#------------------------------------------------------------------------------
#$Date: 2023-03-02 10:43:05 +0200 (Thu, 02 Mar 2023) $
#$Revision: 281243 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/24/7712489.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7712489
loop_
_publ_author_name
'Dissanayake, Deepamali'
'Forsyth, Craig M.'
'Vidovic, Dragoslav'
_publ_section_title
;
 Synthesis, Characterisation and Reactivity studies of Chiral
 β-Diketiminate-like Supported Aluminium Lewis Acid Complexes Towards
 Difficult Diels Alder Cycloadditions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00206C
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         '2(C45 H42 N2 O), C H Cl3'
_chemical_formula_sum            'C91 H85 Cl3 N4 O2'
_chemical_formula_weight         1372.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-01-18 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.6780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.8439(2)
_cell_length_b                   10.55050(10)
_cell_length_c                   28.3697(2)
_cell_measurement_reflns_used    37807
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      75.7570
_cell_measurement_theta_min      4.2540
_cell_volume                     7575.34(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            61556
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.497
_diffrn_reflns_theta_min         4.223
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       plate
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 6461 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.045(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         15643
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0513
_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)+(0.0495P)²+8.0459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                15022
_reflns_number_total             15643
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00206c2.cif
_cod_data_source_block           MX50_20
_cod_original_cell_volume        7575.33(11)
_cod_original_sg_symbol_H-M      'I 2'
_cod_database_code               7712489
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
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
O1 O 0.08218(9) -0.2284(2) 0.33347(9) 0.0408(5) Uani 1 1 d . . . . .
O2 O 0.40168(10) 1.0544(2) 0.65511(9) 0.0414(5) Uani 1 1 d . . . . .
N1 N 0.09147(10) 0.1516(3) 0.37988(10) 0.0331(6) Uani 1 1 d . . . . .
H1N H 0.1108(16) 0.123(4) 0.3581(15) 0.047(11) Uiso 1 1 d . . . . .
N2 N 0.11619(11) -0.0347(3) 0.32432(10) 0.0383(6) Uani 1 1 d . . . . .
N3 N 0.40122(10) 0.6712(3) 0.61411(10) 0.0309(6) Uani 1 1 d . . . . .
H3N H 0.3755(19) 0.703(5) 0.6271(16) 0.060(13) Uiso 1 1 d . . . . .
N4 N 0.36199(10) 0.8651(3) 0.65590(10) 0.0362(6) Uani 1 1 d . . . . .
C1 C 0.05622(12) 0.0690(3) 0.39319(11) 0.0311(6) Uani 1 1 d . . . . .
C2 C 0.02293(13) 0.1074(4) 0.42404(13) 0.0410(8) Uani 1 1 d . . . . .
H2 H 0.025221 0.191751 0.436038 0.049 Uiso 1 1 calc R U . . .
C3 C -0.01294(15) 0.0249(5) 0.43715(15) 0.0500(10) Uani 1 1 d . . . . .
H3 H -0.035353 0.053668 0.457659 0.060 Uiso 1 1 calc R U . . .
C4 C -0.01693(16) -0.0999(5) 0.42087(16) 0.0551(11) Uani 1 1 d . . . . .
H4 H -0.041394 -0.156961 0.430325 0.066 Uiso 1 1 calc R U . . .
C5 C 0.01561(13) -0.1384(4) 0.39065(13) 0.0428(8) Uani 1 1 d . . . . .
H5 H 0.013029 -0.223006 0.378984 0.051 Uiso 1 1 calc R U . . .
C6 C 0.05214(12) -0.0570(4) 0.37672(11) 0.0333(7) Uani 1 1 d . . . . .
C7 C 0.08525(12) -0.1014(3) 0.34398(11) 0.0315(6) Uani 1 1 d . . . . .
C8 C 0.12517(14) -0.2515(4) 0.30870(12) 0.0383(7) Uani 1 1 d . . . . .
H8A H 0.113841 -0.308515 0.280814 0.046 Uiso 1 1 calc R U . . .
H8B H 0.155844 -0.289716 0.330676 0.046 Uiso 1 1 calc R U . . .
C9 C 0.13879(13) -0.1204(3) 0.29231(12) 0.0390(7) Uani 1 1 d . . . . .
H9 H 0.120172 -0.106660 0.258210 0.047 Uiso 1 1 calc R U . . .
C10 C 0.19766(15) -0.1001(4) 0.29637(14) 0.0502(9) Uani 1 1 d . . . . .
