# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_mo_b22_pf309wh_0m_5
_database_code_depnum_ccdc_archive 'CCDC 2179785'
loop_
_audit_author_name
_audit_author_address
'Beatrice Cula'
;Humboldt Universitaet zu Berlin
Germany
;
_audit_update_record             
;
2022-06-17 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C100 H64 Al4 Cl8 O8 P4'
_chemical_formula_weight         1908.91

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'
Al Al 0.0645 0.0514 '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                   12.083(3)
_cell_length_b                   13.097(3)
_cell_length_c                   13.743(3)
_cell_angle_alpha                88.302(7)
_cell_angle_beta                 86.483(8)
_cell_angle_gamma                87.468(8)
_cell_volume                     2167.9(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.27
_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    0.435
_shelx_estimated_absorpt_T_min   0.835
_shelx_estimated_absorpt_T_max   0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.674425
_exptl_absorpt_correction_T_max  0.745687
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10812
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.123
_diffrn_reflns_theta_max         28.425
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             10812
_reflns_number_gt                8696
_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       'Bruker APEX4'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component twin.,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)+(0.0485P)²+1.5665P] 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         10812
_refine_ls_number_parameters     560
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.1148
_refine_ls_wR_factor_gt          0.1029
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
Cl1 Cl 0.40982(6) 0.83851(6) 0.64203(5) 0.03499(17) Uani 1 1 d . . . . .
Cl2 Cl 0.64178(6) 0.88410(5) 0.77155(5) 0.02825(15) Uani 1 1 d . . . . .
P1 P 0.43251(5) 0.49783(5) 0.73226(5) 0.01667(13) Uani 1 1 d . . . . .
Al1 Al 0.50228(6) 0.78984(6) 0.76262(6) 0.01916(16) Uani 1 1 d . . . . .
O1 O 0.55453(16) 0.66176(14) 0.74525(14) 0.0267(4) Uani 1 1 d . . . . .
O2 O 0.62424(19) 0.54582(17) 0.63964(18) 0.0435(6) Uani 1 1 d . . . . .
C1 C 0.4646(2) 0.3734(2) 0.68544(18) 0.0193(5) Uani 1 1 d . . . . .
C2 C 0.3961(2) 0.3279(2) 0.6228(2) 0.0244(6) Uani 1 1 d . . . . .
H2 H 0.328943 0.362123 0.605225 0.029 Uiso 1 1 calc R U . . .
C3 C 0.4266(2) 0.2320(2) 0.5863(2) 0.0276(6) Uani 1 1 d . . . . .
H3 H 0.380483 0.200926 0.543156 0.033 Uiso 1 1 calc R U . . .
C4 C 0.5243(2) 0.1816(2) 0.61262(19) 0.0252(6) Uani 1 1 d . . . . .
H4 H 0.545030 0.116486 0.586868 0.030 Uiso 1 1 calc R U . . .
C5 C 0.5917(2) 0.2258(2) 0.67644(19) 0.0225(5) Uani 1 1 d . . . . .
H5 H 0.657360 0.190297 0.695650 0.027 Uiso 1 1 calc R U . . .
C6 C 0.5629(2) 0.3223(2) 0.71221(18) 0.0203(5) Uani 1 1 d . . . . .
H6 H 0.609785 0.353416 0.754663 0.024 Uiso 1 1 calc R U . . .
C7 C 0.3985(2) 0.49136(19) 0.86057(17) 0.0174(5) Uani 1 1 d . . . . .
C8 C 0.3740(2) 0.3943(2) 0.90635(19) 0.0209(5) Uani 1 1 d . . . . .
H8 H 0.385986 0.333971 0.869747 0.025 Uiso 1 1 calc R U . . .
C9 C 0.3335(2) 0.3865(2) 1.0021(2) 0.0241(6) Uani 1 1 d . . . . .
H9 H 0.320868 0.320578 1.030163 0.029 Uiso 1 1 calc R U . . .
C10 C 0.3101(2) 0.47272(19) 1.05979(19) 0.0208(5) Uani 1 1 d . . . . .
H10 H 0.279825 0.467039 1.125086 0.025 Uiso 1 1 calc R U . . .
C11 C 0.3334(2) 0.5651(2) 1.01625(19) 0.0195(5) Uani 1 1 d . . . . .
C12 C 0.3806(2) 0.57538(19) 0.91865(18) 0.0169(5) Uani 1 1 d . . . . .
C13 C 0.3218(2) 0.55983(18) 0.66946(18) 0.0175(5) Uani 1 1 d . . . . .
C14 C 0.3382(2) 0.5777(2) 0.56892(19) 0.0222(5) Uani 1 1 d . . . . .
H14 H 0.407365 0.559094 0.536198 0.027 Uiso 1 1 calc R U . . .
C15 C 0.2529(2) 0.6227(2) 0.51713(19) 0.0225(5) Uani 1 1 d . . . . .
H15 H 0.263012 0.634098 0.448629 0.027 Uiso 1 1 calc R U . . .
C16 C 0.1528(2) 0.65111(19) 0.56592(19) 0.0219(5) Uani 1 1 d . . . . .
H16 H 0.094759 0.682457 0.530484 0.026 Uiso 1 1 calc R U . . .
C17 C 0.1365(2) 0.6343(2) 0.6656(2) 0.0232(5) Uani 1 1 d . . . . .
H17 H 0.067621 0.654216 0.698116 0.028 Uiso 1 1 calc R U . . .
C18 C 0.2210(2) 0.58818(19) 0.71828(19) 0.0202(5) Uani 1 1 d . . . . .
H18 H 0.210053 0.576179 0.786636 0.024 Uiso 1 1 calc R U . . .
C19 C 0.5559(2) 0.5777(2) 0.69974(19) 0.0211(5) Uani 1 1 d . . . . .
C20 C 0.4187(2) 0.78060(19) 0.88855(19) 0.0197(5) Uani 1 1 d . . . . .
C21 C 0.3841(2) 0.68992(19) 0.93076(18) 0.0165(5) Uani 1 1 d . . . . .
C22 C 0.3336(2) 0.67937(19) 1.02627(18) 0.0184(5) Uani 1 1 d . . . . .
C23 C 0.3079(2) 0.76170(19) 1.08367(19) 0.0202(5) Uani 1 1 d . . . . .
H23 H 0.270904 0.755339 1.146445 0.024 Uiso 1 1 calc R U . . .
C24 C 0.3402(2) 0.8566(2) 1.04292(19) 0.0212(5) Uani 1 1 d . . . . .
