# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_nt0805_LHG192_100K
_database_code_depnum_ccdc_archive 'CCDC 2061849'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
(5r,10s)-4-fluoro-10H-5,10-[1,2]benzenoacridophosphine
_chemical_name_common            
(5r,10s)-4-fluoro-10H-5,10-[1,2]benzenoacridophosphine
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H12 F P'
_chemical_formula_sum            'C19 H12 F P'
_chemical_formula_weight         290.26

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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

_cell_length_a                   13.8967(8)
_cell_length_b                   8.1179(3)
_cell_length_c                   13.4003(7)
_cell_angle_alpha                90
_cell_angle_beta                 113.349(7)
_cell_angle_gamma                90
_cell_volume                     1387.93(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2769
_cell_measurement_theta_min      3.8720
_cell_measurement_theta_max      67.0500

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_F_000             600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.540
_exptl_crystal_size_min          0.410
_exptl_absorpt_coefficient_mu    1.756
_shelx_estimated_absorpt_T_min   0.419
_shelx_estimated_absorpt_T_max   0.533
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_T_max  0.613
_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            3246
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         6.463
_diffrn_reflns_theta_max         67.246
_diffrn_reflns_theta_full        67.246
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             1216
_reflns_number_gt                1191
_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    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+4.8682P] 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         1216
_refine_ls_number_parameters     214
_refine_ls_number_restraints     209
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0690
_refine_ls_wR_factor_ref         0.1536
_refine_ls_wR_factor_gt          0.1533
_refine_ls_goodness_of_fit_ref   1.359
_refine_ls_restrained_S_all      1.247
_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 0.21112(19) 0.4962(3) 0.36134(19) 0.0268(6) Uani 0.5 1 d . . P A -1
F1 F 0.3794(6) 0.3095(10) 0.3100(7) 0.048(3) Uani 0.268(7) 1 d . . P B -1
F2 F 0.0062(15) 0.287(3) 0.2672(15) 0.050(8) Uani 0.103(7) 1 d . . P C -1
C1 C 0.4022(14) 0.312(3) 0.4183(14) 0.029(3) Uani 0.5 1 d D . P A -1
H1 H 0.386668 0.310578 0.342539 0.035 Uiso 0.19(3) 1 calc R U P D -1
C2 C 0.4908(11) 0.234(2) 0.4901(12) 0.027(3) Uani 0.5 1 d D . P A -1
H2 H 0.535308 0.174580 0.464319 0.032 Uiso 0.5 1 calc R U P A -1
C3 C 0.5140(14) 0.243(3) 0.6005(11) 0.033(3) Uani 0.5 1 d D . P A -1
H3 H 0.574788 0.189710 0.650582 0.039 Uiso 0.5 1 calc R U P A -1
C4 C 0.4494(17) 0.329(3) 0.6386(14) 0.030(3) Uani 0.5 1 d D . P A -1
H4 H 0.467214 0.334007 0.714683 0.036 Uiso 0.5 1 calc R U P A -1
C5 C 0.361(3) 0.408(4) 0.5702(17) 0.029(3) Uani 0.5 1 d D . P A -1
C6 C 0.3352(15) 0.393(3) 0.4579(16) 0.024(3) Uani 0.5 1 d D . P A -1
C7 C 0.2765(8) 0.4866(13) 0.5938(8) 0.033(2) Uani 0.5 1 d . . P A -1
H7 H 0.299013 0.484713 0.674570 0.039 Uiso 0.5 1 calc R U P A -1
C14 C 0.1209(14) 0.329(3) 0.5988(14) 0.031(3) Uani 0.5 1 d D . P A -1
H14 H 0.146821 0.334778 0.675857 0.037 Uiso 0.5 1 calc R U P A -1
C15 C 0.0288(14) 0.244(3) 0.5435(11) 0.033(3) Uani 0.5 1 d D . P A -1
H15 H -0.008096 0.195448 0.582469 0.040 Uiso 0.5 1 calc R U P A -1
C16 C -0.0097(13) 0.229(2) 0.4317(12) 0.031(3) Uani 0.5 1 d D . P A -1
H16 H -0.071936 0.168280 0.393613 0.037 Uiso 0.5 1 calc R U P A -1
C17 C 0.0434(17) 0.304(3) 0.3760(15) 0.032(3) Uani 0.5 1 d D . P A -1
H17 H 0.016953 0.297605 0.298963 0.039 Uiso 0.45(3) 1 calc R U P E -1
C18 C 0.137(2) 0.389(4) 0.4340(17) 0.025(3) Uani 0.5 1 d D . P A -1
C19 C 0.1760(18) 0.406(4) 0.5478(17) 0.031(3) Uani 0.5 1 d D . P A -1
F3 F 0.2004(12) 0.8775(19) 0.3060(14) 0.042(5) Uani 0.129(7) 1 d . . P F -1
C8 C 0.2676(19) 0.6610(16) 0.5610(15) 0.026(2) Uani 0.5 1 d D . P A -1
C9 C 0.2842(12) 0.7999(12) 0.6234(10) 0.030(2) Uani 0.5 1 d D . P A -1
H9 H 0.304667 0.788129 0.699584 0.036 Uiso 0.5 1 calc R U P A -1
C10 C 0.2723(10) 0.9564(12) 0.5799(7) 0.036(2) Uani 0.5 1 d D . P A -1
H10 H 0.285848 1.049177 0.626741 0.044 Uiso 0.5 1 calc R U P A -1
C11 C 0.2409(8) 0.9804(9) 0.4691(6) 0.032(3) Uani 0.5 1 d D . P A -1
H11 H 0.232765 1.088374 0.439486 0.038 Uiso 0.5 1 calc R U P A -1
C12 C 0.2219(13) 0.8449(13) 0.4034(10) 0.032(2) Uani 0.5 1 d D . P A -1
H12 H 0.199876 0.858064 0.327045 0.039 Uiso 0.36(3) 1 calc R U P G -1
C13 C 0.235(2) 0.6868(15) 0.4486(16) 0.027(3) Uani 0.5 1 d D . P A -1


_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 C13 1.888(12) . ?
P1 C18 1.890(16) . ?
P1 C6 1.894(14) . ?
C1 C2 1.380(11) . ?
C1 C6 1.404(15) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.366(17) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(12) . ?
C5 C7 1.48(2) . ?
C7 C19 1.44(2) . ?
C7 C8 1.473(17) . ?
C7 H7 1.0000 . ?
C14 C19 1.363(16) . ?
C14 C15 1.384(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(12) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(11) . ?
C16 H16 0.9500 . ?
C17 C18 1.401(16) . ?
C17 H17 0.9500 . ?
C18 C19 1.408(12) . ?
C8 C9 1.368(15) . ?
C8 C13 1.406(9) . ?
C9 C10 1.380(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.368(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.400(14) . ?
C12 H12 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
C13 P1 C18 93.2(14) . . ?
C13 P1 C6 93.0(13) . . ?
C18 P1 C6 88.8(15) . . ?
C2 C1 C6 119.5(12) . . ?
C2 C1 H1 120.3 . . ?
C6 C1 H1 120.3 . . ?
C1 C2 C3 119.1(10) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C2 C3 C4 120.7(11) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 122.1(13) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C4 C5 C6 117.1(16) . . ?
C4 C5 C7 129.7(16) . . ?
C6 C5 C7 112.4(19) . . ?
C1 C6 C5 121.4(15) . . ?
C1 C6 P1 120.7(12) . . ?
C5 C6 P1 117.9(15) . . ?
C19 C7 C8 111(2) . . ?
C19 C7 C5 115(2) . . ?
C8 C7 C5 109(2) . . ?
C19 C7 H7 106.9 . . ?
C8 C7 H7 106.9 . . ?
C5 C7 H7 106.9 . . ?
C19 C14 C15 123.0(12) . . ?
C19 C14 H14 118.5 . . ?
C15 C14 H14 118.5 . . ?
C16 C15 C14 120.2(11) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C17 C16 C15 119.2(11) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C16 C17 C18 119.5(12) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C19 121.7(15) . . ?
C17 C18 P1 121.1(12) . . ?
C19 C18 P1 117.1(15) . . ?
C14 C19 C18 116.4(15) . . ?
C14 C19 C7 129.4(15) . . ?
C18 C19 C7 113.8(18) . . ?
C9 C8 C13 115.9(13) . . ?
C9 C8 C7 129.5(13) . . ?
C13 C8 C7 114.6(15) . . ?
C8 C9 C10 122.6(10) . . ?
C8 C9 H9 118.7 . . ?
C10 C9 H9 118.7 . . ?
C9 C10 C11 121.1(9) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C12 C11 C10 118.4(9) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
C11 C12 C13 119.9(9) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C8 122.2(12) . . ?
C12 C13 P1 121.4(12) . . ?
C8 C13 P1 116.4(14) . . ?

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
C6 C1 C2 C3 -3(3) . . . . ?
C1 C2 C3 C4 0(2) . . . . ?
C2 C3 C4 C5 0(3) . . . . ?
C3 C4 C5 C6 2(5) . . . . ?
C3 C4 C5 C7 171(3) . . . . ?
C2 C1 C6 C5 5(4) . . . . ?
C2 C1 C6 P1 -178.4(17) . . . . ?
C4 C5 C6 C1 -5(5) . . . . ?
C7 C5 C6 C1 -176(2) . . . . ?
C4 C5 C6 P1 179(3) . . . . ?
C7 C5 C6 P1 8(4) . . . . ?
C13 P1 C6 C1 -135(2) . . . . ?
C18 P1 C6 C1 131(2) . . . . ?
C13 P1 C6 C5 41(3) . . . . ?
C18 P1 C6 C5 -52(4) . . . . ?
C4 C5 C7 C19 -112(4) . . . . ?
C6 C5 C7 C19 57(4) . . . . ?
C4 C5 C7 C8 122(4) . . . . ?
C6 C5 C7 C8 -69(4) . . . . ?
C19 C14 C15 C16 2(3) . . . . ?
C14 C15 C16 C17 -2(2) . . . . ?
C15 C16 C17 C18 2(3) . . . . ?
C16 C17 C18 C19 -2(5) . . . . ?
C16 C17 C18 P1 -179(2) . . . . ?
C13 P1 C18 C17 136(3) . . . . ?
C6 P1 C18 C17 -131(3) . . . . ?
C13 P1 C18 C19 -41(3) . . . . ?
C6 P1 C18 C19 52(4) . . . . ?
C15 C14 C19 C18 -2(4) . . . . ?
C15 C14 C19 C7 -174(3) . . . . ?
C17 C18 C19 C14 3(5) . . . . ?
P1 C18 C19 C14 179(2) . . . . ?
C17 C18 C19 C7 176(3) . . . . ?
P1 C18 C19 C7 -8(4) . . . . ?
C8 C7 C19 C14 -120(3) . . . . ?
C5 C7 C19 C14 115(3) . . . . ?
C8 C7 C19 C18 68(3) . . . . ?
C5 C7 C19 C18 -57(4) . . . . ?
C19 C7 C8 C9 115(2) . . . . ?
C5 C7 C8 C9 -116(2) . . . . ?
C19 C7 C8 C13 -63.0(15) . . . . ?
C5 C7 C8 C13 65.3(16) . . . . ?
C13 C8 C9 C10 -1.5(17) . . . . ?
C7 C8 C9 C10 -179.9(17) . . . . ?
C8 C9 C10 C11 1(2) . . . . ?
C9 C10 C11 C12 0.0(14) . . . . ?
C10 C11 C12 C13 0(2) . . . . ?
C11 C12 C13 C8 0(2) . . . . ?
C11 C12 C13 P1 -179.3(14) . . . . ?
C9 C8 C13 C12 1.0(8) . . . . ?
C7 C8 C13 C12 180(3) . . . . ?
C9 C8 C13 P1 -180(2) . . . . ?
C7 C8 C13 P1 -1.0(7) . . . . ?
C18 P1 C13 C12 -136(2) . . . . ?
C6 P1 C13 C12 135(2) . . . . ?
C18 P1 C13 C8 44.7(14) . . . . ?
C6 P1 C13 C8 -44.3(11) . . . . ?

_refine_diff_density_max         0.173
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.048



# start Validation Reply Form
_vrf_PLAT088_nt0805_LHG192_100K  
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.68 Note  
RESPONSE: Disordered structure.
;
_vrf_PLAT029_nt0805_LHG192_100K  
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.970 Why?  
RESPONSE: 11 reflections are missing because of overflow.
;
_vrf_PLAT911_nt0805_LHG192_100K  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.598         36 Report
RESPONSE: 11 reflections are missing because of overflow, the rest is missing
in the lowest and highest resolution shells because of instrucment geometry 
limitations.
;
_vrf_PLAT913_nt0805_LHG192_100K  
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....         11 Note  
RESPONSE: These reflections are missing because of overflow.
;
####################################################################### 
# 
# 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_nt0325_LH104
_database_code_depnum_ccdc_archive 'CCDC 2061856'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        
; phenyl 6-chloro-5-[2-chloro-6-(phenoxycarbonyl)phenyl]-5H-
benzo[b]phosphindole-1-carboxylate
;
_chemical_name_common            
; phenyl 6-chloro-5-[2-chloro-6-(phenoxycarbonyl)phenyl]-5H-
benzo[b]phosphindole-1-carboxylate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H19 Cl2 O4 P'
_chemical_formula_sum            'C32 H19 Cl2 O4 P'
_chemical_formula_weight         569.34

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'
Cl Cl 0.1484 0.1585 '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'

_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                   8.7704(4)
_cell_length_b                   9.6774(3)
_cell_length_c                   16.3912(4)
_cell_angle_alpha                106.886(3)
_cell_angle_beta                 96.369(3)
_cell_angle_gamma                92.054(3)
_cell_volume                     1319.60(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    5157
_cell_measurement_theta_min      2.6170
_cell_measurement_theta_max      30.1780

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_F_000             584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.046
_exptl_absorpt_coefficient_mu    0.345
_shelx_estimated_absorpt_T_min   0.841
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_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            12095
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.205
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5383
_reflns_number_gt                4209
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0463P)²+0.1892P] 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         5383
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.1020
_refine_ls_wR_factor_gt          0.0926
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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
Cl1 Cl 1.04008(7) 0.48284(7) 0.19230(4) 0.07222(18) Uani 1 1 d . . . . .
Cl2 Cl 0.90997(6) 0.36738(6) 0.40623(3) 0.05836(16) Uani 1 1 d . . . . .
P1 P 0.68800(6) 0.45579(5) 0.24469(3) 0.04388(14) Uani 1 1 d . . . . .
O1 O 0.56317(19) 0.84163(14) 0.60719(8) 0.0615(4) Uani 1 1 d . . . . .
O2 O 0.65966(17) 0.95273(14) 0.51993(8) 0.0551(3) Uani 1 1 d . . . . .
O3 O 0.6125(2) 0.1574(2) 0.02641(10) 0.0991(6) Uani 1 1 d . . . . .
O4 O 0.45290(17) 0.22732(15) 0.12625(8) 0.0588(4) Uani 1 1 d . . . . .
C1 C 0.5002(3) 1.0773(2) 0.68890(14) 0.0686(6) Uani 1 1 d . . . . .
H1 H 0.417726 1.074113 0.647349 0.082 Uiso 1 1 calc R U . . .
C2 C 0.5280(4) 1.1937(3) 0.76252(16) 0.0813(8) Uani 1 1 d . . . . .
H2 H 0.463412 1.269417 0.770785 0.098 Uiso 1 1 calc R U . . .
C3 C 0.6494(4) 1.1984(3) 0.82310(15) 0.0855(9) Uani 1 1 d . . . . .
H3 H 0.667259 1.276467 0.872822 0.103 Uiso 1 1 calc R U . . .
C4 C 0.7442(4) 1.0879(3) 0.81021(16) 0.0900(9) Uani 1 1 d . . . . .
H4 H 0.828005 1.091670 0.851093 0.108 Uiso 1 1 calc R U . . .
C5 C 0.7181(3) 0.9710(2) 0.73770(15) 0.0734(7) Uani 1 1 d . . . . .
H5 H 0.782933 0.895511 0.729392 0.088 Uiso 1 1 calc R U . . .
C6 C 0.5959(3) 0.9674(2) 0.67837(12) 0.0532(5) Uani 1 1 d . . . . .
C7 C 0.6004(2) 0.84636(19) 0.53013(11) 0.0445(4) Uani 1 1 d . . . . .
C8 C 0.5533(2) 0.70599(18) 0.46294(11) 0.0422(4) Uani 1 1 d . . . . .
C9 C 0.4113(2) 0.6400(2) 0.46562(13) 0.0516(5) Uani 1 1 d . . . . .
H9 H 0.356062 0.680655 0.510909 0.062 Uiso 1 1 calc R U . . .
C10 C 0.3501(2) 0.5155(2) 0.40278(13) 0.0544(5) Uani 1 1 d . . . . .
H10 H 0.254828 0.473603 0.406140 0.065 Uiso 1 1 calc R U . . .
C11 C 0.4301(2) 0.4537(2) 0.33526(12) 0.0492(5) Uani 1 1 d . . . . .
H11 H 0.387956 0.371647 0.291906 0.059 Uiso 1 1 calc R U . . .
C12 C 0.5743(2) 0.51502(18) 0.33249(11) 0.0414(4) Uani 1 1 d . . . . .
C13 C 0.8416(2) 0.58670(18) 0.30577(11) 0.0424(4) Uani 1 1 d . . . . .
C14 C 0.9861(2) 0.6064(2) 0.28285(12) 0.0483(5) Uani 1 1 d . . . . .
C15 C 1.0902(2) 0.7167(2) 0.33264(14) 0.0556(5) Uani 1 1 d . . . . .
H15 H 1.186895 0.729508 0.316541 0.067 Uiso 1 1 calc R U . . .
C16 C 1.0475(2) 0.8078(2) 0.40695(14) 0.0577(5) Uani 1 1 d . . . . .
H16 H 1.117449 0.881541 0.441695 0.069 Uiso 1 1 calc R U . . .
C17 C 0.9035(2) 0.7924(2) 0.43106(13) 0.0505(5) Uani 1 1 d . . . . .
H17 H 0.877613 0.855821 0.481317 0.061 Uiso 1 1 calc R U . . .
C18 C 0.7966(2) 0.68221(18) 0.38058(11) 0.0403(4) Uani 1 1 d . . . . .
C19 C 0.6403(2) 0.64177(17) 0.39601(10) 0.0394(4) Uani 1 1 d . . . . .
C20 C 0.7454(2) 0.27463(19) 0.24551(11) 0.0433(4) Uani 1 1 d . . . . .
C21 C 0.8402(2) 0.2385(2) 0.30952(11) 0.0481(4) Uani 1 1 d . . . . .
C22 C 0.8832(3) 0.0991(2) 0.29999(14) 0.0666(6) Uani 1 1 d . . . . .
H22 H 0.946185 0.078561 0.343869 0.080 Uiso 1 1 calc R U . . .
C23 C 0.8327(3) -0.0083(2) 0.22577(17) 0.0812(8) Uani 1 1 d . . . . .
H23 H 0.861677 -0.102044 0.219254 0.097 Uiso 1 1 calc R U . . .
C24 C 0.7394(3) 0.0213(2) 0.16077(15) 0.0717(7) Uani 1 1 d . . . . .
H24 H 0.706537 -0.051984 0.110129 0.086 Uiso 1 1 calc R U . . .
C25 C 0.6943(2) 0.1604(2) 0.17075(12) 0.0513(5) Uani 1 1 d . . . . .
C26 C 0.5870(3) 0.1822(2) 0.09893(12) 0.0586(5) Uani 1 1 d . . . . .
C27 C 0.3352(3) 0.2569(2) 0.06892(12) 0.0555(5) Uani 1 1 d . . . . .
C28 C 0.1929(3) 0.1900(2) 0.06300(14) 0.0651(6) Uani 1 1 d . . . . .
H28 H 0.178322 0.123109 0.092754 0.078 Uiso 1 1 calc R U . . .
C29 C 0.0704(3) 0.2225(3) 0.01241(15) 0.0742(7) Uani 1 1 d . . . . .
H29 H -0.027062 0.178072 0.008563 0.089 Uiso 1 1 calc R U . . .
C30 C 0.0927(3) 0.3198(3) -0.03184(15) 0.0780(7) Uani 1 1 d . . . . .
H30 H 0.010772 0.341027 -0.066233 0.094 Uiso 1 1 calc R U . . .
C31 C 0.2349(4) 0.3855(3) -0.02552(17) 0.0866(8) Uani 1 1 d . . . . .
H31 H 0.249473 0.451651 -0.055756 0.104 Uiso 1 1 calc R U . . .
C32 C 0.3593(3) 0.3550(3) 0.02567(16) 0.0778(7) Uani 1 1 d . . . . .
H32 H 0.456352 0.400579 0.030201 0.093 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
Cl1 C14 1.7381(19) . ?
Cl2 C21 1.7389(19) . ?
P1 C13 1.8066(18) . ?
P1 C12 1.8095(19) . ?
P1 C20 1.8445(18) . ?
O1 C7 1.352(2) . ?
O1 C6 1.415(2) . ?
O2 C7 1.199(2) . ?
O3 C26 1.191(2) . ?
O4 C26 1.347(3) . ?
O4 C27 1.412(2) . ?
C1 C6 1.362(3) . ?
C1 C2 1.382(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.361(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.357(3) . ?
C5 H5 0.9300 . ?
C7 C8 1.489(2) . ?
C8 C9 1.390(3) . ?
C8 C19 1.412(2) . ?
C9 C10 1.382(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.376(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.389(3) . ?
C11 H11 0.9300 . ?
C12 C19 1.413(2) . ?
C13 C14 1.384(3) . ?
C13 C18 1.410(2) . ?
C14 C15 1.378(3) . ?
C15 C16 1.379(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.394(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.481(2) . ?
C20 C21 1.398(3) . ?
C20 C25 1.407(2) . ?
C21 C22 1.383(3) . ?
C22 C23 1.368(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.374(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.386(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.493(3) . ?
C27 C32 1.363(3) . ?
C27 C28 1.366(3) . ?
C28 C29 1.385(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.366(3) . ?
C29 H29 0.9300 . ?
C30 C31 1.359(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.394(4) . ?
C31 H31 0.9300 . ?
C32 H32 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 C12 89.29(8) . . ?
C13 P1 C20 107.84(8) . . ?
C12 P1 C20 105.80(8) . . ?
C7 O1 C6 118.41(14) . . ?
C26 O4 C27 120.22(15) . . ?
C6 C1 C2 118.7(2) . . ?
C6 C1 H1 120.6 . . ?
C2 C1 H1 120.6 . . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 119.4(2) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.9(2) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 118.9(2) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C1 121.5(2) . . ?
C5 C6 O1 118.4(2) . . ?
C1 C6 O1 120.0(2) . . ?
O2 C7 O1 122.60(16) . . ?
O2 C7 C8 126.76(16) . . ?
O1 C7 C8 110.62(15) . . ?
C9 C8 C19 119.34(16) . . ?
C9 C8 C7 116.57(17) . . ?
C19 C8 C7 124.02(16) . . ?
C10 C9 C8 121.77(19) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C11 C10 C9 120.01(18) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 119.34(17) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C19 121.93(17) . . ?
C11 C12 P1 124.93(14) . . ?
C19 C12 P1 112.85(13) . . ?
C14 C13 C18 120.16(16) . . ?
C14 C13 P1 127.00(14) . . ?
C18 C13 P1 112.64(13) . . ?
C15 C14 C13 121.41(18) . . ?
C15 C14 Cl1 119.63(16) . . ?
C13 C14 Cl1 118.87(15) . . ?
C14 C15 C16 118.36(19) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
C15 C16 C17 121.67(19) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C16 C17 C18 120.44(18) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C13 117.92(17) . . ?
C17 C18 C19 129.47(16) . . ?
C13 C18 C19 112.48(15) . . ?
C8 C19 C12 117.53(16) . . ?
C8 C19 C18 130.82(15) . . ?
C12 C19 C18 111.63(15) . . ?
C21 C20 C25 116.12(17) . . ?
C21 C20 P1 127.77(14) . . ?
C25 C20 P1 116.00(13) . . ?
C22 C21 C20 122.24(18) . . ?
C22 C21 Cl2 116.27(15) . . ?
C20 C21 Cl2 121.49(15) . . ?
C23 C22 C21 119.7(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
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 . . ?
C24 C25 C20 121.55(19) . . ?
C24 C25 C26 116.66(18) . . ?
C20 C25 C26 121.79(17) . . ?
O3 C26 O4 124.0(2) . . ?
O3 C26 C25 125.2(2) . . ?
O4 C26 C25 110.70(17) . . ?
C32 C27 C28 121.2(2) . . ?
C32 C27 O4 121.7(2) . . ?
C28 C27 O4 116.92(18) . . ?
C27 C28 C29 119.6(2) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C30 C29 C28 120.0(2) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C31 C30 C29 119.9(2) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 120.9(2) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 H31 119.5 . . ?
C27 C32 C31 118.4(2) . . ?
C27 C32 H32 120.8 . . ?
C31 C32 H32 120.8 . . ?

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
C6 C1 C2 C3 0.3(4) . . . . ?
C1 C2 C3 C4 0.6(4) . . . . ?
C2 C3 C4 C5 -0.9(4) . . . . ?
C3 C4 C5 C6 0.4(4) . . . . ?
C4 C5 C6 C1 0.6(4) . . . . ?
C4 C5 C6 O1 -175.3(2) . . . . ?
C2 C1 C6 C5 -0.9(4) . . . . ?
C2 C1 C6 O1 174.9(2) . . . . ?
C7 O1 C6 C5 -104.3(2) . . . . ?
C7 O1 C6 C1 79.8(3) . . . . ?
C6 O1 C7 O2 -0.1(3) . . . . ?
C6 O1 C7 C8 -178.38(17) . . . . ?
O2 C7 C8 C9 -137.3(2) . . . . ?
O1 C7 C8 C9 40.9(2) . . . . ?
O2 C7 C8 C19 39.7(3) . . . . ?
O1 C7 C8 C19 -142.11(17) . . . . ?
C19 C8 C9 C10 -2.3(3) . . . . ?
C7 C8 C9 C10 174.81(17) . . . . ?
C8 C9 C10 C11 0.0(3) . . . . ?
C9 C10 C11 C12 2.0(3) . . . . ?
C10 C11 C12 C19 -1.7(3) . . . . ?
C10 C11 C12 P1 -175.11(14) . . . . ?
C13 P1 C12 C11 -176.27(16) . . . . ?
C20 P1 C12 C11 -67.92(17) . . . . ?
C13 P1 C12 C19 9.75(13) . . . . ?
C20 P1 C12 C19 118.10(13) . . . . ?
C12 P1 C13 C14 176.08(17) . . . . ?
C20 P1 C13 C14 69.70(17) . . . . ?
C12 P1 C13 C18 -9.13(13) . . . . ?
C20 P1 C13 C18 -115.51(13) . . . . ?
C18 C13 C14 C15 1.2(3) . . . . ?
P1 C13 C14 C15 175.68(14) . . . . ?
C18 C13 C14 Cl1 177.77(13) . . . . ?
P1 C13 C14 Cl1 -7.8(2) . . . . ?
C13 C14 C15 C16 0.4(3) . . . . ?
Cl1 C14 C15 C16 -176.09(15) . . . . ?
C14 C15 C16 C17 -1.3(3) . . . . ?
C15 C16 C17 C18 0.5(3) . . . . ?
C16 C17 C18 C13 1.2(3) . . . . ?
C16 C17 C18 C19 176.81(18) . . . . ?
C14 C13 C18 C17 -2.0(3) . . . . ?
P1 C13 C18 C17 -177.20(13) . . . . ?
C14 C13 C18 C19 -178.36(15) . . . . ?
P1 C13 C18 C19 6.45(18) . . . . ?
C9 C8 C19 C12 2.5(2) . . . . ?
C7 C8 C19 C12 -174.36(16) . . . . ?
C9 C8 C19 C18 -175.53(17) . . . . ?
C7 C8 C19 C18 7.6(3) . . . . ?
C11 C12 C19 C8 -0.6(2) . . . . ?
P1 C12 C19 C8 173.58(12) . . . . ?
C11 C12 C19 C18 177.81(16) . . . . ?
P1 C12 C19 C18 -8.01(18) . . . . ?
C17 C18 C19 C8 3.3(3) . . . . ?
C13 C18 C19 C8 179.14(17) . . . . ?
C17 C18 C19 C12 -174.82(17) . . . . ?
C13 C18 C19 C12 1.0(2) . . . . ?
C13 P1 C20 C21 29.88(19) . . . . ?
C12 P1 C20 C21 -64.56(18) . . . . ?
C13 P1 C20 C25 -146.34(15) . . . . ?
C12 P1 C20 C25 119.22(15) . . . . ?
C25 C20 C21 C22 0.7(3) . . . . ?
P1 C20 C21 C22 -175.56(17) . . . . ?
C25 C20 C21 Cl2 -178.97(15) . . . . ?
P1 C20 C21 Cl2 4.8(3) . . . . ?
C20 C21 C22 C23 0.2(4) . . . . ?
Cl2 C21 C22 C23 179.9(2) . . . . ?
C21 C22 C23 C24 -0.1(4) . . . . ?
C22 C23 C24 C25 -0.9(4) . . . . ?
C23 C24 C25 C20 1.8(4) . . . . ?
C23 C24 C25 C26 -177.2(2) . . . . ?
C21 C20 C25 C24 -1.7(3) . . . . ?
P1 C20 C25 C24 175.01(18) . . . . ?
C21 C20 C25 C26 177.30(18) . . . . ?
P1 C20 C25 C26 -6.0(3) . . . . ?
C27 O4 C26 O3 -4.0(3) . . . . ?
C27 O4 C26 C25 179.01(16) . . . . ?
C24 C25 C26 O3 -58.7(3) . . . . ?
C20 C25 C26 O3 122.3(3) . . . . ?
C24 C25 C26 O4 118.2(2) . . . . ?
C20 C25 C26 O4 -60.8(3) . . . . ?
C26 O4 C27 C32 -56.9(3) . . . . ?
C26 O4 C27 C28 127.4(2) . . . . ?
C32 C27 C28 C29 -0.2(3) . . . . ?
O4 C27 C28 C29 175.5(2) . . . . ?
C27 C28 C29 C30 0.7(3) . . . . ?
C28 C29 C30 C31 -0.6(4) . . . . ?
C29 C30 C31 C32 0.0(4) . . . . ?
C28 C27 C32 C31 -0.3(4) . . . . ?
O4 C27 C32 C31 -175.9(2) . . . . ?
C30 C31 C32 C27 0.4(4) . . . . ?

_refine_diff_density_max         0.331
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.036



# start Validation Reply Form
_vrf_PLAT331_nt0325_LH104        
;
PROBLEM: Small Average Phenyl C-C Dist C1       -C6             1.37 Ang.  
RESPONSE: The average ring distance is smaller due to large thermal motion 
of the fragment
;
####################################################################### 
# 
# 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_nt0401_LH139
_database_code_depnum_ccdc_archive 'CCDC 2061854'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
(2-bromo-3-chlorophenyl)bis(2-bromo-6-chlorophenyl)phosphane
_chemical_name_common            
(2-bromo-3-chlorophenyl)bis(2-bromo-6-chlorophenyl)phosphane
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H9 Br3 Cl3 P'
_chemical_formula_sum            'C18 H9 Br3 Cl3 P'
_chemical_formula_weight         602.27

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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   31.4777(8)
_cell_length_b                   8.5972(2)
_cell_length_c                   14.8825(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.161(3)
_cell_angle_gamma                90
_cell_volume                     4016.89(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3786
_cell_measurement_theta_min      4.2320
_cell_measurement_theta_max      62.4940

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_F_000             2304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.012
_exptl_absorpt_coefficient_mu    11.875
_shelx_estimated_absorpt_T_min   0.355
_shelx_estimated_absorpt_T_max   0.871
_exptl_absorpt_correction_T_min  0.373
_exptl_absorpt_correction_T_max  0.863
_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            12995
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.815
_diffrn_reflns_theta_max         62.620
_diffrn_reflns_theta_full        62.620
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             6263
_reflns_number_gt                4873
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0392P)²+3.6151P] 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         6263
_refine_ls_number_parameters     527
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.1032
_refine_ls_wR_factor_gt          0.0939
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.084
_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
C1 C 0.17874(16) 0.9004(6) 0.3724(3) 0.0389(12) Uani 1 1 d . . . . .
P1 P 0.12597(4) 0.99443(15) 0.37324(8) 0.0368(3) Uani 1 1 d . . . . .
Cl1A Cl 0.1555(4) 0.5985(11) 0.4028(11) 0.072(3) Uani 0.784(4) 1 d D . P A 1
Br1A Br 0.20311(18) 1.21945(19) 0.3569(3) 0.0543(7) Uani 0.784(4) 1 d D U P A 1
Cl1B Cl 0.2052(16) 1.1996(15) 0.371(3) 0.053(3) Uani 0.216(4) 1 d D U P A 2
Br1B Br 0.1502(5) 0.5837(17) 0.3882(16) 0.059(2) Uani 0.216(4) 1 d D . P A 2
C2 C 0.18986(16) 0.7421(6) 0.3726(4) 0.0527(14) Uani 1 1 d D . . . .
Cl2A Cl 0.1750(5) 0.8761(11) 0.5765(10) 0.0673(18) Uani 0.827(4) 1 d D . P B 1
Br2A Br 0.07407(14) 1.3083(5) 0.38041(17) 0.0632(6) Uani 0.827(4) 1 d D U P B 1
Cl2B Cl 0.0744(15) 1.321(5) 0.398(2) 0.059(4) Uani 0.173(4) 1 d D U P B 2
Br2B Br 0.1721(11) 0.850(2) 0.581(2) 0.070(5) Uani 0.173(4) 1 d D . P B 2
P2 P 0.36247(4) 0.32062(16) 0.52270(9) 0.0420(3) Uani 1 1 d . . . . .
C3 C 0.2300(2) 0.6910(8) 0.3597(5) 0.0677(18) Uani 1 1 d . . . . .
H3 H 0.235874 0.584935 0.359805 0.081 Uiso 1 1 calc R U . . .
Cl3 Cl 0.01572(6) 0.5611(2) 0.21703(14) 0.0927(6) Uani 1 1 d D . . . .
Br3 Br 0.09645(2) 0.78786(9) 0.20091(4) 0.0709(2) Uani 1 1 d . . . . .
Br4A Br 0.3398(4) 0.7261(14) 0.5523(10) 0.073(3) Uani 0.245(4) 1 d D . P C 1
Cl4A Cl 0.2945(11) 0.1061(14) 0.585(2) 0.075(5) Uani 0.245(4) 1 d D U P C 1
Br4B Br 0.28973(16) 0.0850(3) 0.5696(3) 0.0782(10) Uani 0.755(4) 1 d D . P C 2
Cl4B Cl 0.3417(3) 0.7069(9) 0.5732(7) 0.0614(17) Uani 0.755(4) 1 d D . P C 2
Cl5A Cl 0.4510(3) 0.5723(13) 0.5594(5) 0.123(4) Uani 0.678(4) 1 d D . P D 1
Br5A Br 0.31049(8) 0.3677(4) 0.3396(3) 0.0551(8) Uani 0.678(4) 1 d D U P D 1
Cl5B Cl 0.3144(4) 0.394(2) 0.3303(14) 0.062(2) Uani 0.322(4) 1 d D U P D 2
Br5B Br 0.45263(16) 0.5759(6) 0.5663(3) 0.0506(11) Uani 0.322(4) 1 d D . P D 2
C4 C 0.2619(2) 0.7962(9) 0.3467(5) 0.077(2) Uani 1 1 d . . . . .
H4 H 0.289202 0.761229 0.337864 0.092 Uiso 1 1 calc R U . . .
C5 C 0.25334(18) 0.9529(8) 0.3466(4) 0.0603(16) Uani 1 1 d . . . . .
H5 H 0.274910 1.024626 0.338957 0.072 Uiso 1 1 calc R U . . .
Cl6 Cl 0.49655(5) 0.0541(2) 0.72206(11) 0.0765(5) Uani 1 1 d . . . . .
Br6 Br 0.44706(3) 0.10722(11) 0.52901(5) 0.0853(3) Uani 1 1 d . . . . .
C6 C 0.21243(16) 1.0026(5) 0.3579(3) 0.0434(12) Uani 1 1 d D . . . .
C7 C 0.12648(16) 1.0923(6) 0.4834(3) 0.0398(12) Uani 1 1 d . . . . .
C8 C 0.14555(16) 1.0440(6) 0.5662(4) 0.0505(14) Uani 1 1 d D . . . .
C9 C 0.1430(2) 1.1284(9) 0.6449(4) 0.0671(19) Uani 1 1 d . . . . .
H9 H 0.155534 1.091287 0.699190 0.081 Uiso 1 1 calc R U . . .
C10 C 0.1214(2) 1.2683(9) 0.6415(5) 0.074(2) Uani 1 1 d . . . . .
H10 H 0.119781 1.326486 0.693816 0.088 Uiso 1 1 calc R U . . .
C11 C 0.1026(2) 1.3221(8) 0.5624(5) 0.0666(18) Uani 1 1 d . . . . .
H11 H 0.088740 1.417737 0.560168 0.080 Uiso 1 1 calc R U . . .
C12 C 0.10420(16) 1.2335(6) 0.4854(3) 0.0463(13) Uani 1 1 d D . . . .
C13 C 0.08366(15) 0.8515(6) 0.3844(3) 0.0394(12) Uani 1 1 d . . . . .
C14 C 0.06111(18) 0.8376(7) 0.4613(4) 0.0541(14) Uani 1 1 d . . . . .
H14 H 0.070271 0.891691 0.513232 0.065 Uiso 1 1 calc R U . . .
C15 C 0.0254(2) 0.7448(8) 0.4612(6) 0.074(2) Uani 1 1 d . . . . .
H15 H 0.010439 0.739190 0.512736 0.089 Uiso 1 1 calc R U . . .
C16 C 0.0116(2) 0.6601(8) 0.3861(6) 0.072(2) Uani 1 1 d . . . . .
H16 H -0.012028 0.595347 0.387442 0.087 Uiso 1 1 calc R U . . .
C17 C 0.03299(18) 0.6721(6) 0.3093(4) 0.0563(16) Uani 1 1 d D . . . .
C18 C 0.06803(17) 0.7685(6) 0.3081(4) 0.0457(13) Uani 1 1 d . . . . .
C19 C 0.31340(16) 0.4054(6) 0.5627(3) 0.0428(13) Uani 1 1 d . . . . .
C20 C 0.30294(16) 0.5634(6) 0.5751(4) 0.0527(14) Uani 1 1 d D . . . .
C21 C 0.2636(2) 0.6119(9) 0.5979(5) 0.0725(19) Uani 1 1 d . . . . .
H21 H 0.257786 0.717162 0.604487 0.087 Uiso 1 1 calc R U . . .
C22 C 0.2333(2) 0.5024(13) 0.6106(5) 0.088(3) Uani 1 1 d . . . . .
H22 H 0.206303 0.534537 0.624384 0.105 Uiso 1 1 calc R U . . .
C23 C 0.2415(2) 0.3462(11) 0.6037(5) 0.077(2) Uani 1 1 d . . . . .
H23 H 0.220760 0.273047 0.615101 0.093 Uiso 1 1 calc R U . . .
C24 C 0.28093(18) 0.3002(6) 0.5794(4) 0.0563(15) Uani 1 1 d D U . . .
C25 C 0.38300(17) 0.4718(7) 0.4491(4) 0.0477(13) Uani 1 1 d . . . . .
C26 C 0.36003(16) 0.4864(6) 0.3632(4) 0.0574(15) Uani 1 1 d D U . . .
C27 C 0.3729(2) 0.5810(9) 0.2973(5) 0.0703(19) Uani 1 1 d . . . . .
H27 H 0.356783 0.586758 0.242498 0.084 Uiso 1 1 calc R U . . .
C28 C 0.4090(2) 0.6673(9) 0.3101(5) 0.080(2) Uani 1 1 d . . . . .
H28 H 0.417644 0.730620 0.264144 0.096 Uiso 1 1 calc R U . . .
C29 C 0.4329(2) 0.6605(9) 0.3924(5) 0.0684(18) Uani 1 1 d . . . . .
H29 H 0.457445 0.720161 0.402272 0.082 Uiso 1 1 calc R U . . .
C30 C 0.41971(17) 0.5637(8) 0.4593(3) 0.0566(15) Uani 1 1 d D . . . .
C31 C 0.39552(16) 0.3081(7) 0.6292(3) 0.0444(13) Uani 1 1 d . . . . .
C32 C 0.38494(18) 0.3782(7) 0.7092(4) 0.0542(15) Uani 1 1 d . . . . .
H32 H 0.362018 0.446617 0.708019 0.065 Uiso 1 1 calc R U . . .
C33 C 0.40743(19) 0.3486(8) 0.7889(4) 0.0572(16) Uani 1 1 d . . . . .
H33 H 0.399430 0.395374 0.841437 0.069 Uiso 1 1 calc R U . . .
C34 C 0.44165(19) 0.2506(8) 0.7924(4) 0.0572(16) Uani 1 1 d . . . . .
H34 H 0.456995 0.231381 0.847011 0.069 Uiso 1 1 calc R U . . .
C35 C 0.45338(17) 0.1807(7) 0.7150(4) 0.0535(15) Uani 1 1 d . . . . .
C36 C 0.43025(17) 0.2055(7) 0.6343(3) 0.0470(13) 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
C1 C2 1.405(7) . ?
C1 C6 1.406(7) . ?
C1 P1 1.848(5) . ?
P1 C13 1.829(5) . ?
P1 C7 1.842(5) . ?
Cl1A C2 1.723(7) . ?
Br1A C6 1.887(5) . ?
Cl1B C6 1.722(9) . ?
Br1B C2 1.874(8) . ?
C2 C3 1.366(8) . ?
Cl2A C8 1.717(7) . ?
Br2A C12 1.881(5) . ?
Cl2B C12 1.721(9) . ?
Br2B C8 1.870(8) . ?
P2 C31 1.834(5) . ?
P2 C19 1.846(5) . ?
P2 C25 1.846(6) . ?
C3 C4 1.373(10) . ?
C3 H3 0.9300 . ?
Cl3 C17 1.728(5) . ?
Br3 C18 1.892(6) . ?
Br4A C20 1.863(8) . ?
Cl4A C24 1.723(9) . ?
Br4B C24 1.878(6) . ?
Cl4B C20 1.737(7) . ?
Cl5A C30 1.728(7) . ?
Br5A C26 1.875(6) . ?
Cl5B C26 1.680(8) . ?
Br5B C30 1.839(6) . ?
C4 C5 1.374(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(7) . ?
C5 H5 0.9300 . ?
Cl6 C35 1.738(6) . ?
Br6 C36 1.889(6) . ?
C7 C8 1.393(7) . ?
C7 C12 1.403(7) . ?
C8 C9 1.385(8) . ?
C9 C10 1.380(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.361(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(8) . ?
C11 H11 0.9300 . ?
C13 C14 1.394(7) . ?
C13 C18 1.400(7) . ?
C14 C15 1.378(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.378(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.372(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.380(8) . ?
C19 C24 1.401(8) . ?
C19 C20 1.413(7) . ?
C20 C21 1.371(8) . ?
C21 C22 1.364(11) . ?
C21 H21 0.9300 . ?
C22 C23 1.373(11) . ?
C22 H22 0.9300 . ?
C23 C24 1.377(9) . ?
C23 H23 0.9300 . ?
C25 C30 1.399(8) . ?
C25 C26 1.428(7) . ?
C26 C27 1.359(8) . ?
C27 C28 1.358(10) . ?
C27 H27 0.9300 . ?
C28 C29 1.391(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.384(8) . ?
C29 H29 0.9300 . ?
C31 C32 1.397(8) . ?
C31 C36 1.402(7) . ?
C32 C33 1.361(8) . ?
C32 H32 0.9300 . ?
C33 C34 1.365(8) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(8) . ?
C34 H34 0.9300 . ?
C35 C36 1.376(7) . ?