H10 H 0.215894 -0.115538 0.330467 0.060 Uiso 1 1 calc R U . . .
C11 C 0.21909(16) -0.1948(5) 0.26373(16) 0.0583(11) Uani 1 1 d . . . . .
H11A H 0.209370 -0.281187 0.271261 0.087 Uiso 1 1 calc R U . . .
H11B H 0.257659 -0.187792 0.269218 0.087 Uiso 1 1 calc R U . . .
H11C H 0.203888 -0.175853 0.229956 0.087 Uiso 1 1 calc R U . . .
C12 C 0.2091(2) 0.0343(5) 0.2829(2) 0.0752(16) Uani 1 1 d . . . . .
H12A H 0.189617 0.052572 0.250250 0.113 Uiso 1 1 calc R U . . .
H12B H 0.247107 0.043817 0.284111 0.113 Uiso 1 1 calc R U . . .
H12C H 0.198131 0.093503 0.305604 0.113 Uiso 1 1 calc R U . . .
C13 C 0.10026(12) 0.2762(3) 0.39976(11) 0.0323(7) Uani 1 1 d . . . . .
C14 C 0.07282(12) 0.3783(3) 0.37586(11) 0.0309(6) Uani 1 1 d . . . . .
C15 C 0.08282(12) 0.4994(3) 0.39528(12) 0.0341(7) Uani 1 1 d . . . . .
H15 H 0.064554 0.569753 0.378827 0.041 Uiso 1 1 calc R U . . .
C16 C 0.11905(13) 0.5197(3) 0.43833(11) 0.0341(7) Uani 1 1 d . . . . .
C17 C 0.14521(13) 0.4156(4) 0.46192(12) 0.0370(7) Uani 1 1 d . . . . .
H17 H 0.169469 0.427941 0.491532 0.044 Uiso 1 1 calc R U . . .
C18 C 0.13682(12) 0.2937(3) 0.44333(12) 0.0323(7) Uani 1 1 d . . . . .
C19 C 0.03429(12) 0.3569(3) 0.32783(11) 0.0330(7) Uani 1 1 d . . . . .
H19 H 0.020224 0.268959 0.329093 0.040 Uiso 1 1 calc R U . . .
C20 C -0.01286(12) 0.4448(3) 0.32285(11) 0.0326(7) Uani 1 1 d . . . . .
C21 C -0.05447(14) 0.4111(5) 0.34454(12) 0.0456(9) Uani 1 1 d . . . . .
H21 H -0.054684 0.329792 0.358901 0.055 Uiso 1 1 calc R U . . .
C22 C -0.09572(16) 0.4945(5) 0.34549(15) 0.0547(11) Uani 1 1 d . . . . .
H22 H -0.123906 0.470207 0.360478 0.066 Uiso 1 1 calc R U . . .
C23 C -0.09588(15) 0.6135(5) 0.32458(13) 0.0482(10) Uani 1 1 d . . . . .
H23 H -0.123554 0.671744 0.326060 0.058 Uiso 1 1 calc R U . . .
C24 C -0.05581(14) 0.6467(4) 0.30174(12) 0.0423(8) Uani 1 1 d . . . . .
H24 H -0.056310 0.727026 0.286550 0.051 Uiso 1 1 calc R U . . .
C25 C -0.01445(13) 0.5628(4) 0.30081(12) 0.0357(7) Uani 1 1 d . . . . .
H25 H 0.013060 0.586472 0.284881 0.043 Uiso 1 1 calc R U . . .
C26 C 0.06205(12) 0.3598(3) 0.28525(11) 0.0329(7) Uani 1 1 d . . . . .
C27 C 0.03575(14) 0.3137(4) 0.24080(12) 0.0396(8) Uani 1 1 d . . . . .
H27 H 0.000512 0.283801 0.237307 0.047 Uiso 1 1 calc R U . . .
C28 C 0.06028(16) 0.3108(4) 0.20149(13) 0.0445(9) Uani 1 1 d . . . . .
H28 H 0.041980 0.277544 0.171624 0.053 Uiso 1 1 calc R U . . .
C29 C 0.11155(16) 0.3564(4) 0.20574(14) 0.0484(9) Uani 1 1 d . . . . .
H29 H 0.128474 0.354370 0.178980 0.058 Uiso 1 1 calc R U . . .
C30 C 0.13749(15) 0.4048(4) 0.24944(14) 0.0461(9) Uani 1 1 d . . . . .