H24 H 0.324636 0.916693 1.079294 0.025 Uiso 1 1 calc R U . . .
C25 C 0.3942(2) 0.8647(2) 0.95102(19) 0.0206(5) Uani 1 1 d . . . . .
H25 H 0.416218 0.930451 0.928339 0.025 Uiso 1 1 calc R U . . .
Cl3 Cl 0.90563(7) 0.62121(7) 0.14288(5) 0.0437(2) Uani 1 1 d . . . . .
Cl4 Cl 1.15308(6) 0.59535(5) 0.26024(5) 0.03117(16) Uani 1 1 d . . . . .
P2 P 0.93600(5) 0.99251(5) 0.23158(5) 0.01686(13) Uani 1 1 d . . . . .
Al2 Al 1.00170(6) 0.68567(6) 0.24810(5) 0.01876(16) Uani 1 1 d . . . . .
O3 O 1.03387(17) 0.80911(14) 0.20103(15) 0.0287(4) Uani 1 1 d . . . . .
O4 O 1.15171(16) 0.93243(16) 0.22267(16) 0.0342(5) Uani 1 1 d . . . . .
C26 C 0.9708(2) 1.11620(19) 0.18387(17) 0.0185(5) Uani 1 1 d . . . . .
C27 C 1.0667(2) 1.1608(2) 0.21346(19) 0.0205(5) Uani 1 1 d . . . . .
H27 H 1.111569 1.126206 0.259467 0.025 Uiso 1 1 calc R U . . .
C28 C 1.0951(2) 1.2559(2) 0.17474(19) 0.0220(5) Uani 1 1 d . . . . .
H28 H 1.159812 1.286345 0.194319 0.026 Uiso 1 1 calc R U . . .
C29 C 1.0298(2) 1.3069(2) 0.10781(19) 0.0239(5) Uani 1 1 d . . . . .
H29 H 1.050274 1.371676 0.081314 0.029 Uiso 1 1 calc R U . . .
C30 C 0.9344(2) 1.2633(2) 0.0794(2) 0.0265(6) Uani 1 1 d . . . . .
H30 H 0.889782 1.298811 0.033739 0.032 Uiso 1 1 calc R U . . .
C31 C 0.9039(2) 1.1685(2) 0.11710(19) 0.0234(5) Uani 1 1 d . . . . .
H31 H 0.838293 1.139237 0.097908 0.028 Uiso 1 1 calc R U . . .
C32 C 0.8977(2) 0.99496(19) 0.35908(18) 0.0185(5) Uani 1 1 d . . . . .
C33 C 0.8855(2) 0.9069(2) 0.41551(18) 0.0174(5) Uani 1 1 d . . . . .
C34 C 0.8381(2) 0.91101(19) 0.51293(18) 0.0186(5) Uani 1 1 d . . . . .
C35 C 0.8047(2) 1.0007(2) 0.55622(19) 0.0217(5) Uani 1 1 d . . . . .
H35 H 0.771819 1.002273 0.620771 0.026 Uiso 1 1 calc R U . . .
C36 C 0.8218(2) 1.0908(2) 0.4995(2) 0.0235(5) Uani 1 1 d . . . . .
H36 H 0.802299 1.154983 0.527738 0.028 Uiso 1 1 calc R U . . .
C37 C 0.8661(2) 1.0891(2) 0.40434(19) 0.0208(5) Uani 1 1 d . . . . .
H37 H 0.875575 1.151606 0.368616 0.025 Uiso 1 1 calc R U . . .
C38 C 0.8256(2) 0.94393(19) 0.16806(19) 0.0198(5) Uani 1 1 d . . . . .
C39 C 0.7228(2) 0.9263(2) 0.21603(19) 0.0229(5) Uani 1 1 d . . . . .
H39 H 0.710096 0.940047 0.283377 0.028 Uiso 1 1 calc R U . . .
C40 C 0.6395(2) 0.8885(2) 0.1641(2) 0.0269(6) Uani 1 1 d . . . . .
H40 H 0.569459 0.875437 0.196282 0.032 Uiso 1 1 calc R U . . .
C41 C 0.6576(2) 0.8697(2) 0.0656(2) 0.0268(6) Uani 1 1 d . . . . .
H41 H 0.599532 0.844800 0.030436 0.032 Uiso 1 1 calc R U . . .
C42 C 0.7598(2) 0.8870(2) 0.0179(2) 0.0272(6) Uani 1 1 d . . . . .
H42 H 0.771694 0.873970 -0.049668 0.033 Uiso 1 1 calc R U . . .
C43 C 0.8443(2) 0.9230(2) 0.06873(19) 0.0243(5) Uani 1 1 d . . . . .
H43 H 0.914831 0.933683 0.036588 0.029 Uiso 1 1 calc R U . . .
C44 C 1.0609(2) 0.9009(2) 0.21618(18) 0.0206(5) Uani 1 1 d . . . . .
C45 C 0.9282(2) 0.70165(19) 0.37803(18) 0.0183(5) Uani 1 1 d . . . . .
C46 C 0.9067(2) 0.6131(2) 0.43935(19) 0.0206(5) Uani 1 1 d . . . . .
H46 H 0.928562 0.547919 0.414427 0.025 Uiso 1 1 calc R U . . .
C47 C 0.8561(2) 0.6167(2) 0.53251(19) 0.0215(5) Uani 1 1 d . . . . .
H47 H 0.843410 0.554507 0.567928 0.026 Uiso 1 1 calc R U . . .
C48 C 0.8227(2) 0.7107(2) 0.57650(18) 0.0216(5) Uani 1 1 d . . . . .
H48 H 0.786872 0.713965 0.639883 0.026 Uiso 1 1 calc R U . . .
C49 C 0.8460(2) 0.7965(2) 0.52085(18) 0.0190(5) Uani 1 1 d . . . . .
C50 C 0.8954(2) 0.79099(19) 0.42401(18) 0.0184(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 Al1 2.1219(11) . ?
Cl2 Al1 2.1444(11) . ?
P1 C1 1.788(3) . ?
P1 C7 1.786(3) . ?
P1 C13 1.789(3) . ?
P1 C19 1.882(3) . ?
Al1 O1 1.784(2) . ?
Al1 C20 1.953(3) . ?
O1 C19 1.281(3) . ?
O2 C19 1.202(3) . ?
C1 C2 1.393(4) . ?
C1 C6 1.401(4) . ?
C2 C3 1.393(4) . ?
C3 C4 1.388(4) . ?
C4 C5 1.389(4) . ?
C5 C6 1.391(4) . ?
C7 C12 1.380(3) . ?
C7 C8 1.436(4) . ?
C8 C9 1.378(4) . ?
C9 C10 1.407(4) . ?
C10 C11 1.367(4) . ?
C11 C12 1.430(4) . ?
C11 C22 1.507(4) . ?
C12 C21 1.517(4) . ?
C13 C18 1.395(3) . ?
C13 C14 1.398(3) . ?
C14 C15 1.389(4) . ?
C15 C16 1.388(4) . ?
C16 C17 1.385(4) . ?
C17 C18 1.393(4) . ?
C20 C21 1.376(4) . ?
C20 C25 1.427(4) . ?
C21 C22 1.419(3) . ?
C22 C23 1.368(4) . ?
C23 C24 1.410(4) . ?
C24 C25 1.389(4) . ?
Cl3 Al2 2.1250(11) . ?
Cl4 Al2 2.1465(11) . ?
P2 C32 1.786(3) . ?
P2 C26 1.787(3) . ?
P2 C38 1.788(3) . ?
P2 C44 1.891(3) . ?
Al2 O3 1.774(2) . ?
Al2 C45 1.958(3) . ?
O3 C44 1.285(3) . ?
O4 C44 1.199(3) . ?
C26 C31 1.403(4) . ?
C26 C27 1.407(4) . ?
C27 C28 1.389(4) . ?
C28 C29 1.385(4) . ?
C29 C30 1.390(4) . ?
C30 C31 1.389(4) . ?
C32 C33 1.379(4) . ?
C32 C37 1.424(4) . ?
C33 C34 1.425(3) . ?
C33 C50 1.519(4) . ?
C34 C35 1.366(4) . ?
C34 C49 1.500(4) . ?
C35 C36 1.411(4) . ?
C36 C37 1.383(4) . ?
C38 C39 1.395(3) . ?
C38 C43 1.403(4) . ?
C39 C40 1.386(4) . ?
C40 C41 1.386(4) . ?
C41 C42 1.387(4) . ?
C42 C43 1.379(4) . ?
C45 C50 1.378(4) . ?
C45 C46 1.437(4) . ?
C46 C47 1.386(4) . ?
C47 C48 1.420(4) . ?
C48 C49 1.369(4) . ?
C49 C50 1.428(4) . ?

