6) . . ?
C2 C1 C6 121.15(17) . . ?
C2 C1 P1 125.78(15) . . ?
C6 C1 P1 113.06(13) . . ?
C1 C2 C3 118.8(2) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 120.4(2) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.93(19) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 119.6(2) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 119.09(18) . . ?
C5 C6 C7 123.92(18) . . ?
C1 C6 C7 116.98(15) . . ?
C6 C7 C8 108.31(15) . . ?
C6 C7 C14 108.41(14) . . ?
C8 C7 C14 107.64(14) . . ?
C6 C7 H7 110.8 . . ?
C8 C7 H7 110.8 . . ?
C14 C7 H7 110.8 . . ?
C9 C8 C13 119.16(17) . . ?
C9 C8 C7 123.48(17) . . ?
C13 C8 C7 117.36(15) . . ?
C8 C9 C10 119.4(2) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 121.2(2) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 120.4(2) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C13 C12 C11 118.7(2) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C8 121.19(17) . . ?
C12 C13 P1 126.12(15) . . ?
C8 C13 P1 112.69(13) . . ?
C15 C14 C19 119.25(17) . . ?
C15 C14 C7 124.09(17) . . ?
C19 C14 C7 116.65(16) . . ?
C14 C15 C16 119.3(2) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C17 C16 C15 121.0(2) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 120.30(19) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C19 119.2(2) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C18 C19 C14 120.86(18) . . ?
C18 C19 P1 125.89(16) . . ?
C14 C19 P1 113.22(13) . . ?

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
C13 P1 C1 C2 128.79(16) . . . . ?
C19 P1 C1 C2 -132.01(17) . . . . ?
S1 P1 C1 C2 -2.65(19) . . . . ?
C13 P1 C1 C6 -50.19(14) . . . . ?
C19 P1 C1 C6 49.00(14) . . . . ?
S1 P1 C1 C6 178.37(10) . . . . ?
C6 C1 C2 C3 -0.9(3) . . . . ?
P1 C1 C2 C3 -179.78(15) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C2 C3 C4 C5 0.5(3) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C4 C5 C6 C1 -0.6(3) . . . . ?
C4 C5 C6 C7 178.97(19) . . . . ?
C2 C1 C6 C5 1.2(3) . . . . ?
P1 C1 C6 C5 -179.81(14) . . . . ?
C2 C1 C6 C7 -178.43(16) . . . . ?
P1 C1 C6 C7 0.6(2) . . . . ?
C5 C6 C7 C8 -121.92(19) . . . . ?
C1 C6 C7 C8 57.64(19) . . . . ?
C5 C6 C7 C14 121.55(19) . . . . ?
C1 C6 C7 C14 -58.9(2) . . . . ?
C6 C7 C8 C9 122.43(18) . . . . ?
C14 C7 C8 C9 -120.54(19) . . . . ?
C6 C7 C8 C13 -58.3(2) . . . . ?
C14 C7 C8 C13 58.7(2) . . . . ?
C13 C8 C9 C10 0.2(3) . . . . ?
C7 C8 C9 C10 179.50(18) . . . . ?
C8 C9 C10 C11 -0.3(3) . . . . ?
C9 C10 C11 C12 0.3(3) . . . . ?
C10 C11 C12 C13 -0.3(3) . . . . ?
C11 C12 C13 C8 0.3(3) . . . . ?
C11 C12 C13 P1 -179.37(15) . . . . ?
C9 C8 C13 C12 -0.3(3) . . . . ?
C7 C8 C13 C12 -179.58(17) . . . . ?
C9 C8 C13 P1 179.46(14) . . . . ?
C7 C8 C13 P1 0.1(2) . . . . ?
C1 P1 C13 C12 -130.70(17) . . . . ?
C19 P1 C13 C12 129.41(17) . . . . ?
S1 P1 C13 C12 0.18(19) . . . . ?
C1 P1 C13 C8 49.59(14) . . . . ?
C19 P1 C13 C8 -50.30(14) . . . . ?
S1 P1 C13 C8 -179.53(10) . . . . ?
C6 C7 C14 C15 -122.38(19) . . . . ?
C8 C7 C14 C15 120.67(19) . . . . ?
C6 C7 C14 C19 58.6(2) . . . . ?
C8 C7 C14 C19 -58.4(2) . . . . ?
C19 C14 C15 C16 1.0(3) . . . . ?
C7 C14 C15 C16 -178.03(17) . . . . ?
C14 C15 C16 C17 0.1(3) . . . . ?
C15 C16 C17 C18 -1.0(3) . . . . ?
C16 C17 C18 C19 0.7(3) . . . . ?
C17 C18 C19 C14 0.4(3) . . . . ?
C17 C18 C19 P1 178.31(14) . . . . ?
C15 C14 C19 C18 -1.2(3) . . . . ?
C7 C14 C19 C18 177.85(16) . . . . ?
C15 C14 C19 P1 -179.39(14) . . . . ?
C7 C14 C19 P1 -0.33(19) . . . . ?
C13 P1 C19 C18 -127.49(16) . . . . ?
C1 P1 C19 C18 132.78(16) . . . . ?
S1 P1 C19 C18 2.87(18) . . . . ?
C13 P1 C19 C14 50.58(14) . . . . ?
C1 P1 C19 C14 -49.16(14) . . . . ?
S1 P1 C19 C14 -179.06(10) . . . . ?

_refine_diff_density_max         0.281
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.038



# start Validation Reply Form
_vrf_PLAT911_nt1278_SMC103       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.596          5 Report
RESPONSE: These reflections are missing because of the instrument geometry 
limitations.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt0756_LHG159
_database_code_depnum_ccdc_archive 'CCDC 2313767'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
N-(10H-5λ⁵-5,10-[1,2]benzenoacridophosphin-5-ylidene)pivalamide
_chemical_name_common            
N-(10H-5λ⁵-5,10-[1,2]benzenoacridophosphin-5-ylidene)pivalamide
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 N O P'
_chemical_formula_sum            'C24 H22 N O P'
_chemical_formula_weight         371.39

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'
N N 0.0311 0.0180 '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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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                   17.31590(19)
_cell_length_b                   9.40206(10)
_cell_length_c                   12.48870(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2033.23(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    6185
_cell_measurement_theta_min      5.3210
_cell_measurement_theta_max      67.0330

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_F_000             784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.036
_exptl_absorpt_coefficient_mu    1.284
_shelx_estimated_absorpt_T_min   0.566
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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            9451
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         5.354
_diffrn_reflns_theta_max         67.062
_diffrn_reflns_theta_full        67.062
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_point_group_measured_fraction_full 0.868
_reflns_number_total             3147
_reflns_number_gt                3017
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.661
_reflns_Friedel_fraction_max     0.727
_reflns_Friedel_fraction_full    0.727

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0643P)²+0.1719P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.32(3)
_chemical_absolute_configuration .
_refine_ls_number_reflns         3147
_refine_ls_number_parameters     248
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0953
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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 0.58105(3) 0.72012(6) 0.49479(5) 0.0429(2) Uani 1 1 d . . . . .
N1 N 0.62334(12) 0.8361(2) 0.56834(18) 0.0477(5) Uani 1 1 d . . . . .
O1 O 0.57951(17) 0.7116(3) 0.7122(2) 0.0821(9) Uani 1 1 d . . . . .
C7 C 0.51257(18) 0.5348(3) 0.3482(3) 0.0592(7) Uani 1 1 d . . . . .
H7 H 0.488476 0.470048 0.296627 0.071 Uiso 1 1 calc R U . . .
C8 C 0.56865(17) 0.4546(3) 0.4202(3) 0.0561(7) Uani 1 1 d . . . . .
C14 C 0.45141(17) 0.6054(3) 0.4182(3) 0.0543(6) Uani 1 1 d . . . . .
C2 C 0.63446(18) 0.8647(4) 0.3086(3) 0.0617(8) Uani 1 1 d . . . . .
H2 H 0.658583 0.932556 0.351291 0.074 Uiso 1 1 calc R U . . .
C13 C 0.60775(15) 0.5350(3) 0.4985(3) 0.0507(5) Uani 1 1 d . . . . .
C19 C 0.47744(14) 0.7017(3) 0.4957(3) 0.0499(5) Uani 1 1 d . . . . .
C4 C 0.6026(3) 0.7720(6) 0.1350(3) 0.0958(14) Uani 1 1 d . . . . .
H4 H 0.606052 0.778475 0.060870 0.115 Uiso 1 1 calc R U . . .
C6 C 0.55685(18) 0.6510(4) 0.2907(2) 0.0573(7) Uani 1 1 d . . . . .
C21 C 0.6457(2) 0.9296(4) 0.7506(3) 0.0635(8) Uani 1 1 d . . . . .
C3 C 0.6382(2) 0.8738(5) 0.1980(3) 0.0827(11) Uani 1 1 d . . . . .
H3 H 0.664713 0.948559 0.165907 0.099 Uiso 1 1 calc R U . . .
C9 C 0.5819(2) 0.3098(4) 0.4147(4) 0.0759(10) Uani 1 1 d . . . . .
H9 H 0.556461 0.254907 0.363820 0.091 Uiso 1 1 calc R U . . .
C23 C 0.7221(2) 0.9911(4) 0.7122(4) 0.0804(10) Uani 1 1 d . . . . .
H23A H 0.716335 1.025513 0.640242 0.121 Uiso 1 1 calc R U . . .
H23B H 0.761018 0.918466 0.713891 0.121 Uiso 1 1 calc R U . . .
H23C H 0.737086 1.068147 0.758137 0.121 Uiso 1 1 calc R U . . .
C1 C 0.59432(17) 0.7534(3) 0.3545(3) 0.0513(6) Uani 1 1 d . . . . .
C15 C 0.37313(19) 0.5805(4) 0.4088(3) 0.0714(9) Uani 1 1 d . . . . .
H15 H 0.354769 0.516346 0.358171 0.086 Uiso 1 1 calc R U . . .
C20 C 0.61434(18) 0.8149(3) 0.6747(3) 0.0532(7) Uani 1 1 d . . . . .
C11 C 0.6722(3) 0.3269(4) 0.5598(4) 0.0867(12) Uani 1 1 d . . . . .
H11 H 0.707385 0.283061 0.605366 0.104 Uiso 1 1 calc R U . . .
C12 C 0.6594(2) 0.4709(3) 0.5672(3) 0.0646(8) Uani 1 1 d . . . . .
H12 H 0.685478 0.524733 0.618231 0.077 Uiso 1 1 calc R U . . .
C18 C 0.42627(18) 0.7732(3) 0.5613(3) 0.0617(8) Uani 1 1 d . . . . .
H18 H 0.443987 0.837557 0.612241 0.074 Uiso 1 1 calc R U . . .
C10 C 0.6327(3) 0.2475(4) 0.4848(5) 0.0920(13) Uani 1 1 d . . . . .
H10 H 0.640759 0.149774 0.481557 0.110 Uiso 1 1 calc R U . . .
C17 C 0.3481(2) 0.7469(5) 0.5497(4) 0.0812(11) Uani 1 1 d . . . . .
H17 H 0.312862 0.794656 0.592956 0.097 Uiso 1 1 calc R U . . .
C16 C 0.3221(2) 0.6516(5) 0.4754(4) 0.0831(11) Uani 1 1 d . . . . .
H16 H 0.269424 0.634211 0.469447 0.100 Uiso 1 1 calc R U . . .
C5 C 0.5620(3) 0.6610(5) 0.1803(3) 0.0811(10) Uani 1 1 d . . . . .
H5 H 0.538199 0.593404 0.137079 0.097 Uiso 1 1 calc R U . . .
C24 C 0.5848(3) 1.0489(7) 0.7499(6) 0.124(2) Uani 1 1 d . . . . .
H24A H 0.573079 1.074489 0.677270 0.186 Uiso 1 1 calc R U . . .
H24B H 0.604649 1.130362 0.787142 0.186 Uiso 1 1 calc R U . . .
H24C H 0.538704 1.016164 0.784776 0.186 Uiso 1 1 calc R U . . .
C22 C 0.6546(6) 0.8692(9) 0.8599(4) 0.164(4) Uani 1 1 d . . . . .
H22A H 0.665977 0.944209 0.909581 0.246 Uiso 1 1 calc R U . . .
H22B H 0.696000 0.801310 0.860077 0.246 Uiso 1 1 calc R U . . .
H22C H 0.607468 0.822895 0.880694 0.246 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
P1 N1 1.603(2) . ?
P1 C1 1.794(3) . ?
P1 C13 1.801(3) . ?
P1 C19 1.803(2) . ?
N1 C20 1.353(4) . ?
O1 C20 1.236(4) . ?
C7 C6 1.515(5) . ?
C7 C8 1.524(5) . ?
C7 C14 1.525(5) . ?
C7 H7 0.9800 . ?
C8 C9 1.382(5) . ?
C8 C13 1.409(4) . ?
C14 C15 1.381(4) . ?
C14 C19 1.400(4) . ?
C2 C1 1.381(4) . ?
C2 C3 1.386(6) . ?
C2 H2 0.9300 . ?
C13 C12 1.379(4) . ?
C19 C18 1.381(5) . ?
C4 C5 1.380(7) . ?
C4 C3 1.384(7) . ?
C4 H4 0.9300 . ?
C6 C5 1.384(5) . ?
C6 C1 1.408(5) . ?
C21 C22 1.487(6) . ?
C21 C23 1.522(5) . ?
C21 C20 1.535(4) . ?
C21 C24 1.539(7) . ?
C3 H3 0.9300 . ?
C9 C10 1.373(6) . ?
C9 H9 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C15 C16 1.385(6) . ?
C15 H15 0.9300 . ?
C11 C12 1.375(5) . ?
C11 C10 1.379(6) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C18 C17 1.384(5) . ?
C18 H18 0.9300 . ?
C10 H10 0.9300 . ?
C17 C16 1.366(7) . ?
C17 H17 0.9300 . ?
C16 H16 0.9300 . ?
C5 H5 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?

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
N1 P1 C1 112.50(13) . . ?
N1 P1 C13 121.68(13) . . ?
C1 P1 C13 99.24(15) . . ?
N1 P1 C19 121.09(14) . . ?
C1 P1 C19 98.65(16) . . ?
C13 P1 C19 99.36(12) . . ?
C20 N1 P1 114.24(19) . . ?
C6 C7 C8 108.3(2) . . ?
C6 C7 C14 108.0(3) . . ?
C8 C7 C14 108.6(3) . . ?
C6 C7 H7 110.6 . . ?
C8 C7 H7 110.6 . . ?
C14 C7 H7 110.6 . . ?
C9 C8 C13 118.9(3) . . ?
C9 C8 C7 124.3(3) . . ?
C13 C8 C7 116.7(3) . . ?
C15 C14 C19 119.0(3) . . ?
C15 C14 C7 124.0(3) . . ?
C19 C14 C7 117.0(2) . . ?
C1 C2 C3 118.9(4) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C12 C13 C8 120.6(3) . . ?
C12 C13 P1 127.2(2) . . ?
C8 C13 P1 112.2(2) . . ?
C18 C19 C14 121.2(3) . . ?
C18 C19 P1 126.6(2) . . ?
C14 C19 P1 112.2(2) . . ?
C5 C4 C3 121.2(4) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C5 C6 C1 119.2(3) . . ?
C5 C6 C7 123.6(3) . . ?
C1 C6 C7 117.2(3) . . ?
C22 C21 C23 110.2(5) . . ?
C22 C21 C20 109.6(3) . . ?
C23 C21 C20 112.3(3) . . ?
C22 C21 C24 110.8(6) . . ?
C23 C21 C24 108.5(4) . . ?
C20 C21 C24 105.4(3) . . ?
C4 C3 C2 120.2(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C10 C9 C8 119.7(4) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C2 C1 C6 121.0(3) . . ?
C2 C1 P1 127.0(3) . . ?
C6 C1 P1 112.0(2) . . ?
C14 C15 C16 119.6(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
O1 C20 N1 123.0(3) . . ?
O1 C20 C21 119.4(3) . . ?
N1 C20 C21 117.6(2) . . ?
C12 C11 C10 119.9(4) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 119.5(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C19 C18 C17 118.6(3) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C9 C10 C11 121.3(3) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C16 C17 C18 120.7(4) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C17 C16 C15 121.0(3) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C4 C5 C6 119.5(4) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 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
C1 P1 N1 C20 179.7(2) . . . . ?
C13 P1 N1 C20 -62.9(3) . . . . ?
C19 P1 N1 C20 63.6(3) . . . . ?
C6 C7 C8 C9 -122.8(4) . . . . ?
C14 C7 C8 C9 120.0(4) . . . . ?
C6 C7 C8 C13 58.6(4) . . . . ?
C14 C7 C8 C13 -58.6(3) . . . . ?
C6 C7 C14 C15 121.0(3) . . . . ?
C8 C7 C14 C15 -121.7(3) . . . . ?
C6 C7 C14 C19 -58.5(3) . . . . ?
C8 C7 C14 C19 58.8(3) . . . . ?
C9 C8 C13 C12 1.2(5) . . . . ?
C7 C8 C13 C12 179.9(3) . . . . ?
C9 C8 C13 P1 -178.6(3) . . . . ?
C7 C8 C13 P1 0.1(4) . . . . ?
N1 P1 C13 C12 6.1(4) . . . . ?
C1 P1 C13 C12 129.9(3) . . . . ?
C19 P1 C13 C12 -129.7(3) . . . . ?
N1 P1 C13 C8 -174.2(2) . . . . ?
C1 P1 C13 C8 -50.4(2) . . . . ?
C19 P1 C13 C8 50.1(3) . . . . ?
C15 C14 C19 C18 -0.9(5) . . . . ?
C7 C14 C19 C18 178.6(3) . . . . ?
C15 C14 C19 P1 -179.7(2) . . . . ?
C7 C14 C19 P1 -0.2(4) . . . . ?
N1 P1 C19 C18 -4.9(4) . . . . ?
C1 P1 C19 C18 -127.8(3) . . . . ?
C13 P1 C19 C18 131.2(3) . . . . ?
N1 P1 C19 C14 173.8(2) . . . . ?
C1 P1 C19 C14 50.9(2) . . . . ?
C13 P1 C19 C14 -50.1(3) . . . . ?
C8 C7 C6 C5 121.0(4) . . . . ?
C14 C7 C6 C5 -121.5(4) . . . . ?
C8 C7 C6 C1 -59.2(4) . . . . ?
C14 C7 C6 C1 58.4(3) . . . . ?
C5 C4 C3 C2 0.9(7) . . . . ?
C1 C2 C3 C4 -0.4(6) . . . . ?
C13 C8 C9 C10 -0.3(6) . . . . ?
C7 C8 C9 C10 -178.9(4) . . . . ?
C3 C2 C1 C6 -0.7(5) . . . . ?
C3 C2 C1 P1 -179.6(3) . . . . ?
C5 C6 C1 C2 1.4(5) . . . . ?
C7 C6 C1 C2 -178.5(3) . . . . ?
C5 C6 C1 P1 -179.6(3) . . . . ?
C7 C6 C1 P1 0.5(4) . . . . ?
N1 P1 C1 C2 -1.0(3) . . . . ?
C13 P1 C1 C2 -131.0(3) . . . . ?
C19 P1 C1 C2 127.9(3) . . . . ?
N1 P1 C1 C6 -179.9(2) . . . . ?
C13 P1 C1 C6 50.0(2) . . . . ?
C19 P1 C1 C6 -51.0(2) . . . . ?
C19 C14 C15 C16 0.4(5) . . . . ?
C7 C14 C15 C16 -179.1(3) . . . . ?
P1 N1 C20 O1 3.1(4) . . . . ?
P1 N1 C20 C21 -173.7(2) . . . . ?
C22 C21 C20 O1 21.7(7) . . . . ?
C23 C21 C20 O1 144.5(3) . . . . ?
C24 C21 C20 O1 -97.5(5) . . . . ?
C22 C21 C20 N1 -161.3(5) . . . . ?
C23 C21 C20 N1 -38.5(4) . . . . ?
C24 C21 C20 N1 79.4(4) . . . . ?
C10 C11 C12 C13 -0.7(7) . . . . ?
C8 C13 C12 C11 -0.7(5) . . . . ?
P1 C13 C12 C11 179.1(3) . . . . ?
C14 C19 C18 C17 0.5(5) . . . . ?
P1 C19 C18 C17 179.1(3) . . . . ?
C8 C9 C10 C11 -1.1(7) . . . . ?
C12 C11 C10 C9 1.6(8) . . . . ?
C19 C18 C17 C16 0.5(6) . . . . ?
C18 C17 C16 C15 -1.0(7) . . . . ?
C14 C15 C16 C17 0.5(6) . . . . ?
C3 C4 C5 C6 -0.1(7) . . . . ?
C1 C6 C5 C4 -1.0(6) . . . . ?
C7 C6 C5 C4 178.9(4) . . . . ?

_refine_diff_density_max         0.260
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.031



# start Validation Reply Form
_vrf_STRVA01_nt0756_LHG159       
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: No chiral molecule in the structure.
;
_vrf_PLAT220_nt0756_LHG159       
;
PROBLEM: NonSolvent Resd 1  C   Ueq(max) / Ueq(min) Range        3.3 Ratio 
RESPONSE: Large thermal motion of the terminal t-butyl moiety.
;
_vrf_PLAT242_nt0756_LHG159       
;
PROBLEM: Low    MainMol Ueq as Compared to Neighbors of        C21 Check   
RESPONSE: False alarm for the terminal t-butyl moiety.
;
_vrf_PLAT340_nt0756_LHG159       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00552 Ang.  
RESPONSE: Large thermal motion of the molecule.
;
_vrf_PLAT911_nt0756_LHG159       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.597         10 Report
RESPONSE: These reflections are missing in the highest and lowest resolution
 shells because of the instrument geometry limitations.
;
_vrf_PLAT915_nt0756_LHG159       
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         73 %     
RESPONSE: No chiral molecule in the structure.
;
_vrf_PLAT978_nt0756_LHG159       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: Large thermal motion of the molecule.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1290_SMC_088
_database_code_depnum_ccdc_archive 'CCDC 2313765'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        '9-phosphatriptycene selenide'
_chemical_name_common            '9-phosphatriptycene selenide'
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 P Se'
_chemical_formula_sum            'C19 H13 P Se'
_chemical_formula_weight         351.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se 0.2367 1.4831 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/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'
'-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                   14.1963(6)
_cell_length_b                   13.7375(6)
_cell_length_c                   15.8281(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.8970(10)
_cell_angle_gamma                90
_cell_volume                     3086.4(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    9759
_cell_measurement_theta_min      2.5507
_cell_measurement_theta_max      25.5030

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_F_000             1408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.341
_shelx_estimated_absorpt_T_min   0.571
_shelx_estimated_absorpt_T_max   0.794
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2652
_exptl_absorpt_correction_T_max  0.4645
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            40566
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.928
_diffrn_reflns_theta_max         20.518
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3150
_reflns_number_gt                2866
_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/4 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0512P)²+4.0770P] 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         3150
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.1038
_refine_ls_wR_factor_gt          0.0964
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
Se1 Se 0.60566(2) 0.25561(2) 0.12483(2) 0.05706(13) Uani 1 1 d . . . . .
P1 P 0.66701(4) 0.37911(4) 0.17926(3) 0.03642(15) Uani 1 1 d . . . . .
C1 C 0.68438(16) 0.38420(16) 0.29262(13) 0.0389(5) Uani 1 1 d . . . . .
C2 C 0.65777(18) 0.3136(2) 0.34933(15) 0.0489(5) Uani 1 1 d . . . . .
H2 H 0.628192 0.256976 0.330753 0.059 Uiso 1 1 calc R U . . .
C3 C 0.6761(2) 0.3289(2) 0.43519(16) 0.0615(7) Uani 1 1 d . . . . .
H3 H 0.658560 0.282112 0.474389 0.074 Uiso 1 1 calc R U . . .
C4 C 0.7199(2) 0.4129(3) 0.46205(16) 0.0648(8) Uani 1 1 d . . . . .
H4 H 0.732457 0.421982 0.519350 0.078 Uiso 1 1 calc R U . . .
C5 C 0.74560(19) 0.4840(2) 0.40501(15) 0.0555(6) Uani 1 1 d . . . . .
H5 H 0.774804 0.540715 0.424016 0.067 Uiso 1 1 calc R U . . .
C6 C 0.72767(16) 0.47061(18) 0.31931(13) 0.0414(5) Uani 1 1 d . . . . .
C7 C 0.75261(17) 0.54450(17) 0.25162(15) 0.0429(5) Uani 1 1 d . . . . .
H7 H 0.782122 0.602266 0.276926 0.051 Uiso 1 1 calc R U . . .
C8 C 0.81879(16) 0.49571(17) 0.18966(14) 0.0404(5) Uani 1 1 d . . . . .
C9 C 0.90801(17) 0.5301(2) 0.17150(17) 0.0515(6) Uani 1 1 d . . . . .
H9 H 0.931271 0.585575 0.198180 0.062 Uiso 1 1 calc R U . . .
C10 C 0.96226(19) 0.4810(2) 0.11324(19) 0.0612(7) Uani 1 1 d . . . . .
H10 H 1.022366 0.503569 0.101371 0.073 Uiso 1 1 calc R U . . .
C11 C 0.9283(2) 0.3988(2) 0.07253(17) 0.0577(7) Uani 1 1 d . . . . .
H11 H 0.965328 0.367161 0.033142 0.069 Uiso 1 1 calc R U . . .
C12 C 0.83954(18) 0.36345(19) 0.08999(14) 0.0474(5) Uani 1 1 d . . . . .
H12 H 0.816604 0.308083 0.062837 0.057 Uiso 1 1 calc R U . . .
C13 C 0.78527(16) 0.41199(17) 0.14874(13) 0.0388(4) Uani 1 1 d . . . . .
C14 C 0.61271(16) 0.49659(16) 0.16385(13) 0.0392(5) Uani 1 1 d . . . . .
C15 C 0.53057(17) 0.5147(2) 0.11766(16) 0.0501(6) Uani 1 1 d . . . . .
H15 H 0.497217 0.464004 0.092302 0.060 Uiso 1 1 calc R U . . .
C16 C 0.4994(2) 0.6100(2) 0.1102(2) 0.0648(8) Uani 1 1 d . . . . .
H16 H 0.444920 0.623652 0.078899 0.078 Uiso 1 1 calc R U . . .
C17 C 0.5482(2) 0.6840(2) 0.1485(2) 0.0675(8) Uani 1 1 d . . . . .
H17 H 0.525951 0.747465 0.143344 0.081 Uiso 1 1 calc R U . . .
C19 C 0.66287(16) 0.57191(17) 0.20274(14) 0.0412(5) Uani 1 1 d . . . . .
C18 C 0.6303(2) 0.66645(19) 0.19490(18) 0.0553(6) Uani 1 1 d . . . . .
H18 H 0.663019 0.717570 0.220364 0.066 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
Se1 P1 2.0869(6) . ?
P1 C14 1.804(2) . ?
P1 C1 1.809(2) . ?
P1 C13 1.811(2) . ?
C1 C2 1.378(3) . ?
C1 C6 1.399(3) . ?
C2 C3 1.396(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.375(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.522(3) . ?
C7 C8 1.524(3) . ?
C7 C19 1.527(3) . ?
C7 H7 0.9800 . ?
C8 C9 1.386(3) . ?
C8 C13 1.400(3) . ?
C9 C10 1.386(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.383(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.382(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.388(3) . ?
C12 H12 0.9300 . ?
C14 C15 1.389(3) . ?
C14 C19 1.394(3) . ?
C15 C16 1.387(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.367(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.390(4) . ?
C17 H17 0.9300 . ?
C19 C18 1.383(3) . ?
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
C14 P1 C1 98.68(10) . . ?
C14 P1 C13 97.86(10) . . ?
C1 P1 C13 98.19(10) . . ?
C14 P1 Se1 119.80(8) . . ?
C1 P1 Se1 119.37(8) . . ?
C13 P1 Se1 118.37(8) . . ?
C2 C1 C6 121.6(2) . . ?
C2 C1 P1 125.77(19) . . ?
C6 C1 P1 112.63(16) . . ?
C1 C2 C3 118.7(3) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.9(2) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 119.8(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 118.7(2) . . ?
C5 C6 C7 123.9(2) . . ?
C1 C6 C7 117.35(19) . . ?
C6 C7 C8 108.20(19) . . ?
C6 C7 C19 108.64(19) . . ?
C8 C7 C19 107.47(18) . . ?
C6 C7 H7 110.8 . . ?
C8 C7 H7 110.8 . . ?
C19 C7 H7 110.8 . . ?
C9 C8 C13 119.3(2) . . ?
C9 C8 C7 123.9(2) . . ?
C13 C8 C7 116.8(2) . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 120.9(2) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C12 C11 C10 120.4(2) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 118.8(3) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C12 C13 C8 121.1(2) . . ?
C12 C13 P1 125.84(19) . . ?
C8 C13 P1 113.04(16) . . ?
C15 C14 C19 121.2(2) . . ?
C15 C14 P1 125.8(2) . . ?
C19 C14 P1 112.97(16) . . ?
C16 C15 C14 118.6(3) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C17 C16 C15 120.3(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 121.4(3) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C18 C19 C14 119.3(2) . . ?
C18 C19 C7 123.5(2) . . ?
C14 C19 C7 117.2(2) . . ?
C19 C18 C17 119.1(3) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?

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
C14 P1 C1 C2 129.3(2) . . . . ?
C13 P1 C1 C2 -131.4(2) . . . . ?
Se1 P1 C1 C2 -2.2(2) . . . . ?
C14 P1 C1 C6 -49.57(18) . . . . ?
C13 P1 C1 C6 49.74(18) . . . . ?
Se1 P1 C1 C6 178.93(13) . . . . ?
C6 C1 C2 C3 -1.0(4) . . . . ?
P1 C1 C2 C3 -179.79(19) . . . . ?
C1 C2 C3 C4 -0.1(4) . . . . ?
C2 C3 C4 C5 0.8(4) . . . . ?
C3 C4 C5 C6 -0.5(4) . . . . ?
C4 C5 C6 C1 -0.6(4) . . . . ?
C4 C5 C6 C7 179.7(2) . . . . ?
C2 C1 C6 C5 1.3(3) . . . . ?
P1 C1 C6 C5 -179.76(18) . . . . ?
C2 C1 C6 C7 -178.9(2) . . . . ?
P1 C1 C6 C7 0.0(3) . . . . ?
C5 C6 C7 C8 121.1(2) . . . . ?
C1 C6 C7 C8 -58.7(3) . . . . ?
C5 C6 C7 C19 -122.5(2) . . . . ?
C1 C6 C7 C19 57.7(3) . . . . ?
C6 C7 C8 C9 -122.4(2) . . . . ?
C19 C7 C8 C9 120.5(2) . . . . ?
C6 C7 C8 C13 58.4(3) . . . . ?
C19 C7 C8 C13 -58.7(3) . . . . ?
C13 C8 C9 C10 0.0(4) . . . . ?
C7 C8 C9 C10 -179.2(2) . . . . ?
C8 C9 C10 C11 0.6(4) . . . . ?
C9 C10 C11 C12 -0.7(4) . . . . ?
C10 C11 C12 C13 0.2(4) . . . . ?
C11 C12 C13 C8 0.4(3) . . . . ?
C11 C12 C13 P1 178.88(18) . . . . ?
C9 C8 C13 C12 -0.5(3) . . . . ?
C7 C8 C13 C12 178.7(2) . . . . ?
C9 C8 C13 P1 -179.18(17) . . . . ?
C7 C8 C13 P1 0.1(2) . . . . ?
C14 P1 C13 C12 -128.5(2) . . . . ?
C1 P1 C13 C12 131.5(2) . . . . ?
Se1 P1 C13 C12 1.6(2) . . . . ?
C14 P1 C13 C8 50.10(17) . . . . ?
C1 P1 C13 C8 -49.90(17) . . . . ?
Se1 P1 C13 C8 -179.76(13) . . . . ?
C1 P1 C14 C15 -131.1(2) . . . . ?
C13 P1 C14 C15 129.3(2) . . . . ?
Se1 P1 C14 C15 0.1(2) . . . . ?
C1 P1 C14 C19 49.88(18) . . . . ?
C13 P1 C14 C19 -49.70(18) . . . . ?
Se1 P1 C14 C19 -178.89(13) . . . . ?
C19 C14 C15 C16 0.6(4) . . . . ?
P1 C14 C15 C16 -178.37(19) . . . . ?
C14 C15 C16 C17 -0.8(4) . . . . ?
C15 C16 C17 C18 0.7(4) . . . . ?
C15 C14 C19 C18 -0.2(3) . . . . ?
P1 C14 C19 C18 178.83(18) . . . . ?
C15 C14 C19 C7 -179.6(2) . . . . ?
P1 C14 C19 C7 -0.6(3) . . . . ?
C6 C7 C19 C18 123.1(2) . . . . ?
C8 C7 C19 C18 -120.0(2) . . . . ?
C6 C7 C19 C14 -57.5(3) . . . . ?
C8 C7 C19 C14 59.4(3) . . . . ?
C14 C19 C18 C17 0.1(4) . . . . ?
C7 C19 C18 C17 179.5(2) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?

_refine_diff_density_max         0.674
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.076




# start Validation Reply Form
_vrf_PLAT094_nt1290_SMC_088      
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.03 Report
RESPONSE: Truncation error peak near Se atom.
;
_vrf_PLAT911_nt1290_SMC_088      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         12 Report
RESPONSE: These reflections are missing because of the instrument geometry 
limitations.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt0718_LHB_Ts-N-p-trip
_database_code_depnum_ccdc_archive 'CCDC 2313766'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
;
N-(10H-5l5-5,10-[1,2]benzenoacridophosphin-5-ylidene)-4-
methylbenzenesulfonamide
;
_chemical_name_common            
;
N-(10H-5l5-5,10-[1,2]benzenoacridophosphin-5-ylidene)-4-
methylbenzenesulfonamide
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H20 N O2 P S'
_chemical_formula_sum            'C26 H20 N O2 P S'
_chemical_formula_weight         441.46

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'
N N 0.0311 0.0180 '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                   8.19512(14)
_cell_length_b                   13.9420(2)
_cell_length_c                   19.4641(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.7093(16)
_cell_angle_gamma                90
_cell_volume                     2192.04(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    6607
_cell_measurement_theta_min      3.9010
_cell_measurement_theta_max      66.9650

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_F_000             920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.186
_shelx_estimated_absorpt_T_min   0.433
_shelx_estimated_absorpt_T_max   0.735
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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            11121
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.919
_diffrn_reflns_theta_max         67.067
_diffrn_reflns_theta_full        67.067
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3893
_reflns_number_gt                3579
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0989P)²+1.8333P] 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         3893
_refine_ls_number_parameters     281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0632
_refine_ls_wR_factor_ref         0.1828
_refine_ls_wR_factor_gt          0.1784
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_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
S1 S 0.45198(10) 0.65856(7) 0.27137(4) 0.0595(3) Uani 1 1 d . . . . .
P1 P 0.50690(8) 0.73609(5) 0.40781(4) 0.0392(2) Uani 1 1 d . . . . .
O1 O 0.3392(3) 0.5925(2) 0.29636(17) 0.0898(10) Uani 1 1 d . . . . .
O2 O 0.3922(4) 0.7042(3) 0.20745(14) 0.1000(12) Uani 1 1 d . . . . .
N1 N 0.5203(4) 0.73598(19) 0.32759(15) 0.0531(7) Uani 1 1 d . . . . .
C1 C 0.6003(3) 0.84182(19) 0.44830(16) 0.0414(6) Uani 1 1 d . . . . .
C2 C 0.6795(4) 0.9120(2) 0.41559(18) 0.0510(7) Uani 1 1 d . . . . .
H2 H 0.682523 0.908350 0.368113 0.061 Uiso 1 1 calc R U . . .
C3 C 0.7542(4) 0.9878(2) 0.4553(2) 0.0624(9) Uani 1 1 d . . . . .
H3 H 0.808780 1.035154 0.434289 0.075 Uiso 1 1 calc R U . . .
C4 C 0.7481(4) 0.9934(2) 0.5251(2) 0.0617(9) Uani 1 1 d . . . . .
H4 H 0.798970 1.044535 0.550994 0.074 Uiso 1 1 calc R U . . .
C5 C 0.6670(4) 0.9237(2) 0.55764(18) 0.0516(7) Uani 1 1 d . . . . .
H5 H 0.661652 0.928816 0.604851 0.062 Uiso 1 1 calc R U . . .
C6 C 0.5940(3) 0.8464(2) 0.51916(16) 0.0417(6) Uani 1 1 d . . . . .
C7 C 0.5076(3) 0.7628(2) 0.55045(16) 0.0436(6) Uani 1 1 d . . . . .
H7 H 0.507531 0.772217 0.600334 0.052 Uiso 1 1 calc R U . . .
C8 C 0.3291(3) 0.75440(19) 0.50906(16) 0.0403(6) Uani 1 1 d . . . . .
C9 C 0.1901(4) 0.7587(2) 0.54114(17) 0.0476(7) Uani 1 1 d . . . . .
H9 H 0.200877 0.767175 0.589078 0.057 Uiso 1 1 calc R U . . .
C10 C 0.0338(4) 0.7499(2) 0.49988(19) 0.0528(8) Uani 1 1 d . . . . .
H10 H -0.060196 0.752913 0.520716 0.063 Uiso 1 1 calc R U . . .
C11 C 0.0168(4) 0.7369(2) 0.42928(19) 0.0521(8) Uani 1 1 d . . . . .
H11 H -0.088442 0.731413 0.402823 0.063 Uiso 1 1 calc R U . . .
C12 C 0.1550(3) 0.7320(2) 0.39675(16) 0.0446(7) Uani 1 1 d . . . . .
H12 H 0.143615 0.723050 0.348832 0.054 Uiso 1 1 calc R U . . .
C13 C 0.3106(3) 0.74071(19) 0.43761(16) 0.0401(6) Uani 1 1 d . . . . .
C14 C 0.5993(3) 0.6704(2) 0.53674(15) 0.0441(6) Uani 1 1 d . . . . .
C15 C 0.6747(4) 0.6116(3) 0.58945(18) 0.0559(8) Uani 1 1 d . . . . .
H15 H 0.668970 0.626101 0.635633 0.067 Uiso 1 1 calc R U . . .
C16 C 0.7586(5) 0.5313(3) 0.5735(2) 0.0669(10) Uani 1 1 d . . . . .
H16 H 0.809524 0.491760 0.609299 0.080 Uiso 1 1 calc R U . . .
C17 C 0.7686(4) 0.5084(2) 0.5056(2) 0.0632(9) Uani 1 1 d . . . . .
H17 H 0.825903 0.453813 0.495854 0.076 Uiso 1 1 calc R U . . .
C18 C 0.6929(4) 0.5668(2) 0.45127(18) 0.0512(7) Uani 1 1 d . . . . .
H18 H 0.699135 0.552002 0.405204 0.061 Uiso 1 1 calc R U . . .
C19 C 0.6080(3) 0.64775(19) 0.46750(15) 0.0410(6) Uani 1 1 d . . . . .
C20 C 0.6277(4) 0.5919(2) 0.25851(16) 0.0507(7) Uani 1 1 d . . . . .
C21 C 0.6193(5) 0.4939(3) 0.2570(2) 0.0658(9) Uani 1 1 d . . . . .
H21 H 0.521694 0.463217 0.262714 0.079 Uiso 1 1 calc R U . . .
C22 C 0.7547(6) 0.4405(3) 0.2471(2) 0.0789(12) Uani 1 1 d . . . . .
H22 H 0.747904 0.373948 0.246691 0.095 Uiso 1 1 calc R U . . .
C23 C 0.9016(5) 0.4846(3) 0.2377(2) 0.0720(11) Uani 1 1 d . . . . .
C24 C 1.0480(6) 0.4258(5) 0.2257(3) 0.116(2) Uani 1 1 d . . . . .
H00A H 1.032859 0.405857 0.177826 0.174 Uiso 1 1 calc R U . . .
H00B H 1.057606 0.370266 0.255290 0.174 Uiso 1 1 calc R U . . .
H00C H 1.146876 0.463624 0.236279 0.174 Uiso 1 1 calc R U . . .
C25 C 0.9070(4) 0.5833(3) 0.2395(2) 0.0734(11) Uani 1 1 d . . . . .
H25 H 1.004184 0.614321 0.233674 0.088 Uiso 1 1 calc R U . . .
C26 C 0.7733(4) 0.6369(3) 0.24953(19) 0.0600(8) Uani 1 1 d . . . . .
H26 H 0.780089 0.703511 0.250320 0.072 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
S1 O2 1.409(3) . ?
S1 O1 1.446(3) . ?
S1 N1 1.571(3) . ?
S1 C20 1.767(3) . ?
P1 N1 1.584(3) . ?
P1 C1 1.782(3) . ?
P1 C19 1.797(3) . ?
P1 C13 1.801(3) . ?
C1 C2 1.387(4) . ?
C1 C6 1.390(4) . ?
C2 C3 1.389(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.370(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.542(4) . ?
C7 C14 1.537(4) . ?
C7 C8 1.551(4) . ?
C7 H7 0.9800 . ?
C8 C13 1.387(4) . ?
C8 C9 1.389(4) . ?
C9 C10 1.398(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.370(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.389(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.390(4) . ?
C12 H12 0.9300 . ?
C14 C15 1.375(4) . ?
C14 C19 1.398(4) . ?
C15 C16 1.378(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.376(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.395(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.389(4) . ?
C18 H18 0.9300 . ?
C20 C21 1.368(5) . ?
C20 C26 1.385(5) . ?
C21 C22 1.376(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.391(6) . ?
C22 H22 0.9300 . ?
C23 C25 1.376(6) . ?
C23 C24 1.504(6) . ?
C24 H00A 0.9600 . ?
C24 H00B 0.9600 . ?
C24 H00C 0.9600 . ?
C25 C26 1.367(5) . ?
C25 H25 0.9300 . ?
C26 H26 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
O2 S1 O1 115.9(2) . . ?
O2 S1 N1 109.6(2) . . ?
O1 S1 N1 112.09(16) . . ?
O2 S1 C20 106.41(17) . . ?
O1 S1 C20 107.16(19) . . ?
N1 S1 C20 104.90(15) . . ?
N1 P1 C1 109.93(14) . . ?
N1 P1 C19 122.40(14) . . ?
C1 P1 C19 99.45(13) . . ?
N1 P1 C13 122.12(15) . . ?
C1 P1 C13 99.69(13) . . ?
C19 P1 C13 98.96(13) . . ?
S1 N1 P1 127.70(18) . . ?
C2 C1 C6 121.4(3) . . ?
C2 C1 P1 125.4(2) . . ?
C6 C1 P1 113.1(2) . . ?
C1 C2 C3 118.5(3) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 120.8(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 119.5(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 119.1(3) . . ?
C5 C6 C7 124.0(3) . . ?
C1 C6 C7 117.0(2) . . ?
C14 C7 C6 107.1(2) . . ?
C14 C7 C8 107.0(2) . . ?
C6 C7 C8 107.9(2) . . ?
C14 C7 H7 111.5 . . ?
C6 C7 H7 111.5 . . ?
C8 C7 H7 111.5 . . ?
C13 C8 C9 119.8(3) . . ?
C13 C8 C7 117.7(2) . . ?
C9 C8 C7 122.4(3) . . ?
C8 C9 C10 118.7(3) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 120.7(3) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C13 118.4(3) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C8 C13 C12 121.4(3) . . ?
C8 C13 P1 112.1(2) . . ?
C12 C13 P1 126.6(2) . . ?
C15 C14 C19 119.7(3) . . ?
C15 C14 C7 122.7(3) . . ?
C19 C14 C7 117.5(3) . . ?
C14 C15 C16 119.7(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 121.2(3) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 120.1(3) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C19 C18 C17 118.6(3) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C18 C19 C14 120.8(3) . . ?
C18 C19 P1 127.1(2) . . ?
C14 C19 P1 112.1(2) . . ?
C21 C20 C26 119.4(3) . . ?
C21 C20 S1 119.3(3) . . ?
C26 C20 S1 121.3(3) . . ?
C20 C21 C22 120.3(4) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C21 C22 C23 121.0(4) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C25 C23 C22 117.6(3) . . ?
C25 C23 C24 121.7(4) . . ?
C22 C23 C24 120.6(4) . . ?
C23 C24 H00A 109.5 . . ?
C23 C24 H00B 109.5 . . ?
H00A C24 H00B 109.5 . . ?
C23 C24 H00C 109.5 . . ?
H00A C24 H00C 109.5 . . ?
H00B C24 H00C 109.5 . . ?
C26 C25 C23 121.8(4) . . ?
C26 C25 H25 119.1 . . ?
C23 C25 H25 119.1 . . ?
C25 C26 C20 119.9(4) . . ?
C25 C26 H26 120.1 . . ?
C20 C26 H26 120.1 . . ?