H30 H 0.172257 0.437555 0.252525 0.055 Uiso 1 1 calc R U . . .
C31 C 0.11324(13) 0.4060(4) 0.28887(13) 0.0408(8) Uani 1 1 d . . . . .
H31 H 0.131804 0.438736 0.318731 0.049 Uiso 1 1 calc R U . . .
C32 C 0.12821(14) 0.6518(4) 0.45861(13) 0.0437(9) Uani 1 1 d . . . . .
H32A H 0.154649 0.649106 0.488709 0.065 Uiso 1 1 calc R U . . .
H32B H 0.095002 0.685910 0.464934 0.065 Uiso 1 1 calc R U . . .
H32C H 0.140936 0.706293 0.435385 0.065 Uiso 1 1 calc R U . . .
C33 C 0.16654(13) 0.1773(3) 0.46757(12) 0.0357(7) Uani 1 1 d . . . . .
H33 H 0.140947 0.105097 0.461940 0.043 Uiso 1 1 calc R U . . .
C34 C 0.21235(14) 0.1400(4) 0.44443(12) 0.0387(8) Uani 1 1 d . . . . .
C35 C 0.24132(15) 0.2283(4) 0.42390(14) 0.0470(9) Uani 1 1 d . . . . .
H35 H 0.231855 0.315355 0.423260 0.056 Uiso 1 1 calc R U . . .
C36 C 0.28391(19) 0.1899(5) 0.40436(16) 0.0602(12) Uani 1 1 d . . . . .
H36 H 0.303075 0.251281 0.390367 0.072 Uiso 1 1 calc R U . . .
C37 C 0.2988(2) 0.0657(6) 0.40487(16) 0.0678(15) Uani 1 1 d . . . . .
H37 H 0.328226 0.040774 0.391729 0.081 Uiso 1 1 calc R U . . .
C38 C 0.2703(2) -0.0232(6) 0.42485(15) 0.0677(14) Uani 1 1 d . . . . .
H38 H 0.280078 -0.110033 0.425346 0.081 Uiso 1 1 calc R U . . .
C39 C 0.22755(18) 0.0136(4) 0.44411(14) 0.0518(10) Uani 1 1 d . . . . .
H39 H 0.208178 -0.048720 0.457415 0.062 Uiso 1 1 calc R U . . .
C40 C 0.18244(13) 0.1938(4) 0.52199(12) 0.0374(7) Uani 1 1 d . . . . .
C41 C 0.23138(16) 0.2369(4) 0.54483(13) 0.0453(9) Uani 1 1 d . . . . .
H41 H 0.256963 0.257435 0.526259 0.054 Uiso 1 1 calc R U . . .
C42 C 0.2441(2) 0.2508(5) 0.59453(15) 0.0649(13) Uani 1 1 d . . . . .
H42 H 0.277961 0.281536 0.609573 0.078 Uiso 1 1 calc R U . . .
C43 C 0.2080(3) 0.2205(6) 0.62175(16) 0.0755(17) Uani 1 1 d . . . . .
H43 H 0.216800 0.229206 0.655767 0.091 Uiso 1 1 calc R U . . .
C44 C 0.1592(2) 0.1778(8) 0.59990(18) 0.087(2) Uani 1 1 d . . . . .
H44 H 0.133798 0.158373 0.618739 0.105 Uiso 1 1 calc R U . . .
C45 C 0.14651(17) 0.1623(6) 0.55014(17) 0.0688(15) Uani 1 1 d . . . . .
H45 H 0.112833 0.129807 0.535419 0.083 Uiso 1 1 calc R U . . .
C51 C 0.43732(12) 0.7543(3) 0.60220(11) 0.0314(7) Uani 1 1 d . . . . .
C52 C 0.47436(13) 0.7160(4) 0.57500(12) 0.0366(7) Uani 1 1 d . . . . .
H52 H 0.474330 0.630947 0.564022 0.044 Uiso 1 1 calc R U . . .
C53 C 0.51074(15) 0.8009(5) 0.56412(14) 0.0472(10) Uani 1 1 d . . . . .
H53 H 0.535272 0.773170 0.545499 0.057 Uiso 1 1 calc R U . . .
C54 C 0.51248(15) 0.9249(4) 0.57953(15) 0.0480(9) Uani 1 1 d . . . . .
H54 H 0.538235 0.981623 0.572085 0.058 Uiso 1 1 calc R U . . .
