# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1897901'
loop_
_audit_author_name
_audit_author_address
'Enno Lork'
;Bremen University
Germany
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C98 H76 Cl5 Hg2 Li O4 P4'
_chemical_formula_weight         2026.84

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'
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'
Hg Hg -2.3894 9.2266 '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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.2748(8)
_cell_length_b                   15.6725(8)
_cell_length_c                   21.2164(11)
_cell_angle_alpha                105.246(2)
_cell_angle_beta                 98.704(2)
_cell_angle_gamma                94.464(2)
_cell_volume                     4492.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9905
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      29.20

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2008
_exptl_absorpt_coefficient_mu    3.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5743
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture D8 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            126062
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         28.28
_reflns_number_total             22272
_reflns_number_gt                18428
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 607 162 ' '
_platon_squeeze_details          
;
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0221P)²+54.4256P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         22272
_refine_ls_number_parameters     1027
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1216
_refine_ls_wR_factor_gt          0.1162
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.004
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6418(7) 0.1115(5) 0.7716(4) 0.050(2) Uani 1 1 d . . .
H1A H 0.6373 0.1086 0.7241 0.060 Uiso 1 1 calc R . .
H1B H 0.6903 0.1616 0.7983 0.060 Uiso 1 1 calc R . .
C2 C 0.5446(8) 0.1230(5) 0.7931(5) 0.059(3) Uani 1 1 d . . .
H2A H 0.5482 0.1795 0.8284 0.071 Uiso 1 1 calc R . .
H2B H 0.4953 0.1233 0.7550 0.071 Uiso 1 1 calc R . .
C3 C 0.8786(5) -0.5780(5) 0.9377(4) 0.0347(15) Uani 1 1 d . . .
H3A H 0.8576 -0.5826 0.9792 0.042 Uiso 1 1 calc R . .
H3B H 0.9491 -0.5747 0.9442 0.042 Uiso 1 1 calc R . .
C4 C 0.8319(5) -0.6585(5) 0.8789(4) 0.0345(15) Uani 1 1 d . . .
H4A H 0.8807 -0.6954 0.8617 0.041 Uiso 1 1 calc R . .
H4B H 0.7844 -0.6962 0.8926 0.041 Uiso 1 1 calc R . .
C5 C -0.0137(5) -0.1944(6) 0.8668(4) 0.0430(19) Uani 1 1 d . . .
H5A H -0.0051 -0.1893 0.9148 0.052 Uiso 1 1 calc R . .
H5B H -0.0830 -0.2022 0.8487 0.052 Uiso 1 1 calc R . .
C6 C 0.0372(6) -0.1104(6) 0.8546(4) 0.048(2) Uani 1 1 d . . .
H6A H -0.0084 -0.0820 0.8290 0.058 Uiso 1 1 calc R . .
H6B H 0.0664 -0.0663 0.8972 0.058 Uiso 1 1 calc R . .
C7 C 0.3341(7) -0.8329(6) 0.5024(4) 0.055(2) Uani 1 1 d . . .
H7A H 0.3483 -0.8168 0.4624 0.066 Uiso 1 1 calc R . .
H7B H 0.2890 -0.8885 0.4882 0.066 Uiso 1 1 calc R . .
C8 C 0.4265(7) -0.8446(6) 0.5456(4) 0.047(2) Uani 1 1 d . . .
H8A H 0.4239 -0.9057 0.5507 0.056 Uiso 1 1 calc R . .
H8B H 0.4829 -0.8330 0.5257 0.056 Uiso 1 1 calc R . .
C10 C 0.6752(4) -0.1418(4) 0.8163(3) 0.0244(12) Uani 1 1 d . . .
C11 C 0.7440(5) -0.1054(5) 0.7879(3) 0.0301(14) Uani 1 1 d . . .
H11 H 0.7955 -0.1385 0.7781 0.036 Uiso 1 1 calc R . .
C12 C 0.7434(5) -0.0218(5) 0.7723(3) 0.0365(17) Uani 1 1 d . . .
H12 H 0.7939 0.0008 0.7545 0.044 Uiso 1 1 calc R . .
C13 C 0.6677(6) 0.0237(5) 0.7840(3) 0.0357(16) Uani 1 1 d . . .
C14 C 0.5946(5) -0.0112(4) 0.8122(3) 0.0290(14) Uani 1 1 d . . .
C15 C 0.5212(6) 0.0433(4) 0.8190(4) 0.0380(17) Uani 1 1 d . . .
C16 C 0.4455(6) 0.0204(5) 0.8464(3) 0.0376(17) Uani 1 1 d . . .
H16 H 0.3947 0.0561 0.8509 0.045 Uiso 1 1 calc R . .
C17 C 0.4449(5) -0.0579(4) 0.8680(3) 0.0268(13) Uani 1 1 d . . .
H17 H 0.3926 -0.0742 0.8872 0.032 Uiso 1 1 calc R . .
C18 C 0.5179(4) -0.1122(4) 0.8623(3) 0.0215(12) Uani 1 1 d . . .
C19 C 0.5967(4) -0.0915(4) 0.8307(3) 0.0210(12) Uani 1 1 d . . .
C20 C 0.4074(4) -0.2065(4) 0.9351(3) 0.0183(11) Uani 1 1 d . . .
C21 C 0.3984(4) -0.1449(4) 0.9934(3) 0.0225(12) Uani 1 1 d . . .
H21 H 0.4487 -0.0982 1.0146 0.027 Uiso 1 1 calc R . .
C22 C 0.3169(5) -0.1503(4) 1.0213(3) 0.0263(13) Uani 1 1 d . . .
H22 H 0.3119 -0.1079 1.0615 0.032 Uiso 1 1 calc R . .
C23 C 0.2426(4) -0.2184(4) 0.9898(3) 0.0254(13) Uani 1 1 d . . .
H23 H 0.1863 -0.2219 1.0083 0.030 Uiso 1 1 calc R . .
C24 C 0.2508(4) -0.2816(4) 0.9310(3) 0.0213(12) Uani 1 1 d . . .
H24 H 0.2006 -0.3286 0.9101 0.026 Uiso 1 1 calc R . .
C25 C 0.3332(4) -0.2753(4) 0.9031(3) 0.0218(12) Uani 1 1 d . . .
H25 H 0.3388 -0.3174 0.8629 0.026 Uiso 1 1 calc R . .
C30 C 0.6109(4) -0.1778(4) 0.9671(3) 0.0188(11) Uani 1 1 d . . .
C31 C 0.6655(5) -0.0946(4) 0.9913(3) 0.0251(13) Uani 1 1 d . . .
H31 H 0.6521 -0.0488 0.9708 0.030 Uiso 1 1 calc R . .
C32 C 0.7400(5) -0.0782(5) 1.0457(3) 0.0344(15) Uani 1 1 d . . .
H32 H 0.7773 -0.0214 1.0619 0.041 Uiso 1 1 calc R . .
C33 C 0.7594(5) -0.1445(5) 1.0759(3) 0.0314(15) Uani 1 1 d . . .
H33 H 0.8096 -0.1331 1.1131 0.038 Uiso 1 1 calc R . .
C34 C 0.7051(5) -0.2285(5) 1.0519(3) 0.0299(14) Uani 1 1 d . . .
H34 H 0.7188 -0.2742 1.0725 0.036 Uiso 1 1 calc R . .
C35 C 0.6314(4) -0.2447(4) 0.9982(3) 0.0247(12) Uani 1 1 d . . .
H35 H 0.5944 -0.3016 0.9821 0.030 Uiso 1 1 calc R . .
C40 C 0.7600(4) -0.3735(4) 0.8559(3) 0.0219(12) Uani 1 1 d . . .
C41 C 0.8145(4) -0.3481(4) 0.9199(3) 0.0241(12) Uani 1 1 d . . .
H41 H 0.8229 -0.2868 0.9437 0.029 Uiso 1 1 calc R . .
C42 C 0.8581(5) -0.4080(5) 0.9518(3) 0.0300(14) Uani 1 1 d . . .
H42 H 0.8953 -0.3868 0.9951 0.036 Uiso 1 1 calc R . .
C43 C 0.8452(4) -0.4966(5) 0.9186(3) 0.0274(13) Uani 1 1 d . . .
C44 C 0.7911(4) -0.5244(5) 0.8533(3) 0.0256(13) Uani 1 1 d . . .
C45 C 0.7838(5) -0.6179(4) 0.8267(3) 0.0268(13) Uani 1 1 d . . .
C46 C 0.7385(5) -0.6560(4) 0.7631(3) 0.0290(14) Uani 1 1 d . . .
H46 H 0.7347 -0.7184 0.7437 0.035 Uiso 1 1 calc R . .
C47 C 0.6971(5) -0.6011(4) 0.7265(3) 0.0275(13) Uani 1 1 d . . .
H47 H 0.6656 -0.6279 0.6821 0.033 Uiso 1 1 calc R . .
C48 C 0.7003(4) -0.5086(4) 0.7525(3) 0.0194(11) Uani 1 1 d . . .
C49 C 0.7499(4) -0.4666(4) 0.8198(3) 0.0203(12) Uani 1 1 d . . .
C50 C 0.5884(4) -0.5236(4) 0.6206(3) 0.0222(12) Uani 1 1 d . . .
C51 C 0.6401(5) -0.5755(5) 0.5772(3) 0.0280(13) Uani 1 1 d . . .
H51 H 0.7073 -0.5730 0.5895 0.034 Uiso 1 1 calc R . .
C52 C 0.5933(5) -0.6310(4) 0.5161(3) 0.0302(14) Uani 1 1 d . . .
H52 H 0.6283 -0.6668 0.4869 0.036 Uiso 1 1 calc R . .
C53 C 0.4961(5) -0.6339(5) 0.4980(3) 0.0336(15) Uani 1 1 d . . .
H53 H 0.4645 -0.6716 0.4561 0.040 Uiso 1 1 calc R . .
C54 C 0.4437(5) -0.5827(5) 0.5399(3) 0.0311(14) Uani 1 1 d . . .
H54 H 0.3767 -0.5849 0.5268 0.037 Uiso 1 1 calc R . .
C55 C 0.4899(4) -0.5278(4) 0.6015(3) 0.0241(12) Uani 1 1 d . . .
H55 H 0.4540 -0.4931 0.6306 0.029 Uiso 1 1 calc R . .
C60 C 0.7409(4) -0.3826(4) 0.6802(3) 0.0188(11) Uani 1 1 d . . .
C61 C 0.8337(4) -0.4048(4) 0.6845(3) 0.0236(12) Uani 1 1 d . . .
H61 H 0.8487 -0.4554 0.6989 0.028 Uiso 1 1 calc R . .
C62 C 0.9054(4) -0.3527(5) 0.6677(3) 0.0278(13) Uani 1 1 d . . .
H62 H 0.9687 -0.3680 0.6707 0.033 Uiso 1 1 calc R . .
C63 C 0.8839(5) -0.2799(5) 0.6471(3) 0.0331(15) Uani 1 1 d . . .
H63 H 0.9322 -0.2452 0.6352 0.040 Uiso 1 1 calc R . .
C64 C 0.7915(5) -0.2562(5) 0.6435(4) 0.0388(17) Uani 1 1 d . . .
H64 H 0.7775 -0.2045 0.6303 0.047 Uiso 1 1 calc R . .
C65 C 0.7197(5) -0.3081(5) 0.6592(3) 0.0290(14) Uani 1 1 d . . .
H65 H 0.6563 -0.2928 0.6555 0.035 Uiso 1 1 calc R . .
C70 C 0.1451(4) -0.3887(4) 0.7546(3) 0.0226(12) Uani 1 1 d . . .
C71 C 0.0732(4) -0.4175(5) 0.7849(3) 0.0246(12) Uani 1 1 d . . .
H71 H 0.0614 -0.4797 0.7798 0.030 Uiso 1 1 calc R . .
C72 C 0.0165(4) -0.3613(5) 0.8227(3) 0.0305(14) Uani 1 1 d . . .
H72 H -0.0317 -0.3854 0.8416 0.037 Uiso 1 1 calc R . .
C73 C 0.0328(4) -0.2720(5) 0.8310(3) 0.0287(14) Uani 1 1 d . . .
C74 C 0.1058(5) -0.2392(5) 0.8010(3) 0.0287(14) Uani 1 1 d . . .
C75 C 0.1137(5) -0.1456(5) 0.8149(4) 0.0344(15) Uani 1 1 d . . .
C76 C 0.1815(6) -0.1036(5) 0.7919(4) 0.0395(17) Uani 1 1 d . . .
H76 H 0.1900 -0.0404 0.8020 0.047 Uiso 1 1 calc R . .
C77 C 0.2398(5) -0.1552(5) 0.7523(3) 0.0301(14) Uani 1 1 d . . .
H77 H 0.2873 -0.1253 0.7361 0.036 Uiso 1 1 calc R . .
C78 C 0.2305(4) -0.2468(4) 0.7362(3) 0.0200(11) Uani 1 1 d . . .
C79 C 0.1625(4) -0.2950(4) 0.7624(3) 0.0205(11) Uani 1 1 d . . .
C80 C 0.3694(4) -0.2212(4) 0.6519(3) 0.0218(12) Uani 1 1 d . . .
C81 C 0.3293(5) -0.1712(5) 0.6112(3) 0.0326(15) Uani 1 1 d . . .
H81 H 0.2624 -0.1798 0.5954 0.039 Uiso 1 1 calc R . .
C82 C 0.3876(6) -0.1092(5) 0.5939(3) 0.0372(17) Uani 1 1 d . . .
H82 H 0.3603 -0.0750 0.5666 0.045 Uiso 1 1 calc R . .
C83 C 0.4858(6) -0.0968(5) 0.6164(3) 0.0344(16) Uani 1 1 d . . .
H83 H 0.5253 -0.0544 0.6042 0.041 Uiso 1 1 calc R . .
C84 C 0.5264(5) -0.1461(5) 0.6567(3) 0.0313(14) Uani 1 1 d . . .
H84 H 0.5933 -0.1372 0.6723 0.038 Uiso 1 1 calc R . .