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
O2 S1 N1 P1 142.8(2) . . . . ?
O1 S1 N1 P1 12.6(3) . . . . ?
C20 S1 N1 P1 -103.3(2) . . . . ?
C1 P1 N1 S1 -178.60(19) . . . . ?
C19 P1 N1 S1 65.5(3) . . . . ?
C13 P1 N1 S1 -62.6(3) . . . . ?
N1 P1 C1 C2 -2.6(3) . . . . ?
C19 P1 C1 C2 127.1(3) . . . . ?
C13 P1 C1 C2 -132.0(3) . . . . ?
N1 P1 C1 C6 -179.63(19) . . . . ?
C19 P1 C1 C6 -50.0(2) . . . . ?
C13 P1 C1 C6 50.9(2) . . . . ?
C6 C1 C2 C3 0.3(4) . . . . ?
P1 C1 C2 C3 -176.5(2) . . . . ?
C1 C2 C3 C4 -0.6(5) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
C3 C4 C5 C6 1.3(5) . . . . ?
C4 C5 C6 C1 -1.6(4) . . . . ?
C4 C5 C6 C7 177.2(3) . . . . ?
C2 C1 C6 C5 0.8(4) . . . . ?
P1 C1 C6 C5 178.0(2) . . . . ?
C2 C1 C6 C7 -178.1(3) . . . . ?
P1 C1 C6 C7 -0.9(3) . . . . ?
C5 C6 C7 C14 -120.3(3) . . . . ?
C1 C6 C7 C14 58.5(3) . . . . ?
C5 C6 C7 C8 124.7(3) . . . . ?
C1 C6 C7 C8 -56.5(3) . . . . ?
C14 C7 C8 C13 -57.7(3) . . . . ?
C6 C7 C8 C13 57.3(3) . . . . ?
C14 C7 C8 C9 121.3(3) . . . . ?
C6 C7 C8 C9 -123.7(3) . . . . ?
C13 C8 C9 C10 -0.6(4) . . . . ?
C7 C8 C9 C10 -179.6(3) . . . . ?
C8 C9 C10 C11 0.3(5) . . . . ?
C9 C10 C11 C12 0.1(5) . . . . ?
C10 C11 C12 C13 -0.1(5) . . . . ?
C9 C8 C13 C12 0.6(4) . . . . ?
C7 C8 C13 C12 179.7(3) . . . . ?
C9 C8 C13 P1 -179.3(2) . . . . ?
C7 C8 C13 P1 -0.3(3) . . . . ?
C11 C12 C13 C8 -0.2(4) . . . . ?
C11 C12 C13 P1 179.7(2) . . . . ?
N1 P1 C13 C8 -171.1(2) . . . . ?
C1 P1 C13 C8 -50.0(2) . . . . ?
C19 P1 C13 C8 51.2(2) . . . . ?
N1 P1 C13 C12 9.0(3) . . . . ?
C1 P1 C13 C12 130.0(3) . . . . ?
C19 P1 C13 C12 -128.7(3) . . . . ?
C6 C7 C14 C15 120.5(3) . . . . ?
C8 C7 C14 C15 -124.0(3) . . . . ?
C6 C7 C14 C19 -58.1(3) . . . . ?
C8 C7 C14 C19 57.4(3) . . . . ?
C19 C14 C15 C16 0.3(5) . . . . ?
C7 C14 C15 C16 -178.2(3) . . . . ?
C14 C15 C16 C17 -0.1(5) . . . . ?
C15 C16 C17 C18 0.0(5) . . . . ?
C16 C17 C18 C19 -0.1(5) . . . . ?
C17 C18 C19 C14 0.3(4) . . . . ?
C17 C18 C19 P1 177.7(2) . . . . ?
C15 C14 C19 C18 -0.4(4) . . . . ?
C7 C14 C19 C18 178.2(3) . . . . ?
C15 C14 C19 P1 -178.2(2) . . . . ?
C7 C14 C19 P1 0.4(3) . . . . ?
N1 P1 C19 C18 -6.5(3) . . . . ?
C1 P1 C19 C18 -127.5(3) . . . . ?
C13 P1 C19 C18 131.0(3) . . . . ?
N1 P1 C19 C14 171.0(2) . . . . ?
C1 P1 C19 C14 50.1(2) . . . . ?
C13 P1 C19 C14 -51.4(2) . . . . ?
O2 S1 C20 C21 -109.9(3) . . . . ?
O1 S1 C20 C21 14.7(3) . . . . ?
N1 S1 C20 C21 134.0(3) . . . . ?
O2 S1 C20 C26 69.7(3) . . . . ?
O1 S1 C20 C26 -165.7(3) . . . . ?
N1 S1 C20 C26 -46.4(3) . . . . ?
C26 C20 C21 C22 0.4(6) . . . . ?
S1 C20 C21 C22 -180.0(3) . . . . ?
C20 C21 C22 C23 -0.7(6) . . . . ?
C21 C22 C23 C25 0.7(6) . . . . ?
C21 C22 C23 C24 -178.9(4) . . . . ?
C22 C23 C25 C26 -0.5(6) . . . . ?
C24 C23 C25 C26 179.1(4) . . . . ?
C23 C25 C26 C20 0.2(6) . . . . ?
C21 C20 C26 C25 -0.2(5) . . . . ?
S1 C20 C26 C25 -179.8(3) . . . . ?

_refine_diff_density_max         0.910
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.071



# start Validation Reply Form
_vrf_PLAT242_nt0718_LHB_Ts-N-p-trip 
;
PROBLEM: Low    MainMol Ueq as Compared to Neighbors of        C23 Check   
RESPONSE: Large thermal motion of the 4-methylbenzene fragment.
;
_vrf_PLAT340_nt0718_LHB_Ts-N-p-trip 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00471 Ang.  
RESPONSE: Large thermal motion of the molecule.
;
_vrf_PLAT911_nt0718_LHB_Ts-N-p-trip 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.597         29 Report
RESPONSE: These reflections are missing in the highest and lowest 
resolution shells because of the instrument geometry limitations.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt0726_LHG141_100K
_database_code_depnum_ccdc_archive 'CCDC 2313769'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
;
N-(10H-5λ⁵-5,10-[1,2]benzenoacridophosphin-5-ylidene)-
2,4,6-triisopropylbenzenesulfonamide
;
_chemical_name_common            
;
N-(10H-5λ⁵-5,10-[1,2]benzenoacridophosphin-5-ylidene)-
2,4,6-triisopropylbenzenesulfonamide
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H36 N O2 P S'
_chemical_formula_sum            'C34 H36 N O2 P S'
_chemical_formula_weight         553.67

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.31097(12)
_cell_length_b                   12.97197(17)
_cell_length_c                   24.0692(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2907.12(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15456
_cell_measurement_theta_min      2.6920
_cell_measurement_theta_max      32.2590

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_F_000             1176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.198
_shelx_estimated_absorpt_T_min   0.892
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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            40245
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.308
_diffrn_reflns_theta_max         32.861
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10003
_reflns_number_gt                8710
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.762
_reflns_Friedel_fraction_max     0.895
_reflns_Friedel_fraction_full    1.000

_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0466P)²+0.6017P] 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 3322 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         10003
_refine_ls_number_parameters     494
_refine_ls_number_restraints     216
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0901
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.023
_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
S1 S 0.22434(5) 0.48276(4) 0.60865(2) 0.01945(10) Uani 1 1 d . . . . .
P1 P 0.14409(5) 0.31167(4) 0.67323(2) 0.01593(10) Uani 1 1 d . . . . .
O1 O 0.18553(17) 0.55355(12) 0.65267(7) 0.0300(4) Uani 1 1 d . . . . .
O2 O 0.12678(17) 0.48309(14) 0.56239(7) 0.0315(4) Uani 1 1 d . . . . .
N1 N 0.24904(18) 0.36924(13) 0.63227(7) 0.0204(3) Uani 1 1 d . . . . .
C1 C 0.1801(2) 0.17614(14) 0.67442(9) 0.0193(4) Uani 1 1 d . . . . .
C2 C 0.2851(2) 0.12544(16) 0.64418(9) 0.0236(4) Uani 1 1 d . . . . .
H2 H 0.342315 0.161540 0.617929 0.028 Uiso 1 1 calc R U . . .
C3 C 0.3049(3) 0.02043(18) 0.65313(11) 0.0317(5) Uani 1 1 d . . . . .
H3 H 0.375747 -0.016032 0.632626 0.038 Uiso 1 1 calc R U . . .
C4 C 0.2214(3) -0.03107(16) 0.69190(11) 0.0340(5) Uani 1 1 d . . . . .
H4 H 0.236722 -0.102570 0.698041 0.041 Uiso 1 1 calc R U . . .
C5 C 0.1160(2) 0.01984(17) 0.72183(10) 0.0274(4) Uani 1 1 d . . . . .
H5 H 0.058930 -0.016594 0.747985 0.033 Uiso 1 1 calc R U . . .
C6 C 0.0945(2) 0.12470(16) 0.71328(9) 0.0216(4) Uani 1 1 d . . . . .
C7 C -0.0157(2) 0.18893(17) 0.74529(9) 0.0229(4) Uani 1 1 d . . . . .
H7 H -0.072799 0.144435 0.771041 0.027 Uiso 1 1 calc R U . . .
C8 C 0.0667(2) 0.27136(16) 0.77767(9) 0.0222(4) Uani 1 1 d . . . . .
C9 C 0.0584(3) 0.28384(18) 0.83502(9) 0.0288(5) Uani 1 1 d . . . . .
H9 H -0.000679 0.239660 0.856652 0.035 Uiso 1 1 calc R U . . .
C10 C 0.1378(3) 0.3618(2) 0.86035(9) 0.0335(5) Uani 1 1 d . . . . .
H10 H 0.131026 0.371247 0.899401 0.040 Uiso 1 1 calc R U . . .
C11 C 0.2264(3) 0.42567(18) 0.82948(10) 0.0319(5) Uani 1 1 d . . . . .
H11 H 0.281012 0.477602 0.847584 0.038 Uiso 1 1 calc R U . . .
C12 C 0.2358(3) 0.41418(16) 0.77202(9) 0.0241(4) Uani 1 1 d . . . . .
H12 H 0.296481 0.457713 0.750654 0.029 Uiso 1 1 calc R U . . .
C13 C 0.1546(2) 0.33771(15) 0.74671(8) 0.0199(4) Uani 1 1 d . . . . .
C14 C -0.1136(2) 0.24374(16) 0.70411(9) 0.0219(4) Uani 1 1 d . . . . .
C15 C -0.2619(2) 0.23330(17) 0.70387(10) 0.0258(4) Uani 1 1 d . . . . .
H15 H -0.307034 0.186956 0.728941 0.031 Uiso 1 1 calc R U . . .
C16 C -0.3445(2) 0.29078(18) 0.66686(10) 0.0285(5) Uani 1 1 d . . . . .
H16 H -0.446133 0.284004 0.667141 0.034 Uiso 1 1 calc R U . . .
C17 C -0.2797(3) 0.35774(17) 0.62967(10) 0.0263(4) Uani 1 1 d . . . . .
H17 H -0.337268 0.396803 0.604785 0.032 Uiso 1 1 calc R U . . .
C18 C -0.1311(2) 0.36819(16) 0.62847(9) 0.0214(4) Uani 1 1 d . . . . .
H18 H -0.086448 0.413663 0.602807 0.026 Uiso 1 1 calc R U . . .
C19 C -0.0491(2) 0.31083(15) 0.66557(8) 0.0190(4) Uani 1 1 d . . . . .
C20A C 0.3957(5) 0.5114(3) 0.5802(2) 0.0164(7) Uani 0.869(6) 1 d D U P A 1
C21A C 0.4871(4) 0.5874(3) 0.60308(13) 0.0172(6) Uani 0.869(6) 1 d D U P A 1
C22A C 0.4741(4) 0.6326(3) 0.66152(13) 0.0199(6) Uani 0.869(6) 1 d D U P A 1
H22A H 0.394218 0.595706 0.680911 0.024 Uiso 0.869(6) 1 calc R U P A 1
C23A C 0.6120(4) 0.6137(3) 0.69457(14) 0.0338(7) Uani 0.869(6) 1 d D . P A 1
H23A H 0.633639 0.539779 0.694876 0.051 Uiso 0.869(6) 1 calc R U P A 1
H23B H 0.599045 0.638037 0.732789 0.051 Uiso 0.869(6) 1 calc R U P A 1
H23C H 0.691570 0.651206 0.677207 0.051 Uiso 0.869(6) 1 calc R U P A 1
C24A C 0.4357(4) 0.7471(2) 0.65968(17) 0.0293(7) Uani 0.869(6) 1 d D U P A 1
H24A H 0.506831 0.784070 0.637225 0.044 Uiso 0.869(6) 1 calc R U P A 1
H24B H 0.435383 0.775070 0.697502 0.044 Uiso 0.869(6) 1 calc R U P A 1
H24C H 0.340279 0.755631 0.643119 0.044 Uiso 0.869(6) 1 calc R U P A 1
C25A C 0.5998(3) 0.6242(2) 0.57034(13) 0.0193(5) Uani 0.869(6) 1 d D U P A 1
H25A H 0.661244 0.675780 0.585235 0.023 Uiso 0.869(6) 1 calc R U P A 1
C26A C 0.6256(3) 0.58856(19) 0.51700(12) 0.0194(5) Uani 0.869(6) 1 d D . P A 1
C27A C 0.7430(3) 0.6344(2) 0.48070(11) 0.0241(6) Uani 0.869(6) 1 d D . P A 1
H27A H 0.717605 0.617642 0.441348 0.029 Uiso 0.869(6) 1 calc R U P A 1
C28A C 0.8842(6) 0.5826(6) 0.4926(2) 0.075(2) Uani 0.869(6) 1 d D U P A 1
H28A H 0.917154 0.601910 0.529843 0.113 Uiso 0.869(6) 1 calc R U P A 1
H28B H 0.955450 0.604454 0.465041 0.113 Uiso 0.869(6) 1 calc R U P A 1
H28C H 0.872097 0.507613 0.490674 0.113 Uiso 0.869(6) 1 calc R U P A 1
C29A C 0.7501(7) 0.7498(3) 0.4849(2) 0.065(2) Uani 0.869(6) 1 d D U P A 1
H29A H 0.660663 0.779727 0.470712 0.098 Uiso 0.869(6) 1 calc R U P A 1
H29B H 0.831205 0.775255 0.462804 0.098 Uiso 0.869(6) 1 calc R U P A 1
H29C H 0.763220 0.769853 0.523801 0.098 Uiso 0.869(6) 1 calc R U P A 1
C30A C 0.5424(3) 0.5072(2) 0.49779(12) 0.0211(5) Uani 0.869(6) 1 d D U P A 1
H30A H 0.564612 0.477949 0.462641 0.025 Uiso 0.869(6) 1 calc R U P A 1
C31A C 0.4276(3) 0.4667(3) 0.52795(14) 0.0191(6) Uani 0.869(6) 1 d D U P A 1
C32A C 0.3523(4) 0.3729(3) 0.50343(16) 0.0244(7) Uani 0.869(6) 1 d D U P A 1
H32A H 0.274272 0.352008 0.529668 0.029 Uiso 0.869(6) 1 calc R U P A 1
C33A C 0.4573(5) 0.2823(3) 0.4984(3) 0.0365(11) Uani 0.869(6) 1 d D U P A 1
H33A H 0.531361 0.298974 0.470874 0.055 Uiso 0.869(6) 1 calc R U P A 1
H33B H 0.405069 0.220514 0.486554 0.055 Uiso 0.869(6) 1 calc R U P A 1
H33C H 0.502609 0.269594 0.534485 0.055 Uiso 0.869(6) 1 calc R U P A 1
C34A C 0.2825(5) 0.3982(3) 0.44736(16) 0.0316(8) Uani 0.869(6) 1 d D U P A 1
H34A H 0.216363 0.456391 0.451888 0.047 Uiso 0.869(6) 1 calc R U P A 1
H34B H 0.229241 0.337957 0.433952 0.047 Uiso 0.869(6) 1 calc R U P A 1
H34C H 0.357147 0.416438 0.420407 0.047 Uiso 0.869(6) 1 calc R U P A 1
C20B C 0.402(4) 0.529(3) 0.5807(15) 0.019(3) Uani 0.131(6) 1 d D U P A 2
C21B C 0.488(3) 0.592(3) 0.6145(10) 0.021(2) Uani 0.131(6) 1 d D U P A 2
C22B C 0.457(3) 0.640(2) 0.6702(10) 0.026(2) Uani 0.131(6) 1 d D U P A 2
H22B H 0.356382 0.625418 0.682482 0.031 Uiso 0.131(6) 1 calc R U P A 2
C23B C 0.568(3) 0.596(3) 0.7117(10) 0.051(5) Uani 0.131(6) 1 d D . P A 2
H23D H 0.551142 0.625439 0.748629 0.077 Uiso 0.131(6) 1 calc R U P A 2
H23E H 0.558649 0.520719 0.713599 0.077 Uiso 0.131(6) 1 calc R U P A 2
H23F H 0.665341 0.613752 0.699339 0.077 Uiso 0.131(6) 1 calc R U P A 2
C24B C 0.485(4) 0.7557(19) 0.6643(15) 0.041(4) Uani 0.131(6) 1 d D U P A 2
H24D H 0.466064 0.789906 0.699845 0.061 Uiso 0.131(6) 1 calc R U P A 2
H24E H 0.585408 0.766987 0.653620 0.061 Uiso 0.131(6) 1 calc R U P A 2
H24F H 0.421659 0.784248 0.635686 0.061 Uiso 0.131(6) 1 calc R U P A 2
C25B C 0.617(2) 0.6197(17) 0.5883(8) 0.020(2) Uani 0.131(6) 1 d D U P A 2
H25B H 0.677739 0.666458 0.607491 0.024 Uiso 0.131(6) 1 calc R U P A 2
C26B C 0.663(2) 0.5855(15) 0.5376(9) 0.028(3) Uani 0.131(6) 1 d D . P A 2
C27B C 0.800(2) 0.6307(16) 0.5112(10) 0.042(4) Uani 0.131(6) 1 d D . P A 2
H27B H 0.864564 0.630188 0.544259 0.051 Uiso 0.131(6) 1 calc R U P A 2
C28B C 0.878(5) 0.559(3) 0.4748(16) 0.050(4) Uani 0.131(6) 1 d D U P A 2
H28D H 0.867470 0.488315 0.489026 0.074 Uiso 0.131(6) 1 calc R U P A 2
H28E H 0.838534 0.562464 0.437080 0.074 Uiso 0.131(6) 1 calc R U P A 2
H28F H 0.979894 0.577389 0.474035 0.074 Uiso 0.131(6) 1 calc R U P A 2
C29B C 0.798(5) 0.740(2) 0.500(2) 0.064(5) Uani 0.131(6) 1 d D U P A 2
H29D H 0.740613 0.775570 0.527945 0.097 Uiso 0.131(6) 1 calc R U P A 2
H29E H 0.895940 0.766794 0.499874 0.097 Uiso 0.131(6) 1 calc R U P A 2
H29F H 0.754579 0.751869 0.462918 0.097 Uiso 0.131(6) 1 calc R U P A 2
C30B C 0.586(2) 0.5107(16) 0.5116(8) 0.023(2) Uani 0.131(6) 1 d D U P A 2
H30B H 0.619147 0.484471 0.477036 0.028 Uiso 0.131(6) 1 calc R U P A 2
C31B C 0.459(2) 0.471(2) 0.5353(10) 0.018(2) Uani 0.131(6) 1 d D U P A 2
C32B C 0.386(3) 0.383(2) 0.5058(12) 0.027(2) Uani 0.131(6) 1 d D U P A 2
H32B H 0.305725 0.356932 0.529403 0.032 Uiso 0.131(6) 1 calc R U P A 2
C33B C 0.495(4) 0.294(2) 0.496(2) 0.035(4) Uani 0.131(6) 1 d D U P A 2
H33D H 0.447016 0.237118 0.476591 0.052 Uiso 0.131(6) 1 calc R U P A 2
H33E H 0.575077 0.319150 0.473122 0.052 Uiso 0.131(6) 1 calc R U P A 2
H33F H 0.531943 0.269599 0.531681 0.052 Uiso 0.131(6) 1 calc R U P A 2
C34B C 0.327(3) 0.411(2) 0.4485(11) 0.031(4) Uani 0.131(6) 1 d D U P A 2
H34D H 0.281618 0.350055 0.431866 0.047 Uiso 0.131(6) 1 calc R U P A 2
H34E H 0.255810 0.466045 0.452196 0.047 Uiso 0.131(6) 1 calc R U P A 2
H34F H 0.405752 0.434301 0.424563 0.047 Uiso 0.131(6) 1 calc R 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
S1 O2 1.4369(16) . ?
S1 O1 1.4479(17) . ?
S1 N1 1.5951(17) . ?
S1 C20A 1.776(4) . ?
S1 C20B 1.88(3) . ?
P1 N1 1.5763(18) . ?
P1 C1 1.7899(19) . ?
P1 C13 1.803(2) . ?
P1 C19 1.808(2) . ?
C1 C2 1.385(3) . ?
C1 C6 1.398(3) . ?
C2 C3 1.391(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.530(3) . ?
C7 C14 1.523(3) . ?
C7 C8 1.529(3) . ?
C7 H7 1.0000 . ?
C8 C9 1.392(3) . ?
C8 C13 1.402(3) . ?
C9 C10 1.392(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(3) . ?
C12 H12 0.9500 . ?
C14 C15 1.387(3) . ?
C14 C19 1.406(3) . ?
C15 C16 1.394(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(3) . ?
C18 H18 0.9500 . ?
C20A C21A 1.414(4) . ?
C20A C31A 1.415(4) . ?
C21A C25A 1.397(4) . ?
C21A C22A 1.529(3) . ?
C22A C24A 1.529(4) . ?
C22A C23A 1.530(4) . ?
C22A H22A 1.0000 . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A C26A 1.386(3) . ?
C25A H25A 0.9500 . ?
C26A C30A 1.388(4) . ?
C26A C27A 1.520(3) . ?
C27A C29A 1.503(5) . ?
C27A C28A 1.504(6) . ?
C27A H27A 1.0000 . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C28A H28C 0.9800 . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C30A C31A 1.395(4) . ?
C30A H30A 0.9500 . ?
C31A C32A 1.524(4) . ?
C32A C33A 1.533(4) . ?
C32A C34A 1.534(4) . ?
C32A H32A 1.0000 . ?
C33A H33A 0.9800 . ?
C33A H33B 0.9800 . ?
C33A H33C 0.9800 . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
C20B C21B 1.40(2) . ?
C20B C31B 1.43(2) . ?
C21B C25B 1.40(2) . ?
C21B C22B 1.50(2) . ?
C22B C24B 1.53(2) . ?
C22B C23B 1.55(2) . ?
C22B H22B 1.0000 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25B C26B 1.366(19) . ?
C25B H25B 0.9500 . ?
C26B C30B 1.356(19) . ?
C26B C27B 1.541(18) . ?
C27B C29B 1.45(2) . ?
C27B C28B 1.47(2) . ?
C27B H27B 1.0000 . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 0.9800 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
C30B C31B 1.42(2) . ?
C30B H30B 0.9500 . ?
C31B C32B 1.50(2) . ?
C32B C34B 1.53(2) . ?
C32B C33B 1.56(2) . ?
C32B H32B 1.0000 . ?
C33B H33D 0.9800 . ?
C33B H33E 0.9800 . ?
C33B H33F 0.9800 . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 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
O2 S1 O1 114.04(11) . . ?
O2 S1 N1 111.72(10) . . ?
O1 S1 N1 111.14(10) . . ?
O2 S1 C20A 105.6(2) . . ?
O1 S1 C20A 111.97(12) . . ?
N1 S1 C20A 101.60(19) . . ?
O2 S1 C20B 106.1(13) . . ?
O1 S1 C20B 106.2(7) . . ?
N1 S1 C20B 107.2(15) . . ?
N1 P1 C1 111.05(9) . . ?
N1 P1 C13 119.41(10) . . ?
C1 P1 C13 99.10(9) . . ?
N1 P1 C19 123.76(9) . . ?
C1 P1 C19 100.49(9) . . ?
C13 P1 C19 98.93(10) . . ?
P1 N1 S1 124.81(11) . . ?
C2 C1 C6 121.81(18) . . ?
C2 C1 P1 126.18(16) . . ?
C6 C1 P1 111.88(15) . . ?
C1 C2 C3 118.5(2) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 120.1(2) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 121.2(2) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 119.5(2) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 118.9(2) . . ?
C5 C6 C7 123.7(2) . . ?
C1 C6 C7 117.34(17) . . ?
C14 C7 C8 107.78(17) . . ?
C14 C7 C6 109.14(17) . . ?
C8 C7 C6 107.53(17) . . ?
C14 C7 H7 110.8 . . ?
C8 C7 H7 110.8 . . ?
C6 C7 H7 110.8 . . ?
C9 C8 C13 119.2(2) . . ?
C9 C8 C7 124.0(2) . . ?
C13 C8 C7 116.81(18) . . ?
C8 C9 C10 119.3(2) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 121.0(2) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 120.4(2) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C13 C12 C11 118.5(2) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C12 C13 C8 121.56(19) . . ?
C12 C13 P1 126.43(17) . . ?
C8 C13 P1 112.00(15) . . ?
C15 C14 C19 118.8(2) . . ?
C15 C14 C7 123.6(2) . . ?
C19 C14 C7 117.56(18) . . ?
C14 C15 C16 120.0(2) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C17 C16 C15 120.5(2) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 120.5(2) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C19 C18 C17 118.7(2) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C14 121.35(19) . . ?
C18 C19 P1 127.47(16) . . ?
C14 C19 P1 111.17(15) . . ?
C21A C20A C31A 120.4(3) . . ?
C21A C20A S1 122.4(3) . . ?
C31A C20A S1 116.5(3) . . ?
C25A C21A C20A 118.1(3) . . ?
C25A C21A C22A 116.6(3) . . ?
C20A C21A C22A 125.4(3) . . ?
C24A C22A C21A 111.4(3) . . ?
C24A C22A C23A 111.5(3) . . ?
C21A C22A C23A 110.5(3) . . ?
C24A C22A H22A 107.7 . . ?
C21A C22A H22A 107.7 . . ?
C23A C22A H22A 107.7 . . ?
C22A C23A H23A 109.5 . . ?
C22A C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C22A C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C22A C24A H24A 109.5 . . ?
C22A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C22A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C26A C25A C21A 122.6(2) . . ?
C26A C25A H25A 118.7 . . ?
C21A C25A H25A 118.7 . . ?
C25A C26A C30A 117.8(2) . . ?
C25A C26A C27A 121.8(2) . . ?
C30A C26A C27A 120.4(2) . . ?
C29A C27A C28A 113.2(4) . . ?
C29A C27A C26A 112.5(3) . . ?
C28A C27A C26A 110.1(3) . . ?
C29A C27A H27A 106.9 . . ?
C28A C27A H27A 106.9 . . ?
C26A C27A H27A 106.9 . . ?
C27A C28A H28A 109.5 . . ?
C27A C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C27A C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C27A C29A H29A 109.5 . . ?
C27A C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C27A C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C26A C30A C31A 122.7(2) . . ?
C26A C30A H30A 118.6 . . ?
C31A C30A H30A 118.6 . . ?
C30A C31A C20A 117.9(3) . . ?
C30A C31A C32A 116.9(2) . . ?
C20A C31A C32A 125.1(3) . . ?
C31A C32A C33A 110.4(3) . . ?
C31A C32A C34A 111.4(3) . . ?
C33A C32A C34A 111.4(3) . . ?
C31A C32A H32A 107.8 . . ?
C33A C32A H32A 107.8 . . ?
C34A C32A H32A 107.8 . . ?
C32A C33A H33A 109.5 . . ?
C32A C33A H33B 109.5 . . ?
H33A C33A H33B 109.5 . . ?
C32A C33A H33C 109.5 . . ?
H33A C33A H33C 109.5 . . ?
H33B C33A H33C 109.5 . . ?
C32A C34A H34A 109.5 . . ?
C32A C34A H34B 109.5 . . ?
H34A C34A H34B 109.5 . . ?
C32A C34A H34C 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C21B C20B C31B 123(2) . . ?
C21B C20B S1 118.6(19) . . ?
C31B C20B S1 115.5(16) . . ?
C25B C21B C20B 112.1(18) . . ?
C25B C21B C22B 117.4(19) . . ?
C20B C21B C22B 130(2) . . ?
C21B C22B C24B 107(2) . . ?
C21B C22B C23B 107(2) . . ?
C24B C22B C23B 108(2) . . ?
C21B C22B H22B 111.6 . . ?
C24B C22B H22B 111.6 . . ?
C23B C22B H22B 111.6 . . ?
C22B C23B H23D 109.5 . . ?
C22B C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C22B C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C22B C24B H24D 109.5 . . ?
C22B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C22B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C26B C25B C21B 125.8(17) . . ?
C26B C25B H25B 117.1 . . ?
C21B C25B H25B 117.1 . . ?
C30B C26B C25B 118.8(15) . . ?
C30B C26B C27B 121.0(16) . . ?
C25B C26B C27B 120.2(16) . . ?
C29B C27B C28B 121(2) . . ?
C29B C27B C26B 116(2) . . ?
C28B C27B C26B 114(2) . . ?
C29B C27B H27B 99.7 . . ?
C28B C27B H27B 99.7 . . ?
C26B C27B H27B 99.7 . . ?
C27B C28B H28D 109.5 . . ?
C27B C28B H28E 109.5 . . ?
H28D C28B H28E 109.5 . . ?
C27B C28B H28F 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
C27B C29B H29D 109.5 . . ?
C27B C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C27B C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C26B C30B C31B 121.0(16) . . ?
C26B C30B H30B 119.5 . . ?
C31B C30B H30B 119.5 . . ?
C30B C31B C20B 115.3(18) . . ?
C30B C31B C32B 117.5(18) . . ?
C20B C31B C32B 126.5(19) . . ?
C31B C32B C34B 114(2) . . ?
C31B C32B C33B 110(2) . . ?
C34B C32B C33B 106(2) . . ?
C31B C32B H32B 108.9 . . ?
C34B C32B H32B 108.9 . . ?
C33B C32B H32B 108.9 . . ?
C32B C33B H33D 109.5 . . ?
C32B C33B H33E 109.5 . . ?
H33D C33B H33E 109.5 . . ?
C32B C33B H33F 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C32B C34B H34D 109.5 . . ?
C32B C34B H34E 109.5 . . ?
H34D C34B H34E 109.5 . . ?
C32B C34B H34F 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 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
C1 P1 N1 S1 163.40(13) . . . . ?
C13 P1 N1 S1 -82.30(15) . . . . ?
C19 P1 N1 S1 43.94(18) . . . . ?
O2 S1 N1 P1 -81.17(16) . . . . ?
O1 S1 N1 P1 47.45(16) . . . . ?
C20A S1 N1 P1 166.71(18) . . . . ?
C20B S1 N1 P1 163.1(9) . . . . ?
N1 P1 C1 C2 0.1(2) . . . . ?
C13 P1 C1 C2 -126.4(2) . . . . ?
C19 P1 C1 C2 132.70(19) . . . . ?
N1 P1 C1 C6 176.01(15) . . . . ?
C13 P1 C1 C6 49.53(16) . . . . ?
C19 P1 C1 C6 -51.39(17) . . . . ?
C6 C1 C2 C3 0.0(3) . . . . ?
P1 C1 C2 C3 175.51(18) . . . . ?
C1 C2 C3 C4 -0.5(3) . . . . ?
C2 C3 C4 C5 0.9(4) . . . . ?
C3 C4 C5 C6 -0.7(4) . . . . ?
C4 C5 C6 C1 0.1(3) . . . . ?
C4 C5 C6 C7 -178.1(2) . . . . ?
C2 C1 C6 C5 0.2(3) . . . . ?
P1 C1 C6 C5 -175.90(17) . . . . ?
C2 C1 C6 C7 178.57(19) . . . . ?
P1 C1 C6 C7 2.5(2) . . . . ?
C5 C6 C7 C14 -125.6(2) . . . . ?
C1 C6 C7 C14 56.1(2) . . . . ?
C5 C6 C7 C8 117.7(2) . . . . ?
C1 C6 C7 C8 -60.5(2) . . . . ?
C14 C7 C8 C9 119.4(2) . . . . ?
C6 C7 C8 C9 -123.1(2) . . . . ?
C14 C7 C8 C13 -60.3(2) . . . . ?
C6 C7 C8 C13 57.2(2) . . . . ?
C13 C8 C9 C10 -0.1(3) . . . . ?
C7 C8 C9 C10 -179.8(2) . . . . ?
C8 C9 C10 C11 -1.1(4) . . . . ?
C9 C10 C11 C12 1.1(4) . . . . ?
C10 C11 C12 C13 0.1(3) . . . . ?
C11 C12 C13 C8 -1.3(3) . . . . ?
C11 C12 C13 P1 177.50(17) . . . . ?
C9 C8 C13 C12 1.3(3) . . . . ?
C7 C8 C13 C12 -178.95(19) . . . . ?
C9 C8 C13 P1 -177.65(17) . . . . ?
C7 C8 C13 P1 2.1(2) . . . . ?
N1 P1 C13 C12 8.4(2) . . . . ?
C1 P1 C13 C12 128.90(19) . . . . ?
C19 P1 C13 C12 -128.88(19) . . . . ?
N1 P1 C13 C8 -172.72(14) . . . . ?
C1 P1 C13 C8 -52.20(17) . . . . ?
C19 P1 C13 C8 50.03(17) . . . . ?
C8 C7 C14 C15 -120.3(2) . . . . ?
C6 C7 C14 C15 123.2(2) . . . . ?
C8 C7 C14 C19 57.6(2) . . . . ?
C6 C7 C14 C19 -58.9(2) . . . . ?
C19 C14 C15 C16 -1.7(3) . . . . ?
C7 C14 C15 C16 176.3(2) . . . . ?
C14 C15 C16 C17 0.7(3) . . . . ?
C15 C16 C17 C18 0.4(3) . . . . ?
C16 C17 C18 C19 -0.5(3) . . . . ?
C17 C18 C19 C14 -0.5(3) . . . . ?
C17 C18 C19 P1 -178.98(16) . . . . ?
C15 C14 C19 C18 1.6(3) . . . . ?
C7 C14 C19 C18 -176.50(19) . . . . ?
C15 C14 C19 P1 -179.71(16) . . . . ?
C7 C14 C19 P1 2.2(2) . . . . ?
N1 P1 C19 C18 -8.3(2) . . . . ?
C1 P1 C19 C18 -132.57(19) . . . . ?
C13 P1 C19 C18 126.37(18) . . . . ?
N1 P1 C19 C14 173.08(14) . . . . ?
C1 P1 C19 C14 48.80(16) . . . . ?
C13 P1 C19 C14 -52.26(16) . . . . ?
O2 S1 C20A C21A 131.3(5) . . . . ?
O1 S1 C20A C21A 6.7(6) . . . . ?
N1 S1 C20A C21A -112.0(5) . . . . ?
O2 S1 C20A C31A -38.6(5) . . . . ?
O1 S1 C20A C31A -163.3(4) . . . . ?
N1 S1 C20A C31A 78.1(4) . . . . ?
C31A C20A C21A C25A 6.6(7) . . . . ?
S1 C20A C21A C25A -163.0(4) . . . . ?
C31A C20A C21A C22A -172.8(4) . . . . ?
S1 C20A C21A C22A 17.7(7) . . . . ?
C25A C21A C22A C24A 66.2(5) . . . . ?
C20A C21A C22A C24A -114.5(5) . . . . ?
C25A C21A C22A C23A -58.4(4) . . . . ?
C20A C21A C22A C23A 121.0(5) . . . . ?
C20A C21A C25A C26A -0.6(6) . . . . ?
C22A C21A C25A C26A 178.8(3) . . . . ?
C21A C25A C26A C30A -5.4(5) . . . . ?
C21A C25A C26A C27A 176.1(3) . . . . ?
C25A C26A C27A C29A -41.4(4) . . . . ?
C30A C26A C27A C29A 140.0(3) . . . . ?
C25A C26A C27A C28A 85.9(4) . . . . ?
C30A C26A C27A C28A -92.6(4) . . . . ?
C25A C26A C30A C31A 5.6(4) . . . . ?
C27A C26A C30A C31A -175.8(3) . . . . ?
C26A C30A C31A C20A 0.2(5) . . . . ?
C26A C30A C31A C32A -176.0(3) . . . . ?
C21A C20A C31A C30A -6.3(7) . . . . ?
S1 C20A C31A C30A 163.8(3) . . . . ?
C21A C20A C31A C32A 169.5(4) . . . . ?
S1 C20A C31A C32A -20.4(6) . . . . ?
C30A C31A C32A C33A 61.5(4) . . . . ?
C20A C31A C32A C33A -114.4(5) . . . . ?
C30A C31A C32A C34A -62.9(4) . . . . ?
C20A C31A C32A C34A 121.2(5) . . . . ?
O2 S1 C20B C21B 143(3) . . . . ?
O1 S1 C20B C21B 22(4) . . . . ?
N1 S1 C20B C21B -97(3) . . . . ?
O2 S1 C20B C31B -57(3) . . . . ?
O1 S1 C20B C31B -178(3) . . . . ?
N1 S1 C20B C31B 63(3) . . . . ?
C31B C20B C21B C25B 21(6) . . . . ?
S1 C20B C21B C25B 180(3) . . . . ?
C31B C20B C21B C22B -165(3) . . . . ?
S1 C20B C21B C22B -7(6) . . . . ?
C25B C21B C22B C24B 48(4) . . . . ?
C20B C21B C22B C24B -126(4) . . . . ?
C25B C21B C22B C23B -68(3) . . . . ?
C20B C21B C22B C23B 119(4) . . . . ?
C20B C21B C25B C26B -5(5) . . . . ?
C22B C21B C25B C26B -179(2) . . . . ?
C21B C25B C26B C30B -7(4) . . . . ?
C21B C25B C26B C27B 174(3) . . . . ?
C30B C26B C27B C29B 120(3) . . . . ?
C25B C26B C27B C29B -61(4) . . . . ?
C30B C26B C27B C28B -29(4) . . . . ?
C25B C26B C27B C28B 150(3) . . . . ?
C25B C26B C30B C31B 2(3) . . . . ?
C27B C26B C30B C31B -178(2) . . . . ?
C26B C30B C31B C20B 13(4) . . . . ?
C26B C30B C31B C32B -176(2) . . . . ?
C21B C20B C31B C30B -26(5) . . . . ?
S1 C20B C31B C30B 175(2) . . . . ?
C21B C20B C31B C32B 164(3) . . . . ?
S1 C20B C31B C32B 5(5) . . . . ?
C30B C31B C32B C34B -65(3) . . . . ?
C20B C31B C32B C34B 105(4) . . . . ?
C30B C31B C32B C33B 53(3) . . . . ?
C20B C31B C32B C33B -136(4) . . . . ?