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
C2 C1 C6 114.5(4) . . ?
C2 C1 P1 130.4(4) . . ?
C6 C1 P1 114.6(4) . . ?
C13 P1 C7 100.7(2) . . ?
C13 P1 C1 111.6(2) . . ?
C7 P1 C1 104.8(2) . . ?
C3 C2 C1 123.0(5) . . ?
C3 C2 Cl1A 114.3(6) . . ?
C1 C2 Cl1A 122.3(6) . . ?
C3 C2 Br1B 114.6(7) . . ?
C1 C2 Br1B 122.4(7) . . ?
C31 P2 C19 100.4(2) . . ?
C31 P2 C25 110.7(2) . . ?
C19 P2 C25 104.5(2) . . ?
C2 C3 C4 120.0(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 120.1(6) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 119.2(6) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C1 123.2(5) . . ?
C5 C6 Cl1B 116.8(17) . . ?
C1 C6 Cl1B 119.4(17) . . ?
C5 C6 Br1A 116.8(5) . . ?
C1 C6 Br1A 120.0(4) . . ?
C8 C7 C12 115.0(4) . . ?
C8 C7 P1 128.7(4) . . ?
C12 C7 P1 116.2(4) . . ?
C9 C8 C7 122.9(5) . . ?
C9 C8 Cl2A 115.4(7) . . ?
C7 C8 Cl2A 121.7(6) . . ?
C9 C8 Br2B 114.8(11) . . ?
C7 C8 Br2B 122.0(11) . . ?
C10 C9 C8 119.0(6) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C11 C10 C9 120.7(6) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 119.4(6) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C7 122.9(5) . . ?
C11 C12 Cl2B 109.5(16) . . ?
C7 C12 Cl2B 127.5(16) . . ?
C11 C12 Br2A 117.0(5) . . ?
C7 C12 Br2A 120.1(4) . . ?
C14 C13 C18 116.9(5) . . ?
C14 C13 P1 123.4(4) . . ?
C18 C13 P1 119.0(4) . . ?
C15 C14 C13 120.9(6) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 121.1(6) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C17 C16 C15 119.4(6) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 119.8(5) . . ?
C16 C17 Cl3 118.4(5) . . ?
C18 C17 Cl3 121.8(5) . . ?
C17 C18 C13 122.0(5) . . ?
C17 C18 Br3 119.4(4) . . ?
C13 C18 Br3 118.6(4) . . ?
C24 C19 C20 114.7(5) . . ?
C24 C19 P2 116.1(4) . . ?
C20 C19 P2 129.1(4) . . ?
C21 C20 C19 123.2(5) . . ?
C21 C20 Cl4B 115.8(6) . . ?
C19 C20 Cl4B 120.7(5) . . ?
C21 C20 Br4A 113.7(7) . . ?
C19 C20 Br4A 122.9(6) . . ?
C22 C21 C20 118.6(7) . . ?
C22 C21 H21 120.7 . . ?
C20 C21 H21 120.7 . . ?
C21 C22 C23 121.9(7) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C24 118.6(7) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C23 C24 C19 123.0(6) . . ?
C23 C24 Cl4A 119.5(13) . . ?
C19 C24 Cl4A 116.9(13) . . ?
C23 C24 Br4B 116.4(5) . . ?
C19 C24 Br4B 120.6(5) . . ?
C30 C25 C26 114.1(5) . . ?
C30 C25 P2 130.9(4) . . ?
C26 C25 P2 114.6(4) . . ?
C27 C26 C25 122.7(5) . . ?
C27 C26 Cl5B 111.4(9) . . ?
C25 C26 Cl5B 125.9(9) . . ?
C27 C26 Br5A 118.6(5) . . ?
C25 C26 Br5A 118.7(4) . . ?
C28 C27 C26 121.1(6) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 119.6(7) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C30 C29 C28 119.1(6) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C29 C30 C25 123.4(5) . . ?
C29 C30 Cl5A 114.4(6) . . ?
C25 C30 Cl5A 122.2(5) . . ?
C29 C30 Br5B 114.2(5) . . ?
C25 C30 Br5B 122.3(5) . . ?
C32 C31 C36 117.3(5) . . ?
C32 C31 P2 123.8(4) . . ?
C36 C31 P2 118.3(4) . . ?
C33 C32 C31 121.4(6) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C32 C33 C34 120.5(6) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
C33 C34 C35 119.9(5) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C34 C35 C36 120.5(5) . . ?
C34 C35 Cl6 118.7(4) . . ?
C36 C35 Cl6 120.7(5) . . ?
C35 C36 C31 120.4(5) . . ?
C35 C36 Br6 119.5(4) . . ?
C31 C36 Br6 120.1(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
C2 C1 P1 C13 4.9(6) . . . . ?
C6 C1 P1 C13 176.0(4) . . . . ?
C2 C1 P1 C7 113.0(5) . . . . ?
C6 C1 P1 C7 -75.9(4) . . . . ?
C6 C1 C2 C3 -0.1(8) . . . . ?
P1 C1 C2 C3 170.9(5) . . . . ?
C6 C1 C2 Cl1A 171.8(8) . . . . ?
P1 C1 C2 Cl1A -17.2(10) . . . . ?
C6 C1 C2 Br1B -178.7(10) . . . . ?
P1 C1 C2 Br1B -7.6(12) . . . . ?
C1 C2 C3 C4 0.7(10) . . . . ?
Cl1A C2 C3 C4 -171.8(8) . . . . ?
Br1B C2 C3 C4 179.3(10) . . . . ?
C2 C3 C4 C5 0.0(11) . . . . ?
C3 C4 C5 C6 -1.3(10) . . . . ?
C4 C5 C6 C1 1.9(9) . . . . ?
C4 C5 C6 Cl1B 172.4(15) . . . . ?
C4 C5 C6 Br1A -179.9(5) . . . . ?
C2 C1 C6 C5 -1.2(8) . . . . ?
P1 C1 C6 C5 -173.7(4) . . . . ?
C2 C1 C6 Cl1B -171.4(16) . . . . ?
P1 C1 C6 Cl1B 16.1(16) . . . . ?
C2 C1 C6 Br1A -179.3(4) . . . . ?
P1 C1 C6 Br1A 8.2(6) . . . . ?
C13 P1 C7 C8 80.5(5) . . . . ?
C1 P1 C7 C8 -35.4(5) . . . . ?
C13 P1 C7 C12 -98.4(4) . . . . ?
C1 P1 C7 C12 145.7(4) . . . . ?
C12 C7 C8 C9 -0.1(8) . . . . ?
P1 C7 C8 C9 -179.0(5) . . . . ?
C12 C7 C8 Cl2A -178.7(9) . . . . ?
P1 C7 C8 Cl2A 2.4(11) . . . . ?
C12 C7 C8 Br2B 173.8(15) . . . . ?
P1 C7 C8 Br2B -5.1(16) . . . . ?
C7 C8 C9 C10 -1.5(9) . . . . ?
Cl2A C8 C9 C10 177.2(9) . . . . ?
Br2B C8 C9 C10 -175.9(15) . . . . ?
C8 C9 C10 C11 0.7(10) . . . . ?
C9 C10 C11 C12 1.6(10) . . . . ?
C10 C11 C12 C7 -3.4(9) . . . . ?
C10 C11 C12 Cl2B 175(2) . . . . ?
C10 C11 C12 Br2A 175.6(5) . . . . ?
C8 C7 C12 C11 2.6(8) . . . . ?
P1 C7 C12 C11 -178.3(5) . . . . ?
C8 C7 C12 Cl2B -176(2) . . . . ?
P1 C7 C12 Cl2B 3(3) . . . . ?
C8 C7 C12 Br2A -176.4(4) . . . . ?
P1 C7 C12 Br2A 2.6(6) . . . . ?
C7 P1 C13 C14 0.1(5) . . . . ?
C1 P1 C13 C14 110.9(5) . . . . ?
C7 P1 C13 C18 169.4(4) . . . . ?
C1 P1 C13 C18 -79.8(4) . . . . ?
C18 C13 C14 C15 0.6(8) . . . . ?
P1 C13 C14 C15 170.1(5) . . . . ?
C13 C14 C15 C16 1.6(10) . . . . ?
C14 C15 C16 C17 -2.0(10) . . . . ?
C15 C16 C17 C18 0.1(9) . . . . ?
C15 C16 C17 Cl3 178.5(5) . . . . ?
C16 C17 C18 C13 2.3(8) . . . . ?
Cl3 C17 C18 C13 -176.1(4) . . . . ?
C16 C17 C18 Br3 -178.5(4) . . . . ?
Cl3 C17 C18 Br3 3.1(6) . . . . ?
C14 C13 C18 C17 -2.6(8) . . . . ?
P1 C13 C18 C17 -172.5(4) . . . . ?
C14 C13 C18 Br3 178.2(4) . . . . ?
P1 C13 C18 Br3 8.3(6) . . . . ?
C31 P2 C19 C24 -96.8(4) . . . . ?
C25 P2 C19 C24 148.5(4) . . . . ?
C31 P2 C19 C20 86.5(5) . . . . ?
C25 P2 C19 C20 -28.2(5) . . . . ?
C24 C19 C20 C21 -2.7(8) . . . . ?
P2 C19 C20 C21 174.0(5) . . . . ?
C24 C19 C20 Cl4B 170.7(6) . . . . ?
P2 C19 C20 Cl4B -12.6(8) . . . . ?
C24 C19 C20 Br4A -177.2(7) . . . . ?
P2 C19 C20 Br4A -0.5(9) . . . . ?
C19 C20 C21 C22 1.1(10) . . . . ?
Cl4B C20 C21 C22 -172.6(7) . . . . ?
Br4A C20 C21 C22 176.0(7) . . . . ?
C20 C21 C22 C23 1.8(11) . . . . ?
C21 C22 C23 C24 -2.8(11) . . . . ?
C22 C23 C24 C19 0.9(10) . . . . ?
C22 C23 C24 Cl4A 171.3(14) . . . . ?
C22 C23 C24 Br4B -179.1(6) . . . . ?
C20 C19 C24 C23 1.7(8) . . . . ?
P2 C19 C24 C23 -175.5(5) . . . . ?
C20 C19 C24 Cl4A -168.9(13) . . . . ?
P2 C19 C24 Cl4A 13.9(13) . . . . ?
C20 C19 C24 Br4B -178.2(4) . . . . ?
P2 C19 C24 Br4B 4.6(6) . . . . ?
C31 P2 C25 C30 5.4(6) . . . . ?
C19 P2 C25 C30 112.7(6) . . . . ?
C31 P2 C25 C26 178.0(4) . . . . ?
C19 P2 C25 C26 -74.7(4) . . . . ?
C30 C25 C26 C27 0.2(8) . . . . ?
P2 C25 C26 C27 -173.7(5) . . . . ?
C30 C25 C26 Cl5B -178.9(9) . . . . ?
P2 C25 C26 Cl5B 7.2(10) . . . . ?
C30 C25 C26 Br5A 179.2(4) . . . . ?
P2 C25 C26 Br5A 5.3(6) . . . . ?
C25 C26 C27 C28 0.2(10) . . . . ?
Cl5B C26 C27 C28 179.5(9) . . . . ?
Br5A C26 C27 C28 -178.8(6) . . . . ?
C26 C27 C28 C29 -0.8(11) . . . . ?
C27 C28 C29 C30 0.9(11) . . . . ?
C28 C29 C30 C25 -0.5(10) . . . . ?
C28 C29 C30 Cl5A -177.5(7) . . . . ?
C28 C29 C30 Br5B -176.5(6) . . . . ?
C26 C25 C30 C29 -0.1(9) . . . . ?
P2 C25 C30 C29 172.5(5) . . . . ?
C26 C25 C30 Cl5A 176.7(6) . . . . ?
P2 C25 C30 Cl5A -10.7(9) . . . . ?
C26 C25 C30 Br5B 175.6(5) . . . . ?
P2 C25 C30 Br5B -11.8(8) . . . . ?
C19 P2 C31 C32 -10.9(5) . . . . ?
C25 P2 C31 C32 99.0(5) . . . . ?
C19 P2 C31 C36 159.9(4) . . . . ?
C25 P2 C31 C36 -90.2(5) . . . . ?
C36 C31 C32 C33 0.2(8) . . . . ?
P2 C31 C32 C33 171.1(5) . . . . ?
C31 C32 C33 C34 1.1(9) . . . . ?
C32 C33 C34 C35 -0.4(9) . . . . ?
C33 C34 C35 C36 -1.6(9) . . . . ?
C33 C34 C35 Cl6 -178.9(5) . . . . ?
C34 C35 C36 C31 2.9(9) . . . . ?
Cl6 C35 C36 C31 -179.9(4) . . . . ?
C34 C35 C36 Br6 -179.8(5) . . . . ?
Cl6 C35 C36 Br6 -2.6(7) . . . . ?
C32 C31 C36 C35 -2.1(8) . . . . ?
P2 C31 C36 C35 -173.5(4) . . . . ?
C32 C31 C36 Br6 -179.4(4) . . . . ?
P2 C31 C36 Br6 9.2(6) . . . . ?

_refine_diff_density_max         0.965
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.080



# start Validation Reply Form
_vrf_THETM01_nt0401_LH139        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.590
RESPONSE: Very small and weakly diffracting crystal, resolution in the data
collection strategy was limited to 0.90 \%A.
;
_vrf_PLAT029_nt0401_LH139        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.975 Why?  
RESPONSE: Very small and weakly diffracting crystal, resolution in the data
collection strategy was limited to 0.90 \%A.
;
_vrf_PLAT230_nt0401_LH139        
;
PROBLEM: Hirshfeld Test Diff for    C26      --C27      .        5.5 s.u.  
RESPONSE: Disorderd structure.
;
_vrf_PLAT242_nt0401_LH139        
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C30 Check 
RESPONSE: Disorderd structure.
;
_vrf_PLAT341_nt0401_LH139        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00872 Ang.  
RESPONSE: Disorderd structure.
;
_vrf_PLAT434_nt0401_LH139        
;
PROBLEM: Short Inter HL..HL Contact Br3      ..Br2B             3.30 Ang.  
RESPONSE: Disorderd structure.
;
_vrf_PLAT911_nt0401_LH139        
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.576        161 Report
RESPONSE: Very small and weakly diffracting crystal, resolution in the data
collection strategy was limited to 0.90 \%A.
;
####################################################################### 
# 
# 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_test23_Lie91_lowres
_database_code_depnum_ccdc_archive 'CCDC 2061855'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
(2,3-dibromophenyl)bis(2,6-dibromophenyl)phosphane
_chemical_name_common            
(2,3-dibromophenyl)bis(2,6-dibromophenyl)phosphane
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H9 Br6 P'
_chemical_formula_sum            'C18 H9 Br6 P'
_chemical_formula_weight         735.68

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'
Br Br -0.6763 1.2805 '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                   7.4004(9)
_cell_length_b                   8.9219(12)
_cell_length_c                   15.889(3)
_cell_angle_alpha                78.126(13)
_cell_angle_beta                 82.433(12)
_cell_angle_gamma                81.201(11)
_cell_volume                     1009.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1068
_cell_measurement_theta_min      5.3480
_cell_measurement_theta_max      40.7270

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_F_000             684
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.021
_exptl_absorpt_coefficient_mu    15.123
_shelx_estimated_absorpt_T_min   0.059
_shelx_estimated_absorpt_T_max   0.742
_exptl_absorpt_correction_T_min  0.153
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      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            2316
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.857
_diffrn_reflns_theta_max         40.794
_diffrn_reflns_theta_full        40.794
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.964
_reflns_number_total             2316
_reflns_number_gt                1816
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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 1.171.40.82a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.1624P)²+3.0830P] 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         2316
_refine_ls_number_parameters     227
_refine_ls_number_restraints     171
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0735
_refine_ls_wR_factor_ref         0.2272
_refine_ls_wR_factor_gt          0.2115
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.056
_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
Br1 Br 0.0277(4) 0.5205(3) 0.1893(2) 0.0404(14) Uani 1 1 d . . . . .
Br2 Br 0.1166(4) 0.8011(4) 0.0174(2) 0.0458(14) Uani 1 1 d . . . . .
Br3 Br 0.7583(4) 0.2981(4) 0.3534(2) 0.0409(13) Uani 1 1 d . . . . .
Br4 Br 0.3742(4) 0.0014(3) 0.1520(2) 0.0392(14) Uani 1 1 d . . . . .
Br5 Br 0.3728(5) 0.6483(3) 0.3143(2) 0.0445(14) Uani 1 1 d . . . . .
Br6 Br 0.2953(4) -0.0055(3) 0.4163(2) 0.0405(13) Uani 1 1 d . . . . .
P1 P 0.3544(10) 0.2693(8) 0.2592(5) 0.031(2) Uani 1 1 d . . . . .
C1 C 0.414(4) 0.437(3) 0.1751(18) 0.031(7) Uani 1 1 d . . . . .
C2 C 0.593(4) 0.453(3) 0.1403(17) 0.028(7) Uani 1 1 d . . . . .
H2 H 0.692156 0.381959 0.162734 0.033 Uiso 1 1 calc R U . . .
C3 C 0.629(4) 0.578(3) 0.0703(17) 0.032(7) Uani 1 1 d . . . . .
H3 H 0.751451 0.590588 0.046207 0.038 Uiso 1 1 calc R U . . .
C4 C 0.484(4) 0.680(3) 0.0385(19) 0.036(8) Uani 1 1 d . . . . .
H4 H 0.506361 0.765836 -0.005923 0.043 Uiso 1 1 calc R U . . .
C5 C 0.310(4) 0.657(3) 0.0700(19) 0.032(7) Uani 1 1 d . . . . .
C6 C 0.270(4) 0.540(3) 0.1397(19) 0.034(7) Uani 1 1 d . . . . .
C7 C 0.572(4) 0.143(3) 0.2528(17) 0.029(6) Uani 1 1 d . . . . .
C8 C 0.734(4) 0.147(3) 0.2885(17) 0.026(7) Uani 1 1 d . . . . .
C9 C 0.891(4) 0.045(3) 0.277(2) 0.042(8) Uani 1 1 d . . . . .
H9 H 0.999275 0.054787 0.300859 0.051 Uiso 1 1 calc R U . . .
C10 C 0.891(4) -0.072(3) 0.2304(19) 0.034(7) Uani 1 1 d . . . . .
H10 H 0.998084 -0.144612 0.223598 0.040 Uiso 1 1 calc R U . . .
C11 C 0.734(4) -0.081(3) 0.1945(19) 0.034(7) Uani 1 1 d . . . . .
H11 H 0.731935 -0.157632 0.161334 0.041 Uiso 1 1 calc R U . . .
C12 C 0.579(4) 0.024(3) 0.2075(18) 0.030(7) Uani 1 1 d . . . . .
C13 C 0.325(4) 0.320(3) 0.3670(18) 0.030(7) Uani 1 1 d . . . . .
C14 C 0.308(4) 0.466(3) 0.3907(19) 0.034(7) Uani 1 1 d . . . . .
C15 C 0.257(4) 0.485(4) 0.476(2) 0.046(8) Uani 1 1 d . . . . .
H15 H 0.247240 0.584873 0.490358 0.056 Uiso 1 1 calc R U . . .
C16 C 0.220(4) 0.362(4) 0.538(2) 0.048(8) Uani 1 1 d . . . . .
H16 H 0.188384 0.376258 0.596295 0.057 Uiso 1 1 calc R U . . .
C17 C 0.228(4) 0.218(3) 0.5207(19) 0.036(7) Uani 1 1 d . . . . .
H17 H 0.199695 0.133554 0.564978 0.043 Uiso 1 1 calc R U . . .
C18 C 0.281(3) 0.199(3) 0.4345(19) 0.026(7) 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
Br1 C6 1.88(3) . ?
Br2 C5 1.93(3) . ?
Br3 C8 1.90(3) . ?
Br4 C12 1.90(3) . ?
Br5 C14 1.91(3) . ?
Br6 C18 1.89(3) . ?
P1 C7 1.82(3) . ?
P1 C13 1.84(3) . ?
P1 C1 1.86(3) . ?
C1 C2 1.38(3) . ?
C1 C6 1.40(4) . ?
C2 C3 1.43(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.37(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.35(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.39(4) . ?
C7 C12 1.39(4) . ?
C7 C8 1.40(4) . ?
C8 C9 1.38(4) . ?
C9 C10 1.40(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.38(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.39(4) . ?
C11 H11 0.9500 . ?
C13 C14 1.41(3) . ?
C13 C18 1.40(4) . ?
C14 C15 1.40(4) . ?
C15 C16 1.36(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.36(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.41(4) . ?
C17 H17 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
C7 P1 C13 106.1(13) . . ?
C7 P1 C1 99.5(12) . . ?
C13 P1 C1 110.3(13) . . ?
C2 C1 C6 120(3) . . ?
C2 C1 P1 123(2) . . ?
C6 C1 P1 118(2) . . ?
C1 C2 C3 120(3) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 119(3) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C4 C3 120(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 122(3) . . ?
C4 C5 Br2 117(2) . . ?
C6 C5 Br2 121(2) . . ?
C1 C6 C5 119(3) . . ?
C1 C6 Br1 119(2) . . ?
C5 C6 Br1 122(2) . . ?
C12 C7 C8 115(3) . . ?
C12 C7 P1 116(2) . . ?
C8 C7 P1 129(2) . . ?
C9 C8 C7 123(3) . . ?
C9 C8 Br3 114(2) . . ?
C7 C8 Br3 123(2) . . ?
C8 C9 C10 120(3) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 119(3) . . ?
C11 C10 H10 120.6 . . ?
C9 C10 H10 120.6 . . ?
C12 C11 C10 119(3) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C7 124(3) . . ?
C11 C12 Br4 115(2) . . ?
C7 C12 Br4 121(2) . . ?
C14 C13 C18 115(2) . . ?
C14 C13 P1 130(2) . . ?
C18 C13 P1 114(2) . . ?
C15 C14 C13 122(3) . . ?
C15 C14 Br5 114(2) . . ?
C13 C14 Br5 124(2) . . ?
C16 C15 C14 120(3) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C17 C16 C15 122(3) . . ?
C17 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
C16 C17 C18 118(3) . . ?
C16 C17 H17 121.1 . . ?
C18 C17 H17 121.1 . . ?
C13 C18 C17 123(3) . . ?
C13 C18 Br6 122(2) . . ?
C17 C18 Br6 115(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
C7 P1 C1 C2 -13(3) . . . . ?
C13 P1 C1 C2 98(2) . . . . ?
C7 P1 C1 C6 160(2) . . . . ?
C13 P1 C1 C6 -89(2) . . . . ?
C6 C1 C2 C3 2(4) . . . . ?
P1 C1 C2 C3 174(2) . . . . ?
C1 C2 C3 C4 0(4) . . . . ?
C2 C3 C4 C5 -3(4) . . . . ?
C3 C4 C5 C6 5(4) . . . . ?
C3 C4 C5 Br2 -177(2) . . . . ?
C2 C1 C6 C5 0(4) . . . . ?
P1 C1 C6 C5 -173(2) . . . . ?
C2 C1 C6 Br1 -178(2) . . . . ?
P1 C1 C6 Br1 9(3) . . . . ?
C4 C5 C6 C1 -4(4) . . . . ?
Br2 C5 C6 C1 179(2) . . . . ?
C4 C5 C6 Br1 175(2) . . . . ?
Br2 C5 C6 Br1 -2(3) . . . . ?
C13 P1 C7 C12 144(2) . . . . ?
C1 P1 C7 C12 -102(2) . . . . ?
C13 P1 C7 C8 -35(3) . . . . ?
C1 P1 C7 C8 79(3) . . . . ?
C12 C7 C8 C9 2(4) . . . . ?
P1 C7 C8 C9 -179(2) . . . . ?
C12 C7 C8 Br3 -179.9(19) . . . . ?
P1 C7 C8 Br3 -1(4) . . . . ?
C7 C8 C9 C10 -2(4) . . . . ?
Br3 C8 C9 C10 180(2) . . . . ?
C8 C9 C10 C11 2(4) . . . . ?
C9 C10 C11 C12 -2(4) . . . . ?
C10 C11 C12 C7 2(4) . . . . ?
C10 C11 C12 Br4 179(2) . . . . ?
C8 C7 C12 C11 -2(4) . . . . ?
P1 C7 C12 C11 178(2) . . . . ?
C8 C7 C12 Br4 -178.6(19) . . . . ?
P1 C7 C12 Br4 2(3) . . . . ?
C7 P1 C13 C14 120(3) . . . . ?
C1 P1 C13 C14 13(3) . . . . ?
C7 P1 C13 C18 -73(2) . . . . ?
C1 P1 C13 C18 -179.6(19) . . . . ?
C18 C13 C14 C15 2(4) . . . . ?
P1 C13 C14 C15 169(2) . . . . ?
C18 C13 C14 Br5 176(2) . . . . ?
P1 C13 C14 Br5 -17(4) . . . . ?
C13 C14 C15 C16 -1(5) . . . . ?
Br5 C14 C15 C16 -175(2) . . . . ?
C14 C15 C16 C17 -1(5) . . . . ?
C15 C16 C17 C18 2(4) . . . . ?
C14 C13 C18 C17 -2(4) . . . . ?
P1 C13 C18 C17 -171(2) . . . . ?
C14 C13 C18 Br6 -180.0(19) . . . . ?
P1 C13 C18 Br6 11(3) . . . . ?
C16 C17 C18 C13 0(4) . . . . ?
C16 C17 C18 Br6 178(2) . . . . ?

_refine_diff_density_max         1.023
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.229



# start Validation Reply Form
_vrf_THETM01_test23_Lie91_lowres 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: All obtained crystals of the compound were very thin plates that were 
very weakly diffracting even at 100 K. The lack of reflections also led to 
a number of additional problems (see below). In spite of this, all the non-H 
atoms could easily be located on the electron difference map, and the overall 
shape of the molecule as well as the packing of molecules can be considered 
to be reasonably determined.
;
_vrf_PLAT088_test23_Lie91_lowres 
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.54 Note  
RESPONSE: See above.
;
_vrf_PLAT341_test23_Lie91_lowres 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04056 Ang.  
RESPONSE: See above.
;
_vrf_PLAT029_test23_Lie91_lowres 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.964 Why?  
RESPONSE: See above.
;
_vrf_PLAT906_test23_Lie91_lowres 
;
PROBLEM: Large K Value in the Analysis of Variance ......      4.519 Check 
RESPONSE: See above.
;
_vrf_PLAT911_test23_Lie91_lowres 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.424         33 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_nt0808_LHG200B
_database_code_depnum_ccdc_archive 'CCDC 2061859'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'(acetylacetonato)-carbonylrhodium-9-phosphatriptycene complex'
_chemical_name_common            'Rh(acac)CO(9-phosphatriptycene) complex'
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H20 O3 P Rh'
_chemical_formula_sum            'C25 H20 O3 P Rh'
_chemical_formula_weight         502.29

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'
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'
Rh Rh 0.0927 3.6045 '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                   9.3940(2)
_cell_length_b                   15.7924(3)
_cell_length_c                   16.7012(4)
_cell_angle_alpha                65.676(2)
_cell_angle_beta                 80.915(2)
_cell_angle_gamma                76.193(2)
_cell_volume                     2187.53(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    14304
_cell_measurement_theta_min      2.8920
_cell_measurement_theta_max      67.0450

