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

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

data_ax1787_As3Tipp3_cmp2a
_database_code_depnum_ccdc_archive 'CCDC 2041965'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-02 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA 

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H69 As3'
_chemical_formula_sum            'C45 H69 As3'
_chemical_formula_weight         834.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA


_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4729(6)
_cell_length_b                   13.1325(7)
_cell_length_c                   14.8881(8)
_cell_angle_alpha                94.4180(10)
_cell_angle_beta                 98.3520(10)
_cell_angle_gamma                95.866(2)
_cell_volume                     2198.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9782
_cell_measurement_theta_min      3.92
_cell_measurement_theta_max      66.68

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_F_000             876
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.099
_exptl_absorpt_coefficient_mu    2.908
_shelx_estimated_absorpt_T_min   0.472
_shelx_estimated_absorpt_T_max   0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         microfocus
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            31666
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.398
_diffrn_reflns_theta_max         66.672
_diffrn_reflns_theta_full        66.672
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7775
_reflns_number_gt                7560
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.
 
 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0309P)²+0.9983P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7775
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0215
_refine_ls_wR_factor_ref         0.0573
_refine_ls_wR_factor_gt          0.0566
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.28372(2) 0.35694(2) 0.42798(2) 0.01919(5) Uani 1 1 d . . . . .
As2 As 0.35115(2) 0.18586(2) 0.41454(2) 0.02180(5) Uani 1 1 d . . . . .
As3 As 0.15165(2) 0.20640(2) 0.45307(2) 0.02119(5) Uani 1 1 d . . . . .
C1 C 0.24045(12) 0.40986(11) 0.30773(10) 0.0200(3) Uani 1 1 d . . . . .
C21 C 0.39343(13) 0.17884(12) 0.22457(11) 0.0244(3) Uani 1 1 d . . . . .
C2 C 0.15113(13) 0.36746(11) 0.23580(10) 0.0235(3) Uani 1 1 d . . . . .
C16 C 0.32529(14) 0.13085(12) 0.28457(11) 0.0243(3) Uani 1 1 d . . . . .
C6 C 0.30493(13) 0.50629(11) 0.30108(10) 0.0223(3) Uani 1 1 d . . . . .
C17 C 0.25622(14) 0.03516(12) 0.25514(12) 0.0279(3) Uani 1 1 d . . . . .
C31 C 0.19486(12) 0.22113(11) 0.58836(10) 0.0220(3) Uani 1 1 d . . . . .
C7 C 0.07911(13) 0.26351(11) 0.23497(10) 0.0236(3) Uani 1 1 d . . . . .
H7 H 0.1217 0.2254 0.2828 0.028 Uiso 1 1 calc R U . . .
C32 C 0.24773(14) 0.14364(12) 0.63454(11) 0.0267(3) Uani 1 1 d . . . . .
C13 C 0.40573(13) 0.55707(11) 0.37493(10) 0.0229(3) Uani 1 1 d . . . . .
H13 H 0.4427 0.5009 0.4063 0.027 Uiso 1 1 calc R U . . .
C28 C 0.47955(14) 0.27616(11) 0.25411(11) 0.0250(3) Uani 1 1 d . . . . .
H28 H 0.4509 0.3140 0.3060 0.030 Uiso 1 1 calc R U . . .
C4 C 0.18471(16) 0.51935(14) 0.15486(12) 0.0364(4) Uani 1 1 d . . . . .
C3 C 0.12526(15) 0.42394(13) 0.16136(11) 0.0326(4) Uani 1 1 d . . . . .
H3 H 0.0643 0.3957 0.1131 0.039 Uiso 1 1 calc R U . . .
C19 C 0.32015(16) 0.03898(13) 0.10622(12) 0.0347(4) Uani 1 1 d . . . . .
C5 C 0.27536(15) 0.55853(12) 0.22500(11) 0.0297(3) Uani 1 1 d . . . . .
H5 H 0.3185 0.6232 0.2207 0.036 Uiso 1 1 calc R U . . .
C9 C 0.06860(16) 0.19860(13) 0.14370(11) 0.0333(4) Uani 1 1 d . . . . .
H9A H 0.0189 0.2298 0.0966 0.050 Uiso 1 1 calc R U . . .
H9B H 0.0325 0.1289 0.1493 0.050 Uiso 1 1 calc R U . . .
H9C H 0.1477 0.1956 0.1268 0.050 Uiso 1 1 calc R U . . .
C36 C 0.16620(13) 0.30789(12) 0.63933(10) 0.0245(3) Uani 1 1 d . . . . .
C20 C 0.38821(15) 0.13227(13) 0.13680(12) 0.0315(4) Uani 1 1 d . . . . .
H20 H 0.4328 0.1654 0.0962 0.038 Uiso 1 1 calc R U . . .
C43 C 0.09776(15) 0.39014(13) 0.59717(11) 0.0292(3) Uani 1 1 d . . . . .
H43 H 0.0873 0.3756 0.5294 0.035 Uiso 1 1 calc R U . . .
C18 C 0.25567(15) -0.00753(13) 0.16692(12) 0.0332(4) Uani 1 1 d . . . . .
H18 H 0.2091 -0.0715 0.1472 0.040 Uiso 1 1 calc R U . . .
C34 C 0.25889(15) 0.24657(15) 0.77969(11) 0.0338(4) Uani 1 1 d . . . . .
C33 C 0.27984(15) 0.15939(14) 0.72922(12) 0.0333(4) Uani 1 1 d . . . . .
H33 H 0.3176 0.1081 0.7601 0.040 Uiso 1 1 calc R U . . .
C15 C 0.50357(15) 0.62089(14) 0.33682(12) 0.0345(4) Uani 1 1 d . . . . .
H15A H 0.4739 0.6837 0.3158 0.052 Uiso 1 1 calc R U . . .
H15B H 0.5270 0.5806 0.2856 0.052 Uiso 1 1 calc R U . . .
H15C H 0.5724 0.6392 0.3847 0.052 Uiso 1 1 calc R U . . .
C30 C 0.48662(17) 0.34896(13) 0.17930(12) 0.0369(4) Uani 1 1 d . . . . .
H30A H 0.5238 0.3172 0.1307 0.055 Uiso 1 1 calc R U . . .
H30B H 0.5341 0.4137 0.2050 0.055 Uiso 1 1 calc R U . . .
H30C H 0.4065 0.3627 0.1543 0.055 Uiso 1 1 calc R U . . .
C8 C -0.04370(15) 0.27590(14) 0.26013(13) 0.0370(4) Uani 1 1 d . . . . .
H8A H -0.0350 0.3136 0.3206 0.055 Uiso 1 1 calc R U . . .
H8B H -0.0874 0.2079 0.2609 0.055 Uiso 1 1 calc R U . . .
H8C H -0.0874 0.3141 0.2150 0.055 Uiso 1 1 calc R U . . .
C14 C 0.35781(15) 0.62360(13) 0.44642(12) 0.0332(4) Uani 1 1 d . . . . .
H14A H 0.4229 0.6519 0.4948 0.050 Uiso 1 1 calc R U . . .
H14B H 0.2979 0.5817 0.4726 0.050 Uiso 1 1 calc R U . . .
H14C H 0.3218 0.6800 0.4178 0.050 Uiso 1 1 calc R U . . .
C35 C 0.19959(15) 0.31873(14) 0.73349(11) 0.0311(3) Uani 1 1 d . . . . .
H35 H 0.1812 0.3776 0.7674 0.037 Uiso 1 1 calc R U . . .
C22 C 0.18702(16) -0.02658(12) 0.31690(12) 0.0326(4) Uani 1 1 d . . . . .
H22 H 0.1799 0.0209 0.3712 0.039 Uiso 1 1 calc R U . . .
C29 C 0.60277(15) 0.24739(14) 0.28953(14) 0.0399(4) Uani 1 1 d . . . . .
H29A H 0.6322 0.2080 0.2406 0.060 Uiso 1 1 calc R U . . .
H29B H 0.5979 0.2056 0.3409 0.060 Uiso 1 1 calc R U . . .
H29C H 0.6571 0.3101 0.3097 0.060 Uiso 1 1 calc R U . . .
C37 C 0.26893(15) 0.04154(13) 0.58804(12) 0.0322(4) Uani 1 1 d . . . . .
H37 H 0.2480 0.0445 0.5208 0.039 Uiso 1 1 calc R U . . .
C10 C 0.1524(2) 0.57954(16) 0.07323(15) 0.0571(7) Uani 1 1 d . . . . .
H10 H 0.0828 0.5394 0.0330 0.069 Uiso 1 1 calc R U . . .
C39 C 0.39899(18) 0.02154(17) 0.60729(16) 0.0484(5) Uani 1 1 d . . . . .
H39A H 0.4496 0.0801 0.5915 0.073 Uiso 1 1 calc R U . . .
H39B H 0.4103 -0.0408 0.5705 0.073 Uiso 1 1 calc R U . . .
H39C H 0.4203 0.0125 0.6721 0.073 Uiso 1 1 calc R U . . .
C45 C 0.1660(2) 0.49789(14) 0.62246(14) 0.0466(5) Uani 1 1 d . . . . .
H45A H 0.1710 0.5165 0.6880 0.070 Uiso 1 1 calc R U . . .
H45B H 0.1244 0.5480 0.5885 0.070 Uiso 1 1 calc R U . . .
H45C H 0.2462 0.4979 0.6069 0.070 Uiso 1 1 calc R U . . .
C23 C 0.06168(17) -0.06905(17) 0.27204(16) 0.0468(5) Uani 1 1 d . . . . .
H23A H 0.0182 -0.0124 0.2519 0.070 Uiso 1 1 calc R U . . .
H23B H 0.0208 -0.1047 0.3161 0.070 Uiso 1 1 calc R U . . .
H23C H 0.0655 -0.1174 0.2193 0.070 Uiso 1 1 calc R U . . .
C40 C 0.30302(18) 0.26385(19) 0.88162(12) 0.0469(5) Uani 1 1 d . . . . .
H40 H 0.3304 0.1981 0.9014 0.056 Uiso 1 1 calc R U . . .
C25 C 0.3159(2) -0.00964(16) 0.00986(14) 0.0519(6) Uani 1 1 d . . . . .
H25 H 0.3732 0.0338 -0.0198 0.062 Uiso 1 1 calc R U . . .
C38 C 0.1874(2) -0.04675(15) 0.61522(16) 0.0481(5) Uani 1 1 d . . . . .
H38A H 0.2039 -0.0500 0.6813 0.072 Uiso 1 1 calc R U . . .
H38B H 0.2015 -0.1118 0.5840 0.072 Uiso 1 1 calc R U . . .
H38C H 0.1045 -0.0350 0.5977 0.072 Uiso 1 1 calc R U . . .
C24 C 0.25587(19) -0.11304(16) 0.35146(16) 0.0500(5) Uani 1 1 d . . . . .
H24A H 0.2122 -0.1503 0.3931 0.075 Uiso 1 1 calc R U . . .
H24B H 0.3341 -0.0838 0.3838 0.075 Uiso 1 1 calc R U . . .
H24C H 0.2655 -0.1605 0.2997 0.075 Uiso 1 1 calc R U . . .
C41 C 0.2071(2) 0.2899(2) 0.93676(13) 0.0552(6) Uani 1 1 d . . . . .
H41A H 0.1793 0.3550 0.9199 0.083 Uiso 1 1 calc R U . . .
H41B H 0.2394 0.2966 1.0019 0.083 Uiso 1 1 calc R U . . .
H41C H 0.1407 0.2351 0.9242 0.083 Uiso 1 1 calc R U . . .
C44 C -0.02485(19) 0.38764(19) 0.62516(17) 0.0546(6) Uani 1 1 d . . . . .
H44A H -0.0706 0.3209 0.6034 0.082 Uiso 1 1 calc R U . . .
H44B H -0.0659 0.4425 0.5983 0.082 Uiso 1 1 calc R U . . .
H44C H -0.0170 0.3978 0.6918 0.082 Uiso 1 1 calc R U . . .
C12 C 0.1156(2) 0.6831(2) 0.1037(2) 0.0703(8) Uani 1 1 d . . . . .
H12A H 0.0524 0.6728 0.1410 0.105 Uiso 1 1 calc R U . . .
H12B H 0.0867 0.7174 0.0501 0.105 Uiso 1 1 calc R U . . .
H12C H 0.1840 0.7259 0.1398 0.105 Uiso 1 1 calc R U . . .
C27 C 0.1925(3) -0.0100(3) -0.04545(17) 0.0798(9) Uani 1 1 d . . . . .
H27A H 0.1350 -0.0552 -0.0200 0.120 Uiso 1 1 calc R U . . .
H27B H 0.1937 -0.0349 -0.1090 0.120 Uiso 1 1 calc R U . . .
H27C H 0.1698 0.0600 -0.0428 0.120 Uiso 1 1 calc R U . . .
C11 C 0.2528(3) 0.59407(19) 0.01724(15) 0.0698(8) Uani 1 1 d . . . . .
H11A H 0.3202 0.6378 0.0536 0.105 Uiso 1 1 calc R U . . .
H11B H 0.2255 0.6268 -0.0378 0.105 Uiso 1 1 calc R U . . .
H11C H 0.2775 0.5270 -0.0002 0.105 Uiso 1 1 calc R U . . .
C26 C 0.3543(3) -0.11717(19) 0.0093(2) 0.0814(10) Uani 1 1 d . . . . .
H26A H 0.4334 -0.1143 0.0452 0.122 Uiso 1 1 calc R U . . .
H26B H 0.3563 -0.1443 -0.0536 0.122 Uiso 1 1 calc R U . . .
H26C H 0.2978 -0.1622 0.0360 0.122 Uiso 1 1 calc R U . . .
C42 C 0.4095(2) 0.3455(3) 0.90147(15) 0.0830(10) Uani 1 1 d . . . . .
H42A H 0.4719 0.3247 0.8679 0.125 Uiso 1 1 calc R U . . .
H42B H 0.4394 0.3532 0.9670 0.125 Uiso 1 1 calc R U . . .
H42C H 0.3858 0.4111 0.8824 0.125 Uiso 1 1 calc R U . . .


#==============================================================================

# MOLECULAR GEOMETRY

_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
As1 C1 1.9845(14) . ?
As1 As3 2.4514(2) . ?
As1 As2 2.4530(2) . ?
As2 C16 1.9819(15) . ?
As2 As3 2.4747(2) . ?
As3 C31 1.9926(15) . ?
C1 C2 1.407(2) . ?
C1 C6 1.418(2) . ?
C21 C20 1.390(2) . ?
C21 C16 1.413(2) . ?
C21 C28 1.527(2) . ?
C2 C3 1.394(2) . ?
C2 C7 1.520(2) . ?
C16 C17 1.418(2) . ?
C6 C5 1.387(2) . ?
C6 C13 1.5333(19) . ?
C17 C18 1.387(2) . ?
C17 C22 1.526(2) . ?
C31 C32 1.410(2) . ?
C31 C36 1.413(2) . ?
C7 C9 1.530(2) . ?
C7 C8 1.531(2) . ?
C7 H7 1.0000 . ?
C32 C33 1.398(2) . ?
C32 C37 1.519(2) . ?
C13 C14 1.524(2) . ?
C13 C15 1.533(2) . ?
C13 H13 1.0000 . ?
C28 C30 1.528(2) . ?
C28 C29 1.531(2) . ?
C28 H28 1.0000 . ?
C4 C3 1.381(2) . ?
C4 C5 1.389(2) . ?
C4 C10 1.522(2) . ?
C3 H3 0.9500 . ?
C19 C18 1.387(2) . ?
C19 C20 1.390(2) . ?
C19 C25 1.517(2) . ?
C5 H5 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C36 C35 1.391(2) . ?
C36 C43 1.521(2) . ?
C20 H20 0.9500 . ?
C43 C44 1.522(2) . ?
C43 C45 1.537(3) . ?
C43 H43 1.0000 . ?
C18 H18 0.9500 . ?
C34 C33 1.382(3) . ?
C34 C35 1.389(3) . ?
C34 C40 1.520(2) . ?
C33 H33 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C35 H35 0.9500 . ?
C22 C23 1.525(3) . ?
C22 C24 1.527(3) . ?
C22 H22 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C37 C38 1.531(2) . ?
C37 C39 1.531(3) . ?
C37 H37 1.0000 . ?
C10 C12 1.521(4) . ?
C10 C11 1.522(4) . ?
C10 H10 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C40 C41 1.516(3) . ?
C40 C42 1.519(3) . ?
C40 H40 1.0000 . ?
C25 C26 1.521(4) . ?
C25 C27 1.530(4) . ?
C25 H25 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 As1 As3 113.54(4) . . ?
C1 As1 As2 112.57(4) . . ?
As3 As1 As2 60.609(7) . . ?
C16 As2 As1 109.62(4) . . ?
C16 As2 As3 105.77(4) . . ?
As1 As2 As3 59.664(6) . . ?
C31 As3 As1 95.48(4) . . ?
C31 As3 As2 97.96(4) . . ?
As1 As3 As2 59.727(7) . . ?
C2 C1 C6 119.49(13) . . ?
C2 C1 As1 128.03(11) . . ?
C6 C1 As1 112.29(10) . . ?
C20 C21 C16 118.93(14) . . ?
C20 C21 C28 118.27(14) . . ?
C16 C21 C28 122.65(14) . . ?
C3 C2 C1 118.69(14) . . ?
C3 C2 C7 117.60(13) . . ?
C1 C2 C7 123.70(13) . . ?
C21 C16 C17 119.52(14) . . ?
C21 C16 As2 118.68(11) . . ?
C17 C16 As2 120.86(12) . . ?
C5 C6 C1 119.04(13) . . ?
C5 C6 C13 117.85(13) . . ?
C1 C6 C13 123.11(13) . . ?
C18 C17 C16 118.61(15) . . ?
C18 C17 C22 117.81(14) . . ?
C16 C17 C22 123.51(15) . . ?
C32 C31 C36 119.34(14) . . ?
C32 C31 As3 121.04(11) . . ?
C36 C31 As3 119.53(11) . . ?
C2 C7 C9 112.35(13) . . ?
C2 C7 C8 111.07(13) . . ?
C9 C7 C8 110.72(14) . . ?
C2 C7 H7 107.5 . . ?
C9 C7 H7 107.5 . . ?
C8 C7 H7 107.5 . . ?
C33 C32 C31 118.68(15) . . ?
C33 C32 C37 117.30(15) . . ?
C31 C32 C37 123.99(15) . . ?
C14 C13 C15 109.79(13) . . ?
C14 C13 C6 110.85(13) . . ?
C15 C13 C6 113.35(12) . . ?
C14 C13 H13 107.5 . . ?
C15 C13 H13 107.5 . . ?
C6 C13 H13 107.5 . . ?
C21 C28 C30 113.67(13) . . ?
C21 C28 C29 109.87(13) . . ?
C30 C28 C29 110.46(14) . . ?
C21 C28 H28 107.5 . . ?
C30 C28 H28 107.5 . . ?
C29 C28 H28 107.5 . . ?
C3 C4 C5 117.92(15) . . ?
C3 C4 C10 121.11(15) . . ?
C5 C4 C10 120.98(15) . . ?
C4 C3 C2 122.65(14) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C18 C19 C20 117.50(16) . . ?
C18 C19 C25 121.27(15) . . ?
C20 C19 C25 121.22(16) . . ?
C6 C5 C4 122.16(14) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C35 C36 C31 119.02(15) . . ?
C35 C36 C43 117.38(14) . . ?
C31 C36 C43 123.58(14) . . ?
C21 C20 C19 122.48(15) . . ?
C21 C20 H20 118.8 . . ?
C19 C20 H20 118.8 . . ?
C36 C43 C44 111.37(14) . . ?
C36 C43 C45 111.47(15) . . ?
C44 C43 C45 110.00(16) . . ?
C36 C43 H43 107.9 . . ?
C44 C43 H43 107.9 . . ?
C45 C43 H43 107.9 . . ?
C17 C18 C19 122.93(15) . . ?
C17 C18 H18 118.5 . . ?
C19 C18 H18 118.5 . . ?
C33 C34 C35 117.63(16) . . ?
C33 C34 C40 120.81(17) . . ?
C35 C34 C40 121.53(18) . . ?
C34 C33 C32 122.66(16) . . ?
C34 C33 H33 118.7 . . ?
C32 C33 H33 118.7 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C34 C35 C36 122.39(16) . . ?
C34 C35 H35 118.8 . . ?
C36 C35 H35 118.8 . . ?
C23 C22 C17 113.51(15) . . ?
C23 C22 C24 110.63(15) . . ?
C17 C22 C24 110.24(15) . . ?
C23 C22 H22 107.4 . . ?
C17 C22 H22 107.4 . . ?
C24 C22 H22 107.4 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C32 C37 C38 110.62(14) . . ?
C32 C37 C39 112.31(16) . . ?
C38 C37 C39 110.97(15) . . ?
C32 C37 H37 107.6 . . ?
C38 C37 H37 107.6 . . ?
C39 C37 H37 107.6 . . ?
C12 C10 C4 110.6(2) . . ?
C12 C10 C11 110.32(17) . . ?
C4 C10 C11 112.3(2) . . ?
C12 C10 H10 107.8 . . ?
C4 C10 H10 107.8 . . ?
C11 C10 H10 107.8 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C41 C40 C42 111.1(2) . . ?
C41 C40 C34 113.05(16) . . ?
C42 C40 C34 110.41(16) . . ?
C41 C40 H40 107.3 . . ?
C42 C40 H40 107.3 . . ?
C34 C40 H40 107.3 . . ?
C19 C25 C26 111.6(2) . . ?
C19 C25 C27 110.69(19) . . ?
C26 C25 C27 111.5(2) . . ?
C19 C25 H25 107.6 . . ?
C26 C25 H25 107.6 . . ?
C27 C25 H25 107.6 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -2.6(2) . . . . ?
As1 C1 C2 C3 171.88(13) . . . . ?
C6 C1 C2 C7 178.34(14) . . . . ?
As1 C1 C2 C7 -7.1(2) . . . . ?
C20 C21 C16 C17 1.9(2) . . . . ?
C28 C21 C16 C17 -173.67(14) . . . . ?
C20 C21 C16 As2 170.91(12) . . . . ?
C28 C21 C16 As2 -4.7(2) . . . . ?
C2 C1 C6 C5 2.4(2) . . . . ?
As1 C1 C6 C5 -172.98(12) . . . . ?
C2 C1 C6 C13 -178.44(14) . . . . ?
As1 C1 C6 C13 6.22(18) . . . . ?
C21 C16 C17 C18 -1.4(2) . . . . ?
As2 C16 C17 C18 -170.18(13) . . . . ?
C21 C16 C17 C22 175.30(15) . . . . ?
As2 C16 C17 C22 6.6(2) . . . . ?
C3 C2 C7 C9 46.8(2) . . . . ?
C1 C2 C7 C9 -134.13(16) . . . . ?
C3 C2 C7 C8 -77.80(19) . . . . ?
C1 C2 C7 C8 101.23(18) . . . . ?
C36 C31 C32 C33 -5.6(2) . . . . ?
As3 C31 C32 C33 177.91(11) . . . . ?
C36 C31 C32 C37 172.41(14) . . . . ?
As3 C31 C32 C37 -4.1(2) . . . . ?
C5 C6 C13 C14 90.57(18) . . . . ?
C1 C6 C13 C14 -88.64(18) . . . . ?
C5 C6 C13 C15 -33.4(2) . . . . ?
C1 C6 C13 C15 147.36(15) . . . . ?
C20 C21 C28 C30 39.1(2) . . . . ?
C16 C21 C28 C30 -145.30(16) . . . . ?
C20 C21 C28 C29 -85.26(19) . . . . ?
C16 C21 C28 C29 90.36(18) . . . . ?
C5 C4 C3 C2 1.4(3) . . . . ?
C10 C4 C3 C2 -178.9(2) . . . . ?
C1 C2 C3 C4 0.8(3) . . . . ?
C7 C2 C3 C4 179.84(17) . . . . ?
C1 C6 C5 C4 -0.2(3) . . . . ?
C13 C6 C5 C4 -179.40(17) . . . . ?
C3 C4 C5 C6 -1.7(3) . . . . ?
C10 C4 C5 C6 178.6(2) . . . . ?
C32 C31 C36 C35 5.2(2) . . . . ?
As3 C31 C36 C35 -178.31(11) . . . . ?
C32 C31 C36 C43 -173.45(14) . . . . ?
As3 C31 C36 C43 3.1(2) . . . . ?
C16 C21 C20 C19 -1.3(3) . . . . ?
C28 C21 C20 C19 174.48(16) . . . . ?
C18 C19 C20 C21 0.2(3) . . . . ?
C25 C19 C20 C21 179.71(19) . . . . ?
C35 C36 C43 C44 -67.2(2) . . . . ?
C31 C36 C43 C44 111.46(18) . . . . ?
C35 C36 C43 C45 56.11(19) . . . . ?
C31 C36 C43 C45 -125.26(16) . . . . ?
C16 C17 C18 C19 0.3(3) . . . . ?
C22 C17 C18 C19 -176.62(17) . . . . ?
C20 C19 C18 C17 0.3(3) . . . . ?
C25 C19 C18 C17 -179.20(19) . . . . ?
C35 C34 C33 C32 2.4(3) . . . . ?
C40 C34 C33 C32 -175.70(16) . . . . ?
C31 C32 C33 C34 1.8(2) . . . . ?
C37 C32 C33 C34 -176.31(15) . . . . ?
C33 C34 C35 C36 -2.9(3) . . . . ?
C40 C34 C35 C36 175.19(16) . . . . ?
C31 C36 C35 C34 -0.9(2) . . . . ?
C43 C36 C35 C34 177.81(15) . . . . ?
C18 C17 C22 C23 -47.9(2) . . . . ?
C16 C17 C22 C23 135.33(17) . . . . ?
C18 C17 C22 C24 76.8(2) . . . . ?
C16 C17 C22 C24 -99.94(19) . . . . ?
C33 C32 C37 C38 67.4(2) . . . . ?
C31 C32 C37 C38 -110.65(18) . . . . ?
C33 C32 C37 C39 -57.2(2) . . . . ?
C31 C32 C37 C39 124.76(17) . . . . ?
C3 C4 C10 C12 120.9(2) . . . . ?
C5 C4 C10 C12 -59.4(3) . . . . ?
C3 C4 C10 C11 -115.4(2) . . . . ?
C5 C4 C10 C11 64.3(3) . . . . ?
C33 C34 C40 C41 -129.2(2) . . . . ?
C35 C34 C40 C41 52.8(3) . . . . ?
C33 C34 C40 C42 105.6(2) . . . . ?
C35 C34 C40 C42 -72.4(3) . . . . ?
C18 C19 C25 C26 -57.9(3) . . . . ?
C20 C19 C25 C26 122.6(2) . . . . ?
C18 C19 C25 C27 66.9(3) . . . . ?
C20 C19 C25 C27 -112.6(2) . . . . ?