C55 C 0.47625(13) 0.9657(4) 0.60595(13) 0.0394(8) Uani 1 1 d . . . . .
H55 H 0.477083 1.051280 0.616468 0.047 Uiso 1 1 calc R U . . .
C56 C 0.43827(12) 0.8829(3) 0.61752(11) 0.0308(6) Uani 1 1 d . . . . .
C57 C 0.39905(12) 0.9297(3) 0.64380(11) 0.0310(6) Uani 1 1 d . . . . .
C58 C 0.35999(14) 1.0769(4) 0.68121(14) 0.0440(8) Uani 1 1 d . . . . .
H58A H 0.336558 1.146267 0.666126 0.053 Uiso 1 1 calc R U . . .
H58B H 0.374850 1.099751 0.715091 0.053 Uiso 1 1 calc R U . . .
C59 C 0.32969(12) 0.9515(3) 0.67840(12) 0.0382(7) Uani 1 1 d . . . . .
H59 H 0.294529 0.962368 0.656359 0.046 Uiso 1 1 calc R U . . .
C60 C 0.32122(15) 0.9034(4) 0.72677(13) 0.0460(8) Uani 1 1 d . . . . .
H60 H 0.356345 0.898321 0.749285 0.055 Uiso 1 1 calc R U . . .
C61 C 0.28654(16) 0.9957(5) 0.74757(16) 0.0538(10) Uani 1 1 d . . . . .
H61A H 0.302842 1.079972 0.750284 0.081 Uiso 1 1 calc R U . . .
H61B H 0.282826 0.966545 0.779515 0.081 Uiso 1 1 calc R U . . .
H61C H 0.251607 1.000108 0.726318 0.081 Uiso 1 1 calc R U . . .
C62 C 0.2965(3) 0.7705(6) 0.7218(2) 0.0753(15) Uani 1 1 d . . . . .
H62A H 0.262955 0.772971 0.698370 0.113 Uiso 1 1 calc R U . . .
H62B H 0.290145 0.742662 0.753049 0.113 Uiso 1 1 calc R U . . .
H62C H 0.320671 0.711173 0.710684 0.113 Uiso 1 1 calc R U . . .
C63 C 0.39347(12) 0.5477(3) 0.59374(11) 0.0306(6) Uani 1 1 d . . . . .
C64 C 0.42084(12) 0.4439(3) 0.61826(11) 0.0310(7) Uani 1 1 d . . . . .
C65 C 0.41127(12) 0.3243(3) 0.59804(12) 0.0326(7) Uani 1 1 d . . . . .
H65 H 0.429282 0.253690 0.614505 0.039 Uiso 1 1 calc R U . . .
C66 C 0.37635(12) 0.3042(3) 0.55467(12) 0.0347(7) Uani 1 1 d . . . . .
C67 C 0.35038(12) 0.4084(3) 0.53082(12) 0.0347(7) Uani 1 1 d . . . . .
H67 H 0.326442 0.395992 0.501034 0.042 Uiso 1 1 calc R U . . .
C68 C 0.35853(13) 0.5307(3) 0.54946(12) 0.0340(7) Uani 1 1 d . . . . .
C69 C 0.45861(12) 0.4667(3) 0.66620(11) 0.0314(6) Uani 1 1 d . . . . .
H69 H 0.472443 0.554941 0.664950 0.038 Uiso 1 1 calc R U . . .
C70 C 0.43054(12) 0.4625(3) 0.70901(11) 0.0334(7) Uani 1 1 d . . . . .
C71 C 0.37925(13) 0.4180(4) 0.70483(12) 0.0393(8) Uani 1 1 d . . . . .
H71 H 0.360565 0.387086 0.674710 0.047 Uiso 1 1 calc R U . . .
C72 C 0.35503(14) 0.4181(5) 0.74430(13) 0.0466(9) Uani 1 1 d . . . . .
H72 H 0.320166 0.385943 0.741113 0.056 Uiso 1 1 calc R U . . .
C73 C 0.38110(15) 0.4645(4) 0.78788(13) 0.0458(9) Uani 1 1 d . . . . .
H73 H 0.364219 0.464832 0.814678 0.055 Uiso 1 1 calc R U . . .
C74 C 0.43185(16) 0.5106(4) 0.79270(13) 0.0446(9) Uani 1 1 d . . . . .
H74 H 0.449816 0.543521 0.822744 0.054 Uiso 1 1 calc R U . . .