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.061
_exptl_absorpt_coefficient_mu    7.196
_shelx_estimated_absorpt_T_min   0.200
_shelx_estimated_absorpt_T_max   0.668
_exptl_absorpt_correction_T_min  0.258
_exptl_absorpt_correction_T_max  0.671
_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            21822
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.910
_diffrn_reflns_theta_max         67.147
_diffrn_reflns_theta_full        67.147
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             7739
_reflns_number_gt                7213
_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    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0323P)²+0.5656P] 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         7739
_refine_ls_number_parameters     545
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0632
_refine_ls_wR_factor_gt          0.0618
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Rh1 Rh 0.99780(2) 0.76223(2) 0.05587(2) 0.04329(6) Uani 1 1 d . . . . .
P1 P 0.92024(5) 0.62771(3) 0.13807(3) 0.03548(10) Uani 1 1 d . . . . .
O1 O 0.6933(2) 0.84826(16) 0.0068(2) 0.1118(11) Uani 1 1 d . . . . .
O2 O 1.06023(17) 0.88894(11) -0.02498(12) 0.0570(4) Uani 1 1 d . . . . .
O3 O 1.21125(16) 0.70415(11) 0.08076(11) 0.0530(4) Uani 1 1 d . . . . .
C1 C 0.7579(2) 0.62889(15) 0.21423(13) 0.0416(4) Uani 1 1 d . . . . .
C2 C 0.6835(3) 0.70650(19) 0.23252(17) 0.0581(6) Uani 1 1 d . . . . .
H2 H 0.719360 0.762537 0.208855 0.070 Uiso 1 1 calc R U . . .
C3 C 0.5551(3) 0.6998(2) 0.2864(2) 0.0779(9) Uani 1 1 d . . . . .
H3 H 0.505202 0.751259 0.299761 0.094 Uiso 1 1 calc R U . . .
C4 C 0.5010(3) 0.6173(3) 0.32046(19) 0.0785(9) Uani 1 1 d . . . . .
H4 H 0.413031 0.614213 0.355135 0.094 Uiso 1 1 calc R U . . .
C5 C 0.5759(3) 0.5390(2) 0.30359(16) 0.0611(6) Uani 1 1 d . . . . .
H5 H 0.538996 0.483373 0.327242 0.073 Uiso 1 1 calc R U . . .
C6 C 0.7063(2) 0.54379(16) 0.25135(13) 0.0440(5) Uani 1 1 d . . . . .
C7 C 0.7962(2) 0.46189(15) 0.22824(14) 0.0437(4) Uani 1 1 d . . . . .
H7 H 0.753854 0.404834 0.259459 0.052 Uiso 1 1 calc R U . . .
C8 C 0.9542(2) 0.44383(14) 0.25190(13) 0.0399(4) Uani 1 1 d . . . . .
C9 C 1.0250(3) 0.35695(15) 0.30846(15) 0.0486(5) Uani 1 1 d . . . . .
H9 H 0.975784 0.306512 0.334579 0.058 Uiso 1 1 calc R U . . .
C10 C 1.1700(3) 0.34495(17) 0.32634(16) 0.0533(5) Uani 1 1 d . . . . .
H10 H 1.217334 0.286431 0.364360 0.064 Uiso 1 1 calc R U . . .
C11 C 1.2433(3) 0.41917(17) 0.28805(16) 0.0531(5) Uani 1 1 d . . . . .
H11 H 1.340242 0.410452 0.300118 0.064 Uiso 1 1 calc R U . . .
C12 C 1.1737(2) 0.50738(15) 0.23131(14) 0.0435(4) Uani 1 1 d . . . . .
H12 H 1.223222 0.557715 0.206037 0.052 Uiso 1 1 calc R U . . .
C13 C 1.0296(2) 0.51929(14) 0.21295(12) 0.0372(4) Uani 1 1 d . . . . .
C14 C 0.8532(2) 0.57401(14) 0.07730(13) 0.0376(4) Uani 1 1 d . . . . .
C15 C 0.8555(2) 0.60916(17) -0.01385(14) 0.0474(5) Uani 1 1 d . . . . .
H15 H 0.894663 0.662861 -0.048198 0.057 Uiso 1 1 calc R U . . .
C16 C 0.7992(3) 0.5636(2) -0.05300(17) 0.0594(6) Uani 1 1 d . . . . .
H16 H 0.799323 0.587251 -0.114039 0.071 Uiso 1 1 calc R U . . .
C17 C 0.7432(3) 0.4842(2) -0.0029(2) 0.0668(7) Uani 1 1 d . . . . .
H17 H 0.706090 0.454081 -0.030281 0.080 Uiso 1 1 calc R U . . .
C18 C 0.7409(3) 0.44744(18) 0.08888(19) 0.0577(6) Uani 1 1 d . . . . .
H18 H 0.703107 0.393035 0.122552 0.069 Uiso 1 1 calc R U . . .
C19 C 0.7957(2) 0.49311(15) 0.12924(14) 0.0427(4) Uani 1 1 d . . . . .
C20 C 0.8112(3) 0.81361(17) 0.0276(2) 0.0680(8) Uani 1 1 d . . . . .
C21 C 1.2023(3) 1.0037(2) -0.1043(2) 0.0748(8) Uani 1 1 d . . . . .
H21A H 1.187566 1.011217 -0.162610 0.112 Uiso 1 1 calc R U . . .
H21B H 1.298189 1.014493 -0.103279 0.112 Uiso 1 1 calc R U . . .
H21C H 1.129112 1.048455 -0.087488 0.112 Uiso 1 1 calc R U . . .
C22 C 1.1897(2) 0.90483(16) -0.04078(15) 0.0489(5) Uani 1 1 d . . . . .
C23 C 1.3151(2) 0.83919(18) -0.00724(16) 0.0516(5) Uani 1 1 d . . . . .
H23 H 1.403595 0.860457 -0.023761 0.062 Uiso 1 1 calc R U . . .
C24 C 1.3212(2) 0.74500(17) 0.04851(15) 0.0495(5) Uani 1 1 d . . . . .
C25 C 1.4674(3) 0.6813(2) 0.0740(2) 0.0773(8) Uani 1 1 d . . . . .
H25A H 1.469391 0.653830 0.137018 0.116 Uiso 1 1 calc R U . . .
H25B H 1.543954 0.717420 0.048903 0.116 Uiso 1 1 calc R U . . .
H25C H 1.482536 0.631846 0.052477 0.116 Uiso 1 1 calc R U . . .
Rh2 Rh 0.32026(2) 0.79207(2) 0.57423(2) 0.04722(6) Uani 1 1 d . . . . .
P2 P 0.18415(6) 0.80581(4) 0.47010(3) 0.04127(11) Uani 1 1 d . . . . .
O4 O 0.5786(2) 0.7120(2) 0.48396(17) 0.0954(7) Uani 1 1 d . . . . .
O5 O 0.4557(2) 0.77967(15) 0.66609(13) 0.0704(5) Uani 1 1 d . . . . .
O6 O 0.14511(19) 0.83261(12) 0.64819(11) 0.0566(4) Uani 1 1 d . . . . .
C26 C 0.2407(2) 0.86821(16) 0.35426(15) 0.0488(5) Uani 1 1 d . . . . .
C27 C 0.3556(3) 0.91689(17) 0.32496(19) 0.0608(6) Uani 1 1 d . . . . .
H27 H 0.409322 0.921508 0.364745 0.073 Uiso 1 1 calc R U . . .
C28 C 0.3893(4) 0.9591(2) 0.2341(2) 0.0828(10) Uani 1 1 d . . . . .
H28 H 0.464833 0.993191 0.213287 0.099 Uiso 1 1 calc R U . . .
C29 C 0.3128(4) 0.9507(2) 0.1759(2) 0.0893(11) Uani 1 1 d . . . . .
H29 H 0.339123 0.977104 0.115968 0.107 Uiso 1 1 calc R U . . .
C30 C 0.1961(3) 0.9034(2) 0.20479(17) 0.0742(8) Uani 1 1 d . . . . .
H30 H 0.143914 0.898640 0.164400 0.089 Uiso 1 1 calc R U . . .
C31 C 0.1573(3) 0.86328(18) 0.29428(15) 0.0554(6) Uani 1 1 d . . . . .
C32 C 0.0296(3) 0.8119(2) 0.33272(16) 0.0582(6) Uani 1 1 d . . . . .
H32 H -0.023797 0.814289 0.285740 0.070 Uiso 1 1 calc R U . . .
C33 C -0.0716(3) 0.85924(18) 0.39009(16) 0.0545(5) Uani 1 1 d . . . . .
C34 C -0.2170(3) 0.9002(2) 0.3750(2) 0.0690(7) Uani 1 1 d . . . . .
H34 H -0.258911 0.898450 0.329003 0.083 Uiso 1 1 calc R U . . .
C35 C -0.3006(3) 0.9439(2) 0.4282(2) 0.0765(8) Uani 1 1 d . . . . .
H35 H -0.398261 0.972104 0.417218 0.092 Uiso 1 1 calc R U . . .
C36 C -0.2409(3) 0.9461(2) 0.4970(2) 0.0695(7) Uani 1 1 d . . . . .
H36 H -0.298711 0.975049 0.532741 0.083 Uiso 1 1 calc R U . . .
C37 C -0.0948(3) 0.90521(17) 0.51357(18) 0.0553(5) Uani 1 1 d . . . . .
H37 H -0.053997 0.907053 0.559941 0.066 Uiso 1 1 calc R U . . .
C38 C -0.0104(2) 0.86167(15) 0.46012(15) 0.0468(5) Uani 1 1 d . . . . .
C39 C 0.0901(3) 0.71071(18) 0.39057(15) 0.0517(5) Uani 1 1 d . . . . .
C40 C 0.0743(3) 0.6320(2) 0.3780(2) 0.0676(7) Uani 1 1 d . . . . .
H40 H 0.022048 0.639649 0.331799 0.081 Uiso 1 1 calc R U . . .
C41 C 0.1362(4) 0.5422(2) 0.4340(2) 0.0755(8) Uani 1 1 d . . . . .
H41 H 0.125651 0.489698 0.425054 0.091 Uiso 1 1 calc R U . . .
C42 C 0.2134(4) 0.52952(19) 0.5029(2) 0.0695(7) Uani 1 1 d . . . . .
H42 H 0.254401 0.468849 0.540471 0.083 Uiso 1 1 calc R U . . .
C43 C 0.2295(3) 0.60766(17) 0.51600(15) 0.0542(5) Uani 1 1 d . . . . .
H43 H 0.281206 0.599479 0.562602 0.065 Uiso 1 1 calc R U . . .
C44 C 0.1693(2) 0.69741(15) 0.46026(14) 0.0449(5) Uani 1 1 d . . . . .
C45 C 0.4777(3) 0.7452(2) 0.51643(18) 0.0626(6) Uani 1 1 d . . . . .
C46 C 0.5400(5) 0.7813(4) 0.7900(3) 0.1165(16) Uani 1 1 d . . . . .
H46A H 0.571755 0.715151 0.824590 0.175 Uiso 1 1 calc R U . . .
H46B H 0.507586 0.814746 0.828330 0.175 Uiso 1 1 calc R U . . .
H46C H 0.620339 0.805894 0.750947 0.175 Uiso 1 1 calc R U . . .
C47 C 0.4147(4) 0.7939(2) 0.73681(19) 0.0687(7) Uani 1 1 d . . . . .
C48 C 0.2712(3) 0.8191(2) 0.76600(18) 0.0668(7) Uani 1 1 d . . . . .
H48 H 0.257073 0.824613 0.820167 0.080 Uiso 1 1 calc R U . . .
C49 C 0.1461(3) 0.83702(18) 0.72289(17) 0.0595(6) Uani 1 1 d . . . . .
C50 C -0.0029(4) 0.8643(3) 0.7630(2) 0.0911(10) Uani 1 1 d . . . . .
H50A H -0.042376 0.929706 0.729872 0.137 Uiso 1 1 calc R U . . .
H50B H 0.005214 0.855053 0.822770 0.137 Uiso 1 1 calc R U . . .
H50C H -0.066997 0.825638 0.762106 0.137 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
Rh1 C20 1.794(3) . ?
Rh1 O3 2.0264(15) . ?
Rh1 O2 2.0630(15) . ?
Rh1 P1 2.2246(5) . ?
P1 C14 1.820(2) . ?
P1 C1 1.827(2) . ?
P1 C13 1.8312(19) . ?
O1 C20 1.150(3) . ?
O2 C22 1.266(3) . ?
O3 C24 1.276(3) . ?
C1 C2 1.384(3) . ?
C1 C6 1.398(3) . ?
C2 C3 1.384(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 1.385(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.524(3) . ?
C7 C19 1.519(3) . ?
C7 C8 1.527(3) . ?
C7 H7 0.9800 . ?
C8 C9 1.383(3) . ?
C8 C13 1.401(3) . ?
C9 C10 1.392(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.373(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.393(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(3) . ?
C12 H12 0.9300 . ?
C14 C15 1.387(3) . ?
C14 C19 1.395(3) . ?
C15 C16 1.380(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.364(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.396(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.388(3) . ?
C18 H18 0.9300 . ?
C21 C22 1.503(4) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.386(3) . ?
C23 C24 1.385(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.502(3) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
Rh2 C45 1.811(3) . ?
Rh2 O6 2.0371(16) . ?
Rh2 O5 2.0639(17) . ?
Rh2 P2 2.2283(5) . ?
P2 C44 1.825(2) . ?
P2 C26 1.831(2) . ?
P2 C38 1.831(2) . ?
O4 C45 1.142(3) . ?
O5 C47 1.276(3) . ?
O6 C49 1.279(3) . ?
C26 C27 1.384(3) . ?
C26 C31 1.402(4) . ?
C27 C28 1.402(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.360(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.385(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.388(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.517(4) . ?
C32 C39 1.509(4) . ?
C32 C33 1.531(4) . ?
C32 H32 0.9800 . ?
C33 C34 1.379(4) . ?
C33 C38 1.400(3) . ?
C34 C35 1.380(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.371(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.389(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.385(3) . ?
C37 H37 0.9300 . ?
C39 C40 1.388(4) . ?
C39 C44 1.396(3) . ?
C40 C41 1.382(5) . ?
C40 H40 0.9300 . ?
C41 C42 1.377(5) . ?
C41 H41 0.9300 . ?
C42 C43 1.384(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.376(3) . ?
C43 H43 0.9300 . ?
C46 C47 1.513(4) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C48 1.382(4) . ?
C48 C49 1.385(4) . ?
C48 H48 0.9300 . ?
C49 C50 1.500(4) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 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
C20 Rh1 O3 176.73(12) . . ?
C20 Rh1 O2 90.01(9) . . ?
O3 Rh1 O2 89.01(6) . . ?
C20 Rh1 P1 87.14(8) . . ?
O3 Rh1 P1 93.74(5) . . ?
O2 Rh1 P1 176.74(5) . . ?
C14 P1 C1 96.48(9) . . ?
C14 P1 C13 97.33(9) . . ?
C1 P1 C13 96.22(9) . . ?
C14 P1 Rh1 115.18(7) . . ?
C1 P1 Rh1 119.61(7) . . ?
C13 P1 Rh1 126.07(7) . . ?
C22 O2 Rh1 126.32(15) . . ?
C24 O3 Rh1 126.78(14) . . ?
C2 C1 C6 120.6(2) . . ?
C2 C1 P1 125.23(18) . . ?
C6 C1 P1 114.12(15) . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.7(2) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 119.7(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 119.3(2) . . ?
C5 C6 C7 123.7(2) . . ?
C1 C6 C7 116.88(18) . . ?
C19 C7 C6 107.07(17) . . ?
C19 C7 C8 108.59(16) . . ?
C6 C7 C8 108.86(17) . . ?
C19 C7 H7 110.7 . . ?
C6 C7 H7 110.7 . . ?
C8 C7 H7 110.7 . . ?
C9 C8 C13 119.45(19) . . ?
C9 C8 C7 122.97(19) . . ?
C13 C8 C7 117.57(17) . . ?
C8 C9 C10 120.0(2) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 120.3(2) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.6(2) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 119.2(2) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C8 120.42(18) . . ?
C12 C13 P1 126.23(16) . . ?
C8 C13 P1 113.34(14) . . ?
C15 C14 C19 120.68(19) . . ?
C15 C14 P1 124.23(17) . . ?
C19 C14 P1 115.09(15) . . ?
C16 C15 C14 119.3(2) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C17 C16 C15 120.6(2) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 120.9(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 119.3(2) . . ?
C18 C19 C7 124.4(2) . . ?
C14 C19 C7 116.25(18) . . ?
O1 C20 Rh1 177.8(3) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O2 C22 C23 125.7(2) . . ?
O2 C22 C21 114.4(2) . . ?
C23 C22 C21 119.9(2) . . ?
C24 C23 C22 126.3(2) . . ?
C24 C23 H23 116.9 . . ?
C22 C23 H23 116.9 . . ?
O3 C24 C23 125.9(2) . . ?
O3 C24 C25 114.4(2) . . ?
C23 C24 C25 119.7(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C45 Rh2 O6 174.73(11) . . ?
C45 Rh2 O5 89.61(9) . . ?
O6 Rh2 O5 88.60(7) . . ?
C45 Rh2 P2 87.69(8) . . ?
O6 Rh2 P2 94.19(5) . . ?
O5 Rh2 P2 177.04(6) . . ?
C44 P2 C26 96.31(10) . . ?
C44 P2 C38 96.89(10) . . ?
C26 P2 C38 95.55(10) . . ?
C44 P2 Rh2 117.71(7) . . ?
C26 P2 Rh2 119.22(8) . . ?
C38 P2 Rh2 125.06(8) . . ?
C47 O5 Rh2 126.22(18) . . ?
C49 O6 Rh2 127.49(17) . . ?
C27 C26 C31 120.7(2) . . ?
C27 C26 P2 124.8(2) . . ?
C31 C26 P2 114.44(17) . . ?
C26 C27 C28 118.6(3) . . ?
C26 C27 H27 120.7 . . ?
C28 C27 H27 120.7 . . ?
C29 C28 C27 120.7(3) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 120.9(3) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C29 C30 C31 119.7(3) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C26 119.3(3) . . ?
C30 C31 C32 123.9(3) . . ?
C26 C31 C32 116.8(2) . . ?
C39 C32 C31 108.1(2) . . ?
C39 C32 C33 108.6(2) . . ?
C31 C32 C33 108.1(2) . . ?
C39 C32 H32 110.7 . . ?
C31 C32 H32 110.7 . . ?
C33 C32 H32 110.7 . . ?
C34 C33 C38 119.3(2) . . ?
C34 C33 C32 123.4(2) . . ?
C38 C33 C32 117.3(2) . . ?
C33 C34 C35 120.1(3) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.7(3) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C35 C36 C37 120.4(3) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
C38 C37 C36 119.1(3) . . ?
C38 C37 H37 120.4 . . ?
C36 C37 H37 120.4 . . ?
C37 C38 C33 120.4(2) . . ?
C37 C38 P2 125.67(19) . . ?
C33 C38 P2 113.89(17) . . ?
C40 C39 C44 118.9(2) . . ?
C40 C39 C32 124.6(2) . . ?
C44 C39 C32 116.4(2) . . ?
C41 C40 C39 120.1(3) . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C42 C41 C40 120.7(3) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C41 C42 C43 119.6(3) . . ?
C41 C42 H42 120.2 . . ?
C43 C42 H42 120.2 . . ?
C44 C43 C42 120.2(3) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C39 120.5(2) . . ?
C43 C44 P2 124.30(18) . . ?
C39 C44 P2 115.17(17) . . ?
O4 C45 Rh2 176.5(3) . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O5 C47 C48 125.8(3) . . ?
O5 C47 C46 114.0(3) . . ?
C48 C47 C46 120.2(3) . . ?
C47 C48 C49 126.7(2) . . ?
C47 C48 H48 116.6 . . ?
C49 C48 H48 116.6 . . ?
O6 C49 C48 125.0(2) . . ?
O6 C49 C50 114.5(3) . . ?
C48 C49 C50 120.5(2) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 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 C1 C2 -130.4(2) . . . . ?
C13 P1 C1 C2 131.4(2) . . . . ?
Rh1 P1 C1 C2 -6.6(2) . . . . ?
C14 P1 C1 C6 46.28(16) . . . . ?
C13 P1 C1 C6 -51.86(16) . . . . ?
Rh1 P1 C1 C6 170.14(12) . . . . ?
C6 C1 C2 C3 -1.5(4) . . . . ?
P1 C1 C2 C3 175.0(2) . . . . ?
C1 C2 C3 C4 -0.9(4) . . . . ?
C2 C3 C4 C5 2.0(5) . . . . ?
C3 C4 C5 C6 -0.5(4) . . . . ?
C4 C5 C6 C1 -1.9(3) . . . . ?
C4 C5 C6 C7 -179.4(2) . . . . ?
C2 C1 C6 C5 2.9(3) . . . . ?
P1 C1 C6 C5 -173.96(17) . . . . ?
C2 C1 C6 C7 -179.4(2) . . . . ?
P1 C1 C6 C7 3.8(2) . . . . ?
C5 C6 C7 C19 115.8(2) . . . . ?
C1 C6 C7 C19 -61.8(2) . . . . ?
C5 C6 C7 C8 -127.0(2) . . . . ?
C1 C6 C7 C8 55.4(2) . . . . ?
C19 C7 C8 C9 -120.4(2) . . . . ?
C6 C7 C8 C9 123.3(2) . . . . ?
C19 C7 C8 C13 58.8(2) . . . . ?
C6 C7 C8 C13 -57.5(2) . . . . ?
C13 C8 C9 C10 0.0(3) . . . . ?
C7 C8 C9 C10 179.2(2) . . . . ?
C8 C9 C10 C11 0.1(4) . . . . ?
C9 C10 C11 C12 0.3(4) . . . . ?
C10 C11 C12 C13 -0.8(3) . . . . ?
C11 C12 C13 C8 0.8(3) . . . . ?
C11 C12 C13 P1 -178.05(17) . . . . ?
C9 C8 C13 C12 -0.4(3) . . . . ?
C7 C8 C13 C12 -179.65(18) . . . . ?
C9 C8 C13 P1 178.56(16) . . . . ?
C7 C8 C13 P1 -0.6(2) . . . . ?
C14 P1 C13 C12 131.39(18) . . . . ?
C1 P1 C13 C12 -131.22(18) . . . . ?
Rh1 P1 C13 C12 2.8(2) . . . . ?
C14 P1 C13 C8 -47.55(16) . . . . ?
C1 P1 C13 C8 49.84(16) . . . . ?
Rh1 P1 C13 C8 -176.19(11) . . . . ?
C1 P1 C14 C15 130.41(18) . . . . ?
C13 P1 C14 C15 -132.44(17) . . . . ?
Rh1 P1 C14 C15 3.33(19) . . . . ?
C1 P1 C14 C19 -48.85(16) . . . . ?
C13 P1 C14 C19 48.30(16) . . . . ?
Rh1 P1 C14 C19 -175.93(12) . . . . ?
C19 C14 C15 C16 0.4(3) . . . . ?
P1 C14 C15 C16 -178.78(16) . . . . ?
C14 C15 C16 C17 -0.8(3) . . . . ?
C15 C16 C17 C18 0.3(4) . . . . ?
C16 C17 C18 C19 0.4(4) . . . . ?
C17 C18 C19 C14 -0.7(3) . . . . ?
C17 C18 C19 C7 178.5(2) . . . . ?
C15 C14 C19 C18 0.3(3) . . . . ?
P1 C14 C19 C18 179.58(17) . . . . ?
C15 C14 C19 C7 -178.95(18) . . . . ?
P1 C14 C19 C7 0.3(2) . . . . ?
C6 C7 C19 C18 -120.1(2) . . . . ?
C8 C7 C19 C18 122.5(2) . . . . ?
C6 C7 C19 C14 59.1(2) . . . . ?
C8 C7 C19 C14 -58.3(2) . . . . ?
Rh1 O2 C22 C23 0.8(4) . . . . ?
Rh1 O2 C22 C21 178.59(19) . . . . ?
O2 C22 C23 C24 0.6(4) . . . . ?
C21 C22 C23 C24 -177.1(3) . . . . ?
Rh1 O3 C24 C23 3.2(4) . . . . ?
Rh1 O3 C24 C25 -175.5(2) . . . . ?
C22 C23 C24 O3 -2.8(4) . . . . ?
C22 C23 C24 C25 175.8(3) . . . . ?
C44 P2 C26 C27 -133.5(2) . . . . ?
C38 P2 C26 C27 128.9(2) . . . . ?
Rh2 P2 C26 C27 -6.8(2) . . . . ?
C44 P2 C26 C31 46.25(19) . . . . ?
C38 P2 C26 C31 -51.33(19) . . . . ?
Rh2 P2 C26 C31 172.98(14) . . . . ?
C31 C26 C27 C28 -1.6(4) . . . . ?
P2 C26 C27 C28 178.1(2) . . . . ?
C26 C27 C28 C29 -1.4(4) . . . . ?
C27 C28 C29 C30 2.5(5) . . . . ?
C28 C29 C30 C31 -0.6(5) . . . . ?
C29 C30 C31 C26 -2.4(4) . . . . ?
C29 C30 C31 C32 178.6(3) . . . . ?
C27 C26 C31 C30 3.5(4) . . . . ?
P2 C26 C31 C30 -176.3(2) . . . . ?
C27 C26 C31 C32 -177.4(2) . . . . ?
P2 C26 C31 C32 2.8(3) . . . . ?
C30 C31 C32 C39 118.3(3) . . . . ?
C26 C31 C32 C39 -60.8(3) . . . . ?
C30 C31 C32 C33 -124.3(3) . . . . ?
C26 C31 C32 C33 56.6(3) . . . . ?
C39 C32 C33 C34 -122.6(3) . . . . ?
C31 C32 C33 C34 120.4(3) . . . . ?
C39 C32 C33 C38 58.6(3) . . . . ?
C31 C32 C33 C38 -58.5(3) . . . . ?
C38 C33 C34 C35 0.6(4) . . . . ?
C32 C33 C34 C35 -178.2(3) . . . . ?
C33 C34 C35 C36 -0.8(5) . . . . ?
C34 C35 C36 C37 0.8(5) . . . . ?
C35 C36 C37 C38 -0.5(4) . . . . ?
C36 C37 C38 C33 0.3(4) . . . . ?
C36 C37 C38 P2 178.9(2) . . . . ?
C34 C33 C38 C37 -0.3(4) . . . . ?
C32 C33 C38 C37 178.6(2) . . . . ?
C34 C33 C38 P2 -179.1(2) . . . . ?
C32 C33 C38 P2 -0.2(3) . . . . ?
C44 P2 C38 C37 133.8(2) . . . . ?
C26 P2 C38 C37 -129.2(2) . . . . ?
Rh2 P2 C38 C37 2.7(2) . . . . ?
C44 P2 C38 C33 -47.51(19) . . . . ?
C26 P2 C38 C33 49.55(19) . . . . ?
Rh2 P2 C38 C33 -178.58(14) . . . . ?
C31 C32 C39 C40 -120.3(3) . . . . ?
C33 C32 C39 C40 122.7(3) . . . . ?
C31 C32 C39 C44 58.5(3) . . . . ?
C33 C32 C39 C44 -58.5(3) . . . . ?
C44 C39 C40 C41 0.1(4) . . . . ?
C32 C39 C40 C41 178.9(2) . . . . ?
C39 C40 C41 C42 0.3(4) . . . . ?
C40 C41 C42 C43 -0.2(4) . . . . ?
C41 C42 C43 C44 -0.2(4) . . . . ?
C42 C43 C44 C39 0.7(3) . . . . ?
C42 C43 C44 P2 -179.51(19) . . . . ?
C40 C39 C44 C43 -0.6(3) . . . . ?
C32 C39 C44 C43 -179.5(2) . . . . ?
C40 C39 C44 P2 179.57(18) . . . . ?
C32 C39 C44 P2 0.7(3) . . . . ?
C26 P2 C44 C43 131.7(2) . . . . ?
C38 P2 C44 C43 -131.9(2) . . . . ?
Rh2 P2 C44 C43 3.9(2) . . . . ?
C26 P2 C44 C39 -48.47(18) . . . . ?
C38 P2 C44 C39 47.92(18) . . . . ?
Rh2 P2 C44 C39 -176.27(14) . . . . ?
Rh2 O5 C47 C48 1.0(4) . . . . ?
Rh2 O5 C47 C46 -178.7(3) . . . . ?
O5 C47 C48 C49 -2.6(5) . . . . ?
C46 C47 C48 C49 177.1(3) . . . . ?
Rh2 O6 C49 C48 3.6(4) . . . . ?
Rh2 O6 C49 C50 -176.6(2) . . . . ?
C47 C48 C49 O6 0.1(5) . . . . ?
C47 C48 C49 C50 -179.7(3) . . . . ?

_refine_diff_density_max         0.402
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.057



# start Validation Reply Form
_vrf_PLAT242_nt0808_LHG200B      
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C47 Check 
RESPONSE: Wobbling acetylacetonato- fragment
;
_vrf_PLAT911_nt0808_LHG200B      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.598         83 Report
RESPONSE: These reflections are missing in the highest resolution shell 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_nt0812_LHG203A
_database_code_depnum_ccdc_archive 'CCDC 2061862'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
;
(acetylacetonato)-carbonylrhodium-ortho-trifluoromethyl-9-phosphatriptycene 
complex
;
_chemical_name_common            'Rh(acac)CO(o-CF3-9-phosphatriptycene complex)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H19 F3 O3 P Rh'
_chemical_formula_sum            'C26 H19 F3 O3 P Rh'
_chemical_formula_weight         570.29

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'
F F 0.0727 0.0534 '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'
Rh Rh 0.0927 3.6045 '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                   8.26668(8)
_cell_length_b                   15.72226(15)
_cell_length_c                   17.67340(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2297.03(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    8120
_cell_measurement_theta_min      3.7450
_cell_measurement_theta_max      66.9120

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.054
_exptl_absorpt_coefficient_mu    7.128
_shelx_estimated_absorpt_T_min   0.158
_shelx_estimated_absorpt_T_max   0.699
_exptl_absorpt_correction_T_min  0.110
_exptl_absorpt_correction_T_max  0.688
_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_reflns_number            13181
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.763
_diffrn_reflns_theta_max         67.104
_diffrn_reflns_theta_full        67.104
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             4062
_reflns_number_gt                3941
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.741
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    0.990

_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    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0406P)²+0.2985P] 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_abs_structure_details 
;
 Flack x determined using 1611 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(7)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         4062
_refine_ls_number_parameters     309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0683
_refine_ls_wR_factor_gt          0.0673
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
Rh1 Rh 0.11112(4) 0.45860(2) 0.41523(2) 0.03543(12) Uani 1 1 d . . . . .
P1 P 0.19381(13) 0.57452(7) 0.35351(6) 0.0307(2) Uani 1 1 d . . . . .
F1 F 0.4696(4) 0.4659(3) 0.45569(19) 0.0693(9) Uani 1 1 d . . . . .
F2 F 0.6941(4) 0.4387(3) 0.4021(4) 0.1110(19) Uani 1 1 d . . . . .
F3 F 0.4731(5) 0.4140(2) 0.3433(2) 0.0684(9) Uani 1 1 d . . . . .
O1 O 0.1288(7) 0.3512(2) 0.2785(2) 0.0688(11) Uani 1 1 d . . . . .
O2 O 0.0160(5) 0.3563(2) 0.4734(2) 0.0513(9) Uani 1 1 d . . . . .
O3 O 0.1281(5) 0.5221(2) 0.51541(19) 0.0519(8) Uani 1 1 d . . . . .
C1 C 0.1256(5) 0.5966(3) 0.2567(2) 0.0363(9) Uani 1 1 d . . . . .
C2 C 0.0236(6) 0.5460(3) 0.2146(3) 0.0451(11) Uani 1 1 d . . . . .
H2 H -0.011360 0.494002 0.233583 0.054 Uiso 1 1 calc R U . . .
C3 C -0.0272(8) 0.5734(4) 0.1431(3) 0.0620(15) Uani 1 1 d . . . . .
H3 H -0.096954 0.539719 0.114668 0.074 Uiso 1 1 calc R U . . .
C4 C 0.0256(9) 0.6497(4) 0.1147(3) 0.0625(16) Uani 1 1 d . . . . .
H4 H -0.006565 0.666764 0.066587 0.075 Uiso 1 1 calc R U . . .
C5 C 0.1259(7) 0.7013(3) 0.1568(3) 0.0514(12) Uani 1 1 d . . . . .
H5 H 0.159890 0.753284 0.137298 0.062 Uiso 1 1 calc R U . . .
C6 C 0.1764(6) 0.6759(3) 0.2281(3) 0.0387(10) Uani 1 1 d . . . . .
C7 C 0.2782(6) 0.7308(3) 0.2799(3) 0.0394(10) Uani 1 1 d . . . . .
H7 H 0.307229 0.784180 0.254625 0.047 Uiso 1 1 calc R U . . .
C8 C 0.1788(6) 0.7486(3) 0.3506(3) 0.0400(10) Uani 1 1 d . . . . .
C9 C 0.1340(7) 0.8294(3) 0.3724(3) 0.0532(13) Uani 1 1 d . . . . .
H9 H 0.169981 0.876634 0.345573 0.064 Uiso 1 1 calc R U . . .
C10 C 0.0333(9) 0.8392(4) 0.4357(4) 0.0699(18) Uani 1 1 d . . . . .
H10 H 0.002536 0.893412 0.451041 0.084 Uiso 1 1 calc R U . . .
C11 C -0.0197(9) 0.7702(4) 0.4748(4) 0.0676(17) Uani 1 1 d . . . . .
H11 H -0.088312 0.777783 0.515916 0.081 Uiso 1 1 calc R U . . .
C12 C 0.0266(7) 0.6888(4) 0.4544(3) 0.0512(12) Uani 1 1 d . . . . .
H12 H -0.010059 0.641987 0.481582 0.061 Uiso 1 1 calc R U . . .
C13 C 0.1295(5) 0.6778(3) 0.3922(2) 0.0357(9) Uani 1 1 d . . . . .
C14 C 0.4103(6) 0.6032(3) 0.3378(2) 0.0329(9) Uani 1 1 d . . . . .
C15 C 0.5518(5) 0.5576(3) 0.3570(3) 0.0415(11) Uani 1 1 d . . . . .
C16 C 0.5464(6) 0.4696(4) 0.3895(4) 0.0586(15) Uani 1 1 d . . . . .
C17 C 0.7018(6) 0.5926(4) 0.3426(3) 0.0536(13) Uani 1 1 d . . . . .
H17 H 0.794238 0.562438 0.355968 0.064 Uiso 1 1 calc R U . . .
C18 C 0.7178(7) 0.6715(4) 0.3087(4) 0.0562(14) Uani 1 1 d . . . . .
H18 H 0.819764 0.694525 0.300073 0.067 Uiso 1 1 calc R U . . .
C19 C 0.5815(6) 0.7152(3) 0.2882(3) 0.0456(11) Uani 1 1 d . . . . .
H19 H 0.591341 0.767654 0.264296 0.055 Uiso 1 1 calc R U . . .
C20 C 0.4292(5) 0.6823(3) 0.3025(3) 0.0365(10) Uani 1 1 d . . . . .
C21 C 0.1172(7) 0.3955(3) 0.3300(3) 0.0432(10) Uani 1 1 d . . . . .
C22 C -0.0994(11) 0.2733(4) 0.5694(4) 0.085(2) Uani 1 1 d . . . . .
H22A H -0.185607 0.257552 0.535748 0.128 Uiso 1 1 calc R U . . .
H22B H -0.141674 0.280858 0.619510 0.128 Uiso 1 1 calc R U . . .
H22C H -0.019064 0.229187 0.569850 0.128 Uiso 1 1 calc R U . . .
C23 C -0.0239(7) 0.3552(3) 0.5427(3) 0.0532(13) Uani 1 1 d . . . . .
C24 C -0.0009(8) 0.4207(4) 0.5939(3) 0.0588(14) Uani 1 1 d . . . . .
H24 H -0.039972 0.412198 0.642681 0.071 Uiso 1 1 calc R U . . .
C25 C 0.0750(7) 0.4978(3) 0.5794(3) 0.0515(12) Uani 1 1 d . . . . .
C26 C 0.0977(11) 0.5613(4) 0.6416(3) 0.0770(19) Uani 1 1 d . . . . .
H26A H 0.210269 0.575674 0.645606 0.116 Uiso 1 1 calc R U . . .
H26B H 0.061312 0.537249 0.688561 0.116 Uiso 1 1 calc R U . . .
H26C H 0.036275 0.611556 0.630584 0.116 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
Rh1 C21 1.805(5) . ?
Rh1 O3 2.037(3) . ?
Rh1 O2 2.064(3) . ?
Rh1 P1 2.2312(11) . ?
P1 C1 1.835(4) . ?
P1 C13 1.840(4) . ?
P1 C14 1.866(5) . ?
F1 C16 1.332(7) . ?
F2 C16 1.333(7) . ?
F3 C16 1.341(8) . ?
O1 C21 1.149(6) . ?
O2 C23 1.269(7) . ?
O3 C25 1.272(7) . ?
C1 C2 1.376(7) . ?
C1 C6 1.410(7) . ?
C2 C3 1.400(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.372(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.387(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.513(7) . ?
C7 C20 1.516(6) . ?
C7 C8 1.522(7) . ?
C7 H7 0.9800 . ?
C8 C9 1.378(7) . ?
C8 C13 1.394(7) . ?
C9 C10 1.403(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.359(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.384(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.400(7) . ?
C12 H12 0.9300 . ?
C14 C20 1.401(6) . ?
C14 C15 1.414(7) . ?
C15 C17 1.380(7) . ?
C15 C16 1.498(8) . ?
C17 C18 1.384(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.369(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.385(7) . ?
C19 H19 0.9300 . ?
C22 C23 1.507(8) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.384(9) . ?
C24 C25 1.390(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.496(8) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 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
C21 Rh1 O3 173.2(2) . . ?
C21 Rh1 O2 89.87(18) . . ?
O3 Rh1 O2 88.58(14) . . ?
C21 Rh1 P1 91.87(15) . . ?
O3 Rh1 P1 90.21(10) . . ?
O2 Rh1 P1 175.17(12) . . ?
C1 P1 C13 95.22(19) . . ?
C1 P1 C14 96.4(2) . . ?
C13 P1 C14 96.8(2) . . ?
C1 P1 Rh1 121.07(15) . . ?
C13 P1 Rh1 116.79(15) . . ?
C14 P1 Rh1 124.30(14) . . ?
C23 O2 Rh1 126.2(4) . . ?
C25 O3 Rh1 127.0(3) . . ?
C2 C1 C6 120.0(4) . . ?
C2 C1 P1 125.6(4) . . ?
C6 C1 P1 114.2(3) . . ?
C1 C2 C3 119.6(5) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 120.3(6) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.6(5) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 120.2(5) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 119.4(5) . . ?
C5 C6 C7 123.6(5) . . ?
C1 C6 C7 117.0(4) . . ?
C6 C7 C20 109.3(4) . . ?
C6 C7 C8 107.5(4) . . ?
C20 C7 C8 108.7(4) . . ?
C6 C7 H7 110.4 . . ?
C20 C7 H7 110.4 . . ?
C8 C7 H7 110.4 . . ?
C9 C8 C13 120.7(4) . . ?
C9 C8 C7 122.9(4) . . ?
C13 C8 C7 116.4(4) . . ?
C8 C9 C10 118.9(5) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C11 C10 C9 120.6(5) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 121.1(6) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C13 119.1(5) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C8 C13 C12 119.5(4) . . ?
C8 C13 P1 115.1(3) . . ?
C12 C13 P1 125.1(4) . . ?
C20 C14 C15 117.7(4) . . ?
C20 C14 P1 112.8(3) . . ?
C15 C14 P1 129.5(3) . . ?
C17 C15 C14 119.8(4) . . ?
C17 C15 C16 117.8(4) . . ?
C14 C15 C16 122.4(4) . . ?
F1 C16 F2 105.9(5) . . ?
F1 C16 F3 106.9(5) . . ?
F2 C16 F3 106.2(6) . . ?
F1 C16 C15 113.0(5) . . ?
F2 C16 C15 112.0(5) . . ?
F3 C16 C15 112.4(5) . . ?
C15 C17 C18 121.6(5) . . ?
C15 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C19 C18 C17 119.1(5) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C20 120.9(5) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C19 C20 C14 121.0(4) . . ?
C19 C20 C7 120.9(4) . . ?
C14 C20 C7 118.2(4) . . ?
O1 C21 Rh1 174.9(5) . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C23 C24 125.8(5) . . ?
O2 C23 C22 115.0(5) . . ?
C24 C23 C22 119.2(5) . . ?
C23 C24 C25 126.2(5) . . ?
C23 C24 H24 116.9 . . ?
C25 C24 H24 116.9 . . ?
O3 C25 C24 125.5(5) . . ?
O3 C25 C26 114.2(5) . . ?
C24 C25 C26 120.2(5) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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
C13 P1 C1 C2 -126.4(4) . . . . ?
C14 P1 C1 C2 136.1(4) . . . . ?
Rh1 P1 C1 C2 -0.7(5) . . . . ?
C13 P1 C1 C6 48.7(4) . . . . ?
C14 P1 C1 C6 -48.8(4) . . . . ?
Rh1 P1 C1 C6 174.4(3) . . . . ?
C6 C1 C2 C3 0.9(8) . . . . ?
P1 C1 C2 C3 175.8(4) . . . . ?
C1 C2 C3 C4 0.7(9) . . . . ?
C2 C3 C4 C5 -1.6(10) . . . . ?
C3 C4 C5 C6 0.9(9) . . . . ?
C4 C5 C6 C1 0.7(8) . . . . ?
C4 C5 C6 C7 -176.3(5) . . . . ?
C2 C1 C6 C5 -1.6(7) . . . . ?
P1 C1 C6 C5 -177.1(4) . . . . ?
C2 C1 C6 C7 175.6(4) . . . . ?
P1 C1 C6 C7 0.2(5) . . . . ?
C5 C6 C7 C20 -124.8(5) . . . . ?
C1 C6 C7 C20 58.1(5) . . . . ?
C5 C6 C7 C8 117.4(5) . . . . ?
C1 C6 C7 C8 -59.7(5) . . . . ?
C6 C7 C8 C9 -118.4(5) . . . . ?
C20 C7 C8 C9 123.4(5) . . . . ?
C6 C7 C8 C13 59.5(5) . . . . ?
C20 C7 C8 C13 -58.6(5) . . . . ?
C13 C8 C9 C10 -2.1(8) . . . . ?
C7 C8 C9 C10 175.8(5) . . . . ?
C8 C9 C10 C11 -0.2(10) . . . . ?
C9 C10 C11 C12 1.4(11) . . . . ?
C10 C11 C12 C13 -0.2(10) . . . . ?
C9 C8 C13 C12 3.3(7) . . . . ?
C7 C8 C13 C12 -174.8(4) . . . . ?
C9 C8 C13 P1 177.9(4) . . . . ?
C7 C8 C13 P1 -0.1(5) . . . . ?
C11 C12 C13 C8 -2.1(8) . . . . ?
C11 C12 C13 P1 -176.2(5) . . . . ?
C1 P1 C13 C8 -49.1(4) . . . . ?
C14 P1 C13 C8 48.0(4) . . . . ?
Rh1 P1 C13 C8 -177.9(3) . . . . ?
C1 P1 C13 C12 125.2(4) . . . . ?
C14 P1 C13 C12 -137.7(4) . . . . ?
Rh1 P1 C13 C12 -3.6(5) . . . . ?
C1 P1 C14 C20 49.7(4) . . . . ?
C13 P1 C14 C20 -46.3(4) . . . . ?
Rh1 P1 C14 C20 -175.5(3) . . . . ?
C1 P1 C14 C15 -131.0(4) . . . . ?
C13 P1 C14 C15 133.0(4) . . . . ?
Rh1 P1 C14 C15 3.8(5) . . . . ?
C20 C14 C15 C17 1.9(7) . . . . ?
P1 C14 C15 C17 -177.4(4) . . . . ?
C20 C14 C15 C16 -175.2(5) . . . . ?
P1 C14 C15 C16 5.5(8) . . . . ?
C17 C15 C16 F1 121.5(6) . . . . ?
C14 C15 C16 F1 -61.4(7) . . . . ?
C17 C15 C16 F2 2.0(8) . . . . ?
C14 C15 C16 F2 179.1(6) . . . . ?
C17 C15 C16 F3 -117.4(6) . . . . ?
C14 C15 C16 F3 59.7(7) . . . . ?
C14 C15 C17 C18 -0.8(9) . . . . ?
C16 C15 C17 C18 176.4(6) . . . . ?
C15 C17 C18 C19 -0.9(10) . . . . ?
C17 C18 C19 C20 1.5(9) . . . . ?
C18 C19 C20 C14 -0.5(8) . . . . ?
C18 C19 C20 C7 179.8(5) . . . . ?
C15 C14 C20 C19 -1.2(7) . . . . ?
P1 C14 C20 C19 178.2(4) . . . . ?
C15 C14 C20 C7 178.5(4) . . . . ?
P1 C14 C20 C7 -2.1(5) . . . . ?
C6 C7 C20 C19 122.8(5) . . . . ?
C8 C7 C20 C19 -120.1(5) . . . . ?
C6 C7 C20 C14 -56.9(6) . . . . ?
C8 C7 C20 C14 60.2(5) . . . . ?
Rh1 O2 C23 C24 -4.7(9) . . . . ?
Rh1 O2 C23 C22 176.6(5) . . . . ?
O2 C23 C24 C25 -2.5(10) . . . . ?
C22 C23 C24 C25 176.0(6) . . . . ?
Rh1 O3 C25 C24 2.5(8) . . . . ?
Rh1 O3 C25 C26 -176.5(4) . . . . ?
C23 C24 C25 O3 3.8(10) . . . . ?
C23 C24 C25 C26 -177.2(6) . . . . ?