_refine_diff_density_max         0.298
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.053



# start Validation Reply Form
_vrf_PLAT220_nt0726_LHG141_100K  
;
PROBLEM: NonSolvent Resd 1  C   Ueq(max) / Ueq(min) Range        4.6 Ratio 
RESPONSE: Minor disorder (14% occupancy) of the 2,4,6-triisopropylbenzene 
fragment.
;
_vrf_PLAT222_nt0726_LHG141_100K  
;
PROBLEM: NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        4.9 Ratio 
RESPONSE: Minor disorder (14% occupancy) of the 2,4,6-triisopropylbenzene 
fragment.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1231_SMC037
_database_code_depnum_ccdc_archive 'CCDC 2313774'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        
'N-(p-tritylphenyl)-9-phosphatriptycene-iminium tetrafluoroborate'
_chemical_name_common            
'N-(p-tritylphenyl)-9-phosphatriptycene-iminium tetrafluoroborate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H33 N P 1+, B F4 1-'
_chemical_formula_sum            'C44 H33 B F4 N P'
_chemical_formula_weight         693.49

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'
N N 0.0311 0.0180 '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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

_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, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   12.867(4)
_cell_length_b                   13.069(4)
_cell_length_c                   21.505(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3616.2(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    644
_cell_measurement_theta_max      40.958
_cell_measurement_theta_min      4.112

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             1440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.113
_shelx_estimated_absorpt_T_min   0.962
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0907 before and 0.0581 after correction.
The Ratio of minimum to maximum transmission is 0.5680.
The λ/2 correction factor is Not present.
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   microsource
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_reflns_number            3086
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.111
_diffrn_reflns_theta_max         48.240
_diffrn_reflns_theta_full        48.240
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measured_fraction_theta_full 0.891
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_Laue_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.715
_diffrn_reflns_point_group_measured_fraction_full 0.715
_reflns_number_total             2459
_reflns_number_gt                1312
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.547
_reflns_Friedel_fraction_max     0.525
_reflns_Friedel_fraction_full    0.525

_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0780P)²+8.4136P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 330 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(7)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         2459
_refine_ls_number_parameters     461
_refine_ls_number_restraints     379
_refine_ls_R_factor_all          0.1643
_refine_ls_R_factor_gt           0.0792
_refine_ls_wR_factor_ref         0.2302
_refine_ls_wR_factor_gt          0.1704
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      0.975
_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
F1 F 0.4018(18) 0.668(3) 0.5977(14) 0.308(15) Uani 1 1 d D . . . .
F2 F 0.532(2) 0.642(2) 0.6527(12) 0.289(16) Uani 1 1 d D . . . .
F3 F 0.5270(17) 0.774(2) 0.6056(15) 0.251(11) Uani 1 1 d D . . . .
F4 F 0.4108(16) 0.742(2) 0.6830(12) 0.255(13) Uani 1 1 d D . . . .
B2 B 0.465(2) 0.711(2) 0.6362(13) 0.164(12) Uani 1 1 d D . . . .
P1 P 0.3123(4) 0.2014(5) 0.5985(3) 0.0806(19) Uani 1 1 d . . . . .
N2 N 0.2390(12) 0.3010(15) 0.5879(10) 0.094(6) Uani 1 1 d . . . . .
H2A H 0.190183 0.309386 0.614730 0.113 Uiso 1 1 calc R U . . .
C1 C 0.2842(17) 0.1225(18) 0.6623(11) 0.080(7) Uani 1 1 d . . . . .
C2 C 0.206(2) 0.137(2) 0.7079(13) 0.115(9) Uani 1 1 d . . . . .
H2 H 0.158693 0.190509 0.704864 0.139 Uiso 1 1 calc R U . . .
C3 C 0.200(2) 0.066(3) 0.7584(14) 0.124(11) Uani 1 1 d . . . . .
H3 H 0.149924 0.076875 0.788781 0.149 Uiso 1 1 calc R U . . .
C4 C 0.264(2) -0.017(2) 0.7650(13) 0.110(8) Uani 1 1 d . . . . .
H4 H 0.256949 -0.063097 0.797583 0.132 Uiso 1 1 calc R U . . .
C5 C 0.3384(18) -0.0258(17) 0.7195(11) 0.078(7) Uani 1 1 d . . . . .
H5 H 0.385923 -0.079217 0.722564 0.094 Uiso 1 1 calc R U . . .
C6 C 0.3468(17) 0.041(2) 0.6687(12) 0.084(7) Uani 1 1 d . . . . .
C7 C 0.4331(15) 0.0318(16) 0.6170(10) 0.083(6) Uani 1 1 d . . . . .
H7 H 0.477112 -0.028331 0.624041 0.099 Uiso 1 1 calc R U . . .
C8 C 0.4963(16) 0.1297(19) 0.6187(11) 0.086(7) Uani 1 1 d . . . . .
C9 C 0.6059(17) 0.128(2) 0.6316(14) 0.121(10) Uani 1 1 d . . . . .
H9 H 0.640658 0.066410 0.637615 0.145 Uiso 1 1 calc R U . . .
C10 C 0.659(2) 0.221(3) 0.6348(17) 0.148(13) Uani 1 1 d . . . . .
H10 H 0.730409 0.221188 0.641457 0.177 Uiso 1 1 calc R U . . .
C11 C 0.609(2) 0.311(2) 0.6283(13) 0.120(10) Uani 1 1 d . . . . .
H11 H 0.644320 0.372594 0.632847 0.143 Uiso 1 1 calc R U . . .
C12 C 0.5024(16) 0.3113(18) 0.6147(10) 0.086(7) Uani 1 1 d . . . . .
H12 H 0.467476 0.372728 0.608412 0.103 Uiso 1 1 calc R U . . .
C13 C 0.4522(14) 0.2234(19) 0.6109(12) 0.085(7) Uani 1 1 d . . . . .
C14 C 0.3770(16) 0.0251(19) 0.5543(12) 0.078(6) Uani 1 1 d . . . . .
C15 C 0.3847(19) -0.059(2) 0.5157(13) 0.103(8) Uani 1 1 d . . . . .
H15 H 0.428125 -0.113639 0.525341 0.123 Uiso 1 1 calc R U . . .
C16 C 0.3249(19) -0.059(2) 0.4617(13) 0.105(8) Uani 1 1 d . . . . .
H16 H 0.327190 -0.116084 0.435957 0.126 Uiso 1 1 calc R U . . .
C17 C 0.261(2) 0.023(2) 0.4445(14) 0.113(9) Uani 1 1 d . . . . .
H17 H 0.224284 0.022854 0.407424 0.136 Uiso 1 1 calc R U . . .
C18 C 0.2559(16) 0.107(2) 0.4855(12) 0.090(7) Uani 1 1 d . . . . .
H18 H 0.213631 0.162740 0.476309 0.108 Uiso 1 1 calc R U . . .
C19 C 0.3141(17) 0.1058(18) 0.5401(11) 0.080(7) Uani 1 1 d . . . . .
C20 C 0.2445(18) 0.3771(19) 0.5397(12) 0.077(6) Uani 1 1 d . . . . .
C21 C 0.1668(18) 0.4456(19) 0.5354(12) 0.090(7) Uani 1 1 d . . . . .
H21 H 0.112264 0.442866 0.563689 0.108 Uiso 1 1 calc R U . . .
C22 C 0.1664(19) 0.5208(18) 0.4892(12) 0.095(8) Uani 1 1 d . . . . .
H22 H 0.111109 0.566497 0.486962 0.114 Uiso 1 1 calc R U . . .
C23 C 0.247(2) 0.5283(17) 0.4466(12) 0.085(6) Uani 1 1 d . . . . .
C24 C 0.3257(17) 0.4520(17) 0.4489(12) 0.086(7) Uani 1 1 d . . . . .
H24 H 0.379888 0.453750 0.420300 0.103 Uiso 1 1 calc R U . . .
C25 C 0.3225(16) 0.3739(18) 0.4939(10) 0.074(6) Uani 1 1 d . . . . .
H25 H 0.370946 0.321104 0.493330 0.089 Uiso 1 1 calc R U . . .
C26 C 0.2483(19) 0.5996(19) 0.3910(12) 0.084(5) Uani 1 1 d . . . . .
C27 C 0.160(2) 0.683(2) 0.3973(14) 0.098(8) Uani 1 1 d . . . . .
C28 C 0.150(2) 0.744(2) 0.4471(13) 0.100(8) Uani 1 1 d . . . . .
H28 H 0.194591 0.733053 0.480680 0.120 Uiso 1 1 calc R U . . .
C29 C 0.079(2) 0.822(2) 0.4509(14) 0.120(10) Uani 1 1 d . . . . .
H29 H 0.075471 0.862259 0.486458 0.145 Uiso 1 1 calc R U . . .
C30 C 0.012(3) 0.840(3) 0.4026(18) 0.146(13) Uani 1 1 d . . . . .
H30 H -0.040963 0.888661 0.405627 0.176 Uiso 1 1 calc R U . . .
C31 C 0.025(3) 0.785(3) 0.3514(18) 0.173(16) Uani 1 1 d . . . . .
H31 H -0.013992 0.801014 0.316324 0.207 Uiso 1 1 calc R U . . .
C32 C 0.098(2) 0.702(3) 0.3479(14) 0.131(11) Uani 1 1 d . . . . .
H32 H 0.102982 0.662626 0.312145 0.157 Uiso 1 1 calc R U . . .
C33 C 0.3519(19) 0.6636(19) 0.3854(13) 0.087(7) Uani 1 1 d . . . . .
C34 C 0.4256(18) 0.6683(18) 0.4341(14) 0.102(8) Uani 1 1 d . . . . .
H34 H 0.417151 0.631196 0.470635 0.122 Uiso 1 1 calc R U . . .
C35 C 0.511(2) 0.731(2) 0.4248(15) 0.117(10) Uani 1 1 d . . . . .
H35 H 0.562637 0.732122 0.454947 0.140 Uiso 1 1 calc R U . . .
C36 C 0.522(2) 0.788(2) 0.3753(16) 0.136(12) Uani 1 1 d . . . . .
H36 H 0.581601 0.828337 0.372063 0.164 Uiso 1 1 calc R U . . .
C37 C 0.451(2) 0.793(2) 0.3281(16) 0.128(10) Uani 1 1 d . . . . .
H37 H 0.461273 0.834650 0.293641 0.153 Uiso 1 1 calc R U . . .
C38 C 0.3602(19) 0.731(2) 0.3334(13) 0.098(8) Uani 1 1 d . . . . .
H38 H 0.307582 0.735290 0.303906 0.118 Uiso 1 1 calc R U . . .
C39 C 0.2338(19) 0.5347(18) 0.3348(12) 0.088(7) Uani 1 1 d . . . . .
C40 C 0.141(2) 0.480(3) 0.3266(15) 0.148(14) Uani 1 1 d . . . . .
H40 H 0.088443 0.489171 0.355773 0.177 Uiso 1 1 calc R U . . .
C41 C 0.123(3) 0.414(3) 0.2793(16) 0.149(14) Uani 1 1 d . . . . .
H41 H 0.059712 0.379648 0.276985 0.179 Uiso 1 1 calc R U . . .
C42 C 0.195(3) 0.399(3) 0.2357(18) 0.166(16) Uani 1 1 d . . . . .
H42 H 0.181694 0.356876 0.202022 0.199 Uiso 1 1 calc R U . . .
C43 C 0.296(3) 0.449(3) 0.2411(16) 0.149(12) Uani 1 1 d . . . . .
H43 H 0.349149 0.438940 0.212430 0.179 Uiso 1 1 calc R U . . .
C44 C 0.307(2) 0.512(2) 0.2911(13) 0.117(10) Uani 1 1 d . . . . .
H44 H 0.371693 0.543766 0.295843 0.141 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
F1 B2 1.29(2) . ?
F2 B2 1.30(2) . ?
F3 B2 1.32(2) . ?
F4 B2 1.292(19) . ?
P1 N2 1.624(18) . ?
P1 C1 1.75(2) . ?
P1 C19 1.77(2) . ?
P1 C13 1.843(18) . ?
N2 C20 1.44(3) . ?
N2 H2A 0.8600 . ?
C1 C6 1.34(3) . ?
C1 C2 1.42(3) . ?
C2 C3 1.43(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.36(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.41(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.58(3) . ?
C7 C8 1.52(3) . ?
C7 C14 1.53(3) . ?
C7 H7 0.9800 . ?
C8 C13 1.36(3) . ?
C8 C9 1.44(3) . ?
C9 C10 1.40(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.35(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.40(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.32(3) . ?
C12 H12 0.9300 . ?
C14 C19 1.36(3) . ?
C14 C15 1.38(3) . ?
C15 C16 1.39(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.40(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.41(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.39(3) . ?
C18 H18 0.9300 . ?
C20 C21 1.34(3) . ?
C20 C25 1.41(3) . ?
C21 C22 1.40(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.39(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.42(3) . ?
C23 C26 1.52(3) . ?
C24 C25 1.41(3) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C39 1.49(3) . ?
C26 C33 1.58(3) . ?
C26 C27 1.58(3) . ?
C27 C28 1.34(3) . ?
C27 C32 1.35(3) . ?
C28 C29 1.38(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.37(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.33(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.43(4) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.41(3) . ?
C33 C38 1.43(3) . ?
C34 C35 1.38(3) . ?
C34 H34 0.9300 . ?
C35 C36 1.31(3) . ?
C35 H35 0.9300 . ?
C36 C37 1.37(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.42(3) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 C44 1.37(3) . ?
C39 C40 1.41(3) . ?
C40 C41 1.35(4) . ?
C40 H40 0.9300 . ?
C41 C42 1.34(4) . ?
C41 H41 0.9300 . ?
C42 C43 1.46(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.36(4) . ?
C43 H43 0.9300 . ?
C44 H44 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
F1 B2 F4 107(3) . . ?
F1 B2 F2 107(3) . . ?
F4 B2 F2 111(3) . . ?
F1 B2 F3 109(3) . . ?
F4 B2 F3 121(3) . . ?
F2 B2 F3 100(2) . . ?
N2 P1 C1 117.5(12) . . ?
N2 P1 C19 118.2(11) . . ?
C1 P1 C19 98.2(12) . . ?
N2 P1 C13 117.6(11) . . ?
C1 P1 C13 100.3(11) . . ?
C19 P1 C13 101.6(11) . . ?
C20 N2 P1 128.8(17) . . ?
C20 N2 H2A 115.6 . . ?
P1 N2 H2A 115.6 . . ?
C6 C1 C2 117(2) . . ?
C6 C1 P1 115(2) . . ?
C2 C1 P1 128(2) . . ?
C1 C2 C3 118(3) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 124(3) . . ?
C4 C3 H3 117.8 . . ?
C2 C3 H3 117.8 . . ?
C3 C4 C5 114(3) . . ?
C3 C4 H4 122.8 . . ?
C5 C4 H4 122.8 . . ?
C4 C5 C6 123(3) . . ?
C4 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C1 C6 C5 122(2) . . ?
C1 C6 C7 114(2) . . ?
C5 C6 C7 124(2) . . ?
C8 C7 C14 108.7(18) . . ?
C8 C7 C6 107.1(18) . . ?
C14 C7 C6 107.1(16) . . ?
C8 C7 H7 111.2 . . ?
C14 C7 H7 111.2 . . ?
C6 C7 H7 111.2 . . ?
C13 C8 C9 117(2) . . ?
C13 C8 C7 122.2(19) . . ?
C9 C8 C7 121(2) . . ?
C10 C9 C8 118(3) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C11 C10 C9 121(3) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 119(3) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 119(2) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C8 125(2) . . ?
C12 C13 P1 129(2) . . ?
C8 C13 P1 106.5(17) . . ?
C19 C14 C15 122(3) . . ?
C19 C14 C7 116(2) . . ?
C15 C14 C7 123(2) . . ?
C14 C15 C16 117(3) . . ?
C14 C15 H15 121.3 . . ?
C16 C15 H15 121.3 . . ?
C15 C16 C17 123(3) . . ?
C15 C16 H16 118.6 . . ?
C17 C16 H16 118.6 . . ?
C16 C17 C18 117(3) . . ?
C16 C17 H17 121.3 . . ?
C18 C17 H17 121.3 . . ?
C19 C18 C17 119(2) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C14 C19 C18 121(2) . . ?
C14 C19 P1 113.2(19) . . ?
C18 C19 P1 125.6(19) . . ?
C21 C20 C25 120(2) . . ?
C21 C20 N2 118(2) . . ?
C25 C20 N2 121(2) . . ?
C20 C21 C22 121(2) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C23 C22 C21 121(2) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C22 C23 C24 117(2) . . ?
C22 C23 C26 125(2) . . ?
C24 C23 C26 117(2) . . ?
C25 C24 C23 121(2) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C20 C25 C24 119(2) . . ?
C20 C25 H25 120.6 . . ?
C24 C25 H25 120.6 . . ?
C39 C26 C23 107(2) . . ?
C39 C26 C33 110(2) . . ?
C23 C26 C33 113(2) . . ?
C39 C26 C27 112(2) . . ?
C23 C26 C27 110(2) . . ?
C33 C26 C27 105(2) . . ?
C28 C27 C32 118(3) . . ?
C28 C27 C26 123(3) . . ?
C32 C27 C26 119(3) . . ?
C27 C28 C29 123(3) . . ?
C27 C28 H28 118.5 . . ?
C29 C28 H28 118.5 . . ?
C30 C29 C28 120(3) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C31 C30 C29 117(3) . . ?
C31 C30 H30 121.5 . . ?
C29 C30 H30 121.5 . . ?
C30 C31 C32 123(4) . . ?
C30 C31 H31 118.7 . . ?
C32 C31 H31 118.7 . . ?
C27 C32 C31 119(3) . . ?
C27 C32 H32 120.5 . . ?
C31 C32 H32 120.5 . . ?
C34 C33 C38 120(2) . . ?
C34 C33 C26 122(2) . . ?
C38 C33 C26 117(2) . . ?
C35 C34 C33 117(3) . . ?
C35 C34 H34 121.6 . . ?
C33 C34 H34 121.6 . . ?
C36 C35 C34 123(3) . . ?
C36 C35 H35 118.5 . . ?
C34 C35 H35 118.5 . . ?
C35 C36 C37 124(3) . . ?
C35 C36 H36 118.2 . . ?
C37 C36 H36 118.2 . . ?
C36 C37 C38 118(3) . . ?
C36 C37 H37 121.1 . . ?
C38 C37 H37 121.1 . . ?
C37 C38 C33 118(3) . . ?
C37 C38 H38 120.8 . . ?
C33 C38 H38 120.8 . . ?
C44 C39 C40 113(2) . . ?
C44 C39 C26 126(2) . . ?
C40 C39 C26 120(2) . . ?
C41 C40 C39 125(3) . . ?
C41 C40 H40 117.7 . . ?
C39 C40 H40 117.7 . . ?
C42 C41 C40 120(3) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C43 120(3) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C44 C43 C42 115(3) . . ?
C44 C43 H43 122.3 . . ?
C42 C43 H43 122.3 . . ?
C43 C44 C39 127(3) . . ?
C43 C44 H44 116.6 . . ?
C39 C44 H44 116.6 . . ?

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
C1 P1 N2 C20 -179.7(19) . . . . ?
C19 P1 N2 C20 -62(2) . . . . ?
C13 P1 N2 C20 60(2) . . . . ?
N2 P1 C1 C6 179.7(17) . . . . ?
C19 P1 C1 C6 52(2) . . . . ?
C13 P1 C1 C6 -52(2) . . . . ?
N2 P1 C1 C2 -2(3) . . . . ?
C19 P1 C1 C2 -130(2) . . . . ?
C13 P1 C1 C2 127(2) . . . . ?
C6 C1 C2 C3 2(4) . . . . ?
P1 C1 C2 C3 -176(2) . . . . ?
C1 C2 C3 C4 -2(5) . . . . ?
C2 C3 C4 C5 2(5) . . . . ?
C3 C4 C5 C6 -3(4) . . . . ?
C2 C1 C6 C5 -2(4) . . . . ?
P1 C1 C6 C5 176.1(18) . . . . ?
C2 C1 C6 C7 -179(2) . . . . ?
P1 C1 C6 C7 -1(3) . . . . ?
C4 C5 C6 C1 3(4) . . . . ?
C4 C5 C6 C7 179(2) . . . . ?
C1 C6 C7 C8 58(3) . . . . ?
C5 C6 C7 C8 -119(2) . . . . ?
C1 C6 C7 C14 -59(3) . . . . ?
C5 C6 C7 C14 124(2) . . . . ?
C14 C7 C8 C13 58(3) . . . . ?
C6 C7 C8 C13 -57(3) . . . . ?
C14 C7 C8 C9 -125(2) . . . . ?
C6 C7 C8 C9 120(2) . . . . ?
C13 C8 C9 C10 0(4) . . . . ?
C7 C8 C9 C10 -178(3) . . . . ?
C8 C9 C10 C11 2(5) . . . . ?
C9 C10 C11 C12 -4(5) . . . . ?
C10 C11 C12 C13 3(4) . . . . ?
C11 C12 C13 C8 -1(4) . . . . ?
C11 C12 C13 P1 176(2) . . . . ?
C9 C8 C13 C12 0(4) . . . . ?
C7 C8 C13 C12 177(2) . . . . ?
C9 C8 C13 P1 -177.7(19) . . . . ?
C7 C8 C13 P1 -1(3) . . . . ?
N2 P1 C13 C12 3(3) . . . . ?
C1 P1 C13 C12 -126(3) . . . . ?
C19 P1 C13 C12 133(2) . . . . ?
N2 P1 C13 C8 179.9(17) . . . . ?
C1 P1 C13 C8 51(2) . . . . ?
C19 P1 C13 C8 -49(2) . . . . ?
C8 C7 C14 C19 -57(3) . . . . ?
C6 C7 C14 C19 59(3) . . . . ?
C8 C7 C14 C15 126(2) . . . . ?
C6 C7 C14 C15 -118(2) . . . . ?
C19 C14 C15 C16 -1(4) . . . . ?
C7 C14 C15 C16 176(2) . . . . ?
C14 C15 C16 C17 2(4) . . . . ?
C15 C16 C17 C18 -3(4) . . . . ?
C16 C17 C18 C19 1(4) . . . . ?
C15 C14 C19 C18 -1(4) . . . . ?
C7 C14 C19 C18 -178(2) . . . . ?
C15 C14 C19 P1 177.0(19) . . . . ?
C7 C14 C19 P1 0(3) . . . . ?
C17 C18 C19 C14 0(4) . . . . ?
C17 C18 C19 P1 -177(2) . . . . ?
N2 P1 C19 C14 -179.1(17) . . . . ?
C1 P1 C19 C14 -51.7(19) . . . . ?
C13 P1 C19 C14 51(2) . . . . ?
N2 P1 C19 C18 -1(3) . . . . ?
C1 P1 C19 C18 126(2) . . . . ?
C13 P1 C19 C18 -132(2) . . . . ?
P1 N2 C20 C21 171.2(18) . . . . ?
P1 N2 C20 C25 -2(3) . . . . ?
C25 C20 C21 C22 -6(4) . . . . ?
N2 C20 C21 C22 -179(2) . . . . ?
C20 C21 C22 C23 -1(4) . . . . ?
C21 C22 C23 C24 5(4) . . . . ?
C21 C22 C23 C26 173(2) . . . . ?
C22 C23 C24 C25 -2(4) . . . . ?
C26 C23 C24 C25 -171(2) . . . . ?
C21 C20 C25 C24 9(3) . . . . ?
N2 C20 C25 C24 -178(2) . . . . ?
C23 C24 C25 C20 -5(4) . . . . ?
C22 C23 C26 C39 -108(3) . . . . ?
C24 C23 C26 C39 61(3) . . . . ?
C22 C23 C26 C33 131(3) . . . . ?
C24 C23 C26 C33 -60(3) . . . . ?
C22 C23 C26 C27 14(3) . . . . ?
C24 C23 C26 C27 -177(2) . . . . ?
C39 C26 C27 C28 173(2) . . . . ?
C23 C26 C27 C28 55(3) . . . . ?
C33 C26 C27 C28 -67(3) . . . . ?
C39 C26 C27 C32 -15(4) . . . . ?
C23 C26 C27 C32 -133(3) . . . . ?
C33 C26 C27 C32 105(3) . . . . ?
C32 C27 C28 C29 3(4) . . . . ?
C26 C27 C28 C29 175(2) . . . . ?
C27 C28 C29 C30 0(5) . . . . ?
C28 C29 C30 C31 -5(5) . . . . ?
C29 C30 C31 C32 7(6) . . . . ?
C28 C27 C32 C31 -1(5) . . . . ?
C26 C27 C32 C31 -173(3) . . . . ?
C30 C31 C32 C27 -4(6) . . . . ?
C39 C26 C33 C34 -131(2) . . . . ?
C23 C26 C33 C34 -12(3) . . . . ?
C27 C26 C33 C34 108(3) . . . . ?
C39 C26 C33 C38 59(3) . . . . ?
C23 C26 C33 C38 179(2) . . . . ?
C27 C26 C33 C38 -61(3) . . . . ?
C38 C33 C34 C35 -8(4) . . . . ?
C26 C33 C34 C35 -177(2) . . . . ?
C33 C34 C35 C36 4(4) . . . . ?
C34 C35 C36 C37 0(6) . . . . ?
C35 C36 C37 C38 0(6) . . . . ?
C36 C37 C38 C33 -4(4) . . . . ?
C34 C33 C38 C37 8(4) . . . . ?
C26 C33 C38 C37 178(2) . . . . ?
C23 C26 C39 C44 -109(3) . . . . ?
C33 C26 C39 C44 14(4) . . . . ?
C27 C26 C39 C44 130(3) . . . . ?
C23 C26 C39 C40 64(3) . . . . ?
C33 C26 C39 C40 -173(2) . . . . ?
C27 C26 C39 C40 -57(3) . . . . ?
C44 C39 C40 C41 -2(5) . . . . ?
C26 C39 C40 C41 -176(3) . . . . ?
C39 C40 C41 C42 -1(6) . . . . ?
C40 C41 C42 C43 3(6) . . . . ?
C41 C42 C43 C44 -2(6) . . . . ?
C42 C43 C44 C39 -2(5) . . . . ?
C40 C39 C44 C43 4(4) . . . . ?
C26 C39 C44 C43 177(3) . . . . ?

_refine_diff_density_max         0.222
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.051



# start Validation Reply Form
_vrf_THETM01_nt1231_SMC037       
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: All obtained crystals of the compound were small blocks and were
 weakly diffracting, only up to 1.2 \%A. The lack of reflections also 
led to a number of additional problems (see below).
;
_vrf_PLAT029_nt1231_SMC037       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.891 Why?  
RESPONSE: See above.
;
_vrf_PLAT089_nt1231_SMC037       
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       3.45 Note  
RESPONSE: See above.
;
_vrf_PLAT340_nt1231_SMC037       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03816 Ang.  
RESPONSE: See above.
;
_vrf_PLAT911_nt1231_SMC037       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.484        193 Report
RESPONSE: See above.
;
_vrf_PLAT241_nt1231_SMC037       
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C10 Check 
RESPONSE: See above.
;
_vrf_PLAT242_nt1231_SMC037       
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C5 Check 
RESPONSE: See above.
;
_vrf_PLAT260_nt1231_SMC037       
;
PROBLEM: Large Average Ueq of Residue Including        P1      0.107 Check 
RESPONSE: See above.
;
_vrf_PLAT331_nt1231_SMC037       
;
PROBLEM: Small Aver Phenyl C-C Dist C27      --C32      .       1.36 Ang.  
RESPONSE: See above.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1194_SCM039_100K
_database_code_depnum_ccdc_archive 'CCDC 2313772'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        
;
N-phenyl-5gamma⁵-5,10-[1,2]benzenoacridophosphin-5(10H)-imine trifluoroborane
 complex dichloromethane semisolvate
;
_chemical_name_common            
;
9-phosphatriptycene-N-phenyl imine trifluoroborane complex
 dichloromethane semisolvate
;

_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H18 B F3 N P, 0.5(C H2 Cl2) '
_chemical_formula_sum            'C25.50 H19 B Cl F3 N P'
_chemical_formula_weight         473.65

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'
Cl Cl 0.3639 0.7018 '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'
N N 0.0311 0.0180 '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      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                   9.5904(2)
_cell_length_b                   16.0488(3)
_cell_length_c                   14.2154(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.4060(10)
_cell_angle_gamma                90
_cell_volume                     2144.74(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9857
_cell_measurement_theta_min      4.2017
_cell_measurement_theta_max      68.2898

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_F_000             972
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.018
_exptl_absorpt_coefficient_mu    2.636
_shelx_estimated_absorpt_T_min   0.442
_shelx_estimated_absorpt_T_max   0.954
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5812
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            21498
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.202
_diffrn_reflns_theta_max         68.285
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3919
_reflns_number_gt                3813
_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0311P)²+3.6038P] 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         3919
_refine_ls_number_parameters     317
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1154
_refine_ls_wR_factor_gt          0.1148
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.129
_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 0.76520(6) 0.23663(3) 0.24301(4) 0.01408(15) Uani 1 1 d . . . . .
F1 F 0.44513(18) 0.21042(10) 0.34635(12) 0.0373(4) Uani 1 1 d . . . . .
F2 F 0.40604(16) 0.32512(11) 0.25304(11) 0.0372(4) Uani 1 1 d . . . . .
F3 F 0.60871(15) 0.31666(9) 0.36750(10) 0.0276(3) Uani 1 1 d . . . . .
N1 N 0.5945(2) 0.23144(12) 0.22868(14) 0.0196(4) Uani 1 1 d . . . . .
C1 C 0.8490(2) 0.18899(12) 0.15295(15) 0.0135(4) Uani 1 1 d . . . . .
C2 C 0.7875(2) 0.14774(13) 0.06890(15) 0.0153(4) Uani 1 1 d . . . . .
H2 H 0.687227 0.140874 0.052044 0.018 Uiso 1 1 calc R U . . .
C3 C 0.8754(2) 0.11658(13) 0.00971(15) 0.0167(4) Uani 1 1 d . . . . .
H3 H 0.834803 0.088042 -0.047737 0.020 Uiso 1 1 calc R U . . .
C4 C 1.0210(2) 0.12701(14) 0.03417(15) 0.0173(4) Uani 1 1 d . . . . .
H4 H 1.079759 0.105231 -0.006508 0.021 Uiso 1 1 calc R U . . .
C5 C 1.0827(2) 0.16901(13) 0.11761(16) 0.0161(4) Uani 1 1 d . . . . .
H5 H 1.182955 0.176306 0.133488 0.019 Uiso 1 1 calc R U . . .
C6 C 0.9974(2) 0.20018(13) 0.17749(15) 0.0139(4) Uani 1 1 d . . . . .
C7 C 1.0590(2) 0.24761(13) 0.26976(15) 0.0155(4) Uani 1 1 d . . . . .
H7 H 1.164886 0.251498 0.278925 0.019 Uiso 1 1 calc R U . . .
C8 C 1.0159(2) 0.20151(13) 0.35369(15) 0.0160(4) Uani 1 1 d . . . . .
C9 C 1.1115(3) 0.16838(14) 0.43017(16) 0.0203(5) Uani 1 1 d . . . . .
H9 H 1.210962 0.174085 0.433526 0.024 Uiso 1 1 calc R U . . .
C10 C 1.0601(3) 0.12638(15) 0.50254(17) 0.0253(5) Uani 1 1 d . . . . .
H10 H 1.125383 0.103331 0.555143 0.030 Uiso 1 1 calc R U . . .
C11 C 0.9151(3) 0.11796(15) 0.49847(17) 0.0261(5) Uani 1 1 d . . . . .
H11 H 0.882049 0.089662 0.548523 0.031 Uiso 1 1 calc R U . . .
C12 C 0.8182(3) 0.15050(14) 0.42196(16) 0.0221(5) Uani 1 1 d . . . . .
H12 H 0.718780 0.144777 0.418864 0.027 Uiso 1 1 calc R U . . .
C13 C 0.8696(2) 0.19166(13) 0.34991(15) 0.0164(4) Uani 1 1 d . . . . .
C14 C 0.8435(2) 0.33880(13) 0.24700(15) 0.0161(4) Uani 1 1 d . . . . .
C15 C 0.7719(2) 0.41443(14) 0.23514(15) 0.0187(5) Uani 1 1 d . . . . .
H15 H 0.671013 0.416430 0.225001 0.022 Uiso 1 1 calc R U . . .
C16 C 0.8517(3) 0.48736(14) 0.23848(17) 0.0237(5) Uani 1 1 d . . . . .
H16 H 0.804978 0.539840 0.230925 0.028 Uiso 1 1 calc R U . . .
C17 C 0.9989(3) 0.48371(14) 0.25276(17) 0.0246(5) Uani 1 1 d . . . . .
H17 H 1.051951 0.533891 0.254881 0.029 Uiso 1 1 calc R U . . .
C18 C 1.0702(3) 0.40748(14) 0.26408(16) 0.0197(5) Uani 1 1 d . . . . .
H18 H 1.171059 0.405639 0.273429 0.024 Uiso 1 1 calc R U . . .
C19 C 0.9922(2) 0.33435(13) 0.26151(15) 0.0160(4) Uani 1 1 d . . . . .
C20 C 0.5143(2) 0.17458(14) 0.15874(16) 0.0178(5) Uani 1 1 d . . . . .
C21 C 0.5067(3) 0.09066(15) 0.18077(17) 0.0226(5) Uani 1 1 d . . . . .
H21 H 0.551448 0.070441 0.242145 0.027 Uiso 1 1 calc R U . . .
C22 C 0.4328(3) 0.03632(15) 0.11214(18) 0.0249(5) Uani 1 1 d . . . . .
H22 H 0.427158 -0.021224 0.126597 0.030 Uiso 1 1 calc R U . . .
C23 C 0.3679(2) 0.06610(15) 0.02307(18) 0.0238(5) Uani 1 1 d . . . . .
H23 H 0.319434 0.028697 -0.024079 0.029 Uiso 1 1 calc R U . . .
C24 C 0.3730(2) 0.15031(15) 0.00207(17) 0.0215(5) Uani 1 1 d . . . . .
H24 H 0.326773 0.170609 -0.058917 0.026 Uiso 1 1 calc R U . . .
C25 C 0.4460(2) 0.20504(14) 0.07042(16) 0.0186(5) Uani 1 1 d . . . . .
H25 H 0.448953 0.262859 0.056623 0.022 Uiso 1 1 calc R U . . .
B1 B 0.5106(3) 0.27260(18) 0.3017(2) 0.0232(6) Uani 1 1 d . . . . .
C26A C 0.4723(19) 0.5533(10) 0.0026(12) 0.054(7) Uani 0.175(11) 1 d D U P A -1
H26A H 0.520646 0.588310 0.056645 0.064 Uiso 0.175(11) 1 calc R U P A -1
H26B H 0.384288 0.582868 -0.027738 0.064 Uiso 0.175(11) 1 calc R U P A -1
Cl1A Cl 0.5800(3) 0.5482(2) -0.0795(2) 0.0505(8) Uani 0.25 1 d D . P A -1
Cl2A Cl 0.4250(6) 0.4653(4) 0.0481(4) 0.107(2) Uani 0.25 1 d D . P A -1
C26B C 0.5704(10) 0.5269(6) 0.0367(7) 0.039(3) Uani 0.325(11) 1 d D U P A -2
H26C H 0.565005 0.580145 0.071031 0.046 Uiso 0.325(11) 1 calc R U P A -2
H26D H 0.658780 0.498193 0.067974 0.046 Uiso 0.325(11) 1 calc R U P A -2
Cl1B Cl 0.5800(3) 0.5482(2) -0.0795(2) 0.0505(8) Uani 0.25 1 d D . P A -2
Cl2B Cl 0.4250(6) 0.4653(4) 0.0481(4) 0.107(2) Uani 0.25 1 d D . 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
P1 N1 1.6110(19) . ?
P1 C13 1.798(2) . ?
P1 C14 1.800(2) . ?
P1 C1 1.810(2) . ?
F1 B1 1.397(3) . ?
F2 B1 1.386(3) . ?
F3 B1 1.383(3) . ?
N1 C20 1.453(3) . ?
N1 B1 1.579(3) . ?
C1 C2 1.391(3) . ?
C1 C6 1.408(3) . ?
C2 C3 1.396(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.530(3) . ?
C7 C19 1.527(3) . ?
C7 C8 1.529(3) . ?
C7 H7 1.0000 . ?
C8 C9 1.383(3) . ?
C8 C13 1.402(3) . ?
C9 C10 1.398(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(3) . ?
C12 H12 0.9500 . ?
C14 C15 1.389(3) . ?
C14 C19 1.402(3) . ?
C15 C16 1.394(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.387(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.395(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(3) . ?
C18 H18 0.9500 . ?
C20 C25 1.385(3) . ?
C20 C21 1.388(3) . ?
C21 C22 1.393(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.381(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26A Cl2A 1.654(13) . ?
C26A Cl1A 1.707(13) . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
C26B Cl1B 1.707(8) . ?
C26B Cl2B 1.743(9) . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?

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
N1 P1 C13 117.93(10) . . ?
N1 P1 C14 117.28(10) . . ?
C13 P1 C14 100.36(10) . . ?
N1 P1 C1 118.09(10) . . ?
C13 P1 C1 100.20(10) . . ?
C14 P1 C1 99.57(10) . . ?
C20 N1 B1 116.30(17) . . ?
C20 N1 P1 120.42(15) . . ?
B1 N1 P1 122.18(15) . . ?
C2 C1 C6 120.66(19) . . ?
C2 C1 P1 129.50(17) . . ?
C6 C1 P1 109.82(15) . . ?
C1 C2 C3 118.9(2) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 120.4(2) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.8(2) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 119.7(2) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 119.51(19) . . ?
C5 C6 C7 122.06(19) . . ?
C1 C6 C7 118.42(18) . . ?
C19 C7 C8 109.09(17) . . ?
C19 C7 C6 107.61(17) . . ?
C8 C7 C6 108.05(17) . . ?
C19 C7 H7 110.7 . . ?
C8 C7 H7 110.7 . . ?
C6 C7 H7 110.7 . . ?
C9 C8 C13 119.3(2) . . ?
C9 C8 C7 124.1(2) . . ?
C13 C8 C7 116.59(19) . . ?
C8 C9 C10 119.2(2) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 120.8(2) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C10 120.5(2) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 118.5(2) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C12 C13 C8 121.6(2) . . ?
C12 C13 P1 126.48(18) . . ?
C8 C13 P1 111.91(16) . . ?
C15 C14 C19 121.8(2) . . ?
C15 C14 P1 126.81(17) . . ?
C19 C14 P1 111.37(16) . . ?
C14 C15 C16 118.3(2) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
C17 C16 C15 120.4(2) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 121.0(2) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 119.2(2) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C14 119.2(2) . . ?
C18 C19 C7 123.5(2) . . ?
C14 C19 C7 117.18(19) . . ?
C25 C20 C21 120.7(2) . . ?
C25 C20 N1 119.3(2) . . ?
C21 C20 N1 120.0(2) . . ?
C20 C21 C22 119.4(2) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C23 C22 C21 120.0(2) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.4(2) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C25 119.9(2) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C20 C25 C24 119.5(2) . . ?
C20 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
F3 B1 F2 110.8(2) . . ?
F3 B1 F1 111.4(2) . . ?
F2 B1 F1 108.4(2) . . ?
F3 B1 N1 106.95(19) . . ?
F2 B1 N1 109.8(2) . . ?
F1 B1 N1 109.5(2) . . ?
Cl2A C26A Cl1A 118.5(10) . . ?
Cl2A C26A H26A 107.7 . . ?
Cl1A C26A H26A 107.7 . . ?
Cl2A C26A H26B 107.7 . . ?
Cl1A C26A H26B 107.7 . . ?
H26A C26A H26B 107.1 . . ?
Cl1B C26B Cl2B 113.6(6) . . ?
Cl1B C26B H26C 108.8 . . ?
Cl2B C26B H26C 108.8 . . ?
Cl1B C26B H26D 108.8 . . ?
Cl2B C26B H26D 108.8 . . ?
H26C C26B H26D 107.7 . . ?

_refine_diff_density_max         0.405
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.062



# start Validation Reply Form
_vrf_PLAT042_nt1194_SCM039_100K  
;
PROBLEM: Calc. and Reported MoietyFormula Strings  Differ     Please Check 
RESPONSE: Disordered dichloromethane in the structure.
;

# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt0745_LHG153_100K
_database_code_depnum_ccdc_archive 'CCDC 2313768'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'diphenyl (10H-5l5-5,10-[1,2]benzenoacridophosphin-5-ylidene)phosphoramidate'
_chemical_name_common            
'diphenyl (10H-5l5-5,10-[1,2]benzenoacridophosphin-5-ylidene)phosphoramidate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H23 N O3 P2'
_chemical_formula_sum            'C31 H23 N O3 P2'
_chemical_formula_weight         519.44

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'
N N 0.0311 0.0180 '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      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                   11.81181(13)
_cell_length_b                   19.91502(17)
_cell_length_c                   11.98573(13)
_cell_angle_alpha                90
_cell_angle_beta                 118.9392(15)
_cell_angle_gamma                90
_cell_volume                     2467.38(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11237
_cell_measurement_theta_min      4.2530
_cell_measurement_theta_max      66.9630

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_F_000             1080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.039
_exptl_absorpt_coefficient_mu    1.888
_shelx_estimated_absorpt_T_min   0.458
_shelx_estimated_absorpt_T_max   0.930
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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     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            17799
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.277
_diffrn_reflns_theta_max         67.009
_diffrn_reflns_theta_full        67.009
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4379
_reflns_number_gt                4054
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0436P)²+1.2213P] 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         4379
_refine_ls_number_parameters     434
_refine_ls_number_restraints     121
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0834
_refine_ls_wR_factor_gt          0.0812
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.000
_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 0.67554(3) 0.45127(2) 0.34584(3) 0.01812(11) Uani 1 1 d . U . . .
P2A P 0.70536(4) 0.30462(2) 0.33181(6) 0.02114(17) Uani 0.901(2) 1 d D . P A 1
O1A O 0.84597(11) 0.28209(6) 0.43982(12) 0.0240(3) Uani 0.901(2) 1 d D . P A 1
O2A O 0.6195(3) 0.2531(2) 0.3634(5) 0.0274(6) Uani 0.901(2) 1 d D U P A 1
O3A O 0.68726(12) 0.29510(6) 0.20291(12) 0.0302(3) Uani 0.901(2) 1 d D . P A 1
N1A N 0.6832(2) 0.37516(9) 0.37665(19) 0.0234(4) Uani 0.901(2) 1 d D . P A 1
C20A C 0.8956(2) 0.21914(12) 0.4336(2) 0.0231(6) Uani 0.901(2) 1 d D . P A 1
C21A C 0.9475(4) 0.20968(18) 0.3532(4) 0.0284(6) Uani 0.901(2) 1 d D . P A 1
H21A H 0.944128 0.244537 0.297574 0.034 Uiso 0.901(2) 1 calc R U P A 1
C22A C 1.0051(5) 0.14809(16) 0.3550(5) 0.0325(8) Uani 0.901(2) 1 d D U P A 1
H22A H 1.042418 0.141014 0.301373 0.039 Uiso 0.901(2) 1 calc R U P A 1
C23A C 1.0076(6) 0.0972(2) 0.4357(5) 0.0349(10) Uani 0.901(2) 1 d D . P A 1
H23A H 1.047552 0.055452 0.437796 0.042 Uiso 0.901(2) 1 calc R U P A 1
C24A C 0.9518(6) 0.1072(2) 0.5128(5) 0.0344(9) Uani 0.901(2) 1 d D . P A 1
H24A H 0.952429 0.071864 0.566401 0.041 Uiso 0.901(2) 1 calc R U P A 1
C25A C 0.8949(3) 0.16844(16) 0.5128(3) 0.0297(6) Uani 0.901(2) 1 d D U P A 1
H25A H 0.856566 0.175366 0.565637 0.036 Uiso 0.901(2) 1 calc R U P A 1
P2B P 0.7294(5) 0.3077(3) 0.4105(7) 0.0406(16) Uani 0.099(2) 1 d D . P A 2
O1B O 0.8101(12) 0.2761(6) 0.3469(14) 0.042(3) Uani 0.099(2) 1 d D . P A 2
O2B O 0.611(3) 0.2543(19) 0.354(5) 0.035(5) Uani 0.099(2) 1 d D U P A 2
O3B O 0.8010(14) 0.3123(7) 0.5438(10) 0.046(4) Uani 0.099(2) 1 d D . P A 2
N1B N 0.6638(17) 0.3688(8) 0.3232(13) 0.020(3) Uani 0.099(2) 1 d D U P A 2
C20B C 0.877(2) 0.2150(10) 0.382(2) 0.029(5) Uani 0.099(2) 1 d D . P A 2
C21B C 0.959(5) 0.1959(18) 0.337(5) 0.039(9) Uani 0.099(2) 1 d D . P A 2
H21B H 0.980930 0.225870 0.288970 0.047 Uiso 0.099(2) 1 calc R U P A 2
C22B C 1.008(5) 0.1312(18) 0.365(5) 0.029(5) Uani 0.099(2) 1 d D U P A 2
H22B H 1.049228 0.112475 0.320275 0.035 Uiso 0.099(2) 1 calc R U P A 2
C23B C 0.998(7) 0.094(2) 0.457(6) 0.036(9) Uani 0.099(2) 1 d D . P A 2
H23B H 1.030159 0.049321 0.473937 0.043 Uiso 0.099(2) 1 calc R U P A 2
C24B C 0.941(6) 0.121(2) 0.523(5) 0.033(8) Uani 0.099(2) 1 d D . P A 2
H24B H 0.945342 0.098639 0.595823 0.039 Uiso 0.099(2) 1 calc R U P A 2
C25B C 0.876(4) 0.1807(16) 0.481(3) 0.032(5) Uani 0.099(2) 1 d D U P A 2
H25B H 0.830773 0.198889 0.521011 0.038 Uiso 0.099(2) 1 calc R U P A 2
C1 C 0.53890(13) 0.49532(7) 0.33672(13) 0.0192(3) Uani 1 1 d . . . . .
C2 C 0.43260(14) 0.46642(8) 0.33734(13) 0.0220(3) Uani 1 1 d . . . . .
H2 H 0.428309 0.419221 0.346211 0.026 Uiso 1 1 calc R U . . .
C3 C 0.33218(14) 0.50783(8) 0.32471(14) 0.0254(3) Uani 1 1 d . . . . .
H3 H 0.257693 0.488843 0.323258 0.031 Uiso 1 1 calc R U . . .
C4 C 0.34067(14) 0.57689(9) 0.31422(14) 0.0266(3) Uani 1 1 d . . . . .
H4 H 0.272405 0.604862 0.307276 0.032 Uiso 1 1 calc R U . . .
C5 C 0.44802(14) 0.60574(8) 0.31375(14) 0.0242(3) Uani 1 1 d . . . . .
H5 H 0.452797 0.653019 0.306392 0.029 Uiso 1 1 calc R U . . .
C6 C 0.54759(13) 0.56497(8) 0.32409(13) 0.0204(3) Uani 1 1 d . . . . .
C7 C 0.66763(13) 0.59070(7) 0.31855(14) 0.0206(3) Uani 1 1 d . . . . .
H7 H 0.664511 0.640622 0.308472 0.025 Uiso 1 1 calc R U . . .
C8 C 0.78832(13) 0.56927(8) 0.44159(14) 0.0207(3) Uani 1 1 d . . . . .
C9 C 0.88155(14) 0.61299(8) 0.52690(15) 0.0252(3) Uani 1 1 d . . . . .
H9 H 0.874558 0.659873 0.510217 0.030 Uiso 1 1 calc R U . . .
C10 C 0.98555(14) 0.58752(9) 0.63730(15) 0.0271(3) Uani 1 1 d . . . . .
H10 H 1.049252 0.617413 0.695908 0.032 Uiso 1 1 calc R U . . .
C11 C 0.99739(14) 0.51922(8) 0.66281(14) 0.0252(3) Uani 1 1 d . . . . .
H11 H 1.067665 0.502811 0.739516 0.030 Uiso 1 1 calc R U . . .
C12 C 0.90655(13) 0.47459(8) 0.57631(14) 0.0218(3) Uani 1 1 d . . . . .
H12 H 0.915142 0.427598 0.591820 0.026 Uiso 1 1 calc R U . . .
C13 C 0.80323(13) 0.50042(8) 0.46697(13) 0.0195(3) Uani 1 1 d . . . . .
C14 C 0.67125(13) 0.55622(8) 0.20634(14) 0.0208(3) Uani 1 1 d . . . . .
C15 C 0.67116(14) 0.59095(8) 0.10591(15) 0.0255(3) Uani 1 1 d . . . . .
H15 H 0.670427 0.638648 0.105126 0.031 Uiso 1 1 calc R U . . .
C16 C 0.67216(14) 0.55543(9) 0.00625(15) 0.0283(3) Uani 1 1 d . . . . .
H16 H 0.672412 0.579305 -0.062245 0.034 Uiso 1 1 calc R U . . .
C17 C 0.67278(14) 0.48600(8) 0.00537(14) 0.0261(3) Uani 1 1 d . . . . .
H17 H 0.672867 0.462596 -0.063648 0.031 Uiso 1 1 calc R U . . .
C18 C 0.67327(13) 0.45019(8) 0.10598(14) 0.0225(3) Uani 1 1 d . . . . .
H18 H 0.673312 0.402491 0.105954 0.027 Uiso 1 1 calc R U . . .
C19 C 0.67369(13) 0.48563(8) 0.20583(13) 0.0199(3) Uani 1 1 d . . . . .
C26 C 0.49194(14) 0.26945(7) 0.33078(15) 0.0248(3) Uani 1 1 d . . . . .
C27 C 0.40076(16) 0.28387(8) 0.20622(16) 0.0292(3) Uani 1 1 d . . . . .
H27 H 0.424512 0.284331 0.140981 0.035 Uiso 1 1 calc R U . . .
C28 C 0.27498(16) 0.29759(8) 0.17760(16) 0.0322(4) Uani 1 1 d . . . . .
H28 H 0.211494 0.306671 0.092038 0.039 Uiso 1 1 calc R U . . .
C29 C 0.24110(16) 0.29814(9) 0.27315(18) 0.0346(4) Uani 1 1 d . . . . .
H29 H 0.154598 0.307716 0.253437 0.041 Uiso 1 1 calc R U . . .
C30 C 0.33402(17) 0.28467(9) 0.39773(17) 0.0351(4) Uani 1 1 d . . . . .
H30 H 0.311176 0.285873 0.463578 0.042 Uiso 1 1 calc R U . . .
C31 C 0.46068(16) 0.26935(8) 0.42738(16) 0.0300(4) Uani 1 1 d . . . . .
H31 H 0.523988 0.259087 0.512436 0.036 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
P1 N1A 1.5524(18) . ?
P1 N1B 1.659(16) . ?
P1 C1 1.7933(14) . ?
P1 C13 1.7948(14) . ?
P1 C19 1.8027(15) . ?
P2A O3A 1.4659(14) . ?
P2A N1A 1.5707(18) . ?
P2A O1A 1.5984(13) . ?
P2A O2A 1.611(3) . ?
O1A C20A 1.401(2) . ?
O2A C26 1.400(4) . ?
C20A C21A 1.382(4) . ?
C20A C25A 1.389(3) . ?
C21A C22A 1.397(4) . ?
C21A H21A 0.9500 . ?
C22A C23A 1.391(4) . ?
C22A H22A 0.9500 . ?
C23A C24A 1.385(4) . ?
C23A H23A 0.9500 . ?
C24A C25A 1.393(4) . ?
C24A H24A 0.9500 . ?
C25A H25A 0.9500 . ?
P2B O3B 1.403(12) . ?
P2B N1B 1.547(13) . ?
P2B O1B 1.609(12) . ?
P2B O2B 1.621(17) . ?
O1B C20B 1.399(15) . ?
O2B C26 1.33(4) . ?
C20B C21B 1.368(17) . ?
C20B C25B 1.371(17) . ?
C21B C22B 1.388(18) . ?
C21B H21B 0.9500 . ?
C22B C23B 1.384(18) . ?
C22B H22B 0.9500 . ?
C23B C24B 1.381(18) . ?
C23B H23B 0.9500 . ?
C24B C25B 1.374(18) . ?
C24B H24B 0.9500 . ?
C25B H25B 0.9500 . ?
C1 C2 1.384(2) . ?
C1 C6 1.404(2) . ?
C2 C3 1.392(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.539(2) . ?
C7 C14 1.529(2) . ?
C7 C8 1.534(2) . ?
C7 H7 1.0000 . ?
C8 C9 1.388(2) . ?
C8 C13 1.397(2) . ?
C9 C10 1.394(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.387(2) . ?
C12 H12 0.9500 . ?
C14 C15 1.388(2) . ?
C14 C19 1.406(2) . ?
C15 C16 1.393(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.383(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.399(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.387(2) . ?
C18 H18 0.9500 . ?
C26 C31 1.375(2) . ?
C26 C27 1.384(2) . ?
C27 C28 1.381(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.384(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.386(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.394(2) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?