C75 C 0.45666(14) 0.5090(4) 0.75370(12) 0.0391(8) Uani 1 1 d . . . . .
H75 H 0.491792 0.539732 0.757368 0.047 Uiso 1 1 calc R U . . .
C76 C 0.50628(12) 0.3787(3) 0.67226(11) 0.0326(7) Uani 1 1 d . . . . .
C77 C 0.50651(13) 0.2582(4) 0.69201(12) 0.0366(7) Uani 1 1 d . . . . .
H77 H 0.477599 0.231381 0.705554 0.044 Uiso 1 1 calc R U . . .
C78 C 0.54912(13) 0.1760(4) 0.69209(12) 0.0398(8) Uani 1 1 d . . . . .
H78 H 0.548566 0.092794 0.704802 0.048 Uiso 1 1 calc R U . . .
C79 C 0.59194(15) 0.2160(4) 0.67366(13) 0.0468(9) Uani 1 1 d . . . . .
H79 H 0.620772 0.160232 0.673550 0.056 Uiso 1 1 calc R U . . .
C80 C 0.59276(15) 0.3371(5) 0.65543(14) 0.0503(10) Uani 1 1 d . . . . .
H80 H 0.622540 0.365240 0.643426 0.060 Uiso 1 1 calc R U . . .
C81 C 0.55032(13) 0.4175(4) 0.65458(12) 0.0411(8) Uani 1 1 d . . . . .
H81 H 0.551182 0.500497 0.641759 0.049 Uiso 1 1 calc R U . . .
C82 C 0.36764(15) 0.1720(4) 0.53384(14) 0.0451(9) Uani 1 1 d . . . . .
H82A H 0.349721 0.177382 0.499980 0.068 Uiso 1 1 calc R U . . .
H82B H 0.345755 0.123537 0.551866 0.068 Uiso 1 1 calc R U . . .
H82C H 0.401805 0.129635 0.536188 0.068 Uiso 1 1 calc R U . . .
C83 C 0.32925(13) 0.6447(4) 0.52481(12) 0.0384(8) Uani 1 1 d . . . . .
H83 H 0.355019 0.716532 0.530582 0.046 Uiso 1 1 calc R U . . .
C84 C 0.31378(13) 0.6302(4) 0.47040(12) 0.0386(8) Uani 1 1 d . . . . .
C85 C 0.35064(17) 0.6534(5) 0.44240(17) 0.0614(12) Uani 1 1 d . . . . .
H85 H 0.384994 0.680856 0.457536 0.074 Uiso 1 1 calc R U . . .
C86 C 0.3391(2) 0.6378(6) 0.39291(19) 0.0764(16) Uani 1 1 d . . . . .
H86 H 0.365186 0.654616 0.374498 0.092 Uiso 1 1 calc R U . . .
C87 C 0.2893(2) 0.5976(6) 0.37050(15) 0.0692(15) Uani 1 1 d . . . . .
H87 H 0.280933 0.586331 0.336579 0.083 Uiso 1 1 calc R U . . .
C88 C 0.25212(19) 0.5740(5) 0.39763(14) 0.0546(10) Uani 1 1 d . . . . .
H88 H 0.217820 0.546113 0.382498 0.066 Uiso 1 1 calc R U . . .
C89 C 0.26440(14) 0.5907(4) 0.44697(13) 0.0423(8) Uani 1 1 d . . . . .
H89 H 0.238096 0.574458 0.465230 0.051 Uiso 1 1 calc R U . . .
C90 C 0.28319(14) 0.6845(4) 0.54785(12) 0.0403(8) Uani 1 1 d . . . . .
C91 C 0.26861(18) 0.8119(4) 0.54755(14) 0.0516(10) Uani 1 1 d . . . . .
H91 H 0.287878 0.873077 0.533567 0.062 Uiso 1 1 calc R U . . .
C92 C 0.2264(2) 0.8501(5) 0.56734(15) 0.0667(14) Uani 1 1 d . . . . .
H92 H 0.217043 0.937244 0.566773 0.080 Uiso 1 1 calc R U . . .
C93 C 0.1984(2) 0.7645(7) 0.58754(16) 0.0732(16) Uani 1 1 d . . . . .
H93 H 0.169458 0.791568 0.600955 0.088 Uiso 1 1 calc R U . . .
C94 C 0.2120(2) 0.6382(6) 0.58859(16) 0.0683(15) Uani 1 1 d . . . . .