C85 C 0.4679(4) -0.2091(4) 0.6740(3) 0.0250(13) Uani 1 1 d . . .
H85 H 0.4955 -0.2437 0.7008 0.030 Uiso 1 1 calc R . .
C90 C 0.2123(4) -0.3599(4) 0.6032(3) 0.0206(11) Uani 1 1 d . . .
C91 C 0.1284(5) -0.3243(5) 0.5860(3) 0.0337(15) Uani 1 1 d . . .
H91 H 0.1127 -0.2724 0.6152 0.040 Uiso 1 1 calc R . .
C92 C 0.0680(5) -0.3654(6) 0.5257(4) 0.0435(19) Uani 1 1 d . . .
H92 H 0.0111 -0.3413 0.5136 0.052 Uiso 1 1 calc R . .
C93 C 0.0908(5) -0.4408(6) 0.4837(4) 0.0439(19) Uani 1 1 d . . .
H93 H 0.0500 -0.4677 0.4422 0.053 Uiso 1 1 calc R . .
C94 C 0.1719(5) -0.4779(5) 0.5006(3) 0.0352(16) Uani 1 1 d . . .
H94 H 0.1853 -0.5313 0.4718 0.042 Uiso 1 1 calc R . .
C95 C 0.2342(5) -0.4367(4) 0.5603(3) 0.0270(13) Uani 1 1 d . . .
H95 H 0.2913 -0.4609 0.5716 0.032 Uiso 1 1 calc R . .
C100 C 0.2548(4) -0.6109(4) 0.6499(3) 0.0253(13) Uani 1 1 d . . .
C101 C 0.1970(5) -0.6440(5) 0.5879(4) 0.0346(15) Uani 1 1 d . . .
H101 H 0.1420 -0.6156 0.5793 0.041 Uiso 1 1 calc R . .
C102 C 0.2129(5) -0.7160(5) 0.5365(4) 0.0372(16) Uani 1 1 d . . .
H102 H 0.1694 -0.7355 0.4955 0.045 Uiso 1 1 calc R . .
C103 C 0.2923(6) -0.7574(5) 0.5470(3) 0.0365(16) Uani 1 1 d . . .
C104 C 0.3516(5) -0.7283(4) 0.6098(3) 0.0283(13) Uani 1 1 d . . .
C105 C 0.4311(5) -0.7764(4) 0.6122(3) 0.0294(14) Uani 1 1 d . . .
C106 C 0.4976(5) -0.7572(4) 0.6695(3) 0.0304(14) Uani 1 1 d . . .
H106 H 0.5524 -0.7878 0.6720 0.036 Uiso 1 1 calc R . .
C107 C 0.4814(5) -0.6904(4) 0.7244(3) 0.0249(13) Uani 1 1 d . . .
H107 H 0.5261 -0.6776 0.7647 0.030 Uiso 1 1 calc R . .
C108 C 0.4040(4) -0.6422(4) 0.7233(3) 0.0201(11) Uani 1 1 d . . .
C109 C 0.3355(4) -0.6573(4) 0.6627(3) 0.0206(11) Uani 1 1 d . . .
C110 C 0.4795(4) -0.5708(4) 0.8659(3) 0.0194(11) Uani 1 1 d . . .
C111 C 0.4826(4) -0.6478(4) 0.8879(3) 0.0244(12) Uani 1 1 d . . .
H111 H 0.4365 -0.6983 0.8670 0.029 Uiso 1 1 calc R . .
C112 C 0.5530(5) -0.6502(4) 0.9402(3) 0.0272(13) Uani 1 1 d . . .
H112 H 0.5561 -0.7025 0.9546 0.033 Uiso 1 1 calc R . .
C113 C 0.6196(5) -0.5743(5) 0.9715(3) 0.0292(14) Uani 1 1 d . . .
H113 H 0.6673 -0.5755 1.0075 0.035 Uiso 1 1 calc R . .
C114 C 0.6167(4) -0.4977(4) 0.9505(3) 0.0274(13) Uani 1 1 d . . .
H114 H 0.6619 -0.4467 0.9720 0.033 Uiso 1 1 calc R . .
C115 C 0.5459(4) -0.4965(4) 0.8968(3) 0.0232(12) Uani 1 1 d . . .
H115 H 0.5437 -0.4447 0.8816 0.028 Uiso 1 1 calc R . .
C120 C 0.2772(4) -0.6051(4) 0.8178(3) 0.0200(11) Uani 1 1 d . . .
C121 C 0.2381(5) -0.6947(5) 0.7939(3) 0.0287(14) Uani 1 1 d . . .
H121 H 0.2705 -0.7363 0.7667 0.034 Uiso 1 1 calc R . .
C122 C 0.1524(5) -0.7229(5) 0.8096(3) 0.0343(16) Uani 1 1 d . . .
H122 H 0.1261 -0.7838 0.7936 0.041 Uiso 1 1 calc R . .
C123 C 0.1053(5) -0.6612(6) 0.8491(4) 0.0404(18) Uani 1 1 d . . .
H123 H 0.0458 -0.6799 0.8591 0.049 Uiso 1 1 calc R . .
C124 C 0.1442(5) -0.5732(5) 0.8737(4) 0.0379(17) Uani 1 1 d . . .
H124 H 0.1123 -0.5319 0.9017 0.046 Uiso 1 1 calc R . .
C125 C 0.2293(5) -0.5448(5) 0.8579(3) 0.0275(13) Uani 1 1 d . . .
H125 H 0.2553 -0.4838 0.8745 0.033 Uiso 1 1 calc R . .
C130 C 0.7602(15) 0.1304(8) 0.5965(6) 0.120(7) Uani 1 1 d . . .
H13A H 0.8031 0.1031 0.5664 0.144 Uiso 1 1 calc R . .
H13B H 0.7964 0.1461 0.6424 0.144 Uiso 1 1 calc R . .
C131 C 0.9163(7) 0.1025(6) 0.8997(4) 0.049(2) Uani 1 1 d . . .
H13C H 0.8567 0.1225 0.8812 0.059 Uiso 1 1 calc R . .
H13D H 0.9449 0.0701 0.8621 0.059 Uiso 1 1 calc R . .
O1 O 0.5150(3) -0.2927(3) 0.8497(2) 0.0192(8) Uani 1 1 d . . .
O2 O 0.5742(3) -0.3904(3) 0.72868(19) 0.0212(8) Uani 1 1 d . . .
O3 O 0.3608(3) -0.3659(3) 0.6999(2) 0.0211(8) Uani 1 1 d . . .
O4 O 0.3890(3) -0.4699(3) 0.7955(2) 0.0201(8) Uani 1 1 d . . .
P1 P 0.51279(10) -0.20411(9) 0.89782(7) 0.0167(3) Uani 1 1 d . . .
P2 P 0.64476(10) -0.44802(10) 0.69928(7) 0.0190(3) Uani 1 1 d . . .
P3 P 0.29841(10) -0.30363(10) 0.67659(7) 0.0178(3) Uani 1 1 d . . .
P4 P 0.38893(10) -0.56440(10) 0.79874(7) 0.0176(3) Uani 1 1 d . . .
Hg1 Hg 0.702984(15) -0.265232(15) 0.830817(11) 0.01904(6) Uani 1 1 d . . .
Hg2 Hg 0.214470(15) -0.493668(15) 0.706549(11) 0.01955(6) Uani 1 1 d . . .
Cl1 Cl 0.9123(4) 0.1542(4) 0.7538(2) 0.153(2) Uani 1 1 d . . .
Cl2 Cl 0.7306(4) 0.2268(3) 0.5785(2) 0.1202(15) Uani 1 1 d . . .
Cl3 Cl 0.6721(4) 0.0582(3) 0.5899(3) 0.151(2) Uani 1 1 d . . .
Cl4 Cl 0.99732(14) 0.19721(16) 0.94862(11) 0.0506(5) Uani 1 1 d . . .
Cl5 Cl 0.88901(16) 0.02965(14) 0.94753(11) 0.0480(5) Uani 1 1 d . . .
Li1 Li 0.4606(6) -0.3813(6) 0.7677(4) 0.0152(17) 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 C13 1.529(10) . ?
C1 C2 1.534(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C15 1.524(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C43 1.525(9) . ?
C3 C4 1.543(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C45 1.521(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C73 1.512(9) . ?
C5 C6 1.554(12) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C75 1.527(10) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C103 1.531(10) . ?
C7 C8 1.542(12) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C105 1.519(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 C11 1.387(9) . ?
C10 C19 1.444(9) . ?
C10 Hg1 2.095(6) . ?
C11 C12 1.433(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.360(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.420(10) . ?
C14 C15 1.402(10) . ?
C14 C19 1.415(8) . ?
C15 C16 1.370(11) . ?
C16 C17 1.419(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.395(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.450(8) . ?
C18 P1 1.795(6) . ?
C20 C21 1.384(8) . ?
C20 C25 1.402(8) . ?
C20 P1 1.804(6) . ?
C21 C22 1.390(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.394(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.402(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.403(8) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C30 C31 1.393(8) . ?
C30 C35 1.404(8) . ?
C30 P1 1.806(6) . ?
C31 C32 1.400(9) . ?
C31 H31 0.9500 . ?
C32 C33 1.382(10) . ?
C32 H32 0.9500 . ?
C33 C34 1.400(10) . ?
C33 H33 0.9500 . ?
C34 C35 1.383(9) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C40 C41 1.399(8) . ?
C40 C49 1.443(9) . ?
C40 Hg1 2.094(6) . ?
C41 C42 1.421(9) . ?
C41 H41 0.9500 . ?
C42 C43 1.366(10) . ?
C42 H42 0.9500 . ?
C43 C44 1.419(9) . ?
C44 C49 1.403(8) . ?
C44 C45 1.414(9) . ?
C45 C46 1.360(9) . ?
C46 C47 1.408(9) . ?
C46 H46 0.9500 . ?
C47 C48 1.402(9) . ?
C47 H47 0.9500 . ?
C48 C49 1.448(8) . ?
C48 P2 1.794(6) . ?
C50 C55 1.396(8) . ?
C50 C51 1.400(9) . ?
C50 P2 1.800(6) . ?
C51 C52 1.393(9) . ?
C51 H51 0.9500 . ?
C52 C53 1.377(10) . ?
C52 H52 0.9500 . ?
C53 C54 1.383(10) . ?
C53 H53 0.9500 . ?
C54 C55 1.393(9) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C60 C61 1.392(8) . ?
C60 C65 1.394(9) . ?
C60 P2 1.807(6) . ?
C61 C62 1.405(9) . ?
C61 H61 0.9500 . ?
C62 C63 1.364(10) . ?
C62 H62 0.9500 . ?
C63 C64 1.395(10) . ?
C63 H63 0.9500 . ?
C64 C65 1.393(10) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
C70 C71 1.397(8) . ?
C70 C79 1.432(9) . ?
C70 Hg2 2.098(6) . ?
C71 C72 1.417(9) . ?
C71 H71 0.9500 . ?
C72 C73 1.361(10) . ?
C72 H72 0.9500 . ?
C73 C74 1.430(9) . ?
C74 C75 1.410(10) . ?
C74 C79 1.423(8) . ?
C75 C76 1.350(11) . ?
C76 C77 1.419(10) . ?
C76 H76 0.9500 . ?
C77 C78 1.377(9) . ?
C77 H77 0.9500 . ?
C78 C79 1.445(8) . ?
C78 P3 1.802(6) . ?
C80 C85 1.395(8) . ?
C80 C81 1.402(9) . ?
C80 P3 1.811(6) . ?
C81 C82 1.388(10) . ?
C81 H81 0.9500 . ?
C82 C83 1.392(11) . ?
C82 H82 0.9500 . ?
C83 C84 1.389(10) . ?
C83 H83 0.9500 . ?
C84 C85 1.400(9) . ?
C84 H84 0.9500 . ?
C85 H85 0.9500 . ?
C90 C95 1.394(9) . ?
C90 C91 1.399(9) . ?
C90 P3 1.801(6) . ?
C91 C92 1.393(10) . ?
C91 H91 0.9500 . ?
C92 C93 1.375(12) . ?
C92 H92 0.9500 . ?
C93 C94 1.376(11) . ?
C93 H93 0.9500 . ?
C94 C95 1.398(9) . ?
C94 H94 0.9500 . ?
C95 H95 0.9500 . ?
C100 C101 1.389(10) . ?
C100 C109 1.440(9) . ?
C100 Hg2 2.089(7) . ?
C101 C102 1.407(10) . ?
C101 H101 0.9500 . ?
C102 C103 1.367(11) . ?
C102 H102 0.9500 . ?
C103 C104 1.407(10) . ?
C104 C105 1.411(9) . ?
C104 C109 1.419(9) . ?
C105 C106 1.373(10) . ?
C106 C107 1.410(9) . ?
C106 H106 0.9500 . ?
C107 C108 1.386(8) . ?
C107 H107 0.9500 . ?
C108 C109 1.444(8) . ?
C108 P4 1.793(6) . ?
C110 C115 1.386(8) . ?
C110 C111 1.405(8) . ?
C110 P4 1.803(6) . ?
C111 C112 1.391(9) . ?
C111 H111 0.9500 . ?
C112 C113 1.406(10) . ?
C112 H112 0.9500 . ?
C113 C114 1.388(9) . ?
C113 H113 0.9500 . ?
C114 C115 1.409(8) . ?
C114 H114 0.9500 . ?
C115 H115 0.9500 . ?
C120 C125 1.393(9) . ?
C120 C121 1.399(9) . ?
C120 P4 1.813(6) . ?
C121 C122 1.386(9) . ?
C121 H121 0.9500 . ?
C122 C123 1.391(11) . ?
C122 H122 0.9500 . ?
C123 C124 1.377(12) . ?
C123 H123 0.9500 . ?
C124 C125 1.380(9) . ?
C124 H124 0.9500 . ?
C125 H125 0.9500 . ?
C130 Cl3 1.588(17) . ?
C130 Cl2 1.722(14) . ?
C130 H13A 0.9900 . ?
C130 H13B 0.9900 . ?
C131 Cl5 1.774(9) . ?
C131 Cl4 1.783(9) . ?
C131 H13C 0.9900 . ?
C131 H13D 0.9900 . ?
O1 P1 1.498(4) . ?
O1 Li1 1.926(10) . ?
O2 P2 1.501(4) . ?
O2 Li1 1.927(10) . ?
O3 P3 1.499(4) . ?
O3 Li1 1.941(10) . ?
O4 P4 1.501(4) . ?
O4 Li1 1.928(10) . ?

