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

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

data_XCD71
_database_code_depnum_ccdc_archive 'CCDC 1949410'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record             
;
2019-08-26 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;
_audit_creation_date             2019-07-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3

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

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H62 As2 Cl2 N2 O Zr, C H2 Cl2'
_chemical_formula_sum            'C53 H64 As2 Cl4 N2 O Zr'
_chemical_formula_weight         1127.92
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   12.3693(6)
_cell_length_b                   16.8828(5)
_cell_length_c                   25.0260(11)
_cell_angle_alpha                90
_cell_angle_beta                 102.369(4)
_cell_angle_gamma                90
_cell_volume                     5104.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22326
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      2.03
_shelx_estimated_absorpt_T_max   0.877
_shelx_estimated_absorpt_T_min   0.765
_exptl_absorpt_coefficient_mu    1.751
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_correction_T_min  0.3343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.077
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22922
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.669
_diffrn_reflns_theta_min         2.034
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_details      
;
 386 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7749
_reflns_number_total             12038
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         12038
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0606P)²+0.9247P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1305
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C18(H18), C20(H20),
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C35(H35), C42(H42),
  C44(H44)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Zr Zr 0.47382(4) 0.81963(2) 0.62670(2) 0.02378(11) Uani 1 1 d . . . . .
As1 As 0.21252(4) 0.79910(2) 0.61764(2) 0.02280(11) Uani 1 1 d . . . . .
As2 As 0.40394(4) 0.85681(3) 0.74098(2) 0.02410(11) Uani 1 1 d . . . . .
Cl1 Cl 0.54884(10) 0.95531(6) 0.64758(5) 0.0302(3) Uani 1 1 d . . . . .
Cl2 Cl 0.45367(10) 0.68089(7) 0.59187(5) 0.0336(3) Uani 1 1 d . . . . .
O O 0.6088(3) 0.81724(19) 0.58180(12) 0.0328(8) Uani 1 1 d . . . . .
N1 N 0.3180(3) 0.8482(2) 0.58553(14) 0.0243(8) Uani 1 1 d . . . . .
N2 N 0.4981(3) 0.7941(2) 0.70793(14) 0.0247(8) Uani 1 1 d . . . . .
C1 C 0.3214(4) 0.8609(3) 0.52950(18) 0.0244(9) Uani 1 1 d . . . . .
C2 C 0.3581(4) 0.9344(3) 0.51434(18) 0.0276(10) Uani 1 1 d . . . . .
H2 H 0.374391 0.975796 0.540530 0.033 Uiso 1 1 calc R . . . .
C3 C 0.3706(4) 0.9468(3) 0.46128(19) 0.0310(11) Uani 1 1 d . . . . .
H3 H 0.395714 0.996855 0.451443 0.037 Uiso 1 1 calc R . . . .
C4 C 0.3469(4) 0.8871(3) 0.42219(19) 0.0332(11) Uani 1 1 d . . . . .
H4 H 0.355686 0.896042 0.385885 0.040 Uiso 1 1 calc R . . . .
C5 C 0.3105(4) 0.8144(3) 0.43689(19) 0.0309(11) Uani 1 1 d . . . . .
H5 H 0.294355 0.773272 0.410498 0.037 Uiso 1 1 calc R . . . .
C6 C 0.2973(4) 0.8012(3) 0.48994(18) 0.0268(10) Uani 1 1 d . . . . .
H6 H 0.271666 0.751130 0.499422 0.032 Uiso 1 1 calc R . . . .
C7 C 0.1143(4) 0.8814(2) 0.63733(17) 0.0239(9) Uani 1 1 d . . . . .
C8 C 0.0370(4) 0.8497(3) 0.66551(18) 0.0262(10) Uani 1 1 d . . . . .
C9 C -0.0373(4) 0.8996(3) 0.68279(18) 0.0277(10) Uani 1 1 d . . . . .
H9 H -0.089345 0.877423 0.701460 0.033 Uiso 1 1 calc R . . . .
C10 C -0.0387(4) 0.9805(3) 0.67400(18) 0.0273(10) Uani 1 1 d . . . . .
C11 C 0.0406(4) 1.0113(3) 0.64799(19) 0.0312(11) Uani 1 1 d . . . . .
H11 H 0.042345 1.066892 0.642332 0.037 Uiso 1 1 calc R . . . .
C12 C 0.1176(4) 0.9640(2) 0.62991(17) 0.0250(9) Uani 1 1 d . . . . .
C13 C 0.2018(4) 1.0042(2) 0.60366(18) 0.0279(10) Uani 1 1 d . . . . .
H13A H 0.276442 0.989597 0.623308 0.042 Uiso 1 1 calc GR . . . .
H13B H 0.192670 1.061733 0.605202 0.042 Uiso 1 1 calc GR . . . .
H13C H 0.191041 0.987338 0.565410 0.042 Uiso 1 1 calc GR . . . .
C14 C -0.1232(4) 1.0327(3) 0.6924(2) 0.0345(11) Uani 1 1 d . . . . .
H14A H -0.194590 1.005259 0.686134 0.052 Uiso 1 1 calc GR . . . .
H14B H -0.131210 1.082283 0.671561 0.052 Uiso 1 1 calc GR . . . .
H14C H -0.098443 1.044420 0.731479 0.052 Uiso 1 1 calc GR . . . .
C15 C 0.0303(4) 0.7622(2) 0.67731(18) 0.0272(10) Uani 1 1 d . . . . .
H15A H -0.029061 0.752837 0.696952 0.041 Uiso 1 1 calc GR . . . .
H15B H 0.100922 0.744364 0.699831 0.041 Uiso 1 1 calc GR . . . .
H15C H 0.014738 0.732679 0.642792 0.041 Uiso 1 1 calc GR . . . .
C16 C 0.1063(4) 0.7464(2) 0.55710(17) 0.0236(9) Uani 1 1 d . . . . .
C17 C 0.0979(4) 0.6635(3) 0.56168(18) 0.0267(10) Uani 1 1 d . . . . .
C18 C 0.0169(4) 0.6232(3) 0.52386(18) 0.0294(10) Uani 1 1 d . . . . .
H18 H 0.009223 0.567629 0.527765 0.035 Uiso 1 1 calc R . . . .
C19 C -0.0528(4) 0.6617(3) 0.48085(18) 0.0287(10) Uani 1 1 d . . . . .
C20 C -0.0411(4) 0.7435(3) 0.47686(18) 0.0266(10) Uani 1 1 d . . . . .
H20 H -0.087847 0.770756 0.447553 0.032 Uiso 1 1 calc R . . . .
C21 C 0.0359(4) 0.7867(3) 0.51380(17) 0.0254(10) Uani 1 1 d . . . . .
C22 C 0.0383(4) 0.8749(3) 0.50466(18) 0.0280(10) Uani 1 1 d . . . . .
H22A H 0.002870 0.902064 0.531029 0.042 Uiso 1 1 calc GR . . . .
H22B H -0.001739 0.887370 0.467407 0.042 Uiso 1 1 calc GR . . . .
H22C H 0.115184 0.892734 0.509613 0.042 Uiso 1 1 calc GR . . . .
C23 C -0.1372(4) 0.6167(3) 0.43963(19) 0.0362(11) Uani 1 1 d . . . . .
H23A H -0.102532 0.569612 0.427670 0.054 Uiso 1 1 calc GR . . . .
H23B H -0.165649 0.650698 0.408010 0.054 Uiso 1 1 calc GR . . . .
H23C H -0.198432 0.600463 0.456407 0.054 Uiso 1 1 calc GR . . . .
C24 C 0.1707(4) 0.6162(2) 0.60693(19) 0.0318(11) Uani 1 1 d . . . . .
H24A H 0.248569 0.624426 0.605718 0.048 Uiso 1 1 calc GR . . . .
H24B H 0.152507 0.559860 0.601962 0.048 Uiso 1 1 calc GR . . . .
H24C H 0.158100 0.633880 0.642409 0.048 Uiso 1 1 calc GR . . . .
C25 C 0.6081(4) 0.7688(3) 0.72928(17) 0.0258(10) Uani 1 1 d . . . . .
C26 C 0.6380(4) 0.6913(3) 0.71740(19) 0.0296(10) Uani 1 1 d . . . . .
H26 H 0.583353 0.656715 0.697397 0.035 Uiso 1 1 calc R . . . .
C27 C 0.7461(4) 0.6646(3) 0.7345(2) 0.0367(12) Uani 1 1 d . . . . .
H27 H 0.765128 0.612426 0.725645 0.044 Uiso 1 1 calc R . . . .
C28 C 0.8268(4) 0.7141(3) 0.7646(2) 0.0404(13) Uani 1 1 d . . . . .
H28 H 0.900414 0.695645 0.777183 0.048 Uiso 1 1 calc R . . . .
C29 C 0.7980(4) 0.7912(3) 0.77600(19) 0.0358(12) Uani 1 1 d . . . . .
H29 H 0.852500 0.825200 0.796714 0.043 Uiso 1 1 calc R . . . .
C30 C 0.6911(4) 0.8189(3) 0.75753(18) 0.0294(10) Uani 1 1 d . . . . .
H30 H 0.673959 0.872385 0.764115 0.035 Uiso 1 1 calc R . . . .
C31 C 0.3039(4) 0.7865(3) 0.77267(17) 0.0249(9) Uani 1 1 d . . . . .
C32 C 0.2300(4) 0.8299(3) 0.79643(18) 0.0266(10) Uani 1 1 d . . . . .
C33 C 0.1601(4) 0.7897(3) 0.82390(18) 0.0279(10) Uani 1 1 d . . . . .
H33 H 0.110682 0.819295 0.840397 0.033 Uiso 1 1 calc R . . . .
C34 C 0.1603(4) 0.7083(3) 0.82794(18) 0.0289(10) Uani 1 1 d . . . . .
C35 C 0.2279(4) 0.6661(3) 0.80027(17) 0.0267(10) Uani 1 1 d . . . . .
H35 H 0.225588 0.609851 0.800655 0.032 Uiso 1 1 calc R . . . .
C36 C 0.2990(4) 0.7037(3) 0.77200(18) 0.0270(10) Uani 1 1 d . . . . .
C37 C 0.3667(4) 0.6521(3) 0.74205(18) 0.0286(10) Uani 1 1 d . . . . .
H37A H 0.358843 0.671327 0.704454 0.043 Uiso 1 1 calc GR . . . .
H37B H 0.340393 0.597312 0.741446 0.043 Uiso 1 1 calc GR . . . .
H37C H 0.444785 0.654330 0.760841 0.043 Uiso 1 1 calc GR . . . .
C38 C 0.0897(4) 0.6658(3) 0.86164(19) 0.0330(11) Uani 1 1 d . . . . .
H38A H 0.136820 0.647226 0.895947 0.050 Uiso 1 1 calc GR . . . .
H38B H 0.053018 0.620369 0.840987 0.050 Uiso 1 1 calc GR . . . .
H38C H 0.033765 0.702292 0.869745 0.050 Uiso 1 1 calc GR . . . .
C39 C 0.2223(4) 0.9193(3) 0.79388(19) 0.0301(10) Uani 1 1 d . . . . .
H39A H 0.291136 0.942313 0.814898 0.045 Uiso 1 1 calc GR . . . .
H39B H 0.160041 0.936877 0.809386 0.045 Uiso 1 1 calc GR . . . .
H39C H 0.210803 0.936603 0.755696 0.045 Uiso 1 1 calc GR . . . .
C40 C 0.5038(4) 0.8944(3) 0.80973(18) 0.0259(10) Uani 1 1 d . . . . .
C41 C 0.5230(4) 0.9762(3) 0.81386(18) 0.0270(10) Uani 1 1 d . . . . .
C42 C 0.5954(4) 1.0059(3) 0.8607(2) 0.0340(11) Uani 1 1 d . . . . .
H42 H 0.608225 1.061374 0.863821 0.041 Uiso 1 1 calc R . . . .
C43 C 0.6487(4) 0.9567(3) 0.90272(19) 0.0341(11) Uani 1 1 d . . . . .
C44 C 0.6274(4) 0.8768(3) 0.89783(19) 0.0323(11) Uani 1 1 d . . . . .
H44 H 0.662698 0.842739 0.926535 0.039 Uiso 1 1 calc R . . . .
C45 C 0.5559(4) 0.8433(3) 0.85242(18) 0.0276(10) Uani 1 1 d . . . . .
C46 C 0.5396(4) 0.7551(3) 0.85242(19) 0.0302(10) Uani 1 1 d . . . . .
H46A H 0.461597 0.743305 0.851353 0.045 Uiso 1 1 calc GR . . . .
H46B H 0.585644 0.732463 0.885680 0.045 Uiso 1 1 calc GR . . . .
H46C H 0.560915 0.732097 0.820240 0.045 Uiso 1 1 calc GR . . . .
C47 C 0.7301(4) 0.9902(3) 0.9517(2) 0.0454(14) Uani 1 1 d . . . . .
H47A H 0.717369 0.965509 0.985303 0.068 Uiso 1 1 calc GR . . . .
H47B H 0.719566 1.047565 0.953540 0.068 Uiso 1 1 calc GR . . . .
H47C H 0.805886 0.979046 0.947989 0.068 Uiso 1 1 calc GR . . . .
C48 C 0.4685(4) 1.0343(2) 0.77045(19) 0.0337(11) Uani 1 1 d . . . . .
H48A H 0.484221 1.018939 0.735115 0.051 Uiso 1 1 calc GR . . . .
H48B H 0.497543 1.087557 0.780172 0.051 Uiso 1 1 calc GR . . . .
H48C H 0.388302 1.033963 0.767879 0.051 Uiso 1 1 calc GR . . . .
C49 C 0.7259(4) 0.8262(3) 0.6076(2) 0.0344(11) Uani 1 1 d . . . . .
H49A H 0.743584 0.797854 0.642989 0.041 Uiso 1 1 calc R . . . .
H49B H 0.745089 0.882869 0.614029 0.041 Uiso 1 1 calc R . . . .
C50 C 0.7875(5) 0.7910(4) 0.5681(2) 0.0594(18) Uani 1 1 d . . . . .
H50A H 0.859594 0.817811 0.570369 0.071 Uiso 1 1 calc R . . . .
H50B H 0.800382 0.733697 0.574887 0.071 Uiso 1 1 calc R . . . .
C51 C 0.7120(5) 0.8053(4) 0.5141(2) 0.0574(18) Uani 1 1 d . . . . .
H51A H 0.725301 0.765958 0.486841 0.069 Uiso 1 1 calc R . . . .
H51B H 0.723523 0.859048 0.500459 0.069 Uiso 1 1 calc R . . . .
C52 C 0.5977(4) 0.7971(3) 0.52367(19) 0.0373(12) Uani 1 1 d . . . . .
H52A H 0.546238 0.833958 0.500070 0.045 Uiso 1 1 calc R . . . .
H52B H 0.570194 0.742283 0.516257 0.045 Uiso 1 1 calc R . . . .
Cl3 Cl 0.55685(15) 0.47804(9) 0.65012(6) 0.0613(4) Uani 1 1 d . . . . .
Cl4 Cl 0.47519(15) 0.39536(9) 0.54721(7) 0.0659(5) Uani 1 1 d . . . . .
C53 C 0.4648(5) 0.4792(3) 0.5869(2) 0.0532(15) Uani 1 1 d . . . . .
H53A H 0.478880 0.527047 0.566552 0.064 Uiso 1 1 calc R . . . .
H53B H 0.388358 0.482922 0.592860 0.064 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr As1 3.2101(6) . ?
Zr As2 3.2216(6) . ?
Zr Cl1 2.4846(12) . ?
Zr Cl2 2.4932(12) . ?
Zr O 2.204(3) . ?
Zr N1 2.039(4) . ?
Zr N2 2.036(4) . ?
Zr C1 2.827(5) . ?
As1 N1 1.867(3) . ?
As1 C7 1.977(4) . ?
As1 C16 1.990(4) . ?
As2 N2 1.891(3) . ?
As2 C31 1.998(4) . ?
As2 C40 1.995(5) . ?
O C49 1.461(6) . ?
O C52 1.472(5) . ?
N1 C1 1.428(5) . ?
N2 C25 1.417(6) . ?
C1 C2 1.401(6) . ?
C1 C6 1.399(6) . ?
C2 C3 1.386(6) . ?
C3 C4 1.393(7) . ?
C4 C5 1.383(6) . ?
C5 C6 1.390(6) . ?
C7 C8 1.410(6) . ?
C7 C12 1.408(6) . ?
C8 C9 1.381(6) . ?
C8 C15 1.513(6) . ?
C9 C10 1.383(6) . ?
C10 C11 1.390(6) . ?
C10 C14 1.512(6) . ?
C11 C12 1.391(6) . ?
C12 C13 1.507(6) . ?
C16 C17 1.410(6) . ?
C16 C21 1.411(6) . ?
C17 C18 1.399(6) . ?
C17 C24 1.514(6) . ?
C18 C19 1.388(7) . ?
C19 C20 1.395(6) . ?
C19 C23 1.507(6) . ?
C20 C21 1.384(6) . ?
C21 C22 1.509(6) . ?
C25 C26 1.409(6) . ?
C25 C30 1.399(6) . ?
C26 C27 1.389(7) . ?
C27 C28 1.393(7) . ?
C28 C29 1.395(7) . ?
C29 C30 1.386(7) . ?
C31 C32 1.399(6) . ?
C31 C36 1.399(6) . ?
C32 C33 1.392(6) . ?
C32 C39 1.512(6) . ?
C33 C34 1.378(6) . ?
C34 C35 1.391(6) . ?
C34 C38 1.517(6) . ?
C35 C36 1.394(6) . ?
C36 C37 1.514(6) . ?
C40 C41 1.402(6) . ?
C40 C45 1.415(6) . ?
C41 C42 1.407(7) . ?
C41 C48 1.510(6) . ?
C42 C43 1.390(7) . ?
C43 C44 1.375(7) . ?
C43 C47 1.520(7) . ?
C44 C45 1.400(7) . ?
C45 C46 1.503(6) . ?
C49 C50 1.495(6) . ?
C50 C51 1.489(8) . ?
C51 C52 1.490(7) . ?
Cl3 C53 1.740(7) . ?
Cl4 C53 1.751(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
As1 Zr As2 68.047(15) . . ?
Cl1 Zr As1 116.07(3) . . ?
Cl1 Zr As2 78.05(3) . . ?
Cl1 Zr Cl2 160.84(4) . . ?
Cl1 Zr C1 95.98(9) . . ?
Cl2 Zr As1 81.38(3) . . ?
Cl2 Zr As2 117.88(3) . . ?
Cl2 Zr C1 86.11(9) . . ?
O Zr As1 145.44(9) . . ?
O Zr As2 146.40(9) . . ?
O Zr Cl1 80.47(9) . . ?
O Zr Cl2 80.47(9) . . ?
O Zr C1 90.24(12) . . ?
N1 Zr As2 89.89(9) . . ?
N1 Zr Cl1 99.09(10) . . ?
N1 Zr Cl2 91.88(10) . . ?
N1 Zr O 118.95(13) . . ?
N1 Zr C1 28.72(12) . . ?
N2 Zr As1 88.77(10) . . ?
N2 Zr As2 33.43(10) . . ?
N2 Zr Cl1 90.97(10) . . ?
N2 Zr Cl2 97.59(10) . . ?
N2 Zr O 122.63(14) . . ?
N2 Zr N1 118.42(14) . . ?
N2 Zr C1 147.11(13) . . ?
C1 Zr As1 59.34(8) . . ?
C1 Zr As2 117.37(8) . . ?
N1 As1 C7 108.58(16) . . ?
N1 As1 C16 106.21(16) . . ?
C7 As1 Zr 124.75(13) . . ?
C7 As1 C16 99.39(18) . . ?
C16 As1 Zr 126.34(11) . . ?
N2 As2 C31 109.45(16) . . ?
N2 As2 C40 103.27(17) . . ?
C31 As2 Zr 122.93(12) . . ?
C40 As2 Zr 126.39(12) . . ?
C40 As2 C31 99.70(17) . . ?
C49 O Zr 124.1(3) . . ?
C49 O C52 109.5(3) . . ?
C52 O Zr 126.0(3) . . ?
As1 N1 Zr 110.45(17) . . ?
C1 N1 Zr 107.9(3) . . ?
C1 N1 As1 131.3(3) . . ?
As2 N2 Zr 110.18(18) . . ?
C25 N2 Zr 111.4(3) . . ?
C25 N2 As2 129.4(3) . . ?
C2 C1 Zr 104.8(3) . . ?
C2 C1 N1 118.5(4) . . ?
C6 C1 Zr 115.7(3) . . ?
C6 C1 N1 122.7(4) . . ?
C6 C1 C2 118.6(4) . . ?
C3 C2 C1 120.2(4) . . ?
C2 C3 C4 120.9(4) . . ?
C5 C4 C3 119.2(4) . . ?
C4 C5 C6 120.6(4) . . ?
C5 C6 C1 120.6(4) . . ?
C8 C7 As1 112.2(3) . . ?
C12 C7 As1 128.8(3) . . ?
C12 C7 C8 118.9(4) . . ?
C7 C8 C15 122.6(4) . . ?
C9 C8 C7 119.5(4) . . ?
C9 C8 C15 117.8(4) . . ?
C8 C9 C10 122.6(4) . . ?
C9 C10 C11 117.2(4) . . ?
C9 C10 C14 120.9(4) . . ?
C11 C10 C14 121.9(4) . . ?
C10 C11 C12 122.6(4) . . ?
C7 C12 C13 123.1(4) . . ?
C11 C12 C7 119.0(4) . . ?
C11 C12 C13 117.9(4) . . ?
C17 C16 As1 115.5(3) . . ?
C17 C16 C21 119.8(4) . . ?
C21 C16 As1 124.6(3) . . ?
C16 C17 C24 122.8(4) . . ?
C18 C17 C16 118.8(4) . . ?
C18 C17 C24 118.4(4) . . ?
C19 C18 C17 122.2(4) . . ?
C18 C19 C20 117.5(4) . . ?
C18 C19 C23 121.3(4) . . ?
C20 C19 C23 121.2(4) . . ?
C21 C20 C19 122.8(4) . . ?
C16 C21 C22 124.3(4) . . ?
C20 C21 C16 118.8(4) . . ?
C20 C21 C22 116.9(4) . . ?
C26 C25 N2 118.3(4) . . ?
C30 C25 N2 123.4(4) . . ?
C30 C25 C26 118.1(4) . . ?
C27 C26 C25 121.0(5) . . ?
C26 C27 C28 120.2(5) . . ?
C27 C28 C29 119.1(5) . . ?
C30 C29 C28 120.9(5) . . ?
C29 C30 C25 120.6(5) . . ?
C32 C31 As2 111.9(3) . . ?
C36 C31 As2 128.1(3) . . ?
C36 C31 C32 119.9(4) . . ?
C31 C32 C39 123.1(4) . . ?
C33 C32 C31 119.0(4) . . ?
C33 C32 C39 117.9(4) . . ?
C34 C33 C32 122.2(4) . . ?
C33 C34 C35 117.7(4) . . ?
C33 C34 C38 121.4(4) . . ?
C35 C34 C38 120.9(4) . . ?
C34 C35 C36 122.1(4) . . ?
C31 C36 C37 123.6(4) . . ?
C35 C36 C31 118.6(4) . . ?
C35 C36 C37 117.7(4) . . ?
C41 C40 As2 116.1(3) . . ?
C41 C40 C45 120.1(4) . . ?
C45 C40 As2 123.7(3) . . ?
C40 C41 C42 118.7(4) . . ?
C40 C41 C48 123.0(4) . . ?
C42 C41 C48 118.4(4) . . ?
C43 C42 C41 122.1(4) . . ?
C42 C43 C47 120.8(5) . . ?
C44 C43 C42 118.0(5) . . ?
C44 C43 C47 121.2(5) . . ?
C43 C44 C45 122.9(5) . . ?
C40 C45 C46 124.3(4) . . ?
C44 C45 C40 118.2(4) . . ?
C44 C45 C46 117.4(4) . . ?
O C49 C50 105.3(4) . . ?
C51 C50 C49 103.1(5) . . ?
C50 C51 C52 105.7(4) . . ?
O C52 C51 104.3(4) . . ?
Cl3 C53 Cl4 113.2(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_XCD350
_database_code_depnum_ccdc_archive 'CCDC 1949412'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record             
;
2019-08-26 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;
_audit_creation_date             2019-07-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3