_refine_diff_density_max         0.473
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.054



# start Validation Reply Form
_vrf_PLAT090_nt0812_LHG203A      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       7.55 Note  
RESPONSE: Limited resolution (only Cu radiation was available).
;
_vrf_PLAT911_nt0812_LHG203A      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.597          8 Report
RESPONSE: These reflections are missing in the lowest and highest resolution 
shell 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_nt0589_Lei_trip-Cl
_database_code_depnum_ccdc_archive 'CCDC 2061850'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        4-chloro-10H-5,10-[1,2]benzenoacridophosphine
_chemical_name_common            4-chloro-10H-5,10-[1,2]benzenoacridophosphine
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H12 Cl P'
_chemical_formula_sum            'C19 H12 Cl P'
_chemical_formula_weight         306.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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

_cell_length_a                   7.2135(3)
_cell_length_b                   13.7539(4)
_cell_length_c                   8.1944(3)
_cell_angle_alpha                90
_cell_angle_beta                 113.053(4)
_cell_angle_gamma                90
_cell_volume                     748.07(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1486
_cell_measurement_theta_min      7.3900
_cell_measurement_theta_max      66.3840

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_F_000             316
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.018
_exptl_absorpt_coefficient_mu    3.164
_shelx_estimated_absorpt_T_min   0.585
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.16b (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  
;
Oxford Diffraction Xcalibur, Ruby, Gemini Ultra
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1856
_diffrn_reflns_number            2755
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         5.868
_diffrn_reflns_theta_max         67.188
_diffrn_reflns_theta_full        67.188
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             2755
_reflns_number_gt                1966
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0875P)²+0.3746P] 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         2755
_refine_ls_number_parameters     120
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0664
_refine_ls_wR_factor_ref         0.2080
_refine_ls_wR_factor_gt          0.2007
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.081
_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
Cl1 Cl 0.8899(4) 0.4533(2) 0.8253(4) 0.0809(10) Uani 0.447(3) 1 d . . P A 1
P1 P 0.6957(3) 0.250000 0.5683(2) 0.0629(6) Uani 1 2 d S T P A .
Cl2 Cl 0.774(3) 0.250000 0.180(3) 0.106(9) Uani 0.106(6) 2 d S TU P A 3
C1 C 0.5620(7) 0.3471(3) 0.6288(5) 0.0578(11) Uani 1 1 d . . . . .
C2 C 0.6506(9) 0.4274(4) 0.7369(6) 0.0789(15) Uani 1 1 d . . . . .
H2 H 0.789621 0.435254 0.780550 0.095 Uiso 0.5532 1 calc R U P A 2
C3 C 0.5356(12) 0.4946(4) 0.7796(7) 0.0894(18) Uani 1 1 d . . . . .
H3 H 0.597592 0.546688 0.853116 0.107 Uiso 1 1 calc R U . . .
C4 C 0.3306(12) 0.4853(4) 0.7144(8) 0.0913(18) Uani 1 1 d . . . . .
H4 H 0.253501 0.531496 0.742439 0.110 Uiso 1 1 calc R U . . .
C5 C 0.2379(9) 0.4075(3) 0.6070(6) 0.0736(13) Uani 1 1 d . . . . .
H5 H 0.098551 0.400901 0.563359 0.088 Uiso 1 1 calc R U . . .
C6 C 0.3520(7) 0.3399(3) 0.5647(5) 0.0565(10) Uani 1 1 d . . . . .
C7 C 0.2586(9) 0.250000 0.4521(7) 0.0547(14) Uani 1 2 d S T P . .
H7 H 0.111602 0.250000 0.412883 0.066 Uiso 1 2 calc R U P . .
C8 C 0.3211(10) 0.250000 0.2937(7) 0.0564(14) Uani 1 2 d S T P A .
C9 C 0.1879(11) 0.250000 0.1187(8) 0.0703(18) Uani 1 2 d S T P . .
H9 H 0.049854 0.250000 0.090671 0.084 Uiso 1 2 calc R U P . .
C10 C 0.2593(13) 0.250000 -0.0154(9) 0.076(2) Uani 1 2 d S T P A .
H10 H 0.168248 0.250000 -0.133060 0.092 Uiso 1 2 calc R U P . .
C11 C 0.4574(14) 0.250000 0.0214(9) 0.078(2) Uani 1 2 d S T P . .
H11 H 0.503131 0.250000 -0.070126 0.093 Uiso 1 2 calc R U P A 3
C12 C 0.5951(12) 0.250000 0.1980(9) 0.0712(18) Uani 1 2 d S TU P A .
H12 H 0.732673 0.250000 0.223977 0.085 Uiso 0.894(6) 2 calc R U P A 4
C13 C 0.5276(9) 0.250000 0.3331(7) 0.0558(14) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C2 1.629(6) . ?
P1 C1 1.826(5) 4_565 ?
P1 C1 1.826(5) . ?
P1 C13 1.831(6) . ?
Cl2 C12 1.35(2) . ?
Cl2 C11 2.14(2) . ?
C1 C6 1.399(6) . ?
C1 C2 1.403(6) . ?
C2 C3 1.376(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.367(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.373(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.532(5) . ?
C7 C8 1.532(8) . ?
C7 H7 0.9800 . ?
C8 C9 1.379(9) . ?
C8 C13 1.396(9) . ?
C9 C10 1.384(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.340(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.398(11) . ?
C11 H11 0.9300 . ?
C12 C13 1.373(8) . ?
C12 H12 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
C1 P1 C1 94.0(3) 4_565 . ?
C1 P1 C13 94.80(19) 4_565 . ?
C1 P1 C13 94.80(19) . . ?
C12 Cl2 C11 39.8(7) . . ?
C6 C1 C2 116.8(4) . . ?
C6 C1 P1 117.1(3) . . ?
C2 C1 P1 126.1(4) . . ?
C3 C2 C1 121.2(5) . . ?
C3 C2 Cl1 112.3(5) . . ?
C1 C2 Cl1 126.5(5) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C4 C3 C2 120.4(5) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.1(5) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.8(5) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 121.7(4) . . ?
C5 C6 C7 122.2(4) . . ?
C1 C6 C7 116.0(4) . . ?
C8 C7 C6 107.7(3) . . ?
C8 C7 C6 107.7(3) . 4_565 ?
C6 C7 C6 107.6(4) . 4_565 ?
C8 C7 H7 111.2 . . ?
C6 C7 H7 111.2 . . ?
C6 C7 H7 111.2 4_565 . ?
C9 C8 C13 119.1(6) . . ?
C9 C8 C7 124.4(6) . . ?
C13 C8 C7 116.5(5) . . ?
C8 C9 C10 120.1(7) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 121.1(6) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 119.7(6) . . ?
C10 C11 Cl2 158.0(7) . . ?
C12 C11 Cl2 38.3(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
Cl2 C11 H11 81.8 . . ?
Cl2 C12 C13 137.9(11) . . ?
Cl2 C12 C11 101.9(10) . . ?
C13 C12 C11 120.2(7) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C8 119.8(6) . . ?
C12 C13 P1 123.5(5) . . ?
C8 C13 P1 116.8(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
C1 P1 C1 C6 -48.3(4) 4_565 . . . ?
C13 P1 C1 C6 46.8(3) . . . . ?
C1 P1 C1 C2 130.3(3) 4_565 . . . ?
C13 P1 C1 C2 -134.6(4) . . . . ?
C6 C1 C2 C3 1.1(6) . . . . ?
P1 C1 C2 C3 -177.6(4) . . . . ?
C6 C1 C2 Cl1 -179.0(4) . . . . ?
P1 C1 C2 Cl1 2.4(6) . . . . ?
C1 C2 C3 C4 -1.1(8) . . . . ?
Cl1 C2 C3 C4 178.9(4) . . . . ?
C2 C3 C4 C5 0.8(8) . . . . ?
C3 C4 C5 C6 -0.5(7) . . . . ?
C4 C5 C6 C1 0.5(6) . . . . ?
C4 C5 C6 C7 177.6(4) . . . . ?
C2 C1 C6 C5 -0.7(6) . . . . ?
P1 C1 C6 C5 178.0(3) . . . . ?
C2 C1 C6 C7 -178.0(4) . . . . ?
P1 C1 C6 C7 0.7(5) . . . . ?
C5 C6 C7 C8 124.5(5) . . . . ?
C1 C6 C7 C8 -58.3(5) . . . . ?
C5 C6 C7 C6 -119.6(4) . . . 4_565 ?
C1 C6 C7 C6 57.6(5) . . . 4_565 ?
C6 C7 C8 C9 -122.1(3) . . . . ?
C6 C7 C8 C9 122.1(3) 4_565 . . . ?
C6 C7 C8 C13 57.9(3) . . . . ?
C6 C7 C8 C13 -57.9(3) 4_565 . . . ?
C13 C8 C9 C10 0.000(1) . . . . ?
C7 C8 C9 C10 180.000(1) . . . . ?
C8 C9 C10 C11 0.000(1) . . . . ?
C9 C10 C11 C12 0.000(1) . . . . ?
C9 C10 C11 Cl2 0.000(3) . . . . ?
C11 Cl2 C12 C13 180.000(1) . . . . ?
C10 C11 C12 Cl2 180.000(1) . . . . ?
C10 C11 C12 C13 0.000(1) . . . . ?
Cl2 C11 C12 C13 180.000(1) . . . . ?
Cl2 C12 C13 C8 180.000(1) . . . . ?
C11 C12 C13 C8 0.000(1) . . . . ?
Cl2 C12 C13 P1 0.000(1) . . . . ?
C11 C12 C13 P1 180.000(0) . . . . ?
C9 C8 C13 C12 0.000(1) . . . . ?
C7 C8 C13 C12 180.000(1) . . . . ?
C9 C8 C13 P1 180.000(1) . . . . ?
C7 C8 C13 P1 0.000(1) . . . . ?
C1 P1 C13 C12 -132.79(13) 4_565 . . . ?
C1 P1 C13 C12 132.79(13) . . . . ?
C1 P1 C13 C8 47.21(13) 4_565 . . . ?
C1 P1 C13 C8 -47.21(13) . . . . ?

_refine_diff_density_max         0.311
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.057



# start Validation Reply Form
_vrf_PLAT340_nt0589_Lei_trip-Cl  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00907 Ang.  
RESPONSE: Disordered structure and twinned crystal.
;
_vrf_PLAT911_nt0589_Lei_trip-Cl  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.598         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_nt0816_LHG203B
_database_code_depnum_ccdc_archive 'CCDC 2061860'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
;
(acetylacetonato)-carbonylrhodium-ortho-fluoro-9-phosphatriptycene 
complex
;
_chemical_name_common            
'Rh(acac)CO(o-fluoro-9-phosphatriptycene complex)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H19 F O3 P Rh'
_chemical_formula_sum            'C25 H19 F O3 P Rh'
_chemical_formula_weight         520.28

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'
F F 0.0727 0.0534 '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'
Rh Rh 0.0927 3.6045 '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                   9.5012(2)
_cell_length_b                   15.7667(5)
_cell_length_c                   16.6900(5)
_cell_angle_alpha                65.119(3)
_cell_angle_beta                 80.211(2)
_cell_angle_gamma                75.563(2)
_cell_volume                     2190.45(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    7474
_cell_measurement_theta_min      4.1000
_cell_measurement_theta_max      66.9250

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_F_000             1048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.055
_exptl_absorpt_coefficient_mu    7.277
_shelx_estimated_absorpt_T_min   0.502
_shelx_estimated_absorpt_T_max   0.690
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_T_max  0.727
_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            21134
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.927
_diffrn_reflns_theta_max         67.109
_diffrn_reflns_theta_full        67.109
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             7736
_reflns_number_gt                6495
_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    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0574P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7736
_refine_ls_number_parameters     583
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.1020
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
Rh1 Rh 0.99551(3) 0.76270(2) 0.05472(2) 0.04027(10) Uani 1 1 d . . . . .
P1 P 0.91612(9) 0.62840(6) 0.13746(6) 0.03489(19) Uani 1 1 d . . . . .
F1A F 0.7197(4) 0.7821(3) 0.2103(3) 0.0676(14) Uani 0.686(9) 1 d . . P A 1
F1B F 0.9053(10) 0.6819(6) -0.0700(5) 0.065(3) Uani 0.314(9) 1 d . . P A 2
O1 O 0.6929(4) 0.8483(3) 0.0069(3) 0.0928(14) Uani 1 1 d . . . . .
O2 O 1.0595(3) 0.8894(2) -0.0276(2) 0.0540(7) Uani 1 1 d . . . . .
O3 O 1.2077(3) 0.7023(2) 0.07933(18) 0.0491(6) Uani 1 1 d . . . . .
C1 C 0.7520(4) 0.6274(3) 0.2130(2) 0.0405(8) Uani 1 1 d . . . . .
C2 C 0.6713(5) 0.7027(3) 0.2342(3) 0.0542(10) Uani 1 1 d . . . . .
H2 H 0.706331 0.758824 0.214127 0.065 Uiso 0.314(9) 1 calc R U P A 2
C3 C 0.5395(5) 0.6959(4) 0.2847(3) 0.0707(14) Uani 1 1 d . . . . .
H3 H 0.486523 0.746996 0.298153 0.085 Uiso 1 1 calc R U . . .
C4 C 0.4876(5) 0.6128(4) 0.3148(3) 0.0689(14) Uani 1 1 d . . . . .
H4 H 0.397528 0.608792 0.346819 0.083 Uiso 1 1 calc R U . . .
C5 C 0.5683(4) 0.5352(4) 0.2977(3) 0.0539(10) Uani 1 1 d . . . . .
H5 H 0.533973 0.478632 0.319633 0.065 Uiso 1 1 calc R U . . .
C6 C 0.7002(4) 0.5421(3) 0.2480(2) 0.0409(8) Uani 1 1 d . . . . .
C7 C 0.7951(4) 0.4602(3) 0.2262(2) 0.0416(8) Uani 1 1 d . . . . .
H7 H 0.754087 0.402421 0.256790 0.050 Uiso 1 1 calc R U . . .
C8 C 0.9490(4) 0.4423(3) 0.2521(2) 0.0379(7) Uani 1 1 d . . . . .
C9 C 1.0182(4) 0.3548(3) 0.3101(3) 0.0455(9) Uani 1 1 d . . . . .
H9 H 0.970328 0.303667 0.335332 0.055 Uiso 1 1 calc R U . . .
C10 C 1.1596(5) 0.3432(3) 0.3308(3) 0.0507(9) Uani 1 1 d . . . . .
H10 H 1.205830 0.284589 0.370259 0.061 Uiso 1 1 calc R U . . .
C11 C 1.2308(5) 0.4181(3) 0.2930(3) 0.0510(9) Uani 1 1 d . . . . .
H11 H 1.325918 0.409438 0.306183 0.061 Uiso 1 1 calc R U . . .
C12 C 1.1625(4) 0.5073(3) 0.2349(2) 0.0428(8) Uani 1 1 d . . . . .
H12 H 1.210611 0.558328 0.210549 0.051 Uiso 1 1 calc R U . . .
C13 C 1.0227(4) 0.5186(3) 0.2143(2) 0.0367(7) Uani 1 1 d . . . . .
C14 C 0.8535(4) 0.5750(3) 0.0755(2) 0.0361(7) Uani 1 1 d . . . . .
C15 C 0.8557(4) 0.6106(3) -0.0163(3) 0.0455(9) Uani 1 1 d . . . . .
H15 H 0.893395 0.665187 -0.050550 0.055 Uiso 0.686(9) 1 calc R U P A 1
C16 C 0.8034(5) 0.5667(4) -0.0573(3) 0.0563(11) Uani 1 1 d . . . . .
H16 H 0.803500 0.592124 -0.118693 0.068 Uiso 1 1 calc R U . . .
C17 C 0.7510(5) 0.4848(4) -0.0070(3) 0.0622(12) Uani 1 1 d . . . . .
H17 H 0.717550 0.454191 -0.034809 0.075 Uiso 1 1 calc R U . . .
C18 C 0.7471(5) 0.4470(3) 0.0850(3) 0.0533(10) Uani 1 1 d . . . . .
H18 H 0.710874 0.391763 0.118666 0.064 Uiso 1 1 calc R U . . .
C19 C 0.7981(4) 0.4930(3) 0.1259(2) 0.0406(8) Uani 1 1 d . . . . .
C20 C 0.8094(5) 0.8148(3) 0.0268(3) 0.0623(12) Uani 1 1 d . . . . .
C21 C 1.2025(5) 1.0022(3) -0.1099(4) 0.0706(14) Uani 1 1 d . . . . .
H21A H 1.177665 1.011840 -0.166924 0.106 Uiso 1 1 calc R U . . .
H21B H 1.301040 1.009702 -0.114144 0.106 Uiso 1 1 calc R U . . .
H21C H 1.137802 1.048128 -0.090127 0.106 Uiso 1 1 calc R U . . .
C22 C 1.1885(4) 0.9041(3) -0.0453(3) 0.0454(9) Uani 1 1 d . . . . .
C23 C 1.3123(4) 0.8364(3) -0.0131(3) 0.0464(9) Uani 1 1 d . . . . .
H23 H 1.400914 0.856259 -0.032060 0.056 Uiso 1 1 calc R U . . .
C24 C 1.3172(4) 0.7414(3) 0.0450(2) 0.0447(8) Uani 1 1 d . . . . .
C25 C 1.4625(5) 0.6766(4) 0.0698(4) 0.0703(14) Uani 1 1 d . . . . .
H25A H 1.462143 0.644646 0.133083 0.105 Uiso 1 1 calc R U . . .
H25B H 1.537645 0.713534 0.047908 0.105 Uiso 1 1 calc R U . . .
H25C H 1.480614 0.630208 0.044227 0.105 Uiso 1 1 calc R U . . .
Rh2 Rh 0.32289(3) 0.79525(2) 0.56573(2) 0.04287(10) Uani 1 1 d . . . . .
P2 P 0.18495(10) 0.80650(7) 0.46463(6) 0.0376(2) Uani 1 1 d . . . . .
F2A F 0.4147(3) 0.9390(2) 0.35071(19) 0.0634(9) Uani 0.935(7) 1 d D . P B 1
F2B F 0.326(4) 0.597(3) 0.576(2) 0.065(8) Uani 0.065(7) 1 d D U P B 2
O4 O 0.5778(4) 0.7162(3) 0.4714(3) 0.0854(11) Uani 1 1 d . . . . .
O5 O 0.4581(3) 0.7828(3) 0.6566(2) 0.0669(9) Uani 1 1 d . . . . .
O6 O 0.1501(3) 0.8359(2) 0.64139(18) 0.0519(7) Uani 1 1 d . . . . .
C26 C 0.2292(4) 0.8668(3) 0.3451(2) 0.0394(8) Uani 1 1 d . . . . .
C27 C 0.3346(4) 0.9212(3) 0.3036(3) 0.0496(9) Uani 1 1 d D . . . .
H27 H 0.389675 0.932219 0.337954 0.059 Uiso 0.065(7) 1 calc R U P B 2
C28 C 0.3612(6) 0.9600(4) 0.2114(3) 0.0646(12) Uani 1 1 d . . . . .
H28 H 0.431993 0.996904 0.184740 0.078 Uiso 1 1 calc R U . . .
C29 C 0.2812(6) 0.9427(4) 0.1615(3) 0.0673(13) Uani 1 1 d . . . . .
H29 H 0.300764 0.966022 0.100358 0.081 Uiso 1 1 calc R U . . .
C30 C 0.1723(5) 0.8916(4) 0.1996(3) 0.0593(11) Uani 1 1 d . . . . .
H30 H 0.117646 0.881520 0.164318 0.071 Uiso 1 1 calc R U . . .
C31 C 0.1441(4) 0.8551(3) 0.2909(2) 0.0458(9) Uani 1 1 d . . . . .
C32 C 0.0216(4) 0.8014(3) 0.3381(3) 0.0505(9) Uani 1 1 d . . . . .
H32 H -0.034944 0.799908 0.294980 0.061 Uiso 1 1 calc R U . . .
C33 C -0.0753(4) 0.8504(3) 0.3945(3) 0.0488(9) Uani 1 1 d . . . . .
C34 C -0.2219(5) 0.8879(4) 0.3841(3) 0.0601(11) Uani 1 1 d . . . . .
H34 H -0.266749 0.881962 0.341825 0.072 Uiso 1 1 calc R U . . .
C35 C -0.3021(5) 0.9343(4) 0.4366(4) 0.0674(13) Uani 1 1 d . . . . .
H35 H -0.400600 0.960127 0.428765 0.081 Uiso 1 1 calc R U . . .
C36 C -0.2380(5) 0.9427(4) 0.5004(3) 0.0599(11) Uani 1 1 d . . . . .
H36 H -0.293458 0.973606 0.535549 0.072 Uiso 1 1 calc R U . . .
C37 C -0.0910(4) 0.9052(3) 0.5123(3) 0.0471(9) Uani 1 1 d . . . . .
H37 H -0.047217 0.910690 0.555286 0.057 Uiso 1 1 calc R U . . .
C38 C -0.0100(4) 0.8594(3) 0.4592(2) 0.0416(8) Uani 1 1 d . . . . .
C39 C 0.0904(4) 0.7011(3) 0.3973(3) 0.0480(9) Uani 1 1 d . . . . .
C40 C 0.0781(5) 0.6191(4) 0.3898(3) 0.0609(12) Uani 1 1 d . . . . .
H40 H 0.022683 0.623158 0.346932 0.073 Uiso 1 1 calc R U . . .
C41 C 0.1490(6) 0.5305(4) 0.4467(4) 0.0688(14) Uani 1 1 d . . . . .
H41 H 0.141047 0.475416 0.441566 0.083 Uiso 1 1 calc R U . . .
C42 C 0.2301(6) 0.5241(3) 0.5099(3) 0.0659(13) Uani 1 1 d . . . . .
H42 H 0.276355 0.464512 0.547912 0.079 Uiso 1 1 calc R U . . .
C43 C 0.2438(5) 0.6050(3) 0.5178(3) 0.0548(10) Uani 1 1 d D U . . .
H43 H 0.299293 0.600237 0.560915 0.066 Uiso 0.935(7) 1 calc R U P B 1
C44 C 0.1742(4) 0.6942(3) 0.4611(2) 0.0418(8) Uani 1 1 d . . . . .
C45 C 0.4778(5) 0.7488(3) 0.5064(3) 0.0556(10) Uani 1 1 d . . . . .
C46 C 0.5450(8) 0.7874(7) 0.7768(5) 0.111(3) Uani 1 1 d . . . . .
H46A H 0.582821 0.720894 0.809008 0.167 Uiso 1 1 calc R U . . .
H46B H 0.512085 0.818144 0.817418 0.167 Uiso 1 1 calc R U . . .
H46C H 0.620310 0.816346 0.735745 0.167 Uiso 1 1 calc R U . . .
C47 C 0.4186(6) 0.7983(4) 0.7265(3) 0.0668(13) Uani 1 1 d . . . . .
C48 C 0.2776(6) 0.8232(4) 0.7571(3) 0.0641(12) Uani 1 1 d . . . . .
H48 H 0.264616 0.828747 0.811334 0.077 Uiso 1 1 calc R U . . .
C49 C 0.1534(5) 0.8407(3) 0.7158(3) 0.0548(10) Uani 1 1 d . . . . .
C50 C 0.0052(6) 0.8703(5) 0.7570(4) 0.0831(17) Uani 1 1 d . . . . .
H50A H -0.037735 0.934084 0.719558 0.125 Uiso 1 1 calc R U . . .
H50B H 0.015418 0.867913 0.814133 0.125 Uiso 1 1 calc R U . . .
H50C H -0.056359 0.827559 0.763285 0.125 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
Rh1 C20 1.803(5) . ?
Rh1 O3 2.034(3) . ?
Rh1 O2 2.064(3) . ?
Rh1 P1 2.2230(9) . ?
P1 C14 1.823(4) . ?
P1 C1 1.830(4) . ?
P1 C13 1.835(4) . ?
F1A C2 1.320(6) . ?
F1B C15 1.249(9) . ?
O1 C20 1.140(6) . ?
O2 C22 1.265(5) . ?
O3 C24 1.269(5) . ?
C1 C2 1.390(6) . ?
C1 C6 1.400(6) . ?
C2 C3 1.386(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.522(6) . ?
C7 C8 1.520(5) . ?
C7 C19 1.528(5) . ?
C7 H7 0.9800 . ?
C8 C9 1.384(5) . ?
C8 C13 1.403(5) . ?
C9 C10 1.393(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.369(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.397(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.379(5) . ?
C12 H12 0.9300 . ?
C14 C19 1.389(5) . ?
C14 C15 1.392(5) . ?
C15 C16 1.371(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.373(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.391(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.389(6) . ?
C18 H18 0.9300 . ?
C21 C22 1.491(6) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.385(6) . ?
C23 C24 1.394(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.503(6) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
Rh2 C45 1.806(5) . ?
Rh2 O6 2.038(3) . ?
Rh2 O5 2.067(3) . ?
Rh2 P2 2.2318(9) . ?
P2 C44 1.825(4) . ?
P2 C38 1.832(4) . ?
P2 C26 1.838(4) . ?
F2A C27 1.332(5) . ?
F2B C43 1.293(19) . ?
O4 C45 1.153(6) . ?
O5 C47 1.268(5) . ?
O6 C49 1.282(5) . ?
C26 C27 1.382(6) . ?
C26 C31 1.403(6) . ?
C27 C28 1.399(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.362(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.373(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.388(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.519(6) . ?
C32 C39 1.515(6) . ?
C32 C33 1.514(6) . ?
C32 H32 0.9800 . ?
C33 C34 1.380(6) . ?
C33 C38 1.404(6) . ?
C34 C35 1.386(7) . ?
C34 H34 0.9300 . ?
C35 C36 1.380(7) . ?
C35 H35 0.9300 . ?
C36 C37 1.387(6) . ?
C36 H36 0.9300 . ?
C37 C38 1.390(6) . ?
C37 H37 0.9300 . ?
C39 C44 1.389(6) . ?
C39 C40 1.385(6) . ?
C40 C41 1.392(8) . ?
C40 H40 0.9300 . ?
C41 C42 1.366(8) . ?
C41 H41 0.9300 . ?
C42 C43 1.377(7) . ?
C42 H42 0.9300 . ?
C43 C44 1.392(6) . ?
C43 H43 0.9300 . ?
C46 C47 1.516(8) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C48 1.373(7) . ?
C48 C49 1.377(7) . ?
C48 H48 0.9300 . ?
C49 C50 1.511(7) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 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
C20 Rh1 O3 176.5(2) . . ?
C20 Rh1 O2 90.83(16) . . ?
O3 Rh1 O2 88.82(11) . . ?
C20 Rh1 P1 86.16(14) . . ?
O3 Rh1 P1 94.06(8) . . ?
O2 Rh1 P1 176.40(9) . . ?
C14 P1 C1 95.58(16) . . ?
C14 P1 C13 97.49(16) . . ?
C1 P1 C13 95.40(16) . . ?
C14 P1 Rh1 114.83(12) . . ?
C1 P1 Rh1 121.37(13) . . ?
C13 P1 Rh1 125.84(12) . . ?
C22 O2 Rh1 126.7(3) . . ?
C24 O3 Rh1 126.9(3) . . ?
C2 C1 C6 118.1(3) . . ?
C2 C1 P1 127.1(3) . . ?
C6 C1 P1 114.7(3) . . ?
F1A C2 C3 117.3(4) . . ?
F1A C2 C1 121.4(4) . . ?
C3 C2 C1 121.2(5) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.6(4) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 119.6(5) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 120.8(4) . . ?
C5 C6 C7 122.8(4) . . ?
C1 C6 C7 116.4(3) . . ?
C8 C7 C6 109.6(3) . . ?
C8 C7 C19 109.2(3) . . ?
C6 C7 C19 106.1(3) . . ?
C8 C7 H7 110.6 . . ?
C6 C7 H7 110.6 . . ?
C19 C7 H7 110.6 . . ?
C9 C8 C13 119.4(3) . . ?
C9 C8 C7 122.9(3) . . ?
C13 C8 C7 117.6(3) . . ?
C8 C9 C10 119.9(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 121.0(4) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 118.9(4) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C8 120.7(3) . . ?
C12 C13 P1 125.8(3) . . ?
C8 C13 P1 113.5(3) . . ?
C19 C14 C15 118.9(3) . . ?
C19 C14 P1 115.9(3) . . ?
C15 C14 P1 125.2(3) . . ?
F1B C15 C16 112.7(5) . . ?
F1B C15 C14 126.1(5) . . ?
C16 C15 C14 121.2(4) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 119.5(4) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C16 C17 C18 121.0(4) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 119.0(4) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C14 120.4(4) . . ?
C18 C19 C7 123.9(4) . . ?
C14 C19 C7 115.7(3) . . ?
O1 C20 Rh1 178.2(5) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O2 C22 C23 125.4(4) . . ?
O2 C22 C21 114.8(4) . . ?
C23 C22 C21 119.8(4) . . ?
C22 C23 C24 126.4(4) . . ?
C22 C23 H23 116.8 . . ?
C24 C23 H23 116.8 . . ?
O3 C24 C23 125.7(4) . . ?
O3 C24 C25 115.1(4) . . ?
C23 C24 C25 119.2(4) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C45 Rh2 O6 174.97(17) . . ?
C45 Rh2 O5 89.93(16) . . ?
O6 Rh2 O5 88.34(12) . . ?
C45 Rh2 P2 87.71(13) . . ?
O6 Rh2 P2 94.02(8) . . ?
O5 Rh2 P2 177.64(9) . . ?
C44 P2 C38 97.21(17) . . ?
C44 P2 C26 95.57(17) . . ?
C38 P2 C26 94.61(16) . . ?
C44 P2 Rh2 116.05(13) . . ?
C38 P2 Rh2 124.68(13) . . ?
C26 P2 Rh2 122.30(13) . . ?
C47 O5 Rh2 126.3(3) . . ?
C49 O6 Rh2 127.1(3) . . ?
C27 C26 C31 117.4(3) . . ?
C27 C26 P2 127.9(3) . . ?
C31 C26 P2 114.7(3) . . ?
F2A C27 C26 120.6(4) . . ?
F2A C27 C28 117.4(4) . . ?
C26 C27 C28 122.0(4) . . ?
C26 C27 H27 119.0 . . ?
C28 C27 H27 119.0 . . ?
C29 C28 C27 118.7(4) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
C28 C29 C30 121.4(4) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C29 C30 C31 119.7(4) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C30 C31 C26 120.7(4) . . ?
C30 C31 C32 123.1(4) . . ?
C26 C31 C32 116.2(3) . . ?
C39 C32 C33 109.4(3) . . ?
C39 C32 C31 107.5(3) . . ?
C33 C32 C31 108.8(3) . . ?
C39 C32 H32 110.4 . . ?
C33 C32 H32 110.4 . . ?
C31 C32 H32 110.4 . . ?
C34 C33 C38 119.1(4) . . ?
C34 C33 C32 123.5(4) . . ?
C38 C33 C32 117.4(4) . . ?
C33 C34 C35 119.9(4) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.9(4) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C36 C37 120.1(4) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C36 C37 C38 119.1(4) . . ?
C36 C37 H37 120.5 . . ?
C38 C37 H37 120.5 . . ?
C37 C38 C33 120.9(4) . . ?
C37 C38 P2 125.3(3) . . ?
C33 C38 P2 113.9(3) . . ?
C44 C39 C40 119.6(4) . . ?
C44 C39 C32 115.7(4) . . ?
C40 C39 C32 124.7(4) . . ?
C39 C40 C41 119.7(5) . . ?
C39 C40 H40 120.1 . . ?
C41 C40 H40 120.1 . . ?
C42 C41 C40 120.4(4) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 C43 120.5(5) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
F2B C43 C42 118.9(18) . . ?
F2B C43 C44 121.3(18) . . ?
C42 C43 C44 119.8(5) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C39 C44 C43 120.0(4) . . ?
C39 C44 P2 116.1(3) . . ?
C43 C44 P2 123.9(3) . . ?
O4 C45 Rh2 177.4(4) . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O5 C47 C48 126.1(4) . . ?
O5 C47 C46 113.4(5) . . ?
C48 C47 C46 120.5(4) . . ?
C47 C48 C49 126.7(4) . . ?
C47 C48 H48 116.7 . . ?
C49 C48 H48 116.7 . . ?
O6 C49 C48 125.4(4) . . ?
O6 C49 C50 114.1(4) . . ?
C48 C49 C50 120.5(4) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 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 C1 C2 -131.0(4) . . . . ?
C13 P1 C1 C2 130.9(4) . . . . ?
Rh1 P1 C1 C2 -7.4(4) . . . . ?
C14 P1 C1 C6 45.0(3) . . . . ?
C13 P1 C1 C6 -53.1(3) . . . . ?
Rh1 P1 C1 C6 168.6(2) . . . . ?
C6 C1 C2 F1A 173.9(4) . . . . ?
P1 C1 C2 F1A -10.3(6) . . . . ?
C6 C1 C2 C3 -3.3(6) . . . . ?
P1 C1 C2 C3 172.6(4) . . . . ?
F1A C2 C3 C4 -177.0(5) . . . . ?
C1 C2 C3 C4 0.2(8) . . . . ?
C2 C3 C4 C5 2.4(8) . . . . ?
C3 C4 C5 C6 -1.8(7) . . . . ?
C4 C5 C6 C1 -1.3(6) . . . . ?
C4 C5 C6 C7 -179.9(4) . . . . ?
C2 C1 C6 C5 3.8(6) . . . . ?
P1 C1 C6 C5 -172.5(3) . . . . ?
C2 C1 C6 C7 -177.6(4) . . . . ?
P1 C1 C6 C7 6.1(4) . . . . ?
C5 C6 C7 C8 -127.7(4) . . . . ?
C1 C6 C7 C8 53.7(4) . . . . ?
C5 C6 C7 C19 114.5(4) . . . . ?
C1 C6 C7 C19 -64.1(4) . . . . ?
C6 C7 C8 C9 123.2(4) . . . . ?
C19 C7 C8 C9 -121.0(4) . . . . ?
C6 C7 C8 C13 -57.4(4) . . . . ?
C19 C7 C8 C13 58.5(4) . . . . ?
C13 C8 C9 C10 0.3(5) . . . . ?
C7 C8 C9 C10 179.8(3) . . . . ?
C8 C9 C10 C11 -0.7(6) . . . . ?
C9 C10 C11 C12 1.3(6) . . . . ?
C10 C11 C12 C13 -1.5(6) . . . . ?
C11 C12 C13 C8 1.1(5) . . . . ?
C11 C12 C13 P1 -178.2(3) . . . . ?
C9 C8 C13 C12 -0.5(5) . . . . ?
C7 C8 C13 C12 180.0(3) . . . . ?
C9 C8 C13 P1 178.9(3) . . . . ?
C7 C8 C13 P1 -0.6(4) . . . . ?
C14 P1 C13 C12 132.7(3) . . . . ?
C1 P1 C13 C12 -130.9(3) . . . . ?
Rh1 P1 C13 C12 4.6(4) . . . . ?
C14 P1 C13 C8 -46.7(3) . . . . ?
C1 P1 C13 C8 49.7(3) . . . . ?
Rh1 P1 C13 C8 -174.81(19) . . . . ?
C1 P1 C14 C19 -49.2(3) . . . . ?
C13 P1 C14 C19 47.0(3) . . . . ?
Rh1 P1 C14 C19 -177.6(2) . . . . ?
C1 P1 C14 C15 130.0(3) . . . . ?
C13 P1 C14 C15 -133.8(3) . . . . ?
Rh1 P1 C14 C15 1.6(3) . . . . ?
C19 C14 C15 F1B -178.1(6) . . . . ?
P1 C14 C15 F1B 2.7(7) . . . . ?
C19 C14 C15 C16 0.5(5) . . . . ?
P1 C14 C15 C16 -178.6(3) . . . . ?
F1B C15 C16 C17 177.2(6) . . . . ?
C14 C15 C16 C17 -1.5(6) . . . . ?
C15 C16 C17 C18 1.5(6) . . . . ?
C16 C17 C18 C19 -0.4(6) . . . . ?
C17 C18 C19 C14 -0.6(6) . . . . ?
C17 C18 C19 C7 178.0(4) . . . . ?
C15 C14 C19 C18 0.6(5) . . . . ?
P1 C14 C19 C18 179.8(3) . . . . ?
C15 C14 C19 C7 -178.2(3) . . . . ?
P1 C14 C19 C7 1.0(4) . . . . ?
C8 C7 C19 C18 122.8(4) . . . . ?
C6 C7 C19 C18 -119.1(4) . . . . ?
C8 C7 C19 C14 -58.4(4) . . . . ?
C6 C7 C19 C14 59.6(4) . . . . ?
Rh1 O2 C22 C23 0.8(6) . . . . ?
Rh1 O2 C22 C21 177.8(3) . . . . ?
O2 C22 C23 C24 -0.9(7) . . . . ?
C21 C22 C23 C24 -177.8(4) . . . . ?
Rh1 O3 C24 C23 4.1(6) . . . . ?
Rh1 O3 C24 C25 -174.8(3) . . . . ?
C22 C23 C24 O3 -1.7(7) . . . . ?
C22 C23 C24 C25 177.2(4) . . . . ?
C44 P2 C26 C27 -134.7(4) . . . . ?
C38 P2 C26 C27 127.6(4) . . . . ?
Rh2 P2 C26 C27 -9.0(4) . . . . ?
C44 P2 C26 C31 45.2(3) . . . . ?
C38 P2 C26 C31 -52.5(3) . . . . ?
Rh2 P2 C26 C31 170.9(2) . . . . ?
C31 C26 C27 F2A 176.9(4) . . . . ?
P2 C26 C27 F2A -3.3(6) . . . . ?
C31 C26 C27 C28 -2.7(6) . . . . ?
P2 C26 C27 C28 177.2(3) . . . . ?
F2A C27 C28 C29 179.8(4) . . . . ?
C26 C27 C28 C29 -0.7(7) . . . . ?
C27 C28 C29 C30 2.6(8) . . . . ?
C28 C29 C30 C31 -1.2(8) . . . . ?
C29 C30 C31 C26 -2.3(7) . . . . ?
C29 C30 C31 C32 177.3(4) . . . . ?
C27 C26 C31 C30 4.1(6) . . . . ?
P2 C26 C31 C30 -175.8(3) . . . . ?
C27 C26 C31 C32 -175.5(4) . . . . ?
P2 C26 C31 C32 4.6(5) . . . . ?
C30 C31 C32 C39 117.6(4) . . . . ?
C26 C31 C32 C39 -62.8(4) . . . . ?
C30 C31 C32 C33 -124.1(4) . . . . ?
C26 C31 C32 C33 55.6(5) . . . . ?
C39 C32 C33 C34 -122.4(5) . . . . ?
C31 C32 C33 C34 120.4(5) . . . . ?
C39 C32 C33 C38 59.1(5) . . . . ?
C31 C32 C33 C38 -58.1(5) . . . . ?
C38 C33 C34 C35 0.5(7) . . . . ?
C32 C33 C34 C35 -177.9(5) . . . . ?
C33 C34 C35 C36 -0.8(8) . . . . ?
C34 C35 C36 C37 0.5(8) . . . . ?
C35 C36 C37 C38 0.0(7) . . . . ?
C36 C37 C38 C33 -0.3(6) . . . . ?
C36 C37 C38 P2 179.5(3) . . . . ?
C34 C33 C38 C37 0.1(6) . . . . ?
C32 C33 C38 C37 178.6(4) . . . . ?
C34 C33 C38 P2 -179.8(3) . . . . ?
C32 C33 C38 P2 -1.2(5) . . . . ?
C44 P2 C38 C37 134.3(4) . . . . ?
C26 P2 C38 C37 -129.4(4) . . . . ?
Rh2 P2 C38 C37 5.6(4) . . . . ?
C44 P2 C38 C33 -45.8(3) . . . . ?
C26 P2 C38 C33 50.4(3) . . . . ?
Rh2 P2 C38 C33 -174.6(2) . . . . ?
C33 C32 C39 C44 -58.7(4) . . . . ?
C31 C32 C39 C44 59.3(4) . . . . ?
C33 C32 C39 C40 123.2(4) . . . . ?
C31 C32 C39 C40 -118.8(4) . . . . ?
C44 C39 C40 C41 0.5(6) . . . . ?
C32 C39 C40 C41 178.5(4) . . . . ?
C39 C40 C41 C42 0.2(7) . . . . ?
C40 C41 C42 C43 -0.5(7) . . . . ?
C41 C42 C43 F2B -177(2) . . . . ?
C41 C42 C43 C44 0.1(7) . . . . ?
C40 C39 C44 C43 -0.8(6) . . . . ?
C32 C39 C44 C43 -179.0(3) . . . . ?
C40 C39 C44 P2 179.4(3) . . . . ?
C32 C39 C44 P2 1.1(4) . . . . ?
F2B C43 C44 C39 178(2) . . . . ?
C42 C43 C44 C39 0.5(6) . . . . ?
F2B C43 C44 P2 -2(2) . . . . ?
C42 C43 C44 P2 -179.7(3) . . . . ?
C38 P2 C44 C39 46.6(3) . . . . ?
C26 P2 C44 C39 -48.8(3) . . . . ?
Rh2 P2 C44 C39 -179.0(2) . . . . ?
C38 P2 C44 C43 -133.2(3) . . . . ?
C26 P2 C44 C43 131.4(3) . . . . ?
Rh2 P2 C44 C43 1.2(4) . . . . ?
Rh2 O5 C47 C48 2.5(8) . . . . ?
Rh2 O5 C47 C46 -177.2(5) . . . . ?
O5 C47 C48 C49 -3.6(9) . . . . ?
C46 C47 C48 C49 176.0(6) . . . . ?
Rh2 O6 C49 C48 3.3(7) . . . . ?
Rh2 O6 C49 C50 -177.9(4) . . . . ?
C47 C48 C49 O6 0.5(8) . . . . ?
C47 C48 C49 C50 -178.3(6) . . . . ?