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
N1A P1 C1 116.05(9) . . ?
N1B P1 C1 118.2(6) . . ?
N1A P1 C13 114.25(9) . . ?
N1B P1 C13 130.0(5) . . ?
C1 P1 C13 99.31(7) . . ?
N1A P1 C19 124.42(9) . . ?
N1B P1 C19 105.1(5) . . ?
C1 P1 C19 98.77(7) . . ?
C13 P1 C19 99.96(7) . . ?
O3A P2A N1A 120.85(10) . . ?
O3A P2A O1A 112.44(7) . . ?
N1A P2A O1A 104.71(10) . . ?
O3A P2A O2A 112.20(19) . . ?
N1A P2A O2A 105.1(2) . . ?
O1A P2A O2A 98.98(18) . . ?
C20A O1A P2A 120.37(13) . . ?
C26 O2A P2A 120.0(3) . . ?
P1 N1A P2A 142.37(15) . . ?
C21A C20A C25A 121.9(2) . . ?
C21A C20A O1A 119.8(2) . . ?
C25A C20A O1A 118.2(2) . . ?
C20A C21A C22A 119.0(3) . . ?
C20A C21A H21A 120.5 . . ?
C22A C21A H21A 120.5 . . ?
C23A C22A C21A 119.8(3) . . ?
C23A C22A H22A 120.1 . . ?
C21A C22A H22A 120.1 . . ?
C24A C23A C22A 120.1(3) . . ?
C24A C23A H23A 119.9 . . ?
C22A C23A H23A 119.9 . . ?
C23A C24A C25A 120.8(3) . . ?
C23A C24A H24A 119.6 . . ?
C25A C24A H24A 119.6 . . ?
C20A C25A C24A 118.3(3) . . ?
C20A C25A H25A 120.8 . . ?
C24A C25A H25A 120.8 . . ?
O3B P2B N1B 123.2(9) . . ?
O3B P2B O1B 113.4(9) . . ?
N1B P2B O1B 101.9(9) . . ?
O3B P2B O2B 116(2) . . ?
N1B P2B O2B 100.6(18) . . ?
O1B P2B O2B 97.6(19) . . ?
C20B O1B P2B 125.1(13) . . ?
C26 O2B P2B 123(3) . . ?
P2B N1B P1 133.9(11) . . ?
C21B C20B C25B 120.1(18) . . ?
C21B C20B O1B 122(2) . . ?
C25B C20B O1B 117.0(19) . . ?
C20B C21B C22B 117(2) . . ?
C20B C21B H21B 121.3 . . ?
C22B C21B H21B 121.3 . . ?
C23B C22B C21B 120(2) . . ?
C23B C22B H22B 120.1 . . ?
C21B C22B H22B 120.1 . . ?
C24B C23B C22B 121(2) . . ?
C24B C23B H23B 119.6 . . ?
C22B C23B H23B 119.6 . . ?
C25B C24B C23B 117(2) . . ?
C25B C24B H24B 121.4 . . ?
C23B C24B H24B 121.4 . . ?
C20B C25B C24B 121(2) . . ?
C20B C25B H25B 119.3 . . ?
C24B C25B H25B 119.3 . . ?
C2 C1 C6 121.67(13) . . ?
C2 C1 P1 126.02(12) . . ?
C6 C1 P1 112.28(11) . . ?
C1 C2 C3 118.72(14) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 120.10(14) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.92(14) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 119.52(15) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 119.05(14) . . ?
C5 C6 C7 124.15(14) . . ?
C1 C6 C7 116.77(12) . . ?
C14 C7 C8 108.19(11) . . ?
C14 C7 C6 107.87(11) . . ?
C8 C7 C6 108.22(12) . . ?
C14 C7 H7 110.8 . . ?
C8 C7 H7 110.8 . . ?
C6 C7 H7 110.8 . . ?
C9 C8 C13 118.93(13) . . ?
C9 C8 C7 124.78(14) . . ?
C13 C8 C7 116.28(12) . . ?
C8 C9 C10 119.44(15) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 120.98(14) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 120.19(14) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 118.39(14) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
C12 C13 C8 122.02(13) . . ?
C12 C13 P1 124.95(12) . . ?
C8 C13 P1 113.02(10) . . ?
C15 C14 C19 119.07(14) . . ?
C15 C14 C7 123.40(14) . . ?
C19 C14 C7 117.53(13) . . ?
C14 C15 C16 119.60(15) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 121.10(15) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 120.07(15) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 118.76(14) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C14 121.39(14) . . ?
C18 C19 P1 127.11(12) . . ?
C14 C19 P1 111.50(11) . . ?
O2B C26 C31 121(2) . . ?
O2B C26 C27 118(2) . . ?
C31 C26 C27 121.52(15) . . ?
C31 C26 O2A 117.1(3) . . ?
C27 C26 O2A 121.3(3) . . ?
C28 C27 C26 119.42(16) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C27 C28 C29 120.21(15) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C28 C29 C30 119.65(16) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C29 C30 C31 120.66(17) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C26 C31 C30 118.51(15) . . ?
C26 C31 H31 120.7 . . ?
C30 C31 H31 120.7 . . ?

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
O3A P2A O1A C20A -49.91(18) . . . . ?
N1A P2A O1A C20A 177.08(17) . . . . ?
O2A P2A O1A C20A 68.7(2) . . . . ?
O3A P2A O2A C26 -87.0(4) . . . . ?
N1A P2A O2A C26 46.2(4) . . . . ?
O1A P2A O2A C26 154.2(3) . . . . ?
C1 P1 N1A P2A 131.5(2) . . . . ?
C13 P1 N1A P2A -113.9(2) . . . . ?
C19 P1 N1A P2A 8.7(3) . . . . ?
O3A P2A N1A P1 -20.0(3) . . . . ?
O1A P2A N1A P1 108.1(2) . . . . ?
O2A P2A N1A P1 -148.1(3) . . . . ?
P2A O1A C20A C21A 79.2(3) . . . . ?
P2A O1A C20A C25A -103.0(2) . . . . ?
C25A C20A C21A C22A -2.3(6) . . . . ?
O1A C20A C21A C22A 175.4(4) . . . . ?
C20A C21A C22A C23A 1.0(8) . . . . ?
C21A C22A C23A C24A 0.8(9) . . . . ?
C22A C23A C24A C25A -1.2(9) . . . . ?
C21A C20A C25A C24A 1.8(5) . . . . ?
O1A C20A C25A C24A -175.9(4) . . . . ?
C23A C24A C25A C20A -0.1(7) . . . . ?
O3B P2B O1B C20B 52.7(19) . . . . ?
N1B P2B O1B C20B -172.9(18) . . . . ?
O2B P2B O1B C20B -70(3) . . . . ?
O3B P2B O2B C26 88(4) . . . . ?
N1B P2B O2B C26 -48(4) . . . . ?
O1B P2B O2B C26 -151(4) . . . . ?
O3B P2B N1B P1 13(2) . . . . ?
O1B P2B N1B P1 -115.2(16) . . . . ?
O2B P2B N1B P1 145(2) . . . . ?
C1 P1 N1B P2B -112.3(15) . . . . ?
C13 P1 N1B P2B 21(2) . . . . ?
C19 P1 N1B P2B 138.8(14) . . . . ?
P2B O1B C20B C21B -170(3) . . . . ?
P2B O1B C20B C25B -2(3) . . . . ?
C25B C20B C21B C22B 20(7) . . . . ?
O1B C20B C21B C22B -172(4) . . . . ?
C20B C21B C22B C23B -14(9) . . . . ?
C21B C22B C23B C24B -1(10) . . . . ?
C22B C23B C24B C25B 10(10) . . . . ?
C21B C20B C25B C24B -11(6) . . . . ?
O1B C20B C25B C24B -179(4) . . . . ?
C23B C24B C25B C20B -5(8) . . . . ?
N1A P1 C1 C2 -9.32(17) . . . . ?
N1B P1 C1 C2 13.6(6) . . . . ?
C13 P1 C1 C2 -132.24(13) . . . . ?
C19 P1 C1 C2 126.07(13) . . . . ?
N1A P1 C1 C6 172.72(12) . . . . ?
N1B P1 C1 C6 -164.4(5) . . . . ?
C13 P1 C1 C6 49.81(11) . . . . ?
C19 P1 C1 C6 -51.88(11) . . . . ?
C6 C1 C2 C3 0.2(2) . . . . ?
P1 C1 C2 C3 -177.60(11) . . . . ?
C1 C2 C3 C4 -1.2(2) . . . . ?
C2 C3 C4 C5 1.2(2) . . . . ?
C3 C4 C5 C6 -0.1(2) . . . . ?
C4 C5 C6 C1 -0.9(2) . . . . ?
C4 C5 C6 C7 177.10(13) . . . . ?
C2 C1 C6 C5 0.9(2) . . . . ?
P1 C1 C6 C5 178.95(11) . . . . ?
C2 C1 C6 C7 -177.27(13) . . . . ?
P1 C1 C6 C7 0.79(16) . . . . ?
C5 C6 C7 C14 -120.23(15) . . . . ?
C1 C6 C7 C14 57.84(16) . . . . ?
C5 C6 C7 C8 122.94(15) . . . . ?
C1 C6 C7 C8 -59.00(16) . . . . ?
C14 C7 C8 C9 120.99(15) . . . . ?
C6 C7 C8 C9 -122.38(15) . . . . ?
C14 C7 C8 C13 -58.77(16) . . . . ?
C6 C7 C8 C13 57.87(16) . . . . ?
C13 C8 C9 C10 -1.8(2) . . . . ?
C7 C8 C9 C10 178.44(14) . . . . ?
C8 C9 C10 C11 0.2(2) . . . . ?
C9 C10 C11 C12 1.6(2) . . . . ?
C10 C11 C12 C13 -1.8(2) . . . . ?
C11 C12 C13 C8 0.1(2) . . . . ?
C11 C12 C13 P1 -179.06(11) . . . . ?
C9 C8 C13 C12 1.7(2) . . . . ?
C7 C8 C13 C12 -178.58(13) . . . . ?
C9 C8 C13 P1 -179.06(11) . . . . ?
C7 C8 C13 P1 0.71(17) . . . . ?
N1A P1 C13 C12 4.07(16) . . . . ?
N1B P1 C13 C12 -11.4(8) . . . . ?
C1 P1 C13 C12 128.26(13) . . . . ?
C19 P1 C13 C12 -131.05(13) . . . . ?
N1A P1 C13 C8 -175.19(12) . . . . ?
N1B P1 C13 C8 169.3(8) . . . . ?
C1 P1 C13 C8 -51.00(12) . . . . ?
C19 P1 C13 C8 49.70(12) . . . . ?
C8 C7 C14 C15 -121.20(14) . . . . ?
C6 C7 C14 C15 121.94(14) . . . . ?
C8 C7 C14 C19 59.34(16) . . . . ?
C6 C7 C14 C19 -57.52(16) . . . . ?
C19 C14 C15 C16 0.6(2) . . . . ?
C7 C14 C15 C16 -178.80(13) . . . . ?
C14 C15 C16 C17 0.2(2) . . . . ?
C15 C16 C17 C18 -0.4(2) . . . . ?
C16 C17 C18 C19 -0.3(2) . . . . ?
C17 C18 C19 C14 1.2(2) . . . . ?
C17 C18 C19 P1 -179.51(10) . . . . ?
C15 C14 C19 C18 -1.4(2) . . . . ?
C7 C14 C19 C18 178.12(12) . . . . ?
C15 C14 C19 P1 179.22(11) . . . . ?
C7 C14 C19 P1 -1.29(15) . . . . ?
N1A P1 C19 C18 2.88(18) . . . . ?
N1B P1 C19 C18 -4.8(6) . . . . ?
C1 P1 C19 C18 -127.23(13) . . . . ?
C13 P1 C19 C18 131.62(13) . . . . ?
N1A P1 C19 C14 -177.75(12) . . . . ?
N1B P1 C19 C14 174.6(6) . . . . ?
C1 P1 C19 C14 52.14(11) . . . . ?
C13 P1 C19 C14 -49.01(11) . . . . ?
P2B O2B C26 C31 -81(4) . . . . ?
P2B O2B C26 C27 100(4) . . . . ?
P2A O2A C26 C31 -123.6(3) . . . . ?
P2A O2A C26 C27 57.6(4) . . . . ?
O2B C26 C27 C28 177.8(15) . . . . ?
C31 C26 C27 C28 -0.9(2) . . . . ?
O2A C26 C27 C28 177.9(2) . . . . ?
C26 C27 C28 C29 1.2(2) . . . . ?
C27 C28 C29 C30 -0.2(3) . . . . ?
C28 C29 C30 C31 -1.2(3) . . . . ?
O2B C26 C31 C30 -179.1(16) . . . . ?
C27 C26 C31 C30 -0.4(2) . . . . ?
O2A C26 C31 C30 -179.2(2) . . . . ?
C29 C30 C31 C26 1.5(3) . . . . ?

_refine_diff_density_max         0.298
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.046



# start Validation Reply Form
_vrf_PLAT911_nt0745_LHG153_100K  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.597         28 Report
RESPONSE: These reflection are missing in the highest and lowest resolution
 shells because of the instrument geometry limitations.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1402_SMC190_oxide_100K
_database_code_depnum_ccdc_archive 'CCDC 2347267'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        '9-phosphatriptycene oxide hemihydrate'
_chemical_name_common            '9-phosphatriptycene oxide hemihydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C19 H13 O P), H2 O'
_chemical_formula_sum            'C38 H28 O3 P2'
_chemical_formula_weight         594.54

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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   16.3712(2)
_cell_length_b                   16.2810(2)
_cell_length_c                   22.9501(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6117.11(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9987
_cell_measurement_theta_min      4.2870
_cell_measurement_theta_max      68.2049

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_F_000             2480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.583
_shelx_estimated_absorpt_T_min   0.702
_shelx_estimated_absorpt_T_max   0.845
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_T_max  0.84
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            47278
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.852
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5577
_reflns_number_gt                4794
_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0708P)²+3.7545P] 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         5577
_refine_ls_number_parameters     980
_refine_ls_number_restraints     1099
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1460
_refine_ls_wR_factor_gt          0.1367
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.040
_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
O2A O 0.5890(10) 0.2620(8) 0.6236(6) 0.115(4) Uani 0.289(3) 1 d . U P A 1
H21 H 0.624260 0.278059 0.597598 0.172 Uiso 0.289(3) 1 d R U P A 1
H22 H 0.562233 0.306346 0.632722 0.172 Uiso 0.289(3) 1 d R U P A 1
O2B O 0.6204(6) 0.2807(5) 0.6536(3) 0.127(3) Uani 0.556(3) 1 d . U P B 2
H23 H 0.585322 0.320874 0.653940 0.190 Uiso 0.556(3) 1 d R U P B 2
H24 H 0.653111 0.292353 0.624855 0.190 Uiso 0.556(3) 1 d R U P B 2
O2C O 0.6001(15) 0.3616(12) 0.6011(10) 0.130(4) Uani 0.155(3) 1 d . U P C 3
H25 H 0.581522 0.339655 0.635813 0.194 Uiso 0.155(3) 1 d R U P C 3
H26 H 0.600885 0.319470 0.577864 0.194 Uiso 0.155(3) 1 d R U P C 3
P1B P 0.75761(7) 0.27352(10) 0.49797(6) 0.0358(3) Uani 0.653(3) 1 d D U P D 1
O1B O 0.68921(18) 0.3027(2) 0.53377(14) 0.0622(9) Uani 0.653(3) 1 d D . P D 1
C1B C 0.8591(3) 0.3148(4) 0.5109(2) 0.0344(11) Uani 0.653(3) 1 d D U P D 1
C2B C 0.8789(4) 0.3730(3) 0.5526(2) 0.0485(12) Uani 0.653(3) 1 d D U P D 1
H2B H 0.838339 0.394407 0.577985 0.058 Uiso 0.653(3) 1 calc R U P D 1
C3B C 0.9595(5) 0.3995(5) 0.5563(4) 0.0615(19) Uani 0.653(3) 1 d D U P D 1
H3B H 0.974332 0.440296 0.583967 0.074 Uiso 0.653(3) 1 calc R U P D 1
C4B C 1.0182(3) 0.3663(4) 0.5196(2) 0.0621(14) Uani 0.653(3) 1 d D U P D 1
H4B H 1.073197 0.384421 0.522770 0.075 Uiso 0.653(3) 1 calc R U P D 1
C5B C 0.9983(3) 0.3069(4) 0.4782(3) 0.0558(14) Uani 0.653(3) 1 d D U P D 1
H5B H 1.039162 0.284221 0.453608 0.067 Uiso 0.653(3) 1 calc R U P D 1
C6B C 0.9179(4) 0.2817(6) 0.4738(3) 0.0386(14) Uani 0.653(3) 1 d D U P D 1
C7B C 0.8876(5) 0.2196(5) 0.4303(3) 0.0382(17) Uani 0.653(3) 1 d D U P D 1
H7B H 0.934090 0.199906 0.405763 0.046 Uiso 0.653(3) 1 calc R U P D 1
C8B C 0.8221(4) 0.2570(5) 0.3917(3) 0.0321(12) Uani 0.653(3) 1 d D U P D 1
C9B C 0.8277(3) 0.2621(4) 0.3318(2) 0.0392(10) Uani 0.653(3) 1 d D U P D 1
H9B H 0.873668 0.239765 0.312122 0.047 Uiso 0.653(3) 1 calc R U P D 1
C10B C 0.7660(3) 0.2999(3) 0.3007(2) 0.0488(11) Uani 0.653(3) 1 d D U P D 1
H10B H 0.770380 0.304416 0.259510 0.059 Uiso 0.653(3) 1 calc R U P D 1
C11B C 0.6980(4) 0.3312(6) 0.3285(3) 0.0530(15) Uani 0.653(3) 1 d D U P D 1
H11B H 0.655790 0.356374 0.306396 0.064 Uiso 0.653(3) 1 calc R U P D 1
C12B C 0.6913(3) 0.3260(4) 0.3885(3) 0.0515(12) Uani 0.653(3) 1 d D U P D 1
H12B H 0.644624 0.347409 0.407793 0.062 Uiso 0.653(3) 1 calc R U P D 1
C13B C 0.7535(3) 0.2891(3) 0.4201(2) 0.0339(11) Uani 0.653(3) 1 d D U P D 1
C14B C 0.8509(7) 0.1480(4) 0.4636(4) 0.042(2) Uani 0.653(3) 1 d D U P D 1
C15B C 0.8820(6) 0.0684(4) 0.4607(4) 0.062(2) Uani 0.653(3) 1 d D U P D 1
H15B H 0.925190 0.055846 0.434483 0.075 Uiso 0.653(3) 1 calc R U P D 1
C16B C 0.8500(8) 0.0083(5) 0.4957(5) 0.080(3) Uani 0.653(3) 1 d D U P D 1
H16B H 0.873972 -0.044776 0.496231 0.096 Uiso 0.653(3) 1 calc R U P D 1
C17B C 0.7842(7) 0.0244(5) 0.5297(3) 0.084(3) Uani 0.653(3) 1 d D U P D 1
H17B H 0.760275 -0.018598 0.551899 0.100 Uiso 0.653(3) 1 calc R U P D 1
C18B C 0.7501(5) 0.1055(4) 0.5326(3) 0.0650(17) Uani 0.653(3) 1 d D U P D 1
H18B H 0.704867 0.116926 0.557238 0.078 Uiso 0.653(3) 1 calc R U P D 1
C19B C 0.7846(5) 0.1670(4) 0.4987(4) 0.0422(16) Uani 0.653(3) 1 d D U P D 1
P1C P 0.7495(2) 0.2388(3) 0.51272(16) 0.0545(9) Uani 0.302(3) 1 d D . P E 2
O1C O 0.6809(5) 0.2430(8) 0.5538(4) 0.092(3) Uani 0.302(3) 1 d D . P E 2
C1C C 0.8380(8) 0.3011(8) 0.5282(6) 0.055(3) Uani 0.302(3) 1 d D . P E 2
C2C C 0.8467(11) 0.3537(8) 0.5761(7) 0.090(4) Uani 0.302(3) 1 d D . P E 2
H2C H 0.805257 0.358614 0.604840 0.108 Uiso 0.302(3) 1 calc R U P E 2
C3C C 0.9185(12) 0.3982(9) 0.5795(8) 0.103(6) Uani 0.302(3) 1 d D . P E 2
H3C H 0.924721 0.436736 0.610226 0.123 Uiso 0.302(3) 1 calc R U P E 2
C4C C 0.9806(13) 0.3891(12) 0.5404(9) 0.091(6) Uani 0.302(3) 1 d D . P E 2
H4C H 1.029117 0.420590 0.544603 0.109 Uiso 0.302(3) 1 calc R U P E 2
C5C C 0.9731(9) 0.3332(9) 0.4941(7) 0.072(4) Uani 0.302(3) 1 d D . P E 2
H5C H 1.017227 0.323960 0.468010 0.086 Uiso 0.302(3) 1 calc R U P E 2
C6C C 0.8996(10) 0.2919(12) 0.4874(8) 0.054(4) Uani 0.302(3) 1 d D . P E 2
C7C C 0.8787(11) 0.2363(10) 0.4374(7) 0.055(4) Uani 0.302(3) 1 d D . P E 2
H7C H 0.925926 0.233556 0.409880 0.065 Uiso 0.302(3) 1 calc R U P E 2
C8C C 0.8022(10) 0.2643(14) 0.4045(6) 0.047(4) Uani 0.302(3) 1 d D . P E 2
C9C C 0.8008(8) 0.2846(8) 0.3457(5) 0.059(3) Uani 0.302(3) 1 d D . P E 2
H9C H 0.847952 0.276761 0.322298 0.071 Uiso 0.302(3) 1 calc R U P E 2
C10C C 0.7302(11) 0.3161(15) 0.3217(8) 0.073(5) Uani 0.302(3) 1 d D . P E 2
H10C H 0.728126 0.331335 0.281728 0.088 Uiso 0.302(3) 1 calc R U P E 2
C11C C 0.6626(9) 0.3250(9) 0.3572(7) 0.071(3) Uani 0.302(3) 1 d D . P E 2
H11C H 0.614314 0.347595 0.340775 0.085 Uiso 0.302(3) 1 calc R U P E 2
C12C C 0.6615(8) 0.3028(8) 0.4150(6) 0.067(3) Uani 0.302(3) 1 d D . P E 2
H12C H 0.613120 0.307301 0.437687 0.080 Uiso 0.302(3) 1 calc R U P E 2
C13C C 0.7348(7) 0.2731(8) 0.4394(5) 0.044(3) Uani 0.302(3) 1 d D . P E 2
C14C C 0.8604(14) 0.1511(10) 0.4604(12) 0.049(5) Uani 0.302(3) 1 d D . P E 2
C15C C 0.9076(12) 0.0825(10) 0.4502(11) 0.064(4) Uani 0.302(3) 1 d D . P E 2
H15C H 0.954005 0.086340 0.425486 0.076 Uiso 0.302(3) 1 calc R U P E 2
C16C C 0.8884(12) 0.0096(11) 0.4750(9) 0.078(4) Uani 0.302(3) 1 d D . P E 2
H16C H 0.924219 -0.035547 0.469281 0.094 Uiso 0.302(3) 1 calc R U P E 2
C17C C 0.8208(13) -0.0021(11) 0.5076(14) 0.071(5) Uani 0.302(3) 1 d D . P E 2
H17C H 0.804315 -0.055830 0.518581 0.085 Uiso 0.302(3) 1 calc R U P E 2
C18C C 0.7744(9) 0.0678(9) 0.5252(6) 0.060(3) Uani 0.302(3) 1 d D . P E 2
H18C H 0.731022 0.063820 0.552557 0.073 Uiso 0.302(3) 1 calc R U P E 2
C19C C 0.7971(11) 0.1431(7) 0.4996(8) 0.042(3) Uani 0.302(3) 1 d D . P E 2
P1E P 0.8970(16) 0.2113(19) 0.4171(12) 0.042(4) Uani 0.045(2) 1 d D U P F 3
O1E O 0.964(2) 0.189(3) 0.3776(19) 0.101(15) Uani 0.045(2) 1 d D . P F 3
C1E C 0.909(2) 0.290(4) 0.472(2) 0.038(4) Uani 0.045(2) 1 d D U P F 3
C2E C 0.981(3) 0.334(5) 0.482(3) 0.053(4) Uani 0.045(2) 1 d D U P F 3
H2E H 1.028750 0.323344 0.459087 0.064 Uiso 0.045(2) 1 calc R U P F 3
C3E C 0.982(4) 0.392(5) 0.526(3) 0.062(3) Uani 0.045(2) 1 d D U P F 3
H3E H 1.031077 0.420874 0.533575 0.074 Uiso 0.045(2) 1 calc R U P F 3
C4E C 0.914(4) 0.408(4) 0.558(3) 0.055(3) Uani 0.045(2) 1 d D U P F 3
H4E H 0.914646 0.451066 0.586550 0.066 Uiso 0.045(2) 1 calc R U P F 3
C5E C 0.843(3) 0.362(4) 0.550(2) 0.049(4) Uani 0.045(2) 1 d D U P F 3
H5E H 0.797246 0.369041 0.574775 0.059 Uiso 0.045(2) 1 calc R U P F 3
C6E C 0.839(2) 0.306(3) 0.505(2) 0.036(4) Uani 0.045(2) 1 d D U P F 3
C7E C 0.765(2) 0.259(2) 0.4841(17) 0.037(3) Uani 0.045(2) 1 d D U P F 3
H7E H 0.716785 0.274777 0.508334 0.044 Uiso 0.045(2) 1 calc R U P F 3
C8E C 0.747(3) 0.276(4) 0.4203(19) 0.034(4) Uani 0.045(2) 1 d D U P F 3
C9E C 0.684(4) 0.327(5) 0.402(3) 0.051(4) Uani 0.045(2) 1 d D U P F 3
H9E H 0.644810 0.346822 0.428766 0.061 Uiso 0.045(2) 1 calc R U P F 3
C10E C 0.681(5) 0.350(5) 0.344(3) 0.053(4) Uani 0.045(2) 1 d D U P F 3
H10E H 0.639445 0.386078 0.330944 0.064 Uiso 0.045(2) 1 calc R U P F 3
C11E C 0.737(5) 0.319(5) 0.305(3) 0.050(3) Uani 0.045(2) 1 d D U P F 3
H11E H 0.732389 0.332640 0.265176 0.060 Uiso 0.045(2) 1 calc R U P F 3
C12E C 0.801(4) 0.270(4) 0.3228(17) 0.039(4) Uani 0.045(2) 1 d D U P F 3
H12E H 0.840607 0.250890 0.295741 0.047 Uiso 0.045(2) 1 calc R U P F 3
C13E C 0.806(2) 0.249(4) 0.3818(16) 0.033(4) Uani 0.045(2) 1 d D U P F 3
C14E C 0.782(3) 0.168(3) 0.491(3) 0.043(4) Uani 0.045(2) 1 d D U P F 3
C15E C 0.730(3) 0.116(3) 0.521(2) 0.063(4) Uani 0.045(2) 1 d D U P F 3
H15E H 0.687028 0.137974 0.544135 0.076 Uiso 0.045(2) 1 calc R U P F 3
C16E C 0.741(4) 0.033(3) 0.519(3) 0.082(4) Uani 0.045(2) 1 d D U P F 3
H16E H 0.705245 -0.001873 0.539530 0.098 Uiso 0.045(2) 1 calc R U P F 3
C17E C 0.802(4) -0.001(3) 0.487(3) 0.081(5) Uani 0.045(2) 1 d D U P F 3
H17E H 0.810178 -0.058483 0.487480 0.097 Uiso 0.045(2) 1 calc R U P F 3
C18E C 0.855(4) 0.050(2) 0.453(3) 0.063(4) Uani 0.045(2) 1 d D U P F 3
H18E H 0.892491 0.027305 0.425739 0.076 Uiso 0.045(2) 1 calc R U P F 3
C19E C 0.848(3) 0.135(2) 0.461(2) 0.042(4) Uani 0.045(2) 1 d D U P F 3
P1A P 0.49189(5) 0.44940(4) 0.72727(3) 0.0407(2) Uani 0.904(3) 1 d D U P G 1
O1A O 0.49050(13) 0.37534(14) 0.68968(10) 0.0655(6) Uani 0.904(3) 1 d D . P G 1
C1A C 0.5583(2) 0.4515(2) 0.78832(16) 0.0360(7) Uani 0.904(3) 1 d D U P G 1
C2A C 0.6111(2) 0.3891(2) 0.80494(17) 0.0497(8) Uani 0.904(3) 1 d D U P G 1
H2A H 0.612114 0.338618 0.784216 0.060 Uiso 0.904(3) 1 calc R U P G 1
C3A C 0.6621(2) 0.4015(2) 0.85203(16) 0.0548(9) Uani 0.904(3) 1 d D U P G 1
H3A H 0.699141 0.359477 0.863313 0.066 Uiso 0.904(3) 1 calc R U P G 1
C4A C 0.6599(2) 0.4737(2) 0.88265(16) 0.0504(9) Uani 0.904(3) 1 d D U P G 1
H4A H 0.696027 0.481782 0.914518 0.060 Uiso 0.904(3) 1 calc R U P G 1
C5A C 0.6046(2) 0.5356(2) 0.86722(15) 0.0429(8) Uani 0.904(3) 1 d D U P G 1
H5A H 0.601912 0.584692 0.889486 0.052 Uiso 0.904(3) 1 calc R U P G 1
C6A C 0.5536(2) 0.5252(2) 0.81941(15) 0.0328(7) Uani 0.904(3) 1 d D U P G 1
C7A C 0.4946(4) 0.5888(3) 0.7974(3) 0.0413(11) Uani 0.904(3) 1 d D U P G 1
H7A H 0.496083 0.638420 0.823071 0.050 Uiso 0.904(3) 1 calc R U P G 1
C8A C 0.40821(19) 0.5522(2) 0.79649(16) 0.0410(7) Uani 0.904(3) 1 d D U P G 1
C9A C 0.34122(18) 0.5841(2) 0.82497(13) 0.0533(8) Uani 0.904(3) 1 d D U P G 1
H9A H 0.346007 0.633254 0.846984 0.064 Uiso 0.904(3) 1 calc R U P G 1
C10A C 0.26684(17) 0.5438(3) 0.82124(14) 0.0681(10) Uani 0.904(3) 1 d D . P G 1
H10A H 0.220686 0.566524 0.840484 0.082 Uiso 0.904(3) 1 calc R U P G 1
C11A C 0.25796(19) 0.4715(3) 0.79026(16) 0.0821(14) Uani 0.904(3) 1 d D U P G 1
H11A H 0.206971 0.443637 0.789545 0.098 Uiso 0.904(3) 1 calc R U P G 1
C12A C 0.3247(2) 0.4401(3) 0.76018(15) 0.0691(10) Uani 0.904(3) 1 d D . P G 1
H12A H 0.319242 0.391340 0.737798 0.083 Uiso 0.904(3) 1 calc R U P G 1
C13A C 0.39892(16) 0.47990(19) 0.76290(12) 0.0427(6) Uani 0.904(3) 1 d D U P G
1
C14A C 0.5143(3) 0.6124(2) 0.73550(17) 0.0409(8) Uani 0.904(3) 1 d D U P G 1
C15A C 0.5287(4) 0.6919(3) 0.7168(2) 0.0577(10) Uani 0.904(3) 1 d D U P G 1
H15A H 0.525125 0.736689 0.743198 0.069 Uiso 0.904(3) 1 calc R U P G 1
C16A C 0.5485(4) 0.7052(3) 0.6584(2) 0.0734(13) Uani 0.904(3) 1 d D U P G 1
H16A H 0.558342 0.759621 0.645235 0.088 Uiso 0.904(3) 1 calc R U P G 1
C17A C 0.5542(4) 0.6414(3) 0.61946(19) 0.0705(13) Uani 0.904(3) 1 d D U P G 1
H17A H 0.568483 0.652025 0.580051 0.085 Uiso 0.904(3) 1 calc R U P G 1
C18A C 0.5392(4) 0.5619(3) 0.63742(17) 0.0580(11) Uani 0.904(3) 1 d D U P G 1
H18A H 0.542916 0.517594 0.610657 0.070 Uiso 0.904(3) 1 calc R U P G 1
C19A C 0.5184(3) 0.5478(2) 0.69533(14) 0.0401(8) Uani 0.904(3) 1 d D U P G 1
P1D P 0.4841(13) 0.6035(10) 0.8036(8) 0.062(4) Uani 0.096(3) 1 d D U P G 2
O1D O 0.474(3) 0.6800(16) 0.8366(15) 0.164(15) Uani 0.096(3) 1 d D . P G 2
C1D C 0.560(2) 0.5346(18) 0.8295(14) 0.032(4) Uani 0.096(3) 1 d D U P G 2
C2D C 0.600(2) 0.551(2) 0.8811(13) 0.039(4) Uani 0.096(3) 1 d D U P G 2
H2D H 0.590892 0.600403 0.902551 0.047 Uiso 0.096(3) 1 calc R U P G 2
C3D C 0.655(2) 0.493(2) 0.8991(13) 0.047(5) Uani 0.096(3) 1 d D U P G 2
H3D H 0.685835 0.502285 0.933462 0.056 Uiso 0.096(3) 1 calc R U P G 2
C4D C 0.666(2) 0.422(2) 0.8693(15) 0.055(5) Uani 0.096(3) 1 d D U P G 2
H4D H 0.699275 0.379801 0.885554 0.066 Uiso 0.096(3) 1 calc R U P G 2
C5D C 0.629(2) 0.4083(19) 0.8156(15) 0.050(5) Uani 0.096(3) 1 d D U P G 2
H5D H 0.642244 0.361556 0.792763 0.060 Uiso 0.096(3) 1 calc R U P G 2
C6D C 0.571(2) 0.4656(18) 0.7959(14) 0.034(4) Uani 0.096(3) 1 d D U P G 2
C7D C 0.5232(12) 0.4567(12) 0.7417(9) 0.035(3) Uani 0.096(3) 1 d D U P G 2
H7D H 0.537676 0.405437 0.720096 0.042 Uiso 0.096(3) 1 calc R U P G 2
C8D C 0.4303(12) 0.4603(14) 0.7570(10) 0.042(4) Uani 0.096(3) 1 d D U P G 2
C9D C 0.3712(17) 0.3981(18) 0.7583(17) 0.119(17) Uani 0.096(3) 1 d D . P G 2
H9D H 0.382793 0.347371 0.739643 0.143 Uiso 0.096(3) 1 calc R U P G 2
C10D C 0.296(2) 0.408(2) 0.786(2) 0.16(3) Uani 0.096(3) 1 d D . P G 2
H10D H 0.259241 0.362703 0.786623 0.197 Uiso 0.096(3) 1 calc R U P G 2
C11D C 0.2738(18) 0.481(2) 0.8120(17) 0.088(5) Uani 0.096(3) 1 d D U P G 2
H11D H 0.220462 0.486897 0.827575 0.105 Uiso 0.096(3) 1 calc R U P G 2
C12D C 0.3287(15) 0.544(2) 0.8154(14) 0.063(5) Uani 0.096(3) 1 d D U P G 2
H12D H 0.315984 0.594240 0.834913 0.075 Uiso 0.096(3) 1 calc R U P G 2
C13D C 0.4046(14) 0.5314(16) 0.7884(16) 0.046(4) Uani 0.096(3) 1 d D U P G 2
C14D C 0.527(2) 0.5326(16) 0.7024(12) 0.042(4) Uani 0.096(3) 1 d D U P G 2
C15D C 0.540(3) 0.540(3) 0.6432(13) 0.056(5) Uani 0.096(3) 1 d D U P G 2
H15D H 0.539591 0.492225 0.619783 0.067 Uiso 0.096(3) 1 calc R U P G 2
C16D C 0.554(4) 0.616(3) 0.6165(18) 0.067(5) Uani 0.096(3) 1 d D U P G 2
H16D H 0.561165 0.616603 0.575484 0.081 Uiso 0.096(3) 1 calc R U P G 2
C17D C 0.557(5) 0.689(3) 0.6462(19) 0.074(5) Uani 0.096(3) 1 d D U P G 2
H17D H 0.568065 0.739025 0.626925 0.089 Uiso 0.096(3) 1 calc R U P G 2
C18D C 0.544(4) 0.685(2) 0.7054(19) 0.058(5) Uani 0.096(3) 1 d D U P G 2
H18D H 0.545445 0.733858 0.728452 0.070 Uiso 0.096(3) 1 calc R U P G 2
C19D C 0.527(3) 0.6094(18) 0.7307(12) 0.040(4) Uani 0.096(3) 1 d D U P G 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
P1B O1B 1.468(3) . ?
P1B C19B 1.789(6) . ?
P1B C13B 1.807(5) . ?
P1B C1B 1.816(5) . ?
C1B C2B 1.384(6) . ?
C1B C6B 1.394(7) . ?
C2B C3B 1.391(9) . ?
C3B C4B 1.388(10) . ?
C4B C5B 1.394(8) . ?
C5B C6B 1.383(6) . ?
C6B C7B 1.505(8) . ?
C7B C8B 1.518(8) . ?
C7B C14B 1.519(8) . ?
C8B C9B 1.379(6) . ?
C8B C13B 1.400(6) . ?
C9B C10B 1.383(6) . ?
C10B C11B 1.380(8) . ?
C11B C12B 1.384(8) . ?
C12B C13B 1.386(6) . ?
C14B C19B 1.386(7) . ?
C14B C15B 1.394(7) . ?
C15B C16B 1.371(10) . ?
C16B C17B 1.355(13) . ?
C17B C18B 1.435(11) . ?
C18B C19B 1.388(6) . ?
P1C O1C 1.468(8) . ?
P1C C19C 1.767(12) . ?
P1C C13C 1.788(10) . ?
P1C C1C 1.805(12) . ?
C1C C6C 1.385(14) . ?
C1C C2C 1.400(12) . ?
C2C C3C 1.382(17) . ?
C3C C4C 1.364(19) . ?
C4C C5C 1.405(17) . ?
C5C C6C 1.387(13) . ?
C6C C7C 1.501(15) . ?
C7C C14C 1.513(15) . ?
C7C C8C 1.532(15) . ?
C8C C13C 1.372(13) . ?
C8C C9C 1.387(13) . ?
C9C C10C 1.380(15) . ?
C10C C11C 1.382(17) . ?
C11C C12C 1.376(15) . ?
C12C C13C 1.411(11) . ?
C14C C15C 1.379(14) . ?
C14C C19C 1.379(14) . ?
C15C C16C 1.354(17) . ?
C16C C17C 1.35(2) . ?
C17C C18C 1.425(19) . ?
C18C C19C 1.410(14) . ?
P1E O1E 1.466(16) . ?
P1E C19E 1.784(18) . ?
P1E C1E 1.802(17) . ?
P1E C13E 1.805(17) . ?
C1E C2E 1.394(18) . ?
C1E C6E 1.397(18) . ?
C2E C3E 1.38(2) . ?
C3E C4E 1.37(2) . ?
C4E C5E 1.40(2) . ?
C5E C6E 1.382(18) . ?
C6E C7E 1.509(18) . ?
C7E C14E 1.520(18) . ?
C7E C8E 1.520(18) . ?
C8E C13E 1.382(18) . ?
C8E C9E 1.384(18) . ?
C9E C10E 1.378(19) . ?
C10E C11E 1.38(2) . ?
C11E C12E 1.37(2) . ?
C12E C13E 1.399(18) . ?
C14E C19E 1.387(17) . ?
C14E C15E 1.388(18) . ?
C15E C16E 1.36(2) . ?
C16E C17E 1.35(2) . ?
C17E C18E 1.43(2) . ?
C18E C19E 1.403(19) . ?
P1A O1A 1.483(2) . ?
P1A C1A 1.774(3) . ?
P1A C13A 1.798(3) . ?
P1A C19A 1.815(3) . ?
C1A C2A 1.387(4) . ?
C1A C6A 1.399(4) . ?
C2A C3A 1.381(5) . ?
C3A C4A 1.370(5) . ?
C4A C5A 1.400(4) . ?
C5A C6A 1.389(4) . ?
C6A C7A 1.503(6) . ?
C7A C14A 1.507(7) . ?
C7A C8A 1.536(6) . ?
C8A C9A 1.378(4) . ?
C8A C13A 1.415(4) . ?
C9A C10A 1.385(5) . ?
C10A C11A 1.384(6) . ?
C11A C12A 1.390(5) . ?
C12A C13A 1.378(4) . ?
C14A C15A 1.384(4) . ?
C14A C19A 1.400(4) . ?
C15A C16A 1.396(5) . ?
C16A C17A 1.372(6) . ?
C17A C18A 1.380(6) . ?
C18A C19A 1.391(4) . ?
P1D O1D 1.467(17) . ?
P1D C1D 1.779(18) . ?
P1D C13D 1.788(17) . ?
P1D C19D 1.817(18) . ?
C1D C6D 1.376(18) . ?
C1D C2D 1.380(19) . ?
C2D C3D 1.37(2) . ?
C3D C4D 1.36(2) . ?
C4D C5D 1.39(2) . ?
C5D C6D 1.399(19) . ?
C6D C7D 1.479(18) . ?
C7D C14D 1.531(19) . ?
C7D C8D 1.561(17) . ?
C8D C9D 1.401(18) . ?
C8D C13D 1.429(18) . ?
C9D C10D 1.39(2) . ?
C10D C11D 1.38(2) . ?
C11D C12D 1.37(2) . ?
C12D C13D 1.404(18) . ?
C14D C15D 1.38(2) . ?
C14D C19D 1.408(18) . ?
C15D C16D 1.39(2) . ?
C16D C17D 1.37(2) . ?
C17D C18D 1.38(2) . ?
C18D C19D 1.39(2) . ?