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

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H66 As2 N4 Zr'
_chemical_formula_sum            'C52 H66 As2 N4 Zr'
_chemical_formula_weight         988.14
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3140(6)
_cell_length_b                   13.5043(8)
_cell_length_c                   19.5598(12)
_cell_angle_alpha                95.792(5)
_cell_angle_beta                 95.805(5)
_cell_angle_gamma                103.161(5)
_cell_volume                     2363.7(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    36275
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.67
_cell_measurement_theta_min      1.77
_shelx_estimated_absorpt_T_max   0.624
_shelx_estimated_absorpt_T_min   0.576
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  0.6581
_exptl_absorpt_correction_T_min  0.4374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.336
_exptl_crystal_size_min          0.314
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23999
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.629
_diffrn_reflns_theta_min         1.769
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.810
_diffrn_measurement_details      
;
 419 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10443
_reflns_number_total             12895
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         12895
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0392
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0602P)²+0.5012P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1053
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C18(H18), C20(H20),
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C35(H35), C42(H42),
  C44(H44)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Zr Zr 0.42910(2) 0.27477(2) 0.13951(2) 0.01579(6) Uani 1 1 d . . . . .
As1 As 0.29949(3) 0.12621(2) 0.25644(2) 0.01665(6) Uani 1 1 d . . . . .
As2 As 0.44300(3) 0.39269(2) 0.28420(2) 0.01643(6) Uani 1 1 d . . . . .
N1 N 0.3992(2) 0.13406(14) 0.17764(10) 0.0172(4) Uani 1 1 d . . . . .
N2 N 0.3603(2) 0.39417(14) 0.19364(10) 0.0179(4) Uani 1 1 d . . . . .
N3 N 0.2955(2) 0.25157(16) 0.04716(11) 0.0243(4) Uani 1 1 d . . . . .
N4 N 0.6349(2) 0.33497(14) 0.11419(11) 0.0204(4) Uani 1 1 d . . . . .
C1 C 0.4077(3) 0.04734(17) 0.13166(12) 0.0182(4) Uani 1 1 d . . . . .
C2 C 0.2808(3) -0.01974(18) 0.09546(12) 0.0215(5) Uani 1 1 d . . . . .
H2 H 0.185820 -0.007969 0.101358 0.026 Uiso 1 1 calc R . . . .
C3 C 0.2914(3) -0.10405(18) 0.05064(13) 0.0259(5) Uani 1 1 d . . . . .
H3 H 0.203468 -0.149862 0.026940 0.031 Uiso 1 1 calc R . . . .
C4 C 0.4281(3) -0.12156(19) 0.04037(13) 0.0279(6) Uani 1 1 d . . . . .
H4 H 0.434706 -0.179955 0.010544 0.033 Uiso 1 1 calc R . . . .
C5 C 0.5550(3) -0.05378(19) 0.07368(13) 0.0258(5) Uani 1 1 d . . . . .
H5 H 0.649604 -0.064352 0.065622 0.031 Uiso 1 1 calc R . . . .
C6 C 0.5460(3) 0.03020(18) 0.11911(12) 0.0212(5) Uani 1 1 d . . . . .
H6 H 0.634628 0.076348 0.141831 0.025 Uiso 1 1 calc R . . . .
C7 C 0.1846(3) -0.01735(17) 0.23994(12) 0.0185(4) Uani 1 1 d . . . . .
C8 C 0.0317(3) -0.03226(18) 0.21828(13) 0.0223(5) Uani 1 1 d . . . . .
C9 C -0.0568(3) -0.13073(19) 0.19994(13) 0.0249(5) Uani 1 1 d . . . . .
H9 H -0.159804 -0.140095 0.184943 0.030 Uiso 1 1 calc R . . . .
C10 C 0.0023(3) -0.21575(18) 0.20310(13) 0.0246(5) Uani 1 1 d . . . . .
C11 C 0.1519(3) -0.19985(18) 0.22634(12) 0.0236(5) Uani 1 1 d . . . . .
H11 H 0.192356 -0.257878 0.230149 0.028 Uiso 1 1 calc R . . . .
C12 C 0.2453(3) -0.10307(17) 0.24432(12) 0.0196(4) Uani 1 1 d . . . . .
C13 C 0.4079(3) -0.09528(18) 0.26477(13) 0.0230(5) Uani 1 1 d . . . . .
H13A H 0.466572 -0.051207 0.235656 0.034 Uiso 1 1 calc GR . . . .
H13B H 0.427242 -0.163766 0.258503 0.034 Uiso 1 1 calc GR . . . .
H13C H 0.435861 -0.065777 0.313487 0.034 Uiso 1 1 calc GR . . . .
C14 C -0.0930(3) -0.3218(2) 0.17821(14) 0.0321(6) Uani 1 1 d . . . . .
H14A H -0.194422 -0.325678 0.189073 0.048 Uiso 1 1 calc GR . . . .
H14B H -0.051809 -0.372136 0.201357 0.048 Uiso 1 1 calc GR . . . .
H14C H -0.094782 -0.336543 0.127993 0.048 Uiso 1 1 calc GR . . . .
C15 C -0.0406(3) 0.0559(2) 0.21230(17) 0.0332(6) Uani 1 1 d . . . . .
H15A H -0.016885 0.101925 0.256096 0.050 Uiso 1 1 calc GR . . . .
H15B H -0.148651 0.029634 0.202031 0.050 Uiso 1 1 calc GR . . . .
H15C H -0.003533 0.093616 0.174894 0.050 Uiso 1 1 calc GR . . . .
C16 C 0.4371(3) 0.12540(16) 0.34088(12) 0.0182(4) Uani 1 1 d . . . . .
C17 C 0.5926(3) 0.14415(17) 0.34829(12) 0.0203(4) Uani 1 1 d . . . . .
C18 C 0.6713(3) 0.14750(18) 0.41319(13) 0.0232(5) Uani 1 1 d . . . . .
H18 H 0.776377 0.158580 0.417112 0.028 Uiso 1 1 calc R . . . .
C19 C 0.6021(3) 0.13527(18) 0.47241(13) 0.0236(5) Uani 1 1 d . . . . .
C20 C 0.4485(3) 0.12005(18) 0.46463(13) 0.0229(5) Uani 1 1 d . . . . .
H20 H 0.398622 0.112678 0.504517 0.027 Uiso 1 1 calc R . . . .
C21 C 0.3647(3) 0.11515(17) 0.40079(12) 0.0203(5) Uani 1 1 d . . . . .
C22 C 0.1981(3) 0.09883(19) 0.39834(13) 0.0251(5) Uani 1 1 d . . . . .
H22A H 0.148783 0.032563 0.371245 0.038 Uiso 1 1 calc GR . . . .
H22B H 0.165967 0.153833 0.376635 0.038 Uiso 1 1 calc GR . . . .
H22C H 0.171420 0.099518 0.445565 0.038 Uiso 1 1 calc GR . . . .
C23 C 0.6914(3) 0.1415(2) 0.54181(13) 0.0301(6) Uani 1 1 d . . . . .
H23A H 0.722641 0.213142 0.563168 0.045 Uiso 1 1 calc GR . . . .
H23B H 0.779332 0.114835 0.535782 0.045 Uiso 1 1 calc GR . . . .
H23C H 0.630349 0.100648 0.571759 0.045 Uiso 1 1 calc GR . . . .
C24 C 0.6799(3) 0.1599(2) 0.28815(13) 0.0274(5) Uani 1 1 d . . . . .
H24A H 0.654145 0.096998 0.255145 0.041 Uiso 1 1 calc GR . . . .
H24B H 0.786449 0.176440 0.304895 0.041 Uiso 1 1 calc GR . . . .
H24C H 0.656100 0.216405 0.265175 0.041 Uiso 1 1 calc GR . . . .
C25 C 0.3122(3) 0.47316(17) 0.16284(12) 0.0191(4) Uani 1 1 d . . . . .
C26 C 0.1738(3) 0.45039(19) 0.12192(13) 0.0235(5) Uani 1 1 d . . . . .
H26 H 0.111625 0.383110 0.117480 0.028 Uiso 1 1 calc R . . . .
C27 C 0.1259(3) 0.5243(2) 0.08784(14) 0.0291(6) Uani 1 1 d . . . . .
H27 H 0.030708 0.507599 0.061067 0.035 Uiso 1 1 calc R . . . .
C28 C 0.2152(3) 0.6216(2) 0.09245(14) 0.0312(6) Uani 1 1 d . . . . .
H28 H 0.182222 0.672229 0.069027 0.037 Uiso 1 1 calc R . . . .
C29 C 0.3531(3) 0.64483(19) 0.13142(13) 0.0281(6) Uani 1 1 d . . . . .
H29 H 0.415020 0.711991 0.134610 0.034 Uiso 1 1 calc R . . . .
C30 C 0.4030(3) 0.57194(18) 0.16609(12) 0.0231(5) Uani 1 1 d . . . . .
H30 H 0.499107 0.589141 0.192075 0.028 Uiso 1 1 calc R . . . .
C31 C 0.5476(3) 0.53618(17) 0.31592(12) 0.0185(4) Uani 1 1 d . . . . .
C32 C 0.4775(3) 0.61469(17) 0.33603(12) 0.0203(5) Uani 1 1 d . . . . .
C33 C 0.5654(3) 0.71391(18) 0.35517(12) 0.0239(5) Uani 1 1 d . . . . .
H33 H 0.518661 0.766858 0.369239 0.029 Uiso 1 1 calc R . . . .
C34 C 0.7173(3) 0.73849(19) 0.35455(12) 0.0259(5) Uani 1 1 d . . . . .
C35 C 0.7844(3) 0.66013(19) 0.33484(13) 0.0249(5) Uani 1 1 d . . . . .
H35 H 0.888946 0.675552 0.334195 0.030 Uiso 1 1 calc R . . . .
C36 C 0.7025(3) 0.55990(18) 0.31607(12) 0.0208(5) Uani 1 1 d . . . . .
C37 C 0.7842(3) 0.47953(19) 0.29670(14) 0.0266(5) Uani 1 1 d . . . . .
H37A H 0.762377 0.424761 0.326103 0.040 Uiso 1 1 calc GR . . . .
H37B H 0.891397 0.510460 0.303322 0.040 Uiso 1 1 calc GR . . . .
H37C H 0.752332 0.450912 0.248020 0.040 Uiso 1 1 calc GR . . . .
C38 C 0.8089(4) 0.8469(2) 0.37536(16) 0.0384(7) Uani 1 1 d . . . . .
H38A H 0.745438 0.894888 0.369077 0.058 Uiso 1 1 calc GR . . . .
H38B H 0.889248 0.860883 0.346393 0.058 Uiso 1 1 calc GR . . . .
H38C H 0.851344 0.855213 0.424110 0.058 Uiso 1 1 calc GR . . . .
C39 C 0.3122(3) 0.59892(18) 0.33560(14) 0.0246(5) Uani 1 1 d . . . . .
H39A H 0.260770 0.554146 0.293523 0.037 Uiso 1 1 calc GR . . . .
H39B H 0.285980 0.665284 0.336569 0.037 Uiso 1 1 calc GR . . . .
H39C H 0.282232 0.567070 0.376422 0.037 Uiso 1 1 calc GR . . . .
C40 C 0.2922(3) 0.37299(16) 0.34919(12) 0.0176(4) Uani 1 1 d . . . . .
C41 C 0.3522(3) 0.37539(16) 0.41858(12) 0.0192(4) Uani 1 1 d . . . . .
C42 C 0.2580(3) 0.36808(18) 0.46963(12) 0.0219(5) Uani 1 1 d . . . . .
H42 H 0.298697 0.370390 0.516459 0.026 Uiso 1 1 calc R . . . .
C43 C 0.1060(3) 0.35749(18) 0.45403(13) 0.0232(5) Uani 1 1 d . . . . .
C44 C 0.0482(3) 0.34740(18) 0.38521(12) 0.0218(5) Uani 1 1 d . . . . .
H44 H -0.056414 0.335422 0.373623 0.026 Uiso 1 1 calc R . . . .
C45 C 0.1378(3) 0.35415(17) 0.33201(12) 0.0187(4) Uani 1 1 d . . . . .
C46 C 0.0628(3) 0.34352(18) 0.25905(12) 0.0209(5) Uani 1 1 d . . . . .
H46A H 0.079937 0.410996 0.242731 0.031 Uiso 1 1 calc GR . . . .
H46B H -0.044234 0.315284 0.257841 0.031 Uiso 1 1 calc GR . . . .
H46C H 0.103837 0.297363 0.228985 0.031 Uiso 1 1 calc GR . . . .
C47 C 0.0061(3) 0.3556(2) 0.51019(14) 0.0337(6) Uani 1 1 d . . . . .
H47A H 0.006687 0.295284 0.534115 0.051 Uiso 1 1 calc GR . . . .
H47B H -0.095430 0.352340 0.489509 0.051 Uiso 1 1 calc GR . . . .
H47C H 0.042207 0.417880 0.543447 0.051 Uiso 1 1 calc GR . . . .
C48 C 0.5160(3) 0.38629(18) 0.44026(13) 0.0228(5) Uani 1 1 d . . . . .
H48A H 0.572036 0.453927 0.432163 0.034 Uiso 1 1 calc GR . . . .
H48B H 0.549664 0.332878 0.413059 0.034 Uiso 1 1 calc GR . . . .
H48C H 0.532647 0.379122 0.489604 0.034 Uiso 1 1 calc GR . . . .
C49 C 0.1443(3) 0.1914(2) 0.03971(17) 0.0381(7) Uani 1 1 d . . . . .
H49A H 0.124592 0.162973 0.082933 0.057 Uiso 1 1 calc GR . . . .
H49B H 0.129368 0.135269 0.001822 0.057 Uiso 1 1 calc GR . . . .
H49C H 0.076039 0.234979 0.029293 0.057 Uiso 1 1 calc GR . . . .
C50 C 0.3249(4) 0.3007(2) -0.01446(14) 0.0371(7) Uani 1 1 d . . . . .
H50A H 0.258428 0.346568 -0.021482 0.056 Uiso 1 1 calc GR . . . .
H50B H 0.307671 0.248260 -0.054818 0.056 Uiso 1 1 calc GR . . . .
H50C H 0.428440 0.340427 -0.008610 0.056 Uiso 1 1 calc GR . . . .
C51 C 0.6545(3) 0.43682(19) 0.09277(15) 0.0329(6) Uani 1 1 d . . . . .
H51A H 0.561381 0.458817 0.093603 0.049 Uiso 1 1 calc GR . . . .
H51B H 0.682045 0.435050 0.045688 0.049 Uiso 1 1 calc GR . . . .
H51C H 0.733389 0.485175 0.124588 0.049 Uiso 1 1 calc GR . . . .
C52 C 0.7709(3) 0.3005(2) 0.11175(15) 0.0282(5) Uani 1 1 d . . . . .
H52A H 0.850156 0.345876 0.145026 0.042 Uiso 1 1 calc GR . . . .
H52B H 0.799763 0.301915 0.064978 0.042 Uiso 1 1 calc GR . . . .
H52C H 0.754826 0.230318 0.123594 0.042 Uiso 1 1 calc GR . . . .