_refine_diff_density_max         0.915
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.091



# start Validation Reply Form
_vrf_PLAT911_nt0816_LHG203B      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.597         96 Report
RESPONSE: These reflections are missing in the highest resolution shell 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_nt0764_LHG168
_database_code_depnum_ccdc_archive 'CCDC 2061852'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
(5R/S,10S/R)-2-(tert-butyl)-6-chloro-10H-5,10-[1,2]benzenoacridophosphine
_chemical_name_common            
(5R/S,10S/R)-2-(tert-butyl)-6-chloro-10H-5,10-[1,2]benzenoacridophosphine
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H20 Cl P'
_chemical_formula_sum            'C23 H20 Cl P'
_chemical_formula_weight         362.81

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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

_cell_length_a                   8.1914(2)
_cell_length_b                   13.7899(4)
_cell_length_c                   8.6284(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.365(3)
_cell_angle_gamma                90
_cell_volume                     961.67(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2317
_cell_measurement_theta_min      6.3180
_cell_measurement_theta_max      66.7210

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_F_000             380
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.028
_exptl_absorpt_coefficient_mu    2.537
_shelx_estimated_absorpt_T_min   0.527
_shelx_estimated_absorpt_T_max   0.932
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     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            2998
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.195
_diffrn_reflns_theta_max         67.221
_diffrn_reflns_theta_full        67.221
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             2998
_reflns_number_gt                2585
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component 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)+(0.0460P)²+0.6181P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2998
_refine_ls_number_parameters     140
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1553
_refine_ls_wR_factor_gt          0.1530
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.145
_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
Cl1 Cl 0.8841(3) 0.44281(17) 0.5730(3) 0.0834(7) Uani 0.5 1 d . . P A 1
P1 P 0.65480(16) 0.250000 0.46590(15) 0.0517(4) Uani 1 2 d S T P . .
C1 C 0.5957(4) 0.3479(3) 0.5906(4) 0.0522(8) Uani 1 1 d . . . . .
C2 C 0.6916(5) 0.4293(3) 0.6361(4) 0.0615(9) Uani 1 1 d . . . . .
H2 H 0.793401 0.436404 0.602876 0.074 Uiso 0.5 1 calc R U P A 2
C3 C 0.6385(6) 0.4996(3) 0.7293(5) 0.0725(12) Uani 1 1 d . . . . .
H3 H 0.704370 0.553461 0.759188 0.087 Uiso 1 1 calc R U . . .
C4 C 0.4875(6) 0.4899(3) 0.7785(5) 0.0715(12) Uani 1 1 d . . . . .
H4 H 0.452044 0.537189 0.842371 0.086 Uiso 1 1 calc R U . . .
C5 C 0.3880(5) 0.4101(3) 0.7331(4) 0.0617(10) Uani 1 1 d . . . . .
H5 H 0.285575 0.404475 0.765500 0.074 Uiso 1 1 calc R U . . .
C6 C 0.4405(4) 0.3390(2) 0.6401(4) 0.0519(8) Uani 1 1 d . . . . .
C7 C 0.3393(6) 0.250000 0.5834(5) 0.0497(11) Uani 1 2 d S T P . .
H7 H 0.233501 0.250000 0.622547 0.060 Uiso 1 2 calc R U P . .
C8 C 0.3117(6) 0.250000 0.4035(5) 0.0439(10) Uani 1 2 d S T P . .
C9 C 0.1581(6) 0.250000 0.3118(5) 0.0471(11) Uani 1 2 d S T P . .
H9 H 0.064183 0.250000 0.359525 0.056 Uiso 1 2 calc R U P . .
C10 C 0.1406(6) 0.250000 0.1474(5) 0.0458(11) Uani 1 2 d S T P . .
C11 C -0.0320(6) 0.250000 0.0488(6) 0.0553(13) Uani 1 2 d S T P . .
C12 C -0.1257(5) 0.1587(3) 0.0858(5) 0.0732(12) Uani 1 1 d . . . . .
H12A H -0.136583 0.158721 0.194905 0.110 Uiso 1 1 calc R U . . .
H12B H -0.065649 0.102134 0.062977 0.110 Uiso 1 1 calc R U . . .
H12C H -0.233635 0.158246 0.022608 0.110 Uiso 1 1 calc R U . . .
C13 C -0.0275(8) 0.250000 -0.1281(7) 0.085(2) Uani 1 2 d DS T P . .
H13A H -0.137(3) 0.250000 -0.189(7) 0.128 Uiso 1 2 d DS U P . .
H13B H 0.031(2) 0.3070(2) -0.153(4) 0.128 Uiso 1 1 d D U . . .
C14 C 0.2841(6) 0.250000 0.0800(5) 0.0464(11) Uani 1 2 d S T P . .
H14 H 0.275817 0.250000 -0.028796 0.056 Uiso 1 2 calc R U P . .
C15 C 0.4372(6) 0.250000 0.1718(5) 0.0475(10) Uani 1 2 d S T P . .
H15 H 0.531193 0.250000 0.124134 0.057 Uiso 1 2 calc R U P . .
C16 C 0.4548(6) 0.250000 0.3344(5) 0.0436(10) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C2 1.760(5) . ?
P1 C16 1.835(5) . ?
P1 C1 1.840(4) . ?
P1 C1 1.840(4) 4_565 ?
C1 C2 1.390(5) . ?
C1 C6 1.411(5) . ?
C2 C3 1.374(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.378(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.516(4) . ?
C7 C8 1.532(6) . ?
C7 H7 0.9800 . ?
C8 C9 1.372(6) . ?
C8 C16 1.399(6) . ?
C9 C10 1.402(6) . ?
C9 H9 0.9300 . ?
C10 C14 1.394(7) . ?
C10 C11 1.526(6) . ?
C11 C13 1.533(7) . ?
C11 C12 1.535(5) 4_565 ?
C11 C12 1.535(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.961(7) . ?
C13 H13B 0.961(6) . ?
C13 H13B 0.961(6) 4_565 ?
C14 C15 1.370(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.387(6) . ?
C15 H15 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
C16 P1 C1 93.92(15) . . ?
C16 P1 C1 93.92(15) . 4_565 ?
C1 P1 C1 94.4(2) . 4_565 ?
C2 C1 C6 118.7(3) . . ?
C2 C1 P1 124.6(3) . . ?
C6 C1 P1 116.6(3) . . ?
C3 C2 C1 121.1(4) . . ?
C3 C2 Cl1 119.4(3) . . ?
C1 C2 Cl1 119.4(3) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 119.9(4) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 120.3(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 119.7(3) . . ?
C5 C6 C7 123.9(4) . . ?
C1 C6 C7 116.4(3) . . ?
C6 C7 C6 108.0(4) 4_565 . ?
C6 C7 C8 108.1(3) 4_565 . ?
C6 C7 C8 108.1(3) . . ?
C6 C7 H7 110.9 4_565 . ?
C6 C7 H7 110.9 . . ?
C8 C7 H7 110.9 . . ?
C9 C8 C16 120.5(4) . . ?
C9 C8 C7 123.7(4) . . ?
C16 C8 C7 115.9(4) . . ?
C8 C9 C10 121.1(4) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C14 C10 C9 117.9(4) . . ?
C14 C10 C11 122.3(4) . . ?
C9 C10 C11 119.8(4) . . ?
C10 C11 C13 112.7(4) . . ?
C10 C11 C12 109.5(3) . 4_565 ?
C13 C11 C12 107.5(3) . 4_565 ?
C10 C11 C12 109.5(3) . . ?
C13 C11 C12 107.5(3) . . ?
C12 C11 C12 110.2(4) 4_565 . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 112(4) . . ?
C11 C13 H13B 108(2) . . ?
H13A C13 H13B 109.4(10) . . ?
C11 C13 H13B 108(2) . 4_565 ?
H13A C13 H13B 109.4(10) . 4_565 ?
H13B C13 H13B 109.6(13) . 4_565 ?
C15 C14 C10 120.9(4) . . ?
C15 C14 H14 119.5 . . ?
C10 C14 H14 119.5 . . ?
C14 C15 C16 121.3(5) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C15 C16 C8 118.4(4) . . ?
C15 C16 P1 124.1(4) . . ?
C8 C16 P1 117.5(3) . . ?

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
C16 P1 C1 C2 -131.3(3) . . . . ?
C1 P1 C1 C2 134.4(2) 4_565 . . . ?
C16 P1 C1 C6 47.6(3) . . . . ?
C1 P1 C1 C6 -46.6(3) 4_565 . . . ?
C6 C1 C2 C3 0.9(5) . . . . ?
P1 C1 C2 C3 179.8(3) . . . . ?
C6 C1 C2 Cl1 -179.0(3) . . . . ?
P1 C1 C2 Cl1 -0.1(4) . . . . ?
C1 C2 C3 C4 -0.3(6) . . . . ?
Cl1 C2 C3 C4 179.6(3) . . . . ?
C2 C3 C4 C5 -0.6(6) . . . . ?
C3 C4 C5 C6 0.9(6) . . . . ?
C4 C5 C6 C1 -0.3(5) . . . . ?
C4 C5 C6 C7 -179.2(3) . . . . ?
C2 C1 C6 C5 -0.6(5) . . . . ?
P1 C1 C6 C5 -179.6(3) . . . . ?
C2 C1 C6 C7 178.4(3) . . . . ?
P1 C1 C6 C7 -0.6(4) . . . . ?
C5 C6 C7 C6 -122.2(4) . . . 4_565 ?
C1 C6 C7 C6 58.8(4) . . . 4_565 ?
C5 C6 C7 C8 121.1(4) . . . . ?
C1 C6 C7 C8 -57.8(4) . . . . ?
C6 C7 C8 C9 121.7(3) 4_565 . . . ?
C6 C7 C8 C9 -121.7(3) . . . . ?
C6 C7 C8 C16 -58.3(3) 4_565 . . . ?
C6 C7 C8 C16 58.3(3) . . . . ?
C16 C8 C9 C10 0.000(1) . . . . ?
C7 C8 C9 C10 180.000(1) . . . . ?
C8 C9 C10 C14 0.000(1) . . . . ?
C8 C9 C10 C11 180.000(1) . . . . ?
C14 C10 C11 C13 0.000(0) . . . . ?
C9 C10 C11 C13 180.000(0) . . . . ?
C14 C10 C11 C12 -119.6(3) . . . 4_565 ?
C9 C10 C11 C12 60.4(3) . . . 4_565 ?
C14 C10 C11 C12 119.6(3) . . . . ?
C9 C10 C11 C12 -60.4(3) . . . . ?
C9 C10 C14 C15 0.000(0) . . . . ?
C11 C10 C14 C15 180.000(0) . . . . ?
C10 C14 C15 C16 0.000(0) . . . . ?
C14 C15 C16 C8 0.000(1) . . . . ?
C14 C15 C16 P1 180.000(0) . . . . ?
C9 C8 C16 C15 0.000(1) . . . . ?
C7 C8 C16 C15 180.000(1) . . . . ?
C9 C8 C16 P1 180.000(0) . . . . ?
C7 C8 C16 P1 0.000(1) . . . . ?
C1 P1 C16 C15 132.64(11) . . . . ?
C1 P1 C16 C15 -132.64(11) 4_565 . . . ?
C1 P1 C16 C8 -47.36(11) . . . . ?
C1 P1 C16 C8 47.36(11) 4_565 . . . ?

_refine_diff_density_max         0.380
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.049




# start Validation Reply Form
_vrf_PLAT018_nt0764_LHG168       
;
PROBLEM: _diffrn_measured_fraction_theta_max .NE. *_full           ! Check 
RESPONSE: False alert because of twinned data.
;
_vrf_PLAT340_nt0764_LHG168       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00611 Ang.  
RESPONSE: Large themal motion of the molecule.
;
_vrf_PLAT906_nt0764_LHG168       
;
PROBLEM: Large K Value in the Analysis of Variance ......      4.874 Check 
RESPONSE: Large themal motion of the molecule.
;
_vrf_PLAT911_nt0764_LHG168       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.598         14 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_nt0893UCL_N_DAMA
_database_code_depnum_ccdc_archive 'CCDC 2061853'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
6-chloro-1,4-dimethyl-10H-5,10-[1,2]benzenoacridophosphine
_chemical_name_common            
6-chloro-1,4-dimethyl-10H-5,10-[1,2]benzenoacridophosphine
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H16 Cl P'
_chemical_formula_sum            'C21 H16 Cl P'
_chemical_formula_weight         334.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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                   13.9870(17)
_cell_length_b                   16.009(4)
_cell_length_c                   16.436(4)
_cell_angle_alpha                74.36(2)
_cell_angle_beta                 89.257(14)
_cell_angle_gamma                79.319(16)
_cell_volume                     3480.1(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1162
_cell_measurement_theta_min      2.8000
_cell_measurement_theta_max      19.6100