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
O1B P1B C19B 119.8(3) . . ?
O1B P1B C13B 118.7(2) . . ?
C19B P1B C13B 98.9(3) . . ?
O1B P1B C1B 119.1(2) . . ?
C19B P1B C1B 97.5(3) . . ?
C13B P1B C1B 98.3(2) . . ?
C2B C1B C6B 121.6(5) . . ?
C2B C1B P1B 125.5(5) . . ?
C6B C1B P1B 112.9(4) . . ?
C1B C2B C3B 118.5(5) . . ?
C4B C3B C2B 119.9(6) . . ?
C3B C4B C5B 121.5(5) . . ?
C6B C5B C4B 118.6(5) . . ?
C5B C6B C1B 119.9(5) . . ?
C5B C6B C7B 124.2(6) . . ?
C1B C6B C7B 115.9(5) . . ?
C6B C7B C8B 110.6(7) . . ?
C6B C7B C14B 108.1(6) . . ?
C8B C7B C14B 108.9(6) . . ?
C9B C8B C13B 119.7(5) . . ?
C9B C8B C7B 124.0(5) . . ?
C13B C8B C7B 116.4(5) . . ?
C8B C9B C10B 119.5(5) . . ?
C11B C10B C9B 121.0(5) . . ?
C10B C11B C12B 120.1(5) . . ?
C11B C12B C13B 119.3(5) . . ?
C12B C13B C8B 120.5(5) . . ?
C12B C13B P1B 127.3(5) . . ?
C8B C13B P1B 112.2(4) . . ?
C19B C14B C15B 121.5(6) . . ?
C19B C14B C7B 115.5(5) . . ?
C15B C14B C7B 123.0(6) . . ?
C16B C15B C14B 119.6(7) . . ?
C17B C16B C15B 120.3(8) . . ?
C16B C17B C18B 120.9(6) . . ?
C19B C18B C17B 118.7(6) . . ?
C14B C19B C18B 118.8(6) . . ?
C14B C19B P1B 113.9(4) . . ?
C18B C19B P1B 127.1(5) . . ?
O1C P1C C19C 119.2(7) . . ?
O1C P1C C13C 119.1(5) . . ?
C19C P1C C13C 100.0(7) . . ?
O1C P1C C1C 117.5(6) . . ?
C19C P1C C1C 100.1(7) . . ?
C13C P1C C1C 96.7(6) . . ?
C6C C1C C2C 121.5(12) . . ?
C6C C1C P1C 113.0(8) . . ?
C2C C1C P1C 125.5(11) . . ?
C3C C2C C1C 116.8(14) . . ?
C4C C3C C2C 122.7(14) . . ?
C3C C4C C5C 120.2(16) . . ?
C6C C5C C4C 118.3(15) . . ?
C1C C6C C5C 120.3(12) . . ?
C1C C6C C7C 114.6(11) . . ?
C5C C6C C7C 125.1(14) . . ?
C6C C7C C14C 109.4(15) . . ?
C6C C7C C8C 112.6(13) . . ?
C14C C7C C8C 106.5(15) . . ?
C13C C8C C9C 122.0(11) . . ?
C13C C8C C7C 113.5(11) . . ?
C9C C8C C7C 124.4(13) . . ?
C10C C9C C8C 119.5(13) . . ?
C9C C10C C11C 118.2(13) . . ?
C12C C11C C10C 123.5(12) . . ?
C11C C12C C13C 117.5(12) . . ?
C8C C13C C12C 119.2(11) . . ?
C8C C13C P1C 114.2(7) . . ?
C12C C13C P1C 126.5(10) . . ?
C15C C14C C19C 117.1(13) . . ?
C15C C14C C7C 124.9(14) . . ?
C19C C14C C7C 117.5(13) . . ?
C16C C15C C14C 120.6(14) . . ?
C17C C16C C15C 123.2(16) . . ?
C16C C17C C18C 118.8(15) . . ?
C19C C18C C17C 115.8(12) . . ?
C14C C19C C18C 123.5(12) . . ?
C14C C19C P1C 111.1(9) . . ?
C18C C19C P1C 125.4(11) . . ?
O1E P1E C19E 121(2) . . ?
O1E P1E C1E 121(2) . . ?
C19E P1E C1E 99.0(16) . . ?
O1E P1E C13E 115(2) . . ?
C19E P1E C13E 96.4(16) . . ?
C1E P1E C13E 99.3(17) . . ?
C2E C1E C6E 121(2) . . ?
C2E C1E P1E 125(2) . . ?
C6E C1E P1E 114.6(16) . . ?
C3E C2E C1E 118(2) . . ?
C4E C3E C2E 122(2) . . ?
C3E C4E C5E 119(3) . . ?
C6E C5E C4E 120(2) . . ?
C5E C6E C1E 120(2) . . ?
C5E C6E C7E 127(2) . . ?
C1E C6E C7E 113.5(18) . . ?
C6E C7E C14E 108(2) . . ?
C6E C7E C8E 112(2) . . ?
C14E C7E C8E 108(2) . . ?
C13E C8E C9E 121(2) . . ?
C13E C8E C7E 114.8(19) . . ?
C9E C8E C7E 123(2) . . ?
C10E C9E C8E 119(2) . . ?
C11E C10E C9E 120(2) . . ?
C12E C11E C10E 122(2) . . ?
C11E C12E C13E 118(2) . . ?
C8E C13E C12E 120(2) . . ?
C8E C13E P1E 113.7(16) . . ?
C12E C13E P1E 124(2) . . ?
C19E C14E C15E 120(2) . . ?
C19E C14E C7E 117.6(19) . . ?
C15E C14E C7E 123(2) . . ?
C16E C15E C14E 120(2) . . ?
C17E C16E C15E 122(3) . . ?
C16E C17E C18E 120(2) . . ?
C19E C18E C17E 117(2) . . ?
C14E C19E C18E 120(2) . . ?
C14E C19E P1E 111.5(17) . . ?
C18E C19E P1E 125(2) . . ?
O1A P1A C1A 118.98(15) . . ?
O1A P1A C13A 118.45(13) . . ?
C1A P1A C13A 98.87(15) . . ?
O1A P1A C19A 119.12(16) . . ?
C1A P1A C19A 98.93(16) . . ?
C13A P1A C19A 98.19(16) . . ?
C2A C1A C6A 121.5(3) . . ?
C2A C1A P1A 125.8(3) . . ?
C6A C1A P1A 112.7(2) . . ?
C3A C2A C1A 119.0(3) . . ?
C4A C3A C2A 120.7(3) . . ?
C3A C4A C5A 120.3(3) . . ?
C6A C5A C4A 120.1(3) . . ?
C5A C6A C1A 118.3(3) . . ?
C5A C6A C7A 124.6(3) . . ?
C1A C6A C7A 117.1(3) . . ?
C6A C7A C14A 110.8(4) . . ?
C6A C7A C8A 109.2(4) . . ?
C14A C7A C8A 106.4(4) . . ?
C9A C8A C13A 119.1(3) . . ?
C9A C8A C7A 125.5(3) . . ?
C13A C8A C7A 115.4(3) . . ?
C8A C9A C10A 119.5(3) . . ?
C11A C10A C9A 121.8(3) . . ?
C10A C11A C12A 119.0(3) . . ?
C13A C12A C11A 119.9(3) . . ?
C12A C13A C8A 120.7(3) . . ?
C12A C13A P1A 126.6(2) . . ?
C8A C13A P1A 112.7(2) . . ?
C15A C14A C19A 119.3(3) . . ?
C15A C14A C7A 124.6(4) . . ?
C19A C14A C7A 116.0(3) . . ?
C14A C15A C16A 118.8(4) . . ?
C17A C16A C15A 121.6(4) . . ?
C16A C17A C18A 120.2(4) . . ?
C17A C18A C19A 118.9(4) . . ?
C18A C19A C14A 121.1(3) . . ?
C18A C19A P1A 126.2(3) . . ?
C14A C19A P1A 112.7(3) . . ?
O1D P1D C1D 116.4(18) . . ?
O1D P1D C13D 125(2) . . ?
C1D P1D C13D 99.3(15) . . ?
O1D P1D C19D 118.4(19) . . ?
C1D P1D C19D 94.0(16) . . ?
C13D P1D C19D 97.8(15) . . ?
C6D C1D C2D 125.4(19) . . ?
C6D C1D P1D 114.8(16) . . ?
C2D C1D P1D 119.7(19) . . ?
C3D C2D C1D 116(2) . . ?
C4D C3D C2D 122(2) . . ?
C3D C4D C5D 121(2) . . ?
C4D C5D C6D 118(2) . . ?
C1D C6D C5D 116.9(18) . . ?
C1D C6D C7D 118.7(18) . . ?
C5D C6D C7D 124(2) . . ?
C6D C7D C14D 113.2(19) . . ?
C6D C7D C8D 109.1(18) . . ?
C14D C7D C8D 98.2(18) . . ?
C9D C8D C13D 111.7(17) . . ?
C9D C8D C7D 130.7(19) . . ?
C13D C8D C7D 115.5(15) . . ?
C10D C9D C8D 123(2) . . ?
C11D C10D C9D 122(2) . . ?
C12D C11D C10D 120(2) . . ?
C11D C12D C13D 116(2) . . ?
C12D C13D C8D 127.3(18) . . ?
C12D C13D P1D 117.4(17) . . ?
C8D C13D P1D 114.6(14) . . ?
C15D C14D C19D 112(2) . . ?
C15D C14D C7D 131(2) . . ?
C19D C14D C7D 116.4(19) . . ?
C14D C15D C16D 123(3) . . ?
C17D C16D C15D 124(3) . . ?
C16D C17D C18D 117(3) . . ?
C17D C18D C19D 118(2) . . ?
C18D C19D C14D 127(2) . . ?
C18D C19D P1D 120(2) . . ?
C14D C19D P1D 112.2(18) . . ?

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
O1B P1B C1B C2B -0.1(6) . . . . ?
C19B P1B C1B C2B -130.4(6) . . . . ?
C13B P1B C1B C2B 129.4(5) . . . . ?
O1B P1B C1B C6B -180.0(5) . . . . ?
C19B P1B C1B C6B 49.7(6) . . . . ?
C13B P1B C1B C6B -50.5(6) . . . . ?
C6B C1B C2B C3B 1.0(10) . . . . ?
P1B C1B C2B C3B -178.8(6) . . . . ?
C1B C2B C3B C4B -1.4(11) . . . . ?
C2B C3B C4B C5B 0.6(12) . . . . ?
C3B C4B C5B C6B 0.6(11) . . . . ?
C4B C5B C6B C1B -0.9(12) . . . . ?
C4B C5B C6B C7B 178.5(7) . . . . ?
C2B C1B C6B C5B 0.1(12) . . . . ?
P1B C1B C6B C5B -180.0(7) . . . . ?
C2B C1B C6B C7B -179.4(6) . . . . ?
P1B C1B C6B C7B 0.5(9) . . . . ?
C5B C6B C7B C8B -121.0(9) . . . . ?
C1B C6B C7B C8B 58.5(9) . . . . ?
C5B C6B C7B C14B 119.9(9) . . . . ?
C1B C6B C7B C14B -60.6(9) . . . . ?
C6B C7B C8B C9B 121.2(8) . . . . ?
C14B C7B C8B C9B -120.1(8) . . . . ?
C6B C7B C8B C13B -57.5(9) . . . . ?
C14B C7B C8B C13B 61.2(9) . . . . ?
C13B C8B C9B C10B 0.9(11) . . . . ?
C7B C8B C9B C10B -177.7(7) . . . . ?
C8B C9B C10B C11B -1.3(10) . . . . ?
C9B C10B C11B C12B 0.8(13) . . . . ?
C10B C11B C12B C13B 0.0(12) . . . . ?
C11B C12B C13B C8B -0.4(10) . . . . ?
C11B C12B C13B P1B -178.8(6) . . . . ?
C9B C8B C13B C12B -0.1(11) . . . . ?
C7B C8B C13B C12B 178.7(6) . . . . ?
C9B C8B C13B P1B 178.5(6) . . . . ?
C7B C8B C13B P1B -2.7(9) . . . . ?
O1B P1B C13B C12B -0.5(6) . . . . ?
C19B P1B C13B C12B 130.7(6) . . . . ?
C1B P1B C13B C12B -130.3(5) . . . . ?
O1B P1B C13B C8B -179.0(5) . . . . ?
C19B P1B C13B C8B -47.8(6) . . . . ?
C1B P1B C13B C8B 51.2(6) . . . . ?
C6B C7B C14B C19B 61.3(11) . . . . ?
C8B C7B C14B C19B -58.8(11) . . . . ?
C6B C7B C14B C15B -117.4(11) . . . . ?
C8B C7B C14B C15B 122.5(11) . . . . ?
C19B C14B C15B C16B -4.1(17) . . . . ?
C7B C14B C15B C16B 174.5(10) . . . . ?
C14B C15B C16B C17B 5.3(16) . . . . ?
C15B C16B C17B C18B -4.1(13) . . . . ?
C16B C17B C18B C19B 1.6(12) . . . . ?
C15B C14B C19B C18B 1.7(16) . . . . ?
C7B C14B C19B C18B -177.1(8) . . . . ?
C15B C14B C19B P1B 177.7(9) . . . . ?
C7B C14B C19B P1B -1.1(13) . . . . ?
C17B C18B C19B C14B -0.4(13) . . . . ?
C17B C18B C19B P1B -175.8(7) . . . . ?
O1B P1B C19B C14B -179.2(7) . . . . ?
C13B P1B C19B C14B 50.4(9) . . . . ?
C1B P1B C19B C14B -49.3(9) . . . . ?
O1B P1B C19B C18B -3.5(11) . . . . ?
C13B P1B C19B C18B -134.0(9) . . . . ?
C1B P1B C19B C18B 126.3(9) . . . . ?
O1C P1C C1C C6C 179.2(13) . . . . ?
C19C P1C C1C C6C 48.5(14) . . . . ?
C13C P1C C1C C6C -52.9(13) . . . . ?
O1C P1C C1C C2C -0.4(15) . . . . ?
C19C P1C C1C C2C -131.0(13) . . . . ?
C13C P1C C1C C2C 127.5(13) . . . . ?
C6C C1C C2C C3C 2(2) . . . . ?
P1C C1C C2C C3C -178.2(11) . . . . ?
C1C C2C C3C C4C -4(2) . . . . ?
C2C C3C C4C C5C 1(3) . . . . ?
C3C C4C C5C C6C 4(3) . . . . ?
C2C C1C C6C C5C 2(3) . . . . ?
P1C C1C C6C C5C -177.5(16) . . . . ?
C2C C1C C6C C7C -177.2(15) . . . . ?
P1C C1C C6C C7C 3(2) . . . . ?
C4C C5C C6C C1C -5(3) . . . . ?
C4C C5C C6C C7C 174.2(18) . . . . ?
C1C C6C C7C C14C -61(2) . . . . ?
C5C C6C C7C C14C 120(2) . . . . ?
C1C C6C C7C C8C 57(2) . . . . ?
C5C C6C C7C C8C -122(2) . . . . ?
C6C C7C C8C C13C -56(2) . . . . ?
C14C C7C C8C C13C 64(2) . . . . ?
C6C C7C C8C C9C 120(2) . . . . ?
C14C C7C C8C C9C -120(2) . . . . ?
C13C C8C C9C C10C 1(3) . . . . ?
C7C C8C C9C C10C -174.2(19) . . . . ?
C8C C9C C10C C11C -1(3) . . . . ?
C9C C10C C11C C12C -1(3) . . . . ?
C10C C11C C12C C13C 3(2) . . . . ?
C9C C8C C13C C12C 1(3) . . . . ?
C7C C8C C13C C12C 176.7(14) . . . . ?
C9C C8C C13C P1C 177.2(16) . . . . ?
C7C C8C C13C P1C -7(2) . . . . ?
C11C C12C C13C C8C -3(2) . . . . ?
C11C C12C C13C P1C -178.9(11) . . . . ?
O1C P1C C13C C8C -178.3(13) . . . . ?
C19C P1C C13C C8C -46.6(15) . . . . ?
C1C P1C C13C C8C 55.0(14) . . . . ?
O1C P1C C13C C12C -2.0(15) . . . . ?
C19C P1C C13C C12C 129.8(13) . . . . ?
C1C P1C C13C C12C -128.7(12) . . . . ?
C6C C7C C14C C15C -113(3) . . . . ?
C8C C7C C14C C15C 125(3) . . . . ?
C6C C7C C14C C19C 60(3) . . . . ?
C8C C7C C14C C19C -62(3) . . . . ?
C19C C14C C15C C16C 4(4) . . . . ?
C7C C14C C15C C16C 177(2) . . . . ?
C14C C15C C16C C17C 4(5) . . . . ?
C15C C16C C17C C18C -11(5) . . . . ?
C16C C17C C18C C19C 9(4) . . . . ?
C15C C14C C19C C18C -6(4) . . . . ?
C7C C14C C19C C18C -178.8(19) . . . . ?
C15C C14C C19C P1C 174(2) . . . . ?
C7C C14C C19C P1C 1(3) . . . . ?
C17C C18C C19C C14C -1(3) . . . . ?
C17C C18C C19C P1C 179.1(19) . . . . ?
O1C P1C C19C C14C -179.5(17) . . . . ?
C13C P1C C19C C14C 49(2) . . . . ?
C1C P1C C19C C14C -50(2) . . . . ?
O1C P1C C19C C18C 1(2) . . . . ?
C13C P1C C19C C18C -131.1(18) . . . . ?
C1C P1C C19C C18C 130.1(18) . . . . ?
O1E P1E C1E C2E -2(5) . . . . ?
C19E P1E C1E C2E 133(5) . . . . ?
C13E P1E C1E C2E -129(5) . . . . ?
O1E P1E C1E C6E 178(4) . . . . ?
C19E P1E C1E C6E -47(4) . . . . ?
C13E P1E C1E C6E 51(4) . . . . ?
C6E C1E C2E C3E 1(3) . . . . ?
P1E C1E C2E C3E -179(5) . . . . ?
C1E C2E C3E C4E -1(3) . . . . ?
C2E C3E C4E C5E 4(6) . . . . ?
C3E C4E C5E C6E -7(7) . . . . ?
C4E C5E C6E C1E 6(7) . . . . ?
C4E C5E C6E C7E -172(6) . . . . ?
C2E C1E C6E C5E -3(6) . . . . ?
P1E C1E C6E C5E 176(5) . . . . ?
C2E C1E C6E C7E 175(5) . . . . ?
P1E C1E C6E C7E -5(6) . . . . ?
C5E C6E C7E C14E -119(6) . . . . ?
C1E C6E C7E C14E 63(4) . . . . ?
C5E C6E C7E C8E 122(6) . . . . ?
C1E C6E C7E C8E -56(4) . . . . ?
C6E C7E C8E C13E 65(4) . . . . ?
C14E C7E C8E C13E -54(5) . . . . ?
C6E C7E C8E C9E -103(5) . . . . ?
C14E C7E C8E C9E 138(4) . . . . ?
C13E C8E C9E C10E 2(3) . . . . ?
C7E C8E C9E C10E 169(6) . . . . ?
C8E C9E C10E C11E 2(3) . . . . ?
C9E C10E C11E C12E -4(7) . . . . ?
C10E C11E C12E C13E 2(8) . . . . ?
C9E C8E C13E C12E -3(5) . . . . ?
C7E C8E C13E C12E -172(5) . . . . ?
C9E C8E C13E P1E 161(4) . . . . ?
C7E C8E C13E P1E -7(5) . . . . ?
C11E C12E C13E C8E 1(7) . . . . ?
C11E C12E C13E P1E -161(6) . . . . ?
O1E P1E C13E C8E -175(4) . . . . ?
C19E P1E C13E C8E 57(4) . . . . ?
C1E P1E C13E C8E -43(4) . . . . ?
O1E P1E C13E C12E -11(6) . . . . ?
C19E P1E C13E C12E -139(5) . . . . ?
C1E P1E C13E C12E 120(5) . . . . ?
C6E C7E C14E C19E -60(4) . . . . ?
C8E C7E C14E C19E 61(4) . . . . ?
C6E C7E C14E C15E 127(4) . . . . ?
C8E C7E C14E C15E -112(5) . . . . ?
C19E C14E C15E C16E -4(3) . . . . ?
C7E C14E C15E C16E 170(6) . . . . ?
C14E C15E C16E C17E 0(3) . . . . ?
C15E C16E C17E C18E -3(6) . . . . ?
C16E C17E C18E C19E 9(7) . . . . ?
C15E C14E C19E C18E 10(6) . . . . ?
C7E C14E C19E C18E -163(6) . . . . ?
C15E C14E C19E P1E 172(4) . . . . ?
C7E C14E C19E P1E -2(5) . . . . ?
C17E C18E C19E C14E -13(7) . . . . ?
C17E C18E C19E P1E -172(5) . . . . ?
O1E P1E C19E C14E -175(4) . . . . ?
C1E P1E C19E C14E 50(4) . . . . ?
C13E P1E C19E C14E -51(3) . . . . ?
O1E P1E C19E C18E -14(6) . . . . ?
C1E P1E C19E C18E -149(6) . . . . ?
C13E P1E C19E C18E 110(6) . . . . ?
O1A P1A C1A C2A 0.3(4) . . . . ?
C13A P1A C1A C2A 129.9(3) . . . . ?
C19A P1A C1A C2A -130.2(3) . . . . ?
O1A P1A C1A C6A 179.5(2) . . . . ?
C13A P1A C1A C6A -50.9(3) . . . . ?
C19A P1A C1A C6A 48.9(3) . . . . ?
C6A C1A C2A C3A -2.3(5) . . . . ?
P1A C1A C2A C3A 176.8(3) . . . . ?
C1A C2A C3A C4A 1.1(5) . . . . ?
C2A C3A C4A C5A 1.2(5) . . . . ?
C3A C4A C5A C6A -2.3(4) . . . . ?
C4A C5A C6A C1A 1.1(4) . . . . ?
C4A C5A C6A C7A -177.3(4) . . . . ?
C2A C1A C6A C5A 1.2(5) . . . . ?
P1A C1A C6A C5A -178.0(3) . . . . ?
C2A C1A C6A C7A 179.7(4) . . . . ?
P1A C1A C6A C7A 0.5(5) . . . . ?
C5A C6A C7A C14A 119.9(4) . . . . ?
C1A C6A C7A C14A -58.5(5) . . . . ?
C5A C6A C7A C8A -123.1(4) . . . . ?
C1A C6A C7A C8A 58.5(5) . . . . ?
C6A C7A C8A C9A 123.1(4) . . . . ?
C14A C7A C8A C9A -117.2(4) . . . . ?
C6A C7A C8A C13A -57.2(5) . . . . ?
C14A C7A C8A C13A 62.5(5) . . . . ?
C13A C8A C9A C10A 1.5(5) . . . . ?
C7A C8A C9A C10A -178.9(4) . . . . ?
C8A C9A C10A C11A 0.9(5) . . . . ?
C9A C10A C11A C12A -2.6(6) . . . . ?
C10A C11A C12A C13A 1.8(6) . . . . ?
C11A C12A C13A C8A 0.6(6) . . . . ?
C11A C12A C13A P1A -179.9(3) . . . . ?
C9A C8A C13A C12A -2.2(5) . . . . ?
C7A C8A C13A C12A 178.1(4) . . . . ?
C9A C8A C13A P1A 178.2(3) . . . . ?
C7A C8A C13A P1A -1.5(5) . . . . ?
O1A P1A C13A C12A 1.5(4) . . . . ?
C1A P1A C13A C12A -128.4(3) . . . . ?
C19A P1A C13A C12A 131.1(3) . . . . ?
O1A P1A C13A C8A -178.9(2) . . . . ?
C1A P1A C13A C8A 51.1(3) . . . . ?
C19A P1A C13A C8A -49.3(3) . . . . ?
C6A C7A C14A C15A -124.6(5) . . . . ?
C8A C7A C14A C15A 116.7(5) . . . . ?
C6A C7A C14A C19A 54.9(5) . . . . ?
C8A C7A C14A C19A -63.8(5) . . . . ?
C19A C14A C15A C16A -1.2(6) . . . . ?
C7A C14A C15A C16A 178.2(5) . . . . ?
C14A C15A C16A C17A -0.1(7) . . . . ?
C15A C16A C17A C18A 0.8(7) . . . . ?
C16A C17A C18A C19A -0.1(5) . . . . ?
C17A C18A C19A C14A -1.3(5) . . . . ?
C17A C18A C19A P1A 177.1(4) . . . . ?
C15A C14A C19A C18A 2.0(6) . . . . ?
C7A C14A C19A C18A -177.5(5) . . . . ?
C15A C14A C19A P1A -176.6(4) . . . . ?
C7A C14A C19A P1A 3.9(5) . . . . ?
O1A P1A C19A C18A -0.7(4) . . . . ?
C1A P1A C19A C18A 129.8(4) . . . . ?
C13A P1A C19A C18A -129.8(4) . . . . ?
O1A P1A C19A C14A 177.8(3) . . . . ?
C1A P1A C19A C14A -51.7(3) . . . . ?
C13A P1A C19A C14A 48.7(3) . . . . ?
O1D P1D C1D C6D -177(3) . . . . ?
C13D P1D C1D C6D 46(3) . . . . ?
C19D P1D C1D C6D -52(3) . . . . ?
O1D P1D C1D C2D 6(3) . . . . ?
C13D P1D C1D C2D -131(2) . . . . ?
C19D P1D C1D C2D 130(3) . . . . ?
C6D C1D C2D C3D -1(2) . . . . ?
P1D C1D C2D C3D 177(3) . . . . ?
C1D C2D C3D C4D -3(2) . . . . ?
C2D C3D C4D C5D 7(4) . . . . ?
C3D C4D C5D C6D -8(5) . . . . ?
C2D C1D C6D C5D -1(4) . . . . ?
P1D C1D C6D C5D -178(3) . . . . ?
C2D C1D C6D C7D 180(3) . . . . ?
P1D C1D C6D C7D 2(4) . . . . ?
C4D C5D C6D C1D 5(5) . . . . ?
C4D C5D C6D C7D -176(4) . . . . ?
C1D C6D C7D C14D 50(3) . . . . ?
C5D C6D C7D C14D -129(3) . . . . ?
C1D C6D C7D C8D -58(3) . . . . ?
C5D C6D C7D C8D 123(3) . . . . ?
C6D C7D C8D C9D -107(3) . . . . ?
C14D C7D C8D C9D 135(3) . . . . ?
C6D C7D C8D C13D 55(3) . . . . ?
C14D C7D C8D C13D -63(3) . . . . ?
C13D C8D C9D C10D 1.8(17) . . . . ?
C7D C8D C9D C10D 164(3) . . . . ?
C8D C9D C10D C11D 2(2) . . . . ?
C9D C10D C11D C12D -5(4) . . . . ?
C10D C11D C12D C13D 3(5) . . . . ?
C11D C12D C13D C8D 1(5) . . . . ?
C11D C12D C13D P1D -168(3) . . . . ?
C9D C8D C13D C12D -4(4) . . . . ?
C7D C8D C13D C12D -169(3) . . . . ?
C9D C8D C13D P1D 166(3) . . . . ?
C7D C8D C13D P1D 1(3) . . . . ?
O1D P1D C13D C12D -7(4) . . . . ?
C1D P1D C13D C12D 124(3) . . . . ?
C19D P1D C13D C12D -140(3) . . . . ?
O1D P1D C13D C8D -178(3) . . . . ?
C1D P1D C13D C8D -47(3) . . . . ?
C19D P1D C13D C8D 49(3) . . . . ?
C6D C7D C14D C15D 134(4) . . . . ?
C8D C7D C14D C15D -112(4) . . . . ?
C6D C7D C14D C19D -38(4) . . . . ?
C8D C7D C14D C19D 77(3) . . . . ?
C19D C14D C15D C16D 1.8(19) . . . . ?
C7D C14D C15D C16D -170(4) . . . . ?
C14D C15D C16D C17D 1(2) . . . . ?
C15D C16D C17D C18D -2(5) . . . . ?
C16D C17D C18D C19D -1(6) . . . . ?
C17D C18D C19D C14D 4(6) . . . . ?
C17D C18D C19D P1D -165(4) . . . . ?
C15D C14D C19D C18D -4(4) . . . . ?
C7D C14D C19D C18D 169(4) . . . . ?
C15D C14D C19D P1D 165(3) . . . . ?
C7D C14D C19D P1D -22(4) . . . . ?
O1D P1D C19D C18D -5(5) . . . . ?
C1D P1D C19D C18D -128(4) . . . . ?
C13D P1D C19D C18D 132(4) . . . . ?
O1D P1D C19D C14D -175(3) . . . . ?
C1D P1D C19D C14D 62(3) . . . . ?
C13D P1D C19D C14D -38(3) . . . . ?

_refine_diff_density_max         0.311
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.047





# start Validation Reply Form
_vrf_PLAT088_nt1402_SMC190_oxide_100K 
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.69 Note  
RESPONSE: Whole structure is disordered.
;
_vrf_PLAT213_nt1402_SMC190_oxide_100K 
;
PROBLEM: Atom C4C             has ADP max/min Ratio .....        3.6 prolat
RESPONSE: Minor component of disorder.
;
_vrf_PLAT221_nt1402_SMC190_oxide_100K 
;
PROBLEM: Solv./Anion  Resd 4  C   Ueq(max)/Ueq(min) Range        5.0 Ratio 
RESPONSE: Minor component of disorder.
;
_vrf_PLAT223_nt1402_SMC190_oxide_100K 
;
PROBLEM: Solv./Anion  Resd 4  H   Ueq(max)/Ueq(min) Range        4.7 Ratio 
RESPONSE: Minor component of disorder.
;
_vrf_PLAT250_nt1402_SMC190_oxide_100K 
;
PROBLEM: Large U3/U1 Ratio for <U(i,j)> Tensor(Resd    2)        2.1 Note  
RESPONSE: Minor component of disorder.
;
_vrf_PLAT260_nt1402_SMC190_oxide_100K 
;
PROBLEM: Large Average Ueq of Residue Including       O2B      0.126 Check 
RESPONSE: Disordered (over at least 3 positions) water molecule.

;
_vrf_PLAT911_nt1402_SMC190_oxide_100K 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          3 Report
RESPONSE: These reflections are missing because of the instrument geometry 
limitations.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1368_SMC166_100K
_database_code_depnum_ccdc_archive 'CCDC 2347268'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        
'9-phosphatriptycene oxide hemi (hydrogen peroxide)'
_chemical_name_common            
'9-phosphatriptycene oxide hemi (hydrogen peroxide)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 O P, 0.5(H2 O2)'
_chemical_formula_sum            'C19 H14 O2 P'
_chemical_formula_weight         305.27

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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/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'
'-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                   20.3958(6)
_cell_length_b                   13.4454(6)
_cell_length_c                   12.1945(4)
_cell_angle_alpha                90
_cell_angle_beta                 117.6040(10)
_cell_angle_gamma                90
_cell_volume                     2963.44(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9843
_cell_measurement_theta_min      4.9266
_cell_measurement_theta_max      68.1074

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    1.675
_shelx_estimated_absorpt_T_min   0.642
_shelx_estimated_absorpt_T_max   0.812
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_T_max  0.81
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            24650
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.927
_diffrn_reflns_theta_max         68.112
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             2676
_reflns_number_gt                2671
_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0347P)²+3.9495P] 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     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.00178(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2676
_refine_ls_number_parameters     204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0894
_refine_ls_wR_factor_gt          0.0894
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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 0.33253(2) 0.64438(3) 0.26926(3) 0.01383(14) Uani 1 1 d . . . . .
O1 O 0.35557(6) 0.70484(8) 0.19083(9) 0.0201(2) Uani 1 1 d . . . . .
C1 C 0.23804(8) 0.60262(10) 0.20365(13) 0.0155(3) Uani 1 1 d . . . . .
C2 C 0.18210(8) 0.62364(11) 0.08567(13) 0.0195(3) Uani 1 1 d . . . . .
H2 H 0.191914 0.662452 0.029827 0.023 Uiso 1 1 calc R U . . .
C3 C 0.11109(8) 0.58660(11) 0.05065(14) 0.0225(3) Uani 1 1 d . . . . .
H3 H 0.072001 0.600794 -0.029320 0.027 Uiso 1 1 calc R U . . .
C4 C 0.09768(8) 0.52909(11) 0.13269(14) 0.0219(3) Uani 1 1 d . . . . .
H4 H 0.049267 0.504213 0.108092 0.026 Uiso 1 1 calc R U . . .
C5 C 0.15403(8) 0.50727(10) 0.25046(14) 0.0176(3) Uani 1 1 d . . . . .
H5 H 0.144341 0.466715 0.305108 0.021 Uiso 1 1 calc R U . . .
C6 C 0.22443(8) 0.54520(10) 0.28736(13) 0.0148(3) Uani 1 1 d . . . . .
C7 C 0.28904(7) 0.52983(10) 0.41656(12) 0.0142(3) Uani 1 1 d . . . . .
H7 H 0.273342 0.489102 0.468943 0.017 Uiso 1 1 calc R U . . .
C8 C 0.31742(7) 0.63211(10) 0.47553(13) 0.0137(3) Uani 1 1 d . . . . .
C9 C 0.34183(7) 0.69668(10) 0.41125(12) 0.0147(3) Uani 1 1 d . . . . .
C10 C 0.37260(8) 0.78845(10) 0.45958(13) 0.0175(3) Uani 1 1 d . . . . .
H10 H 0.388971 0.831325 0.415309 0.021 Uiso 1 1 calc R U . . .
C11 C 0.37914(8) 0.81680(11) 0.57397(14) 0.0202(3) Uani 1 1 d . . . . .
H11 H 0.400813 0.879035 0.608902 0.024 Uiso 1 1 calc R U . . .
C12 C 0.35404(8) 0.75430(11) 0.63705(13) 0.0192(3) Uani 1 1 d . . . . .
H12 H 0.358099 0.774548 0.714588 0.023 Uiso 1 1 calc R U . . .
C13 C 0.32292(8) 0.66210(11) 0.58803(13) 0.0161(3) Uani 1 1 d . . . . .
H13 H 0.305572 0.620072 0.631688 0.019 Uiso 1 1 calc R U . . .
C14 C 0.37885(7) 0.52833(10) 0.33084(12) 0.0143(3) Uani 1 1 d . . . . .
C15 C 0.43767(8) 0.49082(11) 0.31651(13) 0.0172(3) Uani 1 1 d . . . . .
H15 H 0.455026 0.524914 0.266768 0.021 Uiso 1 1 calc R U . . .
C16 C 0.47111(8) 0.40248(11) 0.37592(13) 0.0192(3) Uani 1 1 d . . . . .
H16 H 0.511731 0.376191 0.367347 0.023 Uiso 1 1 calc R U . . .
C17 C 0.44492(8) 0.35311(11) 0.44750(13) 0.0192(3) Uani 1 1 d . . . . .
H17 H 0.467904 0.292911 0.487761 0.023 Uiso 1 1 calc R U . . .
C18 C 0.38515(8) 0.39047(11) 0.46149(13) 0.0172(3) Uani 1 1 d . . . . .
H18 H 0.367339 0.355616 0.510100 0.021 Uiso 1 1 calc R U . . .
C19 C 0.35224(7) 0.47883(10) 0.40368(12) 0.0143(3) Uani 1 1 d . . . . .
O2 O 0.48138(7) 0.81836(10) 0.28742(12) 0.0381(3) Uani 1 1 d . . . . .
H2O H 0.4418(14) 0.7752(19) 0.246(2) 0.052(7) Uiso 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 O1 1.4876(10) . ?
P1 C9 1.7956(14) . ?
P1 C14 1.7983(14) . ?
P1 C1 1.8002(14) . ?
C1 C2 1.389(2) . ?
C1 C6 1.406(2) . ?
C2 C3 1.398(2) . ?
C3 C4 1.388(2) . ?
C4 C5 1.393(2) . ?
C5 C6 1.388(2) . ?
C6 C7 1.5289(19) . ?
C7 C19 1.5309(18) . ?
C7 C8 1.5354(19) . ?
C8 C13 1.3837(19) . ?
C8 C9 1.4062(19) . ?
C9 C10 1.386(2) . ?
C10 C11 1.391(2) . ?
C11 C12 1.387(2) . ?
C12 C13 1.395(2) . ?
C14 C15 1.385(2) . ?
C14 C19 1.4048(19) . ?
C15 C16 1.394(2) . ?
C16 C17 1.386(2) . ?
C17 C18 1.400(2) . ?
C18 C19 1.386(2) . ?
O2 O2 1.433(3) 2_655 ?

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
O1 P1 C9 118.84(6) . . ?
O1 P1 C14 118.77(6) . . ?
C9 P1 C14 97.86(6) . . ?
O1 P1 C1 118.48(6) . . ?
C9 P1 C1 99.42(6) . . ?
C14 P1 C1 99.32(6) . . ?
C2 C1 C6 121.32(13) . . ?
C2 C1 P1 126.38(12) . . ?
C6 C1 P1 112.29(10) . . ?
C1 C2 C3 118.77(14) . . ?
C4 C3 C2 120.02(14) . . ?
C3 C4 C5 121.10(14) . . ?
C6 C5 C4 119.50(14) . . ?
C5 C6 C1 119.27(13) . . ?
C5 C6 C7 123.55(13) . . ?
C1 C6 C7 117.16(12) . . ?
C6 C7 C19 108.63(11) . . ?
C6 C7 C8 108.63(11) . . ?
C19 C7 C8 107.25(11) . . ?
C13 C8 C9 119.06(13) . . ?
C13 C8 C7 124.41(12) . . ?
C9 C8 C7 116.48(12) . . ?
C10 C9 C8 121.34(13) . . ?
C10 C9 P1 125.69(11) . . ?
C8 C9 P1 112.91(10) . . ?
C9 C10 C11 118.97(13) . . ?
C12 C11 C10 120.08(13) . . ?
C11 C12 C13 120.82(13) . . ?
C8 C13 C12 119.71(13) . . ?
C15 C14 C19 121.22(13) . . ?
C15 C14 P1 125.55(11) . . ?
C19 C14 P1 113.14(10) . . ?
C14 C15 C16 119.25(13) . . ?
C17 C16 C15 119.80(13) . . ?
C16 C17 C18 121.09(13) . . ?
C19 C18 C17 119.31(13) . . ?
C18 C19 C14 119.32(13) . . ?
C18 C19 C7 124.35(12) . . ?
C14 C19 C7 116.30(12) . . ?

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
O1 P1 C1 C2 -2.07(15) . . . . ?
C9 P1 C1 C2 128.19(13) . . . . ?
C14 P1 C1 C2 -132.16(13) . . . . ?
O1 P1 C1 C6 179.10(9) . . . . ?
C9 P1 C1 C6 -50.64(11) . . . . ?
C14 P1 C1 C6 49.01(11) . . . . ?
C6 C1 C2 C3 0.1(2) . . . . ?
P1 C1 C2 C3 -178.66(11) . . . . ?
C1 C2 C3 C4 -0.7(2) . . . . ?
C2 C3 C4 C5 0.0(2) . . . . ?
C3 C4 C5 C6 1.3(2) . . . . ?
C4 C5 C6 C1 -1.9(2) . . . . ?
C4 C5 C6 C7 176.94(13) . . . . ?
C2 C1 C6 C5 1.2(2) . . . . ?
P1 C1 C6 C5 -179.89(10) . . . . ?
C2 C1 C6 C7 -177.66(12) . . . . ?
P1 C1 C6 C7 1.24(15) . . . . ?
C5 C6 C7 C19 122.08(14) . . . . ?
C1 C6 C7 C19 -59.10(15) . . . . ?
C5 C6 C7 C8 -121.57(14) . . . . ?
C1 C6 C7 C8 57.26(15) . . . . ?
C6 C7 C8 C13 123.99(14) . . . . ?
C19 C7 C8 C13 -118.78(14) . . . . ?
C6 C7 C8 C9 -58.62(15) . . . . ?
C19 C7 C8 C9 58.62(15) . . . . ?
C13 C8 C9 C10 1.4(2) . . . . ?
C7 C8 C9 C10 -176.14(12) . . . . ?
C13 C8 C9 P1 178.61(10) . . . . ?
C7 C8 C9 P1 1.07(15) . . . . ?
O1 P1 C9 C10 -3.49(15) . . . . ?
C14 P1 C9 C10 125.60(13) . . . . ?
C1 P1 C9 C10 -133.52(13) . . . . ?
O1 P1 C9 C8 179.45(9) . . . . ?
C14 P1 C9 C8 -51.46(11) . . . . ?
C1 P1 C9 C8 49.42(11) . . . . ?
C8 C9 C10 C11 -0.1(2) . . . . ?
P1 C9 C10 C11 -176.97(11) . . . . ?
C9 C10 C11 C12 -1.0(2) . . . . ?
C10 C11 C12 C13 0.8(2) . . . . ?
C9 C8 C13 C12 -1.5(2) . . . . ?
C7 C8 C13 C12 175.78(12) . . . . ?
C11 C12 C13 C8 0.5(2) . . . . ?
O1 P1 C14 C15 3.12(15) . . . . ?
C9 P1 C14 C15 -126.03(13) . . . . ?
C1 P1 C14 C15 133.01(12) . . . . ?
O1 P1 C14 C19 179.68(9) . . . . ?
C9 P1 C14 C19 50.54(11) . . . . ?
C1 P1 C14 C19 -50.42(11) . . . . ?
C19 C14 C15 C16 -0.2(2) . . . . ?
P1 C14 C15 C16 176.10(10) . . . . ?
C14 C15 C16 C17 0.5(2) . . . . ?
C15 C16 C17 C18 0.0(2) . . . . ?
C16 C17 C18 C19 -0.7(2) . . . . ?
C17 C18 C19 C14 0.9(2) . . . . ?
C17 C18 C19 C7 -177.04(13) . . . . ?
C15 C14 C19 C18 -0.5(2) . . . . ?
P1 C14 C19 C18 -177.21(10) . . . . ?
C15 C14 C19 C7 177.62(12) . . . . ?
P1 C14 C19 C7 0.89(15) . . . . ?
C6 C7 C19 C18 -124.48(14) . . . . ?
C8 C7 C19 C18 118.28(14) . . . . ?
C6 C7 C19 C14 57.52(15) . . . . ?
C8 C7 C19 C14 -59.71(15) . . . . ?

_refine_diff_density_max         0.410
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.058



# start Validation Reply Form
_vrf_PLAT411_nt1368_SMC166_100K  
;
PROBLEM: Short Inter H...H Contact  H15      ..H15      .       2.06 Ang.  
RESPONSE: This is a feature of the packing.
;
_vrf_PLAT911_nt1368_SMC166_100K  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         36 Report
RESPONSE: These reflections are missing because of the instrument geometry 
limitations.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1366_SMC88_100K
_database_code_depnum_ccdc_archive 'CCDC 2347269'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        '9-phosphatriptycene selenide'
_chemical_name_common            '9-phosphatriptycene selenide'
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 P Se'
_chemical_formula_sum            'C19 H13 P Se'
_chemical_formula_weight         351.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se 0.2367 1.4831 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/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'
'-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                   14.0369(5)
_cell_length_b                   13.6803(5)
_cell_length_c                   15.7202(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.7890(10)
_cell_angle_gamma                90
_cell_volume                     3018.45(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9936
_cell_measurement_theta_min      2.6096
_cell_measurement_theta_max      27.8578

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_F_000             1408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.372
_shelx_estimated_absorpt_T_min   0.692
_shelx_estimated_absorpt_T_max   0.853
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_T_max  0.85
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            17865
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.925
_diffrn_reflns_theta_max         19.502
_diffrn_reflns_theta_full        19.502
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2661
_reflns_number_gt                2503
_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/4 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0334P)²+4.1458P] 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         2661
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0782
_refine_ls_wR_factor_gt          0.0768
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.002
_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
Se1 Se 0.60537(2) 0.25223(2) 0.12410(2) 0.01904(11) Uani 1 1 d . . . . .
P1 P 0.66636(3) 0.37696(3) 0.17912(3) 0.01346(13) Uani 1 1 d . . . . .
C1 C 0.68336(13) 0.38214(13) 0.29345(12) 0.0154(4) Uani 1 1 d . . . . .
C2 C 0.65722(13) 0.31073(14) 0.35052(12) 0.0185(4) Uani 1 1 d . . . . .
H2 H 0.627698 0.252185 0.331141 0.022 Uiso 1 1 calc R U . . .
C3 C 0.67477(14) 0.32572(15) 0.43708(13) 0.0228(4) Uani 1 1 d . . . . .
H3 H 0.656798 0.277430 0.477210 0.027 Uiso 1 1 calc R U . . .
C4 C 0.71858(14) 0.41136(16) 0.46452(12) 0.0237(4) Uani 1 1 d . . . . .
H4 H 0.731146 0.420820 0.523483 0.028 Uiso 1 1 calc R U . . .
C5 C 0.74426(14) 0.48337(15) 0.40686(12) 0.0207(4) Uani 1 1 d . . . . .
H5 H 0.773860 0.541779 0.426448 0.025 Uiso 1 1 calc R U . . .
C6 C 0.72658(13) 0.46978(14) 0.32067(12) 0.0167(4) Uani 1 1 d . . . . .
C7 C 0.75153(13) 0.54385(13) 0.25232(12) 0.0167(4) Uani 1 1 d . . . . .
H7 H 0.781485 0.603288 0.278300 0.020 Uiso 1 1 calc R U . . .
C8 C 0.81917(13) 0.49555(14) 0.19006(12) 0.0160(4) Uani 1 1 d . . . . .
C9 C 0.90927(14) 0.53087(14) 0.17185(12) 0.0200(4) Uani 1 1 d . . . . .
H9 H 0.932724 0.587793 0.199695 0.024 Uiso 1 1 calc R U . . .
C10 C 0.96516(14) 0.48266(15) 0.11269(13) 0.0226(4) Uani 1 1 d . . . . .
H10 H 1.027066 0.506595 0.100668 0.027 Uiso 1 1 calc R U . . .
C11 C 0.93136(14) 0.40001(15) 0.07111(13) 0.0213(4) Uani 1 1 d . . . . .
H11 H 0.969852 0.368269 0.030258 0.026 Uiso 1 1 calc R U . . .
C12 C 0.84124(14) 0.36324(14) 0.08891(12) 0.0181(4) Uani 1 1 d . . . . .
H12 H 0.818022 0.306372 0.060816 0.022 Uiso 1 1 calc R U . . .
C13 C 0.78615(13) 0.41105(14) 0.14826(12) 0.0157(4) Uani 1 1 d . . . . .
C14 C 0.61030(13) 0.49469(13) 0.16324(11) 0.0152(4) Uani 1 1 d . . . . .
C15 C 0.52781(14) 0.51206(15) 0.11572(12) 0.0191(4) Uani 1 1 d . . . . .
H15 H 0.494179 0.459674 0.089369 0.023 Uiso 1 1 calc R U . . .
C16 C 0.49547(14) 0.60797(16) 0.10754(13) 0.0234(4) Uani 1 1 d . . . . .
H16 H 0.439409 0.621452 0.075095 0.028 Uiso 1 1 calc R U . . .
C17 C 0.54473(15) 0.68348(15) 0.14650(13) 0.0249(5) Uani 1 1 d . . . . .
H17 H 0.521817 0.748515 0.140677 0.030 Uiso 1 1 calc R U . . .
C19 C 0.66075(13) 0.57103(14) 0.20278(12) 0.0160(4) Uani 1 1 d . . . . .
C18 C 0.62754(14) 0.66598(14) 0.19426(12) 0.0209(4) Uani 1 1 d . . . . .
H18 H 0.660787 0.718592 0.220651 0.025 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
Se1 P1 2.0910(5) . ?
P1 C14 1.8083(19) . ?
P1 C1 1.8113(19) . ?
P1 C13 1.8174(19) . ?
C1 C2 1.379(3) . ?
C1 C6 1.408(3) . ?
C2 C3 1.395(3) . ?
C3 C4 1.389(3) . ?
C4 C5 1.390(3) . ?
C5 C6 1.387(3) . ?
C6 C7 1.521(3) . ?
C7 C8 1.524(3) . ?
C7 C19 1.530(3) . ?
C8 C9 1.387(3) . ?
C8 C13 1.405(3) . ?
C9 C10 1.391(3) . ?
C10 C11 1.387(3) . ?
C11 C12 1.393(3) . ?
C12 C13 1.384(3) . ?
C14 C15 1.390(3) . ?
C14 C19 1.402(3) . ?
C15 C16 1.394(3) . ?
C16 C17 1.382(3) . ?
C17 C18 1.396(3) . ?
C19 C18 1.386(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
C14 P1 C1 98.81(8) . . ?
C14 P1 C13 97.88(9) . . ?
C1 P1 C13 98.34(8) . . ?
C14 P1 Se1 119.66(6) . . ?
C1 P1 Se1 119.34(6) . . ?
C13 P1 Se1 118.30(6) . . ?
C2 C1 C6 121.53(17) . . ?
C2 C1 P1 125.80(15) . . ?
C6 C1 P1 112.66(14) . . ?
C1 C2 C3 119.04(19) . . ?
C4 C3 C2 119.91(19) . . ?
C3 C4 C5 120.86(18) . . ?
C6 C5 C4 119.86(19) . . ?
C5 C6 C1 118.80(18) . . ?
C5 C6 C7 124.13(18) . . ?
C1 C6 C7 117.07(16) . . ?
C6 C7 C8 108.44(15) . . ?
C6 C7 C19 108.85(15) . . ?
C8 C7 C19 107.48(15) . . ?
C9 C8 C13 119.06(18) . . ?
C9 C8 C7 124.01(17) . . ?
C13 C8 C7 116.92(16) . . ?
C8 C9 C10 119.80(19) . . ?
C11 C10 C9 120.61(18) . . ?
C10 C11 C12 120.37(18) . . ?
C13 C12 C11 118.81(19) . . ?
C12 C13 C8 121.34(18) . . ?
C12 C13 P1 125.89(15) . . ?
C8 C13 P1 112.75(14) . . ?
C15 C14 C19 121.52(17) . . ?
C15 C14 P1 125.75(15) . . ?
C19 C14 P1 112.71(14) . . ?
C14 C15 C16 118.58(19) . . ?
C17 C16 C15 120.18(18) . . ?
C16 C17 C18 121.21(19) . . ?
C18 C19 C14 119.22(18) . . ?
C18 C19 C7 123.61(17) . . ?
C14 C19 C7 117.17(16) . . ?
C19 C18 C17 119.29(19) . . ?