_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
Zr As2 3.0798(4) . ?
Zr N1 2.0813(18) . ?
Zr N2 2.0962(18) . ?
Zr N3 2.040(2) . ?
Zr N4 2.0354(19) . ?
As1 N1 1.8782(18) . ?
As1 C7 1.966(2) . ?
As1 C16 1.988(2) . ?
As2 N2 1.8627(19) . ?
As2 C31 1.966(2) . ?
As2 C40 1.979(2) . ?
N1 C1 1.425(3) . ?
N2 C25 1.412(3) . ?
N3 C49 1.442(4) . ?
N3 C50 1.454(3) . ?
N4 C51 1.455(3) . ?
N4 C52 1.450(3) . ?
C1 C2 1.390(3) . ?
C1 C6 1.401(3) . ?
C2 C3 1.393(3) . ?
C3 C4 1.378(4) . ?
C4 C5 1.375(4) . ?
C5 C6 1.392(3) . ?
C7 C8 1.407(3) . ?
C7 C12 1.405(3) . ?
C8 C9 1.386(3) . ?
C8 C15 1.504(3) . ?
C9 C10 1.386(4) . ?
C10 C11 1.382(4) . ?
C10 C14 1.506(3) . ?
C11 C12 1.384(3) . ?
C12 C13 1.504(3) . ?
C16 C17 1.402(3) . ?
C16 C21 1.413(3) . ?
C17 C18 1.391(3) . ?
C17 C24 1.502(3) . ?
C18 C19 1.387(4) . ?
C19 C20 1.388(4) . ?
C19 C23 1.503(4) . ?
C20 C21 1.391(3) . ?
C21 C22 1.512(3) . ?
C25 C26 1.400(3) . ?
C25 C30 1.399(3) . ?
C26 C27 1.384(3) . ?
C27 C28 1.375(4) . ?
C28 C29 1.378(4) . ?
C29 C30 1.387(3) . ?
C31 C32 1.410(3) . ?
C31 C36 1.405(3) . ?
C32 C33 1.394(3) . ?
C32 C39 1.504(3) . ?
C33 C34 1.379(4) . ?
C34 C35 1.388(4) . ?
C34 C38 1.509(4) . ?
C35 C36 1.386(3) . ?
C36 C37 1.501(3) . ?
C40 C41 1.409(3) . ?
C40 C45 1.402(3) . ?
C41 C42 1.391(3) . ?
C41 C48 1.511(3) . ?
C42 C43 1.389(3) . ?
C43 C44 1.380(3) . ?
C43 C47 1.508(4) . ?
C44 C45 1.396(3) . ?
C45 C46 1.502(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
N1 Zr As2 92.70(5) . . ?
N1 Zr N2 118.94(7) . . ?
N2 Zr As2 36.27(5) . . ?
N3 Zr As2 136.43(6) . . ?
N3 Zr N1 107.03(8) . . ?
N3 Zr N2 101.68(8) . . ?
N4 Zr As2 101.71(6) . . ?
N4 Zr N1 116.37(8) . . ?
N4 Zr N2 107.31(8) . . ?
N4 Zr N3 103.33(9) . . ?
N1 As1 C7 100.94(9) . . ?
N1 As1 C16 111.36(9) . . ?
C7 As1 C16 101.46(9) . . ?
N2 As2 C31 104.34(9) . . ?
N2 As2 C40 112.63(9) . . ?
C31 As2 Zr 126.69(7) . . ?
C31 As2 C40 100.14(9) . . ?
C40 As2 Zr 128.15(7) . . ?
As1 N1 Zr 114.45(9) . . ?
C1 N1 Zr 117.66(14) . . ?
C1 N1 As1 124.24(14) . . ?
As2 N2 Zr 101.98(8) . . ?
C25 N2 Zr 124.63(14) . . ?
C25 N2 As2 129.89(15) . . ?
C49 N3 Zr 120.91(18) . . ?
C49 N3 C50 110.7(2) . . ?
C50 N3 Zr 127.79(19) . . ?
C51 N4 Zr 114.66(16) . . ?
C52 N4 Zr 135.25(16) . . ?
C52 N4 C51 110.1(2) . . ?
C2 C1 N1 121.6(2) . . ?
C2 C1 C6 117.9(2) . . ?
C6 C1 N1 120.4(2) . . ?
C1 C2 C3 120.8(2) . . ?
C4 C3 C2 120.6(2) . . ?
C5 C4 C3 119.4(2) . . ?
C4 C5 C6 120.6(2) . . ?
C5 C6 C1 120.7(2) . . ?
C8 C7 As1 115.50(16) . . ?
C12 C7 As1 125.04(18) . . ?
C12 C7 C8 119.3(2) . . ?
C7 C8 C15 122.2(2) . . ?
C9 C8 C7 120.0(2) . . ?
C9 C8 C15 117.8(2) . . ?
C10 C9 C8 121.2(2) . . ?
C9 C10 C14 120.5(2) . . ?
C11 C10 C9 118.1(2) . . ?
C11 C10 C14 121.3(2) . . ?
C10 C11 C12 122.9(2) . . ?
C7 C12 C13 123.4(2) . . ?
C11 C12 C7 118.5(2) . . ?
C11 C12 C13 118.1(2) . . ?
C17 C16 As1 128.09(18) . . ?
C17 C16 C21 118.5(2) . . ?
C21 C16 As1 112.99(17) . . ?
C16 C17 C24 122.5(2) . . ?
C18 C17 C16 119.8(2) . . ?
C18 C17 C24 117.7(2) . . ?
C19 C18 C17 122.5(2) . . ?
C18 C19 C20 117.0(2) . . ?
C18 C19 C23 120.9(2) . . ?
C20 C19 C23 122.1(2) . . ?
C19 C20 C21 122.7(2) . . ?
C16 C21 C22 122.4(2) . . ?
C20 C21 C16 119.4(2) . . ?
C20 C21 C22 118.2(2) . . ?
C26 C25 N2 119.3(2) . . ?
C30 C25 N2 122.6(2) . . ?
C30 C25 C26 117.8(2) . . ?
C27 C26 C25 121.1(2) . . ?
C28 C27 C26 120.4(3) . . ?
C27 C28 C29 119.3(2) . . ?
C28 C29 C30 121.2(2) . . ?
C29 C30 C25 120.1(2) . . ?
C32 C31 As2 124.62(18) . . ?
C36 C31 As2 115.97(16) . . ?
C36 C31 C32 119.4(2) . . ?
C31 C32 C39 124.0(2) . . ?
C33 C32 C31 118.4(2) . . ?
C33 C32 C39 117.6(2) . . ?
C34 C33 C32 122.8(2) . . ?
C33 C34 C35 118.0(2) . . ?
C33 C34 C38 121.3(2) . . ?
C35 C34 C38 120.6(3) . . ?
C36 C35 C34 121.6(2) . . ?
C31 C36 C37 122.0(2) . . ?
C35 C36 C31 119.8(2) . . ?
C35 C36 C37 118.1(2) . . ?
C41 C40 As2 113.89(17) . . ?
C45 C40 As2 126.57(17) . . ?
C45 C40 C41 119.5(2) . . ?
C40 C41 C48 122.6(2) . . ?
C42 C41 C40 119.2(2) . . ?
C42 C41 C48 118.2(2) . . ?
C43 C42 C41 121.8(2) . . ?
C42 C43 C47 121.4(2) . . ?
C44 C43 C42 118.0(2) . . ?
C44 C43 C47 120.7(2) . . ?
C43 C44 C45 122.4(2) . . ?
C40 C45 C46 123.4(2) . . ?
C44 C45 C40 118.8(2) . . ?
C44 C45 C46 117.7(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_XCD091
_database_code_depnum_ccdc_archive 'CCDC 1949414'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record             
;
2019-08-26 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;
_audit_creation_date             2019-07-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3

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

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H35 Al As Cl2 N O'
_chemical_formula_sum            'C28 H35 Al As Cl2 N O'
_chemical_formula_weight         574.37
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3091(7)
_cell_length_b                   12.8303(10)
_cell_length_c                   13.3272(10)
_cell_angle_alpha                86.646(6)
_cell_angle_beta                 87.317(6)
_cell_angle_gamma                85.587(6)
_cell_volume                     1412.87(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8059
_cell_measurement_temperature    210
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      1.60
_shelx_estimated_absorpt_T_max   0.845
_shelx_estimated_absorpt_T_min   0.706
_exptl_absorpt_coefficient_mu    1.444
_exptl_absorpt_correction_T_max  0.8499
_exptl_absorpt_correction_T_min  0.7119
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.121
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.1076
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14629
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.549
_diffrn_reflns_theta_min         1.594
_diffrn_ambient_temperature      210
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
 204 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           0.000
_diffrn_source_power             0.000
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_source_voltage           0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4720
_reflns_number_total             7780
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         7780
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0575
_refine_ls_restrained_S_all      0.923
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0434P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1172
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H25C(0.5) H25D(0.5) H25A(0.5) H25B(0.5) C26A(0.5) H26A(0.5)
 H26B(0.5) C26B(0.5) H26C(0.5) H26D(0.5) C27A(0.5) H27A(0.5) H27B(0.5)
 C27B(0.5) H27C(0.5) H27D(0.5) H28A(0.5) H28B(0.5) H28C(0.5) H28D(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C25(H25C,H25D), C25(H25A,H25B), C26A(H26A,H26B), C26B(H26C,H26D), C27A(H27A,
 H27B), C27B(H27C,H27D), C28(H28A,H28B), C28(H28C,H28D)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C18(H18), C20(H20)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
As As 0.16931(5) 0.34421(3) 0.27126(3) 0.03284(10) Uani 1 1 d . . . . .
Cl1 Cl 0.65489(14) 0.24695(9) 0.19082(8) 0.0553(3) Uani 1 1 d . . . . .
Cl2 Cl 0.47021(14) 0.03626(7) 0.31653(8) 0.0498(3) Uani 1 1 d . . . . .
Al Al 0.50649(14) 0.19969(8) 0.31635(8) 0.0367(3) Uani 1 1 d . . . . .
O O 0.6500(4) 0.1998(2) 0.4202(2) 0.0464(6) Uani 1 1 d . . . . .
N N 0.3350(4) 0.2874(2) 0.3545(2) 0.0348(6) Uani 1 1 d . . . . .
C1 C 0.2863(5) 0.2941(3) 0.4584(3) 0.0353(7) Uani 1 1 d . . . . .
C2 C 0.3113(5) 0.2088(3) 0.5272(3) 0.0448(9) Uani 1 1 d . . . . .
H2 H 0.360309 0.145454 0.504644 0.054 Uiso 1 1 calc R . . . .
C3 C 0.2653(6) 0.2155(4) 0.6281(3) 0.0538(11) Uani 1 1 d . . . . .
H3 H 0.286044 0.157538 0.673282 0.065 Uiso 1 1 calc R . . . .
C4 C 0.1894(6) 0.3069(4) 0.6626(3) 0.0566(12) Uani 1 1 d . . . . .
H4 H 0.157328 0.311118 0.730893 0.068 Uiso 1 1 calc R . . . .
C5 C 0.1613(6) 0.3913(4) 0.5964(3) 0.0528(11) Uani 1 1 d . . . . .
H5 H 0.109381 0.453502 0.619682 0.063 Uiso 1 1 calc R . . . .
C6 C 0.2084(5) 0.3863(3) 0.4949(3) 0.0432(9) Uani 1 1 d . . . . .
H6 H 0.187890 0.445000 0.450554 0.052 Uiso 1 1 calc R . . . .
C7 C 0.2091(5) 0.4900(3) 0.2231(3) 0.0393(8) Uani 1 1 d . . . . .
C8 C 0.3352(5) 0.5498(3) 0.2460(3) 0.0438(9) Uani 1 1 d . . . . .
C9 C 0.3321(6) 0.6537(3) 0.2078(3) 0.0509(11) Uani 1 1 d . . . . .
H9 H 0.415904 0.694115 0.224072 0.061 Uiso 1 1 calc R . . . .
C10 C 0.2144(7) 0.7000(3) 0.1482(3) 0.0581(13) Uani 1 1 d . . . . .
C11 C 0.0896(6) 0.6403(3) 0.1267(3) 0.0529(11) Uani 1 1 d . . . . .
H11 H 0.007825 0.669958 0.085214 0.063 Uiso 1 1 calc R . . . .
C12 C 0.0827(5) 0.5370(3) 0.1654(3) 0.0425(9) Uani 1 1 d . . . . .
C13 C -0.0584(6) 0.4788(4) 0.1389(3) 0.0562(11) Uani 1 1 d . . . . .
H13A H -0.019856 0.419914 0.099654 0.084 Uiso 1 1 calc GR . . . .
H13B H -0.132168 0.525416 0.099928 0.084 Uiso 1 1 calc GR . . . .
H13C H -0.114056 0.453553 0.200117 0.084 Uiso 1 1 calc GR . . . .
C14 C 0.2182(9) 0.8128(4) 0.1061(5) 0.087(2) Uani 1 1 d . . . . .
H14A H 0.290972 0.815481 0.047052 0.130 Uiso 1 1 calc GR . . . .
H14B H 0.255611 0.855573 0.156655 0.130 Uiso 1 1 calc GR . . . .
H14C H 0.110447 0.839283 0.087665 0.130 Uiso 1 1 calc GR . . . .
C15 C 0.4777(6) 0.5075(3) 0.3054(4) 0.0576(11) Uani 1 1 d . . . . .
H15A H 0.440117 0.480483 0.371143 0.086 Uiso 1 1 calc GR . . . .
H15B H 0.548150 0.563058 0.313269 0.086 Uiso 1 1 calc GR . . . .
H15C H 0.536806 0.451561 0.270065 0.086 Uiso 1 1 calc GR . . . .
C16 C 0.2231(5) 0.2611(3) 0.1516(2) 0.0353(8) Uani 1 1 d . . . . .
C17 C 0.1541(5) 0.1643(3) 0.1596(3) 0.0384(8) Uani 1 1 d . . . . .
C18 C 0.1700(6) 0.0993(3) 0.0785(3) 0.0455(9) Uani 1 1 d . . . . .
H18 H 0.123707 0.034498 0.084180 0.055 Uiso 1 1 calc R . . . .
C19 C 0.2521(6) 0.1285(3) -0.0096(3) 0.0515(11) Uani 1 1 d . . . . .
C20 C 0.3185(6) 0.2248(3) -0.0173(3) 0.0457(9) Uani 1 1 d . . . . .
H20 H 0.373568 0.245257 -0.077582 0.055 Uiso 1 1 calc R . . . .
C21 C 0.3062(5) 0.2929(3) 0.0620(3) 0.0366(8) Uani 1 1 d . . . . .
C22 C 0.3901(5) 0.3931(3) 0.0443(3) 0.0442(9) Uani 1 1 d . . . . .
H22A H 0.464164 0.387545 -0.013905 0.066 Uiso 1 1 calc GR . . . .
H22B H 0.449674 0.404878 0.102972 0.066 Uiso 1 1 calc GR . . . .
H22C H 0.310251 0.451215 0.032464 0.066 Uiso 1 1 calc GR . . . .
C23 C 0.2725(9) 0.0569(4) -0.0978(4) 0.085(2) Uani 1 1 d . . . . .
H23A H 0.236040 0.095240 -0.158500 0.128 Uiso 1 1 calc GR . . . .
H23B H 0.208981 -0.002977 -0.083654 0.128 Uiso 1 1 calc GR . . . .
H23C H 0.385553 0.033006 -0.107323 0.128 Uiso 1 1 calc GR . . . .
C24 C 0.0605(5) 0.1240(3) 0.2527(3) 0.0443(9) Uani 1 1 d . . . . .
H24A H 0.128441 0.120888 0.310223 0.066 Uiso 1 1 calc GR . . . .
H24B H 0.028171 0.054509 0.242294 0.066 Uiso 1 1 calc GR . . . .
H24C H -0.034774 0.170780 0.265056 0.066 Uiso 1 1 calc GR . . . .
C25 C 0.7042(7) 0.2973(4) 0.4568(4) 0.0671(14) Uani 1 1 d . . . . .
H25C H 0.613750 0.349181 0.469452 0.080 Uiso 0.5 1 calc R . P A 2
H25D H 0.784658 0.328329 0.410433 0.080 Uiso 0.5 1 calc R . P A 2
H25A H 0.743301 0.341703 0.399868 0.080 Uiso 0.5 1 calc R . P B 1
H25B H 0.613620 0.336172 0.491084 0.080 Uiso 0.5 1 calc R . P B 1
C26A C 0.8349(18) 0.2709(16) 0.5270(14) 0.062(4) Uani 0.5 1 d . . P C 1
H26A H 0.941348 0.270628 0.492085 0.074 Uiso 0.5 1 calc R . P C 1
H26B H 0.830016 0.319576 0.581179 0.074 Uiso 0.5 1 calc R . P C 1
C26B C 0.776(2) 0.253(2) 0.5522(15) 0.083(6) Uani 0.5 1 d . . P C 2
H26C H 0.692140 0.241792 0.604795 0.100 Uiso 0.5 1 calc R . P C 2
H26D H 0.852293 0.299712 0.576076 0.100 Uiso 0.5 1 calc R . P C 2
C27A C 0.7990(19) 0.1653(13) 0.5653(10) 0.070(3) Uani 0.5 1 d . . P C 1
H27A H 0.713683 0.168614 0.618606 0.084 Uiso 0.5 1 calc R . P C 1
H27B H 0.895597 0.127072 0.592340 0.084 Uiso 0.5 1 calc R . P C 1
C27B C 0.8652(18) 0.1475(12) 0.5246(10) 0.075(4) Uani 0.5 1 d . . P C 2
H27C H 0.963300 0.157113 0.482325 0.090 Uiso 0.5 1 calc R . P C 2
H27D H 0.891662 0.102192 0.584210 0.090 Uiso 0.5 1 calc R . P C 2
C28 C 0.7405(7) 0.1094(4) 0.4701(4) 0.0616(12) Uani 1 1 d . . . . .
H28A H 0.831819 0.082241 0.427669 0.074 Uiso 0.5 1 calc R . P C 1
H28B H 0.670839 0.052944 0.490425 0.074 Uiso 0.5 1 calc R . P C 1
H28C H 0.667885 0.070886 0.516148 0.074 Uiso 0.5 1 calc R . P C 2
H28D H 0.787371 0.061874 0.419847 0.074 Uiso 0.5 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As N 1.884(3) . ?
As C7 1.989(4) . ?
As C16 1.985(3) . ?
Cl1 Al 2.1190(16) . ?
Cl2 Al 2.1411(14) . ?
Al O 1.869(3) . ?
Al N 1.819(3) . ?
O C25 1.479(5) . ?
O C28 1.474(5) . ?
N C1 1.429(4) . ?
C1 C2 1.396(5) . ?
C1 C6 1.405(5) . ?
C2 C3 1.386(5) . ?
C3 C4 1.380(6) . ?
C4 C5 1.369(6) . ?
C5 C6 1.394(5) . ?
C7 C8 1.400(6) . ?
C7 C12 1.407(5) . ?
C8 C9 1.397(5) . ?
C8 C15 1.504(6) . ?
C9 C10 1.367(7) . ?
C10 C11 1.384(7) . ?
C10 C14 1.525(6) . ?
C11 C12 1.398(6) . ?
C12 C13 1.503(6) . ?
C16 C17 1.403(5) . ?
C16 C21 1.406(5) . ?
C17 C18 1.400(5) . ?
C17 C24 1.519(5) . ?
C18 C19 1.378(6) . ?
C19 C20 1.388(6) . ?
C19 C23 1.529(5) . ?
C20 C21 1.405(5) . ?
C21 C22 1.510(5) . ?
C25 C26A 1.473(18) . ?
C25 C26B 1.50(2) . ?
C26A C27A 1.47(2) . ?
C26B C27B 1.54(3) . ?
C27A C28 1.605(14) . ?
C27B C28 1.424(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N As C7 110.56(15) . . ?
N As C16 99.18(13) . . ?
C16 As C7 104.04(14) . . ?
Cl1 Al Cl2 111.07(6) . . ?
O Al Cl1 100.98(11) . . ?
O Al Cl2 100.66(10) . . ?
N Al Cl1 118.45(11) . . ?
N Al Cl2 117.45(12) . . ?
N Al O 104.71(13) . . ?
C25 O Al 122.6(3) . . ?
C28 O Al 128.1(3) . . ?
C28 O C25 108.9(3) . . ?
Al N As 125.87(15) . . ?
C1 N As 110.9(2) . . ?
C1 N Al 120.6(2) . . ?
C2 C1 N 121.4(3) . . ?
C2 C1 C6 117.3(3) . . ?
C6 C1 N 121.3(3) . . ?
C3 C2 C1 121.4(3) . . ?
C4 C3 C2 120.4(4) . . ?
C5 C4 C3 119.4(4) . . ?
C4 C5 C6 121.0(4) . . ?
C5 C6 C1 120.5(4) . . ?
C8 C7 As 128.5(3) . . ?
C8 C7 C12 119.3(3) . . ?
C12 C7 As 112.0(3) . . ?
C7 C8 C15 123.9(3) . . ?
C9 C8 C7 118.1(4) . . ?
C9 C8 C15 118.0(4) . . ?
C10 C9 C8 123.9(4) . . ?
C9 C10 C11 117.5(4) . . ?
C9 C10 C14 122.0(5) . . ?
C11 C10 C14 120.4(5) . . ?
C10 C11 C12 121.4(4) . . ?
C7 C12 C13 122.6(4) . . ?
C11 C12 C7 119.7(4) . . ?
C11 C12 C13 117.7(4) . . ?
C17 C16 As 112.3(3) . . ?
C17 C16 C21 120.1(3) . . ?
C21 C16 As 127.4(3) . . ?
C16 C17 C24 123.9(3) . . ?
C18 C17 C16 119.7(4) . . ?
C18 C17 C24 116.5(3) . . ?
C19 C18 C17 121.2(4) . . ?
C18 C19 C20 118.7(3) . . ?
C18 C19 C23 121.4(4) . . ?
C20 C19 C23 119.8(4) . . ?
C19 C20 C21 122.3(4) . . ?
C16 C21 C22 125.6(3) . . ?
C20 C21 C16 118.0(3) . . ?
C20 C21 C22 116.3(3) . . ?
O C25 C26B 98.6(9) . . ?
C26A C25 O 109.2(9) . . ?
C27A C26A C25 101.7(11) . . ?
C25 C26B C27B 105.0(13) . . ?
C26A C27A C28 105.3(11) . . ?
C28 C27B C26B 97.9(11) . . ?
O C28 C27A 99.2(6) . . ?
C27B C28 O 108.3(7) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_xcd380
_database_code_depnum_ccdc_archive 'CCDC 1949413'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record             
;
2019-08-26 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;
_audit_creation_date             2019-07-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3