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 C1 C2 105.1(6) . . ?
C13 C1 H1A 110.7 . . ?
C2 C1 H1A 110.7 . . ?
C13 C1 H1B 110.7 . . ?
C2 C1 H1B 110.7 . . ?
H1A C1 H1B 108.8 . . ?
C15 C2 C1 105.4(7) . . ?
C15 C2 H2A 110.7 . . ?
C1 C2 H2A 110.7 . . ?
C15 C2 H2B 110.7 . . ?
C1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
C43 C3 C4 105.1(5) . . ?
C43 C3 H3A 110.7 . . ?
C4 C3 H3A 110.7 . . ?
C43 C3 H3B 110.7 . . ?
C4 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
C45 C4 C3 104.8(6) . . ?
C45 C4 H4A 110.8 . . ?
C3 C4 H4A 110.8 . . ?
C45 C4 H4B 110.8 . . ?
C3 C4 H4B 110.8 . . ?
H4A C4 H4B 108.9 . . ?
C73 C5 C6 105.6(6) . . ?
C73 C5 H5A 110.6 . . ?
C6 C5 H5A 110.6 . . ?
C73 C5 H5B 110.6 . . ?
C6 C5 H5B 110.6 . . ?
H5A C5 H5B 108.8 . . ?
C75 C6 C5 104.5(6) . . ?
C75 C6 H6A 110.9 . . ?
C5 C6 H6A 110.9 . . ?
C75 C6 H6B 110.9 . . ?
C5 C6 H6B 110.9 . . ?
H6A C6 H6B 108.9 . . ?
C103 C7 C8 105.0(6) . . ?
C103 C7 H7A 110.7 . . ?
C8 C7 H7A 110.7 . . ?
C103 C7 H7B 110.8 . . ?
C8 C7 H7B 110.8 . . ?
H7A C7 H7B 108.8 . . ?
C105 C8 C7 104.8(6) . . ?
C105 C8 H8A 110.8 . . ?
C7 C8 H8A 110.8 . . ?
C105 C8 H8B 110.8 . . ?
C7 C8 H8B 110.8 . . ?
H8A C8 H8B 108.9 . . ?
C11 C10 C19 117.1(6) . . ?
C11 C10 Hg1 112.9(5) . . ?
C19 C10 Hg1 130.0(4) . . ?
C10 C11 C12 125.2(7) . . ?
C10 C11 H11 117.4 . . ?
C12 C11 H11 117.4 . . ?
C13 C12 C11 117.3(6) . . ?
C13 C12 H12 121.4 . . ?
C11 C12 H12 121.4 . . ?
C12 C13 C14 119.8(6) . . ?
C12 C13 C1 131.7(7) . . ?
C14 C13 C1 108.5(7) . . ?
C15 C14 C19 124.8(6) . . ?
C15 C14 C13 111.8(6) . . ?
C19 C14 C13 123.4(7) . . ?
C16 C15 C14 119.7(6) . . ?
C16 C15 C2 131.2(7) . . ?
C14 C15 C2 109.1(7) . . ?
C15 C16 C17 118.2(7) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 H16 120.9 . . ?
C18 C17 C16 122.7(6) . . ?
C18 C17 H17 118.7 . . ?
C16 C17 H17 118.7 . . ?
C17 C18 C19 120.1(5) . . ?
C17 C18 P1 117.9(5) . . ?
C19 C18 P1 122.0(4) . . ?
C14 C19 C10 117.2(6) . . ?
C14 C19 C18 114.4(6) . . ?
C10 C19 C18 128.5(5) . . ?
C21 C20 C25 119.9(5) . . ?
C21 C20 P1 122.9(5) . . ?
C25 C20 P1 117.2(4) . . ?
C20 C21 C22 121.1(6) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 H21 119.4 . . ?
C21 C22 C23 119.5(6) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C22 C23 C24 120.2(6) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C25 119.8(6) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C20 C25 C24 119.5(6) . . ?
C20 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C31 C30 C35 119.1(5) . . ?
C31 C30 P1 123.1(4) . . ?
C35 C30 P1 117.7(5) . . ?
C30 C31 C32 120.3(6) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C33 C32 C31 120.0(6) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 120.1(6) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C35 C34 C33 119.8(6) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C30 120.6(6) . . ?
C34 C35 H35 119.7 . . ?
C30 C35 H35 119.7 . . ?
C41 C40 C49 117.1(5) . . ?
C41 C40 Hg1 111.6(5) . . ?
C49 C40 Hg1 131.2(4) . . ?
C40 C41 C42 124.4(6) . . ?
C40 C41 H41 117.8 . . ?
C42 C41 H41 117.8 . . ?
C43 C42 C41 118.5(6) . . ?
C43 C42 H42 120.8 . . ?
C41 C42 H42 120.8 . . ?
C42 C43 C44 118.5(6) . . ?
C42 C43 C3 132.5(6) . . ?
C44 C43 C3 109.0(6) . . ?
C49 C44 C45 124.6(6) . . ?
C49 C44 C43 124.3(6) . . ?
C45 C44 C43 111.1(6) . . ?
C46 C45 C44 119.2(6) . . ?
C46 C45 C4 131.2(6) . . ?
C44 C45 C4 109.5(6) . . ?
C45 C46 C47 118.7(6) . . ?
C45 C46 H46 120.7 . . ?
C47 C46 H46 120.7 . . ?
C48 C47 C46 123.2(6) . . ?
C48 C47 H47 118.4 . . ?
C46 C47 H47 118.4 . . ?
C47 C48 C49 119.0(5) . . ?
C47 C48 P2 117.7(5) . . ?
C49 C48 P2 123.3(5) . . ?
C44 C49 C40 117.1(5) . . ?
C44 C49 C48 115.2(6) . . ?
C40 C49 C48 127.7(5) . . ?
C55 C50 C51 119.0(6) . . ?
C55 C50 P2 118.4(5) . . ?
C51 C50 P2 122.6(5) . . ?
C52 C51 C50 120.2(6) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C53 C52 C51 119.8(6) . . ?
C53 C52 H52 120.1 . . ?
C51 C52 H52 120.1 . . ?
C52 C53 C54 120.9(6) . . ?
C52 C53 H53 119.5 . . ?
C54 C53 H53 119.5 . . ?
C53 C54 C55 119.5(6) . . ?
C53 C54 H54 120.2 . . ?
C55 C54 H54 120.2 . . ?
C54 C55 C50 120.4(6) . . ?
C54 C55 H55 119.8 . . ?
C50 C55 H55 119.8 . . ?
C61 C60 C65 119.4(6) . . ?
C61 C60 P2 122.6(5) . . ?
C65 C60 P2 117.9(4) . . ?
C60 C61 C62 120.3(6) . . ?
C60 C61 H61 119.8 . . ?
C62 C61 H61 119.8 . . ?
C63 C62 C61 119.8(6) . . ?
C63 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C62 C63 C64 120.5(6) . . ?
C62 C63 H63 119.8 . . ?
C64 C63 H63 119.8 . . ?
C65 C64 C63 120.1(7) . . ?
C65 C64 H64 119.9 . . ?
C63 C64 H64 119.9 . . ?
C64 C65 C60 119.8(6) . . ?
C64 C65 H65 120.1 . . ?
C60 C65 H65 120.1 . . ?
C71 C70 C79 117.1(6) . . ?
C71 C70 Hg2 112.5(5) . . ?
C79 C70 Hg2 130.3(4) . . ?
C70 C71 C72 125.1(6) . . ?
C70 C71 H71 117.4 . . ?
C72 C71 H71 117.4 . . ?
C73 C72 C71 118.4(6) . . ?
C73 C72 H72 120.8 . . ?
C71 C72 H72 120.8 . . ?
C72 C73 C74 118.5(6) . . ?
C72 C73 C5 132.4(6) . . ?
C74 C73 C5 109.0(6) . . ?
C75 C74 C79 125.2(6) . . ?
C75 C74 C73 111.2(6) . . ?
C79 C74 C73 123.6(6) . . ?
C76 C75 C74 118.8(6) . . ?
C76 C75 C6 131.6(7) . . ?
C74 C75 C6 109.6(7) . . ?
C75 C76 C77 119.0(7) . . ?
C75 C76 H76 120.5 . . ?
C77 C76 H76 120.5 . . ?
C78 C77 C76 122.8(6) . . ?
C78 C77 H77 118.6 . . ?
C76 C77 H77 118.6 . . ?
C77 C78 C79 120.5(5) . . ?
C77 C78 P3 117.5(5) . . ?
C79 C78 P3 121.8(4) . . ?
C74 C79 C70 117.1(6) . . ?
C74 C79 C78 113.6(6) . . ?
C70 C79 C78 129.3(5) . . ?
C85 C80 C81 119.6(6) . . ?
C85 C80 P3 117.8(5) . . ?
C81 C80 P3 122.6(5) . . ?
C82 C81 C80 119.9(7) . . ?
C82 C81 H81 120.1 . . ?
C80 C81 H81 120.1 . . ?
C83 C82 C81 120.4(7) . . ?
C83 C82 H82 119.8 . . ?
C81 C82 H82 119.8 . . ?
C82 C83 C84 120.3(6) . . ?
C82 C83 H83 119.9 . . ?
C84 C83 H83 119.9 . . ?
C83 C84 C85 119.6(7) . . ?
C83 C84 H84 120.2 . . ?
C85 C84 H84 120.2 . . ?
C80 C85 C84 120.3(6) . . ?
C80 C85 H85 119.8 . . ?
C84 C85 H85 119.8 . . ?
C95 C90 C91 119.8(6) . . ?
C95 C90 P3 118.5(5) . . ?
C91 C90 P3 121.5(5) . . ?
C92 C91 C90 119.7(7) . . ?
C92 C91 H91 120.1 . . ?
C90 C91 H91 120.1 . . ?
C93 C92 C91 119.9(7) . . ?
C93 C92 H92 120.1 . . ?
C91 C92 H92 120.1 . . ?
C94 C93 C92 121.2(7) . . ?
C94 C93 H93 119.4 . . ?
C92 C93 H93 119.4 . . ?
C93 C94 C95 119.7(7) . . ?
C93 C94 H94 120.2 . . ?
C95 C94 H94 120.2 . . ?
C90 C95 C94 119.7(6) . . ?
C90 C95 H95 120.1 . . ?
C94 C95 H95 120.1 . . ?
C101 C100 C109 116.2(6) . . ?
C101 C100 Hg2 112.9(5) . . ?
C109 C100 Hg2 130.6(5) . . ?
C100 C101 C102 125.6(7) . . ?
C100 C101 H101 117.2 . . ?
C102 C101 H101 117.2 . . ?
C103 C102 C101 118.5(7) . . ?
C103 C102 H102 120.7 . . ?
C101 C102 H102 120.7 . . ?
C102 C103 C104 118.1(7) . . ?
C102 C103 C7 132.6(7) . . ?
C104 C103 C7 109.2(7) . . ?
C103 C104 C105 111.2(6) . . ?
C103 C104 C109 124.2(6) . . ?
C105 C104 C109 124.6(6) . . ?
C106 C105 C104 119.8(6) . . ?
C106 C105 C8 130.4(6) . . ?
C104 C105 C8 109.8(6) . . ?
C105 C106 C107 117.3(6) . . ?
C105 C106 H106 121.4 . . ?
C107 C106 H106 121.4 . . ?
C108 C107 C106 124.0(6) . . ?
C108 C107 H107 118.0 . . ?
C106 C107 H107 118.0 . . ?
C107 C108 C109 120.1(6) . . ?
C107 C108 P4 118.7(5) . . ?
C109 C108 P4 121.1(4) . . ?
C104 C109 C100 117.2(6) . . ?
C104 C109 C108 114.0(5) . . ?
C100 C109 C108 128.8(5) . . ?
C115 C110 C111 120.2(5) . . ?
C115 C110 P4 118.2(4) . . ?
C111 C110 P4 121.6(5) . . ?
C112 C111 C110 120.1(6) . . ?
C112 C111 H111 119.9 . . ?
C110 C111 H111 119.9 . . ?
C111 C112 C113 119.3(6) . . ?
C111 C112 H112 120.4 . . ?
C113 C112 H112 120.4 . . ?
C114 C113 C112 121.1(6) . . ?
C114 C113 H113 119.5 . . ?
C112 C113 H113 119.5 . . ?
C113 C114 C115 119.1(6) . . ?
C113 C114 H114 120.4 . . ?
C115 C114 H114 120.4 . . ?
C110 C115 C114 120.2(6) . . ?
C110 C115 H115 119.9 . . ?
C114 C115 H115 119.9 . . ?
C125 C120 C121 119.2(6) . . ?
C125 C120 P4 118.5(5) . . ?
C121 C120 P4 122.2(5) . . ?
C122 C121 C120 120.4(7) . . ?
C122 C121 H121 119.8 . . ?
C120 C121 H121 119.8 . . ?
C121 C122 C123 119.3(7) . . ?
C121 C122 H122 120.3 . . ?
C123 C122 H122 120.3 . . ?
C124 C123 C122 120.6(7) . . ?
C124 C123 H123 119.7 . . ?
C122 C123 H123 119.7 . . ?
C123 C124 C125 120.2(7) . . ?
C123 C124 H124 119.9 . . ?
C125 C124 H124 119.9 . . ?
C124 C125 C120 120.3(7) . . ?
C124 C125 H125 119.9 . . ?
C120 C125 H125 119.9 . . ?
Cl3 C130 Cl2 115.0(12) . . ?
Cl3 C130 H13A 108.5 . . ?
Cl2 C130 H13A 108.5 . . ?
Cl3 C130 H13B 108.5 . . ?
Cl2 C130 H13B 108.5 . . ?
H13A C130 H13B 107.5 . . ?
Cl5 C131 Cl4 111.2(5) . . ?
Cl5 C131 H13C 109.4 . . ?
Cl4 C131 H13C 109.4 . . ?
Cl5 C131 H13D 109.4 . . ?
Cl4 C131 H13D 109.4 . . ?
H13C C131 H13D 108.0 . . ?
P1 O1 Li1 149.3(4) . . ?
P2 O2 Li1 148.3(4) . . ?
P3 O3 Li1 147.0(4) . . ?
P4 O4 Li1 141.0(4) . . ?
O1 P1 C18 114.1(3) . . ?
O1 P1 C20 110.0(3) . . ?
C18 P1 C20 109.4(3) . . ?
O1 P1 C30 112.2(3) . . ?
C18 P1 C30 106.2(3) . . ?
C20 P1 C30 104.4(3) . . ?
O2 P2 C48 114.0(3) . . ?
O2 P2 C50 110.0(3) . . ?
C48 P2 C50 110.1(3) . . ?
O2 P2 C60 111.3(3) . . ?
C48 P2 C60 106.1(3) . . ?
C50 P2 C60 104.8(3) . . ?
O3 P3 C90 112.2(3) . . ?
O3 P3 C78 114.7(3) . . ?
C90 P3 C78 105.7(3) . . ?
O3 P3 C80 110.2(3) . . ?
C90 P3 C80 104.7(3) . . ?
C78 P3 C80 108.7(3) . . ?
O4 P4 C108 114.5(2) . . ?
O4 P4 C110 110.3(3) . . ?
C108 P4 C110 109.5(3) . . ?
O4 P4 C120 111.0(3) . . ?
C108 P4 C120 105.9(3) . . ?
C110 P4 C120 105.2(3) . . ?
C40 Hg1 C10 167.5(2) . . ?
C100 Hg2 C70 168.1(2) . . ?
O1 Li1 O4 103.7(5) . . ?
O1 Li1 O2 97.9(4) . . ?
O4 Li1 O2 129.0(5) . . ?
O1 Li1 O3 125.6(5) . . ?
O4 Li1 O3 98.0(4) . . ?
O2 Li1 O3 106.0(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         4.052
_refine_diff_density_min         -3.526
_refine_diff_density_rms         0.183
####################################################################### 
# 
# 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_shelxl_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1897903'
loop_
_audit_author_name
_audit_author_address
'Enno Lork'
;Bremen University
Germany
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H18 Cl3 O P Sn'
_chemical_formula_weight         578.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9934(4)
_cell_length_b                   9.5252(4)
_cell_length_c                   14.9658(6)
_cell_angle_alpha                102.2000(10)
_cell_angle_beta                 98.3920(10)
_cell_angle_gamma                113.2840(10)
_cell_volume                     1112.79(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9901
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      31.61