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 C7 111.16(12) . . ?
C1 P1 C13 110.47(12) . . ?
C7 P1 C13 110.68(11) . . ?
C1 P1 C19 107.22(12) . . ?
C7 P1 C19 112.49(12) . . ?
C13 P1 C19 104.59(12) . . ?
O1 Al1 C20 102.93(10) . . ?
O1 Al1 Cl1 109.26(8) . . ?
C20 Al1 Cl1 116.01(8) . . ?
O1 Al1 Cl2 107.67(7) . . ?
C20 Al1 Cl2 110.54(9) . . ?
Cl1 Al1 Cl2 109.93(5) . . ?
C19 O1 Al1 150.5(2) . . ?
C2 C1 C6 120.1(2) . . ?
C2 C1 P1 121.9(2) . . ?
C6 C1 P1 117.96(19) . . ?
C3 C2 C1 119.5(2) . . ?
C4 C3 C2 120.3(3) . . ?
C3 C4 C5 120.3(3) . . ?
C4 C5 C6 120.0(2) . . ?
C5 C6 C1 119.8(2) . . ?
C12 C7 C8 116.0(2) . . ?
C12 C7 P1 124.49(19) . . ?
C8 C7 P1 119.09(18) . . ?
C9 C8 C7 121.6(2) . . ?
C8 C9 C10 122.4(2) . . ?
C11 C10 C9 116.0(2) . . ?
C10 C11 C12 123.0(2) . . ?
C10 C11 C22 147.0(2) . . ?
C12 C11 C22 90.0(2) . . ?
C7 C12 C11 120.9(2) . . ?
C7 C12 C21 149.5(2) . . ?
C11 C12 C21 89.6(2) . . ?
C18 C13 C14 120.5(2) . . ?
C18 C13 P1 121.47(19) . . ?
C14 C13 P1 117.99(19) . . ?
C15 C14 C13 119.7(2) . . ?
C14 C15 C16 119.7(2) . . ?
C17 C16 C15 120.8(2) . . ?
C16 C17 C18 120.1(2) . . ?
C17 C18 C13 119.2(2) . . ?
O2 C19 O1 128.1(3) . . ?
O2 C19 P1 117.8(2) . . ?
O1 C19 P1 114.03(18) . . ?
C21 C20 C25 112.0(2) . . ?
C21 C20 Al1 123.44(19) . . ?
C25 C20 Al1 124.36(19) . . ?
C20 C21 C22 124.7(2) . . ?
C20 C21 C12 145.2(2) . . ?
C22 C21 C12 90.0(2) . . ?
C23 C22 C21 122.2(2) . . ?
C23 C22 C11 147.5(2) . . ?
C21 C22 C11 90.4(2) . . ?
C22 C23 C24 115.2(2) . . ?
C25 C24 C23 121.8(2) . . ?
C24 C25 C20 124.1(2) . . ?
C32 P2 C26 111.64(12) . . ?
C32 P2 C38 109.68(12) . . ?
C26 P2 C38 110.61(12) . . ?
C32 P2 C44 106.78(11) . . ?
C26 P2 C44 109.67(12) . . ?
C38 P2 C44 108.35(12) . . ?
O3 Al2 C45 107.81(10) . . ?
O3 Al2 Cl3 105.70(8) . . ?
C45 Al2 Cl3 115.77(8) . . ?
O3 Al2 Cl4 108.96(8) . . ?
C45 Al2 Cl4 109.17(8) . . ?
Cl3 Al2 Cl4 109.21(5) . . ?
C44 O3 Al2 149.20(19) . . ?
C31 C26 C27 120.0(2) . . ?
C31 C26 P2 120.60(19) . . ?
C27 C26 P2 119.35(19) . . ?
C28 C27 C26 119.3(2) . . ?
C29 C28 C27 120.6(2) . . ?
C28 C29 C30 120.1(2) . . ?
C29 C30 C31 120.6(3) . . ?
C30 C31 C26 119.3(2) . . ?
C33 C32 C37 116.9(2) . . ?
C33 C32 P2 122.32(19) . . ?
C37 C32 P2 120.40(19) . . ?
C32 C33 C34 120.8(2) . . ?
C32 C33 C50 148.9(2) . . ?
C34 C33 C50 90.3(2) . . ?
C35 C34 C33 122.8(2) . . ?
C35 C34 C49 147.4(3) . . ?
C33 C34 C49 89.8(2) . . ?
C34 C35 C36 116.2(2) . . ?
C37 C36 C35 122.3(2) . . ?
C36 C37 C32 121.0(2) . . ?
C39 C38 C43 120.3(2) . . ?
C39 C38 P2 120.9(2) . . ?
C43 C38 P2 118.8(2) . . ?
C40 C39 C38 119.1(2) . . ?
C41 C40 C39 120.4(3) . . ?
C40 C41 C42 120.5(3) . . ?
C43 C42 C41 119.9(3) . . ?
C42 C43 C38 119.8(3) . . ?
O4 C44 O3 128.5(2) . . ?
O4 C44 P2 119.0(2) . . ?
O3 C44 P2 112.52(19) . . ?
C50 C45 C46 111.9(2) . . ?
C50 C45 Al2 128.09(19) . . ?
C46 C45 Al2 119.99(19) . . ?
C47 C46 C45 124.2(2) . . ?
C46 C47 C48 121.8(2) . . ?
C49 C48 C47 115.1(2) . . ?
C48 C49 C50 122.2(2) . . ?
C48 C49 C34 146.8(3) . . ?
C50 C49 C34 90.9(2) . . ?
C45 C50 C49 124.8(2) . . ?
C45 C50 C33 146.2(2) . . ?
C49 C50 C33 89.0(2) . . ?

_refine_diff_density_max         0.518
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.080



_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_pf445
_database_code_depnum_ccdc_archive 'CCDC 2179787'
loop_
_audit_author_name
_audit_author_address
'Beatrice Cula'
;Humboldt Universitaet zu Berlin
Germany
;
_audit_update_record             
;
2022-06-17 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H20 Al Cl2 P'
_chemical_formula_weight         473.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Al Al 0.0645 0.0514 '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'
P P 0.1023 0.0942 '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                   10.0145(10)
_cell_length_b                   14.1044(13)
_cell_length_c                   16.1893(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2286.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9992
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      28.33

_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.405
_shelx_estimated_absorpt_T_min   0.905
_shelx_estimated_absorpt_T_max   0.934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6584
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46321
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.391
_diffrn_reflns_theta_max         28.327
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             5661
_reflns_number_gt                5571
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.994