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.308
_shelx_estimated_absorpt_T_min   0.941
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_T_min  0.68868
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec I\mS microfocus source'
_diffrn_radiation_monochromator  'Montel multilayer optics ELM33'
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17918
_diffrn_reflns_av_unetI/netI     0.1111
_diffrn_reflns_av_R_equivalents  0.1473
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.817
_diffrn_reflns_theta_max         17.225
_diffrn_reflns_theta_full        17.225
_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             4206
_reflns_number_gt                2334
_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       ?
_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    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0827P)²+11.9855P] 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         4206
_refine_ls_number_parameters     887
_refine_ls_number_restraints     760
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.0877
_refine_ls_wR_factor_ref         0.2354
_refine_ls_wR_factor_gt          0.1992
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      0.966
_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
P1B P 0.8016(3) 0.1482(3) 0.4810(3) 0.0684(14) Uani 1 1 d . U . . .
C1B C 0.8871(11) 0.2178(11) 0.4237(9) 0.055(4) Uani 1 1 d . U . . .
C2B C 0.9689(15) 0.1902(13) 0.3858(11) 0.076(5) Uani 1 1 d D . . . .
C4B C 1.0307(14) 0.2398(18) 0.3436(13) 0.096(7) Uani 1 1 d . . . . .
H4B H 1.087345 0.215672 0.321283 0.116 Uiso 1 1 calc R U . . .
C5B C 1.0042(14) 0.3289(19) 0.3356(11) 0.100(7) Uani 1 1 d . . . . .
H5B H 1.041784 0.366622 0.303036 0.120 Uiso 1 1 calc R U . . .
C6B C 0.9236(16) 0.3653(13) 0.3741(10) 0.096(6) Uani 1 1 d D U . . .
H6B H 0.909876 0.425330 0.370293 0.115 Uiso 0.359(12) 1 calc R U P A 2
Cl1B Cl 0.6221(8) 0.0882(5) 0.3906(11) 0.088(3) Uani 0.641(12) 1 d D U P A 1
C3B C 1.008(8) 0.090(4) 0.380(7) 0.147(10) Uani 0.641(12) 1 d . U P A 1
H31B H 0.975075 0.049973 0.420270 0.220 Uiso 0.641(12) 1 calc R U P A 1
H32B H 1.076581 0.073707 0.392548 0.220 Uiso 0.641(12) 1 calc R U P A 1
H33B H 0.994262 0.086162 0.324132 0.220 Uiso 0.641(12) 1 calc R U P A 1
C7B C 0.8980(18) 0.4656(15) 0.3696(15) 0.107(7) Uani 0.641(12) 1 d D U P A 1
H71B H 0.949308 0.494261 0.343119 0.161 Uiso 0.641(12) 1 calc R U P A 1
H72B H 0.890782 0.472377 0.425733 0.161 Uiso 0.641(12) 1 calc R U P A 1
H73B H 0.838159 0.491731 0.337151 0.161 Uiso 0.641(12) 1 calc R U P A 1
Cl1Y Cl 0.999(4) 0.077(2) 0.393(3) 0.147(8) Uani 0.359(12) 1 d D U P A 2
C3Y C 0.613(5) 0.099(2) 0.398(7) 0.088(6) Uani 0.359(12) 1 d D U P A 2
H31Y H 0.678519 0.067271 0.397669 0.131 Uiso 0.359(12) 1 calc R U P A 2
H32Y H 0.574970 0.093803 0.352571 0.131 Uiso 0.359(12) 1 calc R U P A 2
H33Y H 0.585195 0.075097 0.451026 0.131 Uiso 0.359(12) 1 calc R U P A 2
C7Y C 0.592(3) 0.476(2) 0.368(3) 0.120(18) Uani 0.359(12) 1 d D . P A 2
H71Y H 0.654538 0.492490 0.371126 0.181 Uiso 0.359(12) 1 calc R U P A 2
H72Y H 0.554361 0.488436 0.414456 0.181 Uiso 0.359(12) 1 calc R U P A 2
H73Y H 0.558767 0.509678 0.315781 0.181 Uiso 0.359(12) 1 calc R U P A 2
C8B C 0.8635(10) 0.3077(12) 0.4191(9) 0.063(4) Uani 1 1 d . . . . .
C9B C 0.7681(9) 0.3393(10) 0.4593(8) 0.062(3) Uani 1 1 d . . . . .
H9B H 0.757718 0.403081 0.452420 0.075 Uiso 1 1 calc R U . . .
C10B C 0.6852(10) 0.3157(10) 0.4178(8) 0.057(3) Uani 1 1 d . . . . .
C11B C 0.6067(11) 0.3754(11) 0.3748(9) 0.077(4) Uani 1 1 d D . . . .
H11B H 0.602864 0.434963 0.370796 0.092 Uiso 0.641(12) 1 calc R U P A 1
C12B C 0.5336(11) 0.3502(11) 0.3374(9) 0.080(4) Uani 1 1 d . . . . .
H12B H 0.481273 0.392091 0.308608 0.096 Uiso 1 1 calc R U . . .
C13B C 0.5390(10) 0.2635(11) 0.3430(9) 0.070(4) Uani 1 1 d D . . . .
H13B H 0.490502 0.246588 0.316364 0.084 Uiso 1 1 calc R U . . .
C14B C 0.6155(10) 0.1985(10) 0.3879(8) 0.058(3) Uani 1 1 d D . . . .
C15B C 0.6911(9) 0.2232(10) 0.4254(8) 0.057(3) Uani 1 1 d D U . . .
C16B C 0.7769(9) 0.2879(11) 0.5542(9) 0.067(3) Uani 1 1 d . . . . .
C17B C 0.7671(10) 0.3278(11) 0.6192(10) 0.085(4) Uani 1 1 d . . . . .
H17B H 0.754337 0.389101 0.607367 0.102 Uiso 1 1 calc R U . . .
C18B C 0.7765(10) 0.2755(12) 0.7035(10) 0.084(5) Uani 1 1 d . . . . .
H18B H 0.771443 0.301800 0.747778 0.101 Uiso 1 1 calc R U . . .
C19B C 0.7936(10) 0.1821(12) 0.7204(10) 0.083(4) Uani 1 1 d . . . . .
H19B H 0.798311 0.148029 0.776295 0.100 Uiso 1 1 calc R U . . .
C20B C 0.8034(9) 0.1408(11) 0.6580(9) 0.073(4) Uani 1 1 d . . . . .
H20B H 0.816589 0.079499 0.670250 0.087 Uiso 1 1 calc R U . . .
C21B C 0.7930(9) 0.1942(11) 0.5737(9) 0.061(4) Uani 1 1 d . . . . .
Cl1C Cl 0.9435(11) 0.5888(12) 0.4192(10) 0.166(9) Uani 0.367(10) 1 d . . P B 1
Cl1X Cl 0.5552(5) 0.5891(5) 0.4294(5) 0.097(4) Uani 0.633(10) 1 d . . P B 2
P1C P 0.7376(3) 0.6487(3) 0.5127(3) 0.0807(16) Uani 1 1 d . . . . .
C1C C 0.7292(9) 0.6856(10) 0.6085(9) 0.058(4) Uani 1 1 d . . . . .
C2C C 0.7365(10) 0.6289(12) 0.6908(10) 0.070(4) Uani 1 1 d . . . . .
C3C C 0.7594(11) 0.5270(10) 0.7055(9) 0.097(5) Uani 1 1 d . . . . .
H31C H 0.702610 0.507706 0.690712 0.146 Uiso 1 1 calc R U . . .
H32C H 0.777791 0.498844 0.763878 0.146 Uiso 1 1 calc R U . . .
H33C H 0.811860 0.511632 0.670804 0.146 Uiso 1 1 calc R U . . .
C4C C 0.7315(10) 0.6607(12) 0.7579(10) 0.084(5) Uani 1 1 d . . . . .
H4C H 0.739296 0.621757 0.811793 0.100 Uiso 1 1 calc R U . . .
C5C C 0.7139(9) 0.7550(12) 0.7483(10) 0.072(4) Uani 1 1 d . . . . .
H5C H 0.709658 0.776143 0.795900 0.086 Uiso 1 1 calc R U . . .
C6C C 0.7031(9) 0.8155(11) 0.6658(10) 0.061(4) Uani 1 1 d . . . . .
C7C C 0.6817(11) 0.9130(10) 0.6571(10) 0.099(6) Uani 1 1 d . . . . .
H71C H 0.628736 0.940830 0.616618 0.148 Uiso 1 1 calc R U . . .
H72C H 0.738429 0.937417 0.638382 0.148 Uiso 1 1 calc R U . . .
H73C H 0.664276 0.922940 0.710883 0.148 Uiso 1 1 calc R U . . .
C8C C 0.7104(9) 0.7803(10) 0.5977(9) 0.056(4) Uani 1 1 d . . . . .
C9C C 0.6995(9) 0.8357(9) 0.5034(8) 0.051(3) Uani 1 1 d . . . . .
H9C H 0.686457 0.898848 0.500179 0.061 Uiso 1 1 calc R U . . .
C10C C 0.6147(10) 0.8128(11) 0.4604(9) 0.057(4) Uani 1 1 d . . . . .
C11C C 0.5350(10) 0.8743(10) 0.4201(9) 0.070(4) Uani 1 1 d . . . . .
H11C H 0.531690 0.933639 0.416972 0.084 Uiso 1 1 calc R U . . .
C12C C 0.4592(11) 0.8484(11) 0.3839(9) 0.078(5) Uani 1 1 d . . . . .
H12C H 0.403985 0.889063 0.359121 0.093 Uiso 1 1 calc R U . . .
C13C C 0.4699(11) 0.7587(12) 0.3865(9) 0.072(5) Uani 1 1 d . . . . .
H13C H 0.421531 0.740350 0.361106 0.087 Uiso 1 1 calc R U . . .
C14C C 0.5460(11) 0.6998(11) 0.4237(10) 0.071(5) Uani 1 1 d . . . . .
H14C H 0.548502 0.640784 0.425816 0.086 Uiso 0.367(10) 1 calc R U P B 1
C15C C 0.6236(10) 0.7232(10) 0.4603(8) 0.059(4) Uani 1 1 d . . . . .
C16C C 0.7904(10) 0.8135(11) 0.4604(8) 0.057(4) Uani 1 1 d . . . . .
C17C C 0.8491(10) 0.8738(12) 0.4213(10) 0.090(5) Uani 1 1 d . . . . .
H17C H 0.831792 0.932287 0.422842 0.108 Uiso 1 1 calc R U . . .
C18C C 0.9303(12) 0.8490(14) 0.3813(11) 0.098(6) Uani 1 1 d . . . . .
H18C H 0.966201 0.891355 0.354566 0.117 Uiso 1 1 calc R U . . .
C19C C 0.9616(12) 0.7616(14) 0.3793(11) 0.100(6) Uani 1 1 d . . . . .
H19C H 1.017671 0.745514 0.351687 0.120 Uiso 1 1 calc R U . . .
C20C C 0.9058(11) 0.6978(13) 0.4203(10) 0.093(5) Uani 1 1 d . . . . .
H20C H 0.926014 0.638799 0.421181 0.112 Uiso 0.633(10) 1 calc R U P B 2
C21C C 0.8193(10) 0.7243(11) 0.4599(9) 0.065(4) Uani 1 1 d . . . . .
Cl1A Cl 0.9706(4) 0.4505(4) -0.1450(4) 0.098(3) Uani 0.685(10) 1 d D . P C 1
Cl1Z Cl 0.5637(14) 0.4710(17) -0.1628(13) 0.187(11) Uani 0.315(10) 1 d D . P C
2
P1A P 0.7753(3) 0.3737(3) -0.0452(3) 0.0792(16) Uani 1 1 d . . . . .
C1A C 0.7802(9) 0.3000(10) 0.0626(9) 0.059(4) Uani 1 1 d . . . . .
C2A C 0.7765(9) 0.3300(11) 0.1352(10) 0.061(4) Uani 1 1 d . . . . .
C3A C 0.7617(11) 0.4281(9) 0.1313(9) 0.091(5) Uani 1 1 d . . . . .
H31A H 0.796456 0.457799 0.085102 0.137 Uiso 1 1 calc R U . . .
H32A H 0.785786 0.434487 0.183329 0.137 Uiso 1 1 calc R U . . .
H33A H 0.693581 0.453508 0.123211 0.137 Uiso 1 1 calc R U . . .
C4A C 0.7825(11) 0.2678(12) 0.2132(10) 0.081(5) Uani 1 1 d . . . . .
H4A H 0.777977 0.287782 0.261504 0.097 Uiso 1 1 calc R U . . .
C5A C 0.7948(9) 0.1777(11) 0.2231(10) 0.072(5) Uani 1 1 d . . . . .
H5A H 0.799445 0.138201 0.276673 0.086 Uiso 1 1 calc R U . . .
C6A C 0.8001(10) 0.1475(11) 0.1494(11) 0.072(4) Uani 1 1 d . . . . .
C7A C 0.8174(11) 0.0448(10) 0.1594(11) 0.110(6) Uani 1 1 d . . . . .
H71A H 0.764297 0.031293 0.131931 0.166 Uiso 1 1 calc R U . . .
H72A H 0.821180 0.013587 0.218306 0.166 Uiso 1 1 calc R U . . .
H73A H 0.877153 0.027032 0.133891 0.166 Uiso 1 1 calc R U . . .
C8A C 0.7922(9) 0.2069(11) 0.0696(10) 0.061(4) Uani 1 1 d . . . . .
C9A C 0.7951(9) 0.1823(10) -0.0137(8) 0.064(4) Uani 1 1 d . . . . .
H9A H 0.801375 0.118378 -0.003894 0.076 Uiso 1 1 calc R U . . .
C10A C 0.8821(10) 0.2161(11) -0.0646(9) 0.059(4) Uani 1 1 d . . . . .
C11A C 0.9548(10) 0.1576(11) -0.0913(10) 0.080(5) Uani 1 1 d . . . . .
H11A H 0.952843 0.097855 -0.080771 0.095 Uiso 1 1 calc R U . . .
C12A C 1.0297(12) 0.1936(13) -0.1342(10) 0.089(5) Uani 1 1 d . . . . .
H12A H 1.081427 0.156824 -0.150609 0.107 Uiso 1 1 calc R U . . .
C13A C 1.0288(13) 0.2859(13) -0.1538(11) 0.102(6) Uani 1 1 d . . . . .
H13A H 1.078099 0.308224 -0.186071 0.122 Uiso 1 1 calc R U . . .
C14A C 0.9567(12) 0.3444(11) -0.1264(10) 0.085(5) Uani 1 1 d D . . . .
H14A H 0.959390 0.403985 -0.136716 0.102 Uiso 0.315(10) 1 calc R U P C 2
C15A C 0.8791(10) 0.3082(10) -0.0821(9) 0.064(4) Uani 1 1 d . . . . .
C16A C 0.6986(10) 0.2335(11) -0.0675(9) 0.063(4) Uani 1 1 d . . . . .
C17A C 0.6344(12) 0.1922(14) -0.0965(10) 0.100(6) Uani 1 1 d . . . . .
H17A H 0.646182 0.130864 -0.083050 0.120 Uiso 1 1 calc R U . . .
C18A C 0.553(2) 0.2392(18) -0.1449(16) 0.150(9) Uani 1 1 d . . . . .
H18A H 0.509207 0.209693 -0.161969 0.180 Uiso 1 1 calc R U . . .
C19A C 0.5379(16) 0.3227(15) -0.1663(16) 0.136(9) Uani 1 1 d D . . . .
H19E H 0.483938 0.354419 -0.201049 0.163 Uiso 1 1 calc R U . . .
C20A C 0.6010(13) 0.3673(17) -0.1384(11) 0.114(6) Uani 1 1 d D . . . .
H20A H 0.586797 0.428671 -0.156528 0.136 Uiso 0.685(10) 1 calc R U P C 1
C21A C 0.6818(10) 0.3298(11) -0.0871(9) 0.069(4) Uani 1 1 d D . . . .
Cl1D Cl 0.8988(4) 0.9397(4) 0.8701(4) 0.145(2) Uani 1 1 d . . . . .
P1D P 0.7081(3) 0.8802(3) 0.9809(3) 0.0818(16) Uani 1 1 d . . . . .
C1D C 0.6109(11) 0.8367(12) 0.9402(10) 0.071(4) Uani 1 1 d . . . . .
C2D C 0.5345(13) 0.8977(14) 0.8833(12) 0.090(5) Uani 1 1 d . . . . .
C3D C 0.5228(12) 0.9939(11) 0.8564(11) 0.124(7) Uani 1 1 d . . . . .
H31D H 0.479136 1.017002 0.807601 0.148 Uiso 1 1 calc R U . . .
H32D H 0.584990 1.009991 0.842399 0.148 Uiso 1 1 calc R U . . .
H33D H 0.496695 1.017768 0.901383 0.148 Uiso 1 1 calc R U . . .
C4D C 0.4689(13) 0.8560(14) 0.8581(12) 0.111(6) Uani 1 1 d . . . . .
H4D H 0.416745 0.891918 0.823496 0.133 Uiso 1 1 calc R U . . .
C5D C 0.4709(13) 0.7679(14) 0.8779(11) 0.097(6) Uani 1 1 d . . . . .
H5D H 0.423121 0.745572 0.856197 0.117 Uiso 1 1 calc R U . . .
C6D C 0.5479(12) 0.7102(13) 0.9326(10) 0.079(5) Uani 1 1 d . . . . .
C7D C 0.5528(12) 0.6149(11) 0.9517(11) 0.118(6) Uani 1 1 d . . . . .
H71D H 0.511710 0.602474 0.911773 0.177 Uiso 1 1 calc R U . . .
H72D H 0.531111 0.593274 1.007805 0.177 Uiso 1 1 calc R U . . .
H73D H 0.618717 0.586191 0.948009 0.177 Uiso 1 1 calc R U . . .
C8D C 0.6212(10) 0.7468(11) 0.9600(9) 0.062(4) Uani 1 1 d . . . . .
C9D C 0.7133(9) 0.6906(9) 1.0165(8) 0.054(4) Uani 1 1 d . . . . .
H9D H 0.714107 0.627178 1.027711 0.064 Uiso 1 1 calc R U . . .
C10D C 0.8022(10) 0.7154(11) 0.9708(9) 0.058(4) Uani 1 1 d . . . . .
C11D C 0.8752(11) 0.6545(12) 0.9463(10) 0.087(5) Uani 1 1 d . . . . .
H11D H 0.870794 0.595035 0.960898 0.104 Uiso 1 1 calc R U . . .
C12D C 0.9505(12) 0.6804(13) 0.9027(11) 0.092(6) Uani 1 1 d . . . . .
H12D H 0.998996 0.638703 0.889051 0.110 Uiso 1 1 calc R U . . .
C13D C 0.9571(11) 0.7691(13) 0.8774(10) 0.079(5) Uani 1 1 d . . . . .
H13D H 1.008403 0.787091 0.845082 0.095 Uiso 1 1 calc R U . . .
C14D C 0.8874(12) 0.8302(11) 0.9004(9) 0.072(5) Uani 1 1 d . . . . .
C15D C 0.8069(10) 0.8056(10) 0.9464(8) 0.058(4) Uani 1 1 d . . . . .
C16D C 0.7083(10) 0.8078(11) 1.0894(9) 0.063(4) Uani 1 1 d . . . . .
C17D C 0.7085(10) 0.8396(12) 1.1601(10) 0.080(5) Uani 1 1 d . . . . .
H17D H 0.707597 0.899440 1.152875 0.096 Uiso 1 1 calc R U . . .
C18D C 0.7102(10) 0.7838(12) 1.2418(10) 0.075(5) Uani 1 1 d . . . . .
H18D H 0.707006 0.805871 1.288878 0.090 Uiso 1 1 calc R U . . .
C19D C 0.7168(10) 0.6933(12) 1.2505(11) 0.085(5) Uani 1 1 d . . . . .
H19D H 0.721797 0.654251 1.304351 0.102 Uiso 1 1 calc R U . . .
C20D C 0.7159(10) 0.6613(11) 1.1813(10) 0.077(5) Uani 1 1 d . . . . .
H20D H 0.718100 0.601306 1.188563 0.092 Uiso 1 1 calc R U . . .
C21D C 0.7117(9) 0.7186(11) 1.0995(10) 0.060(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
P1B C15B 1.850(14) . ?
P1B C21B 1.856(14) . ?
P1B C1B 1.861(14) . ?
C1B C2B 1.354(19) . ?
C1B C8B 1.398(17) . ?
C2B C4B 1.34(2) . ?
C2B C3B 1.63(6) . ?
C2B Cl1Y 1.75(3) . ?
C4B C5B 1.38(2) . ?
C4B H4B 0.9300 . ?
C5B C6B 1.39(2) . ?
C5B H5B 0.9300 . ?
C6B C8B 1.417(19) . ?
C6B C7B 1.56(2) . ?
C6B H6B 0.9300 . ?
Cl1B C14B 1.739(18) . ?
C3B H31B 0.9600 . ?
C3B H32B 0.9600 . ?
C3B H33B 0.9600 . ?
C7B H71B 0.9600 . ?
C7B H72B 0.9600 . ?
C7B H73B 0.9600 . ?
C3Y C14B 1.56(3) . ?
C3Y H31Y 0.9600 . ?
C3Y H32Y 0.9600 . ?
C3Y H33Y 0.9600 . ?
C7Y C11B 1.56(3) . ?
C7Y H71Y 0.9600 . ?
C7Y H72Y 0.9600 . ?
C7Y H73Y 0.9600 . ?
C8B C9B 1.543(17) . ?
C9B C10B 1.508(17) . ?
C9B C16B 1.550(18) . ?
C9B H9B 0.9800 . ?
C10B C11B 1.374(17) . ?
C10B C15B 1.439(17) . ?
C11B C12B 1.374(17) . ?
C11B H11B 0.9300 . ?
C12B C13B 1.354(17) . ?
C12B H12B 0.9300 . ?
C13B C14B 1.402(17) . ?
C13B H13B 0.9300 . ?
C14B C15B 1.399(16) . ?
C16B C17B 1.379(17) . ?
C16B C21B 1.421(18) . ?
C17B C18B 1.406(19) . ?
C17B H17B 0.9300 . ?
C18B C19B 1.419(19) . ?
C18B H18B 0.9300 . ?
C19B C20B 1.355(17) . ?
C19B H19B 0.9300 . ?
C20B C21B 1.412(18) . ?
C20B H20B 0.9300 . ?
Cl1C C20C 1.73(2) . ?
Cl1X C14C 1.730(16) . ?
P1C C1C 1.819(14) . ?
P1C C21C 1.856(15) . ?
P1C C15C 1.867(15) . ?
C1C C2C 1.405(19) . ?
C1C C8C 1.452(17) . ?
C2C C4C 1.328(18) . ?
C2C C3C 1.555(19) . ?
C3C H31C 0.9600 . ?
C3C H32C 0.9600 . ?
C3C H33C 0.9600 . ?
C4C C5C 1.449(19) . ?
C4C H4C 0.9300 . ?
C5C C6C 1.430(19) . ?
C5C H5C 0.9300 . ?
C6C C8C 1.377(17) . ?
C6C C7C 1.500(18) . ?
C7C H71C 0.9600 . ?
C7C H72C 0.9600 . ?
C7C H73C 0.9600 . ?
C8C C9C 1.557(17) . ?
C9C C16C 1.480(16) . ?
C9C C10C 1.538(17) . ?
C9C H9C 0.9800 . ?
C10C C11C 1.382(18) . ?
C10C C15C 1.417(17) . ?
C11C C12C 1.400(17) . ?
C11C H11C 0.9300 . ?
C12C C13C 1.406(18) . ?
C12C H12C 0.9300 . ?
C13C C14C 1.316(18) . ?
C13C H13C 0.9300 . ?
C14C C15C 1.403(18) . ?
C14C H14C 0.9300 . ?
C16C C17C 1.401(18) . ?
C16C C21C 1.411(17) . ?
C17C C18C 1.354(19) . ?
C17C H17C 0.9300 . ?
C18C C19C 1.40(2) . ?
C18C H18C 0.9300 . ?
C19C C20C 1.42(2) . ?
C19C H19C 0.9300 . ?
C20C C21C 1.417(18) . ?
C20C H20C 0.9300 . ?
Cl1A C14A 1.690(16) . ?
Cl1Z C20A 1.59(2) . ?
P1A C21A 1.818(15) . ?
P1A C15A 1.825(14) . ?
P1A C1A 1.838(14) . ?
C1A C2A 1.399(17) . ?
C1A C8A 1.441(17) . ?
C2A C4A 1.388(19) . ?
C2A C3A 1.529(17) . ?
C3A H31A 0.9600 . ?
C3A H32A 0.9600 . ?
C3A H33A 0.9600 . ?
C4A C5A 1.385(18) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.418(18) . ?
C5A H5A 0.9300 . ?
C6A C8A 1.389(19) . ?
C6A C7A 1.581(19) . ?
C7A H71A 0.9600 . ?
C7A H72A 0.9600 . ?
C7A H73A 0.9600 . ?
C8A C9A 1.520(17) . ?
C9A C10A 1.564(17) . ?
C9A C16A 1.583(19) . ?
C9A H9A 0.9800 . ?
C10A C11A 1.401(17) . ?
C10A C15A 1.417(17) . ?
C11A C12A 1.382(18) . ?
C11A H11A 0.9300 . ?
C12A C13A 1.42(2) . ?
C12A H12A 0.9300 . ?
C13A C14A 1.40(2) . ?
C13A H13A 0.9300 . ?
C14A C15A 1.424(18) . ?
C14A H14A 0.9300 . ?
C16A C17A 1.368(18) . ?
C16A C21A 1.461(18) . ?
C17A C18A 1.37(3) . ?
C17A H17A 0.9300 . ?
C18A C19A 1.27(3) . ?
C18A H18A 0.9300 . ?
C19A C20A 1.39(3) . ?
C19A H19E 0.9300 . ?
C20A C21A 1.36(2) . ?
C20A H20A 0.9300 . ?
Cl1D C14D 1.725(15) . ?
P1D C15D 1.840(14) . ?
P1D C1D 1.845(16) . ?
P1D C16D 1.847(15) . ?
C1D C8D 1.366(18) . ?
C1D C2D 1.46(2) . ?
C2D C4D 1.36(2) . ?
C2D C3D 1.46(2) . ?
C3D H31D 0.9600 . ?
C3D H32D 0.9600 . ?
C3D H33D 0.9600 . ?
C4D C5D 1.35(2) . ?
C4D H4D 0.9300 . ?
C5D C6D 1.42(2) . ?
C5D H5D 0.9300 . ?
C6D C8D 1.405(19) . ?
C6D C7D 1.462(19) . ?
C7D H71D 0.9600 . ?
C7D H72D 0.9600 . ?
C7D H73D 0.9600 . ?
C8D C9D 1.576(18) . ?
C9D C10D 1.505(16) . ?
C9D C21D 1.545(17) . ?
C9D H9D 0.9800 . ?
C10D C15D 1.404(17) . ?
C10D C11D 1.411(18) . ?
C11D C12D 1.333(19) . ?
C11D H11D 0.9300 . ?
C12D C13D 1.39(2) . ?
C12D H12D 0.9300 . ?
C13D C14D 1.372(18) . ?
C13D H13D 0.9300 . ?
C14D C15D 1.407(17) . ?
C16D C21D 1.384(18) . ?
C16D C17D 1.390(17) . ?
C17D C18D 1.396(19) . ?
C17D H17D 0.9300 . ?
C18D C19D 1.403(19) . ?
C18D H18D 0.9300 . ?
C19D C20D 1.368(17) . ?
C19D H19D 0.9300 . ?
C20D C21D 1.404(18) . ?
C20D H20D 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
C15B P1B C21B 94.6(6) . . ?
C15B P1B C1B 94.6(7) . . ?
C21B P1B C1B 95.4(7) . . ?
C2B C1B C8B 117.2(14) . . ?
C2B C1B P1B 126.6(15) . . ?
C8B C1B P1B 116.1(13) . . ?
C4B C2B C1B 127.3(18) . . ?
C4B C2B C3B 107(4) . . ?
C1B C2B C3B 126(4) . . ?
C4B C2B Cl1Y 116(2) . . ?
C1B C2B Cl1Y 117(2) . . ?
C2B C4B C5B 115(2) . . ?
C2B C4B H4B 122.5 . . ?
C5B C4B H4B 122.5 . . ?
C4B C5B C6B 123(2) . . ?
C4B C5B H5B 118.4 . . ?
C6B C5B H5B 118.4 . . ?
C5B C6B C8B 117.8(17) . . ?
C5B C6B C7B 123(2) . . ?
C8B C6B C7B 119.4(19) . . ?
C5B C6B H6B 121.1 . . ?
C8B C6B H6B 121.1 . . ?
C2B C3B H31B 109.5 . . ?
C2B C3B H32B 109.5 . . ?
H31B C3B H32B 109.5 . . ?
C2B C3B H33B 109.5 . . ?
H31B C3B H33B 109.5 . . ?
H32B C3B H33B 109.5 . . ?
C6B C7B H71B 109.5 . . ?
C6B C7B H72B 109.5 . . ?
H71B C7B H72B 109.5 . . ?
C6B C7B H73B 109.5 . . ?
H71B C7B H73B 109.5 . . ?
H72B C7B H73B 109.5 . . ?
C14B C3Y H31Y 109.5 . . ?
C14B C3Y H32Y 109.5 . . ?
H31Y C3Y H32Y 109.5 . . ?
C14B C3Y H33Y 109.5 . . ?
H31Y C3Y H33Y 109.5 . . ?
H32Y C3Y H33Y 109.5 . . ?
C11B C7Y H71Y 109.5 . . ?
C11B C7Y H72Y 109.5 . . ?
H71Y C7Y H72Y 109.5 . . ?
C11B C7Y H73Y 109.5 . . ?
H71Y C7Y H73Y 109.5 . . ?
H72Y C7Y H73Y 109.5 . . ?
C1B C8B C6B 119.3(14) . . ?
C1B C8B C9B 116.9(15) . . ?
C6B C8B C9B 123.7(17) . . ?
C10B C9B C8B 108.3(11) . . ?
C10B C9B C16B 109.0(11) . . ?
C8B C9B C16B 107.2(12) . . ?
C10B C9B H9B 110.8 . . ?
C8B C9B H9B 110.8 . . ?
C16B C9B H9B 110.8 . . ?
C11B C10B C15B 119.3(14) . . ?
C11B C10B C9B 124.8(15) . . ?
C15B C10B C9B 115.9(13) . . ?
C10B C11B C12B 122.3(16) . . ?
C10B C11B C7Y 122(2) . . ?
C12B C11B C7Y 115(2) . . ?
C10B C11B H11B 118.8 . . ?
C12B C11B H11B 118.8 . . ?
C13B C12B C11B 119.0(16) . . ?
C13B C12B H12B 120.5 . . ?
C11B C12B H12B 120.5 . . ?
C12B C13B C14B 121.9(16) . . ?
C12B C13B H13B 119.0 . . ?
C14B C13B H13B 119.0 . . ?
C15B C14B C13B 119.8(15) . . ?
C15B C14B C3Y 120.6(14) . . ?
C13B C14B C3Y 119.5(14) . . ?
C15B C14B Cl1B 119.5(13) . . ?
C13B C14B Cl1B 120.6(13) . . ?
C14B C15B C10B 117.7(14) . . ?
C14B C15B P1B 126.1(12) . . ?
C10B C15B P1B 116.2(10) . . ?
C17B C16B C21B 119.3(16) . . ?
C17B C16B C9B 123.8(16) . . ?
C21B C16B C9B 116.9(13) . . ?
C16B C17B C18B 119.7(17) . . ?
C16B C17B H17B 120.2 . . ?
C18B C17B H17B 120.2 . . ?
C17B C18B C19B 119.4(16) . . ?
C17B C18B H18B 120.3 . . ?
C19B C18B H18B 120.3 . . ?
C20B C19B C18B 122.4(17) . . ?
C20B C19B H19B 118.8 . . ?
C18B C19B H19B 118.8 . . ?
C19B C20B C21B 117.5(16) . . ?
C19B C20B H20B 121.2 . . ?
C21B C20B H20B 121.2 . . ?
C20B C21B C16B 121.7(14) . . ?
C20B C21B P1B 123.0(13) . . ?
C16B C21B P1B 115.4(12) . . ?
C1C P1C C21C 94.9(6) . . ?
C1C P1C C15C 95.5(7) . . ?
C21C P1C C15C 94.8(7) . . ?
C2C C1C C8C 118.6(14) . . ?
C2C C1C P1C 124.4(13) . . ?
C8C C1C P1C 116.9(11) . . ?
C4C C2C C1C 121.0(18) . . ?
C4C C2C C3C 118.4(17) . . ?
C1C C2C C3C 120.4(15) . . ?
C2C C3C H31C 109.5 . . ?
C2C C3C H32C 109.5 . . ?
H31C C3C H32C 109.5 . . ?
C2C C3C H33C 109.5 . . ?
H31C C3C H33C 109.5 . . ?
H32C C3C H33C 109.5 . . ?
C2C C4C C5C 121.0(18) . . ?
C2C C4C H4C 119.5 . . ?
C5C C4C H4C 119.5 . . ?
C6C C5C C4C 120.1(15) . . ?
C6C C5C H5C 119.9 . . ?
C4C C5C H5C 119.9 . . ?
C8C C6C C5C 117.3(15) . . ?
C8C C6C C7C 123.3(15) . . ?
C5C C6C C7C 119.3(14) . . ?
C6C C7C H71C 109.5 . . ?
C6C C7C H72C 109.5 . . ?
H71C C7C H72C 109.5 . . ?
C6C C7C H73C 109.5 . . ?
H71C C7C H73C 109.5 . . ?
H72C C7C H73C 109.5 . . ?
C6C C8C C1C 121.8(14) . . ?
C6C C8C C9C 124.7(14) . . ?
C1C C8C C9C 113.5(12) . . ?
C16C C9C C10C 109.2(11) . . ?
C16C C9C C8C 109.3(11) . . ?
C10C C9C C8C 108.9(11) . . ?
C16C C9C H9C 109.8 . . ?
C10C C9C H9C 109.8 . . ?
C8C C9C H9C 109.8 . . ?
C11C C10C C15C 119.9(15) . . ?
C11C C10C C9C 124.0(15) . . ?
C15C C10C C9C 116.1(14) . . ?
C10C C11C C12C 120.9(16) . . ?
C10C C11C H11C 119.6 . . ?
C12C C11C H11C 119.6 . . ?
C11C C12C C13C 117.4(16) . . ?
C11C C12C H12C 121.3 . . ?
C13C C12C H12C 121.3 . . ?
C14C C13C C12C 122.2(17) . . ?
C14C C13C H13C 118.9 . . ?
C12C C13C H13C 118.9 . . ?
C13C C14C C15C 122.0(17) . . ?
C13C C14C Cl1X 121.2(14) . . ?
C15C C14C Cl1X 116.8(13) . . ?
C13C C14C H14C 119.0 . . ?
C15C C14C H14C 119.0 . . ?
C14C C15C C10C 117.4(14) . . ?
C14C C15C P1C 127.4(13) . . ?
C10C C15C P1C 115.1(11) . . ?
C17C C16C C21C 118.6(14) . . ?
C17C C16C C9C 124.9(15) . . ?
C21C C16C C9C 116.5(14) . . ?
C18C C17C C16C 121.6(17) . . ?
C18C C17C H17C 119.2 . . ?
C16C C17C H17C 119.2 . . ?
C17C C18C C19C 121.8(19) . . ?
C17C C18C H18C 119.1 . . ?
C19C C18C H18C 119.1 . . ?
C18C C19C C20C 118.4(17) . . ?
C18C C19C H19C 120.8 . . ?
C20C C19C H19C 120.8 . . ?
C21C C20C C19C 119.7(17) . . ?
C21C C20C Cl1C 121.0(15) . . ?
C19C C20C Cl1C 119.3(14) . . ?
C21C C20C H20C 120.1 . . ?
C19C C20C H20C 120.1 . . ?
C16C C21C C20C 119.9(15) . . ?
C16C C21C P1C 115.9(11) . . ?
C20C C21C P1C 124.2(14) . . ?
C21A P1A C15A 96.5(7) . . ?
C21A P1A C1A 96.0(7) . . ?
C15A P1A C1A 95.9(7) . . ?
C2A C1A C8A 120.4(14) . . ?
C2A C1A P1A 123.2(12) . . ?
C8A C1A P1A 116.3(11) . . ?
C4A C2A C1A 118.0(15) . . ?
C4A C2A C3A 119.4(14) . . ?
C1A C2A C3A 122.6(15) . . ?
C2A C3A H31A 109.5 . . ?
C2A C3A H32A 109.5 . . ?
H31A C3A H32A 109.5 . . ?
C2A C3A H33A 109.5 . . ?
H31A C3A H33A 109.5 . . ?
H32A C3A H33A 109.5 . . ?
C5A C4A C2A 123.7(16) . . ?
C5A C4A H4A 118.1 . . ?
C2A C4A H4A 118.1 . . ?
C4A C5A C6A 118.1(17) . . ?
C4A C5A H5A 121.0 . . ?
C6A C5A H5A 121.0 . . ?
C8A C6A C5A 120.7(16) . . ?
C8A C6A C7A 120.4(15) . . ?
C5A C6A C7A 118.9(16) . . ?
C6A C7A H71A 109.5 . . ?
C6A C7A H72A 109.5 . . ?
H71A C7A H72A 109.5 . . ?
C6A C7A H73A 109.5 . . ?
H71A C7A H73A 109.5 . . ?
H72A C7A H73A 109.5 . . ?
C6A C8A C1A 119.1(14) . . ?
C6A C8A C9A 125.3(16) . . ?
C1A C8A C9A 115.6(14) . . ?
C8A C9A C10A 108.8(10) . . ?
C8A C9A C16A 108.3(11) . . ?
C10A C9A C16A 106.9(11) . . ?
C8A C9A H9A 110.9 . . ?
C10A C9A H9A 110.9 . . ?
C16A C9A H9A 110.9 . . ?
C11A C10A C15A 124.3(14) . . ?
C11A C10A C9A 120.7(14) . . ?
C15A C10A C9A 115.0(13) . . ?
C12A C11A C10A 116.2(16) . . ?
C12A C11A H11A 121.9 . . ?
C10A C11A H11A 121.9 . . ?
C11A C12A C13A 121.1(17) . . ?
C11A C12A H12A 119.5 . . ?
C13A C12A H12A 119.5 . . ?
C14A C13A C12A 122.7(18) . . ?
C14A C13A H13A 118.6 . . ?
C12A C13A H13A 118.6 . . ?
C13A C14A C15A 116.7(16) . . ?
C13A C14A Cl1A 118.0(14) . . ?
C15A C14A Cl1A 125.3(13) . . ?
C13A C14A H14A 121.7 . . ?
C15A C14A H14A 121.7 . . ?
C10A C15A C14A 118.8(14) . . ?
C10A C15A P1A 117.4(11) . . ?
C14A C15A P1A 123.8(13) . . ?
C17A C16A C21A 120.6(16) . . ?
C17A C16A C9A 123.4(16) . . ?
C21A C16A C9A 116.0(13) . . ?
C18A C17A C16A 121(2) . . ?
C18A C17A H17A 119.3 . . ?
C16A C17A H17A 119.3 . . ?
C19A C18A C17A 120(3) . . ?
C19A C18A H18A 119.9 . . ?
C17A C18A H18A 119.9 . . ?
C18A C19A C20A 120(3) . . ?
C18A C19A H19E 119.8 . . ?
C20A C19A H19E 119.8 . . ?
C21A C20A C19A 126(2) . . ?
C21A C20A Cl1Z 120.3(18) . . ?
C19A C20A Cl1Z 113.1(17) . . ?
C21A C20A H20A 116.9 . . ?
C19A C20A H20A 116.9 . . ?
C20A C21A C16A 111.2(17) . . ?
C20A C21A P1A 133.8(15) . . ?
C16A C21A P1A 114.8(12) . . ?
C15D P1D C1D 93.8(7) . . ?
C15D P1D C16D 94.8(7) . . ?
C1D P1D C16D 94.3(7) . . ?
C8D C1D C2D 123.9(17) . . ?
C8D C1D P1D 116.5(13) . . ?
C2D C1D P1D 119.3(14) . . ?
C4D C2D C1D 112.5(19) . . ?
C4D C2D C3D 121(2) . . ?
C1D C2D C3D 126.4(18) . . ?
C2D C3D H31D 109.5 . . ?
C2D C3D H32D 109.5 . . ?
H31D C3D H32D 109.5 . . ?
C2D C3D H33D 109.5 . . ?
H31D C3D H33D 109.5 . . ?
H32D C3D H33D 109.5 . . ?
C5D C4D C2D 127(2) . . ?
C5D C4D H4D 116.4 . . ?
C2D C4D H4D 116.4 . . ?
C4D C5D C6D 118.5(18) . . ?
C4D C5D H5D 120.7 . . ?
C6D C5D H5D 120.7 . . ?
C8D C6D C5D 118.6(17) . . ?
C8D C6D C7D 122.3(17) . . ?
C5D C6D C7D 118.9(16) . . ?
C6D C7D H71D 109.5 . . ?
C6D C7D H72D 109.5 . . ?
H71D C7D H72D 109.5 . . ?
C6D C7D H73D 109.5 . . ?
H71D C7D H73D 109.5 . . ?
H72D C7D H73D 109.5 . . ?
C1D C8D C6D 118.8(16) . . ?
C1D C8D C9D 117.1(14) . . ?
C6D C8D C9D 124.0(15) . . ?
C10D C9D C21D 107.4(10) . . ?
C10D C9D C8D 107.7(11) . . ?
C21D C9D C8D 107.9(11) . . ?
C10D C9D H9D 111.2 . . ?
C21D C9D H9D 111.2 . . ?
C8D C9D H9D 111.2 . . ?
C15D C10D C11D 119.5(15) . . ?
C15D C10D C9D 116.7(14) . . ?
C11D C10D C9D 123.5(14) . . ?
C12D C11D C10D 121.2(17) . . ?
C12D C11D H11D 119.4 . . ?
C10D C11D H11D 119.4 . . ?
C11D C12D C13D 120.6(19) . . ?
C11D C12D H12D 119.7 . . ?
C13D C12D H12D 119.7 . . ?
C14D C13D C12D 119.7(18) . . ?
C14D C13D H13D 120.2 . . ?
C12D C13D H13D 120.2 . . ?
C13D C14D C15D 121.5(15) . . ?
C13D C14D Cl1D 118.7(14) . . ?
C15D C14D Cl1D 119.8(13) . . ?
C10D C15D C14D 117.4(14) . . ?
C10D C15D P1D 116.4(11) . . ?
C14D C15D P1D 126.1(12) . . ?
C21D C16D C17D 119.8(15) . . ?
C21D C16D P1D 118.0(12) . . ?
C17D C16D P1D 122.1(13) . . ?
C16D C17D C18D 121.4(17) . . ?
C16D C17D H17D 119.3 . . ?
C18D C17D H17D 119.3 . . ?
C17D C18D C19D 117.7(16) . . ?
C17D C18D H18D 121.2 . . ?
C19D C18D H18D 121.2 . . ?
C20D C19D C18D 121.3(18) . . ?
C20D C19D H19D 119.4 . . ?
C18D C19D H19D 119.4 . . ?
C19D C20D C21D 120.3(16) . . ?
C19D C20D H20D 119.8 . . ?
C21D C20D H20D 119.8 . . ?
C16D C21D C20D 119.4(15) . . ?
C16D C21D C9D 115.1(14) . . ?
C20D C21D C9D 125.5(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
C15B P1B C1B C2B -131.3(13) . . . . ?
C21B P1B C1B C2B 133.6(13) . . . . ?
C15B P1B C1B C8B 48.3(12) . . . . ?
C21B P1B C1B C8B -46.9(12) . . . . ?
C8B C1B C2B C4B 0(2) . . . . ?
P1B C1B C2B C4B 179.3(14) . . . . ?
C8B C1B C2B C3B -177(5) . . . . ?
P1B C1B C2B C3B 2(5) . . . . ?
C8B C1B C2B Cl1Y 179(2) . . . . ?
P1B C1B C2B Cl1Y -1(3) . . . . ?
C1B C2B C4B C5B -3(3) . . . . ?
C3B C2B C4B C5B 175(4) . . . . ?
Cl1Y C2B C4B C5B 178(3) . . . . ?
C2B C4B C5B C6B 5(3) . . . . ?
C4B C5B C6B C8B -4(3) . . . . ?
C4B C5B C6B C7B 176(2) . . . . ?
C2B C1B C8B C6B 2(2) . . . . ?
P1B C1B C8B C6B -178.0(11) . . . . ?
C2B C1B C8B C9B 177.7(12) . . . . ?
P1B C1B C8B C9B -1.9(17) . . . . ?
C5B C6B C8B C1B 0(2) . . . . ?
C7B C6B C8B C1B -179.4(16) . . . . ?
C5B C6B C8B C9B -175.5(13) . . . . ?
C7B C6B C8B C9B 5(2) . . . . ?
C1B C8B C9B C10B -57.9(17) . . . . ?
C6B C8B C9B C10B 118.1(15) . . . . ?
C1B C8B C9B C16B 59.5(16) . . . . ?
C6B C8B C9B C16B -124.5(15) . . . . ?
C8B C9B C10B C11B -120.5(15) . . . . ?
C16B C9B C10B C11B 123.2(15) . . . . ?
C8B C9B C10B C15B 59.7(16) . . . . ?
C16B C9B C10B C15B -56.5(15) . . . . ?
C15B C10B C11B C12B -1(2) . . . . ?
C9B C10B C11B C12B 179.3(13) . . . . ?
C15B C10B C11B C7Y 176(2) . . . . ?
C9B C10B C11B C7Y -3(3) . . . . ?
C10B C11B C12B C13B 0(2) . . . . ?
C7Y C11B C12B C13B -177(2) . . . . ?
C11B C12B C13B C14B 2(2) . . . . ?
C12B C13B C14B C15B -3(2) . . . . ?
C12B C13B C14B C3Y 175(6) . . . . ?
C12B C13B C14B Cl1B -177.7(13) . . . . ?
C13B C14B C15B C10B 1.6(18) . . . . ?
C3Y C14B C15B C10B -176(6) . . . . ?
Cl1B C14B C15B C10B 176.8(11) . . . . ?
C13B C14B C15B P1B -175.9(10) . . . . ?
C3Y C14B C15B P1B 6(6) . . . . ?
Cl1B C14B C15B P1B -0.7(17) . . . . ?
C11B C10B C15B C14B 0.1(19) . . . . ?
C9B C10B C15B C14B 179.9(11) . . . . ?
C11B C10B C15B P1B 177.8(10) . . . . ?
C9B C10B C15B P1B -2.4(15) . . . . ?
C21B P1B C15B C14B -132.7(11) . . . . ?
C1B P1B C15B C14B 131.5(12) . . . . ?
C21B P1B C15B C10B 49.7(11) . . . . ?
C1B P1B C15B C10B -46.1(11) . . . . ?
C10B C9B C16B C17B -119.5(14) . . . . ?
C8B C9B C16B C17B 123.5(14) . . . . ?
C10B C9B C16B C21B 58.4(16) . . . . ?
C8B C9B C16B C21B -58.6(16) . . . . ?
C21B C16B C17B C18B 2(2) . . . . ?
C9B C16B C17B C18B -179.9(13) . . . . ?
C16B C17B C18B C19B -1(2) . . . . ?
C17B C18B C19B C20B 1(2) . . . . ?
C18B C19B C20B C21B -2(2) . . . . ?
C19B C20B C21B C16B 2.7(19) . . . . ?
C19B C20B C21B P1B -178.6(10) . . . . ?
C17B C16B C21B C20B -3(2) . . . . ?
C9B C16B C21B C20B 179.1(11) . . . . ?
C17B C16B C21B P1B 178.3(10) . . . . ?
C9B C16B C21B P1B 0.3(15) . . . . ?
C15B P1B C21B C20B 133.3(11) . . . . ?
C1B P1B C21B C20B -131.6(12) . . . . ?
C15B P1B C21B C16B -47.9(11) . . . . ?
C1B P1B C21B C16B 47.2(11) . . . . ?
C21C P1C C1C C2C -135.4(12) . . . . ?
C15C P1C C1C C2C 129.3(12) . . . . ?
C21C P1C C1C C8C 46.7(11) . . . . ?
C15C P1C C1C C8C -48.7(11) . . . . ?
C8C C1C C2C C4C -3(2) . . . . ?
P1C C1C C2C C4C 178.7(11) . . . . ?
C8C C1C C2C C3C -178.3(11) . . . . ?
P1C C1C C2C C3C 3.8(19) . . . . ?
C1C C2C C4C C5C 3(2) . . . . ?
C3C C2C C4C C5C 177.8(12) . . . . ?
C2C C4C C5C C6C -1(2) . . . . ?
C4C C5C C6C C8C -0.2(19) . . . . ?
C4C C5C C6C C7C 178.0(12) . . . . ?
C5C C6C C8C C1C -0.6(18) . . . . ?
C7C C6C C8C C1C -178.7(12) . . . . ?
C5C C6C C8C C9C 179.3(12) . . . . ?
C7C C6C C8C C9C 1(2) . . . . ?
C2C C1C C8C C6C 2.3(19) . . . . ?
P1C C1C C8C C6C -179.7(10) . . . . ?
C2C C1C C8C C9C -177.6(12) . . . . ?
P1C C1C C8C C9C 0.5(15) . . . . ?
C6C C8C C9C C16C 120.2(14) . . . . ?
C1C C8C C9C C16C -60.0(15) . . . . ?
C6C C8C C9C C10C -120.6(13) . . . . ?
C1C C8C C9C C10C 59.3(14) . . . . ?
C16C C9C C10C C11C -117.6(15) . . . . ?
C8C C9C C10C C11C 123.1(14) . . . . ?
C16C C9C C10C C15C 59.6(16) . . . . ?
C8C C9C C10C C15C -59.7(15) . . . . ?
C15C C10C C11C C12C 4(2) . . . . ?
C9C C10C C11C C12C -178.5(12) . . . . ?
C10C C11C C12C C13C -3(2) . . . . ?
C11C C12C C13C C14C 2(2) . . . . ?
C12C C13C C14C C15C -3(2) . . . . ?
C12C C13C C14C Cl1X 177.6(11) . . . . ?
C13C C14C C15C C10C 4(2) . . . . ?
Cl1X C14C C15C C10C -176.5(10) . . . . ?
C13C C14C C15C P1C -178.3(11) . . . . ?
Cl1X C14C C15C P1C 1.4(18) . . . . ?
C11C C10C C15C C14C -5(2) . . . . ?
C9C C10C C15C C14C 178.2(11) . . . . ?
C11C C10C C15C P1C 177.3(10) . . . . ?
C9C C10C C15C P1C -0.1(15) . . . . ?
C1C P1C C15C C14C -129.2(13) . . . . ?
C21C P1C C15C C14C 135.3(13) . . . . ?
C1C P1C C15C C10C 48.8(11) . . . . ?
C21C P1C C15C C10C -46.7(11) . . . . ?
C10C C9C C16C C17C 120.8(15) . . . . ?
C8C C9C C16C C17C -120.2(15) . . . . ?
C10C C9C C16C C21C -59.7(16) . . . . ?
C8C C9C C16C C21C 59.3(15) . . . . ?
C21C C16C C17C C18C 2(2) . . . . ?
C9C C16C C17C C18C -178.5(14) . . . . ?
C16C C17C C18C C19C -2(3) . . . . ?
C17C C18C C19C C20C 0(3) . . . . ?
C18C C19C C20C C21C 2(3) . . . . ?
C18C C19C C20C Cl1C -179.6(15) . . . . ?
C17C C16C C21C C20C 0(2) . . . . ?
C9C C16C C21C C20C -179.6(12) . . . . ?
C17C C16C C21C P1C -179.9(10) . . . . ?
C9C C16C C21C P1C 0.6(16) . . . . ?
C19C C20C C21C C16C -2(2) . . . . ?
Cl1C C20C C21C C16C 179.6(13) . . . . ?
C19C C20C C21C P1C 178.0(12) . . . . ?
Cl1C C20C C21C P1C -1(2) . . . . ?
C1C P1C C21C C16C -48.6(12) . . . . ?
C15C P1C C21C C16C 47.4(12) . . . . ?
C1C P1C C21C C20C 131.6(13) . . . . ?
C15C P1C C21C C20C -132.4(13) . . . . ?
C21A P1A C1A C2A -131.1(12) . . . . ?
C15A P1A C1A C2A 131.8(12) . . . . ?
C21A P1A C1A C8A 51.3(11) . . . . ?
C15A P1A C1A C8A -45.9(11) . . . . ?
C8A C1A C2A C4A -1(2) . . . . ?
P1A C1A C2A C4A -178.9(11) . . . . ?
C8A C1A C2A C3A -178.6(12) . . . . ?
P1A C1A C2A C3A 3.8(19) . . . . ?
C1A C2A C4A C5A 2(2) . . . . ?
C3A C2A C4A C5A 179.3(13) . . . . ?
C2A C4A C5A C6A -1(2) . . . . ?
C4A C5A C6A C8A -1(2) . . . . ?
C4A C5A C6A C7A 178.2(13) . . . . ?
C5A C6A C8A C1A 1(2) . . . . ?
C7A C6A C8A C1A -177.6(12) . . . . ?
C5A C6A C8A C9A -178.9(12) . . . . ?
C7A C6A C8A C9A 2(2) . . . . ?
C2A C1A C8A C6A 0(2) . . . . ?
P1A C1A C8A C6A 177.6(10) . . . . ?
C2A C1A C8A C9A 179.9(12) . . . . ?
P1A C1A C8A C9A -2.4(15) . . . . ?
C6A C8A C9A C10A -120.5(15) . . . . ?
C1A C8A C9A C10A 59.4(16) . . . . ?
C6A C8A C9A C16A 123.7(15) . . . . ?
C1A C8A C9A C16A -56.4(15) . . . . ?
C8A C9A C10A C11A 123.3(14) . . . . ?
C16A C9A C10A C11A -120.0(14) . . . . ?
C8A C9A C10A C15A -57.9(17) . . . . ?
C16A C9A C10A C15A 58.8(15) . . . . ?
C15A C10A C11A C12A 3(2) . . . . ?
C9A C10A C11A C12A -178.6(13) . . . . ?
C10A C11A C12A C13A -3(2) . . . . ?
C11A C12A C13A C14A 4(3) . . . . ?
C12A C13A C14A C15A -4(3) . . . . ?
C12A C13A C14A Cl1A 173.6(13) . . . . ?
C11A C10A C15A C14A -3(2) . . . . ?
C9A C10A C15A C14A 178.5(12) . . . . ?
C11A C10A C15A P1A 177.6(11) . . . . ?
C9A C10A C15A P1A -1.1(16) . . . . ?
C13A C14A C15A C10A 3(2) . . . . ?
Cl1A C14A C15A C10A -174.2(12) . . . . ?
C13A C14A C15A P1A -177.2(12) . . . . ?
Cl1A C14A C15A P1A 5(2) . . . . ?
C21A P1A C15A C10A -49.2(12) . . . . ?
C1A P1A C15A C10A 47.5(12) . . . . ?
C21A P1A C15A C14A 131.3(13) . . . . ?
C1A P1A C15A C14A -132.0(13) . . . . ?
C8A C9A C16A C17A -122.6(14) . . . . ?
C10A C9A C16A C17A 120.4(14) . . . . ?
C8A C9A C16A C21A 58.8(15) . . . . ?
C10A C9A C16A C21A -58.2(14) . . . . ?
C21A C16A C17A C18A 0(3) . . . . ?
C9A C16A C17A C18A -178.2(17) . . . . ?
C16A C17A C18A C19A 3(4) . . . . ?
C17A C18A C19A C20A -3(5) . . . . ?
C18A C19A C20A C21A -1(4) . . . . ?
C18A C19A C20A Cl1Z -173(3) . . . . ?
C19A C20A C21A C16A 3(2) . . . . ?
Cl1Z C20A C21A C16A 175.5(14) . . . . ?
C19A C20A C21A P1A 178.2(15) . . . . ?
Cl1Z C20A C21A P1A -10(3) . . . . ?
C17A C16A C21A C20A -3.1(19) . . . . ?
C9A C16A C21A C20A 175.6(12) . . . . ?
C17A C16A C21A P1A -179.0(10) . . . . ?
C9A C16A C21A P1A -0.3(15) . . . . ?
C15A P1A C21A C20A -126.2(16) . . . . ?
C1A P1A C21A C20A 137.2(16) . . . . ?
C15A P1A C21A C16A 48.6(11) . . . . ?
C1A P1A C21A C16A -48.1(11) . . . . ?
C15D P1D C1D C8D 47.2(13) . . . . ?
C16D P1D C1D C8D -48.0(12) . . . . ?
C15D P1D C1D C2D -126.8(12) . . . . ?
C16D P1D C1D C2D 138.1(12) . . . . ?
C8D C1D C2D C4D 6(2) . . . . ?
P1D C1D C2D C4D 179.4(12) . . . . ?
C8D C1D C2D C3D -176.5(15) . . . . ?
P1D C1D C2D C3D -3(2) . . . . ?
C1D C2D C4D C5D -3(3) . . . . ?
C3D C2D C4D C5D 179.7(18) . . . . ?
C2D C4D C5D C6D 2(3) . . . . ?
C4D C5D C6D C8D -3(3) . . . . ?
C4D C5D C6D C7D -177.7(15) . . . . ?
C2D C1D C8D C6D -8(2) . . . . ?
P1D C1D C8D C6D 178.2(10) . . . . ?
C2D C1D C8D C9D 174.9(13) . . . . ?
P1D C1D C8D C9D 1.2(17) . . . . ?
C5D C6D C8D C1D 7(2) . . . . ?
C7D C6D C8D C1D -179.4(14) . . . . ?
C5D C6D C8D C9D -176.6(13) . . . . ?
C7D C6D C8D C9D -3(2) . . . . ?
C1D C8D C9D C10D -58.5(16) . . . . ?
C6D C8D C9D C10D 124.7(14) . . . . ?
C1D C8D C9D C21D 57.1(16) . . . . ?
C6D C8D C9D C21D -119.7(14) . . . . ?
C21D C9D C10D C15D -61.9(16) . . . . ?
C8D C9D C10D C15D 54.1(15) . . . . ?
C21D C9D C10D C11D 123.3(15) . . . . ?
C8D C9D C10D C11D -120.8(15) . . . . ?
C15D C10D C11D C12D 2(2) . . . . ?
C9D C10D C11D C12D 177.0(14) . . . . ?
C10D C11D C12D C13D -2(3) . . . . ?
C11D C12D C13D C14D 3(3) . . . . ?
C12D C13D C14D C15D -3(2) . . . . ?
C12D C13D C14D Cl1D 178.6(12) . . . . ?
C11D C10D C15D C14D -2(2) . . . . ?
C9D C10D C15D C14D -177.2(12) . . . . ?
C11D C10D C15D P1D 179.7(10) . . . . ?
C9D C10D C15D P1D 4.6(16) . . . . ?
C13D C14D C15D C10D 2(2) . . . . ?
Cl1D C14D C15D C10D -178.8(11) . . . . ?
C13D C14D C15D P1D -179.7(12) . . . . ?
Cl1D C14D C15D P1D -0.8(18) . . . . ?
C1D P1D C15D C10D -51.1(12) . . . . ?
C16D P1D C15D C10D 43.5(12) . . . . ?
C1D P1D C15D C14D 130.9(13) . . . . ?
C16D P1D C15D C14D -134.5(13) . . . . ?
C15D P1D C16D C21D -45.5(12) . . . . ?
C1D P1D C16D C21D 48.7(12) . . . . ?
C15D P1D C16D C17D 132.2(12) . . . . ?
C1D P1D C16D C17D -133.6(12) . . . . ?
C21D C16D C17D C18D -1(2) . . . . ?
P1D C16D C17D C18D -179.0(11) . . . . ?
C16D C17D C18D C19D 3(2) . . . . ?
C17D C18D C19D C20D -4(2) . . . . ?
C18D C19D C20D C21D 2(2) . . . . ?
C17D C16D C21D C20D 0(2) . . . . ?
P1D C16D C21D C20D 177.4(10) . . . . ?
C17D C16D C21D C9D -178.7(11) . . . . ?
P1D C16D C21D C9D -1.0(17) . . . . ?
C19D C20D C21D C16D 0(2) . . . . ?
C19D C20D C21D C9D 178.1(12) . . . . ?
C10D C9D C21D C16D 59.5(16) . . . . ?
C8D C9D C21D C16D -56.3(15) . . . . ?
C10D C9D C21D C20D -118.8(15) . . . . ?
C8D C9D C21D C20D 125.4(15) . . . . ?