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             572
_exptl_absorpt_coefficient_mu    1.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4419
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture D8 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43017
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         31.61
_reflns_number_total             7411
_reflns_number_gt                6826
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0192P)²+0.9080P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         7411
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0573
_refine_ls_wR_factor_gt          0.0557
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1389(2) 0.31502(19) -0.02011(11) 0.0156(3) Uani 1 1 d . . .
H1A H 0.1373 0.2823 -0.0877 0.019 Uiso 1 1 calc R . .
H1B H 0.0290 0.3121 -0.0155 0.019 Uiso 1 1 calc R . .
C2 C 0.1779(2) 0.20376(19) 0.03189(11) 0.0144(3) Uani 1 1 d . . .
H2A H 0.0868 0.1523 0.0611 0.017 Uiso 1 1 calc R . .
H2B H 0.1919 0.1195 -0.0125 0.017 Uiso 1 1 calc R . .
C10 C 0.56215(18) 0.75803(17) 0.15045(10) 0.0097(2) Uani 1 1 d . . .
C11 C 0.4528(2) 0.76193(18) 0.07635(11) 0.0130(3) Uani 1 1 d . . .
H11 H 0.4751 0.8623 0.0656 0.016 Uiso 1 1 calc R . .
C12 C 0.3102(2) 0.62556(19) 0.01598(11) 0.0139(3) Uani 1 1 d . . .
H12 H 0.2379 0.6345 -0.0332 0.017 Uiso 1 1 calc R . .
C13 C 0.27896(19) 0.48024(18) 0.03010(10) 0.0116(3) Uani 1 1 d . . .
C14 C 0.38999(18) 0.47200(17) 0.10383(10) 0.0093(2) Uani 1 1 d . . .
C15 C 0.33932(19) 0.31283(17) 0.10670(10) 0.0109(3) Uani 1 1 d . . .
C16 C 0.4340(2) 0.28038(18) 0.17245(11) 0.0128(3) Uani 1 1 d . . .
H16 H 0.4057 0.1737 0.1737 0.015 Uiso 1 1 calc R . .
C17 C 0.57478(19) 0.41074(18) 0.23816(11) 0.0120(3) Uani 1 1 d . . .
H17 H 0.6402 0.3895 0.2845 0.014 Uiso 1 1 calc R . .
C18 C 0.62277(18) 0.56908(17) 0.23852(10) 0.0093(2) Uani 1 1 d . . .
C19 C 0.53200(18) 0.60655(17) 0.16714(10) 0.0084(2) Uani 1 1 d . . .
C20 C 0.98527(18) 0.72007(18) 0.32451(11) 0.0107(3) Uani 1 1 d . . .
C21 C 0.9987(2) 0.6123(2) 0.25113(11) 0.0173(3) Uani 1 1 d . . .
H21 H 0.9010 0.5289 0.2065 0.021 Uiso 1 1 calc R . .
C22 C 1.1568(2) 0.6279(3) 0.24366(12) 0.0237(4) Uani 1 1 d . . .
H22 H 1.1670 0.5546 0.1938 0.028 Uiso 1 1 calc R . .
C23 C 1.2990(2) 0.7500(2) 0.30879(13) 0.0220(4) Uani 1 1 d . . .
H23 H 1.4065 0.7612 0.3028 0.026 Uiso 1 1 calc R . .
C24 C 1.2854(2) 0.8559(2) 0.38257(14) 0.0227(4) Uani 1 1 d . . .
H24 H 1.3834 0.9389 0.4272 0.027 Uiso 1 1 calc R . .
C25 C 1.1291(2) 0.8410(2) 0.39140(13) 0.0184(3) Uani 1 1 d . . .
H25 H 1.1196 0.9126 0.4426 0.022 Uiso 1 1 calc R . .
C30 C 0.75781(18) 0.66933(17) 0.44388(10) 0.0097(3) Uani 1 1 d . . .
C31 C 0.82395(19) 0.57471(19) 0.47769(11) 0.0130(3) Uani 1 1 d . . .
H31 H 0.8878 0.5350 0.4440 0.016 Uiso 1 1 calc R . .
C32 C 0.7959(2) 0.5389(2) 0.56088(11) 0.0154(3) Uani 1 1 d . . .
H32 H 0.8391 0.4732 0.5836 0.018 Uiso 1 1 calc R . .
C33 C 0.7049(2) 0.59907(19) 0.61071(11) 0.0150(3) Uani 1 1 d . . .
H33 H 0.6873 0.5755 0.6680 0.018 Uiso 1 1 calc R . .
C34 C 0.6392(2) 0.69354(19) 0.57756(11) 0.0143(3) Uani 1 1 d . . .
H34 H 0.5770 0.7343 0.6121 0.017 Uiso 1 1 calc R . .
C35 C 0.66465(19) 0.72832(18) 0.49394(11) 0.0121(3) Uani 1 1 d . . .
H35 H 0.6189 0.7920 0.4708 0.015 Uiso 1 1 calc R . .
O1 O 0.79017(14) 0.87999(12) 0.34562(7) 0.01072(19) Uani 1 1 d . . .
P1 P 0.78928(5) 0.71728(4) 0.33676(3) 0.00810(7) Uani 1 1 d . . .
Cl1 Cl 0.74979(6) 1.14135(5) 0.12783(3) 0.01908(8) Uani 1 1 d . . .
Cl2 Cl 1.03437(5) 1.03621(5) 0.23088(3) 0.01606(7) Uani 1 1 d . . .
Cl3 Cl 0.71404(6) 1.15635(5) 0.35257(3) 0.01815(8) Uani 1 1 d . . .
Sn1 Sn 0.759359(12) 0.983883(11) 0.234381(7) 0.00955(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
C1 C13 1.512(2) . ?
C1 C2 1.554(2) . ?
C2 C15 1.510(2) . ?
C10 C11 1.388(2) . ?
C10 C19 1.4424(19) . ?
C10 Sn1 2.1313(14) . ?
C11 C12 1.413(2) . ?
C12 C13 1.369(2) . ?
C13 C14 1.414(2) . ?
C14 C15 1.413(2) . ?
C14 C19 1.418(2) . ?
C15 C16 1.371(2) . ?
C16 C17 1.410(2) . ?
C17 C18 1.394(2) . ?
C18 C19 1.439(2) . ?
C18 P1 1.7904(15) . ?
C20 C21 1.391(2) . ?
C20 C25 1.400(2) . ?
C20 P1 1.7890(15) . ?
C21 C22 1.393(2) . ?
C22 C23 1.386(3) . ?
C23 C24 1.385(3) . ?
C24 C25 1.384(2) . ?
C30 C31 1.397(2) . ?
C30 C35 1.399(2) . ?
C30 P1 1.7884(15) . ?
C31 C32 1.390(2) . ?
C32 C33 1.387(2) . ?
C33 C34 1.388(2) . ?
C34 C35 1.388(2) . ?
O1 P1 1.5241(11) . ?
O1 Sn1 2.1461(10) . ?
Cl1 Sn1 2.4234(4) . ?
Cl2 Sn1 2.3330(4) . ?
Cl3 Sn1 2.3463(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
C13 C1 C2 104.87(12) . . ?
C15 C2 C1 104.86(12) . . ?
C11 C10 C19 118.95(13) . . ?
C11 C10 Sn1 115.75(10) . . ?
C19 C10 Sn1 125.26(10) . . ?
C10 C11 C12 123.90(14) . . ?
C13 C12 C11 118.34(14) . . ?
C12 C13 C14 119.06(14) . . ?
C12 C13 C1 131.39(14) . . ?
C14 C13 C1 109.55(13) . . ?
C15 C14 C13 111.05(13) . . ?
C15 C14 C19 124.73(13) . . ?
C13 C14 C19 124.21(13) . . ?
C16 C15 C14 119.56(14) . . ?
C16 C15 C2 130.81(14) . . ?
C14 C15 C2 109.63(13) . . ?
C15 C16 C17 117.75(13) . . ?
C18 C17 C16 123.33(14) . . ?
C17 C18 C19 120.36(13) . . ?
C17 C18 P1 115.80(11) . . ?
C19 C18 P1 123.66(11) . . ?
C14 C19 C18 114.11(12) . . ?
C14 C19 C10 115.51(13) . . ?
C18 C19 C10 130.37(13) . . ?
C21 C20 C25 120.26(15) . . ?
C21 C20 P1 122.96(12) . . ?
C25 C20 P1 116.75(12) . . ?
C20 C21 C22 119.44(16) . . ?
C23 C22 C21 120.09(17) . . ?
C24 C23 C22 120.43(16) . . ?
C25 C24 C23 120.13(17) . . ?
C24 C25 C20 119.64(16) . . ?
C31 C30 C35 120.00(14) . . ?
C31 C30 P1 121.28(11) . . ?
C35 C30 P1 118.72(11) . . ?
C32 C31 C30 119.68(14) . . ?
C33 C32 C31 120.06(15) . . ?
C32 C33 C34 120.50(15) . . ?
C35 C34 C33 119.92(15) . . ?
C34 C35 C30 119.84(14) . . ?
P1 O1 Sn1 127.75(6) . . ?
O1 P1 C30 107.76(6) . . ?
O1 P1 C20 112.05(7) . . ?
C30 P1 C20 106.91(7) . . ?
O1 P1 C18 109.73(6) . . ?
C30 P1 C18 109.91(7) . . ?
C20 P1 C18 110.40(7) . . ?
C10 Sn1 O1 89.20(5) . . ?
C10 Sn1 Cl2 118.75(4) . . ?
O1 Sn1 Cl2 87.34(3) . . ?
C10 Sn1 Cl3 121.39(4) . . ?
O1 Sn1 Cl3 82.17(3) . . ?
Cl2 Sn1 Cl3 118.568(15) . . ?
C10 Sn1 Cl1 99.45(4) . . ?
O1 Sn1 Cl1 170.97(3) . . ?
Cl2 Sn1 Cl1 90.725(15) . . ?
Cl3 Sn1 Cl1 91.046(14) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        31.61
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.636
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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_shelxl_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1897904'
loop_
_audit_author_name
_audit_author_address
'Enno Lork'
;Bremen University
Germany
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H34 Cl3 O3 P Sn'
_chemical_formula_weight         722.60

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8921(3)
_cell_length_b                   10.4750(4)
_cell_length_c                   16.9858(7)
_cell_angle_alpha                85.2910(10)
_cell_angle_beta                 84.1610(10)
_cell_angle_gamma                72.3330(10)
_cell_volume                     1497.51(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9688
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      30.56