_refine_diff_density_max         0.462
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.052


####################################################################### 
# 
# 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_ax1791_Cp2TiAs2Tip2_cmp3a
_database_code_depnum_ccdc_archive 'CCDC 2041967'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-02 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H56 As2 Ti'
_chemical_formula_sum            'C40 H56 As2 Ti'
_chemical_formula_weight         734.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

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

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

_cell_length_a                   18.7002(3)
_cell_length_b                   11.2416(2)
_cell_length_c                   17.3895(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3655.62(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9868
_cell_measurement_theta_min      4.59
_cell_measurement_theta_max      66.61

_exptl_crystal_description       plate
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_F_000             1536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.044
_exptl_absorpt_coefficient_mu    4.170
_shelx_estimated_absorpt_T_min   0.497
_shelx_estimated_absorpt_T_max   0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         microfocus
_diffrn_radiation_monochromator  multilayer
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30223
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.589
_diffrn_reflns_theta_max         66.621
_diffrn_reflns_theta_full        66.621
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3234
_reflns_number_gt                3079
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.
 
 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0372P)²+1.7971P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3234
_refine_ls_number_parameters     201
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0644
_refine_ls_wR_factor_gt          0.0628
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.56589(2) 0.63516(2) 0.24025(2) 0.01951(8) Uani 1 1 d . . . . .
Ti1 Ti 0.5000 0.42949(4) 0.2500 0.02451(11) Uani 1 2 d S T P . .
C1 C 0.56102(11) 0.3945(2) 0.13149(13) 0.0472(5) Uani 1 1 d . . . . .
H1 H 0.6119 0.4158 0.1206 0.057 Uiso 1 1 calc R U . . .
C2 C 0.50225(11) 0.4637(2) 0.11360(12) 0.0456(5) Uani 1 1 d . . . . .
H2 H 0.5035 0.5432 0.0879 0.055 Uiso 1 1 calc R U . . .
C3 C 0.44146(11) 0.3996(2) 0.13110(13) 0.0478(6) Uani 1 1 d . . . . .
H3 H 0.3914 0.4245 0.1189 0.057 Uiso 1 1 calc R U . . .
C4 C 0.46173(12) 0.28879(19) 0.16103(14) 0.0505(6) Uani 1 1 d . . . . .
H4 H 0.4292 0.2201 0.1716 0.061 Uiso 1 1 calc R U . . .
C6 C 0.61686(8) 0.67190(13) 0.33841(8) 0.0196(3) Uani 1 1 d . . . . .
C7 C 0.59413(8) 0.75046(13) 0.39634(9) 0.0242(3) Uani 1 1 d . . . . .
C8 C 0.63721(8) 0.76874(15) 0.46057(9) 0.0272(3) Uani 1 1 d . . . . .
H8 H 0.6206 0.8204 0.4999 0.033 Uiso 1 1 calc R U . . .
C9 C 0.70317(8) 0.71466(15) 0.46935(9) 0.0252(3) Uani 1 1 d . . . . .
C10 C 0.72672(8) 0.64186(13) 0.41034(9) 0.0237(3) Uani 1 1 d . . . . .
H10 H 0.7725 0.6057 0.4145 0.028 Uiso 1 1 calc R U . . .
C11 C 0.68570(8) 0.61971(13) 0.34503(9) 0.0215(3) Uani 1 1 d . . . . .
C18 C 0.71981(8) 0.54450(15) 0.28139(9) 0.0266(3) Uani 1 1 d . . . . .
H18 H 0.6810 0.5214 0.2447 0.032 Uiso 1 1 calc R U . . .
C19 C 0.77367(18) 0.6174(2) 0.23750(14) 0.0607(8) Uani 1 1 d . . . . .
H19A H 0.7498 0.6865 0.2146 0.091 Uiso 1 1 calc R U . . .
H19B H 0.7949 0.5687 0.1967 0.091 Uiso 1 1 calc R U . . .
H19C H 0.8113 0.6445 0.2726 0.091 Uiso 1 1 calc R U . . .
C15 C 0.74905(9) 0.74027(17) 0.53955(9) 0.0314(4) Uani 1 1 d . . . . .
H15 H 0.7183 0.7826 0.5779 0.038 Uiso 1 1 calc R U . . .
C16 C 0.81104(10) 0.82346(17) 0.51882(11) 0.0375(4) Uani 1 1 d . . . . .
H16A H 0.8386 0.8420 0.5653 0.056 Uiso 1 1 calc R U . . .
H16B H 0.7920 0.8972 0.4967 0.056 Uiso 1 1 calc R U . . .
H16C H 0.8422 0.7844 0.4812 0.056 Uiso 1 1 calc R U . . .
C17 C 0.77718(10) 0.62761(18) 0.57793(11) 0.0406(5) Uani 1 1 d . . . . .
H17A H 0.8064 0.5828 0.5412 0.061 Uiso 1 1 calc R U . . .
H17B H 0.7368 0.5784 0.5947 0.061 Uiso 1 1 calc R U . . .
H17C H 0.8064 0.6492 0.6226 0.061 Uiso 1 1 calc R U . . .
C12 C 0.52528(9) 0.82203(17) 0.39041(11) 0.0363(4) Uani 1 1 d . . . . .
H12 H 0.4926 0.7789 0.3544 0.044 Uiso 1 1 calc R U . . .
C14 C 0.48627(11) 0.8355(2) 0.46682(16) 0.0527(6) Uani 1 1 d . . . . .
H14A H 0.5149 0.8849 0.5016 0.079 Uiso 1 1 calc R U . . .
H14B H 0.4791 0.7569 0.4899 0.079 Uiso 1 1 calc R U . . .
H14C H 0.4398 0.8734 0.4581 0.079 Uiso 1 1 calc R U . . .
C20 C 0.75463(15) 0.43135(19) 0.30976(13) 0.0562(6) Uani 1 1 d . . . . .
H20A H 0.7753 0.3883 0.2661 0.084 Uiso 1 1 calc R U . . .
H20B H 0.7187 0.3813 0.3349 0.084 Uiso 1 1 calc R U . . .
H20C H 0.7925 0.4511 0.3466 0.084 Uiso 1 1 calc R U . . .
C13 C 0.54013(15) 0.9437(2) 0.35609(15) 0.0659(8) Uani 1 1 d . . . . .
H13A H 0.5714 0.9887 0.3907 0.099 Uiso 1 1 calc R U . . .
H13B H 0.4950 0.9867 0.3494 0.099 Uiso 1 1 calc R U . . .
H13C H 0.5636 0.9343 0.3061 0.099 Uiso 1 1 calc R U . . .
C5 C 0.53756(12) 0.28607(18) 0.16162(14) 0.0498(5) Uani 1 1 d . . . . .
H5 H 0.5681 0.2153 0.1731 0.060 Uiso 1 1 calc R U . . .


#==============================================================================

# EXPERIMENTAL DATA

_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
As1 C6 1.9982(14) . ?
As1 As1 2.4877(3) 3_655 ?
As1 Ti1 2.6255(4) . ?
Ti1 C4 2.325(2) . ?
Ti1 C4 2.325(2) 3_655 ?
Ti1 C5 2.335(2) . ?
Ti1 C5 2.335(2) 3_655 ?
Ti1 C3 2.363(2) 3_655 ?
Ti1 C3 2.363(2) . ?
Ti1 C1 2.388(2) . ?
Ti1 C1 2.388(2) 3_655 ?
Ti1 C2 2.403(2) 3_655 ?
Ti1 C2 2.403(2) . ?
Ti1 As1 2.6255(4) 3_655 ?
C1 C2 1.382(3) . ?
C1 C5 1.397(3) . ?
C1 H1 1.0000 . ?
C2 C3 1.380(3) . ?
C2 H2 1.0000 . ?
C3 C4 1.403(3) . ?
C3 H3 1.0000 . ?
C4 C5 1.418(3) . ?
C4 H4 1.0000 . ?
C6 C7 1.405(2) . ?
C6 C11 1.419(2) . ?
C7 C8 1.392(2) . ?
C7 C12 1.522(2) . ?
C8 C9 1.384(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(2) . ?
C9 C15 1.520(2) . ?
C10 C11 1.393(2) . ?
C10 H10 0.9500 . ?
C11 C18 1.532(2) . ?
C18 C19 1.506(3) . ?
C18 C20 1.512(3) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C15 C17 1.525(3) . ?
C15 C16 1.532(3) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C12 C13 1.518(3) . ?
C12 C14 1.523(3) . ?
C12 H12 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C5 H5 1.0000 . ?

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
C6 As1 As1 110.86(4) . 3_655 ?
C6 As1 Ti1 110.53(4) . . ?
As1 As1 Ti1 61.721(6) 3_655 . ?
C4 Ti1 C4 94.29(13) . 3_655 ?
C4 Ti1 C5 35.43(8) . . ?
C4 Ti1 C5 82.86(9) 3_655 . ?
C4 Ti1 C5 82.86(9) . 3_655 ?
C4 Ti1 C5 35.43(8) 3_655 3_655 ?
C5 Ti1 C5 92.69(13) . 3_655 ?
C4 Ti1 C3 128.91(9) . 3_655 ?
C4 Ti1 C3 34.80(8) 3_655 3_655 ?
C5 Ti1 C3 109.78(9) . 3_655 ?
C5 Ti1 C3 57.70(7) 3_655 3_655 ?
C4 Ti1 C3 34.80(8) . . ?
C4 Ti1 C3 128.91(9) 3_655 . ?
C5 Ti1 C3 57.70(7) . . ?
C5 Ti1 C3 109.78(9) 3_655 . ?
C3 Ti1 C3 163.68(12) 3_655 . ?
C4 Ti1 C1 57.37(8) . . ?
C4 Ti1 C1 108.36(9) 3_655 . ?
C5 Ti1 C1 34.38(8) . . ?
C5 Ti1 C1 126.71(9) 3_655 . ?
C3 Ti1 C1 120.68(9) 3_655 . ?
C3 Ti1 C1 56.15(8) . . ?
C4 Ti1 C1 108.36(9) . 3_655 ?
C4 Ti1 C1 57.37(8) 3_655 3_655 ?
C5 Ti1 C1 126.71(9) . 3_655 ?
C5 Ti1 C1 34.39(8) 3_655 3_655 ?
C3 Ti1 C1 56.15(8) 3_655 3_655 ?
C3 Ti1 C1 120.68(9) . 3_655 ?
C1 Ti1 C1 161.03(12) . 3_655 ?
C4 Ti1 C2 139.47(8) . 3_655 ?
C4 Ti1 C2 57.15(8) 3_655 3_655 ?
C5 Ti1 C2 139.92(8) . 3_655 ?
C5 Ti1 C2 57.02(8) 3_655 3_655 ?
C3 Ti1 C2 33.63(8) 3_655 3_655 ?
C3 Ti1 C2 151.40(7) . 3_655 ?
C1 Ti1 C2 152.42(7) . 3_655 ?
C1 Ti1 C2 33.52(8) 3_655 3_655 ?
C4 Ti1 C2 57.15(8) . . ?
C4 Ti1 C2 139.47(8) 3_655 . ?
C5 Ti1 C2 57.02(8) . . ?
C5 Ti1 C2 139.92(8) 3_655 . ?
C3 Ti1 C2 151.40(7) 3_655 . ?
C3 Ti1 C2 33.64(8) . . ?
C1 Ti1 C2 33.52(8) . . ?
C1 Ti1 C2 152.42(7) 3_655 . ?
C2 Ti1 C2 161.59(11) 3_655 . ?
C4 Ti1 As1 134.46(6) . . ?
C4 Ti1 As1 119.84(6) 3_655 . ?
C5 Ti1 As1 115.10(6) . . ?
C5 Ti1 As1 142.33(6) 3_655 . ?
C3 Ti1 As1 87.94(5) 3_655 . ?
C3 Ti1 As1 106.61(7) . . ?
C1 Ti1 As1 82.25(6) . . ?
C1 Ti1 As1 115.16(6) 3_655 . ?
C2 Ti1 As1 86.05(5) 3_655 . ?
C2 Ti1 As1 77.71(5) . . ?
C4 Ti1 As1 119.84(6) . 3_655 ?
C4 Ti1 As1 134.46(6) 3_655 3_655 ?
C5 Ti1 As1 142.33(6) . 3_655 ?
C5 Ti1 As1 115.10(6) 3_655 3_655 ?
C3 Ti1 As1 106.61(7) 3_655 3_655 ?
C3 Ti1 As1 87.94(5) . 3_655 ?
C1 Ti1 As1 115.16(6) . 3_655 ?
C1 Ti1 As1 82.25(6) 3_655 3_655 ?
C2 Ti1 As1 77.71(5) 3_655 3_655 ?
C2 Ti1 As1 86.05(5) . 3_655 ?
As1 Ti1 As1 56.558(11) . 3_655 ?
C2 C1 C5 109.01(19) . . ?
C2 C1 Ti1 73.83(12) . . ?
C5 C1 Ti1 70.74(13) . . ?
C2 C1 H1 125.4 . . ?
C5 C1 H1 125.4 . . ?
Ti1 C1 H1 125.4 . . ?
C3 C2 C1 108.2(2) . . ?
C3 C2 Ti1 71.60(13) . . ?
C1 C2 Ti1 72.65(13) . . ?
C3 C2 H2 125.8 . . ?
C1 C2 H2 125.8 . . ?
Ti1 C2 H2 125.8 . . ?
C2 C3 C4 108.82(18) . . ?
C2 C3 Ti1 74.77(12) . . ?
C4 C3 Ti1 71.12(12) . . ?
C2 C3 H3 125.4 . . ?
C4 C3 H3 125.4 . . ?
Ti1 C3 H3 125.4 . . ?
C3 C4 C5 106.98(19) . . ?
C3 C4 Ti1 74.08(11) . . ?
C5 C4 Ti1 72.67(11) . . ?
C3 C4 H4 126.2 . . ?
C5 C4 H4 126.2 . . ?
Ti1 C4 H4 126.2 . . ?
C7 C6 C11 118.42(13) . . ?
C7 C6 As1 126.71(11) . . ?
C11 C6 As1 114.61(11) . . ?
C8 C7 C6 119.52(14) . . ?
C8 C7 C12 117.76(14) . . ?
C6 C7 C12 122.66(14) . . ?
C9 C8 C7 122.65(15) . . ?
C9 C8 H8 118.7 . . ?
C7 C8 H8 118.7 . . ?
C8 C9 C10 117.49(14) . . ?
C8 C9 C15 120.58(15) . . ?
C10 C9 C15 121.85(15) . . ?
C9 C10 C11 122.33(14) . . ?
C9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C10 C11 C6 119.45(14) . . ?
C10 C11 C18 117.29(13) . . ?
C6 C11 C18 123.17(14) . . ?
C19 C18 C20 109.59(18) . . ?
C19 C18 C11 110.13(14) . . ?
C20 C18 C11 114.08(14) . . ?
C19 C18 H18 107.6 . . ?
C20 C18 H18 107.6 . . ?
C11 C18 H18 107.6 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C9 C15 C17 112.88(15) . . ?
C9 C15 C16 110.72(14) . . ?
C17 C15 C16 110.42(15) . . ?
C9 C15 H15 107.5 . . ?
C17 C15 H15 107.5 . . ?
C16 C15 H15 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C12 C7 110.38(16) . . ?
C13 C12 C14 109.94(17) . . ?
C7 C12 C14 113.49(17) . . ?
C13 C12 H12 107.6 . . ?
C7 C12 H12 107.6 . . ?
C14 C12 H12 107.6 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C1 C5 C4 107.00(18) . . ?
C1 C5 Ti1 74.88(11) . . ?
C4 C5 Ti1 71.90(11) . . ?
C1 C5 H5 126.1 . . ?
C4 C5 H5 126.1 . . ?
Ti1 C5 H5 126.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 -0.8(2) . . . . ?
Ti1 C1 C2 C3 -63.21(14) . . . . ?
C5 C1 C2 Ti1 62.40(16) . . . . ?
C1 C2 C3 C4 0.5(2) . . . . ?
Ti1 C2 C3 C4 -63.44(15) . . . . ?
C1 C2 C3 Ti1 63.89(14) . . . . ?
C2 C3 C4 C5 0.1(2) . . . . ?
Ti1 C3 C4 C5 -65.74(15) . . . . ?
C2 C3 C4 Ti1 65.80(14) . . . . ?
C11 C6 C7 C8 -4.2(2) . . . . ?
As1 C6 C7 C8 -178.12(12) . . . . ?
C11 C6 C7 C12 172.78(15) . . . . ?
As1 C6 C7 C12 -1.1(2) . . . . ?
C6 C7 C8 C9 1.7(2) . . . . ?
C12 C7 C8 C9 -175.50(16) . . . . ?
C7 C8 C9 C10 1.4(2) . . . . ?
C7 C8 C9 C15 178.29(16) . . . . ?
C8 C9 C10 C11 -1.8(2) . . . . ?
C15 C9 C10 C11 -178.67(15) . . . . ?
C9 C10 C11 C6 -0.8(2) . . . . ?
C9 C10 C11 C18 175.93(15) . . . . ?
C7 C6 C11 C10 3.8(2) . . . . ?
As1 C6 C11 C10 178.43(11) . . . . ?
C7 C6 C11 C18 -172.69(14) . . . . ?
As1 C6 C11 C18 1.93(19) . . . . ?
C10 C11 C18 C19 -75.4(2) . . . . ?
C6 C11 C18 C19 101.2(2) . . . . ?
C10 C11 C18 C20 48.3(2) . . . . ?
C6 C11 C18 C20 -135.13(18) . . . . ?
C8 C9 C15 C17 131.23(17) . . . . ?
C10 C9 C15 C17 -52.0(2) . . . . ?
C8 C9 C15 C16 -104.40(18) . . . . ?
C10 C9 C15 C16 72.3(2) . . . . ?
C8 C7 C12 C13 84.1(2) . . . . ?
C6 C7 C12 C13 -93.0(2) . . . . ?
C8 C7 C12 C14 -39.9(2) . . . . ?
C6 C7 C12 C14 143.08(17) . . . . ?
C2 C1 C5 C4 0.8(2) . . . . ?
Ti1 C1 C5 C4 65.22(15) . . . . ?
C2 C1 C5 Ti1 -64.38(15) . . . . ?
C3 C4 C5 C1 -0.5(2) . . . . ?
Ti1 C4 C5 C1 -67.24(15) . . . . ?
C3 C4 C5 Ti1 66.69(14) . . . . ?