_refine_diff_density_max         0.595
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.082



# start Validation Reply Form
_vrf_PLAT911_nt1366_SMC88_100K   
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.595         13 Report
RESPONSE: These reflections are missing because of the instrument geometry 
limitations.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1382_SMC166_v2_100K
_database_code_depnum_ccdc_archive 'CCDC 2347266'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        '9-phosphatriptycene oxide'
_chemical_name_common            '9-phosphatriptycene oxide'
_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                   7.2774(2)
_cell_length_b                   8.0944(3)
_cell_length_c                   13.1388(4)
_cell_angle_alpha                81.7506(9)
_cell_angle_beta                 79.8049(10)
_cell_angle_gamma                70.6319(9)
_cell_volume                     715.63(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9819
_cell_measurement_theta_min      3.4321
_cell_measurement_theta_max      68.1731

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_F_000             300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.074
_exptl_absorpt_coefficient_mu    1.649
_shelx_estimated_absorpt_T_min   0.588
_shelx_estimated_absorpt_T_max   0.888
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_T_max  1.000
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            27465
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_limit_h_min       -8
_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         3.432
_diffrn_reflns_theta_max         68.215
_diffrn_reflns_theta_full        67.679
_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             2579
_reflns_number_gt                2578
_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0339P)²+0.4635P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2579
_refine_ls_number_parameters     380
_refine_ls_number_restraints     391
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0857
_refine_ls_wR_factor_gt          0.0857
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.049
_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 0.52918(5) 0.51709(5) 0.22993(3) 0.01048(15) Uani 0.962(2) 1 d D U P A 1
O1 O 0.32719(14) 0.54136(13) 0.21017(8) 0.0164(3) Uani 0.962(2) 1 d D . P A 1
C1 C 0.6017(2) 0.7080(2) 0.23594(17) 0.0123(3) Uani 0.962(2) 1 d D U P A 1
C2 C 0.4869(3) 0.8831(2) 0.22147(17) 0.0144(4) Uani 0.962(2) 1 d D U P A 1
H2 H 0.357222 0.913016 0.204856 0.017 Uiso 0.962(2) 1 calc R U P A 1
C3 C 0.5663(3) 1.0138(2) 0.23191(19) 0.0170(4) Uani 0.962(2) 1 d D U P A 1
H3 H 0.490338 1.134076 0.222136 0.020 Uiso 0.962(2) 1 calc R U P A 1
C4 C 0.7560(3) 0.9690(2) 0.25652(16) 0.0169(4) Uani 0.962(2) 1 d D U P A 1
H4 H 0.807563 1.059096 0.264562 0.020 Uiso 0.962(2) 1 calc R U P A 1
C5 C 0.8717(3) 0.7929(2) 0.2696(3) 0.0150(4) Uani 0.962(2) 1 d D U P A 1
H5 H 1.001819 0.763245 0.285393 0.018 Uiso 0.962(2) 1 calc R U P A 1
C6 C 0.7941(2) 0.6617(2) 0.2592(2) 0.0128(4) Uani 0.962(2) 1 d D U P A 1
C7 C 0.9097(3) 0.4666(3) 0.27058(15) 0.0127(4) Uani 0.962(2) 1 d D U P A 1
H7 H 1.045726 0.448922 0.284904 0.015 Uiso 0.962(2) 1 calc R U P A 1
C8 C 0.7997(2) 0.3765(3) 0.35883(14) 0.0126(4) Uani 0.962(2) 1 d D U P A 1
C9 C 0.8812(3) 0.2766(3) 0.44447(14) 0.0164(4) Uani 0.962(2) 1 d D U P A 1
H9 H 1.012664 0.263557 0.452400 0.020 Uiso 0.962(2) 1 calc R U P A 1
C10 C 0.7683(5) 0.1952(7) 0.5189(2) 0.0199(5) Uani 0.962(2) 1 d D U P A 1
H10 H 0.824453 0.126042 0.577176 0.024 Uiso 0.962(2) 1 calc R U P A 1
C11 C 0.5759(3) 0.2139(3) 0.5090(2) 0.0188(6) Uani 0.962(2) 1 d D U P A 1
H11 H 0.500651 0.158697 0.560492 0.023 Uiso 0.962(2) 1 calc R U P A 1
C12 C 0.4929(3) 0.3140(4) 0.4232(2) 0.0154(4) Uani 0.962(2) 1 d D U P A 1
H12 H 0.361187 0.327226 0.415680 0.019 Uiso 0.962(2) 1 calc R U P A 1
C13 C 0.6054(3) 0.3940(3) 0.34912(14) 0.0128(3) Uani 0.962(2) 1 d D U P A 1
C14 C 0.7351(2) 0.4026(3) 0.14076(12) 0.0123(4) Uani 0.962(2) 1 d D U P A 1
C15 C 0.7257(3) 0.3318(3) 0.05219(15) 0.0152(4) Uani 0.962(2) 1 d D U P A 1
H15 H 0.602197 0.342185 0.033040 0.018 Uiso 0.962(2) 1 calc R U P A 1
C16 C 0.8998(3) 0.2455(2) -0.00802(13) 0.0180(4) Uani 0.962(2) 1 d D U P A 1
H16 H 0.895599 0.196022 -0.068565 0.022 Uiso 0.962(2) 1 calc R U P A 1
C17 C 1.0796(3) 0.2318(3) 0.02032(14) 0.0189(4) Uani 0.962(2) 1 d D U P A 1
H17 H 1.197812 0.172459 -0.021147 0.023 Uiso 0.962(2) 1 calc R U P A 1
C18 C 1.0893(2) 0.3038(2) 0.10891(15) 0.0157(4) Uani 0.962(2) 1 d D U P A 1
H18 H 1.213117 0.295456 0.126911 0.019 Uiso 0.962(2) 1 calc R U P A 1
C19 C 0.9164(2) 0.3879(3) 0.17047(16) 0.0129(4) Uani 0.962(2) 1 d D U P A 1
P1B P 0.992(2) 0.451(2) 0.2692(13) 0.030(3) Uani 0.038(2) 1 d D U P A 2
O1B O 1.202(4) 0.428(6) 0.281(3) 0.062(11) Uani 0.038(2) 1 d D . P A 2
C1B C 0.827(5) 0.673(3) 0.254(5) 0.015(4) Uani 0.038(2) 1 d D U P A 2
C2B C 0.849(8) 0.830(4) 0.272(8) 0.015(4) Uani 0.038(2) 1 d D U P A 2
H2B H 0.954156 0.829950 0.305809 0.018 Uiso 0.038(2) 1 calc R U P A 2
C3B C 0.714(8) 0.988(5) 0.239(5) 0.015(4) Uani 0.038(2) 1 d D U P A 2
H3B H 0.748196 1.093699 0.224117 0.018 Uiso 0.038(2) 1 calc R U P A 2
C4B C 0.529(7) 0.987(5) 0.229(6) 0.014(4) Uani 0.038(2) 1 d D U P A 2
H4B H 0.424314 1.094022 0.222815 0.017 Uiso 0.038(2) 1 calc R U P A 2
C5B C 0.498(6) 0.829(4) 0.227(5) 0.012(4) Uani 0.038(2) 1 d D U P A 2
H5B H 0.373305 0.829300 0.213179 0.014 Uiso 0.038(2) 1 calc R U P A 2
C6B C 0.639(5) 0.671(4) 0.243(5) 0.015(4) Uani 0.038(2) 1 d D U P A 2
C7B C 0.602(4) 0.492(4) 0.251(2) 0.019(3) Uani 0.038(2) 1 d D U P A 2
H7B H 0.463121 0.507701 0.243090 0.023 Uiso 0.038(2) 1 calc R U P A 2
C8B C 0.653(5) 0.395(7) 0.355(3) 0.013(4) Uani 0.038(2) 1 d D U P A 2
C9B C 0.526(7) 0.324(13) 0.425(5) 0.014(5) Uani 0.038(2) 1 d D U P A 2
H9B H 0.389007 0.360404 0.421965 0.017 Uiso 0.038(2) 1 calc R U P A 2
C10B C 0.611(10) 0.195(11) 0.502(6) 0.018(4) Uani 0.038(2) 1 d D U P A 2
H10B H 0.549664 0.109476 0.532975 0.021 Uiso 0.038(2) 1 calc R U P A 2
C11B C 0.785(14) 0.192(19) 0.532(7) 0.018(4) Uani 0.038(2) 1 d D U P A 2
H11B H 0.822732 0.132133 0.596690 0.022 Uiso 0.038(2) 1 calc R U P A 2
C12B C 0.904(8) 0.278(10) 0.466(3) 0.017(4) Uani 0.038(2) 1 d D U P A 2
H12B H 1.022626 0.281736 0.485650 0.020 Uiso 0.038(2) 1 calc R U P A 2
C13B C 0.846(5) 0.358(7) 0.372(3) 0.013(4) Uani 0.038(2) 1 d D U P A 2
C14B C 0.952(5) 0.364(8) 0.161(3) 0.013(4) Uani 0.038(2) 1 d D U P A 2
C15B C 1.092(5) 0.272(8) 0.085(4) 0.014(3) Uani 0.038(2) 1 d D U P A 2
H15B H 1.227782 0.237499 0.090849 0.017 Uiso 0.038(2) 1 calc R U P A 2
C16B C 1.027(6) 0.231(8) 0.002(3) 0.016(3) Uani 0.038(2) 1 d D U P A 2
H16B H 1.118949 0.182342 -0.055325 0.019 Uiso 0.038(2) 1 calc R U P A 2
C17B C 0.830(7) 0.262(7) 0.004(3) 0.015(3) Uani 0.038(2) 1 d D U P A 2
H17B H 0.787364 0.210901 -0.044636 0.018 Uiso 0.038(2) 1 calc R U P A 2
C18B C 0.693(6) 0.366(8) 0.074(3) 0.016(4) Uani 0.038(2) 1 d D U P A 2
H18B H 0.561629 0.420380 0.060589 0.019 Uiso 0.038(2) 1 calc R U P A 2
C19B C 0.749(5) 0.391(7) 0.164(3) 0.014(4) Uani 0.038(2) 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
P1 O1 1.4818(10) . ?
P1 C13 1.8016(17) . ?
P1 C14 1.8016(17) . ?
P1 C1 1.8061(16) . ?
C1 C2 1.392(2) . ?
C1 C6 1.402(2) . ?
C2 C3 1.395(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.523(2) . ?
C7 C8 1.527(2) . ?
C7 C19 1.528(2) . ?
C7 H7 1.0000 . ?
C8 C9 1.389(2) . ?
C8 C13 1.401(2) . ?
C9 C10 1.398(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(2) . ?
C12 H12 0.9500 . ?
C14 C15 1.390(2) . ?
C14 C19 1.405(2) . ?
C15 C16 1.391(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.397(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(2) . ?
C18 H18 0.9500 . ?
P1B O1B 1.512(17) . ?
P1B C14B 1.788(17) . ?
P1B C13B 1.804(17) . ?
P1B C1B 1.807(17) . ?
C1B C2B 1.391(19) . ?
C1B C6B 1.400(18) . ?
C2B C3B 1.40(2) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.38(2) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.378(19) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.368(19) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.542(18) . ?
C7B C8B 1.512(18) . ?
C7B C19B 1.544(18) . ?
C7B H7B 1.0000 . ?
C8B C13B 1.384(18) . ?
C8B C9B 1.395(19) . ?
C9B C10B 1.41(2) . ?
C9B H9B 0.9500 . ?
C10B C11B 1.38(2) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.40(2) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.382(19) . ?
C12B H12B 0.9500 . ?
C14B C15B 1.388(19) . ?
C14B C19B 1.408(18) . ?
C15B C16B 1.380(19) . ?
C15B H15B 0.9500 . ?
C16B C17B 1.37(2) . ?
C16B H16B 0.9500 . ?
C17B C18B 1.38(2) . ?
C17B H17B 0.9500 . ?
C18B C19B 1.379(19) . ?
C18B H18B 0.9500 . ?

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
O1 P1 C13 117.85(7) . . ?
O1 P1 C14 118.98(7) . . ?
C13 P1 C14 98.62(8) . . ?
O1 P1 C1 119.34(7) . . ?
C13 P1 C1 99.26(8) . . ?
C14 P1 C1 98.61(8) . . ?
C2 C1 C6 121.40(15) . . ?
C2 C1 P1 126.61(13) . . ?
C6 C1 P1 111.99(12) . . ?
C1 C2 C3 118.56(16) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 120.39(15) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.82(16) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 119.23(16) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C1 119.58(15) . . ?
C5 C6 C7 123.03(16) . . ?
C1 C6 C7 117.39(14) . . ?
C6 C7 C8 108.57(14) . . ?
C6 C7 C19 108.45(15) . . ?
C8 C7 C19 107.82(15) . . ?
C6 C7 H7 110.6 . . ?
C8 C7 H7 110.6 . . ?
C19 C7 H7 110.6 . . ?
C9 C8 C13 119.11(15) . . ?
C9 C8 C7 124.49(15) . . ?
C13 C8 C7 116.37(14) . . ?
C8 C9 C10 119.51(17) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 121.00(18) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 119.90(17) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 119.06(16) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C8 121.42(15) . . ?
C12 C13 P1 125.50(13) . . ?
C8 C13 P1 112.99(12) . . ?
C15 C14 C19 121.24(15) . . ?
C15 C14 P1 126.38(13) . . ?
C19 C14 P1 112.38(13) . . ?
C14 C15 C16 119.08(16) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C17 C16 C15 120.03(16) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 120.98(15) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 119.44(15) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C14 119.21(15) . . ?
C18 C19 C7 123.89(15) . . ?
C14 C19 C7 116.90(14) . . ?
O1B P1B C14B 117.5(18) . . ?
O1B P1B C13B 118.7(18) . . ?
C14B P1B C13B 99.6(18) . . ?
O1B P1B C1B 117.6(18) . . ?
C14B P1B C1B 99.9(18) . . ?
C13B P1B C1B 100.0(18) . . ?
C2B C1B C6B 119(2) . . ?
C2B C1B P1B 129(2) . . ?
C6B C1B P1B 110.0(17) . . ?
C1B C2B C3B 119(3) . . ?
C1B C2B H2B 120.7 . . ?
C3B C2B H2B 120.7 . . ?
C4B C3B C2B 118(3) . . ?
C4B C3B H3B 121.0 . . ?
C2B C3B H3B 121.0 . . ?
C5B C4B C3B 119(3) . . ?
C5B C4B H4B 120.3 . . ?
C3B C4B H4B 120.3 . . ?
C6B C5B C4B 122(2) . . ?
C6B C5B H5B 118.9 . . ?
C4B C5B H5B 118.9 . . ?
C5B C6B C1B 118(2) . . ?
C5B C6B C7B 123(2) . . ?
C1B C6B C7B 119(2) . . ?
C8B C7B C6B 108(2) . . ?
C8B C7B C19B 108(2) . . ?
C6B C7B C19B 105(2) . . ?
C8B C7B H7B 111.6 . . ?
C6B C7B H7B 111.6 . . ?
C19B C7B H7B 111.6 . . ?
C13B C8B C9B 120(2) . . ?
C13B C8B C7B 116(2) . . ?
C9B C8B C7B 124(2) . . ?
C8B C9B C10B 117(3) . . ?
C8B C9B H9B 121.7 . . ?
C10B C9B H9B 121.7 . . ?
C11B C10B C9B 120(3) . . ?
C11B C10B H10B 120.0 . . ?
C9B C10B H10B 120.0 . . ?
C10B C11B C12B 119(3) . . ?
C10B C11B H11B 120.6 . . ?
C12B C11B H11B 120.6 . . ?
C13B C12B C11B 118(2) . . ?
C13B C12B H12B 120.9 . . ?
C11B C12B H12B 120.9 . . ?
C12B C13B C8B 121(2) . . ?
C12B C13B P1B 125(2) . . ?
C8B C13B P1B 113.4(17) . . ?
C15B C14B C19B 122(2) . . ?
C15B C14B P1B 128(2) . . ?
C19B C14B P1B 109.9(17) . . ?
C16B C15B C14B 118(2) . . ?
C16B C15B H15B 120.9 . . ?
C14B C15B H15B 120.9 . . ?
C17B C16B C15B 119(3) . . ?
C17B C16B H16B 120.5 . . ?
C15B C16B H16B 120.5 . . ?
C16B C17B C18B 121(3) . . ?
C16B C17B H17B 119.5 . . ?
C18B C17B H17B 119.5 . . ?
C17B C18B C19B 119(3) . . ?
C17B C18B H18B 120.3 . . ?
C19B C18B H18B 120.3 . . ?
C18B C19B C14B 115(2) . . ?
C18B C19B C7B 123(2) . . ?
C14B C19B C7B 119(2) . . ?

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
O1 P1 C1 C2 -1.5(2) . . . . ?
C13 P1 C1 C2 -130.9(2) . . . . ?
C14 P1 C1 C2 128.8(2) . . . . ?
O1 P1 C1 C6 177.67(15) . . . . ?
C13 P1 C1 C6 48.28(18) . . . . ?
C14 P1 C1 C6 -51.99(18) . . . . ?
C6 C1 C2 C3 -0.8(3) . . . . ?
P1 C1 C2 C3 178.26(18) . . . . ?
C1 C2 C3 C4 -0.2(3) . . . . ?
C2 C3 C4 C5 1.1(4) . . . . ?
C3 C4 C5 C6 -0.9(4) . . . . ?
C4 C5 C6 C1 -0.1(4) . . . . ?
C4 C5 C6 C7 179.2(2) . . . . ?
C2 C1 C6 C5 1.0(4) . . . . ?
P1 C1 C6 C5 -178.3(2) . . . . ?
C2 C1 C6 C7 -178.3(2) . . . . ?
P1 C1 C6 C7 2.4(3) . . . . ?
C5 C6 C7 C8 120.6(3) . . . . ?
C1 C6 C7 C8 -60.1(2) . . . . ?
C5 C6 C7 C19 -122.5(3) . . . . ?
C1 C6 C7 C19 56.8(2) . . . . ?
C6 C7 C8 C9 -124.6(2) . . . . ?
C19 C7 C8 C9 118.1(2) . . . . ?
C6 C7 C8 C13 57.3(2) . . . . ?
C19 C7 C8 C13 -60.0(2) . . . . ?
C13 C8 C9 C10 0.2(4) . . . . ?
C7 C8 C9 C10 -177.8(3) . . . . ?
C8 C9 C10 C11 -0.5(6) . . . . ?
C9 C10 C11 C12 0.5(7) . . . . ?
C10 C11 C12 C13 -0.2(5) . . . . ?
C11 C12 C13 C8 -0.1(4) . . . . ?
C11 C12 C13 P1 176.2(2) . . . . ?
C9 C8 C13 C12 0.2(4) . . . . ?
C7 C8 C13 C12 178.3(2) . . . . ?
C9 C8 C13 P1 -176.58(18) . . . . ?
C7 C8 C13 P1 1.6(2) . . . . ?
O1 P1 C13 C12 2.3(3) . . . . ?
C14 P1 C13 C12 -127.0(3) . . . . ?
C1 P1 C13 C12 132.7(3) . . . . ?
O1 P1 C13 C8 178.91(14) . . . . ?
C14 P1 C13 C8 49.54(17) . . . . ?
C1 P1 C13 C8 -50.73(17) . . . . ?
O1 P1 C14 C15 0.0(2) . . . . ?
C13 P1 C14 C15 128.64(19) . . . . ?
C1 P1 C14 C15 -130.54(19) . . . . ?
O1 P1 C14 C19 -179.17(14) . . . . ?
C13 P1 C14 C19 -50.56(17) . . . . ?
C1 P1 C14 C19 50.25(16) . . . . ?
C19 C14 C15 C16 -0.3(3) . . . . ?
P1 C14 C15 C16 -179.39(15) . . . . ?
C14 C15 C16 C17 -0.3(3) . . . . ?
C15 C16 C17 C18 -0.1(3) . . . . ?
C16 C17 C18 C19 1.1(3) . . . . ?
C17 C18 C19 C14 -1.7(3) . . . . ?
C17 C18 C19 C7 178.16(19) . . . . ?
C15 C14 C19 C18 1.2(3) . . . . ?
P1 C14 C19 C18 -179.50(17) . . . . ?
C15 C14 C19 C7 -178.58(19) . . . . ?
P1 C14 C19 C7 0.7(2) . . . . ?
C6 C7 C19 C18 121.5(2) . . . . ?
C8 C7 C19 C18 -121.1(2) . . . . ?
C6 C7 C19 C14 -58.7(2) . . . . ?
C8 C7 C19 C14 58.7(2) . . . . ?
O1B P1B C1B C2B -15(8) . . . . ?
C14B P1B C1B C2B -143(8) . . . . ?
C13B P1B C1B C2B 115(8) . . . . ?
O1B P1B C1B C6B 180(4) . . . . ?
C14B P1B C1B C6B 51(5) . . . . ?
C13B P1B C1B C6B -50(5) . . . . ?
C6B C1B C2B C3B -25(11) . . . . ?
P1B C1B C2B C3B 170(6) . . . . ?
C1B C2B C3B C4B 25(12) . . . . ?
C2B C3B C4B C5B -15(11) . . . . ?
C3B C4B C5B C6B 6(12) . . . . ?
C4B C5B C6B C1B -5(11) . . . . ?
C4B C5B C6B C7B 174(6) . . . . ?
C2B C1B C6B C5B 15(10) . . . . ?
P1B C1B C6B C5B -177(5) . . . . ?
C2B C1B C6B C7B -164(6) . . . . ?
P1B C1B C6B C7B 3(7) . . . . ?
C5B C6B C7B C8B -123(6) . . . . ?
C1B C6B C7B C8B 56(6) . . . . ?
C5B C6B C7B C19B 121(6) . . . . ?
C1B C6B C7B C19B -59(5) . . . . ?
C6B C7B C8B C13B -60(5) . . . . ?
C19B C7B C8B C13B 53(5) . . . . ?
C6B C7B C8B C9B 128(7) . . . . ?
C19B C7B C8B C9B -118(7) . . . . ?
C13B C8B C9B C10B -10(12) . . . . ?
C7B C8B C9B C10B 162(7) . . . . ?
C8B C9B C10B C11B 26(14) . . . . ?
C9B C10B C11B C12B -20(18) . . . . ?
C10B C11B C12B C13B -2(18) . . . . ?
C11B C12B C13B C8B 18(13) . . . . ?
C11B C12B C13B P1B -172(9) . . . . ?
C9B C8B C13B C12B -11(11) . . . . ?
C7B C8B C13B C12B 176(6) . . . . ?
C9B C8B C13B P1B 177(6) . . . . ?
C7B C8B C13B P1B 5(7) . . . . ?
O1B P1B C13B C12B 6(7) . . . . ?
C14B P1B C13B C12B 135(7) . . . . ?
C1B P1B C13B C12B -123(7) . . . . ?
O1B P1B C13B C8B 177(4) . . . . ?
C14B P1B C13B C8B -54(4) . . . . ?
C1B P1B C13B C8B 48(4) . . . . ?
O1B P1B C14B C15B 2(8) . . . . ?
C13B P1B C14B C15B -128(7) . . . . ?
C1B P1B C14B C15B 130(7) . . . . ?
O1B P1B C14B C19B 178(4) . . . . ?
C13B P1B C14B C19B 48(4) . . . . ?
C1B P1B C14B C19B -54(4) . . . . ?
C19B C14B C15B C16B 11(10) . . . . ?
P1B C14B C15B C16B -174(5) . . . . ?
C14B C15B C16B C17B -8(10) . . . . ?
C15B C16B C17B C18B 14(10) . . . . ?
C16B C17B C18B C19B -22(10) . . . . ?
C17B C18B C19B C14B 23(9) . . . . ?
C17B C18B C19B C7B -175(5) . . . . ?
C15B C14B C19B C18B -18(9) . . . . ?
P1B C14B C19B C18B 166(5) . . . . ?
C15B C14B C19B C7B 179(5) . . . . ?
P1B C14B C19B C7B 3(7) . . . . ?
C8B C7B C19B C18B 139(6) . . . . ?
C6B C7B C19B C18B -106(6) . . . . ?
C8B C7B C19B C14B -60(5) . . . . ?
C6B C7B C19B C14B 56(5) . . . . ?

_refine_diff_density_max         0.267
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.061




# start Validation Reply Form
_vrf_PLAT088_nt1382_SMC166_v2_100K 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.79 Note  
RESPONSE: Whole molecule disorder
;
_vrf_PLAT911_nt1382_SMC166_v2_100K 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         35 Report
RESPONSE: These reflections are missing because of the instrument geometry 
limitations.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1176_SMC022_100K
_database_code_depnum_ccdc_archive 'CCDC 2313770'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        N-phenyl-5λ⁵-9-phosphatriptycene-imine
_chemical_name_common            N-phenyl-5λ⁵-9-phosphatriptycene-imine
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H18 N P'
_chemical_formula_sum            'C25 H18 N P'
_chemical_formula_weight         363.37

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'
N N 0.0311 0.0180 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.9413(2)
_cell_length_b                   13.6176(3)
_cell_length_c                   15.5673(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1895.46(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9853
_cell_measurement_theta_min      4.3135
_cell_measurement_theta_max      74.4618

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.023
_exptl_absorpt_coefficient_mu    1.332
_shelx_estimated_absorpt_T_min   0.638
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7050
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            46523
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.313
_diffrn_reflns_theta_max         74.543
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3881
_reflns_number_gt                3865
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    1.000

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0362P)²+1.2368P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(3)
_chemical_absolute_configuration .
_refine_ls_number_reflns         3881
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.1011
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_restrained_S_all      1.186
_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 0.55371(7) 0.50299(5) 0.56057(4) 0.01554(17) Uani 1 1 d . . . . .
N1 N 0.4410(3) 0.51796(18) 0.63592(15) 0.0229(5) Uani 1 1 d . . . . .
C1 C 0.7506(3) 0.49039(19) 0.58223(16) 0.0156(5) Uani 1 1 d . . . . .
C4 C 1.0583(3) 0.4792(2) 0.5978(2) 0.0245(6) Uani 1 1 d . . . . .
H4 H 1.163954 0.475209 0.603300 0.029 Uiso 1 1 calc R U . . .
C5 C 0.9933(3) 0.4814(2) 0.51609(19) 0.0225(6) Uani 1 1 d . . . . .
H5 H 1.054483 0.478498 0.466250 0.027 Uiso 1 1 calc R U . . .
C6 C 0.8395(3) 0.48783(19) 0.50824(16) 0.0172(5) Uani 1 1 d . . . . .
C7 C 0.7570(3) 0.4970(2) 0.42277(15) 0.0193(5) Uani 1 1 d . . . . .
H7 H 0.829018 0.495776 0.373619 0.023 Uiso 1 1 calc R U . . .
C8 C 0.6694(3) 0.59371(19) 0.42422(17) 0.0160(5) Uani 1 1 d . . . . .
C9 C 0.6909(3) 0.6688(2) 0.36471(19) 0.0196(6) Uani 1 1 d . . . . .
H9 H 0.763260 0.661933 0.320451 0.023 Uiso 1 1 calc R U . . .
C10 C 0.6049(3) 0.7543(2) 0.3707(2) 0.0235(6) Uani 1 1 d . . . . .
H10 H 0.620182 0.805864 0.330471 0.028 Uiso 1 1 calc R U . . .
C11 C 0.4984(3) 0.7649(2) 0.4341(2) 0.0232(6) Uani 1 1 d . . . . .
H11 H 0.439831 0.823048 0.436732 0.028 Uiso 1 1 calc R U . . .
C12 C 0.4762(3) 0.6903(2) 0.49450(19) 0.0196(6) Uani 1 1 d . . . . .
H12 H 0.403370 0.697245 0.538502 0.023 Uiso 1 1 calc R U . . .
C13 C 0.5622(3) 0.60621(19) 0.48904(17) 0.0165(5) Uani 1 1 d . . . . .
C14 C 0.6454(4) 0.4129(2) 0.41577(19) 0.0219(6) Uani 1 1 d . . . . .
C15 C 0.6461(5) 0.3445(2) 0.3499(2) 0.0316(8) Uani 1 1 d . . . . .
H15 H 0.720760 0.347144 0.306587 0.038 Uiso 1 1 calc R U . . .
C16 C 0.5363(5) 0.2718(2) 0.3477(2) 0.0419(10) Uani 1 1 d . . . . .
H16 H 0.536961 0.224612 0.302767 0.050 Uiso 1 1 calc R U . . .
C17 C 0.4267(5) 0.2674(2) 0.4102(2) 0.0425(10) Uani 1 1 d . . . . .
H17 H 0.352005 0.217884 0.407326 0.051 Uiso 1 1 calc R U . . .
C18 C 0.4248(4) 0.3354(2) 0.4778(2) 0.0306(7) Uani 1 1 d . . . . .
H18 H 0.349624 0.332541 0.520825 0.037 Uiso 1 1 calc R U . . .
C19 C 0.5350(3) 0.4070(2) 0.48048(19) 0.0213(6) Uani 1 1 d . . . . .
C20 C 0.4150(3) 0.4517(2) 0.7031(2) 0.0257(6) Uani 1 1 d . . . . .
C21 C 0.3211(3) 0.4826(3) 0.77021(19) 0.0327(8) Uani 1 1 d . . . . .
H21 H 0.282784 0.547671 0.770036 0.039 Uiso 1 1 calc R U . . .
C22 C 0.2835(4) 0.4196(4) 0.8366(2) 0.0421(10) Uani 1 1 d . . . . .
H22 H 0.218262 0.441711 0.880723 0.051 Uiso 1 1 calc R U . . .
C23 C 0.3394(4) 0.3250(4) 0.8399(2) 0.0446(10) Uani 1 1 d . . . . .
H23 H 0.312624 0.282119 0.885573 0.054 Uiso 1 1 calc R U . . .
C24 C 0.4344(4) 0.2940(3) 0.7759(2) 0.0397(9) Uani 1 1 d . . . . .
H24 H 0.475518 0.229713 0.778179 0.048 Uiso 1 1 calc R U . . .
C25 C 0.4713(4) 0.3560(3) 0.7074(2) 0.0295(7) Uani 1 1 d . . . . .
H25 H 0.535509 0.332721 0.663228 0.035 Uiso 1 1 calc R U . . .
C2 C 0.8151(3) 0.4881(2) 0.66340(17) 0.0180(5) Uani 1 1 d . . . . .
H2 H 0.753985 0.490029 0.713287 0.022 Uiso 1 1 calc R U . . .
C3 C 0.9696(3) 0.4828(2) 0.67100(19) 0.0220(6) Uani 1 1 d . . . . .
H3 H 1.014612 0.481750 0.726265 0.026 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
P1 N1 1.560(2) . ?
P1 C13 1.795(3) . ?
P1 C1 1.801(3) . ?
P1 C19 1.814(3) . ?
N1 C20 1.401(4) . ?
C1 C2 1.389(3) . ?
C1 C6 1.400(3) . ?
C4 C3 1.389(4) . ?
C4 C5 1.399(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.526(3) . ?
C7 C14 1.523(4) . ?
C7 C8 1.533(4) . ?
C7 H7 1.0000 . ?
C8 C9 1.393(4) . ?
C8 C13 1.402(4) . ?
C9 C10 1.398(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.399(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(4) . ?
C12 H12 0.9500 . ?
C14 C15 1.385(4) . ?
C14 C19 1.413(4) . ?
C15 C16 1.395(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.402(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.387(4) . ?
C18 H18 0.9500 . ?
C20 C25 1.399(5) . ?
C20 C21 1.405(4) . ?
C21 C22 1.386(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.377(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.399(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C2 C3 1.388(4) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?

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
N1 P1 C13 113.05(13) . . ?
N1 P1 C1 120.21(12) . . ?
C13 P1 C1 98.60(13) . . ?
N1 P1 C19 123.46(14) . . ?
C13 P1 C19 98.15(12) . . ?
C1 P1 C19 98.65(13) . . ?
C20 N1 P1 125.8(2) . . ?
C2 C1 C6 120.8(2) . . ?
C2 C1 P1 125.33(19) . . ?
C6 C1 P1 113.77(18) . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 119.6(3) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 119.5(2) . . ?
C5 C6 C7 124.2(2) . . ?
C1 C6 C7 116.2(2) . . ?
C14 C7 C6 108.5(2) . . ?
C14 C7 C8 108.2(2) . . ?
C6 C7 C8 107.7(2) . . ?
C14 C7 H7 110.8 . . ?
C6 C7 H7 110.8 . . ?
C8 C7 H7 110.8 . . ?
C9 C8 C13 118.9(3) . . ?
C9 C8 C7 123.4(2) . . ?
C13 C8 C7 117.7(2) . . ?
C8 C9 C10 119.4(3) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 120.9(3) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 120.2(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 118.8(3) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C8 121.7(3) . . ?
C12 C13 P1 126.0(2) . . ?
C8 C13 P1 112.4(2) . . ?
C15 C14 C19 119.5(3) . . ?
C15 C14 C7 123.7(3) . . ?
C19 C14 C7 116.7(2) . . ?
C14 C15 C16 119.5(4) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 120.8(3) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 120.5(3) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C19 C18 C17 118.6(3) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C18 C19 C14 121.0(3) . . ?
C18 C19 P1 126.4(3) . . ?
C14 C19 P1 112.6(2) . . ?
C25 C20 N1 125.2(3) . . ?
C25 C20 C21 117.3(3) . . ?
N1 C20 C21 117.5(3) . . ?
C22 C21 C20 121.0(4) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C23 C22 C21 121.2(4) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C24 C23 C22 118.8(3) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C23 C24 C25 120.8(4) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C24 C25 C20 120.9(3) . . ?
C24 C25 H25 119.5 . . ?
C20 C25 H25 119.5 . . ?
C3 C2 C1 119.4(2) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.0(3) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?

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
C13 P1 N1 C20 -177.5(2) . . . . ?
C1 P1 N1 C20 -61.6(3) . . . . ?
C19 P1 N1 C20 64.8(3) . . . . ?
N1 P1 C1 C2 3.2(3) . . . . ?
C13 P1 C1 C2 126.3(2) . . . . ?
C19 P1 C1 C2 -134.0(2) . . . . ?
N1 P1 C1 C6 -173.63(19) . . . . ?
C13 P1 C1 C6 -50.5(2) . . . . ?
C19 P1 C1 C6 49.1(2) . . . . ?
C3 C4 C5 C6 0.4(4) . . . . ?
C4 C5 C6 C1 -1.1(4) . . . . ?
C4 C5 C6 C7 176.1(2) . . . . ?
C2 C1 C6 C5 1.0(4) . . . . ?
P1 C1 C6 C5 178.0(2) . . . . ?
C2 C1 C6 C7 -176.4(3) . . . . ?
P1 C1 C6 C7 0.6(3) . . . . ?
C5 C6 C7 C14 123.4(3) . . . . ?
C1 C6 C7 C14 -59.3(3) . . . . ?
C5 C6 C7 C8 -119.7(3) . . . . ?
C1 C6 C7 C8 57.6(3) . . . . ?
C14 C7 C8 C9 -122.2(3) . . . . ?
C6 C7 C8 C9 120.7(3) . . . . ?
C14 C7 C8 C13 57.7(3) . . . . ?
C6 C7 C8 C13 -59.4(3) . . . . ?
C13 C8 C9 C10 -0.3(4) . . . . ?
C7 C8 C9 C10 179.6(3) . . . . ?
C8 C9 C10 C11 -0.6(4) . . . . ?
C9 C10 C11 C12 1.0(4) . . . . ?
C10 C11 C12 C13 -0.3(4) . . . . ?
C11 C12 C13 C8 -0.7(4) . . . . ?
C11 C12 C13 P1 179.0(2) . . . . ?
C9 C8 C13 C12 1.0(4) . . . . ?
C7 C8 C13 C12 -178.9(2) . . . . ?
C9 C8 C13 P1 -178.8(2) . . . . ?
C7 C8 C13 P1 1.4(3) . . . . ?
N1 P1 C13 C12 -2.7(3) . . . . ?
C1 P1 C13 C12 -130.9(2) . . . . ?
C19 P1 C13 C12 129.0(3) . . . . ?
N1 P1 C13 C8 176.97(19) . . . . ?
C1 P1 C13 C8 48.8(2) . . . . ?
C19 P1 C13 C8 -51.3(2) . . . . ?
C6 C7 C14 C15 -121.4(3) . . . . ?
C8 C7 C14 C15 122.0(3) . . . . ?
C6 C7 C14 C19 59.3(3) . . . . ?
C8 C7 C14 C19 -57.3(3) . . . . ?
C19 C14 C15 C16 1.0(5) . . . . ?
C7 C14 C15 C16 -178.2(3) . . . . ?
C14 C15 C16 C17 0.3(5) . . . . ?
C15 C16 C17 C18 -0.8(6) . . . . ?
C16 C17 C18 C19 0.1(5) . . . . ?
C17 C18 C19 C14 1.3(5) . . . . ?
C17 C18 C19 P1 179.3(3) . . . . ?
C15 C14 C19 C18 -1.8(4) . . . . ?
C7 C14 C19 C18 177.4(3) . . . . ?
C15 C14 C19 P1 179.9(2) . . . . ?
C7 C14 C19 P1 -0.8(3) . . . . ?
N1 P1 C19 C18 -2.2(3) . . . . ?
C13 P1 C19 C18 -126.8(3) . . . . ?
C1 P1 C19 C18 133.1(3) . . . . ?
N1 P1 C19 C14 175.98(19) . . . . ?
C13 P1 C19 C14 51.3(2) . . . . ?
C1 P1 C19 C14 -48.7(2) . . . . ?
P1 N1 C20 C25 -8.9(4) . . . . ?
P1 N1 C20 C21 173.2(2) . . . . ?
C25 C20 C21 C22 -1.5(4) . . . . ?
N1 C20 C21 C22 176.5(3) . . . . ?
C20 C21 C22 C23 1.2(5) . . . . ?
C21 C22 C23 C24 0.3(5) . . . . ?
C22 C23 C24 C25 -1.6(5) . . . . ?
C23 C24 C25 C20 1.3(5) . . . . ?
N1 C20 C25 C24 -177.6(3) . . . . ?
C21 C20 C25 C24 0.2(5) . . . . ?
C6 C1 C2 C3 -0.2(4) . . . . ?
P1 C1 C2 C3 -176.9(2) . . . . ?
C1 C2 C3 C4 -0.5(4) . . . . ?
C5 C4 C3 C2 0.4(4) . . . . ?