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6472
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture D8 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48875
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         30.58
_reflns_number_total             9171
_reflns_number_gt                8229
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0168P)²+1.4414P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         9171
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0546
_refine_ls_wR_factor_gt          0.0523
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.005
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6904(2) 0.56553(17) 0.54081(10) 0.0160(3) Uani 1 1 d . . .
H1A H 0.6330 0.5255 0.5841 0.019 Uiso 1 1 calc R . .
H1B H 0.7701 0.5970 0.5636 0.019 Uiso 1 1 calc R . .
C2 C 0.7703(2) 0.46245(17) 0.47715(10) 0.0162(3) Uani 1 1 d . . .
H2A H 0.8864 0.4463 0.4718 0.019 Uiso 1 1 calc R . .
H2B H 0.7481 0.3760 0.4914 0.019 Uiso 1 1 calc R . .
C4 C -0.1205(2) 0.9870(2) 0.34585(15) 0.0298(5) Uani 1 1 d . . .
H4A H -0.1569 1.0525 0.3012 0.036 Uiso 1 1 calc R . .
H4B H -0.1434 1.0351 0.3955 0.036 Uiso 1 1 calc R . .
C5 C -0.2003(2) 0.87760(19) 0.35128(12) 0.0226(4) Uani 1 1 d . . .
H5A H -0.2380 0.8696 0.2996 0.027 Uiso 1 1 calc R . .
H5B H -0.2916 0.8967 0.3916 0.027 Uiso 1 1 calc R . .
C6 C -0.0722(2) 0.74843(18) 0.37521(11) 0.0174(3) Uani 1 1 d . . .
H6A H -0.1051 0.7082 0.4263 0.021 Uiso 1 1 calc R . .
H6B H -0.0504 0.6818 0.3342 0.021 Uiso 1 1 calc R . .
C7 C 0.07219(19) 0.79396(16) 0.38245(10) 0.0135(3) Uani 1 1 d . . .
H7A H 0.0800 0.8107 0.4382 0.016 Uiso 1 1 calc R . .
H7B H 0.1702 0.7252 0.3636 0.016 Uiso 1 1 calc R . .
C10 C 0.38809(18) 0.86134(15) 0.38535(9) 0.0100(3) Uani 1 1 d . . .
C11 C 0.38524(19) 0.88848(16) 0.46405(9) 0.0129(3) Uani 1 1 d . . .
H11 H 0.3170 0.9721 0.4811 0.016 Uiso 1 1 calc R . .
C12 C 0.4771(2) 0.80026(17) 0.52077(9) 0.0145(3) Uani 1 1 d . . .
H12 H 0.4699 0.8239 0.5741 0.017 Uiso 1 1 calc R . .
C13 C 0.57650(19) 0.67991(16) 0.49660(9) 0.0121(3) Uani 1 1 d . . .
C14 C 0.58410(18) 0.64993(15) 0.41643(9) 0.0103(3) Uani 1 1 d . . .
C15 C 0.69848(18) 0.52549(16) 0.40098(10) 0.0124(3) Uani 1 1 d . . .
C16 C 0.72922(19) 0.48254(16) 0.32538(10) 0.0145(3) Uani 1 1 d . . .
H16 H 0.8081 0.4007 0.3134 0.017 Uiso 1 1 calc R . .
C17 C 0.63994(19) 0.56367(16) 0.26590(10) 0.0132(3) Uani 1 1 d . . .
H17 H 0.6606 0.5348 0.2132 0.016 Uiso 1 1 calc R . .
C18 C 0.52306(18) 0.68401(15) 0.28052(9) 0.0099(3) Uani 1 1 d . . .
C19 C 0.49296(17) 0.73573(15) 0.35856(9) 0.0088(3) Uani 1 1 d . . .
C20 C 0.26287(18) 0.66796(16) 0.19527(9) 0.0111(3) Uani 1 1 d . . .
C21 C 0.2915(2) 0.53302(17) 0.22040(10) 0.0153(3) Uani 1 1 d . . .
H21 H 0.3873 0.4859 0.2434 0.018 Uiso 1 1 calc R . .
C22 C 0.1799(2) 0.46745(18) 0.21179(11) 0.0200(4) Uani 1 1 d . . .
H22 H 0.1995 0.3757 0.2291 0.024 Uiso 1 1 calc R . .
C23 C 0.0403(2) 0.5356(2) 0.17807(11) 0.0206(4) Uani 1 1 d . . .
H23 H -0.0342 0.4899 0.1708 0.025 Uiso 1 1 calc R . .
C24 C 0.0093(2) 0.6708(2) 0.15494(11) 0.0214(4) Uani 1 1 d . . .
H24 H -0.0877 0.7179 0.1330 0.026 Uiso 1 1 calc R . .
C25 C 0.1194(2) 0.73753(18) 0.16376(10) 0.0173(3) Uani 1 1 d . . .
H25 H 0.0972 0.8302 0.1484 0.021 Uiso 1 1 calc R . .
C30 C 0.52248(18) 0.74977(16) 0.10882(9) 0.0117(3) Uani 1 1 d . . .
C31 C 0.5544(2) 0.64356(17) 0.05932(10) 0.0159(3) Uani 1 1 d . . .
H31 H 0.5157 0.5693 0.0747 0.019 Uiso 1 1 calc R . .
C32 C 0.6433(2) 0.64652(19) -0.01289(10) 0.0202(4) Uani 1 1 d . . .
H32 H 0.6651 0.5741 -0.0467 0.024 Uiso 1 1 calc R . .
C33 C 0.6999(2) 0.75453(19) -0.03562(10) 0.0200(4) Uani 1 1 d . . .
H33 H 0.7599 0.7564 -0.0851 0.024 Uiso 1 1 calc R . .
C35 C 0.6691(2) 0.85988(19) 0.01381(11) 0.0212(4) Uani 1 1 d . . .
H35 H 0.7086 0.9337 -0.0017 0.025 Uiso 1 1 calc R . .
C36 C 0.5805(2) 0.85795(17) 0.08612(10) 0.0171(3) Uani 1 1 d . . .
H36 H 0.5595 0.9303 0.1199 0.021 Uiso 1 1 calc R . .
C40 C 0.6912(2) 0.26830(19) 0.15465(11) 0.0210(4) Uani 1 1 d . . .
H40A H 0.5762 0.3113 0.1514 0.025 Uiso 1 1 calc R . .
H40B H 0.7119 0.2469 0.2111 0.025 Uiso 1 1 calc R . .
C41 C 0.7461(2) 0.1405(2) 0.10883(13) 0.0285(4) Uani 1 1 d . . .
H41A H 0.6595 0.1307 0.0799 0.034 Uiso 1 1 calc R . .
H41B H 0.7831 0.0603 0.1450 0.034 Uiso 1 1 calc R . .
C42 C 0.8823(2) 0.1599(2) 0.05116(11) 0.0251(4) Uani 1 1 d . . .
H42A H 0.9859 0.1178 0.0732 0.030 Uiso 1 1 calc R . .
H42B H 0.8829 0.1222 -0.0005 0.030 Uiso 1 1 calc R . .
C43 C 0.8438(2) 0.3112(2) 0.04329(11) 0.0243(4) Uani 1 1 d . . .
H43A H 0.9408 0.3378 0.0275 0.029 Uiso 1 1 calc R . .
H43B H 0.7667 0.3495 0.0031 0.029 Uiso 1 1 calc R . .
Cl1 Cl 0.10940(5) 1.17021(4) 0.41680(2) 0.01897(8) Uani 1 1 d . . .
Cl2 Cl 0.06731(4) 1.16579(4) 0.22439(2) 0.01319(7) Uani 1 1 d . . .
Cl3 Cl 0.44840(5) 1.13032(4) 0.27249(2) 0.01676(8) Uani 1 1 d . . .
O1 O 0.31570(13) 0.90564(11) 0.21187(7) 0.0121(2) Uani 1 1 d . . .
O2 O 0.04832(13) 0.91703(11) 0.33286(7) 0.0124(2) Uani 1 1 d . . .
O3 O 0.77799(16) 0.35652(13) 0.11964(8) 0.0228(3) Uani 1 1 d . . .
P1 P 0.40312(5) 0.75870(4) 0.20136(2) 0.00896(7) Uani 1 1 d . . .
Sn1 Sn 0.246066(12) 1.022856(10) 0.312431(6) 0.00842(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
C1 C13 1.515(2) . ?
C1 C2 1.552(2) . ?
C2 C15 1.513(2) . ?
C4 O2 1.460(2) . ?
C4 C5 1.513(3) . ?
C5 C6 1.537(3) . ?
C6 C7 1.518(2) . ?
C7 O2 1.4521(19) . ?
C10 C11 1.386(2) . ?
C10 C19 1.441(2) . ?
C10 Sn1 2.1607(15) . ?
C11 C12 1.416(2) . ?
C12 C13 1.369(2) . ?
C13 C14 1.413(2) . ?
C14 C15 1.414(2) . ?
C14 C19 1.416(2) . ?
C15 C16 1.369(2) . ?
C16 C17 1.409(2) . ?
C17 C18 1.391(2) . ?
C18 C19 1.442(2) . ?
C18 P1 1.7804(16) . ?
C20 C21 1.396(2) . ?
C20 C25 1.399(2) . ?
C20 P1 1.7977(16) . ?
C21 C22 1.392(2) . ?
C22 C23 1.385(3) . ?
C23 C24 1.390(3) . ?
C24 C25 1.390(2) . ?
C30 C31 1.392(2) . ?
C30 C36 1.393(2) . ?
C30 P1 1.7973(15) . ?
C31 C32 1.393(2) . ?
C32 C33 1.385(3) . ?
C33 C35 1.386(3) . ?
C35 C36 1.393(2) . ?
C40 O3 1.432(2) . ?
C40 C41 1.527(3) . ?
C41 C42 1.530(3) . ?
C42 C43 1.515(3) . ?
C43 O3 1.424(2) . ?
Cl1 Sn1 2.4238(4) . ?
Cl2 Sn1 2.3824(4) . ?
Cl3 Sn1 2.4124(4) . ?
O1 P1 1.5152(11) . ?
O1 Sn1 2.1158(11) . ?
O2 Sn1 2.3317(11) . ?

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 C1 C2 104.62(13) . . ?
C15 C2 C1 105.22(13) . . ?
O2 C4 C5 104.80(15) . . ?
C4 C5 C6 105.16(14) . . ?
C7 C6 C5 104.25(13) . . ?
O2 C7 C6 105.19(13) . . ?
C11 C10 C19 118.18(14) . . ?
C11 C10 Sn1 115.24(11) . . ?
C19 C10 Sn1 126.36(11) . . ?
C10 C11 C12 124.52(15) . . ?
C13 C12 C11 118.17(14) . . ?
C12 C13 C14 118.76(14) . . ?
C12 C13 C1 131.58(15) . . ?
C14 C13 C1 109.64(14) . . ?
C13 C14 C15 111.17(14) . . ?
C13 C14 C19 124.30(14) . . ?
C15 C14 C19 124.49(14) . . ?
C16 C15 C14 119.77(15) . . ?
C16 C15 C2 130.93(15) . . ?
C14 C15 C2 109.29(14) . . ?
C15 C16 C17 117.81(15) . . ?
C18 C17 C16 123.20(15) . . ?
C17 C18 C19 120.51(14) . . ?
C17 C18 P1 116.32(12) . . ?
C19 C18 P1 122.88(11) . . ?
C14 C19 C10 116.06(13) . . ?
C14 C19 C18 114.10(13) . . ?
C10 C19 C18 129.83(14) . . ?
C21 C20 C25 119.50(15) . . ?
C21 C20 P1 122.95(12) . . ?
C25 C20 P1 117.55(12) . . ?
C22 C21 C20 120.08(16) . . ?
C23 C22 C21 120.19(17) . . ?
C22 C23 C24 119.95(16) . . ?
C23 C24 C25 120.33(17) . . ?
C24 C25 C20 119.89(17) . . ?
C31 C30 C36 119.83(15) . . ?
C31 C30 P1 123.31(12) . . ?
C36 C30 P1 116.83(12) . . ?
C30 C31 C32 119.79(16) . . ?
C33 C32 C31 120.32(16) . . ?
C32 C33 C35 119.95(16) . . ?
C33 C35 C36 120.21(16) . . ?
C35 C36 C30 119.90(16) . . ?
O3 C40 C41 107.51(15) . . ?
C40 C41 C42 104.14(15) . . ?
C43 C42 C41 102.15(15) . . ?
O3 C43 C42 105.44(15) . . ?
P1 O1 Sn1 132.96(7) . . ?
C7 O2 C4 104.76(12) . . ?
C7 O2 Sn1 120.30(9) . . ?
C4 O2 Sn1 124.45(10) . . ?
C43 O3 C40 107.86(14) . . ?
O1 P1 C18 112.65(7) . . ?
O1 P1 C30 106.83(7) . . ?
C18 P1 C30 110.59(7) . . ?
O1 P1 C20 109.56(7) . . ?
C18 P1 C20 108.53(7) . . ?
C30 P1 C20 108.61(7) . . ?
O1 Sn1 C10 90.93(5) . . ?
O1 Sn1 O2 83.31(4) . . ?
C10 Sn1 O2 87.44(5) . . ?
O1 Sn1 Cl2 81.69(3) . . ?
C10 Sn1 Cl2 167.99(4) . . ?
O2 Sn1 Cl2 82.32(3) . . ?
O1 Sn1 Cl3 90.15(3) . . ?
C10 Sn1 Cl3 96.79(4) . . ?
O2 Sn1 Cl3 172.28(3) . . ?
Cl2 Sn1 Cl3 92.705(14) . . ?
O1 Sn1 Cl1 167.44(3) . . ?
C10 Sn1 Cl1 98.23(4) . . ?
O2 Sn1 Cl1 88.49(3) . . ?
Cl2 Sn1 Cl1 87.803(14) . . ?
Cl3 Sn1 Cl1 97.247(15) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        30.58
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.094
####################################################################### 
# 
# 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_shelxl_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1897902'
loop_
_audit_author_name
_audit_author_address
'Enno Lork'
;Bremen University
Germany
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H18 Cl Hg O P'
_chemical_formula_weight         589.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   10.8014(4)
_cell_length_b                   10.3777(4)
_cell_length_c                   18.5406(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.6550(10)
_cell_angle_gamma                90.00
_cell_volume                     2001.19(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9677
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      30.55