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

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H66 As2 Hf N4'
_chemical_formula_sum            'C52 H66 As2 Hf N4'
_chemical_formula_weight         1075.41
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3307(4)
_cell_length_b                   13.5735(6)
_cell_length_c                   19.6583(9)
_cell_angle_alpha                95.723(3)
_cell_angle_beta                 96.008(4)
_cell_angle_gamma                103.085(4)
_cell_volume                     2392.11(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    31157
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      1.55
_shelx_estimated_absorpt_T_max   0.561
_shelx_estimated_absorpt_T_min   0.302
_exptl_absorpt_coefficient_mu    3.592
_exptl_absorpt_correction_T_max  0.5798
_exptl_absorpt_correction_T_min  0.3701
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.182
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26320
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.517
_diffrn_reflns_theta_min         1.760
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
 227 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10830
_reflns_number_total             13191
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_refine_diff_density_max         1.919
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         13191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0431P)²+0.9612P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0789
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C18(H18), C20(H20),
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C35(H35), C42(H42),
  C44(H44)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Hf Hf 0.42897(2) 0.27673(2) 0.13991(2) 0.02010(4) Uani 1 1 d . . . . .
As1 As 0.29908(3) 0.12821(2) 0.25583(2) 0.01975(6) Uani 1 1 d . . . . .
As2 As 0.44437(3) 0.39391(2) 0.28454(2) 0.02110(6) Uani 1 1 d . . . . .
N1 N 0.3975(3) 0.13697(17) 0.17686(12) 0.0214(5) Uani 1 1 d . . . . .
N2 N 0.3622(3) 0.39461(18) 0.19371(12) 0.0214(5) Uani 1 1 d . . . . .
N3 N 0.2997(4) 0.2541(2) 0.04750(14) 0.0342(6) Uani 1 1 d . . . . .
N4 N 0.6368(3) 0.3354(2) 0.11715(15) 0.0311(6) Uani 1 1 d . . . . .
C1 C 0.4072(3) 0.0501(2) 0.13143(14) 0.0219(6) Uani 1 1 d . . . . .
C2 C 0.2804(4) -0.0173(2) 0.09488(16) 0.0282(6) Uani 1 1 d . . . . .
H2 H 0.185389 -0.005693 0.100353 0.034 Uiso 1 1 calc R . . . .
C3 C 0.2914(4) -0.1011(2) 0.05059(17) 0.0339(8) Uani 1 1 d . . . . .
H3 H 0.203850 -0.146210 0.026354 0.041 Uiso 1 1 calc R . . . .
C4 C 0.4281(5) -0.1192(3) 0.04158(18) 0.0379(9) Uani 1 1 d . . . . .
H4 H 0.435248 -0.177481 0.012254 0.045 Uiso 1 1 calc R . . . .
C5 C 0.5535(4) -0.0522(3) 0.07545(18) 0.0367(8) Uani 1 1 d . . . . .
H5 H 0.648194 -0.063131 0.068428 0.044 Uiso 1 1 calc R . . . .
C6 C 0.5441(4) 0.0316(3) 0.11995(16) 0.0280(6) Uani 1 1 d . . . . .
H6 H 0.632612 0.077071 0.142945 0.034 Uiso 1 1 calc R . . . .
C7 C 0.1822(3) -0.0153(2) 0.23784(15) 0.0227(6) Uani 1 1 d . . . . .
C8 C 0.0308(4) -0.0292(2) 0.21599(17) 0.0291(7) Uani 1 1 d . . . . .
C9 C -0.0586(4) -0.1274(3) 0.19776(18) 0.0359(8) Uani 1 1 d . . . . .
H9 H -0.161242 -0.136289 0.182441 0.043 Uiso 1 1 calc R . . . .
C10 C -0.0005(4) -0.2129(3) 0.20156(17) 0.0337(8) Uani 1 1 d . . . . .
C11 C 0.1484(4) -0.1977(2) 0.22531(16) 0.0305(7) Uani 1 1 d . . . . .
H11 H 0.188279 -0.255610 0.229513 0.037 Uiso 1 1 calc R . . . .
C12 C 0.2426(4) -0.1009(2) 0.24337(15) 0.0242(6) Uani 1 1 d . . . . .
C13 C 0.4051(4) -0.0942(2) 0.26413(18) 0.0313(7) Uani 1 1 d . . . . .
H13A H 0.464361 -0.050033 0.235640 0.047 Uiso 1 1 calc GR . . . .
H13B H 0.423792 -0.162507 0.257467 0.047 Uiso 1 1 calc GR . . . .
H13C H 0.432873 -0.065722 0.312787 0.047 Uiso 1 1 calc GR . . . .
C14 C -0.0971(5) -0.3184(3) 0.1772(2) 0.0449(10) Uani 1 1 d . . . . .
H14A H -0.200205 -0.319496 0.183607 0.067 Uiso 1 1 calc GR . . . .
H14B H -0.062643 -0.367753 0.203883 0.067 Uiso 1 1 calc GR . . . .
H14C H -0.091283 -0.336457 0.128176 0.067 Uiso 1 1 calc GR . . . .
C15 C -0.0405(4) 0.0593(3) 0.2091(2) 0.0485(11) Uani 1 1 d . . . . .
H15A H -0.018902 0.104569 0.252915 0.073 Uiso 1 1 calc GR . . . .
H15B H -0.148192 0.033598 0.197452 0.073 Uiso 1 1 calc GR . . . .
H15C H -0.000855 0.097240 0.172631 0.073 Uiso 1 1 calc GR . . . .
C16 C 0.4357(3) 0.1260(2) 0.33975(14) 0.0210(5) Uani 1 1 d . . . . .
C17 C 0.5919(4) 0.1439(2) 0.34788(16) 0.0253(6) Uani 1 1 d . . . . .
C18 C 0.6704(4) 0.1472(2) 0.41273(16) 0.0284(7) Uani 1 1 d . . . . .
H18 H 0.775309 0.157928 0.416963 0.034 Uiso 1 1 calc R . . . .
C19 C 0.6007(4) 0.1352(2) 0.47111(16) 0.0303(7) Uani 1 1 d . . . . .
C20 C 0.4473(4) 0.1204(2) 0.46329(16) 0.0296(7) Uani 1 1 d . . . . .
H20 H 0.397610 0.113189 0.502942 0.036 Uiso 1 1 calc R . . . .
C21 C 0.3634(4) 0.1156(2) 0.39944(16) 0.0246(6) Uani 1 1 d . . . . .
C22 C 0.1981(4) 0.0998(3) 0.39644(18) 0.0318(7) Uani 1 1 d . . . . .
H22A H 0.149092 0.032545 0.371245 0.048 Uiso 1 1 calc GR . . . .
H22B H 0.165880 0.152744 0.372733 0.048 Uiso 1 1 calc GR . . . .
H22C H 0.171536 0.103680 0.443397 0.048 Uiso 1 1 calc GR . . . .
C23 C 0.6890(5) 0.1404(3) 0.54096(18) 0.0399(8) Uani 1 1 d . . . . .
H23A H 0.719696 0.211359 0.562723 0.060 Uiso 1 1 calc GR . . . .
H23B H 0.777099 0.114048 0.535291 0.060 Uiso 1 1 calc GR . . . .
H23C H 0.627401 0.099100 0.570136 0.060 Uiso 1 1 calc GR . . . .
C24 C 0.6801(4) 0.1594(3) 0.28840(17) 0.0353(8) Uani 1 1 d . . . . .
H24A H 0.648913 0.098886 0.253820 0.053 Uiso 1 1 calc GR . . . .
H24B H 0.785925 0.170292 0.304995 0.053 Uiso 1 1 calc GR . . . .
H24C H 0.662914 0.219103 0.267620 0.053 Uiso 1 1 calc GR . . . .
C25 C 0.3126(4) 0.4730(2) 0.16275(15) 0.0243(6) Uani 1 1 d . . . . .
C26 C 0.1741(4) 0.4497(3) 0.12242(16) 0.0290(7) Uani 1 1 d . . . . .
H26 H 0.112222 0.382846 0.118393 0.035 Uiso 1 1 calc R . . . .
C27 C 0.1256(5) 0.5235(3) 0.08799(18) 0.0391(8) Uani 1 1 d . . . . .
H27 H 0.030589 0.506640 0.061125 0.047 Uiso 1 1 calc R . . . .
C28 C 0.2136(5) 0.6203(3) 0.09252(19) 0.0430(9) Uani 1 1 d . . . . .
H28 H 0.179321 0.670479 0.069399 0.052 Uiso 1 1 calc R . . . .
C29 C 0.3526(5) 0.6443(3) 0.13101(18) 0.0380(9) Uani 1 1 d . . . . .
H29 H 0.414306 0.711084 0.133761 0.046 Uiso 1 1 calc R . . . .
C30 C 0.4027(4) 0.5718(2) 0.16562(16) 0.0294(7) Uani 1 1 d . . . . .
H30 H 0.498775 0.589094 0.191469 0.035 Uiso 1 1 calc R . . . .
C31 C 0.5486(3) 0.5378(2) 0.31560(15) 0.0231(6) Uani 1 1 d . . . . .
C32 C 0.4785(4) 0.6162(2) 0.33520(16) 0.0248(6) Uani 1 1 d . . . . .
C33 C 0.5661(4) 0.7154(2) 0.35412(16) 0.0309(7) Uani 1 1 d . . . . .
H33 H 0.518972 0.768016 0.367666 0.037 Uiso 1 1 calc R . . . .
C34 C 0.7175(4) 0.7401(2) 0.35397(16) 0.0334(8) Uani 1 1 d . . . . .
C35 C 0.7843(4) 0.6625(3) 0.33484(17) 0.0337(7) Uani 1 1 d . . . . .
H35 H 0.888696 0.678095 0.334465 0.040 Uiso 1 1 calc R . . . .
C36 C 0.7033(4) 0.5617(2) 0.31603(16) 0.0282(6) Uani 1 1 d . . . . .
C37 C 0.7863(4) 0.4813(3) 0.2979(2) 0.0379(8) Uani 1 1 d . . . . .
H37A H 0.764809 0.427478 0.327678 0.057 Uiso 1 1 calc GR . . . .
H37B H 0.893139 0.512314 0.304531 0.057 Uiso 1 1 calc GR . . . .
H37C H 0.754723 0.451794 0.249558 0.057 Uiso 1 1 calc GR . . . .
C38 C 0.8076(5) 0.8485(3) 0.3733(2) 0.0501(11) Uani 1 1 d . . . . .
H38A H 0.744673 0.895623 0.363741 0.075 Uiso 1 1 calc GR . . . .
H38B H 0.890897 0.860776 0.346271 0.075 Uiso 1 1 calc GR . . . .
H38C H 0.845743 0.859491 0.422559 0.075 Uiso 1 1 calc GR . . . .
C39 C 0.3126(4) 0.5998(2) 0.33459(18) 0.0323(7) Uani 1 1 d . . . . .
H39A H 0.261477 0.554799 0.292844 0.048 Uiso 1 1 calc GR . . . .
H39B H 0.285601 0.665560 0.335162 0.048 Uiso 1 1 calc GR . . . .
H39C H 0.283204 0.568437 0.375363 0.048 Uiso 1 1 calc GR . . . .
C40 C 0.2931(4) 0.3740(2) 0.34902(15) 0.0231(6) Uani 1 1 d . . . . .
C41 C 0.3538(4) 0.3764(2) 0.41816(15) 0.0234(6) Uani 1 1 d . . . . .
C42 C 0.2599(4) 0.3684(2) 0.46871(16) 0.0290(7) Uani 1 1 d . . . . .
H42 H 0.300872 0.370405 0.515289 0.035 Uiso 1 1 calc R . . . .
C43 C 0.1080(4) 0.3575(3) 0.45341(17) 0.0310(7) Uani 1 1 d . . . . .
C44 C 0.0503(4) 0.3483(2) 0.38451(16) 0.0278(6) Uani 1 1 d . . . . .
H44 H -0.054080 0.336658 0.372705 0.033 Uiso 1 1 calc R . . . .
C45 C 0.1397(4) 0.3557(2) 0.33225(15) 0.0235(6) Uani 1 1 d . . . . .
C46 C 0.0634(4) 0.3456(3) 0.25920(16) 0.0281(6) Uani 1 1 d . . . . .
H46A H 0.074443 0.413432 0.244304 0.042 Uiso 1 1 calc GR . . . .
H46B H -0.042269 0.313258 0.257500 0.042 Uiso 1 1 calc GR . . . .
H46C H 0.108639 0.303688 0.228485 0.042 Uiso 1 1 calc GR . . . .
C47 C 0.0083(5) 0.3556(3) 0.50909(19) 0.0446(9) Uani 1 1 d . . . . .
H47A H 0.009606 0.296017 0.533233 0.067 Uiso 1 1 calc GR . . . .
H47B H -0.093257 0.351831 0.488286 0.067 Uiso 1 1 calc GR . . . .
H47C H 0.043750 0.417897 0.541945 0.067 Uiso 1 1 calc GR . . . .
C48 C 0.5170(4) 0.3868(2) 0.44007(17) 0.0284(7) Uani 1 1 d . . . . .
H48A H 0.572970 0.454550 0.433107 0.043 Uiso 1 1 calc GR . . . .
H48B H 0.550902 0.334517 0.412378 0.043 Uiso 1 1 calc GR . . . .
H48C H 0.533015 0.377989 0.488935 0.043 Uiso 1 1 calc GR . . . .
C49 C 0.1494(5) 0.1952(3) 0.0372(2) 0.0554(12) Uani 1 1 d . . . . .
H49A H 0.124978 0.167552 0.079898 0.083 Uiso 1 1 calc GR . . . .
H49B H 0.137479 0.139026 0.000115 0.083 Uiso 1 1 calc GR . . . .
H49C H 0.082747 0.238772 0.024663 0.083 Uiso 1 1 calc GR . . . .
C50 C 0.3323(6) 0.3040(4) -0.0127(2) 0.0585(13) Uani 1 1 d . . . . .
H50A H 0.263945 0.347952 -0.021208 0.088 Uiso 1 1 calc GR . . . .
H50B H 0.320439 0.252460 -0.052807 0.088 Uiso 1 1 calc GR . . . .
H50C H 0.434642 0.345436 -0.004827 0.088 Uiso 1 1 calc GR . . . .
C51 C 0.6586(6) 0.4372(3) 0.0952(3) 0.0557(12) Uani 1 1 d . . . . .
H51A H 0.565174 0.458904 0.093735 0.084 Uiso 1 1 calc GR . . . .
H51B H 0.690219 0.435201 0.049144 0.084 Uiso 1 1 calc GR . . . .
H51C H 0.734981 0.485545 0.127870 0.084 Uiso 1 1 calc GR . . . .
C52 C 0.7650(4) 0.2979(3) 0.1121(2) 0.0431(9) Uani 1 1 d . . . . .
H52A H 0.848133 0.341613 0.143888 0.065 Uiso 1 1 calc GR . . . .
H52B H 0.789219 0.297895 0.064797 0.065 Uiso 1 1 calc GR . . . .
H52C H 0.746612 0.228207 0.124149 0.065 Uiso 1 1 calc GR . . . .


_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
Hf As2 3.0892(3) . ?
Hf N1 2.069(2) . ?
Hf N2 2.078(2) . ?
Hf N3 2.028(3) . ?
Hf N4 2.037(3) . ?
As1 N1 1.885(2) . ?
As1 C7 1.982(3) . ?
As1 C16 1.984(3) . ?
As2 N2 1.870(2) . ?
As2 C31 1.978(3) . ?
As2 C40 1.986(3) . ?
N1 C1 1.432(4) . ?
N2 C25 1.418(4) . ?
N3 C49 1.431(5) . ?
N3 C50 1.447(5) . ?
N4 C51 1.466(5) . ?
N4 C52 1.410(5) . ?
C1 C2 1.397(4) . ?
C1 C6 1.393(4) . ?
C2 C3 1.392(4) . ?
C3 C4 1.379(5) . ?
C4 C5 1.369(6) . ?
C5 C6 1.389(5) . ?
C7 C8 1.398(4) . ?
C7 C12 1.410(4) . ?
C8 C9 1.393(5) . ?
C8 C15 1.510(5) . ?
C9 C10 1.392(5) . ?
C10 C11 1.381(5) . ?
C10 C14 1.511(5) . ?
C11 C12 1.394(4) . ?
C12 C13 1.508(5) . ?
C16 C17 1.411(4) . ?
C16 C21 1.417(4) . ?
C17 C18 1.394(4) . ?
C17 C24 1.504(4) . ?
C18 C19 1.383(5) . ?
C19 C20 1.389(5) . ?
C19 C23 1.512(5) . ?
C20 C21 1.396(5) . ?
C21 C22 1.502(5) . ?
C25 C26 1.396(5) . ?
C25 C30 1.405(4) . ?
C26 C27 1.394(5) . ?
C27 C28 1.371(6) . ?
C28 C29 1.384(6) . ?
C29 C30 1.388(5) . ?
C31 C32 1.412(4) . ?
C31 C36 1.405(5) . ?
C32 C33 1.398(4) . ?
C32 C39 1.512(5) . ?
C33 C34 1.377(5) . ?
C34 C35 1.381(5) . ?
C34 C38 1.509(5) . ?
C35 C36 1.397(5) . ?
C36 C37 1.510(5) . ?
C40 C41 1.411(4) . ?
C40 C45 1.394(4) . ?
C41 C42 1.388(4) . ?
C41 C48 1.509(4) . ?
C42 C43 1.388(5) . ?
C43 C44 1.387(5) . ?
C43 C47 1.507(5) . ?
C44 C45 1.387(4) . ?
C45 C46 1.513(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Hf As2 92.94(7) . . ?
N1 Hf N2 118.94(9) . . ?
N2 Hf As2 36.17(7) . . ?
N3 Hf As2 137.53(8) . . ?
N3 Hf N1 106.72(11) . . ?
N3 Hf N2 102.74(11) . . ?
N3 Hf N4 103.67(12) . . ?
N4 Hf As2 100.78(8) . . ?
N4 Hf N1 115.64(11) . . ?
N4 Hf N2 107.24(10) . . ?
N1 As1 C7 100.64(11) . . ?
N1 As1 C16 111.95(12) . . ?
C7 As1 C16 101.81(12) . . ?
N2 As2 C31 104.12(11) . . ?
N2 As2 C40 112.79(12) . . ?
C31 As2 Hf 126.33(9) . . ?
C31 As2 C40 100.44(12) . . ?
C40 As2 Hf 127.87(9) . . ?
As1 N1 Hf 114.88(11) . . ?
C1 N1 Hf 118.28(18) . . ?
C1 N1 As1 123.77(19) . . ?
As2 N2 Hf 102.84(11) . . ?
C25 N2 Hf 124.31(19) . . ?
C25 N2 As2 129.68(19) . . ?
C49 N3 Hf 122.2(3) . . ?
C49 N3 C50 110.0(4) . . ?
C50 N3 Hf 127.2(3) . . ?
C51 N4 Hf 114.5(3) . . ?
C52 N4 Hf 134.9(2) . . ?
C52 N4 C51 110.4(3) . . ?
C2 C1 N1 121.5(3) . . ?
C6 C1 N1 121.1(3) . . ?
C6 C1 C2 117.3(3) . . ?
C3 C2 C1 121.0(3) . . ?
C4 C3 C2 120.6(3) . . ?
C5 C4 C3 119.1(3) . . ?
C4 C5 C6 120.9(3) . . ?
C5 C6 C1 121.1(3) . . ?
C8 C7 As1 115.6(2) . . ?
C8 C7 C12 119.8(3) . . ?
C12 C7 As1 124.6(2) . . ?
C7 C8 C15 122.3(3) . . ?
C9 C8 C7 119.8(3) . . ?
C9 C8 C15 117.9(3) . . ?
C10 C9 C8 121.3(3) . . ?
C9 C10 C14 120.4(4) . . ?
C11 C10 C9 118.0(3) . . ?
C11 C10 C14 121.5(3) . . ?
C10 C11 C12 122.8(3) . . ?
C7 C12 C13 123.9(3) . . ?
C11 C12 C7 118.3(3) . . ?
C11 C12 C13 117.7(3) . . ?
C17 C16 As1 128.5(2) . . ?
C17 C16 C21 118.1(3) . . ?
C21 C16 As1 113.1(2) . . ?
C16 C17 C24 122.5(3) . . ?
C18 C17 C16 120.2(3) . . ?
C18 C17 C24 117.4(3) . . ?
C19 C18 C17 122.2(3) . . ?
C18 C19 C20 117.5(3) . . ?
C18 C19 C23 121.0(3) . . ?
C20 C19 C23 121.5(3) . . ?
C19 C20 C21 122.6(3) . . ?
C16 C21 C22 122.0(3) . . ?
C20 C21 C16 119.5(3) . . ?
C20 C21 C22 118.5(3) . . ?
C26 C25 N2 119.2(3) . . ?
C26 C25 C30 117.9(3) . . ?
C30 C25 N2 122.6(3) . . ?
C27 C26 C25 120.7(3) . . ?
C28 C27 C26 120.6(4) . . ?
C27 C28 C29 119.5(3) . . ?
C28 C29 C30 120.6(4) . . ?
C29 C30 C25 120.6(4) . . ?
C32 C31 As2 124.8(2) . . ?
C36 C31 As2 116.0(2) . . ?
C36 C31 C32 119.2(3) . . ?
C31 C32 C39 123.6(3) . . ?
C33 C32 C31 118.6(3) . . ?
C33 C32 C39 117.8(3) . . ?
C34 C33 C32 122.8(3) . . ?
C33 C34 C35 117.8(3) . . ?
C33 C34 C38 121.2(3) . . ?
C35 C34 C38 121.0(4) . . ?
C34 C35 C36 122.2(3) . . ?
C31 C36 C37 122.1(3) . . ?
C35 C36 C31 119.4(3) . . ?
C35 C36 C37 118.5(3) . . ?
C41 C40 As2 113.5(2) . . ?
C45 C40 As2 127.0(2) . . ?
C45 C40 C41 119.4(3) . . ?
C40 C41 C48 123.0(3) . . ?
C42 C41 C40 119.0(3) . . ?
C42 C41 C48 118.0(3) . . ?
C43 C42 C41 122.1(3) . . ?
C42 C43 C47 121.8(3) . . ?
C44 C43 C42 117.5(3) . . ?
C44 C43 C47 120.7(3) . . ?
C43 C44 C45 122.2(3) . . ?
C40 C45 C46 123.4(3) . . ?
C44 C45 C40 119.4(3) . . ?
C44 C45 C46 117.2(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_xcd170-1t
_database_code_depnum_ccdc_archive 'CCDC 1949417'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record             
;
2019-08-26 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;
_audit_creation_date             2019-03-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
# start Validation Reply Form
_vrf_PLAT973_xcd170-1t           
;
PROBLEM: Check Calcd Positive Resid. Density on        Pb       1.94 eA-3  
RESPONSE: Probable a fourier truncation error. No obvious signs for twinning
          could be detected for the measured crystal, but others of the same
          batch were twinned. 
;