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

_computing_data_collection       'Bruker APEX4'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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)+(0.0394P)²+0.3955P] 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_abs_structure_details 
;
 Flack x determined using 2423 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5661
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0225
_refine_ls_wR_factor_ref         0.0613
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
Cl1 Cl 0.86048(4) 0.42987(3) 0.74476(3) 0.02030(9) Uani 1 1 d . . . . .
Cl2 Cl 0.75736(5) 0.52525(3) 0.93564(3) 0.02391(10) Uani 1 1 d . . . . .
P1 P 0.30170(4) 0.41444(3) 0.72952(2) 0.01456(9) Uani 1 1 d . . . . .
Al1 Al 0.69533(5) 0.43755(4) 0.83152(3) 0.01610(11) Uani 1 1 d . . . . .
C1 C 0.21829(17) 0.38828(12) 0.63359(10) 0.0179(3) Uani 1 1 d . . . . .
C2 C 0.13835(19) 0.45659(14) 0.59582(11) 0.0225(4) Uani 1 1 d . . . . .
H2 H 0.126976 0.517048 0.620710 0.027 Uiso 1 1 calc R U . . .
C3 C 0.0752(2) 0.43561(16) 0.52126(12) 0.0288(4) Uani 1 1 d . . . . .
H3 H 0.019949 0.481742 0.495571 0.035 Uiso 1 1 calc R U . . .
C4 C 0.0926(2) 0.34795(16) 0.48456(12) 0.0289(4) Uani 1 1 d . . . . .
H4 H 0.050080 0.334414 0.433446 0.035 Uiso 1 1 calc R U . . .
C5 C 0.1720(2) 0.27957(14) 0.52203(12) 0.0266(4) Uani 1 1 d . . . . .
H5 H 0.183689 0.219515 0.496464 0.032 Uiso 1 1 calc R U . . .
C6 C 0.23430(19) 0.29893(13) 0.59698(11) 0.0221(4) Uani 1 1 d . . . . .
H6 H 0.287384 0.251898 0.623169 0.027 Uiso 1 1 calc R U . . .
C7 C 0.28407(16) 0.31049(12) 0.79192(10) 0.0160(3) Uani 1 1 d . . . . .
C8 C 0.15539(18) 0.26561(13) 0.79166(11) 0.0199(3) Uani 1 1 d . . . . .
H8 H 0.084727 0.293703 0.761099 0.024 Uiso 1 1 calc R U . . .
C9 C 0.13154(19) 0.18278(13) 0.83457(12) 0.0217(3) Uani 1 1 d . . . . .
H9 H 0.044900 0.155419 0.832887 0.026 Uiso 1 1 calc R U . . .
C10 C 0.23309(18) 0.13753(12) 0.88110(10) 0.0194(3) Uani 1 1 d . . . . .
H10 H 0.217427 0.080186 0.910321 0.023 Uiso 1 1 calc R U . . .
C11 C 0.35434(18) 0.18106(11) 0.88144(10) 0.0165(3) Uani 1 1 d . . . . .
C12 C 0.38237(16) 0.26731(11) 0.83842(10) 0.0152(3) Uani 1 1 d . . . . .
C13 C 0.22567(15) 0.51442(12) 0.77893(10) 0.0161(3) Uani 1 1 d . . . . .
C14 C 0.25465(19) 0.60516(12) 0.74897(11) 0.0208(3) Uani 1 1 d . . . . .
H14 H 0.312347 0.612684 0.702853 0.025 Uiso 1 1 calc R U . . .
C15 C 0.1991(2) 0.68402(13) 0.78666(11) 0.0246(4) Uani 1 1 d . . . . .
H15 H 0.217780 0.745650 0.766009 0.029 Uiso 1 1 calc R U . . .
C16 C 0.11585(19) 0.67288(14) 0.85477(12) 0.0237(4) Uani 1 1 d . . . . .
H16 H 0.078159 0.727059 0.880683 0.028 Uiso 1 1 calc R U . . .
C17 C 0.08771(19) 0.58349(14) 0.88492(11) 0.0239(4) Uani 1 1 d . . . . .
H17 H 0.031136 0.576513 0.931627 0.029 Uiso 1 1 calc R U . . .
C18 C 0.14175(18) 0.50372(13) 0.84725(11) 0.0198(3) Uani 1 1 d . . . . .
H18 H 0.121754 0.442264 0.867829 0.024 Uiso 1 1 calc R U . . .
C19 C 0.47474(17) 0.44575(12) 0.71202(10) 0.0168(3) Uani 1 1 d . . . . .
C20 C 0.54240(17) 0.50195(12) 0.77865(11) 0.0185(3) Uani 1 1 d . . . . .
H20A H 0.475745 0.517408 0.821748 0.022 Uiso 1 1 calc R U . . .
H20B H 0.574002 0.562506 0.754692 0.022 Uiso 1 1 calc R U . . .
C21 C 0.64739(17) 0.31126(12) 0.87595(10) 0.0170(3) Uani 1 1 d . . . . .
C22 C 0.52567(17) 0.26576(12) 0.87192(10) 0.0160(3) Uani 1 1 d . . . . .
C23 C 0.49486(17) 0.17931(12) 0.91346(10) 0.0169(3) Uani 1 1 d . . . . .
C24 C 0.5861(2) 0.13220(13) 0.96134(10) 0.0207(3) Uani 1 1 d . . . . .
H24 H 0.565429 0.074704 0.989098 0.025 Uiso 1 1 calc R U . . .
C25 C 0.71312(19) 0.17537(13) 0.96641(11) 0.0222(4) Uani 1 1 d . . . . .
H25 H 0.781001 0.145908 0.998372 0.027 Uiso 1 1 calc R U . . .
C26 C 0.74131(19) 0.25995(13) 0.92578(11) 0.0205(3) Uani 1 1 d . . . . .
H26 H 0.828632 0.285458 0.931403 0.025 Uiso 1 1 calc R U . . .
C27 C 0.52978(19) 0.41927(14) 0.64031(11) 0.0231(4) Uani 1 1 d . . . . .
H27A H 0.619481 0.436137 0.628109 0.028 Uiso 1 1 calc R U . . .
H27B H 0.479157 0.383618 0.601613 0.028 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 Al1 2.1725(6) . ?
Cl2 Al1 2.1811(7) . ?
P1 C7 1.7892(17) . ?
P1 C13 1.7911(17) . ?
P1 C1 1.8018(18) . ?
P1 C19 1.8106(17) . ?
Al1 C20 1.9756(18) . ?
Al1 C21 1.9801(18) . ?
C1 C2 1.394(2) . ?
C1 C6 1.402(2) . ?
C2 C3 1.394(3) . ?
C3 C4 1.383(3) . ?
C4 C5 1.389(3) . ?
C5 C6 1.392(3) . ?
C7 C12 1.381(2) . ?
C7 C8 1.436(2) . ?
C8 C9 1.380(2) . ?
C9 C10 1.417(3) . ?
C10 C11 1.361(2) . ?
C11 C12 1.430(2) . ?
C11 C23 1.500(2) . ?
C12 C22 1.534(2) . ?
C13 C18 1.397(2) . ?
C13 C14 1.399(2) . ?
C14 C15 1.385(2) . ?
C15 C16 1.391(3) . ?
C16 C17 1.381(3) . ?
C17 C18 1.389(3) . ?
C19 C27 1.338(2) . ?
C19 C20 1.500(2) . ?
C21 C22 1.379(2) . ?
C21 C26 1.435(2) . ?
C22 C23 1.426(2) . ?
C23 C24 1.370(2) . ?
C24 C25 1.413(3) . ?
C25 C26 1.391(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 P1 C13 110.55(8) . . ?
C7 P1 C1 105.85(8) . . ?
C13 P1 C1 110.43(8) . . ?
C7 P1 C19 112.50(8) . . ?
C13 P1 C19 106.54(8) . . ?
C1 P1 C19 111.03(8) . . ?
C20 Al1 C21 112.52(8) . . ?
C20 Al1 Cl1 109.45(6) . . ?
C21 Al1 Cl1 111.99(5) . . ?
C20 Al1 Cl2 107.15(6) . . ?
C21 Al1 Cl2 107.37(5) . . ?
Cl1 Al1 Cl2 108.12(3) . . ?
C2 C1 C6 120.11(16) . . ?
C2 C1 P1 120.18(14) . . ?
C6 C1 P1 119.71(13) . . ?
C1 C2 C3 119.57(18) . . ?
C4 C3 C2 120.30(19) . . ?
C3 C4 C5 120.35(18) . . ?
C4 C5 C6 120.07(19) . . ?
C5 C6 C1 119.59(18) . . ?
C12 C7 C8 116.56(15) . . ?
C12 C7 P1 126.79(13) . . ?
C8 C7 P1 116.63(12) . . ?
C9 C8 C7 121.81(17) . . ?
C8 C9 C10 121.64(16) . . ?
C11 C10 C9 116.06(15) . . ?
C10 C11 C12 123.86(16) . . ?
C10 C11 C23 146.23(16) . . ?
C12 C11 C23 89.89(14) . . ?
C7 C12 C11 120.06(15) . . ?
C7 C12 C22 149.98(16) . . ?
C11 C12 C22 89.96(13) . . ?
C18 C13 C14 119.87(15) . . ?
C18 C13 P1 121.61(13) . . ?
C14 C13 P1 118.51(12) . . ?
C15 C14 C13 119.90(16) . . ?
C14 C15 C16 119.94(17) . . ?
C17 C16 C15 120.37(17) . . ?
C16 C17 C18 120.31(16) . . ?
C17 C18 C13 119.62(16) . . ?
C27 C19 C20 125.81(16) . . ?
C27 C19 P1 117.51(14) . . ?
C20 C19 P1 116.66(12) . . ?
C19 C20 Al1 114.75(12) . . ?
C22 C21 C26 111.79(15) . . ?
C22 C21 Al1 128.00(13) . . ?
C26 C21 Al1 119.94(13) . . ?
C21 C22 C23 124.52(16) . . ?
C21 C22 C12 146.81(15) . . ?
C23 C22 C12 88.65(13) . . ?
C24 C23 C22 122.49(17) . . ?
C24 C23 C11 146.01(17) . . ?
C22 C23 C11 91.49(13) . . ?
C23 C24 C25 115.11(16) . . ?
C26 C25 C24 121.65(16) . . ?
C25 C26 C21 124.42(17) . . ?