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_exptl_absorpt_coefficient_mu    7.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2649
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture D8 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            76418
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         30.57
_reflns_number_total             6128
_reflns_number_gt                5850
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0187P)²+2.9389P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         6128
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0198
_refine_ls_wR_factor_ref         0.0516
_refine_ls_wR_factor_gt          0.0511
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_restrained_S_all      1.176
_refine_ls_shift/su_max          0.004
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 0.533334(7) 0.709238(7) 0.655475(4) 0.01175(3) Uani 1 1 d . . .
Cl1 Cl 0.60900(6) 0.90560(6) 0.70974(3) 0.02061(11) Uani 1 1 d . . .
P1 P 0.25495(6) 0.71576(5) 0.53128(3) 0.00948(10) Uani 1 1 d . . .
O1 O 0.36336(16) 0.81113(15) 0.54815(10) 0.0141(3) Uani 1 1 d . . .
C10 C 0.4917(2) 0.5215(2) 0.62122(12) 0.0110(4) Uani 1 1 d . . .
C20 C 0.1914(2) 0.6900(2) 0.61113(12) 0.0115(4) Uani 1 1 d . . .
C30 C 0.1243(2) 0.7748(2) 0.45642(13) 0.0107(4) Uani 1 1 d . . .
C11 C 0.5764(2) 0.4297(2) 0.66209(12) 0.0129(4) Uani 1 1 d . . .
H11 H 0.6433 0.4585 0.7035 0.015 Uiso 1 1 calc R . .
C18 C 0.2931(2) 0.5554(2) 0.50713(12) 0.0103(4) Uani 1 1 d . . .
C12 C 0.5688(2) 0.2969(2) 0.64566(14) 0.0139(4) Uani 1 1 d . . .
H12 H 0.6281 0.2379 0.6757 0.017 Uiso 1 1 calc R . .
C13 C 0.4734(2) 0.2549(2) 0.58499(12) 0.0119(4) Uani 1 1 d . . .
C16 C 0.2132(2) 0.3625(2) 0.43036(13) 0.0141(4) Uani 1 1 d . . .
H16 H 0.1561 0.3260 0.3870 0.017 Uiso 1 1 calc R . .
C21 C 0.1503(2) 0.5688(2) 0.62810(12) 0.0134(4) Uani 1 1 d . . .
H21 H 0.1550 0.4971 0.5971 0.016 Uiso 1 1 calc R . .
C19 C 0.3923(2) 0.4804(2) 0.55738(12) 0.0095(4) Uani 1 1 d . . .
C31 C -0.0047(2) 0.7456(2) 0.44987(13) 0.0148(4) Uani 1 1 d . . .
H31 H -0.0269 0.6937 0.4867 0.018 Uiso 1 1 calc R . .
C25 C 0.1838(3) 0.7949(2) 0.65692(15) 0.0181(5) Uani 1 1 d . . .
H25 H 0.2120 0.8776 0.6461 0.022 Uiso 1 1 calc R . .
C14 C 0.3894(2) 0.3466(2) 0.54164(12) 0.0109(4) Uani 1 1 d . . .
C15 C 0.3001(2) 0.2874(2) 0.48005(13) 0.0125(4) Uani 1 1 d . . .
C17 C 0.2106(2) 0.4966(2) 0.44537(12) 0.0126(4) Uani 1 1 d . . .
H17 H 0.1492 0.5486 0.4114 0.015 Uiso 1 1 calc R . .
C35 C 0.1556(2) 0.8549(2) 0.40345(12) 0.0134(4) Uani 1 1 d . . .
H35 H 0.2430 0.8764 0.4081 0.016 Uiso 1 1 calc R . .
C2 C 0.3218(2) 0.1432(2) 0.48391(14) 0.0168(4) Uani 1 1 d . . .
H2A H 0.3397 0.1112 0.4374 0.020 Uiso 1 1 calc R . .
H2B H 0.2455 0.0977 0.4911 0.020 Uiso 1 1 calc R . .
C1 C 0.4399(2) 0.1222(2) 0.55225(14) 0.0169(4) Uani 1 1 d . . .
H1A H 0.4181 0.0639 0.5893 0.020 Uiso 1 1 calc R . .
H1B H 0.5126 0.0848 0.5363 0.020 Uiso 1 1 calc R . .
C22 C 0.1025(2) 0.5524(2) 0.69013(13) 0.0159(4) Uani 1 1 d . . .
H22 H 0.0753 0.4697 0.7017 0.019 Uiso 1 1 calc R . .
C34 C 0.0591(2) 0.9033(2) 0.34369(13) 0.0170(4) Uani 1 1 d . . .
H34 H 0.0807 0.9585 0.3080 0.020 Uiso 1 1 calc R . .
C33 C -0.0684(2) 0.8711(2) 0.33624(14) 0.0176(4) Uani 1 1 d . . .
H33 H -0.1339 0.9025 0.2949 0.021 Uiso 1 1 calc R . .
C24 C 0.1348(3) 0.7780(2) 0.71827(15) 0.0217(5) Uani 1 1 d . . .
H24 H 0.1286 0.8496 0.7490 0.026 Uiso 1 1 calc R . .
C32 C -0.1004(2) 0.7927(2) 0.38944(15) 0.0178(5) Uani 1 1 d . . .
H32 H -0.1878 0.7713 0.3845 0.021 Uiso 1 1 calc R . .
C23 C 0.0948(2) 0.6575(3) 0.73502(13) 0.0186(5) Uani 1 1 d . . .
H23 H 0.0621 0.6468 0.7773 0.022 Uiso 1 1 calc R . .


_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
Hg1 C10 2.061(2) . ?
Hg1 Cl1 2.3215(6) . ?
Hg1 O1 2.5450(17) . ?
P1 O1 1.5003(17) . ?
P1 C30 1.799(2) . ?
P1 C18 1.800(2) . ?
P1 C20 1.812(2) . ?
C10 C11 1.394(3) . ?
C10 C19 1.431(3) . ?
C20 C25 1.397(3) . ?
C20 C21 1.397(3) . ?
C30 C35 1.396(3) . ?
C30 C31 1.398(3) . ?
C11 C12 1.409(3) . ?
C18 C17 1.388(3) . ?
C18 C19 1.443(3) . ?
C12 C13 1.376(3) . ?
C13 C14 1.408(3) . ?
C13 C1 1.509(3) . ?
C16 C15 1.368(3) . ?
C16 C17 1.421(3) . ?
C21 C22 1.392(3) . ?
C19 C14 1.417(3) . ?
C31 C32 1.392(3) . ?
C25 C24 1.389(4) . ?
C14 C15 1.420(3) . ?
C15 C2 1.514(3) . ?
C35 C34 1.394(3) . ?
C2 C1 1.551(3) . ?
C22 C23 1.388(3) . ?
C34 C33 1.388(3) . ?
C33 C32 1.392(3) . ?
C24 C23 1.385(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
C10 Hg1 Cl1 170.22(6) . . ?
C10 Hg1 O1 95.76(7) . . ?
Cl1 Hg1 O1 93.98(4) . . ?
O1 P1 C30 109.97(10) . . ?
O1 P1 C18 116.34(10) . . ?
C30 P1 C18 107.93(10) . . ?
O1 P1 C20 111.94(10) . . ?
C30 P1 C20 106.81(10) . . ?
C18 P1 C20 103.26(10) . . ?
P1 O1 Hg1 104.28(8) . . ?
C11 C10 C19 118.82(19) . . ?
C11 C10 Hg1 114.91(16) . . ?
C19 C10 Hg1 126.07(15) . . ?
C25 C20 C21 119.4(2) . . ?
C25 C20 P1 118.62(18) . . ?
C21 C20 P1 122.00(17) . . ?
C35 C30 C31 119.5(2) . . ?
C35 C30 P1 117.19(17) . . ?
C31 C30 P1 123.28(17) . . ?
C10 C11 C12 124.0(2) . . ?
C17 C18 C19 119.68(19) . . ?
C17 C18 P1 118.21(16) . . ?
C19 C18 P1 121.18(16) . . ?
C13 C12 C11 118.3(2) . . ?
C12 C13 C14 118.6(2) . . ?
C12 C13 C1 131.6(2) . . ?
C14 C13 C1 109.9(2) . . ?
C15 C16 C17 118.2(2) . . ?
C22 C21 C20 120.5(2) . . ?
C14 C19 C10 115.59(19) . . ?
C14 C19 C18 115.05(19) . . ?
C10 C19 C18 129.35(19) . . ?
C32 C31 C30 120.0(2) . . ?
C24 C25 C20 119.8(2) . . ?
C13 C14 C19 124.7(2) . . ?
C13 C14 C15 111.07(19) . . ?
C19 C14 C15 124.2(2) . . ?
C16 C15 C14 119.28(19) . . ?
C16 C15 C2 131.6(2) . . ?
C14 C15 C2 109.1(2) . . ?
C18 C17 C16 123.4(2) . . ?
C34 C35 C30 120.2(2) . . ?
C15 C2 C1 105.05(18) . . ?
C13 C1 C2 104.82(18) . . ?
C23 C22 C21 119.6(2) . . ?
C33 C34 C35 120.1(2) . . ?
C34 C33 C32 120.0(2) . . ?
C23 C24 C25 120.6(2) . . ?
C33 C32 C31 120.2(2) . . ?
C24 C23 C22 120.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.57
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.651
_refine_diff_density_min         -2.109
_refine_diff_density_rms         0.149
####################################################################### 
# 
# 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_shelxl_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1897907'
loop_
_audit_author_name
_audit_author_address
'Enno Lork'
;Bremen University
Germany
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H20 Bi Cl4 O P'
_chemical_formula_weight         718.16

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.1561(3)
_cell_length_b                   11.7354(4)
_cell_length_c                   12.0175(5)
_cell_angle_alpha                90.8000(10)
_cell_angle_beta                 105.1680(10)
_cell_angle_gamma                95.8970(10)
_cell_volume                     1238.58(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9119
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      36.42

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_absorpt_coefficient_mu    7.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3968
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture D8 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            63344
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         35.63
_reflns_number_total             11415
_reflns_number_gt                10581
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0229P)²+1.9152P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         11415
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0577
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.022401(8) 0.347840(6) 0.590571(6) 0.00932(2) Uani 1 1 d . . .
Cl1 Cl 0.21848(6) 0.52835(4) 0.55238(5) 0.01366(8) Uani 1 1 d . . .
Cl2 Cl 0.20848(6) 0.23935(5) 0.73701(5) 0.01680(9) Uani 1 1 d . . .
P1 P -0.31288(6) 0.25136(4) 0.65966(4) 0.00835(8) Uani 1 1 d . . .
Cl4 Cl -0.19652(8) 0.05960(6) 0.27857(6) 0.02857(13) Uani 1 1 d . . .
Cl3 Cl -0.44577(13) 0.20008(13) 0.22690(10) 0.0696(4) Uani 1 1 d . . .
O1 O -0.19172(17) 0.23151(13) 0.59780(14) 0.0114(3) Uani 1 1 d . . .
C10 C -0.0097(2) 0.45278(16) 0.73817(18) 0.0102(3) Uani 1 1 d . . .
C21 C -0.5591(3) 0.30404(19) 0.4887(2) 0.0151(4) Uani 1 1 d . . .
H21 H -0.5045 0.3779 0.4922 0.018 Uiso 1 1 calc R . .
C18 C -0.2953(2) 0.39295(17) 0.72197(18) 0.0102(3) Uani 1 1 d . . .
C19 C -0.1511(2) 0.46113(16) 0.76530(17) 0.0090(3) Uani 1 1 d . . .
C20 C -0.4994(2) 0.22053(17) 0.56390(17) 0.0103(3) Uani 1 1 d . . .
C17 C -0.4236(2) 0.42365(18) 0.7523(2) 0.0138(4) Uani 1 1 d . . .
H17 H -0.5186 0.3792 0.7205 0.017 Uiso 1 1 calc R . .
C13 C -0.0180(2) 0.62041(17) 0.90751(17) 0.0121(3) Uani 1 1 d . . .
C14 C -0.1495(2) 0.54999(16) 0.84697(17) 0.0102(3) Uani 1 1 d . . .
C11 C 0.1190(2) 0.52189(18) 0.79926(19) 0.0138(4) Uani 1 1 d . . .
H11 H 0.2129 0.5134 0.7819 0.017 Uiso 1 1 calc R . .
C12 C 0.1186(3) 0.60470(19) 0.88631(19) 0.0155(4) Uani 1 1 d . . .
H12 H 0.2103 0.6479 0.9286 0.019 Uiso 1 1 calc R . .
C23 C -0.7784(3) 0.1694(2) 0.4033(2) 0.0189(4) Uani 1 1 d . . .
H23 H -0.8739 0.1518 0.3481 0.023 Uiso 1 1 calc R . .
C24 C -0.7189(3) 0.0867(2) 0.4781(2) 0.0193(4) Uani 1 1 d . . .
H24 H -0.7737 0.0128 0.4741 0.023 Uiso 1 1 calc R . .
C16 C -0.4182(3) 0.5181(2) 0.8283(2) 0.0169(4) Uani 1 1 d . . .
H16 H -0.5084 0.5387 0.8447 0.020 Uiso 1 1 calc R . .
C25 C -0.5794(3) 0.11189(19) 0.5588(2) 0.0148(4) Uani 1 1 d . . .
H25 H -0.5386 0.0555 0.6104 0.018 Uiso 1 1 calc R . .
C22 C -0.6995(3) 0.2779(2) 0.4085(2) 0.0186(4) Uani 1 1 d . . .
H22 H -0.7414 0.3342 0.3573 0.022 Uiso 1 1 calc R . .
C15 C -0.2803(3) 0.57896(18) 0.87765(19) 0.0139(4) Uani 1 1 d . . .
C30 C -0.2920(2) 0.15600(17) 0.77748(18) 0.0116(3) Uani 1 1 d . . .
C1 C -0.0595(3) 0.70125(19) 0.99024(19) 0.0156(4) Uani 1 1 d . . .
H1A H -0.0259 0.7818 0.9777 0.019 Uiso 1 1 calc R . .
H1B H -0.0120 0.6838 1.0712 0.019 Uiso 1 1 calc R . .
C2 C -0.2357(3) 0.6805(2) 0.9628(2) 0.0199(4) Uani 1 1 d . . .
H2A H -0.2684 0.6633 1.0336 0.024 Uiso 1 1 calc R . .
H2B H -0.2824 0.7487 0.9285 0.024 Uiso 1 1 calc R . .
C35 C -0.1824(3) 0.07922(18) 0.7897(2) 0.0154(4) Uani 1 1 d . . .
H35 H -0.1229 0.0770 0.7358 0.019 Uiso 1 1 calc R . .
C3 C -0.2603(4) 0.1902(2) 0.3090(2) 0.0261(5) Uani 1 1 d . . .
H3A H -0.2565 0.1962 0.3920 0.031 Uiso 1 1 calc R . .
H3B H -0.1917 0.2547 0.2925 0.031 Uiso 1 1 calc R . .
C31 C -0.3781(3) 0.1594(2) 0.8574(2) 0.0180(4) Uani 1 1 d . . .
H31 H -0.4536 0.2108 0.8487 0.022 Uiso 1 1 calc R . .
C32 C -0.3533(3) 0.0875(2) 0.9499(2) 0.0232(5) Uani 1 1 d . . .
H32 H -0.4102 0.0908 1.0053 0.028 Uiso 1 1 calc R . .
C34 C -0.1609(3) 0.0061(2) 0.8811(2) 0.0217(5) Uani 1 1 d . . .
H34 H -0.0881 -0.0473 0.8887 0.026 Uiso 1 1 calc R . .
C33 C -0.2448(4) 0.0106(2) 0.9612(2) 0.0248(5) Uani 1 1 d . . .
H33 H -0.2283 -0.0390 1.0240 0.030 Uiso 1 1 calc R . .