H94 H 0.192508 0.578240 0.602928 0.082 Uiso 1 1 calc R U . . .
C95 C 0.25453(15) 0.5978(4) 0.56856(14) 0.0482(9) Uani 1 1 d . . . . .
H95 H 0.263664 0.510547 0.569228 0.058 Uiso 1 1 calc R U . . .
C101 C -0.0044(3) 0.4627(8) 0.5186(3) 0.0484(18) Uani 0.5 1 d D . P A -1
H101 H -0.027300 0.433931 0.541041 0.058 Uiso 0.5 1 calc R U P A -1
Cl1 Cl -0.03974(14) 0.4543(5) 0.46018(11) 0.1033(13) Uani 0.5 1 d D . P A -1
Cl2 Cl 0.01433(13) 0.6216(3) 0.53160(13) 0.0842(8) Uani 0.5 1 d D . P A -1
Cl3 Cl 0.05200(9) 0.3677(2) 0.52665(7) 0.0520(5) Uani 0.5 1 d D . P A -1
C102 C 0.5058(3) 0.3591(9) 0.4830(3) 0.052(2) Uani 0.5 1 d D . P B -1
H102 H 0.529708 0.388772 0.461591 0.063 Uiso 0.5 1 calc R U P B -1
Cl4 Cl 0.54008(12) 0.3697(5) 0.54258(9) 0.0933(11) Uani 0.5 1 d D . P B -1
Cl5 Cl 0.44995(8) 0.4591(2) 0.47395(7) 0.0518(5) Uani 0.5 1 d D . P B -1
Cl6 Cl 0.48822(12) 0.2048(3) 0.46817(12) 0.0774(7) Uani 0.5 1 d D . P B -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 O1 C8 104.7(3) . . ?
C57 O2 C58 105.9(3) . . ?
C1 N1 C13 122.5(3) . . ?
C7 N2 C9 106.9(3) . . ?
C51 N3 C63 122.2(3) . . ?
C57 N4 C59 108.0(3) . . ?
N1 C1 C2 121.0(3) . . ?
N1 C1 C6 121.3(3) . . ?
C2 C1 C6 117.7(3) . . ?
C3 C2 C1 121.1(4) . . ?
C2 C3 C4 121.1(4) . . ?
C5 C4 C3 118.1(4) . . ?
C4 C5 C6 122.0(4) . . ?
C5 C6 C1 119.9(3) . . ?
C5 C6 C7 120.0(3) . . ?
C1 C6 C7 120.0(3) . . ?
N2 C7 O1 117.3(3) . . ?
N2 C7 C6 126.9(3) . . ?
O1 C7 C6 115.9(3) . . ?
O1 C8 C9 104.0(3) . . ?
N2 C9 C10 112.4(3) . . ?
N2 C9 C8 102.9(3) . . ?
C10 C9 C8 113.3(3) . . ?
C12 C10 C9 111.0(4) . . ?
C12 C10 C11 110.1(4) . . ?
C9 C10 C11 109.8(3) . . ?
C14 C13 C18 120.8(3) . . ?
C14 C13 N1 119.7(3) . . ?
C18 C13 N1 119.4(3) . . ?
C13 C14 C15 118.8(3) . . ?
C13 C14 C19 119.7(3) . . ?
C15 C14 C19 121.4(3) . . ?
C14 C15 C16 121.6(3) . . ?
C17 C16 C15 118.3(3) . . ?
C17 C16 C32 121.6(3) . . ?
C15 C16 C32 120.1(3) . . ?
C16 C17 C18 121.7(3) . . ?
C17 C18 C13 118.7(3) . . ?
C17 C18 C33 123.0(3) . . ?
C13 C18 C33 118.3(3) . . ?
C20 C19 C26 114.4(3) . . ?
C20 C19 C14 111.0(3) . . ?
C26 C19 C14 112.1(3) . . ?
C21 C20 C25 118.3(3) . . ?
C21 C20 C19 118.8(3) . . ?
C25 C20 C19 122.7(3) . . ?
C22 C21 C20 120.9(4) . . ?
C21 C22 C23 120.1(4) . . ?
C24 C23 C22 119.6(4) . . ?
C23 C24 C25 120.2(4) . . ?
C20 C25 C24 120.9(3) . . ?
C27 C26 C31 118.1(3) . . ?
C27 C26 C19 119.2(3) . . ?
C31 C26 C19 122.7(3) . . ?