_refine_diff_density_max         0.311
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.041



####################################################################### 
# 
# 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_tb13
_database_code_depnum_ccdc_archive 'CCDC 2179789'
loop_
_audit_author_name
_audit_author_address
'Beatrice Cula'
;Humboldt Universitaet zu Berlin
Germany
;
_audit_update_record             
;
2022-06-17 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H25 P Sn'
_chemical_formula_weight         499.13

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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.8677(4)
_cell_length_b                   12.9432(5)
_cell_length_c                   18.0733(8)
_cell_angle_alpha                90
_cell_angle_beta                 94.123(2)
_cell_angle_gamma                90
_cell_volume                     2302.34(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    102(2)
_cell_measurement_reflns_used    9778
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      28.29

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_F_000             1008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    1.189
_shelx_estimated_absorpt_T_min   0.688
_shelx_estimated_absorpt_T_max   0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6335
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      102(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51161
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.937
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.959
_reflns_number_total             5555
_reflns_number_gt                5399
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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)+(0.0144P)²+1.4879P] 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         5555
_refine_ls_number_parameters     265
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0185
_refine_ls_wR_factor_ref         0.0453
_refine_ls_wR_factor_gt          0.0451
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.22448(2) 0.24722(2) 0.08742(2) 0.01833(4) Uani 1 1 d . . . . .
P1 P 0.38353(3) -0.03348(2) 0.13439(2) 0.01708(6) Uani 1 1 d . . . . .
C1 C 0.16635(13) 0.23206(10) 0.19918(7) 0.0189(2) Uani 1 1 d . . . . .
C25 C 0.11390(15) 0.13418(11) 0.02099(8) 0.0277(3) Uani 1 1 d . . . . .
H25A H 0.151286 0.129822 -0.027701 0.042 Uiso 1 1 calc R U . . .
H25B H 0.017995 0.154232 0.014672 0.042 Uiso 1 1 calc R U . . .
H25C H 0.121800 0.066759 0.045594 0.042 Uiso 1 1 calc R U . . .
C21 C 0.12723(12) 0.13748(10) 0.31406(7) 0.0185(2) Uani 1 1 d . . . . .
C2 C 0.18118(12) 0.14541(9) 0.24315(7) 0.0168(2) Uani 1 1 d . . . . .
C26 C 0.43987(15) 0.24212(11) 0.08501(9) 0.0285(3) Uani 1 1 d . . . . .
H26A H 0.479417 0.210084 0.130725 0.043 Uiso 1 1 calc R U . . .
H26B H 0.475186 0.312509 0.081014 0.043 Uiso 1 1 calc R U . . .
H26C H 0.464102 0.201410 0.042190 0.043 Uiso 1 1 calc R U . . .
C4 C 0.30682(12) -0.04496(9) 0.22329(7) 0.0174(2) Uani 1 1 d . . . . .
C22 C 0.05833(14) 0.21624(11) 0.34494(7) 0.0237(3) Uani 1 1 d . . . . .
H22 H 0.021771 0.210131 0.391951 0.028 Uiso 1 1 calc R U . . .
C19 C 0.18888(13) -0.05776(10) 0.36536(7) 0.0213(2) Uani 1 1 d . . . . .
H19 H 0.150719 -0.061350 0.412074 0.026 Uiso 1 1 calc R U . . .
C27 C 0.15700(16) 0.39671(11) 0.04787(8) 0.0303(3) Uani 1 1 d . . . . .
H27A H 0.176110 0.448226 0.086974 0.045 Uiso 1 1 calc R U . . .
H27B H 0.059044 0.394583 0.034414 0.045 Uiso 1 1 calc R U . . .
H27C H 0.205107 0.415412 0.004214 0.045 Uiso 1 1 calc R U . . .
C24 C 0.09628(14) 0.31446(10) 0.23287(7) 0.0236(3) Uani 1 1 d . . . . .
H24 H 0.084120 0.377483 0.206280 0.028 Uiso 1 1 calc R U . . .
C6 C 0.51845(14) -0.22910(11) 0.12441(7) 0.0224(2) Uani 1 1 d . . . . .
H6 H 0.596196 -0.199149 0.150050 0.027 Uiso 1 1 calc R U . . .
C20 C 0.17796(12) 0.02847(10) 0.32203(7) 0.0180(2) Uani 1 1 d . . . . .
C3 C 0.23421(12) 0.03496(9) 0.25162(6) 0.0166(2) Uani 1 1 d . . . . .
C10 C 0.28871(13) -0.21561(11) 0.07132(7) 0.0227(2) Uani 1 1 d . . . . .
H10 H 0.209197 -0.175701 0.059756 0.027 Uiso 1 1 calc R U . . .
C12 C 0.60188(13) 0.03537(10) 0.23420(7) 0.0223(2) Uani 1 1 d . . . . .
H12 H 0.542764 0.028398 0.273125 0.027 Uiso 1 1 calc R U . . .
C9 C 0.29115(15) -0.31902(11) 0.05056(8) 0.0271(3) Uani 1 1 d . . . . .
H9 H 0.212872 -0.349738 0.026002 0.032 Uiso 1 1 calc R U . . .
C5 C 0.40174(12) -0.16971(10) 0.10897(6) 0.0181(2) Uani 1 1 d . . . . .
C23 C 0.04529(14) 0.30749(11) 0.30197(8) 0.0265(3) Uani 1 1 d . . . . .
H23 H 0.000305 0.365514 0.321088 0.032 Uiso 1 1 calc R U . . .
C15 C 0.77809(14) 0.05336(11) 0.12190(8) 0.0268(3) Uani 1 1 d . . . . .
H15 H 0.838760 0.058319 0.083551 0.032 Uiso 1 1 calc R U . . .