_refine_diff_density_max         0.295
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.050


####################################################################### 
# 
# 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_ax1936_Cp2Ti_Cp2TiAs2Ter2_cmp4
_database_code_depnum_ccdc_archive 'CCDC 2041969'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-02 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H60 As2 Ti, C6 D6'
_chemical_formula_sum            'C64 H60 As2 D6 Ti'
_chemical_formula_weight         1038.94

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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   11.4194(6)
_cell_length_b                   11.4914(6)
_cell_length_c                   19.9143(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.4830(10)
_cell_angle_gamma                90
_cell_volume                     2608.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9086
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      30.09

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_F_000             1076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    1.463
_shelx_estimated_absorpt_T_min   0.660
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            79401
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.787
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             15203
_reflns_number_gt                14112
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.
 
 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0357P)²+0.1528P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 6253 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.023(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         15203
_refine_ls_number_parameters     616
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0633
_refine_ls_wR_factor_gt          0.0614
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.73597(2) 0.66646(2) 0.33092(2) 0.01672(5) Uani 1 1 d . . . . .
As2 As 0.65869(2) 0.56572(2) 0.22961(2) 0.01655(5) Uani 1 1 d . . . . .
Ti1 Ti 0.77091(4) 0.43814(4) 0.32447(2) 0.01919(9) Uani 1 1 d . . . . .
C1 C 0.8874(2) 0.7474(2) 0.31549(12) 0.0180(5) Uani 1 1 d . . . . .
C2 C 0.9382(2) 0.7838(2) 0.25590(12) 0.0207(5) Uani 1 1 d . . . . .
C3 C 1.0506(2) 0.8337(3) 0.26036(14) 0.0275(6) Uani 1 1 d . . . . .
H3 H 1.0849 0.8571 0.2202 0.033 Uiso 1 1 calc R U . . .
C4 C 1.1127(2) 0.8500(3) 0.32133(15) 0.0297(6) Uani 1 1 d . . . . .
H4 H 1.1902 0.8804 0.3229 0.036 Uiso 1 1 calc R U . . .
C5 C 1.0607(2) 0.8212(3) 0.38016(14) 0.0248(5) Uani 1 1 d . . . . .
H5 H 1.1018 0.8346 0.4223 0.030 Uiso 1 1 calc R U . . .
C6 C 0.9479(2) 0.7726(2) 0.37809(12) 0.0196(5) Uani 1 1 d . . . . .
C7 C 0.8776(2) 0.7805(2) 0.18694(12) 0.0211(5) Uani 1 1 d . . . . .
C8 C 0.9237(2) 0.7190(2) 0.13349(13) 0.0254(5) Uani 1 1 d . . . . .
C9 C 0.8666(3) 0.7236(3) 0.06967(14) 0.0314(6) Uani 1 1 d . . . . .
H9 H 0.8971 0.6797 0.0343 0.038 Uiso 1 1 calc R U . . .
C10 C 0.7668(3) 0.7904(3) 0.05631(14) 0.0314(6) Uani 1 1 d . . . . .
C11 C 0.7252(2) 0.8556(3) 0.10897(14) 0.0280(6) Uani 1 1 d . . . . .
H11 H 0.6582 0.9037 0.1005 0.034 Uiso 1 1 calc R U . . .
C12 C 0.7789(2) 0.8521(2) 0.17322(12) 0.0230(5) Uani 1 1 d . . . . .
C13 C 1.0381(2) 0.6531(3) 0.14104(14) 0.0354(7) Uani 1 1 d . . . . .
H13A H 1.0352 0.5865 0.1102 0.053 Uiso 1 1 calc R U . . .
H13B H 1.0506 0.6252 0.1874 0.053 Uiso 1 1 calc R U . . .
H13C H 1.1027 0.7046 0.1304 0.053 Uiso 1 1 calc R U . . .
C14 C 0.7078(3) 0.7980(3) -0.01353(15) 0.0457(8) Uani 1 1 d . . . . .
H14A H 0.6236 0.7835 -0.0113 0.068 Uiso 1 1 calc R U . . .
H14B H 0.7417 0.7396 -0.0425 0.068 Uiso 1 1 calc R U . . .
H14C H 0.7199 0.8758 -0.0320 0.068 Uiso 1 1 calc R U . . .
C15 C 0.7347(3) 0.9310(3) 0.22709(14) 0.0297(6) Uani 1 1 d . . . . .
H15A H 0.6797 0.9879 0.2064 0.045 Uiso 1 1 calc R U . . .
H15B H 0.8011 0.9720 0.2498 0.045 Uiso 1 1 calc R U . . .
H15C H 0.6948 0.8843 0.2599 0.045 Uiso 1 1 calc R U . . .
C16 C 0.8936(2) 0.7568(2) 0.44459(12) 0.0199(5) Uani 1 1 d . . . . .
C17 C 0.9321(2) 0.6685(3) 0.49005(12) 0.0231(5) Uani 1 1 d . . . . .
C18 C 0.8841(2) 0.6613(3) 0.55287(12) 0.0281(5) Uani 1 1 d . . . . .
H18 H 0.9100 0.6015 0.5832 0.034 Uiso 1 1 calc R U . . .
C19 C 0.7996(2) 0.7392(3) 0.57211(14) 0.0310(6) Uani 1 1 d . . . . .
C20 C 0.7627(2) 0.8258(3) 0.52698(14) 0.0301(6) Uani 1 1 d . . . . .
H20 H 0.7041 0.8790 0.5393 0.036 Uiso 1 1 calc R U . . .
C21 C 0.8091(2) 0.8370(2) 0.46408(13) 0.0243(5) Uani 1 1 d . . . . .
C22 C 1.0231(3) 0.5812(3) 0.47206(14) 0.0327(6) Uani 1 1 d . . . . .
H22A H 1.1015 0.6150 0.4803 0.049 Uiso 1 1 calc R U . . .
H22B H 1.0109 0.5603 0.4244 0.049 Uiso 1 1 calc R U . . .
H22C H 1.0164 0.5113 0.4998 0.049 Uiso 1 1 calc R U . . .
C23 C 0.7524(3) 0.7342(4) 0.64167(16) 0.0454(9) Uani 1 1 d . . . . .
H23A H 0.7671 0.6569 0.6611 0.068 Uiso 1 1 calc R U . . .
H23B H 0.6678 0.7494 0.6383 0.068 Uiso 1 1 calc R U . . .
H23C H 0.7918 0.7932 0.6705 0.068 Uiso 1 1 calc R U . . .
C24 C 0.7666(3) 0.9347(3) 0.41805(15) 0.0318(6) Uani 1 1 d . . . . .
H24A H 0.7037 0.9061 0.3867 0.048 Uiso 1 1 calc R U . . .
H24B H 0.8318 0.9630 0.3927 0.048 Uiso 1 1 calc R U . . .
H24C H 0.7369 0.9985 0.4449 0.048 Uiso 1 1 calc R U . . .
C25 C 0.4856(2) 0.5389(2) 0.23206(11) 0.0170(5) Uani 1 1 d . . . . .
C26 C 0.4492(2) 0.4462(2) 0.18835(12) 0.0181(4) Uani 1 1 d . . . . .
C27 C 0.3324(2) 0.4093(2) 0.18434(13) 0.0223(5) Uani 1 1 d . . . . .
H27 H 0.3102 0.3448 0.1566 0.027 Uiso 1 1 calc R U . . .
C28 C 0.2490(2) 0.4648(2) 0.21981(13) 0.0246(5) Uani 1 1 d . . . . .
H28 H 0.1700 0.4383 0.2173 0.030 Uiso 1 1 calc R U . . .
C29 C 0.2822(2) 0.5600(3) 0.25922(12) 0.0240(5) Uani 1 1 d . . . . .
H29 H 0.2243 0.6003 0.2824 0.029 Uiso 1 1 calc R U . . .
C30 C 0.3986(2) 0.5985(2) 0.26582(12) 0.0185(5) Uani 1 1 d . . . . .
C31 C 0.5305(2) 0.3866(2) 0.14217(12) 0.0192(5) Uani 1 1 d . . . . .
C32 C 0.5640(2) 0.4444(2) 0.08405(12) 0.0227(5) Uani 1 1 d . . . . .
C33 C 0.6344(3) 0.3876(3) 0.03983(14) 0.0290(6) Uani 1 1 d . . . . .
H33 H 0.6587 0.4282 0.0015 0.035 Uiso 1 1 calc R U . . .
C34 C 0.6703(2) 0.2729(3) 0.05010(14) 0.0283(6) Uani 1 1 d . . . . .
C35 C 0.6323(2) 0.2151(2) 0.10595(14) 0.0265(5) Uani 1 1 d . . . . .
H35 H 0.6547 0.1363 0.1134 0.032 Uiso 1 1 calc R U . . .
C36 C 0.5620(2) 0.2694(2) 0.15154(12) 0.0220(5) Uani 1 1 d . . . . .
C37 C 0.5237(3) 0.5672(3) 0.06770(13) 0.0315(6) Uani 1 1 d . . . . .
H37A H 0.5790 0.6228 0.0894 0.047 Uiso 1 1 calc R U . . .
H37B H 0.4456 0.5795 0.0842 0.047 Uiso 1 1 calc R U . . .
H37C H 0.5205 0.5788 0.0189 0.047 Uiso 1 1 calc R U . . .
C38 C 0.7481(3) 0.2119(3) 0.00214(17) 0.0414(8) Uani 1 1 d . . . . .
H38A H 0.8304 0.2308 0.0142 0.062 Uiso 1 1 calc R U . . .
H38B H 0.7275 0.2378 -0.0440 0.062 Uiso 1 1 calc R U . . .
H38C H 0.7367 0.1276 0.0052 0.062 Uiso 1 1 calc R U . . .
C39 C 0.5221(3) 0.1976(2) 0.20952(15) 0.0305(6) Uani 1 1 d . . . . .
H39A H 0.4811 0.1280 0.1920 0.046 Uiso 1 1 calc R U . . .
H39B H 0.4689 0.2440 0.2356 0.046 Uiso 1 1 calc R U . . .
H39C H 0.5905 0.1744 0.2386 0.046 Uiso 1 1 calc R U . . .
C40 C 0.4193(2) 0.7069(2) 0.30657(12) 0.0183(4) Uani 1 1 d . . . . .
C41 C 0.4453(2) 0.8117(2) 0.27419(12) 0.0200(5) Uani 1 1 d . . . . .
C42 C 0.4576(2) 0.9138(2) 0.31146(13) 0.0236(5) Uani 1 1 d . . . . .
H42 H 0.4750 0.9843 0.2892 0.028 Uiso 1 1 calc R U . . .
C43 C 0.4452(2) 0.9156(2) 0.38056(13) 0.0240(5) Uani 1 1 d . . . . .
C44 C 0.4156(2) 0.8125(2) 0.41166(13) 0.0245(5) Uani 1 1 d . . . . .
H44 H 0.4066 0.8123 0.4588 0.029 Uiso 1 1 calc R U . . .
C45 C 0.3989(2) 0.7091(2) 0.37566(12) 0.0203(5) Uani 1 1 d . . . . .
C46 C 0.4550(3) 0.8153(3) 0.19864(13) 0.0271(6) Uani 1 1 d . . . . .
H46A H 0.4614 0.8963 0.1839 0.041 Uiso 1 1 calc R U . . .
H46B H 0.3851 0.7797 0.1763 0.041 Uiso 1 1 calc R U . . .
H46C H 0.5249 0.7721 0.1869 0.041 Uiso 1 1 calc R U . . .
C47 C 0.4612(3) 1.0259(3) 0.42110(15) 0.0332(6) Uani 1 1 d . . . . .
H47A H 0.3843 1.0554 0.4325 0.050 Uiso 1 1 calc R U . . .
H47B H 0.5005 1.0844 0.3946 0.050 Uiso 1 1 calc R U . . .
H47C H 0.5091 1.0096 0.4625 0.050 Uiso 1 1 calc R U . . .
C48 C 0.3527(3) 0.6044(2) 0.41180(14) 0.0289(6) Uani 1 1 d . . . . .
H48A H 0.3777 0.6087 0.4597 0.043 Uiso 1 1 calc R U . . .
H48B H 0.3837 0.5331 0.3925 0.043 Uiso 1 1 calc R U . . .
H48C H 0.2668 0.6035 0.4066 0.043 Uiso 1 1 calc R U . . .
C49 C 0.6192(3) 0.4645(3) 0.39999(15) 0.0341(7) Uani 1 1 d . . . . .
H49 H 0.5782 0.5363 0.4018 0.041 Uiso 1 1 calc R U . . .
C50 C 0.5884(2) 0.3710(3) 0.35826(15) 0.0323(6) Uani 1 1 d . . . . .
H50 H 0.5225 0.3674 0.3269 0.039 Uiso 1 1 calc R U . . .
C51 C 0.6725(3) 0.2821(3) 0.37075(15) 0.0329(6) Uani 1 1 d . . . . .
H51 H 0.6738 0.2085 0.3491 0.039 Uiso 1 1 calc R U . . .
C52 C 0.7541(3) 0.3231(3) 0.42145(15) 0.0358(7) Uani 1 1 d . . . . .
H52 H 0.8200 0.2813 0.4402 0.043 Uiso 1 1 calc R U . . .
C53 C 0.7217(3) 0.4347(3) 0.43921(14) 0.0357(7) Uani 1 1 d . . . . .
H53 H 0.7616 0.4827 0.4720 0.043 Uiso 1 1 calc R U . . .
C54 C 0.9019(2) 0.4604(3) 0.23617(15) 0.0352(7) Uani 1 1 d . . . . .
H54 H 0.8886 0.5174 0.2021 0.042 Uiso 1 1 calc R U . . .
C55 C 0.9659(2) 0.4766(3) 0.29794(15) 0.0288(6) Uani 1 1 d . . . . .
H55 H 1.0039 0.5465 0.3126 0.035 Uiso 1 1 calc R U . . .
C56 C 0.9642(2) 0.3724(3) 0.33414(15) 0.0316(6) Uani 1 1 d . . . . .
H56 H 0.9998 0.3592 0.3779 0.038 Uiso 1 1 calc R U . . .
C57 C 0.8999(3) 0.2902(3) 0.29374(19) 0.0407(8) Uani 1 1 d . . . . .
H57 H 0.8854 0.2114 0.3052 0.049 Uiso 1 1 calc R U . . .
C58 C 0.8614(3) 0.3464(3) 0.23359(17) 0.0421(8) Uani 1 1 d . . . . .
H58 H 0.8156 0.3122 0.1974 0.051 Uiso 1 1 calc R U . . .
C60 C 1.0838(4) 0.1405(4) 0.1798(2) 0.0607(11) Uani 1 1 d . . . . .
D60 H 1.0742 0.1968 0.2140 0.073 Uiso 1 1 calc R U . . .
C61 C 1.1914(3) 0.0928(4) 0.17184(19) 0.0521(10) Uani 1 1 d . . . . .
D61 H 1.2568 0.1152 0.2007 0.063 Uiso 1 1 calc R U . . .
C62 C 1.2051(3) 0.0119(4) 0.1216(2) 0.0560(10) Uani 1 1 d . . . . .
D62 H 1.2800 -0.0213 0.1158 0.067 Uiso 1 1 calc R U . . .
C63 C 1.1092(4) -0.0207(3) 0.07980(19) 0.0512(9) Uani 1 1 d . . . . .
D63 H 1.1185 -0.0756 0.0449 0.061 Uiso 1 1 calc R U . . .
C64 C 1.0022(3) 0.0257(3) 0.0888(2) 0.0523(9) Uani 1 1 d . . . . .
D64 H 0.9363 0.0020 0.0607 0.063 Uiso 1 1 calc R U . . .
C65 C 0.9886(3) 0.1067(4) 0.1382(2) 0.0606(11) Uani 1 1 d . . . . .
D65 H 0.9136 0.1397 0.1439 0.073 Uiso 1 1 calc R U . . .