_refine_diff_density_max         0.270
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.049




# start Validation Reply Form
_vrf_THETM01_N_DAMA              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: All obtained crystals of the compound were small plates that were 
very weakly diffracting. The lack of reflections also led to a number of 
additional problems (see below). In spite of this, all the non-H atoms could 
easily be located in the electron difference map, and the overall shape of the
 molecule as well as the packing of molecules can be considered to be 
reasonably determined.
;
_vrf_RINTA01_N_DAMA              
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: See above.
;
_vrf_PLAT088_N_DAMA              
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.74 Note  
RESPONSE: See above.
;
_vrf_PLAT234_N_DAMA              
;
PROBLEM: Large Hirshfeld Difference C4B      --C5B      .       0.28 Ang.  
RESPONSE: See above.
;
_vrf_PLAT340_N_DAMA              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02362 Ang.  
RESPONSE: See above.
;
_vrf_PLAT910_N_DAMA              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         18 Note  
RESPONSE: See above.
;
_vrf_PLAT020_N_DAMA              
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.147 Report
RESPONSE: See above.
;
_vrf_PLAT241_N_DAMA              
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        P1C Check 
RESPONSE: See above.
;
_vrf_PLAT242_N_DAMA              
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C2B Check 
RESPONSE: See above.
;
_vrf_PLAT250_N_DAMA              
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.4 Note  
RESPONSE: See above.
;
_vrf_PLAT906_N_DAMA              
;
PROBLEM: Large K Value in the Analysis of Variance ......     27.553 Check 
RESPONSE: See above.
;
_vrf_PLAT911_N_DAMA              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.417          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_nt0800_LHG195A
_database_code_depnum_ccdc_archive 'CCDC 2061858'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
;
chloro(1-trifluoromethyl-9--phosphotriptycene)gold(I) 
toluene hemi-solvate
;
_chemical_name_common            
;
chloro(1-trifluoromethyl-9--phosphotriptycene)gold(I) 
toluene hemi-solvate
;
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C20 H12 Au Cl F3 P), C7 H8'
_chemical_formula_sum            'C47 H32 Au2 Cl2 F6 P2'
_chemical_formula_weight         1237.50

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'
Au Au -4.4197 7.2980 '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'
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                   14.81554(13)
_cell_length_b                   17.38646(13)
_cell_length_c                   16.11733(12)
_cell_angle_alpha                90
_cell_angle_beta                 90.9329(7)
_cell_angle_gamma                90
_cell_volume                     4151.11(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    20062
_cell_measurement_theta_min      3.7120
_cell_measurement_theta_max      67.0660

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_F_000             2360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    15.540
_shelx_estimated_absorpt_T_min   0.090
_shelx_estimated_absorpt_T_max   0.166
_exptl_absorpt_correction_T_min  0.064
_exptl_absorpt_correction_T_max  0.234
_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_detector_area_resol_mean 5.1856
_diffrn_reflns_number            28416
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.740
_diffrn_reflns_theta_max         67.146
_diffrn_reflns_theta_full        67.147
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             7376
_reflns_number_gt                7267
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0267P)²+10.5124P] 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         7376
_refine_ls_number_parameters     598
_refine_ls_number_restraints     105
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.0706
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_restrained_S_all      1.181
_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
Au1 Au 0.41348(2) 0.40598(2) 0.18946(2) 0.02805(6) Uani 1 1 d . . . . .
Cl1 Cl 0.42833(9) 0.30771(7) 0.09665(8) 0.0410(3) Uani 1 1 d . . . . .
P1 P 0.39868(7) 0.50528(6) 0.27477(6) 0.0247(2) Uani 1 1 d . . . . .
F1 F 0.4779(2) 0.35164(18) 0.36363(18) 0.0455(7) Uani 1 1 d . . . . .
F2 F 0.4145(4) 0.30643(19) 0.4706(2) 0.0758(13) Uani 1 1 d . . . . .
F3 F 0.3347(2) 0.33332(18) 0.3615(2) 0.0503(8) Uani 1 1 d . . . . .
C1 C 0.4039(4) 0.3575(3) 0.4100(3) 0.0401(11) Uani 1 1 d . . . . .
C2 C 0.3893(3) 0.4369(3) 0.4415(3) 0.0284(9) Uani 1 1 d . . . . .
C3 C 0.3766(3) 0.4474(3) 0.5268(3) 0.0330(10) Uani 1 1 d . . . . .
H3 H 0.376292 0.403986 0.562582 0.040 Uiso 1 1 calc R U . . .
C4 C 0.3646(3) 0.5196(3) 0.5593(3) 0.0339(10) Uani 1 1 d . . . . .
H4 H 0.356101 0.525902 0.617240 0.041 Uiso 1 1 calc R U . . .
C5 C 0.3649(3) 0.5831(3) 0.5080(3) 0.0311(10) Uani 1 1 d . . . . .
H5 H 0.357706 0.633173 0.530535 0.037 Uiso 1 1 calc R U . . .
C6 C 0.3756(3) 0.5737(3) 0.4234(3) 0.0267(9) Uani 1 1 d . . . . .
C7 C 0.3876(3) 0.5009(3) 0.3888(3) 0.0248(8) Uani 1 1 d . . . . .
C8 C 0.4858(3) 0.5778(2) 0.2730(3) 0.0260(9) Uani 1 1 d . . . . .
C9 C 0.5672(3) 0.5717(3) 0.2315(3) 0.0284(9) Uani 1 1 d . . . . .
H9 H 0.579222 0.527914 0.198119 0.034 Uiso 1 1 calc R U . . .
C10 C 0.6307(3) 0.6302(3) 0.2393(3) 0.0318(10) Uani 1 1 d . . . . .
H10 H 0.686761 0.626511 0.211772 0.038 Uiso 1 1 calc R U . . .
C11 C 0.6115(3) 0.6946(3) 0.2879(3) 0.0302(9) Uani 1 1 d . . . . .
H11 H 0.655378 0.734203 0.293852 0.036 Uiso 1 1 calc R U . . .
C12 C 0.5294(3) 0.7017(3) 0.3275(3) 0.0291(9) Uani 1 1 d . . . . .
H12 H 0.516501 0.746258 0.359322 0.035 Uiso 1 1 calc R U . . .
C13 C 0.4661(3) 0.6428(3) 0.3202(3) 0.0283(9) Uani 1 1 d . . . . .
C14 C 0.3759(3) 0.6430(3) 0.3648(3) 0.0287(9) Uani 1 1 d . . . . .
H14 H 0.368072 0.691917 0.396585 0.034 Uiso 1 1 calc R U . . .
C15 C 0.2983(3) 0.6319(3) 0.3026(3) 0.0275(9) Uani 1 1 d . . . . .
C16 C 0.2251(3) 0.6811(3) 0.2943(3) 0.0318(10) Uani 1 1 d . . . . .
H16 H 0.221839 0.726115 0.327432 0.038 Uiso 1 1 calc R U . . .
C17 C 0.1562(3) 0.6641(3) 0.2368(3) 0.0358(11) Uani 1 1 d . . . . .
H17 H 0.105642 0.697487 0.231431 0.043 Uiso 1 1 calc R U . . .
C18 C 0.1612(3) 0.5987(3) 0.1875(3) 0.0373(11) Uani 1 1 d . . . . .
H18 H 0.114638 0.587984 0.147977 0.045 Uiso 1 1 calc R U . . .
C19 C 0.2340(3) 0.5491(3) 0.1957(3) 0.0338(10) Uani 1 1 d . . . . .
H19 H 0.237619 0.504325 0.162113 0.041 Uiso 1 1 calc R U . . .
C20 C 0.3015(3) 0.5656(3) 0.2537(3) 0.0268(9) Uani 1 1 d . . . . .
Au2 Au 0.91163(2) 0.54700(2) 0.19837(2) 0.02908(6) Uani 1 1 d . . . . .
Cl2 Cl 0.93546(9) 0.63605(7) 0.09664(8) 0.0437(3) Uani 1 1 d . . . . .
P2 P 0.89421(7) 0.45767(6) 0.29476(6) 0.0243(2) Uani 1 1 d . . . . .
F4 F 0.95124(19) 0.63576(16) 0.36217(18) 0.0401(6) Uani 1 1 d . . . . .
F5 F 0.8641(3) 0.68182(16) 0.45475(19) 0.0524(8) Uani 1 1 d . . . . .
F6 F 0.80697(18) 0.62547(16) 0.34751(17) 0.0386(6) Uani 1 1 d . . . . .
C21 C 0.8749(3) 0.6218(3) 0.4037(3) 0.0337(10) Uani 1 1 d . . . . .
C22 C 0.8766(3) 0.5468(2) 0.4488(3) 0.0264(9) Uani 1 1 d . . . . .
C23 C 0.8681(3) 0.5474(3) 0.5349(3) 0.0287(9) Uani 1 1 d . . . . .
H23 H 0.863564 0.594962 0.563469 0.034 Uiso 1 1 calc R U . . .
C24 C 0.8661(3) 0.4790(3) 0.5787(3) 0.0300(9) Uani 1 1 d . . . . .
H24 H 0.861331 0.479913 0.637446 0.036 Uiso 1 1 calc R U . . .
C25 C 0.8711(3) 0.4097(3) 0.5378(3) 0.0273(9) Uani 1 1 d . . . . .
H25 H 0.869878 0.362994 0.568368 0.033 Uiso 1 1 calc R U . . .
C26 C 0.8778(3) 0.4077(2) 0.4522(3) 0.0248(8) Uani 1 1 d . . . . .
C27 C 0.8825(3) 0.4762(3) 0.4067(3) 0.0248(8) Uani 1 1 d . . . . .
C28 C 0.9840(3) 0.3868(2) 0.3026(3) 0.0259(9) Uani 1 1 d . . . . .
C29 C 1.0640(3) 0.3898(3) 0.2584(3) 0.0289(9) Uani 1 1 d . . . . .
H29 H 1.074214 0.429692 0.219458 0.035 Uiso 1 1 calc R U . . .
C30 C 1.1289(3) 0.3325(3) 0.2728(3) 0.0332(10) Uani 1 1 d . . . . .
H30 H 1.184262 0.333856 0.243913 0.040 Uiso 1 1 calc R U . . .
C31 C 1.1129(3) 0.2740(3) 0.3291(3) 0.0331(10) Uani 1 1 d . . . . .
H31 H 1.157521 0.235602 0.338583 0.040 Uiso 1 1 calc R U . . .
C32 C 1.0319(3) 0.2707(3) 0.3720(3) 0.0279(9) Uani 1 1 d . . . . .
H32 H 1.020927 0.230036 0.409860 0.033 Uiso 1 1 calc R U . . .
C33 C 0.9671(3) 0.3279(2) 0.3587(3) 0.0253(8) Uani 1 1 d . . . . .
C34 C 0.8784(3) 0.3318(2) 0.4051(3) 0.0258(9) Uani 1 1 d . . . . .
H34 H 0.872867 0.287373 0.444086 0.031 Uiso 1 1 calc R U . . .
C35 C 0.7996(3) 0.3331(2) 0.3428(3) 0.0256(9) Uani 1 1 d . . . . .
C36 C 0.7292(3) 0.2803(3) 0.3422(3) 0.0297(9) Uani 1 1 d . . . . .
H36 H 0.728175 0.239969 0.381978 0.036 Uiso 1 1 calc R U . . .
C37 C 0.6600(3) 0.2869(3) 0.2830(3) 0.0336(10) Uani 1 1 d . . . . .
H37 H 0.611619 0.251046 0.282798 0.040 Uiso 1 1 calc R U . . .
C38 C 0.6612(3) 0.3449(3) 0.2244(3) 0.0348(10) Uani 1 1 d . . . . .
H38 H 0.614230 0.348142 0.183741 0.042 Uiso 1 1 calc R U . . .
C39 C 0.7307(3) 0.3986(3) 0.2248(3) 0.0316(10) Uani 1 1 d . . . . .
H39 H 0.731265 0.438968 0.185113 0.038 Uiso 1 1 calc R U . . .
C40 C 0.7994(3) 0.3920(3) 0.2842(3) 0.0268(9) Uani 1 1 d . . . . .
C41A C 0.8226(9) 0.3309(8) 0.0189(8) 0.079(5) Uani 0.616(14) 1 d D . P A 1
H41A H 0.883882 0.348652 0.007276 0.119 Uiso 0.616(14) 1 calc R U P A 1
H41B H 0.804277 0.292209 -0.022174 0.119 Uiso 0.616(14) 1 calc R U P A 1
H41C H 0.821348 0.308264 0.074585 0.119 Uiso 0.616(14) 1 calc R U P A 1
C42A C 0.7596(10) 0.3968(7) 0.0147(7) 0.047(3) Uani 0.616(14) 1 d D . P A 1
C43A C 0.7947(9) 0.4706(11) 0.0159(17) 0.055(4) Uani 0.616(14) 1 d D . P A 1
H43A H 0.858173 0.478039 0.015593 0.066 Uiso 0.616(14) 1 calc R U P A 1
C44A C 0.7385(10) 0.5328(7) 0.0177(7) 0.050(3) Uani 0.616(14) 1 d D . P A 1
H44A H 0.762748 0.583297 0.020373 0.060 Uiso 0.616(14) 1 calc R U P A 1
C45A C 0.6449(9) 0.5215(7) 0.0155(8) 0.055(3) Uani 0.616(14) 1 d D . P A 1
H45A H 0.604968 0.564229 0.014853 0.066 Uiso 0.616(14) 1 calc R U P A 1
C46A C 0.6107(10) 0.4452(9) 0.014(2) 0.051(4) Uani 0.616(14) 1 d D . P A 1
H46A H 0.547363 0.436894 0.014425 0.061 Uiso 0.616(14) 1 calc R U P A 1
C47A C 0.6674(11) 0.3845(10) 0.013(2) 0.051(4) Uani 0.616(14) 1 d D . P A 1
H47A H 0.644104 0.333564 0.011523 0.061 Uiso 0.616(14) 1 calc R U P A 1
C41B C 0.9000(12) 0.3949(13) 0.0434(12) 0.077(6) Uani 0.384(14) 1 d D . P A 2
H41D H 0.935173 0.442600 0.042366 0.116 Uiso 0.384(14) 1 calc R U P A 2
H41E H 0.922085 0.359625 0.000907 0.116 Uiso 0.384(14) 1 calc R U P A 2
H41F H 0.906506 0.370790 0.098187 0.116 Uiso 0.384(14) 1 calc R U P A 2
C42B C 0.8041(12) 0.4124(11) 0.0267(11) 0.045(4) Uani 0.384(14) 1 d D . P A 2
C43B C 0.7778(16) 0.4885(11) 0.023(2) 0.044(5) Uani 0.384(14) 1 d D . P A 2
H43B H 0.822941 0.527031 0.028313 0.053 Uiso 0.384(14) 1 calc R U P A 2
C44B C 0.6909(19) 0.5110(15) 0.0105(15) 0.072(6) Uani 0.384(14) 1 d D . P A 2
H44B H 0.674504 0.563765 0.007073 0.087 Uiso 0.384(14) 1 calc R U P A 2
C45B C 0.626(2) 0.4520(19) 0.003(4) 0.079(9) Uani 0.384(14) 1 d D . P A 2
H45B H 0.564474 0.464248 -0.005924 0.095 Uiso 0.384(14) 1 calc R U P A 2
C46B C 0.6541(19) 0.3740(17) 0.010(5) 0.078(10) Uani 0.384(14) 1 d D . P A 2
H46B H 0.609332 0.334964 0.006671 0.094 Uiso 0.384(14) 1 calc R U P A 2
C47B C 0.7404(12) 0.3529(11) 0.0204(10) 0.055(5) Uani 0.384(14) 1 d D . P A 2
H47B H 0.757710 0.300302 0.023407 0.066 Uiso 0.384(14) 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
Au1 P1 2.2201(11) . ?
Au1 Cl1 2.2838(11) . ?
P1 C8 1.805(4) . ?
P1 C20 1.808(4) . ?
P1 C7 1.850(4) . ?
F1 C1 1.341(6) . ?
F2 C1 1.328(6) . ?
F3 C1 1.345(6) . ?
C1 C2 1.488(7) . ?
C2 C7 1.399(6) . ?
C2 C3 1.403(7) . ?
C3 C4 1.373(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(6) . ?
C6 C14 1.532(6) . ?
C8 C9 1.393(6) . ?
C8 C13 1.395(7) . ?
C9 C10 1.391(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.398(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.390(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.528(6) . ?
C14 C15 1.526(6) . ?
C14 H14 1.0000 . ?
C15 C16 1.385(6) . ?
C15 C20 1.397(7) . ?
C16 C17 1.399(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.388(6) . ?
C19 H19 0.9500 . ?
Au2 P2 2.2150(11) . ?
Au2 Cl2 2.2866(12) . ?
P2 C40 1.815(4) . ?
P2 C28 1.816(4) . ?
P2 C27 1.843(4) . ?
F4 C21 1.346(6) . ?
F5 C21 1.339(5) . ?
F6 C21 1.344(5) . ?
C21 C22 1.494(6) . ?
C22 C23 1.394(6) . ?
C22 C27 1.406(6) . ?
C23 C24 1.384(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.400(6) . ?
C26 C34 1.523(6) . ?
C28 C33 1.391(6) . ?
C28 C29 1.394(6) . ?
C29 C30 1.401(7) . ?
C29 H29 0.9500 . ?
C30 C31 1.387(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.396(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.395(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.523(6) . ?
C34 C35 1.528(6) . ?
C34 H34 1.0000 . ?
C35 C36 1.389(6) . ?
C35 C40 1.394(6) . ?
C36 C37 1.394(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.382(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.389(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.392(6) . ?
C39 H39 0.9500 . ?
C41A C42A 1.478(14) . ?
C41A H41A 0.9800 . ?
C41A H41B 0.9800 . ?
C41A H41C 0.9800 . ?
C42A C47A 1.38(2) . ?
C42A C43A 1.384(16) . ?
C43A C44A 1.364(17) . ?
C43A H43A 0.9500 . ?
C44A C45A 1.400(18) . ?
C44A H44A 0.9500 . ?
C45A C46A 1.420(19) . ?
C45A H45A 0.9500 . ?
C46A C47A 1.35(2) . ?
C46A H46A 0.9500 . ?
C47A H47A 0.9500 . ?
C41B C42B 1.474(19) . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
C42B C43B 1.380(17) . ?
C42B C47B 1.40(2) . ?
C43B C44B 1.36(2) . ?
C43B H43B 0.9500 . ?
C44B C45B 1.41(3) . ?
C44B H44B 0.9500 . ?
C45B C46B 1.42(3) . ?
C45B H45B 0.9500 . ?
C46B C47B 1.34(3) . ?
C46B H46B 0.9500 . ?
C47B H47B 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
P1 Au1 Cl1 177.35(4) . . ?
C8 P1 C20 99.2(2) . . ?
C8 P1 C7 96.87(19) . . ?
C20 P1 C7 97.30(19) . . ?
C8 P1 Au1 117.10(15) . . ?
C20 P1 Au1 114.90(15) . . ?
C7 P1 Au1 126.50(15) . . ?
F2 C1 F1 105.7(4) . . ?
F2 C1 F3 107.3(5) . . ?
F1 C1 F3 106.0(4) . . ?
F2 C1 C2 112.7(4) . . ?
F1 C1 C2 112.7(4) . . ?
F3 C1 C2 112.0(4) . . ?
C7 C2 C3 119.3(4) . . ?
C7 C2 C1 122.2(4) . . ?
C3 C2 C1 118.6(4) . . ?
C4 C3 C2 120.9(4) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 119.8(4) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C7 121.2(4) . . ?
C5 C6 C14 121.0(4) . . ?
C7 C6 C14 117.8(4) . . ?
C6 C7 C2 118.7(4) . . ?
C6 C7 P1 111.9(3) . . ?
C2 C7 P1 129.4(3) . . ?
C9 C8 C13 121.0(4) . . ?
C9 C8 P1 125.4(4) . . ?
C13 C8 P1 113.6(3) . . ?
C10 C9 C8 119.3(4) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 119.6(4) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C12 C11 C10 121.1(4) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 119.3(4) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C12 C13 C8 119.7(4) . . ?
C12 C13 C14 123.4(4) . . ?
C8 C13 C14 116.9(4) . . ?
C15 C14 C13 110.2(4) . . ?
C15 C14 C6 107.2(4) . . ?
C13 C14 C6 107.4(3) . . ?
C15 C14 H14 110.6 . . ?
C13 C14 H14 110.6 . . ?
C6 C14 H14 110.6 . . ?
C16 C15 C20 119.3(4) . . ?
C16 C15 C14 124.4(4) . . ?
C20 C15 C14 116.3(4) . . ?
C15 C16 C17 119.7(5) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 120.3(4) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C19 C18 C17 120.3(5) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 119.2(5) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
C19 C20 C15 121.2(4) . . ?
C19 C20 P1 124.7(4) . . ?
C15 C20 P1 114.0(3) . . ?
P2 Au2 Cl2 177.26(4) . . ?
C40 P2 C28 98.3(2) . . ?
C40 P2 C27 96.69(19) . . ?
C28 P2 C27 97.51(19) . . ?
C40 P2 Au2 118.29(15) . . ?
C28 P2 Au2 115.55(15) . . ?
C27 P2 Au2 125.30(15) . . ?
F5 C21 F6 106.4(4) . . ?
F5 C21 F4 106.0(4) . . ?
F6 C21 F4 106.4(4) . . ?
F5 C21 C22 112.5(4) . . ?
F6 C21 C22 112.1(4) . . ?
F4 C21 C22 113.0(4) . . ?
C23 C22 C27 119.6(4) . . ?
C23 C22 C21 118.4(4) . . ?
C27 C22 C21 121.9(4) . . ?
C24 C23 C22 120.3(4) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 120.3(4) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.3(4) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C27 120.4(4) . . ?
C25 C26 C34 121.3(4) . . ?
C27 C26 C34 118.4(4) . . ?
C26 C27 C22 119.0(4) . . ?
C26 C27 P2 111.7(3) . . ?
C22 C27 P2 129.2(3) . . ?
C33 C28 C29 121.5(4) . . ?
C33 C28 P2 113.9(3) . . ?
C29 C28 P2 124.5(4) . . ?
C28 C29 C30 118.4(4) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C31 C30 C29 120.3(4) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C30 C31 C32 120.8(4) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 H31 119.6 . . ?
C33 C32 C31 119.3(4) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C28 C33 C32 119.6(4) . . ?
C28 C33 C34 116.8(4) . . ?
C32 C33 C34 123.6(4) . . ?
C33 C34 C26 107.2(3) . . ?
C33 C34 C35 109.6(3) . . ?
C26 C34 C35 107.7(3) . . ?
C33 C34 H34 110.8 . . ?
C26 C34 H34 110.8 . . ?
C35 C34 H34 110.8 . . ?
C36 C35 C40 119.3(4) . . ?
C36 C35 C34 124.1(4) . . ?
C40 C35 C34 116.6(4) . . ?
C35 C36 C37 119.6(4) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C38 C37 C36 120.7(4) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C37 C38 C39 120.3(4) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C38 C39 C40 118.8(5) . . ?
C38 C39 H39 120.6 . . ?
C40 C39 H39 120.6 . . ?
C39 C40 C35 121.3(4) . . ?
C39 C40 P2 124.7(4) . . ?
C35 C40 P2 114.0(3) . . ?
C42A C41A H41A 109.5 . . ?
C42A C41A H41B 109.5 . . ?
H41A C41A H41B 109.5 . . ?
C42A C41A H41C 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C47A C42A C43A 121.0(13) . . ?
C47A C42A C41A 120.2(14) . . ?
C43A C42A C41A 118.8(16) . . ?
C44A C43A C42A 120.4(12) . . ?
C44A C43A H43A 119.8 . . ?
C42A C43A H43A 119.8 . . ?
C43A C44A C45A 119.5(11) . . ?
C43A C44A H44A 120.2 . . ?
C45A C44A H44A 120.2 . . ?
C44A C45A C46A 118.9(13) . . ?
C44A C45A H45A 120.5 . . ?
C46A C45A H45A 120.5 . . ?
C47A C46A C45A 120.6(15) . . ?
C47A C46A H46A 119.7 . . ?
C45A C46A H46A 119.7 . . ?
C46A C47A C42A 119.5(15) . . ?
C46A C47A H47A 120.3 . . ?
C42A C47A H47A 120.3 . . ?
C42B C41B H41D 109.5 . . ?
C42B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
C42B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C43B C42B C47B 121.0(17) . . ?
C43B C42B C41B 118(2) . . ?
C47B C42B C41B 120.4(16) . . ?
C44B C43B C42B 123.3(18) . . ?
C44B C43B H43B 118.3 . . ?
C42B C43B H43B 118.3 . . ?
C43B C44B C45B 116(2) . . ?
C43B C44B H44B 121.8 . . ?
C45B C44B H44B 121.8 . . ?
C44B C45B C46B 120(2) . . ?
C44B C45B H45B 120.2 . . ?
C46B C45B H45B 120.2 . . ?
C47B C46B C45B 123(3) . . ?
C47B C46B H46B 118.4 . . ?
C45B C46B H46B 118.4 . . ?
C46B C47B C42B 116.5(19) . . ?
C46B C47B H47B 121.8 . . ?
C42B C47B H47B 121.8 . . ?

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
F2 C1 C2 C7 172.0(5) . . . . ?
F1 C1 C2 C7 52.5(6) . . . . ?
F3 C1 C2 C7 -66.9(6) . . . . ?
F2 C1 C2 C3 -8.2(7) . . . . ?
F1 C1 C2 C3 -127.7(4) . . . . ?
F3 C1 C2 C3 112.9(5) . . . . ?
C7 C2 C3 C4 -1.5(7) . . . . ?
C1 C2 C3 C4 178.7(4) . . . . ?
C2 C3 C4 C5 0.0(7) . . . . ?
C3 C4 C5 C6 1.2(7) . . . . ?
C4 C5 C6 C7 -1.0(6) . . . . ?
C4 C5 C6 C14 179.8(4) . . . . ?
C5 C6 C7 C2 -0.4(6) . . . . ?
C14 C6 C7 C2 178.8(4) . . . . ?
C5 C6 C7 P1 179.3(3) . . . . ?
C14 C6 C7 P1 -1.5(5) . . . . ?
C3 C2 C7 C6 1.6(6) . . . . ?
C1 C2 C7 C6 -178.6(4) . . . . ?
C3 C2 C7 P1 -178.0(3) . . . . ?
C1 C2 C7 P1 1.8(7) . . . . ?
C8 P1 C7 C6 51.3(3) . . . . ?
C20 P1 C7 C6 -48.9(3) . . . . ?
Au1 P1 C7 C6 -177.4(2) . . . . ?
C8 P1 C7 C2 -129.1(4) . . . . ?
C20 P1 C7 C2 130.7(4) . . . . ?
Au1 P1 C7 C2 2.2(5) . . . . ?
C20 P1 C8 C9 -133.6(4) . . . . ?
C7 P1 C8 C9 127.8(4) . . . . ?
Au1 P1 C8 C9 -9.4(4) . . . . ?
C20 P1 C8 C13 48.1(3) . . . . ?
C7 P1 C8 C13 -50.4(3) . . . . ?
Au1 P1 C8 C13 172.3(3) . . . . ?
C13 C8 C9 C10 1.9(6) . . . . ?
P1 C8 C9 C10 -176.3(3) . . . . ?
C8 C9 C10 C11 -0.7(6) . . . . ?
C9 C10 C11 C12 -1.0(6) . . . . ?
C10 C11 C12 C13 1.5(6) . . . . ?
C11 C12 C13 C8 -0.3(6) . . . . ?
C11 C12 C13 C14 176.8(4) . . . . ?
C9 C8 C13 C12 -1.4(6) . . . . ?
P1 C8 C13 C12 177.0(3) . . . . ?
C9 C8 C13 C14 -178.7(4) . . . . ?
P1 C8 C13 C14 -0.3(5) . . . . ?
C12 C13 C14 C15 125.8(4) . . . . ?
C8 C13 C14 C15 -57.1(5) . . . . ?
C12 C13 C14 C6 -117.8(4) . . . . ?
C8 C13 C14 C6 59.4(5) . . . . ?
C5 C6 C14 C15 -120.3(4) . . . . ?
C7 C6 C14 C15 60.5(5) . . . . ?
C5 C6 C14 C13 121.3(4) . . . . ?
C7 C6 C14 C13 -57.9(5) . . . . ?
C13 C14 C15 C16 -125.5(4) . . . . ?
C6 C14 C15 C16 117.9(4) . . . . ?
C13 C14 C15 C20 56.9(5) . . . . ?
C6 C14 C15 C20 -59.7(5) . . . . ?
C20 C15 C16 C17 -0.5(6) . . . . ?
C14 C15 C16 C17 -178.0(4) . . . . ?
C15 C16 C17 C18 -0.7(6) . . . . ?
C16 C17 C18 C19 1.0(7) . . . . ?
C17 C18 C19 C20 0.0(7) . . . . ?
C18 C19 C20 C15 -1.3(6) . . . . ?
C18 C19 C20 P1 177.7(3) . . . . ?
C16 C15 C20 C19 1.5(6) . . . . ?
C14 C15 C20 C19 179.2(4) . . . . ?
C16 C15 C20 P1 -177.6(3) . . . . ?
C14 C15 C20 P1 0.1(5) . . . . ?
C8 P1 C20 C19 132.7(4) . . . . ?
C7 P1 C20 C19 -129.1(4) . . . . ?
Au1 P1 C20 C19 7.0(4) . . . . ?
C8 P1 C20 C15 -48.2(3) . . . . ?
C7 P1 C20 C15 50.0(3) . . . . ?
Au1 P1 C20 C15 -173.9(3) . . . . ?
F5 C21 C22 C23 -0.5(6) . . . . ?
F6 C21 C22 C23 -120.4(4) . . . . ?
F4 C21 C22 C23 119.5(4) . . . . ?
F5 C21 C22 C27 176.6(4) . . . . ?
F6 C21 C22 C27 56.7(6) . . . . ?
F4 C21 C22 C27 -63.5(5) . . . . ?
C27 C22 C23 C24 0.5(6) . . . . ?
C21 C22 C23 C24 177.7(4) . . . . ?
C22 C23 C24 C25 -1.1(7) . . . . ?
C23 C24 C25 C26 -0.2(6) . . . . ?
C24 C25 C26 C27 2.1(6) . . . . ?
C24 C25 C26 C34 -176.8(4) . . . . ?
C25 C26 C27 C22 -2.6(6) . . . . ?
C34 C26 C27 C22 176.3(4) . . . . ?
C25 C26 C27 P2 178.4(3) . . . . ?
C34 C26 C27 P2 -2.7(5) . . . . ?
C23 C22 C27 C26 1.3(6) . . . . ?
C21 C22 C27 C26 -175.8(4) . . . . ?
C23 C22 C27 P2 -179.9(3) . . . . ?
C21 C22 C27 P2 3.0(6) . . . . ?
C40 P2 C27 C26 51.5(3) . . . . ?
C28 P2 C27 C26 -47.8(3) . . . . ?
Au2 P2 C27 C26 -176.6(2) . . . . ?
C40 P2 C27 C22 -127.3(4) . . . . ?
C28 P2 C27 C22 133.4(4) . . . . ?
Au2 P2 C27 C22 4.6(5) . . . . ?
C40 P2 C28 C33 -47.9(3) . . . . ?
C27 P2 C28 C33 50.1(3) . . . . ?
Au2 P2 C28 C33 -174.8(2) . . . . ?
C40 P2 C28 C29 133.1(4) . . . . ?
C27 P2 C28 C29 -129.0(4) . . . . ?
Au2 P2 C28 C29 6.2(4) . . . . ?
C33 C28 C29 C30 -1.3(6) . . . . ?
P2 C28 C29 C30 177.7(3) . . . . ?
C28 C29 C30 C31 0.8(6) . . . . ?
C29 C30 C31 C32 0.3(7) . . . . ?
C30 C31 C32 C33 -0.9(6) . . . . ?
C29 C28 C33 C32 0.6(6) . . . . ?
P2 C28 C33 C32 -178.5(3) . . . . ?
C29 C28 C33 C34 178.5(4) . . . . ?
P2 C28 C33 C34 -0.6(5) . . . . ?
C31 C32 C33 C28 0.5(6) . . . . ?
C31 C32 C33 C34 -177.2(4) . . . . ?
C28 C33 C34 C26 -58.6(5) . . . . ?
C32 C33 C34 C26 119.1(4) . . . . ?
C28 C33 C34 C35 58.0(5) . . . . ?
C32 C33 C34 C35 -124.3(4) . . . . ?
C25 C26 C34 C33 -120.3(4) . . . . ?
C27 C26 C34 C33 60.8(5) . . . . ?
C25 C26 C34 C35 121.8(4) . . . . ?
C27 C26 C34 C35 -57.0(5) . . . . ?
C33 C34 C35 C36 123.7(4) . . . . ?
C26 C34 C35 C36 -120.0(4) . . . . ?
C33 C34 C35 C40 -57.1(5) . . . . ?
C26 C34 C35 C40 59.2(5) . . . . ?
C40 C35 C36 C37 0.4(6) . . . . ?
C34 C35 C36 C37 179.6(4) . . . . ?
C35 C36 C37 C38 0.5(6) . . . . ?
C36 C37 C38 C39 -1.2(7) . . . . ?
C37 C38 C39 C40 0.9(7) . . . . ?
C38 C39 C40 C35 0.0(6) . . . . ?
C38 C39 C40 P2 -179.0(3) . . . . ?
C36 C35 C40 C39 -0.6(6) . . . . ?
C34 C35 C40 C39 -179.9(4) . . . . ?
C36 C35 C40 P2 178.5(3) . . . . ?
C34 C35 C40 P2 -0.8(5) . . . . ?
C28 P2 C40 C39 -132.4(4) . . . . ?
C27 P2 C40 C39 129.0(4) . . . . ?
Au2 P2 C40 C39 -7.4(4) . . . . ?
C28 P2 C40 C35 48.6(3) . . . . ?
C27 P2 C40 C35 -50.0(3) . . . . ?
Au2 P2 C40 C35 173.6(2) . . . . ?
C47A C42A C43A C44A 1(3) . . . . ?
C41A C42A C43A C44A -175.6(16) . . . . ?
C42A C43A C44A C45A -2(3) . . . . ?
C43A C44A C45A C46A 2(2) . . . . ?
C44A C45A C46A C47A -2(4) . . . . ?
C45A C46A C47A C42A 1(5) . . . . ?
C43A C42A C47A C46A -1(4) . . . . ?
C41A C42A C47A C46A 176(2) . . . . ?
C47B C42B C43B C44B -1(5) . . . . ?
C41B C42B C43B C44B -178(3) . . . . ?
C42B C43B C44B C45B 1(5) . . . . ?
C43B C44B C45B C46B 1(7) . . . . ?
C44B C45B C46B C47B -2(10) . . . . ?
C45B C46B C47B C42B 1(9) . . . . ?
C43B C42B C47B C46B 0(5) . . . . ?
C41B C42B C47B C46B 176(4) . . . . ?

_refine_diff_density_max         1.117
_refine_diff_density_min         -1.910
_refine_diff_density_rms         0.106



# start Validation Reply Form
_vrf_PLAT911_nt0800_LHG195A      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.598         58 Report
RESPONSE:  These reflections are missing in the highest and lowest 
resolution shells because of the instrument geometry limitations.
;
_vrf_PLAT972_nt0800_LHG195A      
;
PROBLEM: Check Calcd Resid. Dens.  0.81A   From Au1            -2.08 eA-3  
RESPONSE: Truncation peak near Au.
;
####################################################################### 
# 
# 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_nt0815_LHG203D
_database_code_depnum_ccdc_archive 'CCDC 2061861'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
;
(acetylacetonato)-carbonylrhodium-ortho-chloro-9-phosphatriptycene 
complex
;
_chemical_name_common            
'Rh(acac)CO(o-chloro-9-phosphatriptycene complex)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H19 Cl O3 P Rh'
_chemical_formula_sum            'C25 H19 Cl O3 P Rh'
_chemical_formula_weight         536.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Rh Rh 0.0927 3.6045 '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                   8.62702(10)
_cell_length_b                   21.4229(2)
_cell_length_c                   12.62171(15)
_cell_angle_alpha                90
_cell_angle_beta                 107.1655(13)
_cell_angle_gamma                90
_cell_volume                     2228.78(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    7474
_cell_measurement_theta_min      4.1000
_cell_measurement_theta_max      66.9250