C17 C 0.31736(13) -0.13535(10) 0.26889(7) 0.0214(2) Uani 1 1 d . . . . .
H17 H 0.365348 -0.193408 0.252031 0.026 Uiso 1 1 calc R U . . .
C7 C 0.52127(14) -0.33247(11) 0.10227(8) 0.0259(3) Uani 1 1 d . . . . .
H7 H 0.601394 -0.372236 0.112350 0.031 Uiso 1 1 calc R U . . .
C11 C 0.55823(12) 0.00468(9) 0.16240(7) 0.0184(2) Uani 1 1 d . . . . .
C18 C 0.26058(14) -0.14168(10) 0.33649(7) 0.0230(3) Uani 1 1 d . . . . .
H18 H 0.269908 -0.203894 0.364273 0.028 Uiso 1 1 calc R U . . .
C14 C 0.81972(14) 0.08533(11) 0.19331(8) 0.0270(3) Uani 1 1 d . . . . .
H14 H 0.908053 0.113284 0.203712 0.032 Uiso 1 1 calc R U . . .
C16 C 0.64833(13) 0.01422(11) 0.10634(7) 0.0236(3) Uani 1 1 d . . . . .
H16 H 0.620269 -0.006335 0.057145 0.028 Uiso 1 1 calc R U . . .
C8 C 0.40777(15) -0.37733(11) 0.06568(8) 0.0275(3) Uani 1 1 d . . . . .
H8 H 0.409880 -0.447765 0.051012 0.033 Uiso 1 1 calc R U . . .
C13 C 0.73171(14) 0.07621(11) 0.24917(8) 0.0271(3) Uani 1 1 d . . . . .
H13 H 0.759925 0.097922 0.298084 0.033 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
Sn1 C26 2.1300(15) . ?
Sn1 C25 2.1411(14) . ?
Sn1 C1 2.1480(13) . ?
Sn1 C27 2.1517(14) . ?
P1 C11 1.8293(12) . ?
P1 C4 1.8307(12) . ?
P1 C5 1.8342(13) . ?
C1 C2 1.3762(17) . ?
C1 C24 1.4307(18) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C21 C22 1.3666(18) . ?
C21 C2 1.4262(16) . ?
C21 C20 1.5005(17) . ?
C2 C3 1.5262(17) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C4 C3 1.3778(17) . ?
C4 C17 1.4305(17) . ?
C22 C23 1.414(2) . ?
C22 H22 0.9500 . ?
C19 C20 1.3633(18) . ?
C19 C18 1.4162(19) . ?
C19 H19 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C24 C23 1.3824(19) . ?
C24 H24 0.9500 . ?
C6 C5 1.3960(18) . ?
C6 C7 1.3974(19) . ?
C6 H6 0.9500 . ?
C20 C3 1.4269(16) . ?
C10 C9 1.391(2) . ?
C10 C5 1.3967(17) . ?
C10 H10 0.9500 . ?
C12 C13 1.3943(18) . ?
C12 C11 1.3953(17) . ?
C12 H12 0.9500 . ?
C9 C8 1.387(2) . ?
C9 H9 0.9500 . ?
C23 H23 0.9500 . ?
C15 C16 1.3868(19) . ?
C15 C14 1.389(2) . ?
C15 H15 0.9500 . ?
C17 C18 1.3827(18) . ?
C17 H17 0.9500 . ?
C7 C8 1.386(2) . ?
C7 H7 0.9500 . ?
C11 C16 1.4007(17) . ?
C18 H18 0.9500 . ?
C14 C13 1.383(2) . ?
C14 H14 0.9500 . ?
C16 H16 0.9500 . ?
C8 H8 0.9500 . ?
C13 H13 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
C26 Sn1 C25 115.87(6) . . ?
C26 Sn1 C1 110.53(5) . . ?
C25 Sn1 C1 107.76(5) . . ?
C26 Sn1 C27 107.85(6) . . ?
C25 Sn1 C27 107.16(6) . . ?
C1 Sn1 C27 107.30(5) . . ?
C11 P1 C4 102.70(6) . . ?
C11 P1 C5 102.80(6) . . ?
C4 P1 C5 101.30(6) . . ?
C2 C1 C24 113.35(11) . . ?
C2 C1 Sn1 126.37(9) . . ?
C24 C1 Sn1 120.13(9) . . ?
Sn1 C25 H25A 109.5 . . ?
Sn1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Sn1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C21 C2 122.82(12) . . ?
C22 C21 C20 146.57(12) . . ?
C2 C21 C20 90.60(10) . . ?
C1 C2 C21 123.12(11) . . ?
C1 C2 C3 147.42(11) . . ?
C21 C2 C3 89.42(9) . . ?
Sn1 C26 H26A 109.5 . . ?
Sn1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Sn1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C3 C4 C17 114.72(11) . . ?
C3 C4 P1 121.61(9) . . ?
C17 C4 P1 123.67(9) . . ?
C21 C22 C23 115.28(12) . . ?
C21 C22 H22 122.4 . . ?
C23 C22 H22 122.4 . . ?
C20 C19 C18 115.93(11) . . ?
C20 C19 H19 122.0 . . ?
C18 C19 H19 122.0 . . ?
Sn1 C27 H27A 109.5 . . ?
Sn1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Sn1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C23 C24 C1 123.66(12) . . ?
C23 C24 H24 118.2 . . ?
C1 C24 H24 118.2 . . ?
C5 C6 C7 120.21(12) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C19 C20 C3 122.73(12) . . ?
C19 C20 C21 146.83(12) . . ?
C3 C20 C21 90.43(10) . . ?
C4 C3 C20 122.23(11) . . ?
C4 C3 C2 148.18(11) . . ?
C20 C3 C2 89.54(9) . . ?
C9 C10 C5 120.80(12) . . ?
C9 C10 H10 119.6 . . ?
C5 C10 H10 119.6 . . ?
C13 C12 C11 120.43(12) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C8 C9 C10 120.06(12) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C10 C5 C6 118.79(12) . . ?
C10 C5 P1 116.21(10) . . ?
C6 C5 P1 125.00(10) . . ?
C24 C23 C22 121.72(12) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C16 C15 C14 120.28(12) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C18 C17 C4 122.70(12) . . ?
C18 C17 H17 118.7 . . ?
C4 C17 H17 118.7 . . ?
C8 C7 C6 120.37(13) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C12 C11 C16 118.56(11) . . ?
C12 C11 P1 123.78(9) . . ?
C16 C11 P1 117.27(9) . . ?
C17 C18 C19 121.67(12) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C13 C14 C15 119.57(12) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C15 C16 C11 120.69(12) . . ?
C15 C16 H16 119.7 . . ?
C11 C16 H16 119.7 . . ?
C7 C8 C9 119.76(13) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C14 C13 C12 120.46(13) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?