C28 C27 C26 121.0(3) . . ?
C27 C28 C29 120.2(3) . . ?
C30 C29 C28 119.1(3) . . ?
C29 C30 C31 120.7(4) . . ?
C30 C31 C26 120.9(3) . . ?
C34 C33 C40 113.2(3) . . ?
C34 C33 C18 112.1(3) . . ?
C40 C33 C18 111.7(3) . . ?
C39 C34 C35 117.5(4) . . ?
C39 C34 C33 119.8(4) . . ?
C35 C34 C33 122.7(3) . . ?
C36 C35 C34 120.5(4) . . ?
C37 C36 C35 121.3(5) . . ?
C36 C37 C38 118.9(4) . . ?
C39 C38 C37 120.4(5) . . ?
C38 C39 C34 121.4(5) . . ?
C41 C40 C45 117.9(4) . . ?
C41 C40 C33 123.2(3) . . ?
C45 C40 C33 118.9(3) . . ?
C40 C41 C42 121.2(4) . . ?
C43 C42 C41 120.1(5) . . ?
C42 C43 C44 119.7(4) . . ?
C43 C44 C45 120.4(5) . . ?
C40 C45 C44 120.6(5) . . ?
N3 C51 C52 121.6(3) . . ?
N3 C51 C56 120.3(3) . . ?
C52 C51 C56 118.0(3) . . ?
C53 C52 C51 120.5(4) . . ?
C54 C53 C52 121.8(4) . . ?
C53 C54 C55 119.1(4) . . ?
C54 C55 C56 121.1(4) . . ?
C55 C56 C51 119.5(3) . . ?
C55 C56 C57 120.0(3) . . ?
C51 C56 C57 120.5(3) . . ?
N4 C57 O2 117.4(3) . . ?
N4 C57 C56 126.3(3) . . ?
O2 C57 C56 116.3(3) . . ?
O2 C58 C59 104.9(3) . . ?
N4 C59 C60 112.6(3) . . ?
N4 C59 C58 103.3(3) . . ?
C60 C59 C58 114.0(3) . . ?
C59 C60 C61 109.9(3) . . ?
C59 C60 C62 110.8(3) . . ?
C61 C60 C62 110.7(4) . . ?
C68 C63 C64 120.7(3) . . ?
C68 C63 N3 119.6(3) . . ?
C64 C63 N3 119.7(3) . . ?
C65 C64 C63 118.2(3) . . ?
C65 C64 C69 122.7(3) . . ?
C63 C64 C69 119.0(3) . . ?
C66 C65 C64 122.4(3) . . ?
C65 C66 C67 118.3(3) . . ?
C65 C66 C82 120.4(3) . . ?
C67 C66 C82 121.3(3) . . ?
C66 C67 C68 121.8(3) . . ?
C67 C68 C63 118.6(3) . . ?
C67 C68 C83 122.5(3) . . ?
C63 C68 C83 118.9(3) . . ?
C64 C69 C76 111.2(3) . . ?
C64 C69 C70 112.4(2) . . ?
C76 C69 C70 113.2(3) . . ?
C71 C70 C75 118.2(3) . . ?
C71 C70 C69 122.5(3) . . ?
C75 C70 C69 119.2(3) . . ?
C70 C71 C72 120.6(3) . . ?
C73 C72 C71 120.5(4) . . ?
C72 C73 C74 119.9(3) . . ?
C73 C74 C75 120.0(3) . . ?
C74 C75 C70 120.8(3) . . ?
C77 C76 C81 118.5(3) . . ?
C77 C76 C69 122.7(3) . . ?
C81 C76 C69 118.7(3) . . ?
C76 C77 C78 120.4(3) . . ?
C79 C78 C77 119.9(4) . . ?
C80 C79 C78 119.9(4) . . ?
C79 C80 C81 120.1(4) . . ?
C80 C81 C76 121.0(4) . . ?
C68 C83 C84 113.1(3) . . ?
C68 C83 C90 112.4(3) . . ?
C84 C83 C90 113.2(3) . . ?
C89 C84 C85 117.1(4) . . ?
C89 C84 C83 123.2(3) . . ?
C85 C84 C83 119.7(3) . . ?
C84 C85 C86 122.0(4) . . ?
C87 C86 C85 119.5(4) . . ?
C88 C87 C86 119.4(4) . . ?
C87 C88 C89 120.2(4) . . ?
C84 C89 C88 121.8(4) . . ?