_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
Bi1 C10 2.244(2) . ?
Bi1 O1 2.2929(15) . ?
Bi1 Cl2 2.5613(5) . ?
Bi1 Cl1 2.7565(5) . ?
Bi1 Cl1 2.9448(5) 2_566 ?
Cl1 Bi1 2.9449(5) 2_566 ?
P1 O1 1.5223(16) . ?
P1 C18 1.787(2) . ?
P1 C20 1.790(2) . ?
P1 C30 1.800(2) . ?
Cl4 C3 1.761(3) . ?
Cl3 C3 1.743(3) . ?
C10 C11 1.386(3) . ?
C10 C19 1.428(3) . ?
C21 C22 1.392(3) . ?
C21 C20 1.398(3) . ?
C21 H21 0.9500 . ?
C18 C17 1.396(3) . ?
C18 C19 1.437(3) . ?
C19 C14 1.418(3) . ?
C20 C25 1.396(3) . ?
C17 C16 1.415(3) . ?
C17 H17 0.9500 . ?
C13 C12 1.370(3) . ?
C13 C14 1.408(3) . ?
C13 C1 1.510(3) . ?
C14 C15 1.413(3) . ?
C11 C12 1.419(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C23 C24 1.387(4) . ?
C23 C22 1.390(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(3) . ?
C24 H24 0.9500 . ?
C16 C15 1.367(3) . ?
C16 H16 0.9500 . ?
C25 H25 0.9500 . ?
C22 H22 0.9500 . ?
C15 C2 1.511(3) . ?
C30 C31 1.396(3) . ?
C30 C35 1.397(3) . ?
C1 C2 1.552(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C35 C34 1.389(3) . ?
C35 H35 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C31 C32 1.390(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.392(4) . ?
C32 H32 0.9500 . ?
C34 C33 1.383(4) . ?
C34 H34 0.9500 . ?
C33 H33 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
C10 Bi1 O1 87.73(6) . . ?
C10 Bi1 Cl2 88.55(5) . . ?
O1 Bi1 Cl2 95.55(4) . . ?
C10 Bi1 Cl1 88.23(5) . . ?
O1 Bi1 Cl1 163.52(4) . . ?
Cl2 Bi1 Cl1 100.314(17) . . ?
C10 Bi1 Cl1 84.81(5) . 2_566 ?
O1 Bi1 Cl1 78.82(4) . 2_566 ?
Cl2 Bi1 Cl1 171.439(16) . 2_566 ?
Cl1 Bi1 Cl1 84.905(15) . 2_566 ?
Bi1 Cl1 Bi1 95.094(15) . 2_566 ?
O1 P1 C18 114.25(9) . . ?
O1 P1 C20 110.62(9) . . ?
C18 P1 C20 108.70(9) . . ?
O1 P1 C30 107.59(9) . . ?
C18 P1 C30 106.26(10) . . ?
C20 P1 C30 109.23(10) . . ?
P1 O1 Bi1 129.78(9) . . ?
C11 C10 C19 119.28(18) . . ?
C11 C10 Bi1 114.87(15) . . ?
C19 C10 Bi1 125.57(14) . . ?
C22 C21 C20 119.3(2) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C17 C18 C19 119.81(18) . . ?
C17 C18 P1 115.65(15) . . ?
C19 C18 P1 122.80(15) . . ?
C14 C19 C10 115.33(18) . . ?
C14 C19 C18 115.04(18) . . ?
C10 C19 C18 129.63(18) . . ?
C25 C20 C21 120.44(19) . . ?
C25 C20 P1 120.36(16) . . ?
C21 C20 P1 119.04(16) . . ?
C18 C17 C16 122.9(2) . . ?
C18 C17 H17 118.6 . . ?
C16 C17 H17 118.6 . . ?
C12 C13 C14 118.91(19) . . ?
C12 C13 C1 131.8(2) . . ?
C14 C13 C1 109.27(19) . . ?
C13 C14 C15 111.50(18) . . ?
C13 C14 C19 124.44(19) . . ?
C15 C14 C19 124.06(19) . . ?
C10 C11 C12 123.7(2) . . ?
C10 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C13 C12 C11 118.0(2) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
C24 C23 C22 120.5(2) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 120.0(2) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C15 C16 C17 118.4(2) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
C24 C25 C20 119.7(2) . . ?
C24 C25 H25 120.2 . . ?
C20 C25 H25 120.2 . . ?
C23 C22 C21 120.0(2) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C16 C15 C14 119.46(19) . . ?
C16 C15 C2 131.5(2) . . ?
C14 C15 C2 109.05(19) . . ?
C31 C30 C35 119.9(2) . . ?
C31 C30 P1 122.01(17) . . ?
C35 C30 P1 118.04(17) . . ?
C13 C1 C2 104.78(17) . . ?
C13 C1 H1A 110.8 . . ?
C2 C1 H1A 110.8 . . ?
C13 C1 H1B 110.8 . . ?
C2 C1 H1B 110.8 . . ?
H1A C1 H1B 108.9 . . ?
C15 C2 C1 104.88(18) . . ?
C15 C2 H2A 110.8 . . ?
C1 C2 H2A 110.8 . . ?
C15 C2 H2B 110.8 . . ?
C1 C2 H2B 110.8 . . ?
H2A C2 H2B 108.8 . . ?
C34 C35 C30 119.6(2) . . ?
C34 C35 H35 120.2 . . ?
C30 C35 H35 120.2 . . ?
Cl3 C3 Cl4 111.31(15) . . ?
Cl3 C3 H3A 109.4 . . ?
Cl4 C3 H3A 109.4 . . ?
Cl3 C3 H3B 109.4 . . ?
Cl4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C32 C31 C30 119.9(2) . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C32 C33 119.9(2) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C33 C34 C35 120.5(2) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        35.63
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.568
_refine_diff_density_min         -3.007
_refine_diff_density_rms         0.184
####################################################################### 
# 
# 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_shelxl_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1897905'
loop_
_audit_author_name
_audit_author_address
'Enno Lork'
;Bremen University
Germany
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H18 Cl2 O P Sb'
_chemical_formula_weight         546.00

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   8.6794(3)
_cell_length_b                   12.6557(5)
_cell_length_c                   19.5559(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.4970(10)
_cell_angle_gamma                90.00
_cell_volume                     2129.73(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9738
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      30.54

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5134
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture D8 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            98732
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         30.60
_reflns_number_total             6549
_reflns_number_gt                6038
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0287P)²+1.1511P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         6549
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0214
_refine_ls_wR_factor_ref         0.0610
_refine_ls_wR_factor_gt          0.0596
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_restrained_S_all      1.244
_refine_ls_shift/su_max          0.004
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.04744(19) 1.11625(13) 0.42097(9) 0.0155(3) Uani 1 1 d . . .
H1A H 0.0986 1.1832 0.4106 0.019 Uiso 1 1 calc R . .
H1B H -0.0427 1.1326 0.4454 0.019 Uiso 1 1 calc R . .
C2 C -0.00449(19) 1.05338(13) 0.35386(8) 0.0157(3) Uani 1 1 d . . .
H2A H -0.1187 1.0442 0.3467 0.019 Uiso 1 1 calc R . .
H2B H 0.0276 1.0902 0.3133 0.019 Uiso 1 1 calc R . .
C10 C 0.35907(17) 0.87957(12) 0.52174(8) 0.0102(3) Uani 1 1 d . . .
C11 C 0.34701(19) 0.97684(13) 0.55351(8) 0.0139(3) Uani 1 1 d . . .
H11 H 0.4092 0.9885 0.5965 0.017 Uiso 1 1 calc R . .
C12 C 0.24837(19) 1.05977(12) 0.52612(8) 0.0150(3) Uani 1 1 d . . .
H12 H 0.2437 1.1244 0.5504 0.018 Uiso 1 1 calc R . .
C13 C 0.16006(18) 1.04453(12) 0.46385(8) 0.0123(3) Uani 1 1 d . . .
C14 C 0.17158(17) 0.94746(12) 0.42939(8) 0.0100(3) Uani 1 1 d . . .
C15 C 0.07625(17) 0.94809(12) 0.36480(8) 0.0115(3) Uani 1 1 d . . .
C16 C 0.07230(18) 0.86083(13) 0.32320(8) 0.0137(3) Uani 1 1 d . . .
H16 H 0.0105 0.8597 0.2794 0.016 Uiso 1 1 calc R . .
C17 C 0.16283(18) 0.77284(12) 0.34745(8) 0.0123(3) Uani 1 1 d . . .
H17 H 0.1591 0.7115 0.3193 0.015 Uiso 1 1 calc R . .
C18 C 0.25753(17) 0.77136(11) 0.41072(8) 0.0096(3) Uani 1 1 d . . .
C19 C 0.26765(16) 0.86228(12) 0.45549(7) 0.0090(3) Uani 1 1 d . . .
C20 C 0.53366(17) 0.66522(12) 0.37985(8) 0.0109(3) Uani 1 1 d . . .
C21 C 0.56034(19) 0.75603(12) 0.34248(8) 0.0126(3) Uani 1 1 d . . .
H21 H 0.4942 0.8157 0.3434 0.015 Uiso 1 1 calc R . .
C22 C 0.6844(2) 0.75873(14) 0.30385(9) 0.0163(3) Uani 1 1 d . . .
H22 H 0.7037 0.8207 0.2789 0.020 Uiso 1 1 calc R . .
C23 C 0.77975(19) 0.67106(14) 0.30180(9) 0.0178(3) Uani 1 1 d . . .
H23 H 0.8627 0.6725 0.2746 0.021 Uiso 1 1 calc R . .
C24 C 0.75403(19) 0.58105(14) 0.33952(10) 0.0192(3) Uani 1 1 d . . .
H24 H 0.8202 0.5215 0.3383 0.023 Uiso 1 1 calc R . .
C25 C 0.63244(19) 0.57777(13) 0.37894(9) 0.0164(3) Uani 1 1 d . . .
H25 H 0.6162 0.5166 0.4052 0.020 Uiso 1 1 calc R . .
C30 C 0.26232(17) 0.54112(12) 0.39673(8) 0.0110(3) Uani 1 1 d . . .
C31 C 0.26491(18) 0.50232(12) 0.33015(8) 0.0135(3) Uani 1 1 d . . .
H31 H 0.3303 0.5341 0.3006 0.016 Uiso 1 1 calc R . .
C32 C 0.1713(2) 0.41689(13) 0.30712(8) 0.0160(3) Uani 1 1 d . . .
H32 H 0.1729 0.3905 0.2617 0.019 Uiso 1 1 calc R . .
C33 C 0.07606(19) 0.37021(13) 0.34997(9) 0.0156(3) Uani 1 1 d . . .
H33 H 0.0109 0.3128 0.3337 0.019 Uiso 1 1 calc R . .
C34 C 0.07568(19) 0.40741(13) 0.41682(9) 0.0166(3) Uani 1 1 d . . .
H34 H 0.0117 0.3744 0.4465 0.020 Uiso 1 1 calc R . .
C35 C 0.16834(19) 0.49265(13) 0.44047(9) 0.0145(3) Uani 1 1 d . . .
H35 H 0.1679 0.5179 0.4862 0.017 Uiso 1 1 calc R . .
O1 O 0.42052(14) 0.64176(9) 0.50500(6) 0.0136(2) Uani 1 1 d . . .
P1 P 0.37231(4) 0.65508(3) 0.428190(19) 0.00882(7) Uani 1 1 d . . .
Cl1 Cl 0.60100(5) 0.89099(3) 0.67868(2) 0.01891(8) Uani 1 1 d . . .
Cl2 Cl 0.32812(5) 0.69902(3) 0.643512(19) 0.01592(8) Uani 1 1 d . . .
Sb1 Sb 0.519755(11) 0.768212(8) 0.578431(5) 0.00968(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
C1 C13 1.506(2) . ?
C1 C2 1.551(2) . ?
C2 C15 1.508(2) . ?
C10 C11 1.389(2) . ?
C10 C19 1.445(2) . ?
C10 Sb1 2.1810(15) . ?
C11 C12 1.415(2) . ?
C12 C13 1.365(2) . ?
C13 C14 1.411(2) . ?
C14 C19 1.417(2) . ?
C14 C15 1.417(2) . ?
C15 C16 1.369(2) . ?
C16 C17 1.409(2) . ?
C17 C18 1.393(2) . ?
C18 C19 1.442(2) . ?
C18 P1 1.7849(15) . ?
C20 C21 1.397(2) . ?
C20 C25 1.402(2) . ?
C20 P1 1.7936(16) . ?
C21 C22 1.394(2) . ?
C22 C23 1.388(2) . ?
C23 C24 1.391(2) . ?
C24 C25 1.386(2) . ?
C30 C31 1.395(2) . ?
C30 C35 1.398(2) . ?
C30 P1 1.7935(15) . ?
C31 C32 1.391(2) . ?
C32 C33 1.384(2) . ?
C33 C34 1.390(2) . ?
C34 C35 1.388(2) . ?
O1 P1 1.5151(11) . ?
O1 Sb1 2.2455(11) . ?
Cl1 Sb1 2.5287(4) . ?
Cl2 Sb1 2.3886(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
C13 C1 C2 104.94(13) . . ?
C15 C2 C1 104.77(13) . . ?
C11 C10 C19 118.08(14) . . ?
C11 C10 Sb1 115.20(11) . . ?
C19 C10 Sb1 126.72(11) . . ?
C10 C11 C12 124.42(14) . . ?
C13 C12 C11 118.32(14) . . ?
C12 C13 C14 118.85(14) . . ?
C12 C13 C1 131.26(15) . . ?
C14 C13 C1 109.88(13) . . ?
C13 C14 C19 124.44(14) . . ?
C13 C14 C15 110.57(13) . . ?
C19 C14 C15 124.98(14) . . ?
C16 C15 C14 119.44(14) . . ?
C16 C15 C2 130.79(14) . . ?
C14 C15 C2 109.76(13) . . ?
C15 C16 C17 117.89(14) . . ?
C18 C17 C16 123.22(14) . . ?
C17 C18 C19 120.71(13) . . ?
C17 C18 P1 115.52(11) . . ?
C19 C18 P1 123.62(11) . . ?
C14 C19 C18 113.72(13) . . ?
C14 C19 C10 115.88(13) . . ?
C18 C19 C10 130.40(14) . . ?
C21 C20 C25 119.96(14) . . ?
C21 C20 P1 121.91(12) . . ?
C25 C20 P1 118.11(12) . . ?
C22 C21 C20 119.74(15) . . ?
C23 C22 C21 120.11(15) . . ?
C22 C23 C24 120.12(15) . . ?
C25 C24 C23 120.39(16) . . ?
C24 C25 C20 119.66(15) . . ?
C31 C30 C35 119.89(14) . . ?
C31 C30 P1 122.05(12) . . ?
C35 C30 P1 118.03(12) . . ?
C32 C31 C30 119.74(15) . . ?
C33 C32 C31 120.35(15) . . ?
C32 C33 C34 119.99(15) . . ?
C35 C34 C33 120.27(15) . . ?
C34 C35 C30 119.74(15) . . ?
P1 O1 Sb1 126.01(7) . . ?
O1 P1 C18 110.89(7) . . ?
O1 P1 C30 108.44(7) . . ?
C18 P1 C30 109.79(7) . . ?
O1 P1 C20 113.38(7) . . ?
C18 P1 C20 107.14(7) . . ?
C30 P1 C20 107.10(7) . . ?
C10 Sb1 O1 88.22(5) . . ?
C10 Sb1 Cl2 93.68(4) . . ?
O1 Sb1 Cl2 81.01(3) . . ?
C10 Sb1 Cl1 95.29(4) . . ?
O1 Sb1 Cl1 168.13(3) . . ?
Cl2 Sb1 Cl1 87.438(14) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.60
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.559
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.149
####################################################################### 
# 
# 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_shelxl_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 1897906'
loop_
_audit_author_name
_audit_author_address
'Enno Lork'
;Bremen University
Germany
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H26 Cl2 O2 P Sb'
_chemical_formula_weight         618.11