#==============================================================================

# MOLECULAR GEOMETRY

_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
As1 C1 2.004(2) . ?
As1 As2 2.4440(3) . ?
As1 Ti1 2.6581(5) . ?
As2 C25 2.004(2) . ?
As2 Ti1 2.6582(5) . ?
Ti1 C56 2.330(3) . ?
Ti1 C51 2.336(3) . ?
Ti1 C57 2.355(3) . ?
Ti1 C52 2.358(3) . ?
Ti1 C50 2.358(3) . ?
Ti1 C55 2.361(3) . ?
Ti1 C49 2.381(3) . ?
Ti1 C58 2.384(3) . ?
Ti1 C53 2.386(3) . ?
Ti1 C54 2.391(3) . ?
C1 C2 1.415(3) . ?
C1 C6 1.418(3) . ?
C2 C3 1.404(4) . ?
C2 C7 1.500(3) . ?
C3 C4 1.382(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(4) . ?
C5 H5 0.9500 . ?
C6 C16 1.507(3) . ?
C7 C8 1.406(4) . ?
C7 C12 1.409(3) . ?
C8 C9 1.394(4) . ?
C8 C13 1.510(4) . ?
C9 C10 1.386(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.395(4) . ?
C10 C14 1.511(4) . ?
C11 C12 1.385(4) . ?
C11 H11 0.9500 . ?
C12 C15 1.515(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.406(4) . ?
C16 C17 1.412(4) . ?
C17 C18 1.398(3) . ?
C17 C22 1.504(4) . ?
C18 C19 1.387(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(4) . ?
C19 C23 1.518(4) . ?
C20 C21 1.395(4) . ?
C20 H20 0.9500 . ?
C21 C24 1.511(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C30 1.410(3) . ?
C25 C26 1.421(3) . ?
C26 C27 1.397(3) . ?
C26 C31 1.510(3) . ?
C27 C28 1.376(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.386(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.399(3) . ?
C29 H29 0.9500 . ?
C30 C40 1.498(3) . ?
C31 C36 1.404(4) . ?
C31 C32 1.407(3) . ?
C32 C33 1.391(4) . ?
C32 C37 1.514(4) . ?
C33 C34 1.392(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.387(4) . ?
C34 C38 1.515(4) . ?
C35 C36 1.395(4) . ?
C35 H35 0.9500 . ?
C36 C39 1.511(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.406(3) . ?
C40 C45 1.410(3) . ?
C41 C42 1.391(4) . ?
C41 C46 1.516(3) . ?
C42 C43 1.392(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.388(4) . ?
C43 C47 1.508(4) . ?
C44 C45 1.395(4) . ?
C44 H44 0.9500 . ?
C45 C48 1.513(4) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.391(5) . ?
C49 C53 1.409(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.413(4) . ?
C50 H50 0.9500 . ?
C51 C52 1.412(4) . ?
C51 H51 0.9500 . ?
C52 C53 1.387(5) . ?
C52 H52 0.9500 . ?
C53 H53 0.9500 . ?
C54 C58 1.389(5) . ?
C54 C55 1.405(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.398(4) . ?
C55 H55 0.9500 . ?
C56 C57 1.417(5) . ?
C56 H56 0.9500 . ?
C57 C58 1.408(5) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C60 C61 1.363(5) . ?
C60 C65 1.381(6) . ?
C60 D60 0.9500 . ?
C61 C62 1.382(6) . ?
C61 D61 0.9500 . ?
C62 C63 1.386(6) . ?
C62 D62 0.9500 . ?
C63 C64 1.355(5) . ?
C63 D63 0.9500 . ?
C64 C65 1.370(5) . ?
C64 D64 0.9500 . ?
C65 D65 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 As1 As2 111.41(7) . . ?
C1 As1 Ti1 108.50(7) . . ?
As2 As1 Ti1 62.632(13) . . ?
C25 As2 As1 111.10(7) . . ?
C25 As2 Ti1 109.36(7) . . ?
As1 As2 Ti1 62.630(13) . . ?
C56 Ti1 C51 101.24(11) . . ?
C56 Ti1 C57 35.22(11) . . ?
C51 Ti1 C57 82.63(11) . . ?
C56 Ti1 C52 82.80(11) . . ?
C51 Ti1 C52 35.02(11) . . ?
C57 Ti1 C52 83.76(12) . . ?
C56 Ti1 C50 136.02(11) . . ?
C51 Ti1 C50 35.04(11) . . ?
C57 Ti1 C50 114.54(12) . . ?
C52 Ti1 C50 57.68(10) . . ?
C56 Ti1 C55 34.68(10) . . ?
C51 Ti1 C55 135.65(11) . . ?
C57 Ti1 C55 57.58(11) . . ?
C52 Ti1 C55 114.41(11) . . ?
C50 Ti1 C55 170.67(11) . . ?
C56 Ti1 C49 135.30(11) . . ?
C51 Ti1 C49 57.49(11) . . ?
C57 Ti1 C49 138.29(12) . . ?
C52 Ti1 C49 57.00(11) . . ?
C50 Ti1 C49 34.13(11) . . ?
C55 Ti1 C49 148.15(11) . . ?
C56 Ti1 C58 57.80(11) . . ?
C51 Ti1 C58 101.61(12) . . ?
C57 Ti1 C58 34.56(13) . . ?
C52 Ti1 C58 115.75(13) . . ?
C50 Ti1 C58 120.21(12) . . ?
C55 Ti1 C58 56.96(11) . . ?
C49 Ti1 C58 154.34(12) . . ?
C56 Ti1 C53 101.11(11) . . ?
C51 Ti1 C53 57.49(11) . . ?
C57 Ti1 C53 115.11(13) . . ?
C52 Ti1 C53 33.99(12) . . ?
C50 Ti1 C53 57.17(11) . . ?
C55 Ti1 C53 119.83(11) . . ?
C49 Ti1 C53 34.37(11) . . ?
C58 Ti1 C53 149.08(13) . . ?
C56 Ti1 C54 57.54(10) . . ?
C51 Ti1 C54 135.23(12) . . ?
C57 Ti1 C54 57.09(12) . . ?
C52 Ti1 C54 138.43(11) . . ?
C50 Ti1 C54 148.01(11) . . ?
C55 Ti1 C54 34.38(10) . . ?
C49 Ti1 C54 164.30(11) . . ?
C58 Ti1 C54 33.82(12) . . ?
C53 Ti1 C54 154.21(11) . . ?
C56 Ti1 As1 117.39(8) . . ?
C51 Ti1 As1 131.42(8) . . ?
C57 Ti1 As1 145.43(9) . . ?
C52 Ti1 As1 119.60(9) . . ?
C50 Ti1 As1 99.87(8) . . ?
C55 Ti1 As1 88.41(7) . . ?
C49 Ti1 As1 74.14(8) . . ?
C58 Ti1 As1 123.13(10) . . ?
C53 Ti1 As1 85.71(8) . . ?
C54 Ti1 As1 91.87(8) . . ?
C56 Ti1 As2 130.61(8) . . ?
C51 Ti1 As2 118.76(8) . . ?
C57 Ti1 As2 119.72(9) . . ?
C52 Ti1 As2 146.25(8) . . ?
C50 Ti1 As2 89.26(7) . . ?
C55 Ti1 As2 99.10(7) . . ?
C49 Ti1 As2 92.34(8) . . ?
C58 Ti1 As2 85.24(9) . . ?
C53 Ti1 As2 123.92(9) . . ?
C54 Ti1 As2 73.42(7) . . ?
As1 Ti1 As2 54.738(11) . . ?
C2 C1 C6 118.3(2) . . ?
C2 C1 As1 131.84(18) . . ?
C6 C1 As1 109.80(17) . . ?
C3 C2 C1 119.2(2) . . ?
C3 C2 C7 115.9(2) . . ?
C1 C2 C7 124.8(2) . . ?
C4 C3 C2 122.0(2) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C5 119.1(2) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 120.7(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 120.3(2) . . ?
C5 C6 C16 116.6(2) . . ?
C1 C6 C16 122.9(2) . . ?
C8 C7 C12 118.6(2) . . ?
C8 C7 C2 122.2(2) . . ?
C12 C7 C2 118.8(2) . . ?
C9 C8 C7 119.7(2) . . ?
C9 C8 C13 117.6(2) . . ?
C7 C8 C13 122.6(2) . . ?
C10 C9 C8 122.0(3) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C9 C10 C11 117.8(3) . . ?
C9 C10 C14 121.6(3) . . ?
C11 C10 C14 120.5(3) . . ?
C12 C11 C10 121.8(3) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C11 C12 C7 120.0(2) . . ?
C11 C12 C15 119.3(2) . . ?
C7 C12 C15 120.6(2) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 119.1(2) . . ?
C21 C16 C6 119.3(2) . . ?
C17 C16 C6 121.4(2) . . ?
C18 C17 C16 119.5(2) . . ?
C18 C17 C22 119.2(3) . . ?
C16 C17 C22 121.3(2) . . ?
C19 C18 C17 121.7(3) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C20 118.2(2) . . ?
C18 C19 C23 121.3(3) . . ?
C20 C19 C23 120.5(3) . . ?
C19 C20 C21 122.0(3) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C20 C21 C16 119.4(3) . . ?
C20 C21 C24 119.2(2) . . ?
C16 C21 C24 121.4(2) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 117.9(2) . . ?
C30 C25 As2 131.36(18) . . ?
C26 C25 As2 110.62(16) . . ?
C27 C26 C25 120.3(2) . . ?
C27 C26 C31 116.6(2) . . ?
C25 C26 C31 123.1(2) . . ?
C28 C27 C26 121.2(2) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C27 C28 C29 118.8(2) . . ?
C27 C28 H28 120.6 . . ?
C29 C28 H28 120.6 . . ?
C28 C29 C30 121.9(2) . . ?
C28 C29 H29 119.0 . . ?
C30 C29 H29 119.0 . . ?
C29 C30 C25 119.6(2) . . ?
C29 C30 C40 115.5(2) . . ?
C25 C30 C40 124.8(2) . . ?
C36 C31 C32 118.8(2) . . ?
C36 C31 C26 121.1(2) . . ?
C32 C31 C26 119.7(2) . . ?
C33 C32 C31 119.8(2) . . ?
C33 C32 C37 118.8(2) . . ?
C31 C32 C37 121.5(2) . . ?
C32 C33 C34 121.9(3) . . ?
C32 C33 H33 119.1 . . ?
C34 C33 H33 119.1 . . ?
C35 C34 C33 117.8(2) . . ?
C35 C34 C38 120.5(3) . . ?
C33 C34 C38 121.6(3) . . ?
C34 C35 C36 121.9(3) . . ?
C34 C35 H35 119.1 . . ?
C36 C35 H35 119.1 . . ?
C35 C36 C31 119.7(2) . . ?
C35 C36 C39 117.7(2) . . ?
C31 C36 C39 122.6(2) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 C45 119.0(2) . . ?
C41 C40 C30 119.7(2) . . ?
C45 C40 C30 120.9(2) . . ?
C42 C41 C40 119.7(2) . . ?
C42 C41 C46 119.7(2) . . ?
C40 C41 C46 120.5(2) . . ?
C41 C42 C43 121.8(2) . . ?
C41 C42 H42 119.1 . . ?
C43 C42 H42 119.1 . . ?
C44 C43 C42 118.1(2) . . ?
C44 C43 C47 120.2(2) . . ?
C42 C43 C47 121.7(3) . . ?
C43 C44 C45 121.8(2) . . ?
C43 C44 H44 119.1 . . ?
C45 C44 H44 119.1 . . ?
C44 C45 C40 119.4(2) . . ?
C44 C45 C48 118.3(2) . . ?
C40 C45 C48 122.2(2) . . ?
C41 C46 H46A 109.5 . . ?
C41 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C41 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 C53 108.4(3) . . ?
C50 C49 Ti1 72.03(16) . . ?
C53 C49 Ti1 73.01(16) . . ?
C50 C49 H49 125.8 . . ?
C53 C49 H49 125.8 . . ?
Ti1 C49 H49 120.9 . . ?
C49 C50 C51 108.0(3) . . ?
C49 C50 Ti1 73.83(16) . . ?
C51 C50 Ti1 71.60(16) . . ?
C49 C50 H50 126.0 . . ?
C51 C50 H50 126.0 . . ?
Ti1 C50 H50 120.4 . . ?
C52 C51 C50 107.2(3) . . ?
C52 C51 Ti1 73.36(16) . . ?
C50 C51 Ti1 73.36(16) . . ?
C52 C51 H51 126.4 . . ?
C50 C51 H51 126.4 . . ?
Ti1 C51 H51 118.9 . . ?
C53 C52 C51 108.4(3) . . ?
C53 C52 Ti1 74.12(17) . . ?
C51 C52 Ti1 71.62(16) . . ?
C53 C52 H52 125.8 . . ?
C51 C52 H52 125.8 . . ?
Ti1 C52 H52 120.2 . . ?
C52 C53 C49 108.0(3) . . ?
C52 C53 Ti1 71.89(17) . . ?
C49 C53 Ti1 72.62(16) . . ?
C52 C53 H53 126.0 . . ?
C49 C53 H53 126.0 . . ?
Ti1 C53 H53 121.2 . . ?
C58 C54 C55 108.2(3) . . ?
C58 C54 Ti1 72.83(17) . . ?
C55 C54 Ti1 71.68(16) . . ?
C58 C54 H54 125.9 . . ?
C55 C54 H54 125.9 . . ?
Ti1 C54 H54 121.3 . . ?
C56 C55 C54 108.3(3) . . ?
C56 C55 Ti1 71.43(16) . . ?
C54 C55 Ti1 73.94(16) . . ?
C56 C55 H55 125.8 . . ?
C54 C55 H55 125.8 . . ?
Ti1 C55 H55 120.5 . . ?
C55 C56 C57 107.5(3) . . ?
C55 C56 Ti1 73.89(15) . . ?
C57 C56 Ti1 73.34(16) . . ?
C55 C56 H56 126.2 . . ?
C57 C56 H56 126.2 . . ?
Ti1 C56 H56 118.5 . . ?
C58 C57 C56 107.5(3) . . ?
C58 C57 Ti1 73.85(17) . . ?
C56 C57 Ti1 71.44(16) . . ?
C58 C57 H57 126.2 . . ?
C56 C57 H57 126.2 . . ?
Ti1 C57 H57 120.3 . . ?
C54 C58 C57 108.4(3) . . ?
C54 C58 Ti1 73.35(17) . . ?
C57 C58 Ti1 71.59(17) . . ?
C54 C58 H58 125.8 . . ?
C57 C58 H58 125.8 . . ?
Ti1 C58 H58 121.0 . . ?
C61 C60 C65 119.9(4) . . ?
C61 C60 D60 120.0 . . ?
C65 C60 D60 120.0 . . ?
C60 C61 C62 119.8(4) . . ?
C60 C61 D61 120.1 . . ?
C62 C61 D61 120.1 . . ?
C61 C62 C63 119.8(3) . . ?
C61 C62 D62 120.1 . . ?
C63 C62 D62 120.1 . . ?
C64 C63 C62 120.0(4) . . ?
C64 C63 D63 120.0 . . ?
C62 C63 D63 120.0 . . ?
C63 C64 C65 120.3(4) . . ?
C63 C64 D64 119.9 . . ?
C65 C64 D64 119.9 . . ?
C64 C65 C60 120.2(4) . . ?
C64 C65 D65 119.9 . . ?
C60 C65 D65 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 5.6(4) . . . . ?
As1 C1 C2 C3 -176.5(2) . . . . ?
C6 C1 C2 C7 -170.1(2) . . . . ?
As1 C1 C2 C7 7.8(4) . . . . ?
C1 C2 C3 C4 -0.9(4) . . . . ?
C7 C2 C3 C4 175.3(3) . . . . ?
C2 C3 C4 C5 -3.1(5) . . . . ?
C3 C4 C5 C6 2.1(4) . . . . ?
C4 C5 C6 C1 2.7(4) . . . . ?
C4 C5 C6 C16 -173.4(3) . . . . ?
C2 C1 C6 C5 -6.6(4) . . . . ?
As1 C1 C6 C5 175.1(2) . . . . ?
C2 C1 C6 C16 169.3(2) . . . . ?
As1 C1 C6 C16 -9.1(3) . . . . ?
C3 C2 C7 C8 61.6(3) . . . . ?
C1 C2 C7 C8 -122.5(3) . . . . ?
C3 C2 C7 C12 -110.9(3) . . . . ?
C1 C2 C7 C12 65.0(3) . . . . ?
C12 C7 C8 C9 -4.4(4) . . . . ?
C2 C7 C8 C9 -176.9(3) . . . . ?
C12 C7 C8 C13 171.6(3) . . . . ?
C2 C7 C8 C13 -0.8(4) . . . . ?
C7 C8 C9 C10 2.1(4) . . . . ?
C13 C8 C9 C10 -174.2(3) . . . . ?
C8 C9 C10 C11 1.1(5) . . . . ?
C8 C9 C10 C14 178.0(3) . . . . ?
C9 C10 C11 C12 -1.8(4) . . . . ?
C14 C10 C11 C12 -178.8(3) . . . . ?
C10 C11 C12 C7 -0.6(4) . . . . ?
C10 C11 C12 C15 175.8(3) . . . . ?
C8 C7 C12 C11 3.7(4) . . . . ?
C2 C7 C12 C11 176.4(2) . . . . ?
C8 C7 C12 C15 -172.7(2) . . . . ?
C2 C7 C12 C15 0.0(4) . . . . ?
C5 C6 C16 C21 101.5(3) . . . . ?
C1 C6 C16 C21 -74.5(3) . . . . ?
C5 C6 C16 C17 -73.6(3) . . . . ?
C1 C6 C16 C17 110.4(3) . . . . ?
C21 C16 C17 C18 1.1(4) . . . . ?
C6 C16 C17 C18 176.2(2) . . . . ?
C21 C16 C17 C22 -179.4(2) . . . . ?
C6 C16 C17 C22 -4.3(4) . . . . ?
C16 C17 C18 C19 -0.3(4) . . . . ?
C22 C17 C18 C19 -179.8(3) . . . . ?
C17 C18 C19 C20 0.1(4) . . . . ?
C17 C18 C19 C23 -177.0(3) . . . . ?
C18 C19 C20 C21 -0.9(4) . . . . ?
C23 C19 C20 C21 176.3(3) . . . . ?
C19 C20 C21 C16 1.7(4) . . . . ?
C19 C20 C21 C24 -178.8(3) . . . . ?
C17 C16 C21 C20 -1.8(4) . . . . ?
C6 C16 C21 C20 -177.0(2) . . . . ?
C17 C16 C21 C24 178.7(2) . . . . ?
C6 C16 C21 C24 3.5(4) . . . . ?
C30 C25 C26 C27 -5.9(3) . . . . ?
As2 C25 C26 C27 177.27(19) . . . . ?
C30 C25 C26 C31 171.3(2) . . . . ?
As2 C25 C26 C31 -5.6(3) . . . . ?
C25 C26 C27 C28 3.1(4) . . . . ?
C31 C26 C27 C28 -174.2(2) . . . . ?
C26 C27 C28 C29 1.0(4) . . . . ?
C27 C28 C29 C30 -2.4(4) . . . . ?
C28 C29 C30 C25 -0.5(4) . . . . ?
C28 C29 C30 C40 176.3(2) . . . . ?
C26 C25 C30 C29 4.5(3) . . . . ?
As2 C25 C30 C29 -179.38(19) . . . . ?
C26 C25 C30 C40 -171.9(2) . . . . ?
As2 C25 C30 C40 4.2(4) . . . . ?
C27 C26 C31 C36 -68.7(3) . . . . ?
C25 C26 C31 C36 114.1(3) . . . . ?
C27 C26 C31 C32 103.5(3) . . . . ?
C25 C26 C31 C32 -73.8(3) . . . . ?
C36 C31 C32 C33 -4.7(4) . . . . ?
C26 C31 C32 C33 -177.0(2) . . . . ?
C36 C31 C32 C37 174.4(2) . . . . ?
C26 C31 C32 C37 2.1(4) . . . . ?
C31 C32 C33 C34 2.1(4) . . . . ?
C37 C32 C33 C34 -177.0(3) . . . . ?
C32 C33 C34 C35 0.9(4) . . . . ?
C32 C33 C34 C38 -179.3(3) . . . . ?
C33 C34 C35 C36 -1.1(4) . . . . ?
C38 C34 C35 C36 179.1(3) . . . . ?
C34 C35 C36 C31 -1.6(4) . . . . ?
C34 C35 C36 C39 178.1(3) . . . . ?
C32 C31 C36 C35 4.4(4) . . . . ?
C26 C31 C36 C35 176.7(2) . . . . ?
C32 C31 C36 C39 -175.2(2) . . . . ?
C26 C31 C36 C39 -3.0(4) . . . . ?
C29 C30 C40 C41 -107.8(3) . . . . ?
C25 C30 C40 C41 68.7(3) . . . . ?
C29 C30 C40 C45 64.2(3) . . . . ?
C25 C30 C40 C45 -119.2(3) . . . . ?
C45 C40 C41 C42 4.0(4) . . . . ?
C30 C40 C41 C42 176.2(2) . . . . ?
C45 C40 C41 C46 -173.4(2) . . . . ?
C30 C40 C41 C46 -1.2(3) . . . . ?
C40 C41 C42 C43 0.2(4) . . . . ?
C46 C41 C42 C43 177.6(2) . . . . ?
C41 C42 C43 C44 -2.3(4) . . . . ?
C41 C42 C43 C47 178.6(2) . . . . ?
C42 C43 C44 C45 0.2(4) . . . . ?
C47 C43 C44 C45 179.3(2) . . . . ?
C43 C44 C45 C40 4.0(4) . . . . ?
C43 C44 C45 C48 -172.7(2) . . . . ?
C41 C40 C45 C44 -6.0(3) . . . . ?
C30 C40 C45 C44 -178.1(2) . . . . ?
C41 C40 C45 C48 170.6(2) . . . . ?
C30 C40 C45 C48 -1.5(4) . . . . ?
C53 C49 C50 C51 -0.5(3) . . . . ?
Ti1 C49 C50 C51 63.9(2) . . . . ?
C53 C49 C50 Ti1 -64.46(19) . . . . ?
C49 C50 C51 C52 0.7(3) . . . . ?
Ti1 C50 C51 C52 66.1(2) . . . . ?
C49 C50 C51 Ti1 -65.38(19) . . . . ?
C50 C51 C52 C53 -0.6(3) . . . . ?
Ti1 C51 C52 C53 65.5(2) . . . . ?
C50 C51 C52 Ti1 -66.07(19) . . . . ?
C51 C52 C53 C49 0.2(3) . . . . ?
Ti1 C52 C53 C49 64.11(19) . . . . ?
C51 C52 C53 Ti1 -63.9(2) . . . . ?
C50 C49 C53 C52 0.2(3) . . . . ?
Ti1 C49 C53 C52 -63.6(2) . . . . ?
C50 C49 C53 Ti1 63.82(19) . . . . ?
C58 C54 C55 C56 -0.5(3) . . . . ?
Ti1 C54 C55 C56 63.61(19) . . . . ?
C58 C54 C55 Ti1 -64.1(2) . . . . ?
C54 C55 C56 C57 0.9(3) . . . . ?
Ti1 C55 C56 C57 66.2(2) . . . . ?
C54 C55 C56 Ti1 -65.24(19) . . . . ?
C55 C56 C57 C58 -1.0(3) . . . . ?
Ti1 C56 C57 C58 65.6(2) . . . . ?
C55 C56 C57 Ti1 -66.53(19) . . . . ?
C55 C54 C58 C57 -0.1(3) . . . . ?
Ti1 C54 C58 C57 -63.5(2) . . . . ?
C55 C54 C58 Ti1 63.39(19) . . . . ?
C56 C57 C58 C54 0.7(3) . . . . ?
Ti1 C57 C58 C54 64.6(2) . . . . ?
C56 C57 C58 Ti1 -64.0(2) . . . . ?
C65 C60 C61 C62 0.8(7) . . . . ?
C60 C61 C62 C63 -0.3(6) . . . . ?
C61 C62 C63 C64 -0.8(6) . . . . ?
C62 C63 C64 C65 1.3(6) . . . . ?
C63 C64 C65 C60 -0.8(7) . . . . ?
C61 C60 C65 C64 -0.2(7) . . . . ?