_refine_diff_density_max         0.459
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.070


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1332_SMC132_100K
_database_code_depnum_ccdc_archive 'CCDC 2313773'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        
;
(N-phenyl-9-phosphatriptycene-iminium)-2,3,5,6-tetrafluorophenyl]-
bis(2,3,4,5,6-pentafluorophenyl)-fluoroborate dichloromethane solvate
;
_chemical_name_common            
;
(N-phenyl-9-phosphatriptycene-iminium)-2,3,5,6-tetrafluorophenyl]-
bis(2,3,4,5,6-pentafluorophenyl)-fluoroborate dichloromethane solvate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C43 H18 B F15 N P, C H2 Cl2'
_chemical_formula_sum            'C44 H20 B Cl2 F15 N P'
_chemical_formula_weight         960.29

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'
Cl Cl 0.3639 0.7018 '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'
N N 0.0311 0.0180 '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                   11.2365(2)
_cell_length_b                   12.2624(2)
_cell_length_c                   14.8185(3)
_cell_angle_alpha                83.3900(10)
_cell_angle_beta                 78.0600(10)
_cell_angle_gamma                74.6010(10)
_cell_volume                     1921.98(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9798
_cell_measurement_theta_min      3.7465
_cell_measurement_theta_max      68.2509



_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_F_000             960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.065
_exptl_absorpt_coefficient_mu    2.915
_shelx_estimated_absorpt_T_min   0.496
_shelx_estimated_absorpt_T_max   0.833
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            71257
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.054
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7031
_reflns_number_gt                6547
_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0434P)²+1.5189P] 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         7031
_refine_ls_number_parameters     605
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0895
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.033
_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 0.28346(4) 0.34830(3) 0.32830(3) 0.01264(10) Uani 1 1 d . . . . .
F1 F 0.38370(10) 0.07727(8) 0.44979(6) 0.0225(2) Uani 1 1 d . . . . .
F2 F 0.36552(10) 0.02057(8) 0.62950(6) 0.0233(2) Uani 1 1 d . . . . .
F3 F 0.38786(10) 0.38974(8) 0.67991(6) 0.0218(2) Uani 1 1 d . . . . .
F4 F 0.40747(9) 0.44242(8) 0.50077(6) 0.0209(2) Uani 1 1 d . . . . .
F5 F 0.12772(10) 0.16108(9) 0.71416(7) 0.0277(2) Uani 1 1 d . . . . .
F6 F -0.02779(10) 0.03124(10) 0.79147(9) 0.0356(3) Uani 1 1 d . . . . .
F7 F 0.02130(10) -0.11576(10) 0.93948(8) 0.0341(3) Uani 1 1 d . . . . .
F8 F 0.22913(11) -0.12925(10) 1.00961(7) 0.0321(3) Uani 1 1 d . . . . .
F9 F 0.38849(9) -0.00277(9) 0.93331(6) 0.0229(2) Uani 1 1 d . . . . .
F10 F 0.16924(9) 0.34920(9) 0.80742(7) 0.0246(2) Uani 1 1 d . . . . .
F11 F 0.13543(11) 0.50877(9) 0.92598(8) 0.0329(3) Uani 1 1 d . . . . .
F12 F 0.31319(12) 0.49853(10) 1.02973(8) 0.0370(3) Uani 1 1 d . . . . .
F13 F 0.52213(11) 0.32322(10) 1.01444(7) 0.0349(3) Uani 1 1 d . . . . .
F14 F 0.55682(9) 0.16305(9) 0.89874(7) 0.0247(2) Uani 1 1 d . . . . .
F15 F 0.49866(9) 0.07266(8) 0.76664(6) 0.0215(2) Uani 1 1 d . . . . .
N1 N 0.40923(12) 0.29145(11) 0.37402(9) 0.0160(3) Uani 1 1 d . . . . .
C1 C 0.13084(15) 0.35907(13) 0.40052(11) 0.0149(3) Uani 1 1 d . . . . .
C2 C 0.09540(16) 0.32729(13) 0.49336(11) 0.0176(3) Uani 1 1 d . . . . .
H2 H 0.156925 0.295864 0.530817 0.021 Uiso 1 1 calc R U . . .
C3 C -0.03191(16) 0.34237(14) 0.53039(11) 0.0204(3) Uani 1 1 d . . . . .
H3 H -0.057567 0.320656 0.593579 0.024 Uiso 1 1 calc R U . . .
C4 C -0.12128(16) 0.38880(14) 0.47573(12) 0.0209(3) Uani 1 1 d . . . . .
H4 H -0.207758 0.397689 0.501633 0.025 Uiso 1 1 calc R U . . .
C5 C -0.08608(15) 0.42261(14) 0.38335(12) 0.0186(3) Uani 1 1 d . . . . .
H5 H -0.148377 0.455541 0.346820 0.022 Uiso 1 1 calc R U . . .
C6 C 0.03996(15) 0.40820(13) 0.34468(11) 0.0155(3) Uani 1 1 d . . . . .
C7 C 0.08418(15) 0.44255(13) 0.24273(11) 0.0159(3) Uani 1 1 d . . . . .
H7 H 0.010467 0.477069 0.211892 0.019 Uiso 1 1 calc R U . . .
C8 C 0.16487(15) 0.33537(13) 0.19630(10) 0.0152(3) Uani 1 1 d . . . . .
C9 C 0.13634(15) 0.28998(14) 0.12434(11) 0.0174(3) Uani 1 1 d . . . . .
H9 H 0.064682 0.327749 0.098197 0.021 Uiso 1 1 calc R U . . .
C10 C 0.21362(16) 0.18857(15) 0.09071(11) 0.0195(3) Uani 1 1 d . . . . .
H10 H 0.194304 0.157945 0.041059 0.023 Uiso 1 1 calc R U . . .
C11 C 0.31846(16) 0.13115(14) 0.12825(11) 0.0192(3) Uani 1 1 d . . . . .
H11 H 0.369565 0.061777 0.104575 0.023 Uiso 1 1 calc R U . . .
C12 C 0.34848(15) 0.17552(13) 0.20067(11) 0.0166(3) Uani 1 1 d . . . . .
H12 H 0.419779 0.137209 0.227035 0.020 Uiso 1 1 calc R U . . .
C13 C 0.27153(15) 0.27710(13) 0.23327(10) 0.0146(3) Uani 1 1 d . . . . .
C14 C 0.16346(15) 0.52742(13) 0.23909(10) 0.0161(3) Uani 1 1 d . . . . .
C15 C 0.13676(16) 0.63697(14) 0.19872(11) 0.0202(3) Uani 1 1 d . . . . .
H15 H 0.066608 0.663271 0.168569 0.024 Uiso 1 1 calc R U . . .
C16 C 0.21351(17) 0.70798(14) 0.20274(12) 0.0232(4) Uani 1 1 d . . . . .
H16 H 0.196071 0.782424 0.174053 0.028 Uiso 1 1 calc R U . . .
C17 C 0.31530(17) 0.67183(14) 0.24803(12) 0.0217(4) Uani 1 1 d . . . . .
H17 H 0.365215 0.722234 0.251501 0.026 Uiso 1 1 calc R U . . .
C18 C 0.34417(16) 0.56230(14) 0.28819(11) 0.0183(3) Uani 1 1 d . . . . .
H18 H 0.413831 0.536502 0.318899 0.022 Uiso 1 1 calc R U . . .
C19 C 0.26827(15) 0.49142(13) 0.28220(10) 0.0154(3) Uani 1 1 d . . . . .
C20 C 0.53577(15) 0.28305(13) 0.32178(11) 0.0157(3) Uani 1 1 d . . . . .
C21 C 0.55638(16) 0.32117(14) 0.22906(11) 0.0182(3) Uani 1 1 d . . . . .
H21 H 0.487528 0.351933 0.198153 0.022 Uiso 1 1 calc R U . . .
C22 C 0.67886(16) 0.31380(15) 0.18202(12) 0.0213(3) Uani 1 1 d . . . . .
H22 H 0.693380 0.339621 0.118721 0.026 Uiso 1 1 calc R U . . .
C23 C 0.77977(16) 0.26917(15) 0.22669(13) 0.0240(4) Uani 1 1 d . . . . .
H23 H 0.863006 0.266025 0.194716 0.029 Uiso 1 1 calc R U . . .
C24 C 0.75813(17) 0.22917(16) 0.31839(13) 0.0253(4) Uani 1 1 d . . . . .
H24 H 0.827152 0.196883 0.348844 0.030 Uiso 1 1 calc R U . . .
C25 C 0.63668(16) 0.23580(14) 0.36619(12) 0.0208(3) Uani 1 1 d . . . . .
H25 H 0.622651 0.208125 0.429050 0.025 Uiso 1 1 calc R U . . .
C26 C 0.39502(15) 0.26154(14) 0.47138(11) 0.0157(3) Uani 1 1 d . . . . .
C27 C 0.38522(15) 0.15412(14) 0.50700(11) 0.0169(3) Uani 1 1 d . . . . .
C28 C 0.37498(15) 0.12683(13) 0.60088(11) 0.0175(3) Uani 1 1 d . . . . .
C29 C 0.37355(15) 0.20168(14) 0.66527(11) 0.0168(3) Uani 1 1 d . . . . .
C30 C 0.38457(15) 0.30790(14) 0.62661(11) 0.0164(3) Uani 1 1 d . . . . .
C31 C 0.39545(15) 0.33818(13) 0.53300(11) 0.0157(3) Uani 1 1 d . . . . .
C32 C 0.26936(15) 0.08310(14) 0.81768(11) 0.0174(3) Uani 1 1 d . . . . .
C33 C 0.15871(16) 0.08954(15) 0.78709(11) 0.0208(3) Uani 1 1 d . . . . .
C34 C 0.07579(16) 0.02412(16) 0.82615(13) 0.0241(4) Uani 1 1 d . . . . .
C35 C 0.10009(17) -0.05044(15) 0.90065(12) 0.0235(4) Uani 1 1 d . . . . .
C36 C 0.20616(17) -0.05815(15) 0.93575(11) 0.0213(4) Uani 1 1 d . . . . .
C37 C 0.28722(15) 0.00780(14) 0.89419(11) 0.0182(3) Uani 1 1 d . . . . .
C38 C 0.36518(16) 0.24908(14) 0.84566(11) 0.0175(3) Uani 1 1 d . . . . .
C39 C 0.26013(16) 0.33949(15) 0.85794(11) 0.0199(3) Uani 1 1 d . . . . .
C40 C 0.24046(17) 0.42319(15) 0.91781(12) 0.0234(4) Uani 1 1 d . . . . .
C41 C 0.33015(19) 0.41840(16) 0.97027(12) 0.0257(4) Uani 1 1 d . . . . .
C42 C 0.43573(18) 0.32978(16) 0.96221(11) 0.0242(4) Uani 1 1 d . . . . .
C43 C 0.45106(16) 0.24704(14) 0.90133(11) 0.0193(3) Uani 1 1 d . . . . .
B1 B 0.37877(17) 0.15158(15) 0.77340(12) 0.0165(4) Uani 1 1 d . . . . .
Cl1A Cl 0.76470(8) 0.14306(6) 0.56757(6) 0.04249(19) Uani 0.9283(16) 1 d . . P
A 1
Cl2A Cl 0.89828(5) -0.08806(5) 0.61935(5) 0.04181(18) Uani 0.9283(16) 1 d . . P
A 1
C44A C 0.7818(2) 0.03490(18) 0.65516(14) 0.0292(5) Uani 0.9283(16) 1 d . . P A
1
H44A H 0.700517 0.014745 0.676975 0.035 Uiso 0.9283(16) 1 calc R U P A 1
H44B H 0.803716 0.063265 0.707917 0.035 Uiso 0.9283(16) 1 calc R U P A 1
Cl1B Cl 0.8792(5) -0.0403(4) 0.4504(4) 0.0195(16) Uani 0.0717(16) 1 d . U P A 2
Cl2B Cl 0.7786(14) 0.1147(11) 0.6003(8) 0.086(6) Uani 0.0717(16) 1 d . U P A 2
C44B C 0.899(2) 0.0046(18) 0.5524(16) 0.019(5) Uani 0.0717(16) 1 d . U P A 2
H44C H 0.907185 -0.060832 0.598557 0.022 Uiso 0.0717(16) 1 calc R U P A 2
H44D H 0.978142 0.028701 0.540272 0.022 Uiso 0.0717(16) 1 calc R 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
P1 N1 1.6452(13) . ?
P1 C13 1.7851(16) . ?
P1 C19 1.7857(16) . ?
P1 C1 1.8046(16) . ?
F1 C27 1.3436(19) . ?
F2 C28 1.3478(19) . ?
F3 C30 1.3589(18) . ?
F4 C31 1.3434(18) . ?
F5 C33 1.354(2) . ?
F6 C34 1.345(2) . ?
F7 C35 1.348(2) . ?
F8 C36 1.343(2) . ?
F9 C37 1.3510(19) . ?
F10 C39 1.3598(19) . ?
F11 C40 1.350(2) . ?
F12 C41 1.345(2) . ?
F13 C42 1.343(2) . ?
F14 C43 1.347(2) . ?
F15 B1 1.427(2) . ?
N1 C26 1.4336(19) . ?
N1 C20 1.455(2) . ?
C1 C2 1.391(2) . ?
C1 C6 1.414(2) . ?
C2 C3 1.393(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.536(2) . ?
C7 C14 1.529(2) . ?
C7 C8 1.530(2) . ?
C7 H7 1.0000 . ?
C8 C9 1.387(2) . ?
C8 C13 1.405(2) . ?
C9 C10 1.392(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.390(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(2) . ?
C12 H12 0.9500 . ?
C14 C15 1.388(2) . ?
C14 C19 1.400(2) . ?
C15 C16 1.392(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.391(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(2) . ?
C18 H18 0.9500 . ?
C20 C25 1.388(2) . ?
C20 C21 1.392(2) . ?
C21 C22 1.393(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.385(2) . ?
C26 C31 1.385(2) . ?
C27 C28 1.381(2) . ?
C28 C29 1.393(2) . ?
C29 C30 1.387(2) . ?
C29 B1 1.656(2) . ?
C30 C31 1.383(2) . ?
C32 C33 1.389(2) . ?
C32 C37 1.390(2) . ?
C32 B1 1.654(2) . ?
C33 C34 1.383(3) . ?
C34 C35 1.374(3) . ?
C35 C36 1.373(3) . ?
C36 C37 1.381(2) . ?
C38 C39 1.385(2) . ?
C38 C43 1.387(2) . ?
C38 B1 1.652(2) . ?
C39 C40 1.377(3) . ?
C40 C41 1.380(3) . ?
C41 C42 1.374(3) . ?
C42 C43 1.388(3) . ?
Cl1A C44A 1.747(2) . ?
Cl2A C44A 1.765(2) . ?
C44A H44A 0.9900 . ?
C44A H44B 0.9900 . ?
Cl1B C44B 1.74(2) . ?
Cl2B C44B 1.73(3) . ?
C44B H44C 0.9900 . ?
C44B H44D 0.9900 . ?

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
N1 P1 C13 114.62(7) . . ?
N1 P1 C19 115.60(7) . . ?
C13 P1 C19 103.01(7) . . ?
N1 P1 C1 118.72(7) . . ?
C13 P1 C1 101.80(7) . . ?
C19 P1 C1 100.76(7) . . ?
C26 N1 C20 117.86(13) . . ?
C26 N1 P1 119.31(11) . . ?
C20 N1 P1 122.38(11) . . ?
C2 C1 C6 121.06(15) . . ?
C2 C1 P1 131.51(13) . . ?
C6 C1 P1 107.43(11) . . ?
C1 C2 C3 118.79(15) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 120.43(15) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.83(16) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 119.92(16) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C1 118.95(14) . . ?
C5 C6 C7 122.11(14) . . ?
C1 C6 C7 118.93(14) . . ?
C14 C7 C8 109.86(13) . . ?
C14 C7 C6 108.15(13) . . ?
C8 C7 C6 107.47(12) . . ?
C14 C7 H7 110.4 . . ?
C8 C7 H7 110.4 . . ?
C6 C7 H7 110.4 . . ?
C9 C8 C13 118.69(15) . . ?
C9 C8 C7 124.57(14) . . ?
C13 C8 C7 116.66(14) . . ?
C8 C9 C10 119.43(15) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 121.42(15) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C10 C11 C12 119.92(15) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 118.29(15) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
C12 C13 C8 122.25(15) . . ?
C12 C13 P1 127.49(12) . . ?
C8 C13 P1 110.16(12) . . ?
C15 C14 C19 118.57(15) . . ?
C15 C14 C7 124.77(15) . . ?
C19 C14 C7 116.64(14) . . ?
C14 C15 C16 119.53(16) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 121.14(15) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C18 C17 C16 120.20(16) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 118.14(16) . . ?
C17 C18 H18 120.9 . . ?
C19 C18 H18 120.9 . . ?
C18 C19 C14 122.40(15) . . ?
C18 C19 P1 127.25(13) . . ?
C14 C19 P1 110.33(12) . . ?
C25 C20 C21 120.17(15) . . ?
C25 C20 N1 118.66(14) . . ?
C21 C20 N1 121.17(14) . . ?
C20 C21 C22 119.40(15) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C23 C22 C21 120.63(16) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C22 119.40(16) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 120.66(16) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C24 C25 C20 119.71(16) . . ?
C24 C25 H25 120.1 . . ?
C20 C25 H25 120.1 . . ?
C27 C26 C31 117.54(14) . . ?
C27 C26 N1 121.49(14) . . ?
C31 C26 N1 120.92(14) . . ?
F1 C27 C28 120.24(15) . . ?
F1 C27 C26 119.56(14) . . ?
C28 C27 C26 120.20(15) . . ?
F2 C28 C27 116.20(14) . . ?
F2 C28 C29 119.71(14) . . ?
C27 C28 C29 124.09(15) . . ?
C30 C29 C28 113.82(14) . . ?
C30 C29 B1 127.42(14) . . ?
C28 C29 B1 118.18(14) . . ?
F3 C30 C31 115.17(14) . . ?
F3 C30 C29 121.08(14) . . ?
C31 C30 C29 123.73(15) . . ?
F4 C31 C30 120.15(14) . . ?
F4 C31 C26 119.24(14) . . ?
C30 C31 C26 120.61(15) . . ?
C33 C32 C37 113.79(15) . . ?
C33 C32 B1 127.93(15) . . ?
C37 C32 B1 118.27(14) . . ?
F5 C33 C34 116.05(15) . . ?
F5 C33 C32 120.33(16) . . ?
C34 C33 C32 123.60(16) . . ?
F6 C34 C35 119.33(17) . . ?
F6 C34 C33 120.92(16) . . ?
C35 C34 C33 119.74(16) . . ?
F7 C35 C36 119.78(16) . . ?
F7 C35 C34 120.88(16) . . ?
C36 C35 C34 119.34(16) . . ?
F8 C36 C35 119.59(16) . . ?
F8 C36 C37 121.28(16) . . ?
C35 C36 C37 119.13(16) . . ?
F9 C37 C36 115.90(14) . . ?
F9 C37 C32 119.74(15) . . ?
C36 C37 C32 124.35(16) . . ?
C39 C38 C43 114.12(16) . . ?
C39 C38 B1 120.91(14) . . ?
C43 C38 B1 124.91(15) . . ?
F10 C39 C40 116.35(15) . . ?
F10 C39 C38 119.05(15) . . ?
C40 C39 C38 124.59(16) . . ?
F11 C40 C39 121.15(16) . . ?
F11 C40 C41 119.91(16) . . ?
C39 C40 C41 118.94(16) . . ?
F12 C41 C42 120.47(17) . . ?
F12 C41 C40 120.29(18) . . ?
C42 C41 C40 119.24(16) . . ?
F13 C42 C41 119.59(16) . . ?
F13 C42 C43 120.66(17) . . ?
C41 C42 C43 119.74(16) . . ?
F14 C43 C38 121.16(15) . . ?
F14 C43 C42 115.50(15) . . ?
C38 C43 C42 123.34(16) . . ?
F15 B1 C38 110.74(13) . . ?
F15 B1 C32 108.50(13) . . ?
C38 B1 C32 106.51(13) . . ?
F15 B1 C29 103.52(13) . . ?
C38 B1 C29 114.24(13) . . ?
C32 B1 C29 113.27(13) . . ?
Cl1A C44A Cl2A 113.13(12) . . ?
Cl1A C44A H44A 109.0 . . ?
Cl2A C44A H44A 109.0 . . ?
Cl1A C44A H44B 109.0 . . ?
Cl2A C44A H44B 109.0 . . ?
H44A C44A H44B 107.8 . . ?
Cl2B C44B Cl1B 115.4(14) . . ?
Cl2B C44B H44C 108.4 . . ?
Cl1B C44B H44C 108.4 . . ?
Cl2B C44B H44D 108.4 . . ?
Cl1B C44B H44D 108.4 . . ?
H44C C44B H44D 107.5 . . ?

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
C13 P1 N1 C26 -126.16(12) . . . . ?
C19 P1 N1 C26 114.23(13) . . . . ?
C1 P1 N1 C26 -5.66(15) . . . . ?
C13 P1 N1 C20 61.72(14) . . . . ?
C19 P1 N1 C20 -57.89(14) . . . . ?
C1 P1 N1 C20 -177.78(11) . . . . ?
N1 P1 C1 C2 0.26(19) . . . . ?
C13 P1 C1 C2 127.11(16) . . . . ?
C19 P1 C1 C2 -127.01(16) . . . . ?
N1 P1 C1 C6 -178.82(10) . . . . ?
C13 P1 C1 C6 -51.98(12) . . . . ?
C19 P1 C1 C6 53.91(12) . . . . ?
C6 C1 C2 C3 1.4(2) . . . . ?
P1 C1 C2 C3 -177.57(13) . . . . ?
C1 C2 C3 C4 -0.4(2) . . . . ?
C2 C3 C4 C5 -0.8(3) . . . . ?
C3 C4 C5 C6 1.1(2) . . . . ?
C4 C5 C6 C1 0.0(2) . . . . ?
C4 C5 C6 C7 179.18(15) . . . . ?
C2 C1 C6 C5 -1.2(2) . . . . ?
P1 C1 C6 C5 178.00(12) . . . . ?
C2 C1 C6 C7 179.56(14) . . . . ?
P1 C1 C6 C7 -1.24(17) . . . . ?
C5 C6 C7 C14 122.58(16) . . . . ?
C1 C6 C7 C14 -58.20(18) . . . . ?
C5 C6 C7 C8 -118.88(16) . . . . ?
C1 C6 C7 C8 60.34(18) . . . . ?
C14 C7 C8 C9 -124.75(16) . . . . ?
C6 C7 C8 C9 117.81(16) . . . . ?
C14 C7 C8 C13 58.57(17) . . . . ?
C6 C7 C8 C13 -58.87(18) . . . . ?
C13 C8 C9 C10 -0.1(2) . . . . ?
C7 C8 C9 C10 -176.67(14) . . . . ?
C8 C9 C10 C11 0.5(2) . . . . ?
C9 C10 C11 C12 -0.5(2) . . . . ?
C10 C11 C12 C13 0.0(2) . . . . ?
C11 C12 C13 C8 0.5(2) . . . . ?
C11 C12 C13 P1 176.47(12) . . . . ?
C9 C8 C13 C12 -0.5(2) . . . . ?
C7 C8 C13 C12 176.40(14) . . . . ?
C9 C8 C13 P1 -177.05(12) . . . . ?
C7 C8 C13 P1 -0.17(17) . . . . ?
N1 P1 C13 C12 6.70(17) . . . . ?
C19 P1 C13 C12 133.11(14) . . . . ?
C1 P1 C13 C12 -122.77(15) . . . . ?
N1 P1 C13 C8 -176.96(10) . . . . ?
C19 P1 C13 C8 -50.54(12) . . . . ?
C1 P1 C13 C8 53.58(12) . . . . ?
C8 C7 C14 C15 122.09(16) . . . . ?
C6 C7 C14 C15 -120.89(16) . . . . ?
C8 C7 C14 C19 -59.72(17) . . . . ?
C6 C7 C14 C19 57.29(17) . . . . ?
C19 C14 C15 C16 -0.5(2) . . . . ?
C7 C14 C15 C16 177.61(15) . . . . ?
C14 C15 C16 C17 -1.2(2) . . . . ?
C15 C16 C17 C18 1.7(3) . . . . ?
C16 C17 C18 C19 -0.5(2) . . . . ?
C17 C18 C19 C14 -1.3(2) . . . . ?
C17 C18 C19 P1 -179.41(12) . . . . ?
C15 C14 C19 C18 1.8(2) . . . . ?
C7 C14 C19 C18 -176.48(14) . . . . ?
C15 C14 C19 P1 -179.79(12) . . . . ?
C7 C14 C19 P1 1.91(17) . . . . ?
N1 P1 C19 C18 -6.27(17) . . . . ?
C13 P1 C19 C18 -132.05(14) . . . . ?
C1 P1 C19 C18 123.03(15) . . . . ?
N1 P1 C19 C14 175.44(10) . . . . ?
C13 P1 C19 C14 49.66(12) . . . . ?
C1 P1 C19 C14 -55.26(12) . . . . ?
C26 N1 C20 C25 6.6(2) . . . . ?
P1 N1 C20 C25 178.78(12) . . . . ?
C26 N1 C20 C21 -173.55(15) . . . . ?
P1 N1 C20 C21 -1.3(2) . . . . ?
C25 C20 C21 C22 -1.5(2) . . . . ?
N1 C20 C21 C22 178.65(14) . . . . ?
C20 C21 C22 C23 -0.1(3) . . . . ?
C21 C22 C23 C24 1.5(3) . . . . ?
C22 C23 C24 C25 -1.5(3) . . . . ?
C23 C24 C25 C20 -0.1(3) . . . . ?
C21 C20 C25 C24 1.5(3) . . . . ?
N1 C20 C25 C24 -178.58(15) . . . . ?
C20 N1 C26 C27 -95.59(18) . . . . ?
P1 N1 C26 C27 91.94(17) . . . . ?
C20 N1 C26 C31 81.92(19) . . . . ?
P1 N1 C26 C31 -90.56(17) . . . . ?
C31 C26 C27 F1 179.61(14) . . . . ?
N1 C26 C27 F1 -2.8(2) . . . . ?
C31 C26 C27 C28 0.7(2) . . . . ?
N1 C26 C27 C28 178.27(15) . . . . ?
F1 C27 C28 F2 0.9(2) . . . . ?
C26 C27 C28 F2 179.82(14) . . . . ?
F1 C27 C28 C29 -178.87(15) . . . . ?
C26 C27 C28 C29 0.1(3) . . . . ?
F2 C28 C29 C30 179.71(14) . . . . ?
C27 C28 C29 C30 -0.5(2) . . . . ?
F2 C28 C29 B1 7.8(2) . . . . ?
C27 C28 C29 B1 -172.44(15) . . . . ?
C28 C29 C30 F3 -178.37(14) . . . . ?
B1 C29 C30 F3 -7.4(2) . . . . ?
C28 C29 C30 C31 0.3(2) . . . . ?
B1 C29 C30 C31 171.30(15) . . . . ?
F3 C30 C31 F4 -0.4(2) . . . . ?
C29 C30 C31 F4 -179.09(14) . . . . ?
F3 C30 C31 C26 179.16(14) . . . . ?
C29 C30 C31 C26 0.4(3) . . . . ?
C27 C26 C31 F4 178.62(14) . . . . ?
N1 C26 C31 F4 1.0(2) . . . . ?
C27 C26 C31 C30 -0.9(2) . . . . ?
N1 C26 C31 C30 -178.51(14) . . . . ?
C37 C32 C33 F5 178.75(14) . . . . ?
B1 C32 C33 F5 -2.2(3) . . . . ?
C37 C32 C33 C34 -2.6(2) . . . . ?
B1 C32 C33 C34 176.52(16) . . . . ?
F5 C33 C34 F6 1.1(2) . . . . ?
C32 C33 C34 F6 -177.64(15) . . . . ?
F5 C33 C34 C35 -179.80(15) . . . . ?
C32 C33 C34 C35 1.5(3) . . . . ?
F6 C34 C35 F7 -0.4(3) . . . . ?
C33 C34 C35 F7 -179.48(15) . . . . ?
F6 C34 C35 C36 179.66(15) . . . . ?
C33 C34 C35 C36 0.5(3) . . . . ?
F7 C35 C36 F8 -1.2(2) . . . . ?
C34 C35 C36 F8 178.73(16) . . . . ?
F7 C35 C36 C37 178.82(15) . . . . ?
C34 C35 C36 C37 -1.2(3) . . . . ?
F8 C36 C37 F9 -1.0(2) . . . . ?
C35 C36 C37 F9 178.94(15) . . . . ?
F8 C36 C37 C32 180.00(15) . . . . ?
C35 C36 C37 C32 -0.1(3) . . . . ?
C33 C32 C37 F9 -177.11(14) . . . . ?
B1 C32 C37 F9 3.7(2) . . . . ?
C33 C32 C37 C36 1.9(2) . . . . ?
B1 C32 C37 C36 -177.30(15) . . . . ?
C43 C38 C39 F10 -179.41(14) . . . . ?
B1 C38 C39 F10 -2.0(2) . . . . ?
C43 C38 C39 C40 1.5(2) . . . . ?
B1 C38 C39 C40 178.86(15) . . . . ?
F10 C39 C40 F11 0.9(2) . . . . ?
C38 C39 C40 F11 -179.98(15) . . . . ?
F10 C39 C40 C41 -179.38(15) . . . . ?
C38 C39 C40 C41 -0.2(3) . . . . ?
F11 C40 C41 F12 0.2(2) . . . . ?
C39 C40 C41 F12 -179.59(15) . . . . ?
F11 C40 C41 C42 179.02(15) . . . . ?
C39 C40 C41 C42 -0.7(3) . . . . ?
F12 C41 C42 F13 0.2(2) . . . . ?
C40 C41 C42 F13 -178.59(15) . . . . ?
F12 C41 C42 C43 179.22(15) . . . . ?
C40 C41 C42 C43 0.4(2) . . . . ?
C39 C38 C43 F14 178.63(14) . . . . ?
B1 C38 C43 F14 1.3(2) . . . . ?
C39 C38 C43 C42 -1.8(2) . . . . ?
B1 C38 C43 C42 -179.11(15) . . . . ?
F13 C42 C43 F14 -0.5(2) . . . . ?
C41 C42 C43 F14 -179.44(15) . . . . ?
F13 C42 C43 C38 179.96(15) . . . . ?
C41 C42 C43 C38 1.0(3) . . . . ?
C39 C38 B1 F15 175.17(14) . . . . ?
C43 C38 B1 F15 -7.7(2) . . . . ?
C39 C38 B1 C32 -67.05(18) . . . . ?
C43 C38 B1 C32 110.06(17) . . . . ?
C39 C38 B1 C29 58.8(2) . . . . ?
C43 C38 B1 C29 -124.12(16) . . . . ?
C33 C32 B1 F15 -133.61(16) . . . . ?
C37 C32 B1 F15 45.43(19) . . . . ?
C33 C32 B1 C38 107.15(18) . . . . ?
C37 C32 B1 C38 -73.82(17) . . . . ?
C33 C32 B1 C29 -19.3(2) . . . . ?
C37 C32 B1 C29 159.77(14) . . . . ?
C30 C29 B1 F15 -106.52(18) . . . . ?
C28 C29 B1 F15 64.14(18) . . . . ?
C30 C29 B1 C38 14.0(2) . . . . ?
C28 C29 B1 C38 -175.35(14) . . . . ?
C30 C29 B1 C32 136.18(17) . . . . ?
C28 C29 B1 C32 -53.16(19) . . . . ?

_refine_diff_density_max         0.650
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.053



# start Validation Reply Form
_vrf_PLAT042_nt1332_SMC132_100K  
;
PROBLEM: Calc. and Reported MoietyFormula Strings  Differ     Please Check 
RESPONSE: The reported formula is correct, the asymmetric unit contains 
disordered dichloromethane.
;
_vrf_PLAT221_nt1332_SMC132_100K  
;
PROBLEM: Solv./Anion  Resd 2 Cl   Ueq(max)/Ueq(min) Range        4.4 Ratio 
RESPONSE: Minor component of disordered dichloromethane.
;

_vrf_PLAT911_nt1332_SMC132_100K  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         17 Report
RESPONSE: These reflections are missing because of the instrument geometry 
limitations.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1400_SMC190_cryst2_full_100K
_database_code_depnum_ccdc_archive 'CCDC 2347270'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        
'N-(ortho diisopropylphenyl)-5λ⁵-9-phosphatriptycene-imine'
_chemical_name_common            
'N-(ortho diisopropylphenyl)-5λ⁵-9-phosphatriptycene-imine'
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H30 N P'
_chemical_formula_sum            'C31 H30 N P'
_chemical_formula_weight         447.53

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'
N N 0.0311 0.0180 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.0484(3)
_cell_length_b                   18.3060(6)
_cell_length_c                   14.4219(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.4144(18)
_cell_angle_gamma                90
_cell_volume                     2388.78(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9929
_cell_measurement_theta_min      3.9021
_cell_measurement_theta_max      66.7521

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.149
_shelx_estimated_absorpt_T_min   0.803
_shelx_estimated_absorpt_T_max   0.977
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.98
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            23060
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.902
_diffrn_reflns_theta_max         66.763
_diffrn_reflns_theta_full        66.763
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             4145
_reflns_number_gt                3529
_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0198P)²+7.5014P] 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         4145
_refine_ls_number_parameters     386
_refine_ls_number_restraints     201
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0776
_refine_ls_wR_factor_ref         0.1771
_refine_ls_wR_factor_gt          0.1705
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.133
_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 0.60196(11) 0.32340(6) 0.65652(6) 0.0268(2) Uani 1 1 d . . . . .
N1 N 0.4815(4) 0.2659(2) 0.6560(2) 0.0359(8) Uani 1 1 d D . . . .
C1 C 0.7967(4) 0.3007(2) 0.6694(2) 0.0241(8) Uani 1 1 d . . . . .
C2 C 0.8540(4) 0.2307(2) 0.6799(2) 0.0277(8) Uani 1 1 d . . . . .
H2 H 0.790406 0.189561 0.683940 0.033 Uiso 1 1 calc R U . . .
C3 C 1.0064(5) 0.2225(2) 0.6844(3) 0.0354(9) Uani 1 1 d . . . . .
H3 H 1.047954 0.175197 0.691963 0.042 Uiso 1 1 calc R U . . .
C4 C 1.0977(4) 0.2824(2) 0.6781(3) 0.0350(9) Uani 1 1 d . . . . .
H4 H 1.201763 0.275787 0.680281 0.042 Uiso 1 1 calc R U . . .
C5 C 1.0402(4) 0.3520(2) 0.6686(2) 0.0313(9) Uani 1 1 d . . . . .
H5 H 1.104348 0.393007 0.665370 0.038 Uiso 1 1 calc R U . . .
C6 C 0.8886(4) 0.3616(2) 0.6638(2) 0.0267(8) Uani 1 1 d . . . . .
C7 C 0.8152(4) 0.4361(2) 0.6514(2) 0.0300(9) Uani 1 1 d . . . . .
H7 H 0.890939 0.475801 0.649174 0.036 Uiso 1 1 calc R U . . .
C8 C 0.7059(5) 0.4491(2) 0.7308(2) 0.0340(9) Uani 1 1 d . . . . .
C9 C 0.7120(5) 0.5086(2) 0.7896(3) 0.0411(11) Uani 1 1 d . . . . .
H9 H 0.789691 0.543250 0.784385 0.049 Uiso 1 1 calc R U . . .
C10 C 0.6034(6) 0.5174(3) 0.8564(3) 0.0469(12) Uani 1 1 d . . . . .
H10 H 0.607295 0.558294 0.896910 0.056 Uiso 1 1 calc R U . . .
C11 C 0.4906(6) 0.4676(3) 0.8647(3) 0.0488(12) Uani 1 1 d . . . . .
H11 H 0.416391 0.474803 0.910010 0.059 Uiso 1 1 calc R U . . .
C12 C 0.4844(5) 0.4066(3) 0.8071(3) 0.0418(11) Uani 1 1 d . . . . .
H12 H 0.407368 0.371714 0.813199 0.050 Uiso 1 1 calc R U . . .
C13 C 0.5934(5) 0.3977(2) 0.7404(2) 0.0322(9) Uani 1 1 d . . . . .
C14 C 0.6145(4) 0.3805(2) 0.5547(2) 0.0301(9) Uani 1 1 d . . . . .
C15 C 0.5249(5) 0.3758(3) 0.4770(3) 0.0387(10) Uani 1 1 d . . . . .
H15 H 0.450315 0.339400 0.472978 0.046 Uiso 1 1 calc R U . . .
C16 C 0.5452(6) 0.4256(3) 0.4041(3) 0.0468(13) Uani 1 1 d . . . . .
H16 H 0.484621 0.422708 0.350176 0.056 Uiso 1 1 calc R U . . .
C17 C 0.6524(6) 0.4781(3) 0.4107(3) 0.0485(13) Uani 1 1 d . . . . .
H17 H 0.664832 0.511716 0.361144 0.058 Uiso 1 1 calc R U . . .
C18 C 0.7434(6) 0.4832(2) 0.4886(3) 0.0435(11) Uani 1 1 d . . . . .
H18 H 0.817938 0.519702 0.492205 0.052 Uiso 1 1 calc R U . . .
C19 C 0.7236(5) 0.4341(2) 0.5613(2) 0.0328(9) Uani 1 1 d . . . . .
C20A C 0.460(5) 0.1890(8) 0.6633(11) 0.035(4) Uani 0.467(12) 1 d D U P A 1
C21A C 0.455(6) 0.1574(15) 0.7530(12) 0.043(5) Uani 0.467(12) 1 d D U P A 1
C22A C 0.416(4) 0.0853(14) 0.7643(13) 0.047(4) Uani 0.467(12) 1 d D U P A 1
H22A H 0.395581 0.067559 0.824759 0.056 Uiso 0.467(12) 1 calc R U P A 1
C23A C 0.405(2) 0.0368(9) 0.6875(11) 0.045(4) Uani 0.467(12) 1 d D U P A 1
H23A H 0.388405 -0.013968 0.696349 0.054 Uiso 0.467(12) 1 calc R U P A 1
C24A C 0.4208(17) 0.0656(8) 0.5999(10) 0.047(4) Uani 0.467(12) 1 d D U P A 1
H24A H 0.403641 0.035362 0.547394 0.056 Uiso 0.467(12) 1 calc R U P A 1
C25A C 0.4607(15) 0.1379(7) 0.5867(8) 0.038(3) Uani 0.467(12) 1 d D U P A 1
C26A C 0.4778(18) 0.1671(8) 0.4887(8) 0.055(3) Uani 0.467(12) 1 d D U P A 1
H26A H 0.530313 0.215079 0.492623 0.066 Uiso 0.467(12) 1 calc R U P A 1
C27A C 0.5675(17) 0.1172(7) 0.4285(8) 0.079(5) Uani 0.467(12) 1 d D . P A 1
H27A H 0.507324 0.075042 0.410184 0.118 Uiso 0.467(12) 1 calc R U P A 1
H27B H 0.654697 0.100390 0.463095 0.118 Uiso 0.467(12) 1 calc R U P A 1
H27C H 0.599008 0.143678 0.372990 0.118 Uiso 0.467(12) 1 calc R U P A 1
C28A C 0.3267(17) 0.1804(10) 0.4456(10) 0.077(4) Uani 0.467(12) 1 d D U P A 1
H28A H 0.338386 0.202896 0.384437 0.115 Uiso 0.467(12) 1 calc R U P A 1
H28B H 0.269780 0.213150 0.485572 0.115 Uiso 0.467(12) 1 calc R U P A 1
H28C H 0.274334 0.133828 0.439033 0.115 Uiso 0.467(12) 1 calc R U P A 1
C20B C 0.465(5) 0.1921(6) 0.6761(10) 0.042(4) Uani 0.533(12) 1 d D U P A 2
C21B C 0.469(5) 0.1626(12) 0.7660(11) 0.041(3) Uani 0.533(12) 1 d D U P A 2
C22B C 0.434(4) 0.0900(13) 0.7777(12) 0.057(5) Uani 0.533(12) 1 d D U P A 2
H22B H 0.456238 0.065920 0.834479 0.069 Uiso 0.533(12) 1 calc R U P A 2
C23B C 0.365(2) 0.0519(9) 0.7044(11) 0.055(4) Uani 0.533(12) 1 d D U P A 2
H23B H 0.319120 0.006206 0.716278 0.066 Uiso 0.533(12) 1 calc R U P A 2
C24B C 0.3634(15) 0.0797(7) 0.6160(10) 0.049(3) Uani 0.533(12) 1 d D U P A 2
H24B H 0.332828 0.049673 0.565612 0.059 Uiso 0.533(12) 1 calc R U P A 2
C25B C 0.4057(13) 0.1509(7) 0.5998(7) 0.037(3) Uani 0.533(12) 1 d D U P A 2
C26B C 0.4061(17) 0.1817(8) 0.5025(7) 0.061(3) Uani 0.533(12) 1 d D U P A 2
H26B H 0.378475 0.234412 0.507265 0.073 Uiso 0.533(12) 1 calc R U P A 2
C27B C 0.5593(14) 0.1784(8) 0.4585(7) 0.076(4) Uani 0.533(12) 1 d D U P A 2
H27D H 0.552477 0.194174 0.393714 0.115 Uiso 0.533(12) 1 calc R U P A 2
H27E H 0.596559 0.128154 0.461188 0.115 Uiso 0.533(12) 1 calc R U P A 2
H27F H 0.626915 0.210702 0.492501 0.115 Uiso 0.533(12) 1 calc R U P A 2
C28B C 0.2921(19) 0.1453(8) 0.4393(10) 0.093(5) Uani 0.533(12) 1 d D U P A 2
H28D H 0.281043 0.173833 0.382220 0.140 Uiso 0.533(12) 1 calc R U P A 2
H28E H 0.196858 0.142820 0.471136 0.140 Uiso 0.533(12) 1 calc R U P A 2
H28F H 0.325008 0.095743 0.423984 0.140 Uiso 0.533(12) 1 calc R U P A 2
C29 C 0.5037(6) 0.2053(3) 0.8443(3) 0.0550(14) Uani 1 1 d . . . . .
H29 H 0.556355 0.250113 0.822763 0.066 Uiso 1 1 calc R U . A 1
C30 C 0.6060(8) 0.1635(4) 0.9103(4) 0.082(2) Uani 1 1 d . . . . .
H30A H 0.554512 0.120437 0.934107 0.122 Uiso 1 1 calc R U . . .
H30B H 0.634589 0.195289 0.962077 0.122 Uiso 1 1 calc R U . . .
H30C H 0.694673 0.148100 0.876884 0.122 Uiso 1 1 calc R U . . .
C31 C 0.3660(7) 0.2288(4) 0.8968(4) 0.0762(19) Uani 1 1 d . . . . .
H31A H 0.302967 0.258496 0.856075 0.114 Uiso 1 1 calc R U . . .
H31B H 0.395070 0.257573 0.951218 0.114 Uiso 1 1 calc R U . . .
H31C H 0.311285 0.185411 0.916776 0.114 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
P1 N1 1.515(4) . ?
P1 C14 1.806(4) . ?
P1 C1 1.819(4) . ?
P1 C13 1.822(4) . ?
N1 C20B 1.391(11) . ?
N1 C20A 1.426(12) . ?
C1 C2 1.389(5) . ?
C1 C6 1.395(5) . ?
C2 C3 1.389(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.376(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.526(5) . ?
C7 C19 1.536(5) . ?
C7 C8 1.537(5) . ?
C7 H7 1.0000 . ?
C8 C9 1.382(6) . ?
C8 C13 1.393(6) . ?
C9 C10 1.391(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.374(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(5) . ?
C12 H12 0.9500 . ?
C14 C15 1.381(5) . ?
C14 C19 1.396(6) . ?
C15 C16 1.404(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.369(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.394(5) . ?
C18 H18 0.9500 . ?
C20A C21A 1.418(12) . ?
C20A C25A 1.448(16) . ?
C21A C22A 1.374(13) . ?
C21A C29 1.64(2) . ?
C22A C23A 1.423(17) . ?
C22A H22A 0.9500 . ?
C23A C24A 1.378(12) . ?
C23A H23A 0.9500 . ?
C24A C25A 1.384(12) . ?
C24A H24A 0.9500 . ?
C25A C26A 1.521(12) . ?
C26A C27A 1.502(16) . ?
C26A C28A 1.518(15) . ?
C26A H26A 1.0000 . ?
C27A H27A 0.9800 . ?
C27A H27B 0.9800 . ?
C27A H27C 0.9800 . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C28A H28C 0.9800 . ?
C20B C21B 1.405(11) . ?
C20B C25B 1.434(15) . ?
C21B C22B 1.376(12) . ?
C21B C29 1.407(18) . ?
C22B C23B 1.409(16) . ?
C22B H22B 0.9500 . ?
C23B C24B 1.373(12) . ?
C23B H23B 0.9500 . ?
C24B C25B 1.379(11) . ?
C24B H24B 0.9500 . ?
C25B C26B 1.512(11) . ?
C26B C28B 1.525(13) . ?
C26B C27B 1.529(16) . ?
C26B H26B 1.0000 . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 0.9800 . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 0.9800 . ?
C29 C31 1.524(7) . ?
C29 C30 1.527(7) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 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
N1 P1 C14 116.57(19) . . ?
N1 P1 C1 122.57(19) . . ?
C14 P1 C1 98.55(17) . . ?
N1 P1 C13 119.17(19) . . ?
C14 P1 C13 96.35(17) . . ?
C1 P1 C13 98.58(18) . . ?
C20B N1 P1 138.9(18) . . ?
C20A N1 P1 141.8(18) . . ?
C2 C1 C6 121.5(3) . . ?
C2 C1 P1 125.6(3) . . ?
C6 C1 P1 112.9(3) . . ?
C3 C2 C1 118.3(4) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 121.0(4) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 119.6(4) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 119.1(4) . . ?
C5 C6 C7 123.3(4) . . ?
C1 C6 C7 117.6(3) . . ?
C6 C7 C19 108.1(3) . . ?
C6 C7 C8 109.4(3) . . ?
C19 C7 C8 106.7(3) . . ?
C6 C7 H7 110.8 . . ?
C19 C7 H7 110.8 . . ?
C8 C7 H7 110.8 . . ?
C9 C8 C13 119.8(4) . . ?
C9 C8 C7 123.8(4) . . ?
C13 C8 C7 116.3(3) . . ?
C8 C9 C10 119.4(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 120.8(4) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 120.5(4) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C13 C12 C11 118.7(5) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C12 C13 C8 120.8(4) . . ?
C12 C13 P1 125.4(4) . . ?
C8 C13 P1 113.8(3) . . ?
C15 C14 C19 120.7(4) . . ?
C15 C14 P1 125.7(3) . . ?
C19 C14 P1 113.6(3) . . ?
C14 C15 C16 119.2(5) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 120.0(4) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 121.2(4) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C19 119.1(5) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C18 C19 C14 119.8(4) . . ?
C18 C19 C7 123.4(4) . . ?
C14 C19 C7 116.8(3) . . ?
C21A C20A N1 118.4(14) . . ?
C21A C20A C25A 115.6(13) . . ?
N1 C20A C25A 125.5(12) . . ?
C22A C21A C20A 120.6(14) . . ?
C22A C21A C29 119.1(13) . . ?
C20A C21A C29 120.2(15) . . ?
C21A C22A C23A 121.6(15) . . ?
C21A C22A H22A 119.2 . . ?
C23A C22A H22A 119.2 . . ?
C24A C23A C22A 117.9(12) . . ?
C24A C23A H23A 121.1 . . ?
C22A C23A H23A 121.1 . . ?
C23A C24A C25A 121.4(12) . . ?
C23A C24A H24A 119.3 . . ?
C25A C24A H24A 119.3 . . ?
C24A C25A C20A 120.7(10) . . ?
C24A C25A C26A 119.5(11) . . ?
C20A C25A C26A 118.9(11) . . ?
C27A C26A C28A 110.5(12) . . ?
C27A C26A C25A 112.5(10) . . ?
C28A C26A C25A 109.9(12) . . ?
C27A C26A H26A 108.0 . . ?
C28A C26A H26A 108.0 . . ?
C25A C26A H26A 108.0 . . ?
C26A C27A H27A 109.5 . . ?
C26A C27A H27B 109.5 . . ?
H27A C27A H27B 109.5 . . ?
C26A C27A H27C 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C26A C28A H28A 109.5 . . ?
C26A C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C26A C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
N1 C20B C21B 124.3(12) . . ?
N1 C20B C25B 113.1(12) . . ?
C21B C20B C25B 120.9(12) . . ?
C22B C21B C20B 118.6(13) . . ?
C22B C21B C29 119.2(13) . . ?
C20B C21B C29 122.1(15) . . ?
C21B C22B C23B 119.1(15) . . ?
C21B C22B H22B 120.4 . . ?
C23B C22B H22B 120.4 . . ?
C24B C23B C22B 121.0(12) . . ?
C24B C23B H23B 119.5 . . ?
C22B C23B H23B 119.5 . . ?
C23B C24B C25B 120.4(11) . . ?
C23B C24B H24B 119.8 . . ?
C25B C24B H24B 119.8 . . ?
C24B C25B C20B 118.0(9) . . ?
C24B C25B C26B 120.8(10) . . ?
C20B C25B C26B 120.8(10) . . ?
C25B C26B C28B 112.7(10) . . ?
C25B C26B C27B 112.3(10) . . ?
C28B C26B C27B 110.2(12) . . ?
C25B C26B H26B 107.1 . . ?
C28B C26B H26B 107.1 . . ?
C27B C26B H26B 107.1 . . ?
C26B C27B H27D 109.5 . . ?
C26B C27B H27E 109.5 . . ?
H27D C27B H27E 109.5 . . ?
C26B C27B H27F 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
C26B C28B H28D 109.5 . . ?
C26B C28B H28E 109.5 . . ?
H28D C28B H28E 109.5 . . ?
C26B C28B H28F 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
C21B C29 C31 112(2) . . ?
C21B C29 C30 110.7(15) . . ?
C31 C29 C30 109.1(4) . . ?
C31 C29 C21A 109(2) . . ?
C30 C29 C21A 113.1(16) . . ?
C31 C29 H29 108.4 . . ?
C30 C29 H29 108.4 . . ?
C21A C29 H29 108.4 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 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
C14 P1 N1 C20B 133.1(13) . . . . ?
C1 P1 N1 C20B 12.0(14) . . . . ?
C13 P1 N1 C20B -112.0(13) . . . . ?
C14 P1 N1 C20A 121.5(12) . . . . ?
C1 P1 N1 C20A 0.4(12) . . . . ?
C13 P1 N1 C20A -123.6(12) . . . . ?
N1 P1 C1 C2 -0.1(4) . . . . ?
C14 P1 C1 C2 -129.4(3) . . . . ?
C13 P1 C1 C2 132.8(3) . . . . ?
N1 P1 C1 C6 177.4(2) . . . . ?
C14 P1 C1 C6 48.1(3) . . . . ?
C13 P1 C1 C6 -49.7(3) . . . . ?
C6 C1 C2 C3 -0.3(5) . . . . ?
P1 C1 C2 C3 177.0(3) . . . . ?
C1 C2 C3 C4 -0.3(6) . . . . ?
C2 C3 C4 C5 1.0(6) . . . . ?
C3 C4 C5 C6 -1.1(6) . . . . ?
C4 C5 C6 C1 0.5(5) . . . . ?
C4 C5 C6 C7 -178.7(3) . . . . ?
C2 C1 C6 C5 0.2(5) . . . . ?
P1 C1 C6 C5 -177.4(3) . . . . ?
C2 C1 C6 C7 179.5(3) . . . . ?
P1 C1 C6 C7 1.9(4) . . . . ?
C5 C6 C7 C19 120.0(4) . . . . ?
C1 C6 C7 C19 -59.2(4) . . . . ?
C5 C6 C7 C8 -124.1(4) . . . . ?
C1 C6 C7 C8 56.7(4) . . . . ?
C6 C7 C8 C9 123.5(4) . . . . ?
C19 C7 C8 C9 -119.8(4) . . . . ?
C6 C7 C8 C13 -58.3(4) . . . . ?
C19 C7 C8 C13 58.4(4) . . . . ?
C13 C8 C9 C10 -1.4(6) . . . . ?
C7 C8 C9 C10 176.7(4) . . . . ?
C8 C9 C10 C11 0.1(7) . . . . ?
C9 C10 C11 C12 1.1(7) . . . . ?
C10 C11 C12 C13 -0.9(7) . . . . ?
C11 C12 C13 C8 -0.5(6) . . . . ?
C11 C12 C13 P1 -178.2(3) . . . . ?
C9 C8 C13 C12 1.6(6) . . . . ?
C7 C8 C13 C12 -176.6(4) . . . . ?
C9 C8 C13 P1 179.5(3) . . . . ?
C7 C8 C13 P1 1.3(5) . . . . ?
N1 P1 C13 C12 1.0(4) . . . . ?
C14 P1 C13 C12 126.3(4) . . . . ?
C1 P1 C13 C12 -134.1(4) . . . . ?
N1 P1 C13 C8 -176.8(3) . . . . ?
C14 P1 C13 C8 -51.6(3) . . . . ?
C1 P1 C13 C8 48.1(3) . . . . ?
N1 P1 C14 C15 -0.4(4) . . . . ?
C1 P1 C14 C15 132.7(3) . . . . ?
C13 P1 C14 C15 -127.6(4) . . . . ?
N1 P1 C14 C19 177.5(3) . . . . ?
C1 P1 C14 C19 -49.4(3) . . . . ?
C13 P1 C14 C19 50.3(3) . . . . ?
C19 C14 C15 C16 0.4(6) . . . . ?
P1 C14 C15 C16 178.2(3) . . . . ?
C14 C15 C16 C17 -0.4(6) . . . . ?
C15 C16 C17 C18 0.4(6) . . . . ?
C16 C17 C18 C19 -0.5(6) . . . . ?
C17 C18 C19 C14 0.5(6) . . . . ?
C17 C18 C19 C7 -178.5(4) . . . . ?
C15 C14 C19 C18 -0.5(6) . . . . ?
P1 C14 C19 C18 -178.5(3) . . . . ?
C15 C14 C19 C7 178.6(3) . . . . ?
P1 C14 C19 C7 0.6(4) . . . . ?
C6 C7 C19 C18 -123.3(4) . . . . ?
C8 C7 C19 C18 119.1(4) . . . . ?
C6 C7 C19 C14 57.7(4) . . . . ?
C8 C7 C19 C14 -59.9(4) . . . . ?
P1 N1 C20A C21A 83(4) . . . . ?
P1 N1 C20A C25A -89(3) . . . . ?
N1 C20A C21A C22A 172(4) . . . . ?
C25A C20A C21A C22A -16(6) . . . . ?
N1 C20A C21A C29 -11(6) . . . . ?
C25A C20A C21A C29 161(3) . . . . ?
C20A C21A C22A C23A 11(7) . . . . ?
C29 C21A C22A C23A -165(3) . . . . ?
C21A C22A C23A C24A -6(5) . . . . ?
C22A C23A C24A C25A 7(3) . . . . ?
C23A C24A C25A C20A -12(3) . . . . ?
C23A C24A C25A C26A 179.4(14) . . . . ?
C21A C20A C25A C24A 16(4) . . . . ?
N1 C20A C25A C24A -172(2) . . . . ?
C21A C20A C25A C26A -175(3) . . . . ?
N1 C20A C25A C26A -4(5) . . . . ?
C24A C25A C26A C27A -47.1(17) . . . . ?
C20A C25A C26A C27A 144(2) . . . . ?
C24A C25A C26A C28A 76.4(17) . . . . ?
C20A C25A C26A C28A -92(2) . . . . ?
P1 N1 C20B C21B 71(5) . . . . ?
P1 N1 C20B C25B -124(2) . . . . ?
N1 C20B C21B C22B 173(4) . . . . ?
C25B C20B C21B C22B 9(6) . . . . ?
N1 C20B C21B C29 -6(6) . . . . ?
C25B C20B C21B C29 -170(3) . . . . ?
C20B C21B C22B C23B -14(6) . . . . ?
C29 C21B C22B C23B 165(3) . . . . ?
C21B C22B C23B C24B 15(5) . . . . ?
C22B C23B C24B C25B -11(3) . . . . ?
C23B C24B C25B C20B 6(3) . . . . ?
C23B C24B C25B C26B 179.2(12) . . . . ?
N1 C20B C25B C24B -170(2) . . . . ?
C21B C20B C25B C24B -5(5) . . . . ?
N1 C20B C25B C26B 16(4) . . . . ?
C21B C20B C25B C26B -178(3) . . . . ?
C24B C25B C26B C28B 28.5(18) . . . . ?
C20B C25B C26B C28B -158(2) . . . . ?
C24B C25B C26B C27B -96.7(13) . . . . ?
C20B C25B C26B C27B 76(2) . . . . ?
C22B C21B C29 C31 -79(4) . . . . ?
C20B C21B C29 C31 100(4) . . . . ?
C22B C21B C29 C30 43(4) . . . . ?
C20B C21B C29 C30 -138(4) . . . . ?
C22A C21A C29 C31 -79(4) . . . . ?
C20A C21A C29 C31 104(4) . . . . ?
C22A C21A C29 C30 43(5) . . . . ?
C20A C21A C29 C30 -134(4) . . . . ?