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

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C48 H54 As2 N2 Pb), C7 H8'
_chemical_formula_sum            'C103 H116 As4 N4 Pb2'
_chemical_formula_weight         2124.05
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   23.7152(8)
_cell_length_b                   23.7152(8)
_cell_length_c                   31.4568(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17691.6(14)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    28328
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.12
_cell_measurement_theta_min      2.43
_shelx_estimated_absorpt_T_max   0.811
_shelx_estimated_absorpt_T_min   0.232
_exptl_absorpt_coefficient_mu    5.337
_exptl_absorpt_correction_T_max  0.1507
_exptl_absorpt_correction_T_min  0.0586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens published in F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different 
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol.9, no.2, 2016, pp. 136-140. 
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             8464
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.041
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.815
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            26155
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.020
_diffrn_reflns_theta_min         2.429
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7840
_reflns_number_total             11522
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_refine_diff_density_max         1.556
_refine_diff_density_min         -2.362
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         11522
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0582
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0864P)²+69.3220P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1620
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C35(H35),
  C42(H42), C44(H44)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Pb Pb 0.76683(2) 0.51198(2) 0.69147(2) 0.02443(9) Uani 1 1 d . . . . .
As1 As 0.66784(3) 0.61374(3) 0.66786(2) 0.02243(16) Uani 1 1 d . . . . .
As2 As 0.74642(3) 0.37060(3) 0.72675(2) 0.02362(16) Uani 1 1 d . . . . .
N1 N 0.6917(2) 0.5407(2) 0.6543(2) 0.0258(13) Uani 1 1 d . . . . .
N2 N 0.7239(3) 0.4462(3) 0.7293(2) 0.0288(13) Uani 1 1 d . . . . .
C1 C 0.6504(3) 0.6550(3) 0.6143(2) 0.0233(14) Uani 1 1 d . . . . .
C2 C 0.6496(3) 0.6343(3) 0.5723(2) 0.0254(15) Uani 1 1 d . . . . .
C3 C 0.6343(3) 0.6712(3) 0.5398(2) 0.0218(13) Uani 1 1 d . . . . .
H3 H 0.635719 0.657797 0.511354 0.026 Uiso 1 1 calc R . . . .
C4 C 0.6173(3) 0.7261(3) 0.5466(2) 0.0256(15) Uani 1 1 d . . . . .
C5 C 0.6175(3) 0.7455(3) 0.5884(2) 0.0292(16) Uani 1 1 d . . . . .
H5 H 0.606037 0.783112 0.594262 0.035 Uiso 1 1 calc R . . . .
C6 C 0.6342(3) 0.7107(3) 0.6216(2) 0.0214(13) Uani 1 1 d . . . . .
C7 C 0.6350(3) 0.7378(3) 0.6655(2) 0.0289(16) Uani 1 1 d . . . . .
H7A H 0.610694 0.716264 0.684715 0.043 Uiso 1 1 calc GR . . . .
H7B H 0.621089 0.776649 0.663402 0.043 Uiso 1 1 calc GR . . . .
H7C H 0.673630 0.738015 0.676470 0.043 Uiso 1 1 calc GR . . . .
C8 C 0.5992(4) 0.7646(3) 0.5118(2) 0.0320(17) Uani 1 1 d . . . . .
H8A H 0.617952 0.753746 0.485297 0.048 Uiso 1 1 calc GR . . . .
H8B H 0.609480 0.803494 0.519072 0.048 Uiso 1 1 calc GR . . . .
H8C H 0.558248 0.762022 0.508171 0.048 Uiso 1 1 calc GR . . . .
C9 C 0.6633(3) 0.5747(3) 0.5602(2) 0.0318(17) Uani 1 1 d . . . . .
H9A H 0.631196 0.550319 0.566929 0.048 Uiso 1 1 calc GR . . . .
H9B H 0.696516 0.562102 0.576106 0.048 Uiso 1 1 calc GR . . . .
H9C H 0.671202 0.572861 0.529650 0.048 Uiso 1 1 calc GR . . . .
C10 C 0.7436(3) 0.6453(3) 0.6810(2) 0.0237(14) Uani 1 1 d . . . . .
C11 C 0.7520(3) 0.6659(3) 0.7223(2) 0.0232(14) Uani 1 1 d . . . . .
C12 C 0.8026(3) 0.6921(3) 0.7325(2) 0.0223(14) Uani 1 1 d . . . . .
H12 H 0.807426 0.706167 0.760498 0.027 Uiso 1 1 calc R . . . .
C13 C 0.8459(3) 0.6985(3) 0.7040(2) 0.0261(15) Uani 1 1 d . . . . .
C14 C 0.8376(3) 0.6768(3) 0.6634(2) 0.0266(15) Uani 1 1 d . . . . .
H14 H 0.867137 0.679835 0.643184 0.032 Uiso 1 1 calc R . . . .
C15 C 0.7878(3) 0.6508(3) 0.6515(2) 0.0241(14) Uani 1 1 d . . . . .
C16 C 0.7833(3) 0.6319(3) 0.6060(2) 0.0270(15) Uani 1 1 d . . . . .
H16A H 0.766161 0.594368 0.604904 0.041 Uiso 1 1 calc GR . . . .
H16B H 0.821002 0.630557 0.593310 0.041 Uiso 1 1 calc GR . . . .
H16C H 0.759781 0.658629 0.590140 0.041 Uiso 1 1 calc GR . . . .
C17 C 0.8996(3) 0.7297(3) 0.7152(2) 0.0297(16) Uani 1 1 d . . . . .
H17A H 0.895134 0.769834 0.708428 0.045 Uiso 1 1 calc GR . . . .
H17B H 0.931068 0.714154 0.698827 0.045 Uiso 1 1 calc GR . . . .
H17C H 0.907243 0.725463 0.745655 0.045 Uiso 1 1 calc GR . . . .
C18 C 0.7075(3) 0.6604(3) 0.7565(2) 0.0255(15) Uani 1 1 d . . . . .
H18A H 0.670400 0.669164 0.744495 0.038 Uiso 1 1 calc GR . . . .
H18B H 0.715872 0.686660 0.779694 0.038 Uiso 1 1 calc GR . . . .
H18C H 0.707443 0.621701 0.767471 0.038 Uiso 1 1 calc GR . . . .
C19 C 0.6494(3) 0.5012(3) 0.6450(2) 0.0256(15) Uani 1 1 d . . . . .
C20 C 0.5921(3) 0.5105(3) 0.6494(2) 0.0309(16) Uani 1 1 d . . . . .
H20 H 0.579622 0.545509 0.660580 0.037 Uiso 1 1 calc R . . . .
C21 C 0.5524(3) 0.4705(3) 0.6380(3) 0.0343(18) Uani 1 1 d . . . . .
H21 H 0.513365 0.478708 0.641023 0.041 Uiso 1 1 calc R . . . .
C22 C 0.5690(3) 0.4193(3) 0.6224(2) 0.0327(17) Uani 1 1 d . . . . .
H22 H 0.541886 0.391312 0.615409 0.039 Uiso 1 1 calc R . . . .
C23 C 0.6262(3) 0.4088(3) 0.6171(3) 0.0340(17) Uani 1 1 d . . . . .
H23 H 0.638061 0.373708 0.605643 0.041 Uiso 1 1 calc R . . . .
C24 C 0.6662(3) 0.4486(3) 0.6281(2) 0.0250(14) Uani 1 1 d . . . . .
H24 H 0.705101 0.440634 0.624328 0.030 Uiso 1 1 calc R . . . .
C25 C 0.6666(3) 0.4564(3) 0.7399(2) 0.0288(16) Uani 1 1 d . . . . .
C26 C 0.6539(3) 0.5084(3) 0.7587(2) 0.0316(17) Uani 1 1 d . . . . .
H26 H 0.683634 0.533816 0.765046 0.038 Uiso 1 1 calc R . . . .
C27 C 0.5990(4) 0.5236(4) 0.7682(3) 0.041(2) Uani 1 1 d . . . . .
H27 H 0.591438 0.559798 0.779707 0.049 Uiso 1 1 calc R . . . .
C28 C 0.5549(4) 0.4863(4) 0.7610(3) 0.042(2) Uani 1 1 d . . . . .
H28 H 0.517102 0.496707 0.767217 0.050 Uiso 1 1 calc R . . . .
C29 C 0.5675(3) 0.4332(4) 0.7445(3) 0.040(2) Uani 1 1 d . . . . .
H29 H 0.537928 0.406705 0.740298 0.048 Uiso 1 1 calc R . . . .
C30 C 0.6222(3) 0.4184(4) 0.7342(3) 0.0341(18) Uani 1 1 d . . . . .
H30 H 0.629758 0.381877 0.723041 0.041 Uiso 1 1 calc R . . . .
C31 C 0.8131(3) 0.3836(3) 0.6906(2) 0.0241(14) Uani 1 1 d . . . . .
C32 C 0.8110(3) 0.3584(3) 0.6504(2) 0.0268(15) Uani 1 1 d . . . . .
C33 C 0.8572(3) 0.3625(3) 0.6236(3) 0.0315(16) Uani 1 1 d . . . . .
H33 H 0.854943 0.346553 0.595930 0.038 Uiso 1 1 calc R . . . .
C34 C 0.9068(3) 0.3892(3) 0.6361(3) 0.0347(18) Uani 1 1 d . . . . .
C35 C 0.9081(3) 0.4139(3) 0.6752(3) 0.0306(16) Uani 1 1 d . . . . .
H35 H 0.940902 0.433976 0.683544 0.037 Uiso 1 1 calc R . . . .
C36 C 0.8631(3) 0.4105(3) 0.7030(2) 0.0258(15) Uani 1 1 d . . . . .
C37 C 0.8713(3) 0.4370(3) 0.7465(2) 0.0327(17) Uani 1 1 d . . . . .
H37A H 0.834408 0.444591 0.759331 0.049 Uiso 1 1 calc GR . . . .
H37B H 0.892205 0.472414 0.743534 0.049 Uiso 1 1 calc GR . . . .
H37C H 0.892535 0.411071 0.764732 0.049 Uiso 1 1 calc GR . . . .
C38 C 0.9557(4) 0.3936(4) 0.6049(3) 0.043(2) Uani 1 1 d . . . . .
H38A H 0.950803 0.365739 0.582196 0.065 Uiso 1 1 calc GR . . . .
H38B H 0.991221 0.386406 0.619838 0.065 Uiso 1 1 calc GR . . . .
H38C H 0.956514 0.431561 0.592550 0.065 Uiso 1 1 calc GR . . . .
C39 C 0.7600(3) 0.3266(3) 0.6346(2) 0.0307(16) Uani 1 1 d . . . . .
H39A H 0.758031 0.289806 0.648626 0.046 Uiso 1 1 calc GR . . . .
H39B H 0.762966 0.321280 0.603779 0.046 Uiso 1 1 calc GR . . . .
H39C H 0.725793 0.348232 0.641060 0.046 Uiso 1 1 calc GR . . . .
C40 C 0.7831(3) 0.3503(3) 0.7814(2) 0.0266(15) Uani 1 1 d . . . . .
C41 C 0.7703(3) 0.3751(3) 0.8209(2) 0.0299(16) Uani 1 1 d . . . . .
C42 C 0.7925(3) 0.3505(3) 0.8575(2) 0.0320(17) Uani 1 1 d . . . . .
H42 H 0.785096 0.368156 0.884004 0.038 Uiso 1 1 calc R . . . .
C43 C 0.8243(3) 0.3020(3) 0.8574(3) 0.0327(17) Uani 1 1 d . . . . .
C44 C 0.8358(3) 0.2775(3) 0.8184(2) 0.0307(16) Uani 1 1 d . . . . .
H44 H 0.858066 0.244241 0.817289 0.037 Uiso 1 1 calc R . . . .
C45 C 0.8156(3) 0.3005(3) 0.7812(3) 0.0311(17) Uani 1 1 d . . . . .
C46 C 0.8279(4) 0.2690(3) 0.7405(3) 0.0338(17) Uani 1 1 d . . . . .
H46A H 0.856415 0.289445 0.724157 0.051 Uiso 1 1 calc GR . . . .
H46B H 0.793224 0.265773 0.723728 0.051 Uiso 1 1 calc GR . . . .
H46C H 0.841935 0.231172 0.747374 0.051 Uiso 1 1 calc GR . . . .
C47 C 0.8456(4) 0.2764(4) 0.8981(3) 0.0376(19) Uani 1 1 d . . . . .
H47A H 0.844448 0.304701 0.920747 0.056 Uiso 1 1 calc GR . . . .
H47B H 0.884561 0.263540 0.894089 0.056 Uiso 1 1 calc GR . . . .
H47C H 0.821807 0.244271 0.905872 0.056 Uiso 1 1 calc GR . . . .
C48 C 0.7355(3) 0.4276(3) 0.8248(2) 0.0325(17) Uani 1 1 d . . . . .
H48A H 0.731209 0.437419 0.854841 0.049 Uiso 1 1 calc GR . . . .
H48B H 0.698225 0.421070 0.812204 0.049 Uiso 1 1 calc GR . . . .
H48C H 0.754226 0.458581 0.809757 0.049 Uiso 1 1 calc GR . . . .


_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
Pb N1 2.236(6) . ?
Pb N2 2.211(6) . ?
As1 N1 1.872(6) . ?
As1 C1 1.994(7) . ?
As1 C10 1.989(7) . ?
As2 N2 1.873(6) . ?
As2 C31 1.972(7) . ?
As2 C40 1.986(7) . ?
N1 C19 1.403(9) . ?
N2 C25 1.420(9) . ?
C1 C2 1.409(10) . ?
C1 C6 1.393(9) . ?
C2 C3 1.393(10) . ?
C2 C9 1.498(10) . ?
C3 C4 1.381(10) . ?
C4 C5 1.391(10) . ?
C4 C8 1.489(10) . ?
C5 C6 1.389(10) . ?
C6 C7 1.523(9) . ?
C10 C11 1.402(9) . ?
C10 C15 1.407(10) . ?
C11 C12 1.389(9) . ?
C11 C18 1.512(10) . ?
C12 C13 1.373(10) . ?
C13 C14 1.391(10) . ?
C13 C17 1.513(10) . ?
C14 C15 1.384(10) . ?
C15 C16 1.502(10) . ?
C19 C20 1.383(10) . ?
C19 C24 1.411(10) . ?
C20 C21 1.383(10) . ?
C21 C22 1.368(11) . ?
C22 C23 1.389(11) . ?
C23 C24 1.382(10) . ?
C25 C26 1.401(11) . ?
C25 C30 1.396(10) . ?
C26 C27 1.383(11) . ?
C27 C28 1.387(13) . ?
C28 C29 1.395(13) . ?
C29 C30 1.384(11) . ?
C31 C32 1.397(10) . ?
C31 C36 1.404(10) . ?
C32 C33 1.387(10) . ?
C32 C39 1.510(10) . ?
C33 C34 1.394(11) . ?
C34 C35 1.361(11) . ?
C34 C38 1.522(11) . ?
C35 C36 1.383(11) . ?
C36 C37 1.517(10) . ?
C40 C41 1.407(10) . ?
C40 C45 1.410(11) . ?
C41 C42 1.394(11) . ?
C41 C48 1.499(10) . ?
C42 C43 1.376(11) . ?
C43 C44 1.383(11) . ?
C43 C47 1.505(11) . ?
C44 C45 1.378(11) . ?
C45 C46 1.509(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pb N1 97.4(2) . . ?
N1 As1 C1 109.0(3) . . ?
N1 As1 C10 97.1(3) . . ?
C10 As1 C1 100.3(3) . . ?
N2 As2 C31 96.0(3) . . ?
N2 As2 C40 108.7(3) . . ?
C31 As2 C40 100.8(3) . . ?
As1 N1 Pb 113.8(3) . . ?
C19 N1 Pb 118.4(4) . . ?
C19 N1 As1 116.7(5) . . ?
As2 N2 Pb 121.4(3) . . ?
C25 N2 Pb 116.6(5) . . ?
C25 N2 As2 116.5(5) . . ?
C2 C1 As1 128.6(5) . . ?
C6 C1 As1 112.5(5) . . ?
C6 C1 C2 118.8(6) . . ?
C1 C2 C9 124.3(7) . . ?
C3 C2 C1 118.1(6) . . ?
C3 C2 C9 117.5(6) . . ?
C4 C3 C2 123.7(6) . . ?
C3 C4 C5 117.3(7) . . ?
C3 C4 C8 123.3(7) . . ?
C5 C4 C8 119.5(7) . . ?
C6 C5 C4 120.9(7) . . ?
C1 C6 C7 123.1(6) . . ?
C5 C6 C1 121.2(6) . . ?
C5 C6 C7 115.7(6) . . ?
C11 C10 As1 116.9(5) . . ?
C11 C10 C15 118.3(6) . . ?
C15 C10 As1 124.7(5) . . ?
C10 C11 C18 122.0(6) . . ?
C12 C11 C10 119.5(7) . . ?
C12 C11 C18 118.5(6) . . ?
C13 C12 C11 123.2(7) . . ?
C12 C13 C14 116.8(7) . . ?
C12 C13 C17 122.2(7) . . ?
C14 C13 C17 121.0(7) . . ?
C15 C14 C13 122.5(7) . . ?
C10 C15 C16 123.3(6) . . ?
C14 C15 C10 119.8(7) . . ?
C14 C15 C16 116.9(6) . . ?
N1 C19 C24 117.8(6) . . ?
C20 C19 N1 125.1(7) . . ?
C20 C19 C24 117.1(7) . . ?
C21 C20 C19 122.3(7) . . ?
C22 C21 C20 120.3(7) . . ?
C21 C22 C23 118.9(7) . . ?
C24 C23 C22 121.2(8) . . ?
C23 C24 C19 120.3(7) . . ?
C26 C25 N2 117.0(7) . . ?
C30 C25 N2 125.5(7) . . ?
C30 C25 C26 117.5(7) . . ?
C27 C26 C25 121.5(8) . . ?
C26 C27 C28 120.6(8) . . ?
C27 C28 C29 118.3(8) . . ?
C30 C29 C28 121.2(8) . . ?
C29 C30 C25 120.8(8) . . ?
C32 C31 As2 115.2(5) . . ?
C32 C31 C36 118.5(7) . . ?
C36 C31 As2 126.0(5) . . ?
C31 C32 C39 122.7(7) . . ?
C33 C32 C31 119.5(7) . . ?
C33 C32 C39 117.8(7) . . ?
C32 C33 C34 121.8(7) . . ?
C33 C34 C38 119.5(7) . . ?
C35 C34 C33 117.9(7) . . ?
C35 C34 C38 122.4(8) . . ?
C34 C35 C36 122.1(7) . . ?
C31 C36 C37 123.2(7) . . ?
C35 C36 C31 120.1(7) . . ?
C35 C36 C37 116.7(7) . . ?
C41 C40 As2 124.6(6) . . ?
C41 C40 C45 118.2(7) . . ?
C45 C40 As2 116.0(5) . . ?
C40 C41 C48 122.5(7) . . ?
C42 C41 C40 118.2(7) . . ?
C42 C41 C48 119.2(7) . . ?
C43 C42 C41 123.7(7) . . ?
C42 C43 C44 117.5(7) . . ?
C42 C43 C47 121.3(8) . . ?
C44 C43 C47 121.2(7) . . ?
C45 C44 C43 121.2(7) . . ?
C40 C45 C46 121.7(7) . . ?
C44 C45 C40 121.1(7) . . ?
C44 C45 C46 117.2(7) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.250 0.625 502.0 95.4 ?
2 0.000 0.250 0.125 12.6 0.0 ?
3 0.000 0.750 0.375 502.0 95.4 ?
4 0.000 0.750 0.875 12.6 0.0 ?
5 0.500 0.250 -0.125 502.0 95.4 ?
6 0.500 0.750 0.125 502.0 95.4 ?
7 0.500 0.250 0.375 12.6 0.0 ?
8 0.500 0.750 0.625 12.6 0.0 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_xcd160
_database_code_depnum_ccdc_archive 'CCDC 1949416'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record             
;
2019-08-26 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;
_audit_creation_date             2019-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3