_refine_diff_density_max         0.571
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.052


####################################################################### 
# 
# 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_ks1484_TipAsIiPr2_cmp5ab
_database_code_depnum_ccdc_archive 'CCDC 2041971'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-02 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H39 As N2, 0.5 (C5 H12)'
_chemical_formula_sum            'C26.50 H45 As N2'
_chemical_formula_weight         466.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   36.358(7)
_cell_length_b                   9.3907(19)
_cell_length_c                   15.843(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.12(3)
_cell_angle_gamma                90
_cell_volume                     5408.2(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    14119
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      29.46

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_F_000             2008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.260
_exptl_absorpt_coefficient_mu    1.271
_shelx_estimated_absorpt_T_min   0.630
_shelx_estimated_absorpt_T_max   0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_process_details   'LANA (Stoe & Cie, 2012)'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_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  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50734
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.240
_diffrn_reflns_theta_max         29.332
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7312
_reflns_number_gt                4947
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.
 
 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 > 2σ(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 0.500 0.000 0.362 420 77 ' '
2 0.000 0.500 0.250 420 77 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;                       
The unit cell contains four pentane molecules, which have
been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0509P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7312
_refine_ls_number_parameters     254
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0783
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_restrained_S_all      0.855
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.63389(4) 0.43228(17) 0.42172(9) 0.0314(3) Uani 1 1 d . . . . .
C2 C 0.64130(4) 0.57865(17) 0.43041(9) 0.0332(3) Uani 1 1 d . . . . .
C3 C 0.67530(4) 0.63270(17) 0.40564(9) 0.0347(3) Uani 1 1 d . . . . .
H3 H 0.6802 0.7313 0.4132 0.042 Uiso 1 1 calc R U . . .
C4 C 0.70192(4) 0.54710(18) 0.37050(9) 0.0346(3) Uani 1 1 d . . . . .
C5 C 0.69344(4) 0.40464(18) 0.35786(9) 0.0350(3) Uani 1 1 d . . . . .
H5 H 0.7110 0.3455 0.3313 0.042 Uiso 1 1 calc R U . . .
C6 C 0.66034(4) 0.34474(17) 0.38241(9) 0.0332(3) Uani 1 1 d . . . . .
C7 C 0.61373(5) 0.68471(18) 0.46498(10) 0.0377(4) Uani 1 1 d . . . . .
H7 H 0.5910 0.6300 0.4788 0.045 Uiso 1 1 calc R U . . .
C8 C 0.60267(6) 0.7960(2) 0.39936(13) 0.0529(5) Uani 1 1 d . . . . .
H8A H 0.6243 0.8514 0.3838 0.079 Uiso 1 1 calc R U . . .
H8B H 0.5841 0.8597 0.4229 0.079 Uiso 1 1 calc R U . . .
H8C H 0.5924 0.7484 0.3491 0.079 Uiso 1 1 calc R U . . .
C9 C 0.62728(6) 0.7553(2) 0.54616(12) 0.0532(5) Uani 1 1 d . . . . .
H9A H 0.6344 0.6819 0.5873 0.080 Uiso 1 1 calc R U . . .
H9B H 0.6076 0.8141 0.5692 0.080 Uiso 1 1 calc R U . . .
H9C H 0.6486 0.8154 0.5343 0.080 Uiso 1 1 calc R U . . .
C10 C 0.74055(5) 0.5987(2) 0.35201(11) 0.0424(4) Uani 1 1 d . . . . .
H10 H 0.7497 0.5418 0.3034 0.051 Uiso 1 1 calc R U . . .
C11 C 0.76549(5) 0.5658(2) 0.42823(14) 0.0577(5) Uani 1 1 d . . . . .
H11A H 0.7570 0.6189 0.4774 0.087 Uiso 1 1 calc R U . . .
H11B H 0.7908 0.5939 0.4159 0.087 Uiso 1 1 calc R U . . .
H11C H 0.7647 0.4635 0.4403 0.087 Uiso 1 1 calc R U . . .
C12 C 0.74334(5) 0.7549(2) 0.32821(12) 0.0509(5) Uani 1 1 d . . . . .
H12A H 0.7274 0.7740 0.2790 0.076 Uiso 1 1 calc R U . . .
H12B H 0.7689 0.7776 0.3145 0.076 Uiso 1 1 calc R U . . .
H12C H 0.7356 0.8138 0.3757 0.076 Uiso 1 1 calc R U . . .
C13 C 0.65308(5) 0.18748(17) 0.36611(10) 0.0383(4) Uani 1 1 d . . . . .
H13 H 0.6387 0.1512 0.4148 0.046 Uiso 1 1 calc R U . . .
C14 C 0.68734(6) 0.0965(2) 0.36108(17) 0.0637(6) Uani 1 1 d . . . . .
H14A H 0.7007 0.1208 0.3099 0.096 Uiso 1 1 calc R U . . .
H14B H 0.6804 -0.0042 0.3593 0.096 Uiso 1 1 calc R U . . .
H14C H 0.7032 0.1141 0.4108 0.096 Uiso 1 1 calc R U . . .
C15 C 0.62907(7) 0.1682(2) 0.28733(13) 0.0629(6) Uani 1 1 d . . . . .
H15A H 0.6062 0.2218 0.2935 0.094 Uiso 1 1 calc R U . . .
H15B H 0.6234 0.0669 0.2797 0.094 Uiso 1 1 calc R U . . .
H15C H 0.6422 0.2034 0.2381 0.094 Uiso 1 1 calc R U . . .
C16 C 0.59423(4) 0.40410(18) 0.57728(9) 0.0356(3) Uani 1 1 d . . . . .
C17 C 0.58240(5) 0.4868(2) 0.70625(11) 0.0471(4) Uani 1 1 d . . . . .
H17 H 0.5696 0.5268 0.7523 0.057 Uiso 1 1 calc R U . . .
C18 C 0.61713(5) 0.4419(2) 0.70762(10) 0.0443(4) Uani 1 1 d . . . . .
H18 H 0.6338 0.4453 0.7544 0.053 Uiso 1 1 calc R U . . .
C19 C 0.53086(5) 0.5020(2) 0.59625(12) 0.0509(5) Uani 1 1 d . . . . .
H19 H 0.5310 0.5041 0.5331 0.061 Uiso 1 1 calc R U . . .
C20 C 0.50409(7) 0.3896(4) 0.62161(18) 0.0944(10) Uani 1 1 d . . . . .
H20A H 0.5112 0.2981 0.5972 0.142 Uiso 1 1 calc R U . . .
H20B H 0.4794 0.4154 0.6010 0.142 Uiso 1 1 calc R U . . .
H20C H 0.5041 0.3817 0.6833 0.142 Uiso 1 1 calc R U . . .
C21 C 0.52053(8) 0.6485(3) 0.6258(2) 0.1023(11) Uani 1 1 d . . . . .
H21A H 0.5173 0.6474 0.6870 0.153 Uiso 1 1 calc R U . . .
H21B H 0.4975 0.6778 0.5978 0.153 Uiso 1 1 calc R U . . .
H21C H 0.5401 0.7159 0.6117 0.153 Uiso 1 1 calc R U . . .
C22 C 0.65765(5) 0.30815(19) 0.60840(11) 0.0426(4) Uani 1 1 d . . . . .
H22 H 0.6552 0.2748 0.5486 0.051 Uiso 1 1 calc R U . . .
C23 C 0.69137(5) 0.4014(2) 0.61531(13) 0.0548(5) Uani 1 1 d . . . . .
H23A H 0.6887 0.4823 0.5766 0.082 Uiso 1 1 calc R U . . .
H23B H 0.7131 0.3460 0.6005 0.082 Uiso 1 1 calc R U . . .
H23C H 0.6942 0.4365 0.6733 0.082 Uiso 1 1 calc R U . . .
C24 C 0.65957(6) 0.1776(2) 0.66480(14) 0.0574(5) Uani 1 1 d . . . . .
H24A H 0.6610 0.2075 0.7240 0.086 Uiso 1 1 calc R U . . .
H24B H 0.6815 0.1217 0.6514 0.086 Uiso 1 1 calc R U . . .
H24C H 0.6375 0.1193 0.6554 0.086 Uiso 1 1 calc R U . . .
N1 N 0.56832(4) 0.46483(17) 0.62556(8) 0.0415(3) Uani 1 1 d . . . . .
N2 N 0.62427(4) 0.38956(15) 0.62821(8) 0.0371(3) Uani 1 1 d . . . . .
As1 As 0.58746(2) 0.34525(2) 0.46079(2) 0.03730(6) Uani 1 1 d . . . . .


#==============================================================================

# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.407(2) . ?
C1 C6 1.418(2) . ?
C1 As1 1.9854(15) . ?
C2 C3 1.399(2) . ?
C2 C7 1.523(2) . ?
C3 C4 1.384(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(2) . ?
C4 C10 1.520(2) . ?
C5 C6 1.391(2) . ?
C5 H5 0.9500 . ?
C6 C13 1.521(2) . ?
C7 C9 1.520(2) . ?
C7 C8 1.522(3) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.518(3) . ?
C10 C11 1.527(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.513(3) . ?
C13 C15 1.520(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 N1 1.351(2) . ?
C16 N2 1.352(2) . ?
C16 As1 1.9376(16) . ?
C17 C18 1.331(3) . ?
C17 N1 1.383(2) . ?
C17 H17 0.9500 . ?
C18 N2 1.380(2) . ?
C18 H18 0.9500 . ?
C19 N1 1.472(2) . ?
C19 C20 1.496(3) . ?
C19 C21 1.504(3) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N2 1.473(2) . ?
C22 C23 1.509(3) . ?
C22 C24 1.518(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 118.62(13) . . ?
C2 C1 As1 122.28(11) . . ?
C6 C1 As1 119.08(12) . . ?
C3 C2 C1 119.70(14) . . ?
C3 C2 C7 117.07(15) . . ?
C1 C2 C7 123.23(14) . . ?
C4 C3 C2 122.06(15) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C5 117.60(14) . . ?
C3 C4 C10 123.29(15) . . ?
C5 C4 C10 118.92(14) . . ?
C4 C5 C6 122.75(15) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C5 C6 C1 119.09(15) . . ?
C5 C6 C13 119.55(14) . . ?
C1 C6 C13 121.36(14) . . ?
C9 C7 C8 110.81(16) . . ?
C9 C7 C2 112.62(14) . . ?
C8 C7 C2 111.73(13) . . ?
C9 C7 H7 107.1 . . ?
C8 C7 H7 107.1 . . ?
C2 C7 H7 107.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C4 114.98(15) . . ?
C12 C10 C11 110.50(16) . . ?
C4 C10 C11 108.64(15) . . ?
C12 C10 H10 107.5 . . ?
C4 C10 H10 107.5 . . ?
C11 C10 H10 107.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C15 110.45(17) . . ?
C14 C13 C6 114.62(15) . . ?
C15 C13 C6 110.48(14) . . ?
C14 C13 H13 107.0 . . ?
C15 C13 H13 107.0 . . ?
C6 C13 H13 107.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C16 N2 105.59(13) . . ?
N1 C16 As1 125.63(13) . . ?
N2 C16 As1 128.73(12) . . ?
C18 C17 N1 107.55(15) . . ?
C18 C17 H17 126.2 . . ?
N1 C17 H17 126.2 . . ?
C17 C18 N2 107.07(16) . . ?
C17 C18 H18 126.5 . . ?
N2 C18 H18 126.5 . . ?
N1 C19 C20 110.55(18) . . ?
N1 C19 C21 110.73(18) . . ?
C20 C19 C21 113.2(2) . . ?
N1 C19 H19 107.4 . . ?
C20 C19 H19 107.4 . . ?
C21 C19 H19 107.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 C23 110.78(16) . . ?
N2 C22 C24 108.80(15) . . ?
C23 C22 C24 113.46(17) . . ?
N2 C22 H22 107.9 . . ?
C23 C22 H22 107.9 . . ?
C24 C22 H22 107.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C16 N1 C17 109.67(15) . . ?
C16 N1 C19 124.91(14) . . ?
C17 N1 C19 125.42(14) . . ?
C16 N2 C18 110.11(14) . . ?
C16 N2 C22 125.76(14) . . ?
C18 N2 C22 123.34(14) . . ?
C16 As1 C1 94.97(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -4.3(2) . . . . ?
As1 C1 C2 C3 176.73(11) . . . . ?
C6 C1 C2 C7 174.89(14) . . . . ?
As1 C1 C2 C7 -4.1(2) . . . . ?
C1 C2 C3 C4 1.7(2) . . . . ?
C7 C2 C3 C4 -177.60(14) . . . . ?
C2 C3 C4 C5 2.0(2) . . . . ?
C2 C3 C4 C10 -172.96(15) . . . . ?
C3 C4 C5 C6 -3.0(2) . . . . ?
C10 C4 C5 C6 172.19(15) . . . . ?
C4 C5 C6 C1 0.3(2) . . . . ?
C4 C5 C6 C13 179.87(15) . . . . ?
C2 C1 C6 C5 3.4(2) . . . . ?
As1 C1 C6 C5 -177.64(11) . . . . ?
C2 C1 C6 C13 -176.19(14) . . . . ?
As1 C1 C6 C13 2.8(2) . . . . ?
C3 C2 C7 C9 -63.29(19) . . . . ?
C1 C2 C7 C9 117.48(18) . . . . ?
C3 C2 C7 C8 62.2(2) . . . . ?
C1 C2 C7 C8 -117.05(18) . . . . ?
C3 C4 C10 C12 -32.0(2) . . . . ?
C5 C4 C10 C12 153.12(16) . . . . ?
C3 C4 C10 C11 92.4(2) . . . . ?
C5 C4 C10 C11 -82.47(19) . . . . ?
C5 C6 C13 C14 26.2(2) . . . . ?
C1 C6 C13 C14 -154.21(17) . . . . ?
C5 C6 C13 C15 -99.33(19) . . . . ?
C1 C6 C13 C15 80.2(2) . . . . ?
N1 C17 C18 N2 -1.2(2) . . . . ?
N2 C16 N1 C17 -0.32(19) . . . . ?
As1 C16 N1 C17 177.43(13) . . . . ?
N2 C16 N1 C19 179.54(16) . . . . ?
As1 C16 N1 C19 -2.7(2) . . . . ?
C18 C17 N1 C16 0.9(2) . . . . ?
C18 C17 N1 C19 -178.91(17) . . . . ?
C20 C19 N1 C16 98.8(2) . . . . ?
C21 C19 N1 C16 -134.9(2) . . . . ?
C20 C19 N1 C17 -81.3(3) . . . . ?
C21 C19 N1 C17 45.0(3) . . . . ?
N1 C16 N2 C18 -0.41(19) . . . . ?
As1 C16 N2 C18 -178.06(13) . . . . ?
N1 C16 N2 C22 169.61(15) . . . . ?
As1 C16 N2 C22 -8.0(2) . . . . ?
C17 C18 N2 C16 1.0(2) . . . . ?
C17 C18 N2 C22 -169.31(16) . . . . ?
C23 C22 N2 C16 123.88(18) . . . . ?
C24 C22 N2 C16 -110.74(19) . . . . ?
C23 C22 N2 C18 -67.4(2) . . . . ?
C24 C22 N2 C18 58.0(2) . . . . ?

_refine_diff_density_max         0.500
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.052





####################################################################### 
# 
# 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_ax1818_Cp2Ti_As2Dipp2_cmp3b
_database_code_depnum_ccdc_archive 'CCDC 2041968'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-02 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H44 As2 Ti'
_chemical_formula_sum            'C34 H44 As2 Ti'
_chemical_formula_weight         650.43

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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'

#==============================================================================

# CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   12.0242(12)
_cell_length_b                   19.595(2)
_cell_length_c                   13.3094(14)
_cell_angle_alpha                90
_cell_angle_beta                 100.2503(18)
_cell_angle_gamma                90
_cell_volume                     3085.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9956
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      29.74

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.426
_shelx_estimated_absorpt_T_min   0.451
_shelx_estimated_absorpt_T_max   0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6004
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            56172
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.870
_diffrn_reflns_theta_max         29.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9006
_reflns_number_gt                7109
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Apex3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine. One of the isopropyl groups was found to be
 disordered and was split in two parts. The occupancy of each part was allowed 
 to refine freely.