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
C24 C1 C2 C21 2.29(17) . . . . ?
Sn1 C1 C2 C21 -173.18(9) . . . . ?
C24 C1 C2 C3 179.35(17) . . . . ?
Sn1 C1 C2 C3 3.9(3) . . . . ?
C22 C21 C2 C1 -1.28(19) . . . . ?
C20 C21 C2 C1 177.81(12) . . . . ?
C22 C21 C2 C3 -179.69(12) . . . . ?
C20 C21 C2 C3 -0.61(9) . . . . ?
C11 P1 C4 C3 95.80(11) . . . . ?
C5 P1 C4 C3 -158.14(10) . . . . ?
C11 P1 C4 C17 -83.73(11) . . . . ?
C5 P1 C4 C17 22.33(12) . . . . ?
C2 C21 C22 C23 -0.74(19) . . . . ?
C20 C21 C22 C23 -179.08(17) . . . . ?
C2 C1 C24 C23 -1.49(19) . . . . ?
Sn1 C1 C24 C23 174.29(11) . . . . ?
C18 C19 C20 C3 0.26(18) . . . . ?
C18 C19 C20 C21 -178.12(17) . . . . ?
C22 C21 C20 C19 -2.1(4) . . . . ?
C2 C21 C20 C19 179.29(19) . . . . ?
C22 C21 C20 C3 179.3(2) . . . . ?
C2 C21 C20 C3 0.65(9) . . . . ?
C17 C4 C3 C20 1.84(17) . . . . ?
P1 C4 C3 C20 -177.73(9) . . . . ?
C17 C4 C3 C2 178.07(17) . . . . ?
P1 C4 C3 C2 -1.5(3) . . . . ?
C19 C20 C3 C4 -1.71(19) . . . . ?
C21 C20 C3 C4 177.40(11) . . . . ?
C19 C20 C3 C2 -179.72(12) . . . . ?
C21 C20 C3 C2 -0.61(9) . . . . ?
C1 C2 C3 C4 6.3(3) . . . . ?
C21 C2 C3 C4 -176.17(19) . . . . ?
C1 C2 C3 C20 -176.90(19) . . . . ?
C21 C2 C3 C20 0.64(9) . . . . ?
C5 C10 C9 C8 -1.5(2) . . . . ?
C9 C10 C5 C6 1.04(19) . . . . ?
C9 C10 C5 P1 -178.98(10) . . . . ?
C7 C6 C5 C10 0.11(19) . . . . ?
C7 C6 C5 P1 -179.87(10) . . . . ?
C11 P1 C5 C10 -167.90(10) . . . . ?
C4 P1 C5 C10 86.12(10) . . . . ?
C11 P1 C5 C6 12.07(12) . . . . ?
C4 P1 C5 C6 -93.91(12) . . . . ?
C1 C24 C23 C22 -0.4(2) . . . . ?
C21 C22 C23 C24 1.5(2) . . . . ?
C3 C4 C17 C18 -0.73(18) . . . . ?
P1 C4 C17 C18 178.84(10) . . . . ?
C5 C6 C7 C8 -0.8(2) . . . . ?
C13 C12 C11 C16 1.1(2) . . . . ?
C13 C12 C11 P1 -171.55(11) . . . . ?
C4 P1 C11 C12 -11.01(12) . . . . ?
C5 P1 C11 C12 -115.91(11) . . . . ?
C4 P1 C11 C16 176.29(10) . . . . ?
C5 P1 C11 C16 71.39(11) . . . . ?
C4 C17 C18 C19 -0.6(2) . . . . ?
C20 C19 C18 C17 0.87(19) . . . . ?
C16 C15 C14 C13 1.1(2) . . . . ?
C14 C15 C16 C11 -1.1(2) . . . . ?
C12 C11 C16 C15 0.0(2) . . . . ?
P1 C11 C16 C15 173.07(11) . . . . ?
C6 C7 C8 C9 0.4(2) . . . . ?
C10 C9 C8 C7 0.7(2) . . . . ?
C15 C14 C13 C12 -0.1(2) . . . . ?
C11 C12 C13 C14 -1.0(2) . . . . ?

_refine_diff_density_max         0.369
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.046



####################################################################### 
# 
# 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_pf282
_database_code_depnum_ccdc_archive 'CCDC 2179788'
loop_
_audit_author_name
_audit_author_address
'Beatrice Cula'
;Humboldt Universitaet zu Berlin
Germany
;
_audit_update_record             
;
2022-06-17 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H16 Al Cl2 P'
_chemical_formula_weight         433.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Al Al 0.0645 0.0514 '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'
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                   11.3572(10)
_cell_length_b                   12.4085(11)
_cell_length_c                   14.7374(9)
_cell_angle_alpha                90
_cell_angle_beta                 97.645(2)
_cell_angle_gamma                90
_cell_volume                     2058.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9721
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      25.38