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

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C48 H54 As2 N2 Sn), C5 H12'
_chemical_formula_sum            'C101 H120 As4 N4 Sn2'
_chemical_formula_weight         1927.06
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   23.6642(5)
_cell_length_b                   23.6642(5)
_cell_length_c                   31.7406(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17774.6(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    41855
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.03
_shelx_estimated_absorpt_T_max   0.873
_shelx_estimated_absorpt_T_min   0.489
_exptl_absorpt_coefficient_mu    2.089
_exptl_absorpt_correction_T_max  0.7968
_exptl_absorpt_correction_T_min  0.6515
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             7888
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.067
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            114872
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.725
_diffrn_reflns_theta_min         2.108
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details      
;
 819 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                71631
_reflns_number_total             114872
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         114872
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0539
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0622P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1352
_refine_special_details          
;
 Refined as a 2-component perfect twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C53_1 \\sim C52_1 \\sim C51_1 \\sim C50_1 \\sim C49_1: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
3. Others
 Fixed Sof: C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C50(0.5) H50A(0.5)
 H50B(0.5) C51(0.5) H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) C53(0.5)
 H53A(0.5) H53B(0.5) H53C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C35(H35),
  C42(H42), C44(H44)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C53(H53A,H53B,H53C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Sn Sn 0.25963(2) 0.51210(2) 0.44176(2) 0.01699(10) Uani 1 1 d . . . . .
As1 As 0.36302(2) 0.41746(2) 0.41893(2) 0.01530(13) Uani 1 1 d . . . . .
As2 As 0.12048(2) 0.49634(2) 0.47600(2) 0.01591(13) Uani 1 1 d . . . . .
N1 N 0.28882(18) 0.44113(18) 0.40728(12) 0.0166(10) Uani 1 1 d . . . . .
N2 N 0.19565(18) 0.47070(18) 0.47659(13) 0.0173(10) Uani 1 1 d . . . . .
C1 C 0.4034(2) 0.4008(2) 0.36515(15) 0.0156(11) Uani 1 1 d . . . . .
C2 C 0.3827(2) 0.3997(2) 0.32342(16) 0.0167(11) Uani 1 1 d . . . . .
C3 C 0.4193(2) 0.3848(2) 0.29068(16) 0.0175(11) Uani 1 1 d . . . . .
H3 H 0.405594 0.385693 0.262551 0.021 Uiso 1 1 calc R . . . .
C4 C 0.4749(2) 0.3686(2) 0.29774(16) 0.0194(12) Uani 1 1 d . . . . .
C5 C 0.4942(2) 0.3678(2) 0.33877(16) 0.0196(12) Uani 1 1 d . . . . .
H5 H 0.531825 0.355968 0.344308 0.024 Uiso 1 1 calc R . . . .
C6 C 0.4596(2) 0.3841(2) 0.37234(16) 0.0177(11) Uani 1 1 d . . . . .
C7 C 0.4862(2) 0.3844(2) 0.41596(15) 0.0226(13) Uani 1 1 d . . . . .
H7A H 0.489108 0.423375 0.426141 0.034 Uiso 1 1 calc GR . . . .
H7B H 0.524034 0.367602 0.414521 0.034 Uiso 1 1 calc GR . . . .
H7C H 0.462658 0.362368 0.435330 0.034 Uiso 1 1 calc GR . . . .
C8 C 0.5133(2) 0.3512(3) 0.26210(16) 0.0255(13) Uani 1 1 d . . . . .
H8A H 0.513680 0.309898 0.259834 0.038 Uiso 1 1 calc GR . . . .
H8B H 0.551673 0.364854 0.267645 0.038 Uiso 1 1 calc GR . . . .
H8C H 0.499470 0.367514 0.235655 0.038 Uiso 1 1 calc GR . . . .
C9 C 0.3221(2) 0.4133(2) 0.31193(15) 0.0204(12) Uani 1 1 d . . . . .
H9A H 0.298440 0.379871 0.316672 0.031 Uiso 1 1 calc GR . . . .
H9B H 0.320106 0.424193 0.282186 0.031 Uiso 1 1 calc GR . . . .
H9C H 0.308511 0.444494 0.329497 0.031 Uiso 1 1 calc GR . . . .
C10 C 0.3945(2) 0.4933(2) 0.43160(15) 0.0165(11) Uani 1 1 d . . . . .
C11 C 0.4156(2) 0.5014(2) 0.47296(15) 0.0171(11) Uani 1 1 d . . . . .
C12 C 0.4417(2) 0.5522(2) 0.48324(16) 0.0179(12) Uani 1 1 d . . . . .
H12 H 0.455777 0.557135 0.511035 0.021 Uiso 1 1 calc R . . . .
C13 C 0.4482(2) 0.5960(2) 0.45450(16) 0.0178(11) Uani 1 1 d . . . . .
C14 C 0.4266(2) 0.5878(2) 0.41446(16) 0.0177(11) Uani 1 1 d . . . . .
H14 H 0.429720 0.617567 0.394548 0.021 Uiso 1 1 calc R . . . .
C15 C 0.4005(2) 0.5375(2) 0.40206(15) 0.0162(11) Uani 1 1 d . . . . .
C16 C 0.3804(2) 0.5334(2) 0.35718(15) 0.0197(12) Uani 1 1 d . . . . .
H16A H 0.405567 0.508366 0.341281 0.030 Uiso 1 1 calc GR . . . .
H16B H 0.380545 0.571057 0.344364 0.030 Uiso 1 1 calc GR . . . .
H16C H 0.341907 0.518070 0.356679 0.030 Uiso 1 1 calc GR . . . .
C17 C 0.4792(2) 0.6494(2) 0.46545(17) 0.0222(12) Uani 1 1 d . . . . .
H17A H 0.474995 0.657102 0.495627 0.033 Uiso 1 1 calc GR . . . .
H17B H 0.463421 0.680922 0.449234 0.033 Uiso 1 1 calc GR . . . .
H17C H 0.519332 0.645028 0.458634 0.033 Uiso 1 1 calc GR . . . .
C18 C 0.4101(2) 0.4573(2) 0.50706(16) 0.0210(12) Uani 1 1 d . . . . .
H18A H 0.371316 0.457170 0.517887 0.032 Uiso 1 1 calc GR . . . .
H18B H 0.436352 0.466005 0.530039 0.032 Uiso 1 1 calc GR . . . .
H18C H 0.419085 0.419987 0.495409 0.032 Uiso 1 1 calc GR . . . .
C19 C 0.2499(2) 0.3982(2) 0.39583(15) 0.0167(11) Uani 1 1 d . . . . .
C20 C 0.2601(2) 0.3405(2) 0.40084(16) 0.0212(12) Uani 1 1 d . . . . .
H20 H 0.294805 0.328078 0.412721 0.025 Uiso 1 1 calc R . . . .
C21 C 0.2198(3) 0.3009(2) 0.38855(17) 0.0259(13) Uani 1 1 d . . . . .
H21 H 0.227553 0.261778 0.391840 0.031 Uiso 1 1 calc R . . . .
C22 C 0.1688(3) 0.3175(2) 0.37170(17) 0.0256(13) Uani 1 1 d . . . . .
H22 H 0.141196 0.290233 0.364098 0.031 Uiso 1 1 calc R . . . .
C23 C 0.1583(2) 0.3748(2) 0.36596(16) 0.0225(12) Uani 1 1 d . . . . .
H23 H 0.123318 0.386815 0.354318 0.027 Uiso 1 1 calc R . . . .
C24 C 0.1988(2) 0.4144(2) 0.37723(15) 0.0203(12) Uani 1 1 d . . . . .
H24 H 0.191689 0.453303 0.372201 0.024 Uiso 1 1 calc R . . . .
C25 C 0.2042(2) 0.4136(2) 0.48821(15) 0.0179(11) Uani 1 1 d . . . . .
C26 C 0.1649(3) 0.3702(2) 0.48150(16) 0.0242(13) Uani 1 1 d . . . . .
H26 H 0.129288 0.378802 0.469213 0.029 Uiso 1 1 calc R . . . .
C27 C 0.1774(3) 0.3145(3) 0.49268(18) 0.0315(15) Uani 1 1 d . . . . .
H27 H 0.150015 0.285734 0.488465 0.038 Uiso 1 1 calc R . . . .
C28 C 0.2296(3) 0.3008(3) 0.50989(18) 0.0342(16) Uani 1 1 d . . . . .
H28 H 0.238289 0.262755 0.516835 0.041 Uiso 1 1 calc R . . . .
C29 C 0.2686(3) 0.3431(3) 0.51680(17) 0.0302(15) Uani 1 1 d . . . . .
H29 H 0.304488 0.334177 0.528470 0.036 Uiso 1 1 calc R . . . .
C30 C 0.2557(2) 0.3988(2) 0.50675(16) 0.0230(13) Uani 1 1 d . . . . .
H30 H 0.282540 0.427581 0.512644 0.028 Uiso 1 1 calc R . . . .
C31 C 0.1334(2) 0.5639(2) 0.44040(15) 0.0162(11) Uani 1 1 d . . . . .
C32 C 0.1604(2) 0.6137(2) 0.45342(16) 0.0195(12) Uani 1 1 d . . . . .
C33 C 0.1624(2) 0.6596(2) 0.42538(17) 0.0254(13) Uani 1 1 d . . . . .
H33 H 0.180666 0.693424 0.434003 0.030 Uiso 1 1 calc R . . . .
C34 C 0.1386(2) 0.6570(3) 0.38546(17) 0.0259(13) Uani 1 1 d . . . . .
C35 C 0.1123(2) 0.6076(2) 0.37368(17) 0.0230(13) Uani 1 1 d . . . . .
H35 H 0.095890 0.605384 0.346411 0.028 Uiso 1 1 calc R . . . .
C36 C 0.1087(2) 0.5610(2) 0.40005(16) 0.0188(12) Uani 1 1 d . . . . .
C37 C 0.0773(2) 0.5095(2) 0.38447(16) 0.0233(13) Uani 1 1 d . . . . .
H37A H 0.099429 0.475541 0.390728 0.035 Uiso 1 1 calc GR . . . .
H37B H 0.071619 0.512540 0.353968 0.035 Uiso 1 1 calc GR . . . .
H37C H 0.040581 0.507153 0.398583 0.035 Uiso 1 1 calc GR . . . .
C38 C 0.1424(3) 0.7067(3) 0.3557(2) 0.0412(17) Uani 1 1 d . . . . .
H38A H 0.180993 0.709599 0.344683 0.062 Uiso 1 1 calc GR . . . .
H38B H 0.132735 0.741481 0.370809 0.062 Uiso 1 1 calc GR . . . .
H38C H 0.115985 0.701223 0.332270 0.062 Uiso 1 1 calc GR . . . .
C39 C 0.1870(2) 0.6218(2) 0.49637(16) 0.0241(13) Uani 1 1 d . . . . .
H39A H 0.159256 0.638418 0.515615 0.036 Uiso 1 1 calc GR . . . .
H39B H 0.219699 0.646988 0.493923 0.036 Uiso 1 1 calc GR . . . .
H39C H 0.199331 0.585078 0.507375 0.036 Uiso 1 1 calc GR . . . .
C40 C 0.1017(2) 0.5318(2) 0.53127(15) 0.0177(11) Uani 1 1 d . . . . .
C41 C 0.0516(2) 0.5643(2) 0.53148(16) 0.0195(12) Uani 1 1 d . . . . .
C42 C 0.0297(2) 0.5839(2) 0.56948(16) 0.0222(13) Uani 1 1 d . . . . .
H42 H -0.003465 0.606517 0.569198 0.027 Uiso 1 1 calc R . . . .
C43 C 0.0552(2) 0.5714(2) 0.60783(17) 0.0233(13) Uani 1 1 d . . . . .
C44 C 0.1037(2) 0.5393(2) 0.60721(17) 0.0230(13) Uani 1 1 d . . . . .
H44 H 0.121456 0.530470 0.633231 0.028 Uiso 1 1 calc R . . . .
C45 C 0.1281(2) 0.5192(2) 0.56993(16) 0.0207(12) Uani 1 1 d . . . . .
C46 C 0.1809(3) 0.4844(3) 0.57296(16) 0.0260(14) Uani 1 1 d . . . . .
H46A H 0.173722 0.446595 0.561576 0.039 Uiso 1 1 calc GR . . . .
H46B H 0.192358 0.481350 0.602535 0.039 Uiso 1 1 calc GR . . . .
H46C H 0.211070 0.502600 0.556748 0.039 Uiso 1 1 calc GR . . . .
C47 C 0.0298(3) 0.5911(3) 0.64898(17) 0.0305(14) Uani 1 1 d . . . . .
H47A H 0.005641 0.561306 0.660561 0.046 Uiso 1 1 calc GR . . . .
H47B H 0.007235 0.625186 0.644054 0.046 Uiso 1 1 calc GR . . . .
H47C H 0.060168 0.599670 0.669010 0.046 Uiso 1 1 calc GR . . . .
C48 C 0.0194(2) 0.5783(2) 0.49176(16) 0.0237(13) Uani 1 1 d . . . . .
H48A H 0.040224 0.606906 0.475717 0.036 Uiso 1 1 calc GR . . . .
H48B H -0.017996 0.592919 0.499153 0.036 Uiso 1 1 calc GR . . . .
H48C H 0.015253 0.544076 0.474627 0.036 Uiso 1 1 calc GR . . . .
C49_1 C -0.0208(7) 0.2541(10) 0.5536(5) 0.073(5) Uani 0.5 1 d . U P A -1
H49A_1 H -0.045322 0.220827 0.552178 0.109 Uiso 0.5 1 calc GR . P A -1
H49B_1 H -0.043911 0.288431 0.552979 0.109 Uiso 0.5 1 calc GR . P A -1
H49C_1 H 0.001137 0.253093 0.579813 0.109 Uiso 0.5 1 calc GR . P A -1
C50_1 C 0.0195(7) 0.2541(9) 0.5160(5) 0.064(4) Uani 0.5 1 d . U P A -1
H50A_1 H 0.043540 0.288251 0.517524 0.077 Uiso 0.5 1 calc R . P A -1
H50B_1 H 0.044618 0.220742 0.518205 0.077 Uiso 0.5 1 calc R . P A -1
C51_1 C -0.0077(12) 0.2529(17) 0.4764(4) 0.061(4) Uani 0.5 1 d . U P A -1
H51A_1 H -0.033561 0.285758 0.475080 0.073 Uiso 0.5 1 calc R . P A -1
H51B_1 H -0.031441 0.218496 0.475359 0.073 Uiso 0.5 1 calc R . P A -1
C52_1 C 0.0264(7) 0.2537(8) 0.4392(5) 0.065(4) Uani 0.5 1 d . U P A -1
H52A_1 H 0.051017 0.219905 0.439221 0.078 Uiso 0.5 1 calc R . P A -1
H52B_1 H 0.051099 0.287445 0.440069 0.078 Uiso 0.5 1 calc R . P A -1
C53_1 C -0.0086(14) 0.2547(18) 0.3973(5) 0.074(6) Uani 0.5 1 d . U P A -1
H53A_1 H 0.017073 0.250673 0.373204 0.111 Uiso 0.5 1 calc GR . P A -1
H53B_1 H -0.028957 0.290639 0.395034 0.111 Uiso 0.5 1 calc GR . P A -1
H53C_1 H -0.035722 0.223419 0.397285 0.111 Uiso 0.5 1 calc GR . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn N1 2.120(4) . ?
Sn N2 2.115(4) . ?
As1 N1 1.880(4) . ?
As1 C1 1.996(5) . ?
As1 C10 1.985(5) . ?
As2 N2 1.880(4) . ?
As2 C31 1.981(5) . ?
As2 C40 1.995(5) . ?
N1 C19 1.419(6) . ?
N2 C25 1.416(7) . ?
C1 C2 1.413(7) . ?
C1 C6 1.407(7) . ?
C2 C3 1.398(7) . ?
C2 C9 1.514(7) . ?
C3 C4 1.388(7) . ?
C4 C5 1.380(7) . ?
C4 C8 1.509(7) . ?
C5 C6 1.397(7) . ?
C6 C7 1.521(7) . ?
C10 C11 1.417(7) . ?
C10 C15 1.410(7) . ?
C11 C12 1.391(7) . ?
C11 C18 1.510(7) . ?
C12 C13 1.389(7) . ?
C13 C14 1.383(7) . ?
C13 C17 1.502(7) . ?
C14 C15 1.398(7) . ?
C15 C16 1.505(7) . ?
C19 C20 1.396(7) . ?
C19 C24 1.400(7) . ?
C20 C21 1.393(8) . ?
C21 C22 1.377(8) . ?
C22 C23 1.389(8) . ?
C23 C24 1.387(7) . ?
C25 C26 1.401(7) . ?
C25 C30 1.397(8) . ?
C26 C27 1.397(8) . ?
C27 C28 1.388(9) . ?
C28 C29 1.380(9) . ?
C29 C30 1.389(8) . ?
C31 C32 1.404(7) . ?
C31 C36 1.409(7) . ?
C32 C33 1.404(7) . ?
C32 C39 1.514(7) . ?
C33 C34 1.388(8) . ?
C34 C35 1.376(8) . ?
C34 C38 1.511(8) . ?
C35 C36 1.388(7) . ?
C36 C37 1.509(7) . ?
C40 C41 1.414(7) . ?
C40 C45 1.409(7) . ?
C41 C42 1.392(7) . ?
C41 C48 1.509(7) . ?
C42 C43 1.391(8) . ?
C43 C44 1.376(8) . ?
C43 C47 1.512(7) . ?
C44 C45 1.400(7) . ?
C45 C46 1.498(8) . ?
C49_1 C50_1 1.527(18) . ?
C50_1 C51_1 1.41(2) . ?
C51_1 C52_1 1.43(2) . ?
C52_1 C53_1 1.57(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
N2 Sn N1 97.82(16) . . ?
N1 As1 C1 109.77(19) . . ?
N1 As1 C10 97.0(2) . . ?
C10 As1 C1 99.9(2) . . ?
N2 As2 C31 96.9(2) . . ?
N2 As2 C40 109.7(2) . . ?
C31 As2 C40 101.4(2) . . ?
As1 N1 Sn 116.0(2) . . ?
C19 N1 Sn 119.2(3) . . ?
C19 N1 As1 116.3(3) . . ?
As2 N2 Sn 121.5(2) . . ?
C25 N2 Sn 118.4(3) . . ?
C25 N2 As2 116.5(3) . . ?
C2 C1 As1 129.7(4) . . ?
C6 C1 As1 111.7(4) . . ?
C6 C1 C2 118.4(5) . . ?
C1 C2 C9 123.4(5) . . ?
C3 C2 C1 119.1(5) . . ?
C3 C2 C9 117.5(4) . . ?
C4 C3 C2 122.4(5) . . ?
C3 C4 C8 121.7(5) . . ?
C5 C4 C3 118.0(5) . . ?
C5 C4 C8 120.3(5) . . ?
C4 C5 C6 121.5(5) . . ?
C1 C6 C7 122.5(4) . . ?
C5 C6 C1 120.5(5) . . ?
C5 C6 C7 117.0(5) . . ?
C11 C10 As1 116.2(4) . . ?
C15 C10 As1 124.9(4) . . ?
C15 C10 C11 118.7(5) . . ?
C10 C11 C18 122.8(5) . . ?
C12 C11 C10 119.3(5) . . ?
C12 C11 C18 117.9(4) . . ?
C13 C12 C11 122.7(5) . . ?
C12 C13 C17 122.0(5) . . ?
C14 C13 C12 117.3(5) . . ?
C14 C13 C17 120.7(5) . . ?
C13 C14 C15 122.8(5) . . ?
C10 C15 C16 123.3(5) . . ?
C14 C15 C10 119.2(5) . . ?
C14 C15 C16 117.5(5) . . ?
C20 C19 N1 124.0(5) . . ?
C20 C19 C24 117.8(5) . . ?
C24 C19 N1 118.2(5) . . ?
C21 C20 C19 120.5(5) . . ?
C22 C21 C20 121.1(5) . . ?
C21 C22 C23 119.1(5) . . ?
C24 C23 C22 120.1(5) . . ?
C23 C24 C19 121.4(5) . . ?
C26 C25 N2 124.4(5) . . ?
C30 C25 N2 118.2(5) . . ?
C30 C25 C26 117.4(5) . . ?
C27 C26 C25 120.7(6) . . ?
C28 C27 C26 120.6(6) . . ?
C29 C28 C27 119.2(6) . . ?
C28 C29 C30 120.3(6) . . ?
C29 C30 C25 121.7(6) . . ?
C32 C31 As2 125.5(4) . . ?
C32 C31 C36 119.8(5) . . ?
C36 C31 As2 114.5(4) . . ?
C31 C32 C33 118.6(5) . . ?
C31 C32 C39 124.1(5) . . ?
C33 C32 C39 117.4(5) . . ?
C34 C33 C32 122.1(5) . . ?
C33 C34 C38 120.8(6) . . ?
C35 C34 C33 118.0(5) . . ?
C35 C34 C38 121.2(5) . . ?
C34 C35 C36 122.6(5) . . ?
C31 C36 C37 122.7(5) . . ?
C35 C36 C31 119.0(5) . . ?
C35 C36 C37 118.3(5) . . ?
C41 C40 As2 114.8(4) . . ?
C45 C40 As2 125.3(4) . . ?
C45 C40 C41 118.9(5) . . ?
C40 C41 C48 122.6(5) . . ?
C42 C41 C40 119.8(5) . . ?
C42 C41 C48 117.6(5) . . ?
C43 C42 C41 121.7(5) . . ?
C42 C43 C47 121.2(5) . . ?
C44 C43 C42 117.9(5) . . ?
C44 C43 C47 121.0(5) . . ?
C43 C44 C45 122.9(5) . . ?
C40 C45 C46 122.8(5) . . ?
C44 C45 C40 118.8(5) . . ?
C44 C45 C46 118.4(5) . . ?
C51_1 C50_1 C49_1 114.3(16) . . ?
C50_1 C51_1 C52_1 119(2) . . ?
C51_1 C52_1 C53_1 113.8(19) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_xcd250
_database_code_depnum_ccdc_archive 'CCDC 1949415'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record             
;
2019-08-26 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;
_audit_creation_date             2019-07-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3