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2077(3)
_cell_length_b                   9.6481(4)
_cell_length_c                   15.3566(6)
_cell_angle_alpha                97.5470(10)
_cell_angle_beta                 97.8930(10)
_cell_angle_gamma                110.3930(10)
_cell_volume                     1242.80(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9674
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      28.37

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             620
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5825
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Venture D8 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            73343
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         28.42
_reflns_number_total             6215
_reflns_number_gt                5770
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0269P)²+1.1137P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         6215
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0589
_refine_ls_wR_factor_gt          0.0571
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C13 C 0.4125(2) -0.3133(2) 0.56951(11) 0.0134(3) Uani 1 1 d . . .
C14 C 0.4960(2) -0.35468(19) 0.63913(11) 0.0110(3) Uani 1 1 d . . .
C1 C 0.2827(2) -0.4524(2) 0.51201(12) 0.0178(4) Uani 1 1 d . . .
H1A H 0.2971 -0.4637 0.4504 0.021 Uiso 1 1 calc R . .
H1B H 0.1798 -0.4468 0.5132 0.021 Uiso 1 1 calc R . .
C2 C 0.2983(2) -0.5852(2) 0.55442(12) 0.0173(4) Uani 1 1 d . . .
H2A H 0.2022 -0.6386 0.5744 0.021 Uiso 1 1 calc R . .
H2B H 0.3194 -0.6555 0.5116 0.021 Uiso 1 1 calc R . .
C3 C 1.1802(2) 0.0678(2) 0.70931(13) 0.0196(4) Uani 1 1 d . . .
H3A H 1.2492 0.0440 0.7535 0.024 Uiso 1 1 calc R . .
H3B H 1.1945 0.1728 0.7264 0.024 Uiso 1 1 calc R . .
C4 C 1.2162(3) 0.0375(2) 0.61720(14) 0.0225(4) Uani 1 1 d . . .
H4A H 1.3258 0.0485 0.6208 0.027 Uiso 1 1 calc R . .
H4B H 1.1938 0.1048 0.5804 0.027 Uiso 1 1 calc R . .
C5 C 1.1049(2) -0.1254(2) 0.58046(13) 0.0184(4) Uani 1 1 d . . .
H5A H 1.0837 -0.1479 0.5155 0.022 Uiso 1 1 calc R . .
H5B H 1.1472 -0.1956 0.6032 0.022 Uiso 1 1 calc R . .
C6 C 0.9587(2) -0.1289(2) 0.61608(12) 0.0171(4) Uani 1 1 d . . .
H6A H 0.8936 -0.0938 0.5763 0.021 Uiso 1 1 calc R . .
H6B H 0.8965 -0.2303 0.6220 0.021 Uiso 1 1 calc R . .
C10 C 0.6698(2) -0.09427(19) 0.69908(11) 0.0110(3) Uani 1 1 d . . .
C11 C 0.5842(2) -0.0584(2) 0.62995(12) 0.0150(3) Uani 1 1 d . . .
H11 H 0.6124 0.0428 0.6264 0.018 Uiso 1 1 calc R . .
C12 C 0.4571(2) -0.1648(2) 0.56440(12) 0.0157(3) Uani 1 1 d . . .
H12 H 0.4052 -0.1340 0.5189 0.019 Uiso 1 1 calc R . .
C15 C 0.4357(2) -0.5129(2) 0.63300(11) 0.0128(3) Uani 1 1 d . . .
C16 C 0.5049(2) -0.5755(2) 0.69321(12) 0.0150(3) Uani 1 1 d . . .
H16 H 0.4706 -0.6794 0.6887 0.018 Uiso 1 1 calc R . .
C17 C 0.6293(2) -0.4776(2) 0.76191(12) 0.0133(3) Uani 1 1 d . . .
H17 H 0.6749 -0.5191 0.8040 0.016 Uiso 1 1 calc R . .
C18 C 0.6881(2) -0.32167(19) 0.77028(11) 0.0106(3) Uani 1 1 d . . .
C19 C 0.62410(19) -0.25156(19) 0.70555(11) 0.0100(3) Uani 1 1 d . . .
C20 C 1.0217(2) -0.23061(19) 0.84953(11) 0.0106(3) Uani 1 1 d . . .
C21 C 1.0319(2) -0.3319(2) 0.77906(12) 0.0138(3) Uani 1 1 d . . .
H21 H 0.9405 -0.4024 0.7417 0.017 Uiso 1 1 calc R . .
C22 C 1.1796(2) -0.3268(2) 0.76506(12) 0.0172(4) Uani 1 1 d . . .
H22 H 1.1870 -0.3944 0.7184 0.021 Uiso 1 1 calc R . .
C23 C 1.3156(2) -0.2215(2) 0.82032(14) 0.0205(4) Uani 1 1 d . . .
H23 H 1.4141 -0.2164 0.8096 0.025 Uiso 1 1 calc R . .
C24 C 1.3054(2) -0.1233(2) 0.89171(14) 0.0234(4) Uani 1 1 d . . .
H24 H 1.3972 -0.0544 0.9295 0.028 Uiso 1 1 calc R . .
C25 C 1.1588(2) -0.1274(2) 0.90708(13) 0.0177(4) Uani 1 1 d . . .
H25 H 1.1520 -0.0622 0.9552 0.021 Uiso 1 1 calc R . .
C30 C 0.7835(2) -0.30527(19) 0.96025(11) 0.0110(3) Uani 1 1 d . . .
C31 C 0.8451(2) -0.4080(2) 0.98920(13) 0.0193(4) Uani 1 1 d . . .
H31 H 0.9175 -0.4330 0.9603 0.023 Uiso 1 1 calc R . .
C32 C 0.7985(2) -0.4730(3) 1.06117(14) 0.0228(4) Uani 1 1 d . . .
H32 H 0.8389 -0.5424 1.0800 0.027 Uiso 1 1 calc R . .
C33 C 0.6921(2) -0.4348(2) 1.10506(12) 0.0174(4) Uani 1 1 d . . .
H33 H 0.6628 -0.4772 1.1540 0.021 Uiso 1 1 calc R . .
C34 C 0.6290(2) -0.3338(2) 1.07632(12) 0.0159(3) Uani 1 1 d . . .
H34 H 0.5566 -0.3092 1.1055 0.019 Uiso 1 1 calc R . .
C35 C 0.6740(2) -0.2692(2) 1.00375(12) 0.0134(3) Uani 1 1 d . . .
H35 H 0.6312 -0.2019 0.9841 0.016 Uiso 1 1 calc R . .
O1 O 0.84660(15) -0.05693(14) 0.88764(8) 0.0129(2) Uani 1 1 d . . .
O2 O 1.01660(15) -0.02901(14) 0.70287(8) 0.0143(2) Uani 1 1 d . . .
P1 P 0.83703(5) -0.21826(5) 0.86719(3) 0.00902(8) Uani 1 1 d . . .
Cl1 Cl 0.88502(6) 0.26068(5) 0.66390(3) 0.02125(10) Uani 1 1 d . . .
Cl2 Cl 0.66544(6) 0.18250(6) 0.84608(3) 0.02340(10) Uani 1 1 d . . .
Sb1 Sb 0.861826(13) 0.099223(12) 0.786542(7) 0.01063(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
C13 C12 1.362(3) . ?
C13 C14 1.412(2) . ?
C13 C1 1.513(2) . ?
C14 C15 1.416(2) . ?
C14 C19 1.417(2) . ?
C1 C2 1.552(3) . ?
C2 C15 1.513(2) . ?
C3 O2 1.451(2) . ?
C3 C4 1.511(3) . ?
C4 C5 1.525(3) . ?
C5 C6 1.513(3) . ?
C6 O2 1.449(2) . ?
C10 C11 1.387(2) . ?
C10 C19 1.448(2) . ?
C10 Sb1 2.1920(17) . ?
C11 C12 1.416(3) . ?
C15 C16 1.370(3) . ?
C16 C17 1.404(2) . ?
C17 C18 1.391(2) . ?
C18 C19 1.444(2) . ?
C18 P1 1.7851(17) . ?
C20 C21 1.396(2) . ?
C20 C25 1.397(2) . ?
C20 P1 1.7992(17) . ?
C21 C22 1.391(3) . ?
C22 C23 1.384(3) . ?
C23 C24 1.387(3) . ?
C24 C25 1.391(3) . ?
C30 C31 1.393(2) . ?
C30 C35 1.397(2) . ?
C30 P1 1.7917(17) . ?
C31 C32 1.387(3) . ?
C32 C33 1.385(3) . ?
C33 C34 1.386(3) . ?
C34 C35 1.390(2) . ?
O1 P1 1.5158(13) . ?
O1 Sb1 2.2863(12) . ?
O2 Sb1 2.5548(13) . ?
Cl1 Sb1 2.5824(5) . ?
Cl2 Sb1 2.4546(5) . ?

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
C12 C13 C14 118.74(16) . . ?
C12 C13 C1 131.50(16) . . ?
C14 C13 C1 109.76(16) . . ?
C13 C14 C15 110.96(15) . . ?
C13 C14 C19 124.40(16) . . ?
C15 C14 C19 124.64(16) . . ?
C13 C1 C2 104.73(14) . . ?
C15 C2 C1 105.07(15) . . ?
O2 C3 C4 105.82(15) . . ?
C3 C4 C5 102.71(15) . . ?
C6 C5 C4 101.43(15) . . ?
O2 C6 C5 105.34(14) . . ?
C11 C10 C19 117.64(16) . . ?
C11 C10 Sb1 114.73(12) . . ?
C19 C10 Sb1 127.63(12) . . ?
C10 C11 C12 124.71(17) . . ?
C13 C12 C11 118.40(16) . . ?
C16 C15 C14 119.64(16) . . ?
C16 C15 C2 130.89(17) . . ?
C14 C15 C2 109.46(15) . . ?
C15 C16 C17 117.81(16) . . ?
C18 C17 C16 123.41(16) . . ?
C17 C18 C19 120.56(16) . . ?
C17 C18 P1 115.82(13) . . ?
C19 C18 P1 123.56(13) . . ?
C14 C19 C18 113.83(15) . . ?
C14 C19 C10 116.09(15) . . ?
C18 C19 C10 130.08(16) . . ?
C21 C20 C25 120.22(16) . . ?
C21 C20 P1 122.70(13) . . ?
C25 C20 P1 116.99(13) . . ?
C22 C21 C20 119.57(17) . . ?
C23 C22 C21 120.24(17) . . ?
C22 C23 C24 120.18(18) . . ?
C23 C24 C25 120.36(19) . . ?
C24 C25 C20 119.38(18) . . ?
C31 C30 C35 119.58(16) . . ?
C31 C30 P1 122.41(13) . . ?
C35 C30 P1 118.00(13) . . ?
C32 C31 C30 120.02(17) . . ?
C33 C32 C31 120.17(18) . . ?
C32 C33 C34 120.29(17) . . ?
C33 C34 C35 119.84(17) . . ?
C34 C35 C30 120.08(16) . . ?
P1 O1 Sb1 125.56(7) . . ?
C6 O2 C3 109.37(13) . . ?
C6 O2 Sb1 126.10(10) . . ?
C3 O2 Sb1 113.35(10) . . ?
O1 P1 C18 110.42(8) . . ?
O1 P1 C30 108.50(8) . . ?
C18 P1 C30 108.11(8) . . ?
O1 P1 C20 112.62(8) . . ?
C18 P1 C20 108.85(8) . . ?
C30 P1 C20 108.22(8) . . ?
C10 Sb1 O1 85.17(5) . . ?
C10 Sb1 Cl2 89.54(5) . . ?
O1 Sb1 Cl2 90.28(3) . . ?
C10 Sb1 O2 78.70(5) . . ?
O1 Sb1 O2 89.74(4) . . ?
Cl2 Sb1 O2 168.20(3) . . ?
C10 Sb1 Cl1 92.66(5) . . ?
O1 Sb1 Cl1 175.39(3) . . ?
Cl2 Sb1 Cl1 93.778(17) . . ?
O2 Sb1 Cl1 85.84(3) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.42
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.567
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.098