 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0249P)²+0.9647P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9006
_refine_ls_number_parameters     368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0625
_refine_ls_wR_factor_gt          0.0569
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.40296(19) 0.84895(11) 0.59621(16) 0.0382(5) Uani 1 1 d . . . . .
H1 H 0.3291 0.8594 0.5611 0.046 Uiso 1 1 calc R U . . .
C2 C 0.5046(2) 0.87303(10) 0.57152(16) 0.0394(5) Uani 1 1 d . . . . .
H2 H 0.5117 0.9025 0.5164 0.047 Uiso 1 1 calc R U . . .
C3 C 0.59314(19) 0.84616(10) 0.64201(16) 0.0360(5) Uani 1 1 d . . . . .
H3 H 0.6713 0.8541 0.6431 0.043 Uiso 1 1 calc R U . . .
C4 C 0.54778(18) 0.80547(10) 0.71106(15) 0.0338(4) Uani 1 1 d . . . . .
H4 H 0.5896 0.7814 0.7674 0.041 Uiso 1 1 calc R U . . .
C5 C 0.43013(19) 0.80635(11) 0.68267(15) 0.0353(5) Uani 1 1 d . . . . .
H5 H 0.3779 0.7826 0.7156 0.042 Uiso 1 1 calc R U . . .
C6 C 0.35215(19) 0.67451(12) 0.55640(19) 0.0431(6) Uani 1 1 d . . . . .
H6 H 0.3268 0.6687 0.6195 0.052 Uiso 1 1 calc R U . . .
C7 C 0.43849(16) 0.63793(9) 0.52374(15) 0.0302(4) Uani 1 1 d . . . . .
H7 H 0.4821 0.6025 0.5603 0.036 Uiso 1 1 calc R U . . .
C8 C 0.44936(17) 0.66253(10) 0.42846(15) 0.0324(4) Uani 1 1 d . . . . .
H8 H 0.5024 0.6470 0.3885 0.039 Uiso 1 1 calc R U . . .
C9 C 0.3699(2) 0.71369(12) 0.40097(19) 0.0491(7) Uani 1 1 d . . . . .
H9 H 0.3589 0.7390 0.3391 0.059 Uiso 1 1 calc R U . . .
C10 C 0.30956(18) 0.72123(12) 0.4799(2) 0.0538(7) Uani 1 1 d . . . . .
H10 H 0.2498 0.7526 0.4817 0.065 Uiso 1 1 calc R U . . .
C11 C 0.72932(14) 0.85002(8) 0.44765(12) 0.0186(3) Uani 1 1 d . . . . .
C12 C 0.66751(14) 0.90244(9) 0.38939(13) 0.0203(3) Uani 1 1 d . . . . .
C13 C 0.71176(16) 0.96835(9) 0.39344(14) 0.0255(4) Uani 1 1 d . . . . .
H13 H 0.6691 1.0038 0.3562 0.031 Uiso 1 1 calc R U . . .
C14 C 0.81617(16) 0.98292(9) 0.45043(15) 0.0274(4) Uani 1 1 d . . . . .
H14 H 0.8444 1.0283 0.4538 0.033 Uiso 1 1 calc R U . . .
C15 C 0.87953(15) 0.93113(9) 0.50257(13) 0.0248(4) Uani 1 1 d . . . . .
H15 H 0.9525 0.9412 0.5401 0.030 Uiso 1 1 calc R U . . .
C16 C 0.83913(15) 0.86428(9) 0.50161(12) 0.0207(3) Uani 1 1 d . . . . .
C17 C 0.55782(16) 0.88843(9) 0.31540(14) 0.0271(4) Uani 1 1 d . . . . .
H17 H 0.5157 0.8524 0.3465 0.032 Uiso 1 1 calc R U . . .
C18 C 0.5851(2) 0.85978(12) 0.21524(15) 0.0411(5) Uani 1 1 d . . . . .
H18A H 0.6249 0.8945 0.1822 0.062 Uiso 1 1 calc R U . . .
H18B H 0.5147 0.8473 0.1698 0.062 Uiso 1 1 calc R U . . .
H18C H 0.6331 0.8193 0.2298 0.062 Uiso 1 1 calc R U . . .
C19 C 0.47949(18) 0.95005(11) 0.29197(18) 0.0408(5) Uani 1 1 d . . . . .
H19A H 0.4639 0.9693 0.3560 0.061 Uiso 1 1 calc R U . . .
H19B H 0.4084 0.9357 0.2493 0.061 Uiso 1 1 calc R U . . .
H19C H 0.5159 0.9846 0.2557 0.061 Uiso 1 1 calc R U . . .
C20A C 0.9194(11) 0.8060(9) 0.5507(10) 0.024(2) Uani 0.632(8) 1 d . . P A 1
H20A H 0.8742 0.7710 0.5806 0.029 Uiso 0.632(8) 1 calc R U P A 1
C21A C 1.0139(5) 0.8357(2) 0.6383(4) 0.0559(17) Uani 0.632(8) 1 d . . P A 1
H21A H 0.9779 0.8571 0.6909 0.084 Uiso 0.632(8) 1 calc R U P A 1
H21B H 1.0632 0.7986 0.6688 0.084 Uiso 0.632(8) 1 calc R U P A 1
H21C H 1.0588 0.8698 0.6093 0.084 Uiso 0.632(8) 1 calc R U P A 1
C22A C 0.9738(4) 0.7733(2) 0.4703(4) 0.0436(12) Uani 0.632(8) 1 d . . P A 1
H22A H 1.0242 0.7367 0.5009 0.065 Uiso 0.632(8) 1 calc R U P A 1
H22B H 0.9153 0.7542 0.4170 0.065 Uiso 0.632(8) 1 calc R U P A 1
H22C H 1.0174 0.8075 0.4402 0.065 Uiso 0.632(8) 1 calc R U P A 1
C20B C 0.9163(19) 0.8162(16) 0.5566(17) 0.023(4) Uani 0.368(8) 1 d . . P A 2
H20B H 0.8723 0.7727 0.5502 0.028 Uiso 0.368(8) 1 calc R U P A 2
C21B C 1.0186(7) 0.7996(4) 0.5062(6) 0.040(2) Uani 0.368(8) 1 d . . P A 2
H21D H 1.0672 0.7665 0.5483 0.059 Uiso 0.368(8) 1 calc R U P A 2
H21E H 0.9923 0.7802 0.4382 0.059 Uiso 0.368(8) 1 calc R U P A 2
H21F H 1.0615 0.8414 0.4999 0.059 Uiso 0.368(8) 1 calc R U P A 2
C22B C 0.9490(7) 0.8257(4) 0.6691(5) 0.041(2) Uani 0.368(8) 1 d . . P A 2
H22D H 1.0019 0.7897 0.6974 0.061 Uiso 0.368(8) 1 calc R U P A 2
H22E H 0.9852 0.8704 0.6832 0.061 Uiso 0.368(8) 1 calc R U P A 2
H22F H 0.8813 0.8234 0.7006 0.061 Uiso 0.368(8) 1 calc R U P A 2
C23 C 0.71051(14) 0.60160(8) 0.58792(12) 0.0188(3) Uani 1 1 d . . . . .
C24 C 0.76793(15) 0.56749(9) 0.51904(13) 0.0212(3) Uani 1 1 d . . . . .
C25 C 0.78712(16) 0.49739(9) 0.53078(14) 0.0259(4) Uani 1 1 d . . . . .
H25 H 0.8244 0.4743 0.4835 0.031 Uiso 1 1 calc R U . . .
C26 C 0.75386(16) 0.46077(9) 0.60829(15) 0.0280(4) Uani 1 1 d . . . . .
H26 H 0.7699 0.4134 0.6156 0.034 Uiso 1 1 calc R U . . .
C27 C 0.69694(16) 0.49368(9) 0.67533(14) 0.0261(4) Uani 1 1 d . . . . .
H27 H 0.6728 0.4684 0.7284 0.031 Uiso 1 1 calc R U . . .
C28 C 0.67401(15) 0.56343(9) 0.66679(13) 0.0213(3) Uani 1 1 d . . . . .
C29 C 0.81036(15) 0.60240(9) 0.43119(13) 0.0247(4) Uani 1 1 d . . . . .
H29 H 0.8027 0.6528 0.4398 0.030 Uiso 1 1 calc R U . . .
C30 C 0.73749(18) 0.58238(12) 0.32943(15) 0.0380(5) Uani 1 1 d . . . . .
H30A H 0.7439 0.5332 0.3188 0.057 Uiso 1 1 calc R U . . .
H30B H 0.7634 0.6071 0.2738 0.057 Uiso 1 1 calc R U . . .
H30C H 0.6584 0.5940 0.3304 0.057 Uiso 1 1 calc R U . . .
C31 C 0.93487(16) 0.58708(11) 0.42972(15) 0.0328(4) Uani 1 1 d . . . . .
H31A H 0.9807 0.6000 0.4954 0.049 Uiso 1 1 calc R U . . .
H31B H 0.9595 0.6132 0.3748 0.049 Uiso 1 1 calc R U . . .
H31C H 0.9442 0.5382 0.4180 0.049 Uiso 1 1 calc R U . . .
C32 C 0.61653(16) 0.59600(10) 0.74817(14) 0.0264(4) Uani 1 1 d . . . . .
H32 H 0.5869 0.6415 0.7219 0.032 Uiso 1 1 calc R U . . .
C33 C 0.70409(18) 0.60828(12) 0.84523(15) 0.0370(5) Uani 1 1 d . . . . .
H33A H 0.7365 0.5645 0.8716 0.056 Uiso 1 1 calc R U . . .
H33B H 0.6675 0.6303 0.8969 0.056 Uiso 1 1 calc R U . . .
H33C H 0.7643 0.6379 0.8293 0.056 Uiso 1 1 calc R U . . .
C34 C 0.51685(18) 0.55456(11) 0.77261(17) 0.0384(5) Uani 1 1 d . . . . .
H34A H 0.4658 0.5430 0.7090 0.058 Uiso 1 1 calc R U . . .
H34B H 0.4759 0.5816 0.8162 0.058 Uiso 1 1 calc R U . . .
H34C H 0.5450 0.5126 0.8083 0.058 Uiso 1 1 calc R U . . .
Ti1 Ti 0.49611(3) 0.75266(2) 0.54836(2) 0.02148(7) Uani 1 1 d . . . . .
As1 As 0.70068(2) 0.70238(2) 0.60353(2) 0.01874(5) Uani 1 1 d . . . . .
As2 As 0.65617(2) 0.75818(2) 0.43584(2) 0.01856(5) Uani 1 1 d . . . . .


#==============================================================================

# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.402(3) . ?
C1 C5 1.412(3) . ?
C1 Ti1 2.3396(19) . ?
C1 H1 0.9500 . ?
C2 C3 1.392(3) . ?
C2 Ti1 2.379(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.399(3) . ?
C3 Ti1 2.3987(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(3) . ?
C4 Ti1 2.3805(19) . ?
C4 H4 0.9500 . ?
C5 Ti1 2.3316(19) . ?
C5 H5 0.9500 . ?
C6 C7 1.393(3) . ?
C6 C10 1.397(4) . ?
C6 Ti1 2.328(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.384(3) . ?
C7 Ti1 2.3581(18) . ?
C7 H7 0.9500 . ?
C8 C9 1.388(3) . ?
C8 Ti1 2.3796(19) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(4) . ?
C9 Ti1 2.382(2) . ?
C9 H9 0.9500 . ?
C10 Ti1 2.348(2) . ?
C10 H10 0.9500 . ?
C11 C16 1.414(2) . ?
C11 C12 1.416(2) . ?
C11 As2 1.9968(16) . ?
C12 C13 1.394(2) . ?
C12 C17 1.524(2) . ?
C13 C14 1.376(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.396(2) . ?
C15 H15 0.9500 . ?
C16 C20B 1.43(3) . ?
C16 C20A 1.562(15) . ?
C17 C19 1.529(3) . ?
C17 C18 1.535(3) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20A C22A 1.494(16) . ?
C20A C21A 1.586(15) . ?
C20A H20A 1.0000 . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C20B C22B 1.49(2) . ?
C20B C21B 1.54(2) . ?
C20B H20B 1.0000 . ?
C21B H21D 0.9800 . ?
C21B H21E 0.9800 . ?
C21B H21F 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C24 1.410(2) . ?
C23 C28 1.421(2) . ?
C23 As1 1.9914(17) . ?
C24 C25 1.397(2) . ?
C24 C29 1.519(2) . ?
C25 C26 1.373(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.378(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.395(2) . ?
C27 H27 0.9500 . ?
C28 C32 1.525(2) . ?
C29 C30 1.528(3) . ?
C29 C31 1.530(3) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C34 1.530(3) . ?
C32 C33 1.533(3) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
Ti1 As1 2.6302(4) . ?
Ti1 As2 2.6428(4) . ?
As1 As2 2.4572(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C5 107.8(2) . . ?
C2 C1 Ti1 74.24(11) . . ?
C5 C1 Ti1 72.09(11) . . ?
C2 C1 H1 126.1 . . ?
C5 C1 H1 126.1 . . ?
Ti1 C1 H1 119.4 . . ?
C3 C2 C1 107.99(19) . . ?
C3 C2 Ti1 73.86(11) . . ?
C1 C2 Ti1 71.20(11) . . ?
C3 C2 H2 126.0 . . ?
C1 C2 H2 126.0 . . ?
Ti1 C2 H2 120.7 . . ?
C2 C3 C4 108.52(19) . . ?
C2 C3 Ti1 72.27(11) . . ?
C4 C3 Ti1 72.27(11) . . ?
C2 C3 H3 125.7 . . ?
C4 C3 H3 125.7 . . ?
Ti1 C3 H3 121.4 . . ?
C5 C4 C3 108.04(19) . . ?
C5 C4 Ti1 70.84(11) . . ?
C3 C4 Ti1 73.70(11) . . ?
C5 C4 H4 126.0 . . ?
C3 C4 H4 126.0 . . ?
Ti1 C4 H4 121.2 . . ?
C4 C5 C1 107.69(19) . . ?
C4 C5 Ti1 74.67(11) . . ?
C1 C5 Ti1 72.71(11) . . ?
C4 C5 H5 126.2 . . ?
C1 C5 H5 126.2 . . ?
Ti1 C5 H5 118.4 . . ?
C7 C6 C10 107.9(2) . . ?
C7 C6 Ti1 73.90(11) . . ?
C10 C6 Ti1 73.42(12) . . ?
C7 C6 H6 126.1 . . ?
C10 C6 H6 126.1 . . ?
Ti1 C6 H6 118.6 . . ?
C8 C7 C6 107.68(19) . . ?
C8 C7 Ti1 73.86(11) . . ?
C6 C7 Ti1 71.52(11) . . ?
C8 C7 H7 126.2 . . ?
C6 C7 H7 126.2 . . ?
Ti1 C7 H7 120.3 . . ?
C7 C8 C9 108.7(2) . . ?
C7 C8 Ti1 72.16(11) . . ?
C9 C8 Ti1 73.15(12) . . ?
C7 C8 H8 125.7 . . ?
C9 C8 H8 125.7 . . ?
Ti1 C8 H8 120.8 . . ?
C10 C9 C8 107.8(2) . . ?
C10 C9 Ti1 71.61(13) . . ?
C8 C9 Ti1 72.95(12) . . ?
C10 C9 H9 126.1 . . ?
C8 C9 H9 126.1 . . ?
Ti1 C9 H9 121.1 . . ?
C9 C10 C6 108.0(2) . . ?
C9 C10 Ti1 74.29(13) . . ?
C6 C10 Ti1 71.83(12) . . ?
C9 C10 H10 126.0 . . ?
C6 C10 H10 126.0 . . ?
Ti1 C10 H10 119.7 . . ?
C16 C11 C12 119.12(15) . . ?
C16 C11 As2 125.20(12) . . ?
C12 C11 As2 115.46(12) . . ?
C13 C12 C11 119.43(16) . . ?
C13 C12 C17 118.19(16) . . ?
C11 C12 C17 122.20(15) . . ?
C14 C13 C12 121.20(17) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 119.51(17) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C14 C15 C16 121.69(17) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C15 C16 C11 118.81(16) . . ?
C15 C16 C20B 114.9(11) . . ?
C11 C16 C20B 126.3(11) . . ?
C15 C16 C20A 119.6(6) . . ?
C11 C16 C20A 121.3(6) . . ?
C12 C17 C19 114.86(16) . . ?
C12 C17 C18 109.44(16) . . ?
C19 C17 C18 109.33(16) . . ?
C12 C17 H17 107.7 . . ?
C19 C17 H17 107.7 . . ?
C18 C17 H17 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22A C20A C16 109.3(8) . . ?
C22A C20A C21A 109.7(9) . . ?
C16 C20A C21A 110.3(11) . . ?
C22A C20A H20A 109.2 . . ?
C16 C20A H20A 109.2 . . ?
C21A C20A H20A 109.2 . . ?
C20A C21A H21A 109.5 . . ?
C20A C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
C20A C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C20A C22A H22A 109.5 . . ?
C20A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C20A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C16 C20B C22B 118(2) . . ?
C16 C20B C21B 114.4(13) . . ?
C22B C20B C21B 112.1(15) . . ?
C16 C20B H20B 103.5 . . ?
C22B C20B H20B 103.5 . . ?
C21B C20B H20B 103.5 . . ?
C20B C21B H21D 109.5 . . ?
C20B C21B H21E 109.5 . . ?
H21D C21B H21E 109.5 . . ?
C20B C21B H21F 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
C20B C22B H22D 109.5 . . ?
C20B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C20B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C24 C23 C28 118.83(15) . . ?
C24 C23 As1 125.65(12) . . ?
C28 C23 As1 114.40(12) . . ?
C25 C24 C23 118.91(16) . . ?
C25 C24 C29 117.23(16) . . ?
C23 C24 C29 123.86(15) . . ?
C26 C25 C24 122.25(17) . . ?
C26 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
C25 C26 C27 119.11(17) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.4 . . ?
C26 C27 C28 121.32(17) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C27 C28 C23 119.57(16) . . ?
C27 C28 C32 117.40(15) . . ?
C23 C28 C32 122.92(15) . . ?
C24 C29 C30 110.40(16) . . ?
C24 C29 C31 112.63(15) . . ?
C30 C29 C31 110.27(16) . . ?
C24 C29 H29 107.8 . . ?
C30 C29 H29 107.8 . . ?
C31 C29 H29 107.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C32 C34 113.60(16) . . ?
C28 C32 C33 109.52(16) . . ?
C34 C32 C33 110.53(16) . . ?
C28 C32 H32 107.7 . . ?
C34 C32 H32 107.7 . . ?
C33 C32 H32 107.7 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C6 Ti1 C5 84.51(8) . . ?
C6 Ti1 C1 97.01(8) . . ?
C5 Ti1 C1 35.19(7) . . ?
C6 Ti1 C10 34.76(9) . . ?
C5 Ti1 C10 89.08(9) . . ?
C1 Ti1 C10 81.17(8) . . ?
C6 Ti1 C7 34.59(7) . . ?
C5 Ti1 C7 113.89(7) . . ?
C1 Ti1 C7 131.57(8) . . ?
C10 Ti1 C7 57.27(7) . . ?
C6 Ti1 C2 131.41(8) . . ?
C5 Ti1 C2 57.71(7) . . ?
C1 Ti1 C2 34.57(8) . . ?
C10 Ti1 C2 109.04(8) . . ?
C7 Ti1 C2 165.49(8) . . ?
C6 Ti1 C8 56.89(7) . . ?
C5 Ti1 C8 140.99(7) . . ?
C1 Ti1 C8 135.53(8) . . ?
C10 Ti1 C8 56.62(8) . . ?
C7 Ti1 C8 33.98(7) . . ?
C2 Ti1 C8 145.33(8) . . ?
C6 Ti1 C4 108.66(8) . . ?
C5 Ti1 C4 34.49(7) . . ?
C1 Ti1 C4 57.45(7) . . ?
C10 Ti1 C4 122.93(9) . . ?
C7 Ti1 C4 124.30(7) . . ?
C2 Ti1 C4 56.83(7) . . ?
C8 Ti1 C4 157.65(7) . . ?
C6 Ti1 C9 57.12(9) . . ?
C5 Ti1 C9 121.49(9) . . ?
C1 Ti1 C9 102.54(9) . . ?
C10 Ti1 C9 34.10(9) . . ?
C7 Ti1 C9 56.74(7) . . ?
C2 Ti1 C9 115.52(8) . . ?
C8 Ti1 C9 33.90(8) . . ?
C4 Ti1 C9 155.97(9) . . ?
C6 Ti1 C3 140.85(8) . . ?
C5 Ti1 C3 57.14(7) . . ?
C1 Ti1 C3 56.96(8) . . ?
C10 Ti1 C3 138.13(8) . . ?
C7 Ti1 C3 154.70(7) . . ?
C2 Ti1 C3 33.87(8) . . ?
C8 Ti1 C3 161.87(7) . . ?
C4 Ti1 C3 34.03(7) . . ?
C9 Ti1 C3 148.47(8) . . ?
C6 Ti1 As1 114.01(6) . . ?
C5 Ti1 As1 112.58(6) . . ?
C1 Ti1 As1 134.06(6) . . ?
C10 Ti1 As1 142.32(6) . . ?
C7 Ti1 As1 85.34(5) . . ?
C2 Ti1 As1 108.60(6) . . ?
C8 Ti1 As1 90.39(5) . . ?
C4 Ti1 As1 80.17(5) . . ?
C9 Ti1 As1 122.46(7) . . ?
C3 Ti1 As1 78.28(5) . . ?
C6 Ti1 As2 132.49(6) . . ?
C5 Ti1 As2 142.89(6) . . ?
C1 Ti1 As2 123.60(6) . . ?
C10 Ti1 As2 122.18(8) . . ?
C7 Ti1 As2 100.71(5) . . ?
C2 Ti1 As2 90.81(5) . . ?
C8 Ti1 As2 76.07(5) . . ?
C4 Ti1 As2 113.53(5) . . ?
C9 Ti1 As2 88.15(7) . . ?
C3 Ti1 As2 85.83(5) . . ?
As1 Ti1 As2 55.549(10) . . ?
C23 As1 As2 110.73(5) . . ?
C23 As1 Ti1 114.35(5) . . ?
As2 As1 Ti1 62.487(9) . . ?
C11 As2 As1 107.93(5) . . ?
C11 As2 Ti1 110.32(5) . . ?
As1 As2 Ti1 61.964(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 -0.4(2) . . . . ?
Ti1 C1 C2 C3 -65.21(14) . . . . ?
C5 C1 C2 Ti1 64.80(14) . . . . ?
C1 C2 C3 C4 -0.2(2) . . . . ?
Ti1 C2 C3 C4 -63.63(13) . . . . ?
C1 C2 C3 Ti1 63.46(14) . . . . ?
C2 C3 C4 C5 0.7(2) . . . . ?
Ti1 C3 C4 C5 -62.94(14) . . . . ?
C2 C3 C4 Ti1 63.63(14) . . . . ?
C3 C4 C5 C1 -0.9(2) . . . . ?
Ti1 C4 C5 C1 -65.74(14) . . . . ?
C3 C4 C5 Ti1 64.80(13) . . . . ?
C2 C1 C5 C4 0.8(2) . . . . ?
Ti1 C1 C5 C4 67.05(14) . . . . ?
C2 C1 C5 Ti1 -66.22(14) . . . . ?
C10 C6 C7 C8 0.6(2) . . . . ?
Ti1 C6 C7 C8 -65.54(13) . . . . ?
C10 C6 C7 Ti1 66.10(15) . . . . ?
C6 C7 C8 C9 -0.5(2) . . . . ?
Ti1 C7 C8 C9 -64.52(14) . . . . ?
C6 C7 C8 Ti1 63.99(14) . . . . ?
C7 C8 C9 C10 0.3(2) . . . . ?
Ti1 C8 C9 C10 -63.58(15) . . . . ?
C7 C8 C9 Ti1 63.88(14) . . . . ?
C8 C9 C10 C6 0.1(2) . . . . ?
Ti1 C9 C10 C6 -64.41(16) . . . . ?
C8 C9 C10 Ti1 64.46(15) . . . . ?
C7 C6 C10 C9 -0.4(2) . . . . ?
Ti1 C6 C10 C9 66.04(16) . . . . ?
C7 C6 C10 Ti1 -66.42(14) . . . . ?
C16 C11 C12 C13 -5.6(2) . . . . ?
As2 C11 C12 C13 179.59(13) . . . . ?
C16 C11 C12 C17 169.55(15) . . . . ?
As2 C11 C12 C17 -5.3(2) . . . . ?
C11 C12 C13 C14 2.2(3) . . . . ?
C17 C12 C13 C14 -173.15(17) . . . . ?
C12 C13 C14 C15 1.6(3) . . . . ?
C13 C14 C15 C16 -1.9(3) . . . . ?
C14 C15 C16 C11 -1.5(3) . . . . ?
C14 C15 C16 C20B 178.1(10) . . . . ?
C14 C15 C16 C20A 172.6(6) . . . . ?
C12 C11 C16 C15 5.2(2) . . . . ?
As2 C11 C16 C15 179.53(12) . . . . ?
C12 C11 C16 C20B -174.3(11) . . . . ?
As2 C11 C16 C20B 0.0(12) . . . . ?
C12 C11 C16 C20A -168.8(6) . . . . ?
As2 C11 C16 C20A 5.5(6) . . . . ?
C13 C12 C17 C19 -28.1(2) . . . . ?
C11 C12 C17 C19 156.69(17) . . . . ?
C13 C12 C17 C18 95.25(19) . . . . ?
C11 C12 C17 C18 -79.9(2) . . . . ?
C15 C16 C20A C22A -93.5(9) . . . . ?
C11 C16 C20A C22A 80.5(10) . . . . ?
C15 C16 C20A C21A 27.2(10) . . . . ?
C11 C16 C20A C21A -158.8(6) . . . . ?
C15 C16 C20B C22B 64.2(17) . . . . ?
C11 C16 C20B C22B -116.3(17) . . . . ?
C15 C16 C20B C21B -71(2) . . . . ?
C11 C16 C20B C21B 109.0(16) . . . . ?
C28 C23 C24 C25 -0.1(2) . . . . ?
As1 C23 C24 C25 167.07(13) . . . . ?
C28 C23 C24 C29 179.53(16) . . . . ?
As1 C23 C24 C29 -13.3(2) . . . . ?
C23 C24 C25 C26 -1.3(3) . . . . ?
C29 C24 C25 C26 179.09(17) . . . . ?
C24 C25 C26 C27 1.8(3) . . . . ?
C25 C26 C27 C28 -0.9(3) . . . . ?
C26 C27 C28 C23 -0.4(3) . . . . ?
C26 C27 C28 C32 -176.60(17) . . . . ?
C24 C23 C28 C27 0.9(2) . . . . ?
As1 C23 C28 C27 -167.68(13) . . . . ?
C24 C23 C28 C32 176.89(16) . . . . ?
As1 C23 C28 C32 8.3(2) . . . . ?
C25 C24 C29 C30 72.1(2) . . . . ?
C23 C24 C29 C30 -107.49(19) . . . . ?
C25 C24 C29 C31 -51.6(2) . . . . ?
C23 C24 C29 C31 128.77(18) . . . . ?
C27 C28 C32 C34 -45.5(2) . . . . ?
C23 C28 C32 C34 138.46(18) . . . . ?
C27 C28 C32 C33 78.6(2) . . . . ?
C23 C28 C32 C33 -97.4(2) . . . . ?