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

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H27 As Cl3 In N, C16 H32 Li O4'
_chemical_formula_sum            'C40 H59 As Cl3 In Li N O4'
_chemical_formula_weight         920.91
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   15.2723(8)
_cell_length_b                   13.4957(5)
_cell_length_c                   20.3619(11)
_cell_angle_alpha                90
_cell_angle_beta                 95.307(4)
_cell_angle_gamma                90
_cell_volume                     4178.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    37803
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.53
_cell_measurement_theta_min      1.82
_shelx_estimated_absorpt_T_max   0.722
_shelx_estimated_absorpt_T_min   0.564
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_T_max  0.6621
_exptl_absorpt_correction_T_min  0.3715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.315
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27310
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.908
_diffrn_reflns_theta_min         1.813
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_details      
;
 279 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10457
_reflns_number_total             14135
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_refine_diff_density_max         0.930
_refine_diff_density_min         -1.500
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         14135
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0415
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0424P)²+7.6068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1060
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C18(H18), C20(H20)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
In In 0.97802(2) 0.26654(2) 0.78969(2) 0.01436(5) Uani 1 1 d . . . . .
As As 0.88575(2) 0.33318(2) 0.63120(2) 0.01262(6) Uani 1 1 d . . . . .
Cl1 Cl 1.12745(4) 0.23282(6) 0.82843(4) 0.02352(14) Uani 1 1 d . . . . .
Cl2 Cl 0.91408(5) 0.10805(5) 0.79236(3) 0.02119(13) Uani 1 1 d . . . . .
Cl3 Cl 0.91921(5) 0.36550(6) 0.87252(3) 0.02428(14) Uani 1 1 d . . . . .
N N 0.97288(14) 0.34365(17) 0.70106(10) 0.0147(4) Uani 1 1 d . . . . .
C1 C 1.03241(16) 0.4212(2) 0.69498(13) 0.0152(5) Uani 1 1 d . . . . .
C2 C 1.08106(18) 0.4616(2) 0.75075(14) 0.0197(5) Uani 1 1 d . . . . .
H2 H 1.073412 0.435434 0.793140 0.024 Uiso 1 1 calc R . . . .
C3 C 1.13963(19) 0.5385(2) 0.74524(16) 0.0230(6) Uani 1 1 d . . . . .
H3 H 1.172704 0.562783 0.783684 0.028 Uiso 1 1 calc R . . . .
C4 C 1.15101(19) 0.5807(2) 0.68451(16) 0.0234(6) Uani 1 1 d . . . . .
H4 H 1.190512 0.634464 0.681065 0.028 Uiso 1 1 calc R . . . .
C5 C 1.10339(19) 0.5427(2) 0.62908(15) 0.0226(6) Uani 1 1 d . . . . .
H5 H 1.109650 0.571609 0.587239 0.027 Uiso 1 1 calc R . . . .
C6 C 1.04690(19) 0.4634(2) 0.63338(14) 0.0198(5) Uani 1 1 d . . . . .
H6 H 1.017276 0.436845 0.594227 0.024 Uiso 1 1 calc R . . . .
C7 C 0.92931(16) 0.2387(2) 0.56765(12) 0.0141(5) Uani 1 1 d . . . . .
C8 C 0.88169(17) 0.2423(2) 0.50455(12) 0.0160(5) Uani 1 1 d . . . . .
C9 C 0.91336(18) 0.1937(2) 0.45116(12) 0.0184(5) Uani 1 1 d . . . . .
H9 H 0.881088 0.197680 0.409058 0.022 Uiso 1 1 calc R . . . .
C10 C 0.99055(19) 0.1401(2) 0.45812(13) 0.0185(5) Uani 1 1 d . . . . .
C11 C 1.03519(18) 0.1336(2) 0.52076(13) 0.0176(5) Uani 1 1 d . . . . .
H11 H 1.087339 0.095009 0.526444 0.021 Uiso 1 1 calc R . . . .
C12 C 1.00647(17) 0.1816(2) 0.57550(12) 0.0145(5) Uani 1 1 d . . . . .
C13 C 1.05820(18) 0.1658(2) 0.64137(13) 0.0192(5) Uani 1 1 d . . . . .
H13A H 1.086497 0.228019 0.656253 0.029 Uiso 1 1 calc GR . . . .
H13B H 1.103245 0.115059 0.637035 0.029 Uiso 1 1 calc GR . . . .
H13C H 1.018487 0.143897 0.673640 0.029 Uiso 1 1 calc GR . . . .
C14 C 1.0256(2) 0.0895(2) 0.39997(14) 0.0261(6) Uani 1 1 d . . . . .
H14A H 1.054911 0.138366 0.373932 0.039 Uiso 1 1 calc GR . . . .
H14B H 0.976881 0.059017 0.372422 0.039 Uiso 1 1 calc GR . . . .
H14C H 1.067858 0.038179 0.415746 0.039 Uiso 1 1 calc GR . . . .
C15 C 0.79465(18) 0.2947(2) 0.49371(13) 0.0211(5) Uani 1 1 d . . . . .
H15A H 0.754218 0.267769 0.523856 0.032 Uiso 1 1 calc GR . . . .
H15B H 0.769890 0.284777 0.448047 0.032 Uiso 1 1 calc GR . . . .
H15C H 0.803117 0.365710 0.502158 0.032 Uiso 1 1 calc GR . . . .
C16 C 0.79135(16) 0.2689(2) 0.67455(12) 0.0133(4) Uani 1 1 d . . . . .
C17 C 0.74617(17) 0.3364(2) 0.71224(12) 0.0157(5) Uani 1 1 d . . . . .
C18 C 0.66905(18) 0.3070(2) 0.73823(13) 0.0189(5) Uani 1 1 d . . . . .
H18 H 0.640775 0.351650 0.765516 0.023 Uiso 1 1 calc R . . . .
C19 C 0.63280(17) 0.2148(2) 0.72533(13) 0.0187(5) Uani 1 1 d . . . . .
C20 C 0.67711(18) 0.1489(2) 0.68746(13) 0.0183(5) Uani 1 1 d . . . . .
H20 H 0.652261 0.085440 0.677901 0.022 Uiso 1 1 calc R . . . .
C21 C 0.75685(17) 0.1732(2) 0.66310(12) 0.0145(5) Uani 1 1 d . . . . .
C22 C 0.80070(19) 0.0932(2) 0.62668(14) 0.0193(5) Uani 1 1 d . . . . .
H22A H 0.800062 0.111405 0.580040 0.029 Uiso 1 1 calc GR . . . .
H22B H 0.769013 0.030648 0.630560 0.029 Uiso 1 1 calc GR . . . .
H22C H 0.861649 0.085371 0.645663 0.029 Uiso 1 1 calc GR . . . .
C23 C 0.54534(18) 0.1867(3) 0.74853(16) 0.0261(6) Uani 1 1 d . . . . .
H23A H 0.533084 0.228970 0.785710 0.039 Uiso 1 1 calc GR . . . .
H23B H 0.547016 0.117182 0.762610 0.039 Uiso 1 1 calc GR . . . .
H23C H 0.499008 0.195465 0.712379 0.039 Uiso 1 1 calc GR . . . .
C24 C 0.77593(19) 0.4416(2) 0.72391(14) 0.0213(6) Uani 1 1 d . . . . .
H24A H 0.834848 0.442035 0.747488 0.032 Uiso 1 1 calc GR . . . .
H24B H 0.734854 0.475895 0.750378 0.032 Uiso 1 1 calc GR . . . .
H24C H 0.777473 0.475531 0.681474 0.032 Uiso 1 1 calc GR . . . .
O1 O 0.48058(14) 0.32346(18) 0.53720(10) 0.0248(5) Uani 1 1 d . . . . .
O2 O 0.35874(14) 0.14372(18) 0.56894(12) 0.0281(5) Uani 1 1 d . . . . .
O3 O 0.27223(15) 0.3311(2) 0.50015(11) 0.0324(6) Uani 1 1 d . . . . .
O4 O 0.34964(14) 0.34853(16) 0.64451(10) 0.0232(4) Uani 1 1 d . . . . .
C25 C 0.5176(2) 0.3421(2) 0.47575(14) 0.0240(6) Uani 1 1 d . . . . .
H25A H 0.472326 0.368663 0.442461 0.029 Uiso 1 1 calc R . . . .
H25B H 0.541861 0.280366 0.458428 0.029 Uiso 1 1 calc R . . . .
C26 C 0.59001(18) 0.4175(2) 0.49144(14) 0.0215(6) Uani 1 1 d . . . . .
H26A H 0.569834 0.484955 0.478168 0.026 Uiso 1 1 calc R . . . .
H26B H 0.642607 0.401001 0.468613 0.026 Uiso 1 1 calc R . . . .
C27 C 0.6103(2) 0.4105(3) 0.56701(14) 0.0260(6) Uani 1 1 d . . . . .
H27A H 0.673571 0.397686 0.579045 0.031 Uiso 1 1 calc R . . . .
H27B H 0.593354 0.472256 0.588827 0.031 Uiso 1 1 calc R . . . .
C28 C 0.5549(2) 0.3242(3) 0.58603(15) 0.0302(7) Uani 1 1 d . . . . .
H28A H 0.588225 0.261328 0.585137 0.036 Uiso 1 1 calc R . . . .
H28B H 0.535813 0.333690 0.630748 0.036 Uiso 1 1 calc R . . . .
C29 C 0.2743(2) 0.0985(3) 0.5548(2) 0.0383(9) Uani 1 1 d . . . . .
H29A H 0.249261 0.115372 0.509642 0.046 Uiso 1 1 calc R . . . .
H29B H 0.233154 0.121214 0.586536 0.046 Uiso 1 1 calc R . . . .
C30 C 0.2896(2) -0.0108(3) 0.56126(17) 0.0356(8) Uani 1 1 d . . . . .
H30A H 0.243549 -0.048779 0.534654 0.043 Uiso 1 1 calc R . . . .
H30B H 0.291755 -0.032433 0.607831 0.043 Uiso 1 1 calc R . . . .
C31 C 0.3781(2) -0.0215(3) 0.53441(18) 0.0343(8) Uani 1 1 d . . . . .
H31A H 0.409048 -0.081879 0.551769 0.041 Uiso 1 1 calc R . . . .
H31B H 0.372127 -0.023908 0.485607 0.041 Uiso 1 1 calc R . . . .
C32 C 0.4254(2) 0.0710(3) 0.55945(17) 0.0286(7) Uani 1 1 d . . . . .
H32A H 0.461042 0.057494 0.601601 0.034 Uiso 1 1 calc R . . . .
H32B H 0.464891 0.095072 0.526987 0.034 Uiso 1 1 calc R . . . .
C33 C 0.1933(2) 0.3664(3) 0.52528(16) 0.0347(8) Uani 1 1 d . . . . .
H33A H 0.205296 0.427515 0.551481 0.042 Uiso 1 1 calc R . . . .
H33B H 0.169273 0.315721 0.553837 0.042 Uiso 1 1 calc R . . . .
C34 C 0.1290(2) 0.3873(3) 0.46626(18) 0.0367(8) Uani 1 1 d . . . . .
H34A H 0.069931 0.361132 0.472939 0.044 Uiso 1 1 calc R . . . .
H34B H 0.124431 0.459360 0.457443 0.044 Uiso 1 1 calc R . . . .
C35 C 0.1675(3) 0.3343(4) 0.41100(19) 0.0526(12) Uani 1 1 d . . . . .
H35A H 0.144763 0.265717 0.406666 0.063 Uiso 1 1 calc R . . . .
H35B H 0.153166 0.369471 0.368681 0.063 Uiso 1 1 calc R . . . .
C36 C 0.2626(3) 0.3345(4) 0.42935(17) 0.0457(10) Uani 1 1 d . . . . .
H36A H 0.290582 0.276080 0.410618 0.055 Uiso 1 1 calc R . . . .
H36B H 0.289839 0.395303 0.413177 0.055 Uiso 1 1 calc R . . . .
C37 C 0.3695(2) 0.4502(2) 0.66080(14) 0.0244(6) Uani 1 1 d . . . . .
H37A H 0.321909 0.494307 0.641788 0.029 Uiso 1 1 calc R . . . .
H37B H 0.425350 0.470450 0.643599 0.029 Uiso 1 1 calc R . . . .
C38 C 0.3774(2) 0.4554(3) 0.73627(15) 0.0313(7) Uani 1 1 d . . . . .
H38A H 0.347923 0.515341 0.751538 0.038 Uiso 1 1 calc R . . . .
H38B H 0.439863 0.456277 0.754294 0.038 Uiso 1 1 calc R . . . .
C39 C 0.3313(2) 0.3609(3) 0.75748(14) 0.0254(6) Uani 1 1 d . . . . .
H39A H 0.373841 0.315009 0.781175 0.030 Uiso 1 1 calc R . . . .
H39B H 0.284475 0.376988 0.786264 0.030 Uiso 1 1 calc R . . . .
C40 C 0.2929(2) 0.3163(2) 0.69264(14) 0.0250(6) Uani 1 1 d . . . . .
H40A H 0.291995 0.243110 0.695355 0.030 Uiso 1 1 calc R . . . .
H40B H 0.232135 0.340330 0.681224 0.030 Uiso 1 1 calc R . . . .
Li Li 0.3670(4) 0.2858(4) 0.5599(3) 0.0267(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
In Cl1 2.3884(7) . ?
In Cl2 2.3540(7) . ?
In Cl3 2.3906(7) . ?
In N 2.078(2) . ?
As N 1.861(2) . ?
As C7 1.976(3) . ?
As C16 1.961(3) . ?
N C1 1.400(3) . ?
C1 C2 1.408(4) . ?
C1 C6 1.414(4) . ?
C2 C3 1.381(4) . ?
C3 C4 1.387(4) . ?
C4 C5 1.384(4) . ?
C5 C6 1.382(4) . ?
C7 C8 1.418(3) . ?
C7 C12 1.404(4) . ?
C8 C9 1.394(4) . ?
C8 C15 1.504(4) . ?
C9 C10 1.380(4) . ?
C10 C11 1.392(4) . ?
C10 C14 1.507(4) . ?
C11 C12 1.394(4) . ?
C12 C13 1.508(4) . ?
C16 C17 1.412(4) . ?
C16 C21 1.406(4) . ?
C17 C18 1.393(4) . ?
C17 C24 1.503(4) . ?
C18 C19 1.377(4) . ?
C19 C20 1.393(4) . ?
C19 C23 1.506(4) . ?
C20 C21 1.396(4) . ?
C21 C22 1.502(4) . ?
O1 C25 1.442(3) . ?
O1 C28 1.438(4) . ?
O1 Li 1.904(6) . ?
O2 C29 1.432(4) . ?
O2 C32 1.440(4) . ?
O2 Li 1.932(7) . ?
O3 C33 1.435(4) . ?
O3 C36 1.436(4) . ?
O3 Li 1.903(6) . ?
O4 C37 1.438(4) . ?
O4 C40 1.434(4) . ?
O4 Li 1.960(6) . ?
C25 C26 1.515(4) . ?
C26 C27 1.544(4) . ?
C27 C28 1.511(5) . ?
C29 C30 1.497(6) . ?
C30 C31 1.512(5) . ?
C31 C32 1.508(5) . ?
C33 C34 1.506(5) . ?
C34 C35 1.498(6) . ?
C35 C36 1.466(6) . ?
C37 C38 1.532(4) . ?
C38 C39 1.537(5) . ?
C39 C40 1.519(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 In Cl3 106.46(3) . . ?
Cl2 In Cl1 101.83(3) . . ?
Cl2 In Cl3 107.92(3) . . ?
N In Cl1 109.89(6) . . ?
N In Cl2 119.51(6) . . ?
N In Cl3 110.27(7) . . ?
N As C7 106.81(10) . . ?
N As C16 101.13(10) . . ?
C16 As C7 108.39(11) . . ?
As N In 126.33(12) . . ?
C1 N In 118.60(16) . . ?
C1 N As 114.43(17) . . ?
N C1 C2 121.1(2) . . ?
N C1 C6 122.4(2) . . ?
C2 C1 C6 116.4(3) . . ?
C3 C2 C1 121.5(3) . . ?
C2 C3 C4 121.1(3) . . ?
C5 C4 C3 118.3(3) . . ?
C6 C5 C4 121.3(3) . . ?
C5 C6 C1 121.2(3) . . ?
C8 C7 As 113.29(19) . . ?
C12 C7 As 127.55(19) . . ?
C12 C7 C8 118.5(2) . . ?
C7 C8 C15 121.5(2) . . ?
C9 C8 C7 120.3(2) . . ?
C9 C8 C15 118.2(2) . . ?
C10 C9 C8 121.4(2) . . ?
C9 C10 C11 117.9(2) . . ?
C9 C10 C14 121.3(3) . . ?
C11 C10 C14 120.8(3) . . ?
C10 C11 C12 122.7(3) . . ?
C7 C12 C13 123.0(2) . . ?
C11 C12 C7 119.1(2) . . ?
C11 C12 C13 117.9(2) . . ?
C17 C16 As 112.1(2) . . ?
C21 C16 As 127.69(19) . . ?
C21 C16 C17 119.2(2) . . ?
C16 C17 C24 122.7(2) . . ?
C18 C17 C16 119.7(3) . . ?
C18 C17 C24 117.6(2) . . ?
C19 C18 C17 121.6(3) . . ?
C18 C19 C20 118.4(3) . . ?
C18 C19 C23 121.4(3) . . ?
C20 C19 C23 120.2(3) . . ?
C19 C20 C21 122.1(3) . . ?
C16 C21 C22 124.4(2) . . ?
C20 C21 C16 118.9(2) . . ?
C20 C21 C22 116.8(2) . . ?
C25 O1 Li 134.1(2) . . ?
C28 O1 C25 104.5(2) . . ?
C28 O1 Li 120.8(2) . . ?
C29 O2 C32 108.5(3) . . ?
C29 O2 Li 118.0(3) . . ?
C32 O2 Li 127.6(3) . . ?
C33 O3 C36 109.6(3) . . ?
C33 O3 Li 119.6(2) . . ?
C36 O3 Li 130.8(3) . . ?
C37 O4 Li 124.9(2) . . ?
C40 O4 C37 105.0(2) . . ?
C40 O4 Li 127.6(3) . . ?
O1 C25 C26 105.8(2) . . ?
C25 C26 C27 104.1(2) . . ?
C28 C27 C26 103.7(2) . . ?
O1 C28 C27 104.6(2) . . ?
O2 C29 C30 105.8(3) . . ?
C29 C30 C31 101.6(3) . . ?
C32 C31 C30 102.4(3) . . ?
O2 C32 C31 106.7(3) . . ?
O3 C33 C34 106.6(3) . . ?
C35 C34 C33 103.8(3) . . ?
C36 C35 C34 104.8(3) . . ?
O3 C36 C35 105.2(3) . . ?
O4 C37 C38 105.7(2) . . ?
C37 C38 C39 104.4(3) . . ?
C40 C39 C38 103.5(2) . . ?
O4 C40 C39 105.4(2) . . ?
O1 Li O2 110.9(3) . . ?
O1 Li O4 107.3(3) . . ?
O2 Li O4 109.2(3) . . ?
O3 Li O1 114.6(3) . . ?
O3 Li O2 109.1(3) . . ?
O3 Li O4 105.4(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_XCD130-2
_database_code_depnum_ccdc_archive 'CCDC 1949411'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record             
;
2019-08-26 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;
_audit_creation_date             2019-07-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3