_refine_diff_density_max         0.515
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.066



# start Validation Reply Form
_vrf_PLAT029_nt1400_SMC190_cryst2_full_100K 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.979 Why?  
RESPONSE: These reflections are missing because of the instrument geometry 
limitations.
;
_vrf_PLAT220_nt1400_SMC190_cryst2_full_100K 
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        3.9 Ratio 
RESPONSE: Disordered diisopropylphenyl group in the structure.
;
_vrf_PLAT222_nt1400_SMC190_cryst2_full_100K 
;
PROBLEM: NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        4.2 Ratio 
RESPONSE: Disordered diisopropylphenyl group in the structure.
;
_vrf_PLAT340_nt1400_SMC190_cryst2_full_100K 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.006 Ang.  
RESPONSE: Disordered diisopropylphenyl group in the structure.
;
_vrf_PLAT906_nt1400_SMC190_cryst2_full_100K 
;
PROBLEM: Large K Value in the Analysis of Variance ......      9.962 Check 
RESPONSE: Even the best selected crystal was weakly diffracting thin plate.
;
_vrf_PLAT911_nt1400_SMC190_cryst2_full_100K 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.596         90 Report
RESPONSE: These reflections are missing because of the instrument geometry 
limitations.
;
# end Validation Reply Form


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nt1318_SMC038_100K
_database_code_depnum_ccdc_archive 'CCDC 2313771'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2024-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        '9-phosphatriptycene-iminium bistriflimidate'
_chemical_name_common            '9-phosphatriptycene-iminium bistriflimidate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H19 N P, C2 F6 N O4 S2'
_chemical_formula_sum            'C27 H19 F6 N2 O4 P S2'
_chemical_formula_weight         644.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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'
F F 0.0096 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0826 0.0763 '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                   8.3718(3)
_cell_length_b                   17.3368(6)
_cell_length_c                   20.1621(8)
_cell_angle_alpha                113.9252(10)
_cell_angle_beta                 91.4063(12)
_cell_angle_gamma                93.9353(11)
_cell_volume                     2664.18(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9881
_cell_measurement_theta_min      2.3928
_cell_measurement_theta_max      23.6001


_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    0.182
_shelx_estimated_absorpt_T_min   0.921
_shelx_estimated_absorpt_T_max   0.958
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            151281
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.927
_diffrn_reflns_theta_max         23.631
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             16187
_reflns_number_gt                14930
_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       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 4.0 (Macrae et al, 2020)'
_computing_publication_material  'enCIFer (Allen et al, 2004)'
_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)+(0.0746P)²+1.0557P] 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         16187
_refine_ls_number_parameters     1029
_refine_ls_number_restraints     404
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1252
_refine_ls_wR_factor_gt          0.1218
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.003
_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
P2 P 1.00178(3) 0.24821(2) 0.14209(2) 0.01522(7) Uani 1 1 d . . . . .
N2 N 0.96769(12) 0.27790(7) 0.22755(5) 0.01923(18) Uani 1 1 d . . . . .
H2N H 0.866413 0.281676 0.238199 0.023 Uiso 1 1 calc R U . . .
C26 C 1.09743(13) 0.15314(7) 0.09866(6) 0.01709(19) Uani 1 1 d . . . . .
C27 C 1.16223(14) 0.10302(7) 0.12975(6) 0.0206(2) Uani 1 1 d . . . . .
H27 H 1.155373 0.116519 0.180154 0.025 Uiso 1 1 calc R U . . .
C28 C 1.23747(15) 0.03251(8) 0.08522(7) 0.0240(2) Uani 1 1 d . . . . .
H28 H 1.283338 -0.002405 0.105368 0.029 Uiso 1 1 calc R U . . .
C29 C 1.24578(15) 0.01293(8) 0.01125(7) 0.0231(2) Uani 1 1 d . . . . .
H29 H 1.297816 -0.035183 -0.018523 0.028 Uiso 1 1 calc R U . . .
C30 C 1.17865(13) 0.06306(7) -0.01974(6) 0.0196(2) Uani 1 1 d . . . . .
H30 H 1.183840 0.048726 -0.070336 0.024 Uiso 1 1 calc R U . . .
C31 C 1.10431(13) 0.13397(7) 0.02392(6) 0.01662(18) Uani 1 1 d . . . . .
C32 C 1.03215(13) 0.19472(7) -0.00401(6) 0.01665(18) Uani 1 1 d . . . . .
H32 H 1.042806 0.174803 -0.057576 0.020 Uiso 1 1 calc R U . . .
C33 C 1.12079(13) 0.28255(7) 0.03667(6) 0.01685(19) Uani 1 1 d . . . . .
C34 C 1.20101(14) 0.32838(8) 0.00326(6) 0.0207(2) Uani 1 1 d . . . . .
H34 H 1.205935 0.305269 -0.048098 0.025 Uiso 1 1 calc R U . . .
C35 C 1.27458(15) 0.40898(8) 0.04592(7) 0.0241(2) Uani 1 1 d . . . . .
H35 H 1.328567 0.440748 0.023047 0.029 Uiso 1 1 calc R U . . .
C36 C 1.27026(15) 0.44346(8) 0.12107(7) 0.0246(2) Uani 1 1 d . . . . .
H36 H 1.321315 0.498301 0.149076 0.030 Uiso 1 1 calc R U . . .
C37 C 1.19131(13) 0.39794(7) 0.15557(6) 0.0204(2) Uani 1 1 d . . . . .
H37 H 1.188169 0.420914 0.207002 0.024 Uiso 1 1 calc R U . . .
C38 C 1.11730(12) 0.31813(7) 0.11292(6) 0.01674(19) Uani 1 1 d . . . . .
C39 C 0.85550(13) 0.20057(7) 0.01391(6) 0.01596(18) Uani 1 1 d . . . . .
C40 C 0.72989(13) 0.18111(7) -0.03802(6) 0.0186(2) Uani 1 1 d . . . . .
H40 H 0.751230 0.164218 -0.087797 0.022 Uiso 1 1 calc R U . . .
C41 C 0.57216(14) 0.18644(8) -0.01684(7) 0.0223(2) Uani 1 1 d . . . . .
H41 H 0.486259 0.172949 -0.052439 0.027 Uiso 1 1 calc R U . . .
C42 C 0.53948(14) 0.21136(8) 0.05604(7) 0.0235(2) Uani 1 1 d . . . . .
H42 H 0.431526 0.214671 0.069703 0.028 Uiso 1 1 calc R U . . .
C43 C 0.66364(13) 0.23143(7) 0.10892(6) 0.0198(2) Uani 1 1 d . . . . .
H43 H 0.641816 0.248166 0.158628 0.024 Uiso 1 1 calc R U . . .
C44 C 0.82049(13) 0.22643(7) 0.08736(6) 0.01652(18) Uani 1 1 d . . . . .
C45 C 1.24443(14) 0.29462(8) 0.27948(6) 0.0205(2) Uani 1 1 d . . . . .
H45 H 1.285993 0.277503 0.232686 0.025 Uiso 1 1 calc R U . . .
C46 C 1.34757(14) 0.31603(8) 0.34097(7) 0.0221(2) Uani 1 1 d . . . . .
H46 H 1.459636 0.312481 0.335763 0.027 Uiso 1 1 calc R U . . .
C47 C 1.28790(16) 0.34244(8) 0.40957(7) 0.0237(2) Uani 1 1 d . . . . .
H47 H 1.358895 0.357980 0.451274 0.028 Uiso 1 1 calc R U . . .
C48 C 1.12392(16) 0.34601(8) 0.41692(6) 0.0244(2) Uani 1 1 d . . . . .
H48 H 1.082659 0.363873 0.463822 0.029 Uiso 1 1 calc R U . . .
C49 C 1.01980(14) 0.32366(8) 0.35621(6) 0.0210(2) Uani 1 1 d . . . . .
H49 H 0.907470 0.325389 0.361421 0.025 Uiso 1 1 calc R U . . .
C50 C 1.08080(13) 0.29860(7) 0.28742(6) 0.01726(19) Uani 1 1 d . . . . .
P1 P 0.48747(3) 0.76083(2) 0.36533(2) 0.01805(7) Uani 1 1 d . . . . .
N1 N 0.51254(13) 0.74008(9) 0.28080(6) 0.0310(3) Uani 1 1 d . . . . .
H1 H 0.612590 0.746871 0.270403 0.037 Uiso 1 1 calc R U . . .
C1 C 0.39136(14) 0.85349(7) 0.41639(7) 0.0208(2) Uani 1 1 d . . . . .
C2 C 0.32390(17) 0.90829(9) 0.39126(9) 0.0308(3) Uani 1 1 d . . . . .
H2 H 0.328011 0.899649 0.341720 0.037 Uiso 1 1 calc R U . . .
C3 C 0.2502(2) 0.97609(9) 0.44050(11) 0.0407(4) Uani 1 1 d . . . . .
H3 H 0.201813 1.013841 0.424306 0.049 Uiso 1 1 calc R U . . .
C4 C 0.24661(18) 0.98916(9) 0.51255(10) 0.0384(4) Uani 1 1 d . . . . .
H4 H 0.195457 1.035801 0.545371 0.046 Uiso 1 1 calc R U . . .
C5 C 0.31703(15) 0.93488(8) 0.53809(8) 0.0278(3) Uani 1 1 d . . . . .
H5 H 0.315218 0.944809 0.587984 0.033 Uiso 1 1 calc R U . . .
C6 C 0.38951(13) 0.86639(7) 0.48967(7) 0.0196(2) Uani 1 1 d . . . . .
C7 C 0.46809(13) 0.80223(7) 0.51093(6) 0.01744(19) Uani 1 1 d . . . . .
H7 H 0.461637 0.817366 0.564165 0.021 Uiso 1 1 calc R U . . .
C8 C 0.38031(13) 0.71510(7) 0.46648(6) 0.01713(19) Uani 1 1 d . . . . .
C9 C 0.30446(14) 0.66467(8) 0.49689(7) 0.0218(2) Uani 1 1 d . . . . .
H9 H 0.305208 0.683423 0.548195 0.026 Uiso 1 1 calc R U . . .
C10 C 0.22688(15) 0.58607(8) 0.45160(8) 0.0254(2) Uani 1 1 d . . . . .
H10 H 0.175208 0.551488 0.472500 0.031 Uiso 1 1 calc R U . . .
C11 C 0.22419(16) 0.55785(8) 0.37672(8) 0.0266(2) Uani 1 1 d . . . . .
H11 H 0.169781 0.504515 0.346825 0.032 Uiso 1 1 calc R U . . .
C12 C 0.30086(14) 0.60722(8) 0.34484(7) 0.0227(2) Uani 1 1 d . . . . .
H12 H 0.300257 0.587968 0.293493 0.027 Uiso 1 1 calc R U . . .
C13 C 0.37804(13) 0.68519(7) 0.39011(6) 0.01747(19) Uani 1 1 d . . . . .
C14 C 0.67274(13) 0.77908(7) 0.41697(6) 0.0186(2) Uani 1 1 d . . . . .
C15 C 0.82767(14) 0.77460(8) 0.39307(7) 0.0227(2) Uani 1 1 d . . . . .
H15 H 0.845950 0.760116 0.343286 0.027 Uiso 1 1 calc R U . . .
C16 C 0.95528(14) 0.79191(9) 0.44403(8) 0.0267(2) Uani 1 1 d . . . . .
H16 H 1.062122 0.789172 0.428935 0.032 Uiso 1 1 calc R U . . .
C17 C 0.92765(15) 0.81315(8) 0.51681(8) 0.0257(2) Uani 1 1 d . . . . .
H17 H 1.015971 0.824987 0.550962 0.031 Uiso 1 1 calc R U . . .
C18 C 0.77185(14) 0.81732(7) 0.54036(7) 0.0211(2) Uani 1 1 d . . . . .
H18 H 0.754050 0.831827 0.590195 0.025 Uiso 1 1 calc R U . . .
C19 C 0.64309(13) 0.80008(7) 0.49031(6) 0.01746(19) Uani 1 1 d . . . . .
C20 C 0.39905(15) 0.71263(8) 0.22054(7) 0.0227(2) Uani 1 1 d . . . . .
C21 C 0.23580(16) 0.71848(9) 0.22917(7) 0.0269(2) Uani 1 1 d . . . . .
H21 H 0.195856 0.740489 0.276391 0.032 Uiso 1 1 calc R U . . .
C22 C 0.13096(17) 0.69165(9) 0.16766(8) 0.0288(3) Uani 1 1 d . . . . .
H22 H 0.018976 0.695297 0.173092 0.035 Uiso 1 1 calc R U . . .
C23 C 0.18884(19) 0.65977(9) 0.09881(8) 0.0320(3) Uani 1 1 d . . . . .
H23 H 0.116902 0.641418 0.057115 0.038 Uiso 1 1 calc R U . . .
C24 C 0.35236(19) 0.65474(10) 0.09098(7) 0.0322(3) Uani 1 1 d . . . . .
H24 H 0.392157 0.633204 0.043719 0.039 Uiso 1 1 calc R U . . .
C25 C 0.45839(17) 0.68083(9) 0.15143(7) 0.0264(2) Uani 1 1 d . . . . .
H25 H 0.570295 0.677067 0.145782 0.032 Uiso 1 1 calc R U . . .
S1A S 0.78021(4) 0.89536(2) 0.22696(2) 0.02084(8) Uani 0.9532(11) 1 d D U P A 1
S2A S 0.53329(4) 1.00436(2) 0.25187(2) 0.02343(8) Uani 0.9532(11) 1 d D U P A 1
F1A F 1.08909(12) 0.90034(8) 0.21989(8) 0.0498(3) Uani 0.9532(11) 1 d D . P A 1
F2A F 0.99041(15) 1.01558(9) 0.23080(11) 0.0663(5) Uani 0.9532(11) 1 d D U P A
1
F3A F 1.01128(16) 0.98367(12) 0.32194(7) 0.0702(5) Uani 0.9532(11) 1 d D U P A
1
F4A F 0.72465(14) 1.07346(7) 0.18523(6) 0.0428(3) Uani 0.9532(11) 1 d D . P A 1
F5A F 0.71786(15) 1.14669(8) 0.30060(7) 0.0474(3) Uani 0.9532(11) 1 d D U P A 1
F6A F 0.51866(14) 1.14082(7) 0.22854(7) 0.0454(3) Uani 0.9532(11) 1 d D . P A 1
O1A O 0.75718(14) 0.87124(8) 0.15018(6) 0.0333(2) Uani 0.9532(11) 1 d D U P A 1
O2A O 0.79168(14) 0.82899(8) 0.25130(8) 0.0403(3) Uani 0.9532(11) 1 d D . P A 1
O3A O 0.45591(15) 0.95287(8) 0.18266(6) 0.0341(2) Uani 0.9532(11) 1 d D U P A 1
O4A O 0.43700(16) 1.04314(9) 0.31281(7) 0.0339(3) Uani 0.9532(11) 1 d D U P A 1
N3A N 0.67343(14) 0.96439(8) 0.27706(6) 0.0253(2) Uani 0.9532(11) 1 d D . P A 1
C51A C 0.98028(18) 0.95220(11) 0.25152(9) 0.0307(3) Uani 0.9532(11) 1 d D U P A
1
C52A C 0.6303(2) 1.09639(10) 0.24077(9) 0.0311(3) Uani 0.9532(11) 1 d D U P A 1
S1B S 0.9625(12) 0.9929(9) 0.2507(6) 0.047(2) Uani 0.0468(11) 1 d D U P A 2
S2B S 0.7097(11) 1.1015(7) 0.2683(6) 0.0408(19) Uani 0.0468(11) 1 d D U P A 2
F1B F 0.968(3) 0.8576(18) 0.2679(18) 0.074(7) Uani 0.0468(11) 1 d D . P A 2
F2B F 0.761(3) 0.911(2) 0.3052(11) 0.070(7) Uani 0.0468(11) 1 d D U P A 2
F3B F 0.779(3) 0.8455(15) 0.1826(10) 0.049(4) Uani 0.0468(11) 1 d D U P A 2
F4B F 0.490(3) 0.9931(17) 0.1799(11) 0.058(5) Uani 0.0468(11) 1 d D U P A 2
F5B F 0.450(3) 1.0173(15) 0.2915(12) 0.045(4) Uani 0.0468(11) 1 d D U P A 2
F6B F 0.403(3) 1.1113(18) 0.267(2) 0.088(9) Uani 0.0468(11) 1 d D . P A 2
O1B O 1.054(3) 0.9588(15) 0.1867(11) 0.042(5) Uani 0.0468(11) 1 d D . P A 2
O2B O 1.039(3) 1.038(2) 0.3166(11) 0.058(5) Uani 0.0468(11) 1 d D U P A 2
O3B O 0.709(5) 1.170(2) 0.247(3) 0.130(17) Uani 0.0468(11) 1 d D . P A 2
O4B O 0.745(3) 1.1231(19) 0.3444(10) 0.056(5) Uani 0.0468(11) 1 d D U P A 2
N3B N 0.819(3) 1.0306(19) 0.2245(13) 0.070(8) Uani 0.0468(11) 1 d D . P A 2
C51B C 0.853(3) 0.8961(12) 0.2487(11) 0.041(4) Uani 0.0468(11) 1 d D U P A 2
C52B C 0.508(2) 1.0516(14) 0.2483(12) 0.045(4) Uani 0.0468(11) 1 d D U P A 2
S3A S 0.82903(9) 0.54068(4) 0.22563(4) 0.02967(13) Uani 0.8805(13) 1 d D . P B
1
S4A S 0.66661(5) 0.44062(3) 0.28536(2) 0.01917(9) Uani 0.8805(13) 1 d D . P B 1
F7A F 0.78506(18) 0.54752(8) 0.10055(7) 0.0498(3) Uani 0.8805(13) 1 d D . P B 1
F8A F 0.87548(15) 0.43147(9) 0.09277(6) 0.0407(3) Uani 0.8805(13) 1 d D . P B 1
F9A F 0.63126(12) 0.45193(9) 0.11417(6) 0.0455(3) Uani 0.8805(13) 1 d D . P B 1
F10A F 0.70310(18) 0.58975(7) 0.39612(6) 0.0356(3) Uani 0.8805(13) 1 d D U P B
1
F11A F 0.58719(13) 0.48960(7) 0.41959(5) 0.0343(2) Uani 0.8805(13) 1 d D . P B
1
F12A F 0.84174(11) 0.49548(6) 0.40772(5) 0.0294(2) Uani 0.8805(13) 1 d D U P B
1
O5A O 0.9942(2) 0.57029(13) 0.23117(12) 0.0514(6) Uani 0.8805(13) 1 d D . P B 1
O6A O 0.7115(2) 0.60017(8) 0.25258(7) 0.0467(4) Uani 0.8805(13) 1 d D . P B 1
O7A O 0.68470(12) 0.35729(6) 0.28329(6) 0.0219(2) Uani 0.8805(13) 1 d D . P B 1
O8A O 0.51315(18) 0.45764(11) 0.26523(9) 0.0295(3) Uani 0.8805(13) 1 d D . P B
1
N4A N 0.81680(15) 0.46402(8) 0.24975(7) 0.0226(2) Uani 0.8805(13) 1 d D . P B 1
C53A C 0.7772(3) 0.48895(17) 0.12770(14) 0.0273(5) Uani 0.8805(13) 1 d D U P B
1
C54A C 0.7022(3) 0.50849(12) 0.38301(11) 0.0223(4) Uani 0.8805(13) 1 d D U P B
1
S3B S 0.8199(6) 0.5614(3) 0.2161(3) 0.0276(9) Uani 0.1195(13) 1 d D . P B 2
S4B S 0.6456(6) 0.4656(3) 0.2782(2) 0.0318(9) Uani 0.1195(13) 1 d D . P B 2
F7B F 0.6496(8) 0.5088(5) 0.0931(4) 0.0292(14) Uani 0.1195(13) 1 d D . P B 2
F8B F 0.9028(9) 0.5078(5) 0.0826(4) 0.0363(17) Uani 0.1195(13) 1 d D . P B 2
F9B F 0.7773(13) 0.4112(4) 0.1066(4) 0.0389(19) Uani 0.1195(13) 1 d D . P B 2
F10B F 0.6270(12) 0.5808(6) 0.4120(5) 0.040(2) Uani 0.1195(13) 1 d D . P B 2
F11B F 0.6965(14) 0.4609(6) 0.4047(5) 0.050(2) Uani 0.1195(13) 1 d D . P B 2
F12B F 0.8622(9) 0.5476(6) 0.3852(4) 0.0414(17) Uani 0.1195(13) 1 d D U P B 2
O5B O 0.9727(11) 0.5414(7) 0.2359(6) 0.033(3) Uani 0.1195(13) 1 d D . P B 2
O6B O 0.8087(10) 0.6441(5) 0.2182(4) 0.0279(16) Uani 0.1195(13) 1 d D . P B 2
O7B O 0.7564(15) 0.4006(7) 0.2494(5) 0.049(3) Uani 0.1195(13) 1 d D . P B 2
O8B O 0.4809(15) 0.4414(10) 0.2775(9) 0.043(4) Uani 0.1195(13) 1 d D . P B 2
N4B N 0.6656(10) 0.5387(5) 0.2506(5) 0.0232(16) Uani 0.1195(13) 1 d D . P B 2
C53B C 0.7855(19) 0.4918(9) 0.1190(7) 0.021(2) Uani 0.1195(13) 1 d D U P B 2
C54B C 0.7086(19) 0.5175(10) 0.3746(7) 0.025(2) Uani 0.1195(13) 1 d D U P B 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
P2 N2 1.6248(10) . ?
P2 C44 1.7790(11) . ?
P2 C26 1.7804(11) . ?
P2 C38 1.7876(11) . ?
N2 C50 1.4243(14) . ?
C26 C27 1.3902(15) . ?
C26 C31 1.4089(15) . ?
C27 C28 1.3930(17) . ?
C28 C29 1.3935(18) . ?
C29 C30 1.3970(16) . ?
C30 C31 1.3884(15) . ?
C31 C32 1.5307(15) . ?
C32 C33 1.5310(15) . ?
C32 C39 1.5314(15) . ?
C33 C34 1.3854(15) . ?
C33 C38 1.4073(15) . ?
C34 C35 1.3973(17) . ?
C35 C36 1.3875(18) . ?
C36 C37 1.3927(17) . ?
C37 C38 1.3889(15) . ?
C39 C40 1.3879(15) . ?
C39 C44 1.4075(15) . ?
C40 C41 1.3953(16) . ?
C41 C42 1.3935(17) . ?
C42 C43 1.3904(16) . ?
C43 C44 1.3907(15) . ?
C45 C50 1.3862(16) . ?
C45 C46 1.3966(16) . ?
C46 C47 1.3871(17) . ?
C47 C48 1.3873(18) . ?
C48 C49 1.3873(16) . ?
C49 C50 1.3964(15) . ?
P1 N1 1.6152(11) . ?
P1 C1 1.7790(13) . ?
P1 C14 1.7821(12) . ?
P1 C13 1.7881(11) . ?
N1 C20 1.4205(16) . ?
C1 C2 1.3884(16) . ?
C1 C6 1.4026(17) . ?
C2 C3 1.389(2) . ?
C3 C4 1.378(3) . ?
C4 C5 1.397(2) . ?
C5 C6 1.3852(17) . ?
C6 C7 1.5256(16) . ?
C7 C8 1.5304(15) . ?
C7 C19 1.5315(15) . ?
C8 C9 1.3860(15) . ?
C8 C13 1.4107(15) . ?
C9 C10 1.3974(17) . ?
C10 C11 1.3845(19) . ?
C11 C12 1.3960(18) . ?
C12 C13 1.3886(15) . ?
C14 C15 1.3909(15) . ?
C14 C19 1.4052(16) . ?
C15 C16 1.3925(18) . ?
C16 C17 1.390(2) . ?
C17 C18 1.3955(17) . ?
C18 C19 1.3883(15) . ?
C20 C21 1.3873(18) . ?
C20 C25 1.3931(17) . ?
C21 C22 1.3955(18) . ?
C22 C23 1.384(2) . ?
C23 C24 1.386(2) . ?
C24 C25 1.3866(19) . ?
S1A O2A 1.4300(11) . ?
S1A O1A 1.4345(11) . ?
S1A N3A 1.5692(12) . ?
S1A C51A 1.8327(15) . ?
S2A O3A 1.4246(11) . ?
S2A O4A 1.4368(13) . ?
S2A N3A 1.5755(12) . ?
S2A C52A 1.8374(16) . ?
F1A C51A 1.312(2) . ?
F2A C51A 1.323(2) . ?
F3A C51A 1.310(2) . ?
F4A C52A 1.3272(17) . ?
F5A C52A 1.330(2) . ?
F6A C52A 1.3300(19) . ?
S1B O2B 1.353(16) . ?
S1B O1B 1.446(16) . ?
S1B N3B 1.584(16) . ?
S1B C51B 1.840(16) . ?
S2B O3B 1.427(16) . ?
S2B O4B 1.440(16) . ?
S2B N3B 1.563(16) . ?
S2B C52B 1.802(16) . ?
F1B C51B 1.341(18) . ?
F2B C51B 1.340(17) . ?
F3B C51B 1.365(17) . ?
F4B C52B 1.337(17) . ?
F5B C52B 1.325(18) . ?
F6B C52B 1.345(18) . ?
S3A O5A 1.4272(19) . ?
S3A O6A 1.4274(17) . ?
S3A N4A 1.5879(13) . ?
S3A C53A 1.833(3) . ?
S4A O8A 1.4233(15) . ?
S4A O7A 1.4469(11) . ?
S4A N4A 1.5719(13) . ?
S4A C54A 1.842(2) . ?
F7A C53A 1.334(3) . ?
F8A C53A 1.318(3) . ?
F9A C53A 1.309(3) . ?
F10A C54A 1.323(2) . ?
F11A C54A 1.329(3) . ?
F12A C54A 1.328(3) . ?
S3B O6B 1.427(9) . ?
S3B O5B 1.437(9) . ?
S3B N4B 1.582(9) . ?
S3B C53B 1.838(13) . ?
S4B O8B 1.411(12) . ?
S4B O7B 1.452(10) . ?
S4B N4B 1.579(9) . ?
S4B C54B 1.826(13) . ?
F7B C53B 1.339(16) . ?
F8B C53B 1.319(16) . ?
F9B C53B 1.314(15) . ?
F10B C54B 1.303(15) . ?
F11B C54B 1.347(15) . ?
F12B C54B 1.333(15) . ?

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
N2 P2 C44 111.64(5) . . ?
N2 P2 C26 117.86(5) . . ?
C44 P2 C26 102.03(5) . . ?
N2 P2 C38 119.84(5) . . ?
C44 P2 C38 102.13(5) . . ?
C26 P2 C38 100.79(5) . . ?
C50 N2 P2 128.28(8) . . ?
C27 C26 C31 121.94(10) . . ?
C27 C26 P2 128.38(9) . . ?
C31 C26 P2 109.66(8) . . ?
C26 C27 C28 118.39(11) . . ?
C27 C28 C29 120.32(11) . . ?
C28 C29 C30 120.93(11) . . ?
C31 C30 C29 119.55(11) . . ?
C30 C31 C26 118.86(10) . . ?
C30 C31 C32 123.73(10) . . ?
C26 C31 C32 117.38(9) . . ?
C31 C32 C33 107.96(8) . . ?
C31 C32 C39 108.96(9) . . ?
C33 C32 C39 108.17(9) . . ?
C34 C33 C38 118.98(10) . . ?
C34 C33 C32 124.31(10) . . ?
C38 C33 C32 116.71(9) . . ?
C33 C34 C35 119.29(11) . . ?
C36 C35 C34 121.22(11) . . ?
C35 C36 C37 120.22(11) . . ?
C38 C37 C36 118.36(11) . . ?
C37 C38 C33 121.92(10) . . ?
C37 C38 P2 127.84(9) . . ?
C33 C38 P2 110.20(8) . . ?
C40 C39 C44 118.91(10) . . ?
C40 C39 C32 123.71(10) . . ?
C44 C39 C32 117.38(9) . . ?
C39 C40 C41 119.75(11) . . ?
C42 C41 C40 120.62(10) . . ?
C43 C42 C41 120.51(11) . . ?
C42 C43 C44 118.47(11) . . ?
C43 C44 C39 121.73(10) . . ?
C43 C44 P2 128.54(9) . . ?
C39 C44 P2 109.73(8) . . ?
C50 C45 C46 119.34(11) . . ?
C47 C46 C45 120.61(11) . . ?
C46 C47 C48 119.60(11) . . ?
C49 C48 C47 120.41(11) . . ?
C48 C49 C50 119.73(11) . . ?
C45 C50 C49 120.29(10) . . ?
C45 C50 N2 122.82(10) . . ?
C49 C50 N2 116.88(10) . . ?
N1 P1 C1 117.41(7) . . ?
N1 P1 C14 112.44(6) . . ?
C1 P1 C14 101.84(5) . . ?
N1 P1 C13 120.14(6) . . ?
C1 P1 C13 100.35(5) . . ?
C14 P1 C13 102.00(5) . . ?
C20 N1 P1 130.37(9) . . ?
C2 C1 C6 121.61(12) . . ?
C2 C1 P1 127.73(11) . . ?
C6 C1 P1 110.66(8) . . ?
C1 C2 C3 118.25(14) . . ?
C4 C3 C2 120.72(13) . . ?
C3 C4 C5 121.02(14) . . ?
C6 C5 C4 119.11(14) . . ?
C5 C6 C1 119.28(11) . . ?
C5 C6 C7 123.85(11) . . ?
C1 C6 C7 116.87(10) . . ?
C6 C7 C8 107.58(9) . . ?
C6 C7 C19 108.74(9) . . ?
C8 C7 C19 108.44(9) . . ?
C9 C8 C13 118.84(10) . . ?
C9 C8 C7 123.89(10) . . ?
C13 C8 C7 117.27(9) . . ?
C8 C9 C10 119.59(11) . . ?
C11 C10 C9 120.98(11) . . ?
C10 C11 C12 120.47(11) . . ?
C13 C12 C11 118.30(11) . . ?
C12 C13 C8 121.83(10) . . ?
C12 C13 P1 128.37(9) . . ?
C8 C13 P1 109.80(8) . . ?
C15 C14 C19 121.76(11) . . ?
C15 C14 P1 128.57(9) . . ?
C19 C14 P1 109.67(8) . . ?
C14 C15 C16 118.27(12) . . ?
C17 C16 C15 120.56(11) . . ?
C16 C17 C18 120.85(11) . . ?
C19 C18 C17 119.40(12) . . ?
C18 C19 C14 119.16(10) . . ?
C18 C19 C7 123.11(10) . . ?
C14 C19 C7 117.73(9) . . ?
C21 C20 C25 120.65(12) . . ?
C21 C20 N1 122.12(11) . . ?
C25 C20 N1 117.22(12) . . ?
C20 C21 C22 119.22(12) . . ?
C23 C22 C21 120.52(13) . . ?
C22 C23 C24 119.66(13) . . ?
C23 C24 C25 120.67(13) . . ?
C24 C25 C20 119.28(13) . . ?
O2A S1A O1A 117.35(8) . . ?
O2A S1A N3A 111.00(7) . . ?
O1A S1A N3A 116.61(6) . . ?
O2A S1A C51A 103.03(8) . . ?
O1A S1A C51A 104.81(7) . . ?
N3A S1A C51A 101.43(7) . . ?
O3A S2A O4A 119.07(8) . . ?
O3A S2A N3A 115.58(7) . . ?
O4A S2A N3A 107.98(7) . . ?
O3A S2A C52A 104.85(8) . . ?
O4A S2A C52A 102.45(8) . . ?
N3A S2A C52A 105.05(8) . . ?
S1A N3A S2A 126.90(7) . . ?
F3A C51A F1A 108.55(15) . . ?
F3A C51A F2A 107.99(18) . . ?
F1A C51A F2A 109.01(15) . . ?
F3A C51A S1A 110.90(12) . . ?
F1A C51A S1A 109.85(12) . . ?
F2A C51A S1A 110.48(11) . . ?
F4A C52A F6A 108.04(14) . . ?
F4A C52A F5A 108.44(15) . . ?
F6A C52A F5A 108.15(13) . . ?
F4A C52A S2A 111.88(11) . . ?
F6A C52A S2A 109.46(12) . . ?
F5A C52A S2A 110.76(11) . . ?
O2B S1B O1B 120.1(17) . . ?
O2B S1B N3B 119.5(18) . . ?
O1B S1B N3B 103.0(14) . . ?
O2B S1B C51B 111.0(16) . . ?
O1B S1B C51B 101.3(12) . . ?
N3B S1B C51B 98.6(15) . . ?
O3B S2B O4B 117(2) . . ?
O3B S2B N3B 115(2) . . ?
O4B S2B N3B 107.4(15) . . ?
O3B S2B C52B 105.3(18) . . ?
O4B S2B C52B 106.1(13) . . ?
N3B S2B C52B 105.5(14) . . ?
S2B N3B S1B 130.9(16) . . ?
F2B C51B F1B 99(2) . . ?
F2B C51B F3B 114.7(19) . . ?
F1B C51B F3B 112(2) . . ?
F2B C51B S1B 113.0(17) . . ?
F1B C51B S1B 103.0(17) . . ?
F3B C51B S1B 113.9(15) . . ?
F5B C52B F4B 108(2) . . ?
F5B C52B F6B 93.4(19) . . ?
F4B C52B F6B 116(2) . . ?
F5B C52B S2B 118.1(18) . . ?
F4B C52B S2B 110.6(16) . . ?
F6B C52B S2B 109.6(17) . . ?
O5A S3A O6A 119.69(13) . . ?
O5A S3A N4A 107.92(10) . . ?
O6A S3A N4A 115.78(9) . . ?
O5A S3A C53A 104.62(13) . . ?
O6A S3A C53A 103.70(11) . . ?
N4A S3A C53A 103.05(10) . . ?
O8A S4A O7A 118.00(9) . . ?
O8A S4A N4A 118.04(9) . . ?
O7A S4A N4A 106.73(7) . . ?
O8A S4A C54A 105.78(10) . . ?
O7A S4A C54A 101.98(8) . . ?
N4A S4A C54A 104.16(9) . . ?
S4A N4A S3A 123.65(9) . . ?
F9A C53A F8A 107.9(2) . . ?
F9A C53A F7A 108.0(2) . . ?
F8A C53A F7A 108.0(2) . . ?
F9A C53A S3A 111.37(17) . . ?
F8A C53A S3A 112.55(17) . . ?
F7A C53A S3A 108.79(17) . . ?
F10A C54A F12A 108.51(17) . . ?
F10A C54A F11A 108.61(18) . . ?
F12A C54A F11A 108.09(17) . . ?
F10A C54A S4A 111.60(15) . . ?
F12A C54A S4A 110.47(14) . . ?
F11A C54A S4A 109.46(14) . . ?
O6B S3B O5B 117.7(7) . . ?
O6B S3B N4B 107.6(5) . . ?
O5B S3B N4B 118.4(7) . . ?
O6B S3B C53B 103.4(7) . . ?
O5B S3B C53B 104.3(7) . . ?
N4B S3B C53B 103.1(6) . . ?
O8B S4B O7B 119.2(9) . . ?
O8B S4B N4B 109.3(7) . . ?
O7B S4B N4B 114.8(6) . . ?
O8B S4B C54B 104.2(8) . . ?
O7B S4B C54B 103.2(7) . . ?
N4B S4B C54B 104.2(6) . . ?
S4B N4B S3B 125.5(6) . . ?
F9B C53B F8B 108.8(12) . . ?
F9B C53B F7B 109.4(11) . . ?
F8B C53B F7B 106.9(12) . . ?
F9B C53B S3B 112.5(10) . . ?
F8B C53B S3B 109.4(9) . . ?
F7B C53B S3B 109.6(10) . . ?
F10B C54B F12B 106.4(12) . . ?
F10B C54B F11B 108.2(12) . . ?
F12B C54B F11B 105.7(12) . . ?
F10B C54B S4B 114.2(10) . . ?
F12B C54B S4B 112.0(10) . . ?
F11B C54B S4B 109.9(10) . . ?

_refine_diff_density_max         0.597
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.087