_refine_diff_density_max         0.414
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.068


####################################################################### 
# 
# 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_ks1502_TipAsIMe4_cmp5aa
_database_code_depnum_ccdc_archive 'CCDC 2041970'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-02 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H35 As N2'
_chemical_formula_sum            'C22 H35 As N2'
_chemical_formula_weight         402.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_H-M_alt        'P 32'
_space_group_name_Hall           'P 32'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'

_cell_length_a                   9.2425(13)
_cell_length_b                   9.2425(13)
_cell_length_c                   22.020(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1629.0(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2151
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      29.04

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_F_000             642
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.572
_shelx_estimated_absorpt_T_min   0.609
_shelx_estimated_absorpt_T_max   0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_process_details   'LANA (Stoe & Cie, 2012)'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_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  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21626
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.708
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             5731
_reflns_number_gt                4349
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_max     0.954
_reflns_Friedel_fraction_full    0.974

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

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine.
 
 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0263P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1776 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5731
_refine_ls_number_parameters     236
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0540
_refine_ls_wR_factor_gt          0.0518
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_restrained_S_all      0.837
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.37814(4) 0.78165(4) 0.59994(2) 0.03484(9) Uani 1 1 d . . . . .
N1 N 0.0720(3) 0.4698(3) 0.55447(11) 0.0314(6) Uani 1 1 d . . . . .
N2 N 0.0576(3) 0.5460(3) 0.64590(11) 0.0285(5) Uani 1 1 d . . . . .
C1 C 0.4700(4) 0.8017(4) 0.51671(13) 0.0276(6) Uani 1 1 d . . . . .
C2 C 0.4227(4) 0.8696(4) 0.46848(14) 0.0297(7) Uani 1 1 d . . . . .
C3 C 0.5177(4) 0.9190(4) 0.41519(15) 0.0314(7) Uani 1 1 d . . . . .
H3 H 0.4851 0.9653 0.3831 0.038 Uiso 1 1 calc R U . . .
C4 C 0.6583(4) 0.9028(4) 0.40766(14) 0.0299(7) Uani 1 1 d . . . . .
C5 C 0.6980(4) 0.8286(4) 0.45452(16) 0.0316(7) Uani 1 1 d . . . . .
H5 H 0.7906 0.8116 0.4495 0.038 Uiso 1 1 calc R U . . .
C6 C 0.6076(4) 0.7776(4) 0.50883(13) 0.0303(7) Uani 1 1 d . . . . .
C7 C 0.2730(4) 0.8959(4) 0.47247(15) 0.0369(7) Uani 1 1 d . . . . .
H7 H 0.2041 0.8298 0.5079 0.044 Uiso 1 1 calc R U . . .
C8 C 0.1613(5) 0.8337(6) 0.41608(19) 0.0596(12) Uani 1 1 d . . . . .
H8A H 0.0576 0.8349 0.4239 0.089 Uiso 1 1 calc R U . . .
H8B H 0.1351 0.7194 0.4067 0.089 Uiso 1 1 calc R U . . .
H8C H 0.2198 0.9068 0.3816 0.089 Uiso 1 1 calc R U . . .
C9 C 0.3274(5) 1.0762(5) 0.48426(19) 0.0545(10) Uani 1 1 d . . . . .
H9A H 0.3970 1.1448 0.4505 0.082 Uiso 1 1 calc R U . . .
H9B H 0.3918 1.1123 0.5221 0.082 Uiso 1 1 calc R U . . .
H9C H 0.2287 1.0891 0.4879 0.082 Uiso 1 1 calc R U . . .
C10 C 0.7705(4) 0.9629(4) 0.35191(15) 0.0361(7) Uani 1 1 d . . . . .
H10 H 0.7958 0.8732 0.3404 0.043 Uiso 1 1 calc R U . . .
C11 C 0.6944(5) 0.9975(5) 0.29734(17) 0.0490(10) Uani 1 1 d . . . . .
H11A H 0.6918 1.1011 0.3039 0.073 Uiso 1 1 calc R U . . .
H11B H 0.5803 0.9047 0.2914 0.073 Uiso 1 1 calc R U . . .
H11C H 0.7616 1.0094 0.2613 0.073 Uiso 1 1 calc R U . . .
C12 C 0.9353(4) 1.1183(5) 0.36742(17) 0.0477(9) Uani 1 1 d . . . . .
H12A H 1.0085 1.1537 0.3318 0.072 Uiso 1 1 calc R U . . .
H12B H 0.9892 1.0933 0.4009 0.072 Uiso 1 1 calc R U . . .
H12C H 0.9143 1.2082 0.3796 0.072 Uiso 1 1 calc R U . . .
C13 C 0.6644(4) 0.6967(4) 0.55631(15) 0.0383(7) Uani 1 1 d . . . . .
H13 H 0.5812 0.6575 0.5902 0.046 Uiso 1 1 calc R U . . .
C14 C 0.6652(7) 0.5440(6) 0.5308(2) 0.0643(12) Uani 1 1 d . . . . .
H14A H 0.5573 0.4698 0.5115 0.096 Uiso 1 1 calc R U . . .
H14B H 0.6843 0.4843 0.5638 0.096 Uiso 1 1 calc R U . . .
H14C H 0.7546 0.5795 0.5006 0.096 Uiso 1 1 calc R U . . .
C15 C 0.8326(5) 0.8193(6) 0.5829(2) 0.0620(12) Uani 1 1 d . . . . .
H15A H 0.9166 0.8630 0.5506 0.093 Uiso 1 1 calc R U . . .
H15B H 0.8639 0.7628 0.6134 0.093 Uiso 1 1 calc R U . . .
H15C H 0.8263 0.9118 0.6020 0.093 Uiso 1 1 calc R U . . .
C16 C 0.1599(4) 0.5898(4) 0.59670(13) 0.0273(6) Uani 1 1 d . . . . .
C17 C -0.0847(4) 0.3522(4) 0.57766(16) 0.0339(8) Uani 1 1 d . . . . .
C18 C -0.0928(4) 0.3993(4) 0.63443(15) 0.0332(7) Uani 1 1 d . . . . .
C19 C 0.1362(5) 0.4487(5) 0.49728(16) 0.0467(9) Uani 1 1 d . . . . .
H19A H 0.2548 0.5328 0.4938 0.070 Uiso 1 1 calc R U . . .
H19B H 0.0741 0.4621 0.4638 0.070 Uiso 1 1 calc R U . . .
H19C H 0.1231 0.3368 0.4956 0.070 Uiso 1 1 calc R U . . .
C20 C 0.1051(4) 0.6360(4) 0.70265(14) 0.0342(7) Uani 1 1 d . . . . .
H20A H 0.1803 0.6087 0.7248 0.051 Uiso 1 1 calc R U . . .
H20B H 0.0049 0.6041 0.7271 0.051 Uiso 1 1 calc R U . . .
H20C H 0.1622 0.7564 0.6946 0.051 Uiso 1 1 calc R U . . .
C21 C -0.2104(4) 0.2125(4) 0.53995(18) 0.0481(9) Uani 1 1 d . . . . .
H21A H -0.3132 0.1478 0.5635 0.072 Uiso 1 1 calc R U . . .
H21B H -0.1663 0.1399 0.5279 0.072 Uiso 1 1 calc R U . . .
H21C H -0.2348 0.2577 0.5036 0.072 Uiso 1 1 calc R U . . .
C22 C -0.2293(5) 0.3222(5) 0.68008(18) 0.0497(9) Uani 1 1 d . . . . .
H22A H -0.3237 0.2212 0.6629 0.075 Uiso 1 1 calc R U . . .
H22B H -0.2657 0.4018 0.6910 0.075 Uiso 1 1 calc R U . . .
H22C H -0.1885 0.2927 0.7164 0.075 Uiso 1 1 calc R U . . .


#==============================================================================

# MOLECULAR GEOMETRY

_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
As1 C16 1.909(3) . ?
As1 C1 1.989(3) . ?
N1 C16 1.361(4) . ?
N1 C17 1.402(4) . ?
N1 C19 1.446(4) . ?
N2 C16 1.360(4) . ?
N2 C18 1.396(4) . ?
N2 C20 1.443(4) . ?
C1 C6 1.407(4) . ?
C1 C2 1.410(4) . ?
C2 C3 1.399(4) . ?
C2 C7 1.522(4) . ?
C3 C4 1.391(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(5) . ?
C4 C10 1.521(4) . ?
C5 C6 1.399(4) . ?
C5 H5 0.9500 . ?
C6 C13 1.523(4) . ?
C7 C9 1.504(5) . ?
C7 C8 1.531(5) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.506(5) . ?
C10 C12 1.520(5) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C15 1.511(5) . ?
C13 C14 1.523(5) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C17 C18 1.338(5) . ?
C17 C21 1.486(5) . ?
C18 C22 1.487(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C16 As1 C1 104.83(12) . . ?
C16 N1 C17 110.3(3) . . ?
C16 N1 C19 126.0(3) . . ?
C17 N1 C19 123.2(3) . . ?
C16 N2 C18 110.6(2) . . ?
C16 N2 C20 123.5(3) . . ?
C18 N2 C20 125.8(3) . . ?
C6 C1 C2 118.9(3) . . ?
C6 C1 As1 118.5(2) . . ?
C2 C1 As1 121.5(2) . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 C7 117.9(3) . . ?
C1 C2 C7 122.5(3) . . ?
C4 C3 C2 122.2(3) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C5 C4 C3 117.2(3) . . ?
C5 C4 C10 118.7(3) . . ?
C3 C4 C10 124.0(3) . . ?
C4 C5 C6 122.8(3) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C5 C6 C1 119.2(3) . . ?
C5 C6 C13 117.2(3) . . ?
C1 C6 C13 123.6(3) . . ?
C9 C7 C2 111.1(3) . . ?
C9 C7 C8 110.2(3) . . ?
C2 C7 C8 112.9(3) . . ?
C9 C7 H7 107.5 . . ?
C2 C7 H7 107.5 . . ?
C8 C7 H7 107.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C12 109.4(3) . . ?
C11 C10 C4 114.6(3) . . ?
C12 C10 C4 110.0(3) . . ?
C11 C10 H10 107.5 . . ?
C12 C10 H10 107.5 . . ?
C4 C10 H10 107.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 C13 C14 111.0(3) . . ?
C15 C13 C6 112.1(3) . . ?
C14 C13 C6 111.4(3) . . ?
C15 C13 H13 107.4 . . ?
C14 C13 H13 107.4 . . ?
C6 C13 H13 107.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C16 N1 105.0(2) . . ?
N2 C16 As1 120.1(2) . . ?
N1 C16 As1 134.8(2) . . ?
C18 C17 N1 107.0(3) . . ?
C18 C17 C21 131.2(3) . . ?
N1 C17 C21 121.7(3) . . ?
C17 C18 N2 107.1(3) . . ?
C17 C18 C22 130.4(3) . . ?
N2 C18 C22 122.5(3) . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -3.1(4) . . . . ?
As1 C1 C2 C3 164.5(2) . . . . ?
C6 C1 C2 C7 178.5(3) . . . . ?
As1 C1 C2 C7 -13.9(4) . . . . ?
C1 C2 C3 C4 0.4(5) . . . . ?
C7 C2 C3 C4 178.9(3) . . . . ?
C2 C3 C4 C5 2.5(5) . . . . ?
C2 C3 C4 C10 -176.7(3) . . . . ?
C3 C4 C5 C6 -2.8(5) . . . . ?
C10 C4 C5 C6 176.5(3) . . . . ?
C4 C5 C6 C1 0.1(5) . . . . ?
C4 C5 C6 C13 179.6(3) . . . . ?
C2 C1 C6 C5 2.9(4) . . . . ?
As1 C1 C6 C5 -165.2(2) . . . . ?
C2 C1 C6 C13 -176.6(3) . . . . ?
As1 C1 C6 C13 15.4(4) . . . . ?
C3 C2 C7 C9 -76.4(4) . . . . ?
C1 C2 C7 C9 102.0(4) . . . . ?
C3 C2 C7 C8 48.0(4) . . . . ?
C1 C2 C7 C8 -133.6(4) . . . . ?
C5 C4 C10 C11 164.1(3) . . . . ?
C3 C4 C10 C11 -16.6(5) . . . . ?
C5 C4 C10 C12 -72.2(4) . . . . ?
C3 C4 C10 C12 107.1(4) . . . . ?
C5 C6 C13 C15 67.9(4) . . . . ?
C1 C6 C13 C15 -112.7(4) . . . . ?
C5 C6 C13 C14 -57.2(4) . . . . ?
C1 C6 C13 C14 122.3(4) . . . . ?
C18 N2 C16 N1 0.2(3) . . . . ?
C20 N2 C16 N1 177.0(3) . . . . ?
C18 N2 C16 As1 -177.9(2) . . . . ?
C20 N2 C16 As1 -1.0(4) . . . . ?
C17 N1 C16 N2 0.2(3) . . . . ?
C19 N1 C16 N2 -171.2(3) . . . . ?
C17 N1 C16 As1 177.8(3) . . . . ?
C19 N1 C16 As1 6.4(5) . . . . ?
C16 N1 C17 C18 -0.5(4) . . . . ?
C19 N1 C17 C18 171.1(3) . . . . ?
C16 N1 C17 C21 176.5(3) . . . . ?
C19 N1 C17 C21 -11.9(5) . . . . ?
N1 C17 C18 N2 0.6(4) . . . . ?
C21 C17 C18 N2 -176.0(3) . . . . ?
N1 C17 C18 C22 179.6(3) . . . . ?
C21 C17 C18 C22 3.1(6) . . . . ?
C16 N2 C18 C17 -0.5(4) . . . . ?
C20 N2 C18 C17 -177.2(3) . . . . ?
C16 N2 C18 C22 -179.6(3) . . . . ?
C20 N2 C18 C22 3.6(5) . . . . ?

_refine_diff_density_max         0.314
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.051


####################################################################### 
# 
# 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_ax1757_As3Dipp3_cmp2b
_database_code_depnum_ccdc_archive 'CCDC 2041966'
loop_
_audit_author_name
_audit_author_address
'Hering-Junghans C.'
;LIKAT Rostock
Germany
;
_audit_update_record             
;
2020-11-02 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H51 As3'
_chemical_formula_sum            'C36 H51 As3'
_chemical_formula_weight         708.52

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

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

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

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

_cell_length_a                   11.6003(5)
_cell_length_b                   18.1155(7)
_cell_length_c                   16.1710(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.3360(10)
_cell_angle_gamma                90
_cell_volume                     3397.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9146
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      30.34

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_F_000             1464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.163
_exptl_absorpt_coefficient_mu    2.956
_shelx_estimated_absorpt_T_min   0.502
_shelx_estimated_absorpt_T_max   0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_absorpt_special_details   ?

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            81028
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.688
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9924
_reflns_number_gt                8366
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

#==============================================================================

# REFINEMENT DATA 

_refine_special_details          
;
 All H atoms 
 were positioned geometrically and refined using a riding model, with C---H = 
 0.98 (methyl groups), 0.99Å (methylene groups), 1.00Å (methine groups) or 
 0.95 Å (aryl CH) and with Uiso(H) = 1.5 times Ueq(C) 
 (methyl groups) or with Uiso(H) = 1.2 times Ueq(C) 
 (methylene  groups, aryl CH, methine groups). Torsion angles of all methyl 
 groups were allowed to refine. One isopropyl group (C22-C24) was
 found to be disordered and was split in two parts, which were allowed to
 refine freely.
 