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

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H62 As2 Cl2 Hf N2 O, C H2 Cl2'
_chemical_formula_sum            'C53 H64 As2 Cl4 Hf N2 O'
_chemical_formula_weight         1215.19
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   12.3504(5)
_cell_length_b                   16.8952(5)
_cell_length_c                   24.8854(10)
_cell_angle_alpha                90
_cell_angle_beta                 102.520(3)
_cell_angle_gamma                90
_cell_volume                     5069.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    38614
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.99
_cell_measurement_theta_min      2.37
_shelx_estimated_absorpt_T_max   0.766
_shelx_estimated_absorpt_T_min   0.324
_exptl_absorpt_coefficient_mu    3.60
_exptl_absorpt_correction_T_max  0.4329
_exptl_absorpt_correction_T_min  0.2035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.078
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            29684
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.010
_diffrn_reflns_theta_min         2.411
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_details      
;
 265 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10823
_reflns_number_total             13188
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_refine_diff_density_max         1.159
_refine_diff_density_min         -1.234
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         13188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0422P)²+7.6411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0843
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C18(H18), C20(H20),
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C35(H35), C42(H42),
  C44(H44)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Hf Hf 0.47684(2) 0.81973(2) 0.62602(2) 0.01379(4) Uani 1 1 d . . . . .
As1 As 0.21297(3) 0.79823(2) 0.61810(2) 0.01291(7) Uani 1 1 d . . . . .
As2 As 0.40363(3) 0.85723(2) 0.74056(2) 0.01438(7) Uani 1 1 d . . . . .
Cl1 Cl 0.54805(7) 0.95462(5) 0.64595(3) 0.02041(16) Uani 1 1 d . . . . .
Cl2 Cl 0.45900(8) 0.68199(5) 0.59262(4) 0.02410(18) Uani 1 1 d . . . . .
O O 0.60990(19) 0.81820(16) 0.58133(10) 0.0222(5) Uani 1 1 d . . . . .
N1 N 0.3204(2) 0.84647(17) 0.58652(11) 0.0143(5) Uani 1 1 d . . . . .
N2 N 0.4966(2) 0.79551(17) 0.70697(11) 0.0156(5) Uani 1 1 d . . . . .
C1 C 0.3221(3) 0.8597(2) 0.53034(13) 0.0169(7) Uani 1 1 d . . . . .
C2 C 0.3588(3) 0.9328(2) 0.51504(14) 0.0192(7) Uani 1 1 d . . . . .
H2 H 0.376552 0.973807 0.541640 0.023 Uiso 1 1 calc R . . . .
C3 C 0.3696(3) 0.9463(2) 0.46149(14) 0.0225(7) Uani 1 1 d . . . . .
H3 H 0.393565 0.996573 0.451494 0.027 Uiso 1 1 calc R . . . .
C4 C 0.3457(3) 0.8868(2) 0.42266(14) 0.0229(7) Uani 1 1 d . . . . .
H4 H 0.352777 0.896088 0.385926 0.027 Uiso 1 1 calc R . . . .
C5 C 0.3114(3) 0.8136(2) 0.43759(14) 0.0220(7) Uani 1 1 d . . . . .
H5 H 0.295766 0.772540 0.410961 0.026 Uiso 1 1 calc R . . . .
C6 C 0.2994(3) 0.7994(2) 0.49086(13) 0.0178(7) Uani 1 1 d . . . . .
H6 H 0.275867 0.748846 0.500578 0.021 Uiso 1 1 calc R . . . .
C7 C 0.1142(2) 0.88063(19) 0.63706(13) 0.0142(6) Uani 1 1 d . . . . .
C8 C 0.0369(3) 0.8488(2) 0.66537(13) 0.0162(6) Uani 1 1 d . . . . .
C9 C -0.0374(3) 0.8993(2) 0.68302(13) 0.0182(7) Uani 1 1 d . . . . .
H9 H -0.089297 0.877450 0.702055 0.022 Uiso 1 1 calc R . . . .
C10 C -0.0385(3) 0.9802(2) 0.67385(14) 0.0194(7) Uani 1 1 d . . . . .
C11 C 0.0412(3) 1.0111(2) 0.64786(14) 0.0190(7) Uani 1 1 d . . . . .
H11 H 0.043155 1.066566 0.642058 0.023 Uiso 1 1 calc R . . . .
C12 C 0.1189(3) 0.9627(2) 0.62993(13) 0.0171(6) Uani 1 1 d . . . . .
C13 C 0.2026(3) 1.0036(2) 0.60341(15) 0.0206(7) Uani 1 1 d . . . . .
H13A H 0.277498 0.993371 0.625074 0.031 Uiso 1 1 calc GR . . . .
H13B H 0.188440 1.060714 0.601950 0.031 Uiso 1 1 calc GR . . . .
H13C H 0.196158 0.983238 0.565973 0.031 Uiso 1 1 calc GR . . . .
C14 C -0.1217(3) 1.0323(2) 0.69298(16) 0.0257(8) Uani 1 1 d . . . . .
H14A H -0.194897 1.007050 0.684076 0.038 Uiso 1 1 calc GR . . . .
H14B H -0.125384 1.083697 0.674425 0.038 Uiso 1 1 calc GR . . . .
H14C H -0.099110 1.040001 0.732870 0.038 Uiso 1 1 calc GR . . . .
C15 C 0.0295(3) 0.7616(2) 0.67703(14) 0.0197(7) Uani 1 1 d . . . . .
H15A H -0.027176 0.752749 0.698502 0.029 Uiso 1 1 calc GR . . . .
H15B H 0.101441 0.742773 0.697965 0.029 Uiso 1 1 calc GR . . . .
H15C H 0.009545 0.732515 0.642201 0.029 Uiso 1 1 calc GR . . . .
C16 C 0.1079(2) 0.7463(2) 0.55672(12) 0.0137(6) Uani 1 1 d . . . . .
C17 C 0.0986(3) 0.6641(2) 0.56163(14) 0.0177(7) Uani 1 1 d . . . . .
C18 C 0.0181(3) 0.6231(2) 0.52343(14) 0.0193(7) Uani 1 1 d . . . . .
H18 H 0.011079 0.567480 0.527123 0.023 Uiso 1 1 calc R . . . .
C19 C -0.0515(3) 0.6618(2) 0.48053(14) 0.0198(7) Uani 1 1 d . . . . .
C20 C -0.0405(3) 0.7434(2) 0.47650(13) 0.0182(7) Uani 1 1 d . . . . .
H20 H -0.087831 0.770449 0.447066 0.022 Uiso 1 1 calc R . . . .
C21 C 0.0370(3) 0.7868(2) 0.51373(13) 0.0159(6) Uani 1 1 d . . . . .
C22 C 0.0402(3) 0.8748(2) 0.50479(14) 0.0196(7) Uani 1 1 d . . . . .
H22A H 0.003205 0.901880 0.530644 0.029 Uiso 1 1 calc GR . . . .
H22B H 0.002057 0.887343 0.466977 0.029 Uiso 1 1 calc GR . . . .
H22C H 0.117539 0.892405 0.510919 0.029 Uiso 1 1 calc GR . . . .
C23 C -0.1357(3) 0.6172(2) 0.43901(15) 0.0262(8) Uani 1 1 d . . . . .
H23A H -0.097925 0.578355 0.420289 0.039 Uiso 1 1 calc GR . . . .
H23B H -0.177170 0.654342 0.411907 0.039 Uiso 1 1 calc GR . . . .
H23C H -0.187063 0.589859 0.457704 0.039 Uiso 1 1 calc GR . . . .
C24 C 0.1720(3) 0.6158(2) 0.60637(15) 0.0213(7) Uani 1 1 d . . . . .
H24A H 0.249903 0.624253 0.605082 0.032 Uiso 1 1 calc GR . . . .
H24B H 0.153701 0.559578 0.600663 0.032 Uiso 1 1 calc GR . . . .
H24C H 0.159928 0.632386 0.642358 0.032 Uiso 1 1 calc GR . . . .
C25 C 0.6075(3) 0.7696(2) 0.72854(13) 0.0188(7) Uani 1 1 d . . . . .
C26 C 0.6376(3) 0.6920(2) 0.71784(15) 0.0215(7) Uani 1 1 d . . . . .
H26 H 0.583153 0.656794 0.698262 0.026 Uiso 1 1 calc R . . . .
C27 C 0.7464(3) 0.6663(2) 0.73565(16) 0.0272(8) Uani 1 1 d . . . . .
H27 H 0.765845 0.613991 0.727319 0.033 Uiso 1 1 calc R . . . .
C28 C 0.8263(3) 0.7155(3) 0.76515(16) 0.0311(9) Uani 1 1 d . . . . .
H28 H 0.900052 0.697137 0.778156 0.037 Uiso 1 1 calc R . . . .
C29 C 0.7976(3) 0.7922(3) 0.77558(15) 0.0278(8) Uani 1 1 d . . . . .
H29 H 0.852531 0.826266 0.796176 0.033 Uiso 1 1 calc R . . . .
C30 C 0.6909(3) 0.8207(2) 0.75679(15) 0.0229(7) Uani 1 1 d . . . . .
H30 H 0.674086 0.874398 0.762905 0.027 Uiso 1 1 calc R . . . .
C31 C 0.3055(3) 0.7869(2) 0.77262(13) 0.0149(6) Uani 1 1 d . . . . .
C32 C 0.2307(3) 0.8301(2) 0.79656(14) 0.0173(7) Uani 1 1 d . . . . .
C33 C 0.1601(3) 0.7899(2) 0.82384(14) 0.0199(7) Uani 1 1 d . . . . .
H33 H 0.110257 0.819485 0.840150 0.024 Uiso 1 1 calc R . . . .
C34 C 0.1602(3) 0.7077(2) 0.82799(14) 0.0189(7) Uani 1 1 d . . . . .
C35 C 0.2288(3) 0.6664(2) 0.80011(13) 0.0172(7) Uani 1 1 d . . . . .
H35 H 0.226985 0.610187 0.800495 0.021 Uiso 1 1 calc R . . . .
C36 C 0.2999(3) 0.7038(2) 0.77171(13) 0.0172(7) Uani 1 1 d . . . . .
C37 C 0.3672(3) 0.6524(2) 0.74183(14) 0.0187(7) Uani 1 1 d . . . . .
H37A H 0.362357 0.673251 0.704622 0.028 Uiso 1 1 calc GR . . . .
H37B H 0.338227 0.598261 0.739534 0.028 Uiso 1 1 calc GR . . . .
H37C H 0.444808 0.652404 0.761861 0.028 Uiso 1 1 calc GR . . . .
C38 C 0.0897(3) 0.6655(2) 0.86101(15) 0.0232(7) Uani 1 1 d . . . . .
H38A H 0.137188 0.642960 0.894157 0.035 Uiso 1 1 calc GR . . . .
H38B H 0.048247 0.623039 0.838809 0.035 Uiso 1 1 calc GR . . . .
H38C H 0.037600 0.703114 0.871625 0.035 Uiso 1 1 calc GR . . . .
C39 C 0.2230(3) 0.9196(2) 0.79389(15) 0.0216(7) Uani 1 1 d . . . . .
H39A H 0.291243 0.942653 0.815861 0.032 Uiso 1 1 calc GR . . . .
H39B H 0.159486 0.937199 0.808533 0.032 Uiso 1 1 calc GR . . . .
H39C H 0.213353 0.936926 0.755555 0.032 Uiso 1 1 calc GR . . . .
C40 C 0.5039(3) 0.8938(2) 0.80948(14) 0.0176(7) Uani 1 1 d . . . . .
C41 C 0.5233(3) 0.9760(2) 0.81350(14) 0.0200(7) Uani 1 1 d . . . . .
C42 C 0.5948(3) 1.0060(2) 0.86005(16) 0.0245(8) Uani 1 1 d . . . . .
H42 H 0.606949 1.061495 0.863046 0.029 Uiso 1 1 calc R . . . .
C43 C 0.6490(3) 0.9571(2) 0.90231(15) 0.0253(8) Uani 1 1 d . . . . .
C44 C 0.6273(3) 0.8765(2) 0.89766(15) 0.0232(8) Uani 1 1 d . . . . .
H44 H 0.662492 0.842650 0.926709 0.028 Uiso 1 1 calc R . . . .
C45 C 0.5560(3) 0.8432(2) 0.85210(14) 0.0193(7) Uani 1 1 d . . . . .
C46 C 0.5405(3) 0.7554(2) 0.85181(14) 0.0197(7) Uani 1 1 d . . . . .
H46A H 0.462771 0.743157 0.851347 0.030 Uiso 1 1 calc GR . . . .
H46B H 0.588015 0.732618 0.884881 0.030 Uiso 1 1 calc GR . . . .
H46C H 0.560670 0.732935 0.819011 0.030 Uiso 1 1 calc GR . . . .
C47 C 0.7290(3) 0.9898(3) 0.95170(17) 0.0370(10) Uani 1 1 d . . . . .
H47A H 0.715141 0.965088 0.985195 0.056 Uiso 1 1 calc GR . . . .
H47B H 0.718616 1.047207 0.953562 0.056 Uiso 1 1 calc GR . . . .
H47C H 0.805140 0.978564 0.948503 0.056 Uiso 1 1 calc GR . . . .
C48 C 0.4692(3) 1.0336(2) 0.77028(16) 0.0262(8) Uani 1 1 d . . . . .
H48A H 0.487720 1.019887 0.735084 0.039 Uiso 1 1 calc GR . . . .
H48B H 0.495815 1.087204 0.781027 0.039 Uiso 1 1 calc GR . . . .
H48C H 0.388562 1.031583 0.766423 0.039 Uiso 1 1 calc GR . . . .
C49 C 0.7278(3) 0.8270(3) 0.60786(16) 0.0268(8) Uani 1 1 d . . . . .
H49A H 0.745444 0.798126 0.643302 0.032 Uiso 1 1 calc R . . . .
H49B H 0.747313 0.883498 0.614712 0.032 Uiso 1 1 calc R . . . .
C50 C 0.7886(4) 0.7923(4) 0.56786(18) 0.0534(15) Uani 1 1 d . . . . .
H50A H 0.801053 0.734879 0.574467 0.064 Uiso 1 1 calc R . . . .
H50B H 0.861193 0.818668 0.570568 0.064 Uiso 1 1 calc R . . . .
C51 C 0.7141(3) 0.8069(4) 0.51297(17) 0.0440(13) Uani 1 1 d . . . . .
H51A H 0.727816 0.767880 0.485546 0.053 Uiso 1 1 calc R . . . .
H51B H 0.725351 0.860862 0.499604 0.053 Uiso 1 1 calc R . . . .
C52 C 0.5996(3) 0.7979(3) 0.52304(15) 0.0276(8) Uani 1 1 d . . . . .
H52A H 0.547234 0.834161 0.499149 0.033 Uiso 1 1 calc R . . . .
H52B H 0.572895 0.742877 0.515753 0.033 Uiso 1 1 calc R . . . .
Cl3 Cl 0.55529(12) 0.47855(8) 0.64953(5) 0.0517(3) Uani 1 1 d . . . . .
Cl4 Cl 0.47436(12) 0.39615(8) 0.54636(6) 0.0569(3) Uani 1 1 d . . . . .
C53 C 0.4622(4) 0.4795(3) 0.5861(2) 0.0456(12) Uani 1 1 d . . . . .
H53A H 0.475079 0.527612 0.565650 0.055 Uiso 1 1 calc R . . . .
H53B H 0.385695 0.482270 0.592241 0.055 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf As1 3.2423(4) . ?
Hf As2 3.2342(4) . ?
Hf Cl1 2.4543(8) . ?
Hf Cl2 2.4650(9) . ?
Hf O 2.175(2) . ?
Hf N1 2.020(3) . ?
Hf N2 2.018(3) . ?
Hf C1 2.794(3) . ?
As1 N1 1.870(3) . ?
As1 C7 1.974(3) . ?
As1 C16 1.982(3) . ?
As2 N2 1.877(3) . ?
As2 C31 1.984(3) . ?
As2 C40 1.984(3) . ?
O C49 1.470(4) . ?
O C52 1.469(4) . ?
N1 C1 1.421(4) . ?
N2 C25 1.427(4) . ?
C1 C2 1.397(5) . ?
C1 C6 1.401(5) . ?
C2 C3 1.387(5) . ?
C3 C4 1.381(5) . ?
C4 C5 1.384(5) . ?
C5 C6 1.386(5) . ?
C7 C8 1.410(4) . ?
C7 C12 1.401(5) . ?
C8 C9 1.392(5) . ?
C8 C15 1.509(5) . ?
C9 C10 1.386(5) . ?
C10 C11 1.391(5) . ?
C10 C14 1.506(5) . ?
C11 C12 1.404(5) . ?
C12 C13 1.509(5) . ?
C16 C17 1.402(5) . ?
C16 C21 1.405(4) . ?
C17 C18 1.401(5) . ?
C17 C24 1.512(5) . ?
C18 C19 1.381(5) . ?
C19 C20 1.390(5) . ?
C19 C23 1.501(4) . ?
C20 C21 1.389(5) . ?
C21 C22 1.504(5) . ?
C25 C26 1.404(5) . ?
C25 C30 1.409(5) . ?
C26 C27 1.391(5) . ?
C27 C28 1.375(6) . ?
C28 C29 1.383(6) . ?
C29 C30 1.386(5) . ?
C31 C32 1.407(5) . ?
C31 C36 1.406(5) . ?
C32 C33 1.392(5) . ?
C32 C39 1.516(5) . ?
C33 C34 1.393(5) . ?
C34 C35 1.393(5) . ?
C34 C38 1.500(5) . ?
C35 C36 1.392(5) . ?
C36 C37 1.504(5) . ?
C40 C41 1.409(5) . ?
C40 C45 1.405(5) . ?
C41 C42 1.391(5) . ?
C41 C48 1.497(5) . ?
C42 C43 1.390(5) . ?
C43 C44 1.387(6) . ?
C43 C47 1.505(5) . ?
C44 C45 1.395(5) . ?
C45 C46 1.495(5) . ?
C49 C50 1.491(6) . ?
C50 C51 1.493(6) . ?
C51 C52 1.497(5) . ?
Cl3 C53 1.739(5) . ?
Cl4 C53 1.747(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
As2 Hf As1 66.812(9) . . ?
Cl1 Hf As1 115.32(2) . . ?
Cl1 Hf As2 78.26(2) . . ?
Cl1 Hf Cl2 161.21(3) . . ?
Cl1 Hf C1 95.55(7) . . ?
Cl2 Hf As1 81.87(2) . . ?
Cl2 Hf As2 117.42(2) . . ?
Cl2 Hf C1 86.91(8) . . ?
O Hf As1 145.94(6) . . ?
O Hf As2 147.09(6) . . ?
O Hf Cl1 80.62(7) . . ?
O Hf Cl2 80.71(7) . . ?
O Hf C1 91.15(9) . . ?
N1 Hf As1 32.08(8) . . ?
N1 Hf As2 87.97(8) . . ?
N1 Hf Cl1 98.84(8) . . ?
N1 Hf Cl2 92.34(8) . . ?
N1 Hf O 120.18(10) . . ?
N1 Hf C1 29.04(10) . . ?
N2 Hf As1 86.60(7) . . ?
N2 Hf As2 32.48(8) . . ?
N2 Hf Cl1 91.49(8) . . ?
N2 Hf Cl2 97.35(8) . . ?
N2 Hf O 124.51(10) . . ?
N2 Hf N1 115.30(11) . . ?
N2 Hf C1 144.33(10) . . ?
C1 Hf As1 58.83(7) . . ?
C1 Hf As2 115.69(7) . . ?
N1 As1 C7 108.94(13) . . ?
N1 As1 C16 105.97(12) . . ?
C7 As1 Hf 124.84(9) . . ?
C7 As1 C16 99.26(13) . . ?
C16 As1 Hf 125.33(9) . . ?
N2 As2 C31 109.42(13) . . ?
N2 As2 C40 103.32(13) . . ?
C31 As2 Hf 123.29(9) . . ?
C31 As2 C40 99.22(13) . . ?
C40 As2 Hf 125.55(9) . . ?
C49 O Hf 123.6(2) . . ?
C52 O Hf 126.5(2) . . ?
C52 O C49 109.4(3) . . ?
As1 N1 Hf 112.90(13) . . ?
C1 N1 Hf 107.33(19) . . ?
C1 N1 As1 130.2(2) . . ?
As2 N2 Hf 112.24(13) . . ?
C25 N2 Hf 109.7(2) . . ?
C25 N2 As2 129.3(2) . . ?
C2 C1 Hf 104.1(2) . . ?
C2 C1 N1 118.8(3) . . ?
C2 C1 C6 118.7(3) . . ?
C6 C1 Hf 114.7(2) . . ?
C6 C1 N1 122.2(3) . . ?
C3 C2 C1 120.8(3) . . ?
C4 C3 C2 120.2(3) . . ?
C3 C4 C5 119.6(3) . . ?
C4 C5 C6 120.9(3) . . ?
C5 C6 C1 119.9(3) . . ?
C8 C7 As1 111.8(2) . . ?
C12 C7 As1 128.6(2) . . ?
C12 C7 C8 119.4(3) . . ?
C7 C8 C15 122.9(3) . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 C15 117.8(3) . . ?
C10 C9 C8 122.4(3) . . ?
C9 C10 C11 117.6(3) . . ?
C9 C10 C14 120.5(3) . . ?
C11 C10 C14 121.9(3) . . ?
C10 C11 C12 122.1(3) . . ?
C7 C12 C11 119.1(3) . . ?
C7 C12 C13 124.0(3) . . ?
C11 C12 C13 116.9(3) . . ?
C17 C16 As1 115.1(2) . . ?
C17 C16 C21 120.0(3) . . ?
C21 C16 As1 124.6(2) . . ?
C16 C17 C24 123.5(3) . . ?
C18 C17 C16 119.3(3) . . ?
C18 C17 C24 117.2(3) . . ?
C19 C18 C17 121.4(3) . . ?
C18 C19 C20 118.1(3) . . ?
C18 C19 C23 121.1(3) . . ?
C20 C19 C23 120.8(3) . . ?
C21 C20 C19 122.7(3) . . ?
C16 C21 C22 124.2(3) . . ?
C20 C21 C16 118.4(3) . . ?
C20 C21 C22 117.4(3) . . ?
C26 C25 N2 119.1(3) . . ?
C26 C25 C30 118.1(3) . . ?
C30 C25 N2 122.5(3) . . ?
C27 C26 C25 120.6(4) . . ?
C28 C27 C26 120.9(4) . . ?
C27 C28 C29 118.9(3) . . ?
C28 C29 C30 121.7(4) . . ?
C29 C30 C25 119.6(4) . . ?
C32 C31 As2 112.0(2) . . ?
C36 C31 As2 128.6(2) . . ?
C36 C31 C32 119.3(3) . . ?
C31 C32 C39 122.6(3) . . ?
C33 C32 C31 119.4(3) . . ?
C33 C32 C39 117.9(3) . . ?
C34 C33 C32 122.2(3) . . ?
C33 C34 C35 116.9(3) . . ?
C33 C34 C38 121.5(3) . . ?
C35 C34 C38 121.5(3) . . ?
C36 C35 C34 123.0(3) . . ?
C31 C36 C37 123.6(3) . . ?
C35 C36 C31 118.6(3) . . ?
C35 C36 C37 117.8(3) . . ?
C41 C40 As2 115.7(2) . . ?
C45 C40 As2 124.1(3) . . ?
C45 C40 C41 120.2(3) . . ?
C40 C41 C48 123.2(3) . . ?
C42 C41 C40 119.0(3) . . ?
C42 C41 C48 117.7(3) . . ?
C43 C42 C41 121.9(4) . . ?
C42 C43 C47 121.5(4) . . ?
C44 C43 C42 117.9(3) . . ?
C44 C43 C47 120.6(4) . . ?
C43 C44 C45 122.7(3) . . ?
C40 C45 C46 124.3(3) . . ?
C44 C45 C40 118.2(3) . . ?
C44 C45 C46 117.5(3) . . ?
O C49 C50 104.7(3) . . ?
C49 C50 C51 104.2(4) . . ?
C50 C51 C52 104.3(4) . . ?
O C52 C51 105.0(3) . . ?
Cl3 C53 Cl4 112.7(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