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_F_000             1080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    8.182
_shelx_estimated_absorpt_T_min   0.157
_shelx_estimated_absorpt_T_max   0.354
_exptl_absorpt_correction_T_min  0.230
_exptl_absorpt_correction_T_max  0.416
_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            11623
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.127
_diffrn_reflns_theta_max         67.027
_diffrn_reflns_theta_full        67.027
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             3948
_reflns_number_gt                3716
_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    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0315P)²+1.3985P] 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         3948
_refine_ls_number_parameters     292
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0736
_refine_ls_wR_factor_gt          0.0723
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_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
Rh1 Rh 0.37704(3) 0.70574(2) 0.65113(2) 0.04533(9) Uani 1 1 d . . . . .
Cl1 Cl 0.74794(13) 0.72642(5) 0.61671(9) 0.0734(4) Uani 0.912(3) 1 d . . P A 1
Cl2 Cl 0.3720(12) 0.6878(6) 0.9033(9) 0.070(4) Uani 0.088(3) 1 d . . P A 2
P1 P 0.52054(7) 0.62009(3) 0.71410(5) 0.03571(15) Uani 1 1 d . . . . .
O1 O 0.5825(7) 0.77240(16) 0.8440(3) 0.153(2) Uani 1 1 d . . . . .
O2 O 0.2375(3) 0.78550(10) 0.6059(2) 0.0629(6) Uani 1 1 d . . . . .
O3 O 0.2443(3) 0.66532(10) 0.50680(18) 0.0576(5) Uani 1 1 d . . . . .
C1 C 0.4564(3) 0.54213(12) 0.6590(2) 0.0379(5) Uani 1 1 d . . . . .
C2 C 0.3171(3) 0.52885(14) 0.5735(2) 0.0465(6) Uani 1 1 d . . . . .
H2 H 0.248861 0.560923 0.537777 0.056 Uiso 1 1 calc R U . . .
C3 C 0.2804(4) 0.46725(16) 0.5418(3) 0.0593(8) Uani 1 1 d . . . . .
H3 H 0.186314 0.458081 0.485222 0.071 Uiso 1 1 calc R U . . .
C4 C 0.3810(5) 0.41999(15) 0.5928(3) 0.0608(8) Uani 1 1 d . . . . .
H4 H 0.355926 0.378995 0.569902 0.073 Uiso 1 1 calc R U . . .
C5 C 0.5209(4) 0.43269(14) 0.6789(3) 0.0521(7) Uani 1 1 d . . . . .
H5 H 0.588422 0.400301 0.713988 0.063 Uiso 1 1 calc R U . . .
C6 C 0.5588(3) 0.49377(13) 0.7119(2) 0.0398(6) Uani 1 1 d . . . . .
C7 C 0.7073(3) 0.51202(13) 0.8053(2) 0.0427(6) Uani 1 1 d . . . . .
H7 H 0.771074 0.474968 0.836528 0.051 Uiso 1 1 calc R U . . .
C8 C 0.6543(3) 0.54643(13) 0.8944(2) 0.0396(6) Uani 1 1 d . . . . .
C9 C 0.6981(4) 0.52795(15) 1.0045(2) 0.0492(7) Uani 1 1 d . . . . .
H9 H 0.762266 0.492701 1.027090 0.059 Uiso 1 1 calc R U . . .
C10 C 0.6461(4) 0.56206(17) 1.0810(3) 0.0572(8) Uani 1 1 d . . . . .
H10 H 0.678312 0.550306 1.155232 0.069 Uiso 1 1 calc R U . . .
C11 C 0.5478(4) 0.61286(17) 1.0479(3) 0.0576(8) Uani 1 1 d . . . . .
H11 H 0.510689 0.634691 1.099333 0.069 Uiso 1 1 calc R U . . .
C12 C 0.5030(4) 0.63210(14) 0.9375(3) 0.0483(7) Uani 1 1 d . . . . .
H12 H 0.435970 0.666620 0.915154 0.058 Uiso 0.912(3) 1 calc R U P A 1
C13 C 0.5589(3) 0.59956(12) 0.8613(2) 0.0372(5) Uani 1 1 d . . . . .
C14 C 0.7339(3) 0.61304(14) 0.7145(2) 0.0412(6) Uani 1 1 d . . . . .
C15 C 0.8253(4) 0.65598(16) 0.6763(2) 0.0517(7) Uani 1 1 d . . . . .
H15 H 0.778087 0.693209 0.644702 0.062 Uiso 0.088(3) 1 calc R U P A 2
C16 C 0.9866(4) 0.6438(2) 0.6847(3) 0.0700(11) Uani 1 1 d . . . . .
H16 H 1.047745 0.673318 0.660647 0.084 Uiso 1 1 calc R U . . .
C17 C 1.0558(4) 0.5885(2) 0.7284(3) 0.0730(11) Uani 1 1 d . . . . .
H17 H 1.163573 0.580563 0.733164 0.088 Uiso 1 1 calc R U . . .
C18 C 0.9678(4) 0.54450(19) 0.7655(3) 0.0604(9) Uani 1 1 d . . . . .
H18 H 1.015146 0.506708 0.794005 0.072 Uiso 1 1 calc R U . . .
C19 C 0.8080(3) 0.55698(14) 0.7601(2) 0.0436(6) Uani 1 1 d . . . . .
C20 C 0.5012(6) 0.74557(16) 0.7724(4) 0.0836(13) Uani 1 1 d . . . . .
C21 C 0.0282(6) 0.8526(2) 0.5139(4) 0.0866(13) Uani 1 1 d . . . . .
H21A H -0.053145 0.855736 0.443301 0.130 Uiso 1 1 calc R U . . .
H21B H 0.104363 0.886241 0.521607 0.130 Uiso 1 1 calc R U . . .
H21C H -0.022288 0.855028 0.572078 0.130 Uiso 1 1 calc R U . . .
C22 C 0.1154(4) 0.79146(16) 0.5211(3) 0.0602(9) Uani 1 1 d . . . . .
C23 C 0.0597(5) 0.74806(18) 0.4392(3) 0.0665(9) Uani 1 1 d . . . . .
H23 H -0.030855 0.759113 0.381215 0.080 Uiso 1 1 calc R U . . .
C24 C 0.1243(4) 0.68912(18) 0.4338(3) 0.0616(8) Uani 1 1 d . . . . .
C25 C 0.0497(7) 0.6481(3) 0.3351(4) 0.1082(19) Uani 1 1 d . . . . .
H25A H -0.025493 0.672110 0.278493 0.162 Uiso 1 1 calc R U . . .
H25B H -0.006378 0.614076 0.356970 0.162 Uiso 1 1 calc R U . . .
H25C H 0.133501 0.632017 0.306736 0.162 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
Rh1 C20 1.803(4) . ?
Rh1 O3 2.037(2) . ?
Rh1 O2 2.071(2) . ?
Rh1 P1 2.2248(7) . ?
Cl1 C15 1.730(4) . ?
Cl2 C12 1.612(11) . ?
P1 C1 1.831(3) . ?
P1 C13 1.842(3) . ?
P1 C14 1.845(3) . ?
O1 C20 1.124(5) . ?
O2 C22 1.268(4) . ?
O3 C24 1.272(4) . ?
C1 C2 1.387(4) . ?
C1 C6 1.397(4) . ?
C2 C3 1.388(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.365(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.514(4) . ?
C7 C19 1.517(4) . ?
C7 C8 1.524(4) . ?
C7 H7 0.9800 . ?
C8 C9 1.386(4) . ?
C8 C13 1.394(4) . ?
C9 C10 1.386(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.367(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.394(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.385(4) . ?
C12 H12 0.9300 . ?
C14 C15 1.388(4) . ?
C14 C19 1.402(4) . ?
C15 C16 1.389(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.367(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.386(4) . ?
C18 H18 0.9300 . ?
C21 C22 1.500(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.367(5) . ?
C23 C24 1.390(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.505(6) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 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
C20 Rh1 O3 175.48(17) . . ?
C20 Rh1 O2 89.69(14) . . ?
O3 Rh1 O2 88.67(9) . . ?
C20 Rh1 P1 87.62(12) . . ?
O3 Rh1 P1 94.34(6) . . ?
O2 Rh1 P1 174.71(7) . . ?
C1 P1 C13 96.30(12) . . ?
C1 P1 C14 96.66(12) . . ?
C13 P1 C14 95.47(12) . . ?
C1 P1 Rh1 122.86(9) . . ?
C13 P1 Rh1 118.21(9) . . ?
C14 P1 Rh1 121.19(10) . . ?
C22 O2 Rh1 125.9(2) . . ?
C24 O3 Rh1 126.9(2) . . ?
C2 C1 C6 120.0(3) . . ?
C2 C1 P1 125.3(2) . . ?
C6 C1 P1 114.64(19) . . ?
C1 C2 C3 119.4(3) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
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 119.8(3) . . ?
C5 C6 C7 123.3(3) . . ?
C1 C6 C7 116.8(2) . . ?
C6 C7 C19 108.6(2) . . ?
C6 C7 C8 109.3(2) . . ?
C19 C7 C8 107.5(2) . . ?
C6 C7 H7 110.5 . . ?
C19 C7 H7 110.5 . . ?
C8 C7 H7 110.5 . . ?
C9 C8 C13 119.7(3) . . ?
C9 C8 C7 123.3(3) . . ?
C13 C8 C7 116.9(2) . . ?
C8 C9 C10 119.9(3) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 120.4(3) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 120.3(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 119.7(3) . . ?
C13 C12 Cl2 123.2(4) . . ?
C11 C12 Cl2 116.9(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C8 119.9(3) . . ?
C12 C13 P1 125.8(2) . . ?
C8 C13 P1 114.32(19) . . ?
C15 C14 C19 118.3(3) . . ?
C15 C14 P1 127.8(2) . . ?
C19 C14 P1 113.9(2) . . ?
C14 C15 C16 120.5(3) . . ?
C14 C15 Cl1 122.9(2) . . ?
C16 C15 Cl1 116.5(3) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 120.1(3) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.8(3) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C19 119.4(4) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C18 C19 C14 120.8(3) . . ?
C18 C19 C7 122.0(3) . . ?
C14 C19 C7 117.1(2) . . ?
O1 C20 Rh1 175.8(5) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O2 C22 C23 126.1(3) . . ?
O2 C22 C21 114.6(3) . . ?
C23 C22 C21 119.3(3) . . ?
C22 C23 C24 126.7(3) . . ?
C22 C23 H23 116.6 . . ?
C24 C23 H23 116.6 . . ?
O3 C24 C23 125.5(3) . . ?
O3 C24 C25 115.1(3) . . ?
C23 C24 C25 119.4(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 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
C13 P1 C1 C2 130.7(2) . . . . ?
C14 P1 C1 C2 -133.0(2) . . . . ?
Rh1 P1 C1 C2 1.1(3) . . . . ?
C13 P1 C1 C6 -47.9(2) . . . . ?
C14 P1 C1 C6 48.4(2) . . . . ?
Rh1 P1 C1 C6 -177.53(16) . . . . ?
C6 C1 C2 C3 0.3(4) . . . . ?
P1 C1 C2 C3 -178.2(2) . . . . ?
C1 C2 C3 C4 -0.9(5) . . . . ?
C2 C3 C4 C5 1.1(5) . . . . ?
C3 C4 C5 C6 -0.7(5) . . . . ?
C4 C5 C6 C1 0.2(4) . . . . ?
C4 C5 C6 C7 179.4(3) . . . . ?
C2 C1 C6 C5 0.0(4) . . . . ?
P1 C1 C6 C5 178.7(2) . . . . ?
C2 C1 C6 C7 -179.3(2) . . . . ?
P1 C1 C6 C7 -0.6(3) . . . . ?
C5 C6 C7 C19 122.3(3) . . . . ?
C1 C6 C7 C19 -58.4(3) . . . . ?
C5 C6 C7 C8 -120.7(3) . . . . ?
C1 C6 C7 C8 58.5(3) . . . . ?
C6 C7 C8 C9 124.2(3) . . . . ?
C19 C7 C8 C9 -118.2(3) . . . . ?
C6 C7 C8 C13 -56.8(3) . . . . ?
C19 C7 C8 C13 60.8(3) . . . . ?
C13 C8 C9 C10 0.4(4) . . . . ?
C7 C8 C9 C10 179.4(3) . . . . ?
C8 C9 C10 C11 1.9(5) . . . . ?
C9 C10 C11 C12 -2.1(5) . . . . ?
C10 C11 C12 C13 -0.1(5) . . . . ?
C10 C11 C12 Cl2 173.7(5) . . . . ?
C11 C12 C13 C8 2.5(4) . . . . ?
Cl2 C12 C13 C8 -170.9(5) . . . . ?
C11 C12 C13 P1 -177.0(2) . . . . ?
Cl2 C12 C13 P1 9.6(6) . . . . ?
C9 C8 C13 C12 -2.6(4) . . . . ?
C7 C8 C13 C12 178.3(2) . . . . ?
C9 C8 C13 P1 176.9(2) . . . . ?
C7 C8 C13 P1 -2.1(3) . . . . ?
C1 P1 C13 C12 -131.2(2) . . . . ?
C14 P1 C13 C12 131.5(3) . . . . ?
Rh1 P1 C13 C12 1.5(3) . . . . ?
C1 P1 C13 C8 49.3(2) . . . . ?
C14 P1 C13 C8 -48.0(2) . . . . ?
Rh1 P1 C13 C8 -177.95(16) . . . . ?
C1 P1 C14 C15 133.5(3) . . . . ?
C13 P1 C14 C15 -129.4(3) . . . . ?
Rh1 P1 C14 C15 -1.6(3) . . . . ?
C1 P1 C14 C19 -46.7(2) . . . . ?
C13 P1 C14 C19 50.3(2) . . . . ?
Rh1 P1 C14 C19 178.12(16) . . . . ?
C19 C14 C15 C16 -1.0(4) . . . . ?
P1 C14 C15 C16 178.7(2) . . . . ?
C19 C14 C15 Cl1 179.1(2) . . . . ?
P1 C14 C15 Cl1 -1.1(4) . . . . ?
C14 C15 C16 C17 1.7(5) . . . . ?
Cl1 C15 C16 C17 -178.5(3) . . . . ?
C15 C16 C17 C18 -0.6(5) . . . . ?
C16 C17 C18 C19 -1.1(5) . . . . ?
C17 C18 C19 C14 1.8(5) . . . . ?
C17 C18 C19 C7 -176.6(3) . . . . ?
C15 C14 C19 C18 -0.7(4) . . . . ?
P1 C14 C19 C18 179.5(2) . . . . ?
C15 C14 C19 C7 177.7(2) . . . . ?
P1 C14 C19 C7 -2.1(3) . . . . ?
C6 C7 C19 C18 -121.6(3) . . . . ?
C8 C7 C19 C18 120.3(3) . . . . ?
C6 C7 C19 C14 60.0(3) . . . . ?
C8 C7 C19 C14 -58.1(3) . . . . ?
Rh1 O2 C22 C23 -5.0(6) . . . . ?
Rh1 O2 C22 C21 174.9(3) . . . . ?
O2 C22 C23 C24 0.8(7) . . . . ?
C21 C22 C23 C24 -179.1(4) . . . . ?
Rh1 O3 C24 C23 -0.3(6) . . . . ?
Rh1 O3 C24 C25 179.9(3) . . . . ?
C22 C23 C24 O3 2.2(7) . . . . ?
C22 C23 C24 C25 -178.1(5) . . . . ?

_refine_diff_density_max         0.521
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.053



# start Validation Reply Form
_vrf_PLAT242_nt0815_LHG203D      
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C24 Check 
RESPONSE: Wobbling neighboring fragment.
;
_vrf_PLAT911_nt0815_LHG203D      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.597         32 Report
RESPONSE: These reflections are missing in the lowest and highest resolution 
shells because of instrucment 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_nt0758_DAMA105C
_database_code_depnum_ccdc_archive 'CCDC 2061851'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
(5s,10s)-1,4-dimethyl-10H-5,10-[1,2]benzenoacridophosphine
_chemical_name_common            
(5s,10s)-1,4-dimethyl-10H-5,10-[1,2]benzenoacridophosphine
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H17 P'
_chemical_formula_sum            'C21 H17 P'
_chemical_formula_weight         300.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   8.6630(4)
_cell_length_b                   8.8328(4)
_cell_length_c                   20.9003(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.024(4)
_cell_angle_gamma                90
_cell_volume                     1583.62(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4485
_cell_measurement_theta_min      2.3360
_cell_measurement_theta_max      32.4480

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_F_000             632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.660
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.370
_exptl_absorpt_coefficient_mu    0.167
_shelx_estimated_absorpt_T_min   0.898
_shelx_estimated_absorpt_T_max   0.941
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Oxford Diffraction Xcalibur, Ruby, Gemini Ultra
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1856
_diffrn_reflns_number            10088
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.507
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4830
_reflns_number_gt                3752
_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    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0569P)²+0.3057P] 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         4830
_refine_ls_number_parameters     220
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1274
_refine_ls_wR_factor_gt          0.1166
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1A P 0.56707(6) 0.83067(6) 0.40339(3) 0.03800(16) Uani 0.899(2) 1 d . U P A 1
C7A C 0.3958(2) 0.6070(3) 0.32176(10) 0.0380(4) Uani 0.899(2) 1 d . U P A 1
H7A H 0.336923 0.531708 0.293856 0.046 Uiso 0.899(2) 1 calc R U P A 1
P1B P 0.3459(8) 0.5791(8) 0.3014(3) 0.060(2) Uani 0.101(2) 1 d . U P A 2
C7B C 0.523(3) 0.796(3) 0.3900(11) 0.050(4) Uani 0.101(2) 1 d . U P A 2
H7B H 0.579610 0.872569 0.418019 0.060 Uiso 0.101(2) 1 calc R U P A 2
C1 C 0.35336(15) 0.81950(15) 0.39348(6) 0.0387(3) Uani 1 1 d . U . . .
C2 C 0.2629(2) 0.91591(19) 0.42541(7) 0.0520(4) Uani 1 1 d . . . . .
H2 H 0.309701 0.992104 0.452093 0.062 Uiso 1 1 calc R U . . .
C3 C 0.1021(2) 0.8976(2) 0.41716(9) 0.0654(5) Uani 1 1 d . . . . .
H3 H 0.040816 0.961966 0.438247 0.079 Uiso 1 1 calc R U . . .
C4 C 0.03360(19) 0.7850(3) 0.37810(9) 0.0661(5) Uani 1 1 d . . . . .
H4 H -0.074080 0.773097 0.373137 0.079 Uiso 1 1 calc R U . . .
C5 C 0.12283(17) 0.6880(2) 0.34570(7) 0.0526(4) Uani 1 1 d . . . . .
H5 H 0.075401 0.611690 0.319264 0.063 Uiso 1 1 calc R U . . .
C6 C 0.28309(15) 0.70642(16) 0.35328(6) 0.0391(3) Uani 1 1 d . . . . .
C8 C 0.48889(15) 0.70647(17) 0.28157(6) 0.0400(3) Uani 1 1 d . . . . .
C9 C 0.49436(18) 0.6892(2) 0.21622(7) 0.0523(4) Uani 1 1 d . . . . .
H9 H 0.436978 0.613185 0.193085 0.063 Uiso 1 1 calc R U . . .
C10 C 0.5865(2) 0.7866(3) 0.18530(8) 0.0672(6) Uani 1 1 d . . . . .
H10 H 0.590170 0.775431 0.141291 0.081 Uiso 1 1 calc R U . . .
C11 C 0.6719(2) 0.8988(3) 0.21910(9) 0.0684(6) Uani 1 1 d . . . . .
H11 H 0.732621 0.963428 0.197870 0.082 Uiso 1 1 calc R U . . .
C12 C 0.66794(17) 0.9162(2) 0.28482(8) 0.0546(4) Uani 1 1 d . . . . .
H12 H 0.726167 0.991979 0.307763 0.066 Uiso 1 1 calc R U . . .
C13 C 0.57628(15) 0.81949(16) 0.31615(7) 0.0403(3) Uani 1 1 d . U . . .
C14 C 0.59553(14) 0.62512(15) 0.41678(6) 0.0362(3) Uani 1 1 d . U . . .
C15 C 0.70224(15) 0.56753(17) 0.46722(6) 0.0404(3) Uani 1 1 d . . . . .
C16 C 0.80134(19) 0.6664(2) 0.51552(8) 0.0565(4) Uani 1 1 d . . . . .
H16A H 0.878102 0.605279 0.541173 0.085 Uiso 1 1 calc R U . . .
H16B H 0.736448 0.714830 0.543091 0.085 Uiso 1 1 calc R U . . .
H16C H 0.852519 0.741971 0.493017 0.085 Uiso 1 1 calc R U . . .
C17 C 0.71408(16) 0.41086(18) 0.47284(6) 0.0460(3) Uani 1 1 d . . . . .
H17 H 0.783600 0.369570 0.506215 0.055 Uiso 1 1 calc R U . . .
C18 C 0.62607(18) 0.31548(17) 0.43052(7) 0.0463(3) Uani 1 1 d . . . . .
H18 H 0.637730 0.211394 0.435906 0.056 Uiso 1 1 calc R U . . .
C19 C 0.51957(16) 0.37081(16) 0.37964(6) 0.0393(3) Uani 1 1 d . . . . .
C20 C 0.4288(2) 0.2626(2) 0.33338(8) 0.0600(4) Uani 1 1 d . . . . .
H20A H 0.459618 0.274342 0.291293 0.090 Uiso 1 1 calc R U . . .
H20B H 0.319418 0.283549 0.331137 0.090 Uiso 1 1 calc R U . . .
H20C H 0.449251 0.160681 0.348144 0.090 Uiso 1 1 calc R U . . .
C21 C 0.50522(14) 0.52768(15) 0.37377(6) 0.0351(3) 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
P1A C1 1.8366(14) . ?
P1A C13 1.8388(15) . ?
P1A C14 1.8483(15) . ?
C7A C21 1.511(2) . ?
C7A C8 1.522(3) . ?
C7A C6 1.529(3) . ?
C7A H7A 0.9800 . ?
P1B C6 1.704(7) . ?
P1B C8 1.764(7) . ?
P1B C21 1.954(7) . ?
C7B C1 1.50(2) . ?
C7B C13 1.68(2) . ?
C7B C14 1.70(2) . ?
C7B H7B 0.9800 . ?
C1 C2 1.389(2) . ?
C1 C6 1.3898(19) . ?
C2 C3 1.390(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.368(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.3848(19) . ?
C5 H5 0.9300 . ?
C8 C9 1.3816(19) . ?
C8 C13 1.393(2) . ?
C9 C10 1.392(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.372(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.391(2) . ?
C12 H12 0.9300 . ?
C14 C15 1.3974(18) . ?
C14 C21 1.4017(18) . ?
C15 C17 1.391(2) . ?
C15 C16 1.509(2) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.373(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.395(2) . ?
C18 H18 0.9300 . ?
C19 C21 1.3950(19) . ?
C19 C20 1.502(2) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 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
C1 P1A C13 93.89(6) . . ?
C1 P1A C14 94.32(6) . . ?
C13 P1A C14 94.25(6) . . ?
C21 C7A C8 109.72(14) . . ?
C21 C7A C6 109.31(14) . . ?
C8 C7A C6 109.02(16) . . ?
C21 C7A H7A 109.6 . . ?
C8 C7A H7A 109.6 . . ?
C6 C7A H7A 109.6 . . ?
C6 P1B C8 91.5(3) . . ?
C6 P1B C21 85.1(3) . . ?
C8 P1B C21 83.5(3) . . ?
C1 C7B C13 115.1(14) . . ?
C1 C7B C14 115.3(15) . . ?
C13 C7B C14 106.1(12) . . ?
C1 C7B H7B 106.6 . . ?
C13 C7B H7B 106.6 . . ?
C14 C7B H7B 106.6 . . ?
C2 C1 C6 120.15(13) . . ?
C2 C1 C7B 137.1(9) . . ?
C6 C1 C7B 102.8(9) . . ?
C2 C1 P1A 122.68(12) . . ?
C6 C1 P1A 117.15(10) . . ?
C1 C2 C3 119.46(16) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 120.17(16) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.91(15) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 119.22(16) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C1 120.08(14) . . ?
C5 C6 C7A 125.01(15) . . ?
C1 C6 C7A 114.89(13) . . ?
C5 C6 P1B 104.7(3) . . ?
C1 C6 P1B 135.0(3) . . ?
C9 C8 C13 120.06(14) . . ?
C9 C8 C7A 125.17(15) . . ?
C13 C8 C7A 114.75(13) . . ?
C9 C8 P1B 106.5(3) . . ?
C13 C8 P1B 133.1(3) . . ?
C8 C9 C10 119.46(17) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 120.66(15) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 120.25(15) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 119.52(17) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C8 120.04(14) . . ?
C12 C13 C7B 139.0(9) . . ?
C8 C13 C7B 100.9(9) . . ?
C12 C13 P1A 122.72(12) . . ?
C8 C13 P1A 117.22(10) . . ?
C15 C14 C21 120.77(13) . . ?
C15 C14 C7B 138.3(8) . . ?
C21 C14 C7B 100.8(8) . . ?
C15 C14 P1A 122.14(11) . . ?
C21 C14 P1A 117.09(10) . . ?
C17 C15 C14 117.32(13) . . ?
C17 C15 C16 119.39(13) . . ?
C14 C15 C16 123.28(14) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C15 121.88(12) . . ?
C18 C17 H17 119.1 . . ?
C15 C17 H17 119.1 . . ?
C17 C18 C19 121.65(13) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C21 C19 C18 117.14(13) . . ?
C21 C19 C20 122.92(13) . . ?
C18 C19 C20 119.93(14) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 C14 121.24(12) . . ?
C19 C21 C7A 124.29(14) . . ?
C14 C21 C7A 114.47(13) . . ?
C19 C21 P1B 110.1(2) . . ?
C14 C21 P1B 128.6(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
C13 C7B C1 C2 -119.0(12) . . . . ?
C14 C7B C1 C2 117.1(13) . . . . ?
C13 C7B C1 C6 62.6(15) . . . . ?
C14 C7B C1 C6 -61.3(14) . . . . ?
C13 P1A C1 C2 -133.50(12) . . . . ?
C14 P1A C1 C2 131.94(12) . . . . ?
C13 P1A C1 C6 48.08(11) . . . . ?
C14 P1A C1 C6 -46.48(11) . . . . ?
C6 C1 C2 C3 0.5(2) . . . . ?
C7B C1 C2 C3 -177.7(13) . . . . ?
P1A C1 C2 C3 -177.91(11) . . . . ?
C1 C2 C3 C4 0.3(2) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
C3 C4 C5 C6 -0.1(2) . . . . ?
C4 C5 C6 C1 0.8(2) . . . . ?
C4 C5 C6 C7A 178.87(16) . . . . ?
C4 C5 C6 P1B -175.0(3) . . . . ?
C2 C1 C6 C5 -1.0(2) . . . . ?
C7B C1 C6 C5 177.7(9) . . . . ?
P1A C1 C6 C5 177.46(10) . . . . ?
C2 C1 C6 C7A -179.26(14) . . . . ?
P1A C1 C6 C7A -0.80(17) . . . . ?
C2 C1 C6 P1B 173.2(3) . . . . ?
C7B C1 C6 P1B -8.1(10) . . . . ?
C21 C7A C6 C5 -117.43(16) . . . . ?
C8 C7A C6 C5 122.64(15) . . . . ?
C21 C7A C6 C1 60.74(18) . . . . ?
C8 C7A C6 C1 -59.19(18) . . . . ?
C8 P1B C6 C5 142.5(2) . . . . ?
C21 P1B C6 C5 -134.16(19) . . . . ?
C8 P1B C6 C1 -32.3(5) . . . . ?
C21 P1B C6 C1 51.1(4) . . . . ?
C21 C7A C8 C9 117.97(16) . . . . ?
C6 C7A C8 C9 -122.35(15) . . . . ?
C21 C7A C8 C13 -60.35(19) . . . . ?
C6 C7A C8 C13 59.33(18) . . . . ?
C6 P1B C8 C9 -141.8(2) . . . . ?
C21 P1B C8 C9 133.35(17) . . . . ?
C6 P1B C8 C13 31.4(5) . . . . ?
C21 P1B C8 C13 -53.4(4) . . . . ?
C13 C8 C9 C10 -0.7(2) . . . . ?
C7A C8 C9 C10 -178.90(16) . . . . ?
P1B C8 C9 C10 173.6(3) . . . . ?
C8 C9 C10 C11 0.2(2) . . . . ?
C9 C10 C11 C12 0.3(3) . . . . ?
C10 C11 C12 C13 -0.3(2) . . . . ?
C11 C12 C13 C8 -0.2(2) . . . . ?
C11 C12 C13 C7B -176.0(12) . . . . ?
C11 C12 C13 P1A 178.50(12) . . . . ?
C9 C8 C13 C12 0.7(2) . . . . ?
C7A C8 C13 C12 179.08(14) . . . . ?
P1B C8 C13 C12 -171.8(3) . . . . ?
C9 C8 C13 C7B 177.9(8) . . . . ?
P1B C8 C13 C7B 5.4(8) . . . . ?
C9 C8 C13 P1A -178.10(10) . . . . ?
C7A C8 C13 P1A 0.31(17) . . . . ?
C1 C7B C13 C12 114.6(14) . . . . ?
C14 C7B C13 C12 -116.7(11) . . . . ?
C1 C7B C13 C8 -61.7(15) . . . . ?
C14 C7B C13 C8 67.0(12) . . . . ?
C1 P1A C13 C12 133.34(12) . . . . ?
C14 P1A C13 C12 -132.03(12) . . . . ?
C1 P1A C13 C8 -47.93(11) . . . . ?
C14 P1A C13 C8 46.71(11) . . . . ?
C1 C7B C14 C15 -114.1(14) . . . . ?
C13 C7B C14 C15 117.3(10) . . . . ?
C1 C7B C14 C21 61.3(14) . . . . ?
C13 C7B C14 C21 -67.3(12) . . . . ?
C1 P1A C14 C15 -132.99(11) . . . . ?
C13 P1A C14 C15 132.78(11) . . . . ?
C1 P1A C14 C21 47.19(10) . . . . ?
C13 P1A C14 C21 -47.04(10) . . . . ?
C21 C14 C15 C17 -0.24(18) . . . . ?
C7B C14 C15 C17 174.5(12) . . . . ?
P1A C14 C15 C17 179.95(10) . . . . ?
C21 C14 C15 C16 -179.26(12) . . . . ?
C7B C14 C15 C16 -4.5(12) . . . . ?
P1A C14 C15 C16 0.93(18) . . . . ?
C14 C15 C17 C18 0.5(2) . . . . ?
C16 C15 C17 C18 179.59(13) . . . . ?
C15 C17 C18 C19 -0.2(2) . . . . ?
C17 C18 C19 C21 -0.5(2) . . . . ?
C17 C18 C19 C20 178.34(14) . . . . ?
C18 C19 C21 C14 0.76(18) . . . . ?
C20 C19 C21 C14 -178.02(13) . . . . ?
C18 C19 C21 C7A -179.93(14) . . . . ?
C20 C19 C21 C7A 1.3(2) . . . . ?
C18 C19 C21 P1B -178.2(2) . . . . ?
C20 C19 C21 P1B 3.0(3) . . . . ?
C15 C14 C21 C19 -0.41(18) . . . . ?
C7B C14 C21 C19 -176.8(8) . . . . ?
P1A C14 C21 C19 179.41(10) . . . . ?
C15 C14 C21 C7A -179.79(13) . . . . ?
P1A C14 C21 C7A 0.03(16) . . . . ?
C15 C14 C21 P1B 178.4(3) . . . . ?
C7B C14 C21 P1B 1.9(8) . . . . ?
C8 C7A C21 C19 -119.59(15) . . . . ?
C6 C7A C21 C19 120.90(15) . . . . ?
C8 C7A C21 C14 59.77(18) . . . . ?
C6 C7A C21 C14 -59.74(17) . . . . ?

_refine_diff_density_max         0.294
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.038




# start Validation Reply Form
_vrf_PLAT911_nt0758_DAMA105C     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         10 Report
RESPONSE: 4 reflections are missing because of overflow, the rest is missing 
in the lowest resolution shell because of the instrument geometry limitations.
;
_vrf_PLAT913_nt0758_DAMA105C     
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....          4 Note  
RESPONSE: These reflections are missing because of overflow.
;
####################################################################### 
# 
# 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_nt0818_LHG205A
_database_code_depnum_ccdc_archive 'CCDC 2061857'
loop_
_audit_author_name
_audit_author_address
'Nikolay Tumanov'
;Universite de Namur
Belgium
;
_audit_update_record             
;
2021-02-08 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        chloro(9-phosphotriptycene)gold(I)
_chemical_name_common            chloro(9-phosphotriptycene)gold(I)
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 Au Cl P'
_chemical_formula_sum            'C19 H13 Au Cl P'
_chemical_formula_weight         504.68

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'
Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   8.26532(9)
_cell_length_b                   14.28693(14)
_cell_length_c                   14.00053(14)
_cell_angle_alpha                90
_cell_angle_beta                 91.8231(9)
_cell_angle_gamma                90
_cell_volume                     1652.43(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    5149
_cell_measurement_theta_min      4.3960
_cell_measurement_theta_max      66.9840

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.058
_exptl_absorpt_coefficient_mu    19.060
_shelx_estimated_absorpt_T_min   0.055
_shelx_estimated_absorpt_T_max   0.404
_exptl_absorpt_correction_T_min  0.062
_exptl_absorpt_correction_T_max  0.495
_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            7819
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.423
_diffrn_reflns_theta_max         67.148
_diffrn_reflns_theta_full        67.148
_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             2934
_reflns_number_gt                2690
_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    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0438P)²] 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         2934
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_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
Au1 Au 0.21185(2) 0.57069(2) 0.56174(2) 0.05175(11) Uani 1 1 d . . . . .
Cl1 Cl 0.2261(2) 0.45761(11) 0.44634(10) 0.0740(4) Uani 1 1 d . . . . .
P1 P 0.20123(13) 0.67960(8) 0.67377(7) 0.0440(2) Uani 1 1 d . . . . .
C1 C 0.3896(5) 0.7266(3) 0.7214(3) 0.0445(9) Uani 1 1 d . . . . .
C2 C 0.5421(5) 0.6988(4) 0.6957(4) 0.0556(11) Uani 1 1 d . . . . .
H2 H 0.555410 0.651690 0.650743 0.067 Uiso 1 1 calc R U . . .
C3 C 0.6762(6) 0.7434(5) 0.7389(4) 0.0688(14) Uani 1 1 d . . . . .
H3 H 0.779945 0.726115 0.722031 0.083 Uiso 1 1 calc R U . . .
C4 C 0.6570(6) 0.8118(5) 0.8054(4) 0.0684(14) Uani 1 1 d . . . . .
H4 H 0.747698 0.840993 0.832770 0.082 Uiso 1 1 calc R U . . .
C5 C 0.5041(6) 0.8386(4) 0.8327(4) 0.0545(11) Uani 1 1 d . . . . .
H5 H 0.492058 0.884784 0.878801 0.065 Uiso 1 1 calc R U . . .
C6 C 0.3690(5) 0.7957(3) 0.7906(3) 0.0461(9) Uani 1 1 d . . . . .
C7 C 0.1948(5) 0.8200(3) 0.8159(3) 0.0474(9) Uani 1 1 d . . . . .
H7 H 0.192967 0.868603 0.865243 0.057 Uiso 1 1 calc R U . . .
C8 C 0.1054(5) 0.8521(3) 0.7246(3) 0.0491(10) Uani 1 1 d . . . . .
C9 C 0.0278(7) 0.9377(4) 0.7155(5) 0.0651(14) Uani 1 1 d . . . . .
H9 H 0.033062 0.980550 0.765489 0.078 Uiso 1 1 calc R U . . .
C10 C -0.0569(8) 0.9593(5) 0.6324(6) 0.0796(17) Uani 1 1 d . . . . .
H10 H -0.108380 1.017011 0.626550 0.095 Uiso 1 1 calc R U . . .
C11 C -0.0668(7) 0.8967(5) 0.5575(5) 0.0783(17) Uani 1 1 d . . . . .
H11 H -0.126457 0.911915 0.502206 0.094 Uiso 1 1 calc R U . . .
C12 C 0.0118(6) 0.8113(4) 0.5643(4) 0.0618(12) Uani 1 1 d . . . . .
H12 H 0.006892 0.769317 0.513538 0.074 Uiso 1 1 calc R U . . .
C13 C 0.0980(5) 0.7891(3) 0.6479(3) 0.0473(9) Uani 1 1 d . . . . .
C14 C 0.1065(5) 0.6553(3) 0.7856(3) 0.0465(9) Uani 1 1 d . . . . .
C15 C 0.0286(7) 0.5730(4) 0.8104(4) 0.0609(13) Uani 1 1 d . . . . .
H15 H 0.024470 0.522401 0.768521 0.073 Uiso 1 1 calc R U . . .
C16 C -0.0426(8) 0.5674(5) 0.8980(5) 0.0765(18) Uani 1 1 d . . . . .
H16 H -0.094857 0.512558 0.915168 0.092 Uiso 1 1 calc R U . . .
C17 C -0.0373(7) 0.6416(6) 0.9603(4) 0.0805(18) Uani 1 1 d . . . . .
H17 H -0.086698 0.636613 1.018833 0.097 Uiso 1 1 calc R U . . .
C18 C 0.0407(6) 0.7235(5) 0.9368(4) 0.0639(13) Uani 1 1 d . . . . .
H18 H 0.044624 0.773247 0.979638 0.077 Uiso 1 1 calc R U . . .
C19 C 0.1131(5) 0.7312(4) 0.8491(3) 0.0496(10) 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
Au1 P1 2.2131(11) . ?
Au1 Cl1 2.2905(12) . ?
P1 C1 1.804(4) . ?
P1 C14 1.807(5) . ?
P1 C13 1.813(5) . ?
C1 C2 1.381(6) . ?
C1 C6 1.397(6) . ?
C2 C3 1.399(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.362(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.533(6) . ?
C7 C19 1.518(7) . ?
C7 C8 1.527(6) . ?
C7 H7 0.9800 . ?
C8 C9 1.385(7) . ?
C8 C13 1.401(7) . ?
C9 C10 1.374(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.378(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.385(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(6) . ?
C12 H12 0.9300 . ?
C14 C15 1.390(7) . ?
C14 C19 1.402(7) . ?
C15 C16 1.380(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.372(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.380(10) . ?
C17 H17 0.9300 . ?
C18 C19 1.388(7) . ?
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
P1 Au1 Cl1 179.30(5) . . ?
C1 P1 C14 98.27(19) . . ?
C1 P1 C13 98.5(2) . . ?
C14 P1 C13 97.2(2) . . ?
C1 P1 Au1 118.07(15) . . ?
C14 P1 Au1 120.47(16) . . ?
C13 P1 Au1 119.61(15) . . ?
C2 C1 C6 121.1(4) . . ?
C2 C1 P1 125.5(4) . . ?
C6 C1 P1 113.4(3) . . ?
C1 C2 C3 118.2(5) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 120.9(5) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.9(5) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 119.2(5) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C1 119.5(4) . . ?
C5 C6 C7 123.4(4) . . ?
C1 C6 C7 117.1(4) . . ?
C19 C7 C8 107.4(3) . . ?
C19 C7 C6 108.2(4) . . ?
C8 C7 C6 107.9(4) . . ?
C19 C7 H7 111.1 . . ?
C8 C7 H7 111.1 . . ?
C6 C7 H7 111.1 . . ?
C9 C8 C13 119.2(5) . . ?
C9 C8 C7 123.6(5) . . ?
C13 C8 C7 117.2(4) . . ?
C10 C9 C8 119.9(6) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 121.0(6) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C12 120.2(6) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 119.1(6) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C8 120.5(4) . . ?
C12 C13 P1 126.3(4) . . ?
C8 C13 P1 113.1(3) . . ?
C15 C14 C19 120.3(4) . . ?
C15 C14 P1 126.6(4) . . ?
C19 C14 P1 113.0(3) . . ?
C16 C15 C14 119.0(5) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C17 C16 C15 121.0(5) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 120.6(5) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C17 C18 C19 119.7(6) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C18 C19 C14 119.4(5) . . ?
C18 C19 C7 123.1(5) . . ?
C14 C19 C7 117.5(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 129.5(4) . . . . ?
C13 P1 C1 C2 -131.9(4) . . . . ?
Au1 P1 C1 C2 -1.7(5) . . . . ?
C14 P1 C1 C6 -49.7(4) . . . . ?
C13 P1 C1 C6 48.9(4) . . . . ?
Au1 P1 C1 C6 179.1(3) . . . . ?
C6 C1 C2 C3 -1.6(7) . . . . ?
P1 C1 C2 C3 179.2(4) . . . . ?
C1 C2 C3 C4 0.6(8) . . . . ?
C2 C3 C4 C5 0.6(9) . . . . ?
C3 C4 C5 C6 -0.9(8) . . . . ?
C4 C5 C6 C1 -0.1(7) . . . . ?
C4 C5 C6 C7 179.8(5) . . . . ?
C2 C1 C6 C5 1.3(7) . . . . ?
P1 C1 C6 C5 -179.4(4) . . . . ?
C2 C1 C6 C7 -178.6(4) . . . . ?
P1 C1 C6 C7 0.7(5) . . . . ?
C5 C6 C7 C19 -122.5(5) . . . . ?
C1 C6 C7 C19 57.4(5) . . . . ?
C5 C6 C7 C8 121.5(5) . . . . ?
C1 C6 C7 C8 -58.6(5) . . . . ?
C19 C7 C8 C9 119.6(5) . . . . ?
C6 C7 C8 C9 -124.0(5) . . . . ?
C19 C7 C8 C13 -58.1(5) . . . . ?
C6 C7 C8 C13 58.3(5) . . . . ?
C13 C8 C9 C10 0.9(8) . . . . ?
C7 C8 C9 C10 -176.7(5) . . . . ?
C8 C9 C10 C11 0.3(10) . . . . ?
C9 C10 C11 C12 -1.3(10) . . . . ?
C10 C11 C12 C13 1.1(9) . . . . ?
C11 C12 C13 C8 0.1(8) . . . . ?
C11 C12 C13 P1 177.0(4) . . . . ?
C9 C8 C13 C12 -1.1(7) . . . . ?
C7 C8 C13 C12 176.7(4) . . . . ?
C9 C8 C13 P1 -178.4(4) . . . . ?
C7 C8 C13 P1 -0.6(5) . . . . ?
C1 P1 C13 C12 133.9(4) . . . . ?
C14 P1 C13 C12 -126.5(4) . . . . ?
Au1 P1 C13 C12 4.7(5) . . . . ?
C1 P1 C13 C8 -49.0(4) . . . . ?
C14 P1 C13 C8 50.5(4) . . . . ?
Au1 P1 C13 C8 -178.2(3) . . . . ?
C1 P1 C14 C15 -132.6(4) . . . . ?
C13 P1 C14 C15 127.6(4) . . . . ?
Au1 P1 C14 C15 -3.0(5) . . . . ?
C1 P1 C14 C19 49.2(3) . . . . ?
C13 P1 C14 C19 -50.5(3) . . . . ?
Au1 P1 C14 C19 178.8(3) . . . . ?
C19 C14 C15 C16 0.3(7) . . . . ?
P1 C14 C15 C16 -177.7(4) . . . . ?
C14 C15 C16 C17 0.0(9) . . . . ?
C15 C16 C17 C18 -0.5(10) . . . . ?
C16 C17 C18 C19 0.6(9) . . . . ?
C17 C18 C19 C14 -0.2(7) . . . . ?
C17 C18 C19 C7 177.2(5) . . . . ?
C15 C14 C19 C18 -0.2(7) . . . . ?
P1 C14 C19 C18 178.0(4) . . . . ?
C15 C14 C19 C7 -177.8(4) . . . . ?
P1 C14 C19 C7 0.4(5) . . . . ?
C8 C7 C19 C18 -119.2(5) . . . . ?
C6 C7 C19 C18 124.5(5) . . . . ?
C8 C7 C19 C14 58.3(5) . . . . ?
C6 C7 C19 C14 -58.0(5) . . . . ?

_refine_diff_density_max         1.637
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.154



# start Validation Reply Form
_vrf_PLAT911_nt0818_LHG205A      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.598         20 Report
RESPONSE: These reflections are missing in the highest resolution shell because 
of the instrument geometry limitations.
;
_vrf_PLAT971_nt0818_LHG205A      
;
PROBLEM: Check Calcd Resid. Dens.  1.73A   From Cl1             1.58 eA-3  
RESPONSE: Truncation error peak - gold atom in the structure.
;