 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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0316P)²+1.0696P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9924
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0614
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.60215(12) 0.33848(9) 0.73960(9) 0.0207(3) Uani 1 1 d . . . . .
C2 C 0.64455(13) 0.38426(9) 0.80414(10) 0.0238(3) Uani 1 1 d . . . . .
C3 C 0.72279(14) 0.35452(11) 0.86197(10) 0.0304(4) Uani 1 1 d . . . . .
H3 H 0.7499 0.3844 0.9066 0.037 Uiso 1 1 calc R U . . .
C4 C 0.76136(14) 0.28330(11) 0.85594(10) 0.0327(4) Uani 1 1 d . . . . .
H4 H 0.8127 0.2639 0.8971 0.039 Uiso 1 1 calc R U . . .
C5 C 0.72567(14) 0.23982(10) 0.79022(10) 0.0291(3) Uani 1 1 d . . . . .
H5 H 0.7551 0.1911 0.7853 0.035 Uiso 1 1 calc R U . . .
C6 C 0.64682(12) 0.26649(9) 0.73078(10) 0.0233(3) Uani 1 1 d . . . . .
C7 C 0.61599(14) 0.46587(10) 0.81152(11) 0.0310(4) Uani 1 1 d . . . . .
H7 H 0.5509 0.4769 0.7718 0.037 Uiso 1 1 calc R U . . .
C8 C 0.7188(2) 0.51240(14) 0.7870(2) 0.0676(8) Uani 1 1 d . . . . .
H8A H 0.7861 0.4990 0.8216 0.101 Uiso 1 1 calc R U . . .
H8B H 0.7009 0.5648 0.7949 0.101 Uiso 1 1 calc R U . . .
H8C H 0.7357 0.5034 0.7288 0.101 Uiso 1 1 calc R U . . .
C9 C 0.5771(2) 0.48639(13) 0.89873(14) 0.0559(6) Uani 1 1 d . . . . .
H9A H 0.5058 0.4600 0.9109 0.084 Uiso 1 1 calc R U . . .
H9B H 0.5634 0.5397 0.9016 0.084 Uiso 1 1 calc R U . . .
H9C H 0.6374 0.4726 0.9393 0.084 Uiso 1 1 calc R U . . .
C10 C 0.61907(14) 0.21846(9) 0.65576(11) 0.0288(3) Uani 1 1 d . . . . .
H10 H 0.5392 0.2314 0.6362 0.035 Uiso 1 1 calc R U . . .
C11 C 0.6998(2) 0.23679(16) 0.58589(13) 0.0593(7) Uani 1 1 d . . . . .
H11A H 0.7787 0.2227 0.6020 0.089 Uiso 1 1 calc R U . . .
H11B H 0.6968 0.2899 0.5746 0.089 Uiso 1 1 calc R U . . .
H11C H 0.6758 0.2096 0.5360 0.089 Uiso 1 1 calc R U . . .
C12 C 0.6202(3) 0.13642(12) 0.67396(18) 0.0672(8) Uani 1 1 d . . . . .
H12A H 0.6003 0.1090 0.6233 0.101 Uiso 1 1 calc R U . . .
H12B H 0.5638 0.1254 0.7164 0.101 Uiso 1 1 calc R U . . .
H12C H 0.6973 0.1218 0.6939 0.101 Uiso 1 1 calc R U . . .
C13 C 0.21370(13) 0.46865(9) 0.72162(10) 0.0252(3) Uani 1 1 d . . . . .
C14 C 0.19550(13) 0.49972(8) 0.64263(10) 0.0236(3) Uani 1 1 d . . . . .
C15 C 0.09981(15) 0.54537(9) 0.62986(12) 0.0335(4) Uani 1 1 d . . . . .
H15 H 0.0856 0.5660 0.5766 0.040 Uiso 1 1 calc R U . . .
C16 C 0.02551(15) 0.56123(10) 0.69257(13) 0.0378(4) Uani 1 1 d . . . . .
H16 H -0.0396 0.5919 0.6821 0.045 Uiso 1 1 calc R U . . .
C17 C 0.04533(15) 0.53286(11) 0.76986(12) 0.0370(4) Uani 1 1 d . . . . .
H17 H -0.0052 0.5452 0.8131 0.044 Uiso 1 1 calc R U . . .
C18 C 0.13828(15) 0.48622(12) 0.78630(11) 0.0363(4) Uani 1 1 d . . . . .
C19 C 0.27836(14) 0.48942(9) 0.57252(10) 0.0259(3) Uani 1 1 d . . . . .
H19 H 0.3181 0.4410 0.5813 0.031 Uiso 1 1 calc R U . . .
C20 C 0.37060(17) 0.54982(10) 0.57738(12) 0.0367(4) Uani 1 1 d . . . . .
H20A H 0.3340 0.5983 0.5705 0.055 Uiso 1 1 calc R U . . .
H20B H 0.4262 0.5422 0.5334 0.055 Uiso 1 1 calc R U . . .
H20C H 0.4107 0.5476 0.6313 0.055 Uiso 1 1 calc R U . . .
C21 C 0.22081(19) 0.48760(12) 0.48649(11) 0.0419(5) Uani 1 1 d . . . . .
H21A H 0.1578 0.4515 0.4859 0.063 Uiso 1 1 calc R U . . .
H21B H 0.2778 0.4735 0.4455 0.063 Uiso 1 1 calc R U . . .
H21C H 0.1900 0.5366 0.4729 0.063 Uiso 1 1 calc R U . . .
C22A C 0.1609(3) 0.4702(2) 0.8747(2) 0.0271(8) Uani 0.562(5) 1 d . . P A 1
H22A H 0.2447 0.4583 0.8820 0.033 Uiso 0.562(5) 1 calc R U P A 1
C23A C 0.0934(5) 0.4014(2) 0.8932(2) 0.0403(10) Uani 0.562(5) 1 d . . P A 1
H23A H 0.1052 0.3880 0.9515 0.060 Uiso 0.562(5) 1 calc R U P A 1
H23B H 0.0112 0.4104 0.8820 0.060 Uiso 0.562(5) 1 calc R U P A 1
H23C H 0.1198 0.3609 0.8582 0.060 Uiso 0.562(5) 1 calc R U P A 1
C24A C 0.1314(3) 0.5306(2) 0.9371(2) 0.0439(10) Uani 0.562(5) 1 d . . P A 1
H24A H 0.1503 0.5133 0.9933 0.066 Uiso 0.562(5) 1 calc R U P A 1
H24B H 0.1762 0.5751 0.9255 0.066 Uiso 0.562(5) 1 calc R U P A 1
H24C H 0.0489 0.5420 0.9326 0.066 Uiso 0.562(5) 1 calc R U P A 1
C22B C 0.1412(4) 0.4364(3) 0.8727(3) 0.0239(9) Uani 0.438(5) 1 d . . P A 2
H22B H 0.1843 0.3898 0.8618 0.029 Uiso 0.438(5) 1 calc R U P A 2
C23B C 0.2121(4) 0.4824(3) 0.9341(3) 0.0419(13) Uani 0.438(5) 1 d . . P A 2
H23D H 0.2863 0.4949 0.9099 0.063 Uiso 0.438(5) 1 calc R U P A 2
H23E H 0.1702 0.5279 0.9467 0.063 Uiso 0.438(5) 1 calc R U P A 2
H23F H 0.2253 0.4541 0.9850 0.063 Uiso 0.438(5) 1 calc R U P A 2
C24B C 0.0249(4) 0.4160(3) 0.9082(3) 0.0379(11) Uani 0.438(5) 1 d . . P A 2
H24D H -0.0191 0.3864 0.8677 0.057 Uiso 0.438(5) 1 calc R U P A 2
H24E H 0.0371 0.3872 0.9590 0.057 Uiso 0.438(5) 1 calc R U P A 2
H24F H -0.0180 0.4610 0.9207 0.057 Uiso 0.438(5) 1 calc R U P A 2
C25 C 0.22818(12) 0.29956(8) 0.57624(9) 0.0207(3) Uani 1 1 d . . . . .
C26 C 0.10889(13) 0.30731(9) 0.58927(9) 0.0218(3) Uani 1 1 d . . . . .
C27 C 0.03308(14) 0.30529(10) 0.52128(10) 0.0290(3) Uani 1 1 d . . . . .
H27 H -0.0472 0.3113 0.5294 0.035 Uiso 1 1 calc R U . . .
C28 C 0.07233(15) 0.29482(10) 0.44243(11) 0.0328(4) Uani 1 1 d . . . . .
H28 H 0.0193 0.2937 0.3968 0.039 Uiso 1 1 calc R U . . .
C29 C 0.18904(15) 0.28589(10) 0.42981(10) 0.0296(4) Uani 1 1 d . . . . .
H29 H 0.2154 0.2787 0.3752 0.036 Uiso 1 1 calc R U . . .
C30 C 0.26865(13) 0.28728(9) 0.49564(10) 0.0232(3) Uani 1 1 d . . . . .
C31 C 0.05785(13) 0.31051(10) 0.67478(10) 0.0257(3) Uani 1 1 d . . . . .
H31 H 0.1178 0.3316 0.7135 0.031 Uiso 1 1 calc R U . . .
C32 C 0.03181(16) 0.23192(11) 0.70357(12) 0.0386(4) Uani 1 1 d . . . . .
H32A H -0.0207 0.2081 0.6635 0.058 Uiso 1 1 calc R U . . .
H32B H -0.0043 0.2337 0.7577 0.058 Uiso 1 1 calc R U . . .
H32C H 0.1038 0.2037 0.7079 0.058 Uiso 1 1 calc R U . . .
C33 C -0.04966(14) 0.35915(10) 0.67955(11) 0.0322(4) Uani 1 1 d . . . . .
H33A H -0.0337 0.4075 0.6553 0.048 Uiso 1 1 calc R U . . .
H33B H -0.0704 0.3654 0.7375 0.048 Uiso 1 1 calc R U . . .
H33C H -0.1137 0.3357 0.6489 0.048 Uiso 1 1 calc R U . . .
C34 C 0.39356(14) 0.26885(10) 0.47828(10) 0.0292(3) Uani 1 1 d . . . . .
H34 H 0.4426 0.2926 0.5224 0.035 Uiso 1 1 calc R U . . .
C35 C 0.43482(17) 0.29671(14) 0.39514(12) 0.0461(5) Uani 1 1 d . . . . .
H35A H 0.3968 0.2686 0.3505 0.069 Uiso 1 1 calc R U . . .
H35B H 0.5185 0.2902 0.3923 0.069 Uiso 1 1 calc R U . . .
H35C H 0.4157 0.3492 0.3892 0.069 Uiso 1 1 calc R U . . .
C36 C 0.41049(17) 0.18516(11) 0.48537(14) 0.0439(5) Uani 1 1 d . . . . .
H36A H 0.3876 0.1686 0.5403 0.066 Uiso 1 1 calc R U . . .
H36B H 0.4918 0.1731 0.4773 0.066 Uiso 1 1 calc R U . . .
H36C H 0.3629 0.1603 0.4430 0.066 Uiso 1 1 calc R U . . .
As1 As 0.48810(2) 0.37916(2) 0.65738(2) 0.01998(4) Uani 1 1 d . . . . .
As2 As 0.33737(2) 0.39960(2) 0.75818(2) 0.02180(4) Uani 1 1 d . . . . .
As3 As 0.33293(2) 0.28678(2) 0.67400(2) 0.02120(4) Uani 1 1 d . . . . .



#==============================================================================

# MOLECULAR GEOMETRY

_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 C6 1.412(2) . ?
C1 C2 1.412(2) . ?
C1 As1 1.9949(15) . ?
C2 C3 1.396(2) . ?
C2 C7 1.520(2) . ?
C3 C4 1.370(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(2) . ?
C5 H5 0.9500 . ?
C6 C10 1.521(2) . ?
C7 C8 1.520(3) . ?
C7 C9 1.536(3) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.515(3) . ?
C10 C11 1.521(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.407(2) . ?
C13 C18 1.415(2) . ?
C13 As2 1.9831(16) . ?
C14 C15 1.396(2) . ?
C14 C19 1.515(2) . ?
C15 C16 1.376(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.366(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(2) . ?
C17 H17 0.9500 . ?
C18 C22A 1.477(4) . ?
C18 C22B 1.663(5) . ?
C19 C21 1.529(2) . ?
C19 C20 1.531(2) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22A C23A 1.507(5) . ?
C22A C24A 1.532(5) . ?
C22A H22A 1.0000 . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C22B C23B 1.523(7) . ?
C22B C24B 1.524(6) . ?
C22B H22B 1.0000 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25 C26 1.412(2) . ?
C25 C30 1.413(2) . ?
C25 As3 1.9849(15) . ?
C26 C27 1.392(2) . ?
C26 C31 1.518(2) . ?
C27 C28 1.377(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.383(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.393(2) . ?
C29 H29 0.9500 . ?
C30 C34 1.520(2) . ?
C31 C32 1.530(2) . ?
C31 C33 1.530(2) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.524(3) . ?
C34 C36 1.533(3) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
As1 As2 2.4463(2) . ?
As1 As3 2.4769(2) . ?
As2 As3 2.4554(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 119.66(14) . . ?
C6 C1 As1 120.87(11) . . ?
C2 C1 As1 119.32(11) . . ?
C3 C2 C1 118.57(15) . . ?
C3 C2 C7 117.52(15) . . ?
C1 C2 C7 123.79(14) . . ?
C4 C3 C2 121.61(16) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 120.01(15) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.85(16) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.05(15) . . ?
C5 C6 C10 118.28(15) . . ?
C1 C6 C10 122.53(14) . . ?
C8 C7 C2 110.18(16) . . ?
C8 C7 C9 110.72(19) . . ?
C2 C7 C9 112.11(16) . . ?
C8 C7 H7 107.9 . . ?
C2 C7 H7 107.9 . . ?
C9 C7 H7 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C11 110.85(19) . . ?
C12 C10 C6 113.92(17) . . ?
C11 C10 C6 110.19(14) . . ?
C12 C10 H10 107.2 . . ?
C11 C10 H10 107.2 . . ?
C6 C10 H10 107.2 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 119.91(15) . . ?
C14 C13 As2 127.95(12) . . ?
C18 C13 As2 112.14(12) . . ?
C15 C14 C13 118.24(15) . . ?
C15 C14 C19 118.60(15) . . ?
C13 C14 C19 123.07(14) . . ?
C16 C15 C14 121.62(17) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C17 C16 C15 120.05(16) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 121.12(17) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C13 119.02(17) . . ?
C17 C18 C22A 115.1(2) . . ?
C13 C18 C22A 124.94(19) . . ?
C17 C18 C22B 119.4(2) . . ?
C13 C18 C22B 119.9(2) . . ?
C14 C19 C21 114.35(14) . . ?
C14 C19 C20 109.18(13) . . ?
C21 C19 C20 110.59(15) . . ?
C14 C19 H19 107.5 . . ?
C21 C19 H19 107.5 . . ?
C20 C19 H19 107.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22A C23A 105.9(3) . . ?
C18 C22A C24A 117.4(3) . . ?
C23A C22A C24A 109.6(3) . . ?
C18 C22A H22A 107.9 . . ?
C23A C22A H22A 107.9 . . ?
C24A C22A H22A 107.9 . . ?
C22A C23A H23A 109.5 . . ?
C22A C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C22A C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C22A C24A H24A 109.5 . . ?
C22A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C22A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C23B C22B C24B 110.9(4) . . ?
C23B C22B C18 104.5(4) . . ?
C24B C22B C18 116.6(3) . . ?
C23B C22B H22B 108.2 . . ?
C24B C22B H22B 108.2 . . ?
C18 C22B H22B 108.2 . . ?
C22B C23B H23D 109.5 . . ?
C22B C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C22B C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C22B C24B H24D 109.5 . . ?
C22B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C22B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C26 C25 C30 120.08(13) . . ?
C26 C25 As3 118.48(11) . . ?
C30 C25 As3 120.38(11) . . ?
C27 C26 C25 118.87(14) . . ?
C27 C26 C31 117.89(13) . . ?
C25 C26 C31 122.98(13) . . ?
C28 C27 C26 121.23(15) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C27 C28 C29 119.90(15) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 121.25(15) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 H29 119.4 . . ?
C29 C30 C25 118.62(14) . . ?
C29 C30 C34 118.21(14) . . ?
C25 C30 C34 122.94(14) . . ?
C26 C31 C32 109.00(14) . . ?
C26 C31 C33 113.79(13) . . ?
C32 C31 C33 110.70(13) . . ?
C26 C31 H31 107.7 . . ?
C32 C31 H31 107.7 . . ?
C33 C31 H31 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 C35 114.26(15) . . ?
C30 C34 C36 108.94(14) . . ?
C35 C34 C36 110.57(16) . . ?
C30 C34 H34 107.6 . . ?
C35 C34 H34 107.6 . . ?
C36 C34 H34 107.6 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C1 As1 As2 94.88(4) . . ?
C1 As1 As3 98.65(4) . . ?
As2 As1 As3 59.831(6) . . ?
C13 As2 As1 114.85(5) . . ?
C13 As2 As3 110.74(5) . . ?
As1 As2 As3 60.705(6) . . ?
C25 As3 As2 110.42(4) . . ?
C25 As3 As1 105.53(4) . . ?
As2 As3 As1 59.464(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -5.5(2) . . . . ?
As1 C1 C2 C3 178.90(12) . . . . ?
C6 C1 C2 C7 170.44(14) . . . . ?
As1 C1 C2 C7 -5.2(2) . . . . ?
C1 C2 C3 C4 2.0(2) . . . . ?
C7 C2 C3 C4 -174.22(15) . . . . ?
C2 C3 C4 C5 2.0(3) . . . . ?
C3 C4 C5 C6 -2.4(3) . . . . ?
C4 C5 C6 C1 -1.1(2) . . . . ?
C4 C5 C6 C10 174.62(15) . . . . ?
C2 C1 C6 C5 5.1(2) . . . . ?
As1 C1 C6 C5 -179.35(11) . . . . ?
C2 C1 C6 C10 -170.48(14) . . . . ?
As1 C1 C6 C10 5.1(2) . . . . ?
C3 C2 C7 C8 70.9(2) . . . . ?
C1 C2 C7 C8 -105.1(2) . . . . ?
C3 C2 C7 C9 -52.9(2) . . . . ?
C1 C2 C7 C9 131.13(18) . . . . ?
C5 C6 C10 C12 34.0(2) . . . . ?
C1 C6 C10 C12 -150.39(18) . . . . ?
C5 C6 C10 C11 -91.3(2) . . . . ?
C1 C6 C10 C11 84.3(2) . . . . ?
C18 C13 C14 C15 -2.3(2) . . . . ?
As2 C13 C14 C15 177.79(13) . . . . ?
C18 C13 C14 C19 174.11(16) . . . . ?
As2 C13 C14 C19 -5.8(2) . . . . ?
C13 C14 C15 C16 1.1(3) . . . . ?
C19 C14 C15 C16 -175.43(16) . . . . ?
C14 C15 C16 C17 0.9(3) . . . . ?
C15 C16 C17 C18 -1.7(3) . . . . ?
C16 C17 C18 C13 0.5(3) . . . . ?
C16 C17 C18 C22A 169.9(3) . . . . ?
C16 C17 C18 C22B -164.6(3) . . . . ?
C14 C13 C18 C17 1.5(3) . . . . ?
As2 C13 C18 C17 -178.58(15) . . . . ?
C14 C13 C18 C22A -166.7(3) . . . . ?
As2 C13 C18 C22A 13.2(3) . . . . ?
C14 C13 C18 C22B 166.5(3) . . . . ?
As2 C13 C18 C22B -13.6(3) . . . . ?
C15 C14 C19 C21 -35.9(2) . . . . ?
C13 C14 C19 C21 147.68(16) . . . . ?
C15 C14 C19 C20 88.57(18) . . . . ?
C13 C14 C19 C20 -87.84(19) . . . . ?
C17 C18 C22A C23A 91.4(3) . . . . ?
C13 C18 C22A C23A -100.0(3) . . . . ?
C17 C18 C22A C24A -31.3(4) . . . . ?
C13 C18 C22A C24A 137.3(3) . . . . ?
C17 C18 C22B C23B -95.0(3) . . . . ?
C13 C18 C22B C23B 100.0(3) . . . . ?
C17 C18 C22B C24B 27.8(6) . . . . ?
C13 C18 C22B C24B -137.2(4) . . . . ?
C30 C25 C26 C27 -2.3(2) . . . . ?
As3 C25 C26 C27 -170.57(12) . . . . ?
C30 C25 C26 C31 171.73(14) . . . . ?
As3 C25 C26 C31 3.4(2) . . . . ?
C25 C26 C27 C28 1.0(3) . . . . ?
C31 C26 C27 C28 -173.33(16) . . . . ?
C26 C27 C28 C29 0.2(3) . . . . ?
C27 C28 C29 C30 0.0(3) . . . . ?
C28 C29 C30 C25 -1.3(3) . . . . ?
C28 C29 C30 C34 173.48(16) . . . . ?
C26 C25 C30 C29 2.4(2) . . . . ?
As3 C25 C30 C29 170.47(12) . . . . ?
C26 C25 C30 C34 -172.06(15) . . . . ?
As3 C25 C30 C34 -4.0(2) . . . . ?
C27 C26 C31 C32 85.74(18) . . . . ?
C25 C26 C31 C32 -88.33(18) . . . . ?
C27 C26 C31 C33 -38.3(2) . . . . ?
C25 C26 C31 C33 147.59(15) . . . . ?
C29 C30 C34 C35 36.4(2) . . . . ?
C25 C30 C34 C35 -149.05(16) . . . . ?
C29 C30 C34 C36 -87.76(19) . . . . ?
C25 C30 C34 C36 86.74(19) . . . . ?

_refine_diff_density_max         0.572
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.064