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_F_000             888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.443
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6453
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            95869
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.132
_diffrn_reflns_theta_max         25.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3775
_reflns_number_gt                3615
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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)+(0.0303P)²+1.4173P] 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         3775
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0632
_refine_ls_wR_factor_gt          0.0623
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
Cl1 Cl 0.69348(3) 0.58880(3) 0.26800(2) 0.02137(9) Uani 1 1 d . . . . .
Al1 Al 0.75830(3) 0.61580(3) 0.40885(3) 0.01423(10) Uani 1 1 d . . . . .
C1 C 0.71456(11) 0.50610(11) 0.49404(9) 0.0146(3) Uani 1 1 d . . . . .
Cl2 Cl 0.93987(3) 0.66471(3) 0.42628(2) 0.02216(9) Uani 1 1 d . . . . .
P2 P 0.65457(3) 0.78682(3) 0.45137(2) 0.01331(9) Uani 1 1 d . . . . .
C2 C 0.74794(12) 0.39771(11) 0.51850(9) 0.0177(3) Uani 1 1 d . . . . .
H2 H 0.799032 0.360301 0.483235 0.021 Uiso 1 1 calc R U . . .
C4 C 0.63047(12) 0.39282(11) 0.64889(10) 0.0190(3) Uani 1 1 d . . . . .
H4 H 0.605042 0.355860 0.699288 0.023 Uiso 1 1 calc R U . . .
C3 C 0.70833(12) 0.34522(11) 0.59195(10) 0.0197(3) Uani 1 1 d . . . . .
H3 H 0.734596 0.273506 0.604997 0.024 Uiso 1 1 calc R U . . .
C5 C 0.59506(11) 0.49579(11) 0.62556(9) 0.0157(3) Uani 1 1 d . . . . .
C6 C 0.63809(11) 0.54642(11) 0.55013(9) 0.0149(3) Uani 1 1 d . . . . .
C7 C 0.58019(11) 0.64883(11) 0.56989(9) 0.0146(3) Uani 1 1 d . . . . .
C9 C 0.51024(12) 0.82100(12) 0.60138(9) 0.0191(3) Uani 1 1 d . . . . .
H9 H 0.501731 0.895898 0.588822 0.023 Uiso 1 1 calc R U . . .
C8 C 0.57233(11) 0.75436(11) 0.54462(9) 0.0148(3) Uani 1 1 d . . . . .
C10 C 0.46241(13) 0.77696(12) 0.67460(10) 0.0216(3) Uani 1 1 d . . . . .
H10 H 0.419866 0.823129 0.710095 0.026 Uiso 1 1 calc R U . . .
C11 C 0.47345(12) 0.66608(12) 0.69972(9) 0.0197(3) Uani 1 1 d . . . . .
H11 H 0.440526 0.637977 0.750778 0.024 Uiso 1 1 calc R U . . .
C12 C 0.53420(12) 0.60264(11) 0.64602(9) 0.0161(3) Uani 1 1 d . . . . .
C13 C 0.55532(12) 0.84383(11) 0.35712(9) 0.0156(3) Uani 1 1 d . . . . .
C14 C 0.59518(13) 0.85245(12) 0.27171(10) 0.0209(3) Uani 1 1 d . . . . .
H14 H 0.672110 0.827300 0.263647 0.025 Uiso 1 1 calc R U . . .
C15 C 0.52214(14) 0.89783(13) 0.19867(10) 0.0254(3) Uani 1 1 d . . . . .
H15 H 0.549170 0.903715 0.140574 0.030 Uiso 1 1 calc R U . . .
C16 C 0.40962(14) 0.93466(13) 0.21029(10) 0.0266(3) Uani 1 1 d . . . . .
H16 H 0.360020 0.965992 0.160211 0.032 Uiso 1 1 calc R U . . .
C17 C 0.36969(13) 0.92582(12) 0.29453(11) 0.0249(3) Uani 1 1 d . . . . .
H17 H 0.292390 0.950514 0.302022 0.030 Uiso 1 1 calc R U . . .
C18 C 0.44208(12) 0.88097(11) 0.36838(10) 0.0189(3) Uani 1 1 d . . . . .
H18 H 0.414613 0.875589 0.426343 0.023 Uiso 1 1 calc R U . . .
C19 C 0.75335(11) 0.89657(11) 0.49406(9) 0.0154(3) Uani 1 1 d . . . . .
C20 C 0.83367(12) 0.87921(12) 0.57331(9) 0.0200(3) Uani 1 1 d . . . . .
H20 H 0.837234 0.810977 0.602792 0.024 Uiso 1 1 calc R U . . .
C21 C 0.90812(13) 0.96215(13) 0.60866(10) 0.0239(3) Uani 1 1 d . . . . .
H21 H 0.962584 0.950537 0.662507 0.029 Uiso 1 1 calc R U . . .
C22 C 0.90338(13) 1.06194(13) 0.56575(10) 0.0243(3) Uani 1 1 d . . . . .
H22 H 0.954069 1.118560 0.590537 0.029 Uiso 1 1 calc R U . . .
C23 C 0.82484(13) 1.07901(12) 0.48684(10) 0.0228(3) Uani 1 1 d . . . . .
H23 H 0.822083 1.147191 0.457312 0.027 Uiso 1 1 calc R U . . .
C24 C 0.74992(12) 0.99644(11) 0.45070(9) 0.0184(3) Uani 1 1 d . . . . .
H24 H 0.696366 1.008225 0.396388 0.022 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 Al1 2.1346(5) . ?
Al1 C1 1.9600(14) . ?
Al1 Cl2 2.1321(5) . ?
Al1 P2 2.5456(5) . ?
C1 C6 1.3707(19) . ?
C1 C2 1.4305(19) . ?
P2 C8 1.8068(13) . ?
P2 C13 1.8122(13) . ?
P2 C19 1.8224(14) . ?
C2 C3 1.388(2) . ?
C2 H2 0.9500 . ?
C4 C5 1.369(2) . ?
C4 C3 1.426(2) . ?
C4 H4 0.9500 . ?
C3 H3 0.9500 . ?
C5 C6 1.4192(18) . ?
C5 C12 1.5434(19) . ?
C6 C7 1.4775(19) . ?
C7 C8 1.3611(19) . ?
C7 C12 1.4200(18) . ?
C9 C10 1.384(2) . ?
C9 C8 1.4275(19) . ?
C9 H9 0.9500 . ?
C10 C11 1.426(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.367(2) . ?
C11 H11 0.9500 . ?
C13 C18 1.3966(19) . ?
C13 C14 1.397(2) . ?
C14 C15 1.388(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(2) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.3924(19) . ?
C19 C20 1.3998(19) . ?
C20 C21 1.389(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.385(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(2) . ?
C23 H23 0.9500 . ?
C24 H24 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
C1 Al1 Cl2 116.36(4) . . ?
C1 Al1 Cl1 115.46(4) . . ?
Cl2 Al1 Cl1 111.39(2) . . ?
C1 Al1 P2 104.85(4) . . ?
Cl2 Al1 P2 101.82(2) . . ?
Cl1 Al1 P2 105.02(2) . . ?
C6 C1 C2 111.04(12) . . ?
C6 C1 Al1 111.57(10) . . ?
C2 C1 Al1 137.15(10) . . ?
C8 P2 C13 109.77(6) . . ?
C8 P2 C19 105.12(6) . . ?
C13 P2 C19 105.34(6) . . ?
C8 P2 Al1 107.72(5) . . ?
C13 P2 Al1 113.44(5) . . ?
C19 P2 Al1 115.10(4) . . ?
C3 C2 C1 122.35(13) . . ?
C3 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
C5 C4 C3 115.04(13) . . ?
C5 C4 H4 122.5 . . ?
C3 C4 H4 122.5 . . ?
C2 C3 C4 123.72(13) . . ?
C2 C3 H3 118.1 . . ?
C4 C3 H3 118.1 . . ?
C4 C5 C6 119.30(12) . . ?
C4 C5 C12 151.24(13) . . ?
C6 C5 C12 89.00(11) . . ?
C1 C6 C5 128.51(13) . . ?
C1 C6 C7 140.09(13) . . ?
C5 C6 C7 91.01(11) . . ?
C8 C7 C12 125.94(12) . . ?
C8 C7 C6 142.02(12) . . ?
C12 C7 C6 91.64(11) . . ?
C10 C9 C8 120.27(13) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C7 C8 C9 114.61(12) . . ?
C7 C8 P2 113.63(10) . . ?
C9 C8 P2 131.47(11) . . ?
C9 C10 C11 123.61(13) . . ?
C9 C10 H10 118.2 . . ?
C11 C10 H10 118.2 . . ?
C12 C11 C10 116.06(13) . . ?
C12 C11 H11 122.0 . . ?
C10 C11 H11 122.0 . . ?
C11 C12 C7 119.49(13) . . ?
C11 C12 C5 151.86(13) . . ?
C7 C12 C5 88.34(10) . . ?
C18 C13 C14 119.71(12) . . ?
C18 C13 P2 121.76(10) . . ?
C14 C13 P2 118.51(10) . . ?
C15 C14 C13 119.86(13) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 120.17(14) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 120.13(13) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.31(14) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C13 119.82(13) . . ?
C17 C18 H18 120.1 . . ?
C13 C18 H18 120.1 . . ?
C24 C19 C20 119.69(13) . . ?
C24 C19 P2 121.89(10) . . ?
C20 C19 P2 118.42(11) . . ?
C21 C20 C19 119.71(13) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C22 C21 C20 120.36(13) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C21 120.04(14) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.11(14) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C19 120.08(13) . . ?
C23 C24 H24 120.0 . . ?
C19 C24 H24 120.0 . . ?

_refine_diff_density_max         0.349
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.042