C95 C90 C91 118.2(4) . . ?
C95 C90 C83 122.1(4) . . ?
C91 C90 C83 119.7(4) . . ?
C92 C91 C90 120.8(5) . . ?
C93 C92 C91 120.6(5) . . ?
C92 C93 C94 119.9(5) . . ?
C93 C94 C95 120.2(5) . . ?
C90 C95 C94 120.2(5) . . ?
Cl1 C101 Cl3 111.2(4) . . ?
Cl1 C101 Cl2 108.6(5) . . ?
Cl3 C101 Cl2 109.4(4) . . ?
Cl6 C102 Cl4 110.8(5) . . ?
Cl6 C102 Cl5 111.3(5) . . ?
Cl4 C102 Cl5 110.0(4) . . ?
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
O1 C7 1.371(4) . ?
O1 C8 1.451(4) . ?
O2 C57 1.352(4) . ?
O2 C58 1.445(4) . ?
N1 C1 1.367(4) . ?
N1 C13 1.430(5) . ?
N2 C7 1.276(4) . ?
N2 C9 1.483(4) . ?
N3 C51 1.371(4) . ?
N3 C63 1.423(4) . ?
N4 C57 1.278(4) . ?
N4 C59 1.467(4) . ?
C1 C2 1.405(5) . ?
C1 C6 1.406(5) . ?
C2 C3 1.377(6) . ?
C3 C4 1.393(7) . ?
C4 C5 1.378(5) . ?
C5 C6 1.391(5) . ?
C6 C7 1.462(4) . ?
C8 C9 1.522(5) . ?
C9 C10 1.518(5) . ?
C10 C12 1.513(7) . ?
C10 C11 1.540(6) . ?
C13 C14 1.389(5) . ?
C13 C18 1.408(4) . ?
C14 C15 1.395(5) . ?
C14 C19 1.533(4) . ?
C15 C16 1.397(4) . ?
C16 C17 1.389(5) . ?
C16 C32 1.508(5) . ?
C17 C18 1.390(5) . ?
C18 C33 1.535(5) . ?
C19 C20 1.515(4) . ?
C19 C26 1.525(5) . ?
C20 C21 1.389(5) . ?
C20 C25 1.390(5) . ?
C21 C22 1.387(6) . ?
C22 C23 1.388(7) . ?
C23 C24 1.373(6) . ?
C24 C25 1.392(5) . ?
C26 C27 1.394(4) . ?
C26 C31 1.394(5) . ?
C27 C28 1.390(5) . ?
C28 C29 1.392(6) . ?
C29 C30 1.382(6) . ?
C30 C31 1.389(5) . ?
C33 C34 1.517(5) . ?
C33 C40 1.525(5) . ?
C34 C39 1.390(6) . ?
C34 C35 1.394(6) . ?
C35 C36 1.389(6) . ?
C36 C37 1.364(8) . ?
C37 C38 1.383(8) . ?
C38 C39 1.383(7) . ?
C40 C41 1.376(5) . ?
C40 C45 1.382(6) . ?
C41 C42 1.389(5) . ?
C42 C43 1.363(8) . ?
C43 C44 1.364(9) . ?
C44 C45 1.392(7) . ?
C51 C52 1.405(5) . ?
C51 C56 1.423(5) . ?
C52 C53 1.378(5) . ?
C53 C54 1.377(6) . ?
C54 C55 1.381(5) . ?
C55 C56 1.402(5) . ?
C56 C57 1.461(5) . ?
C58 C59 1.531(5) . ?
C59 C60 1.520(5) . ?
C60 C61 1.521(5) . ?
C60 C62 1.535(7) . ?
C63 C68 1.402(4) . ?
C63 C64 1.408(4) . ?
C64 C65 1.387(5) . ?
C64 C69 1.524(4) . ?
C65 C66 1.387(4) . ?
C66 C67 1.391(5) . ?
C66 C82 1.513(5) . ?
C67 C68 1.394(5) . ?
C68 C83 1.515(5) . ?
C69 C76 1.525(4) . ?
C69 C70 1.536(4) . ?
C70 C71 1.389(5) . ?
C70 C75 1.399(5) . ?
C71 C72 1.389(5) . ?
C72 C73 1.373(5) . ?
C73 C74 1.380(6) . ?
C74 C75 1.387(5) . ?
C76 C77 1.389(5) . ?
C76 C81 1.395(5) . ?
C77 C78 1.402(5) . ?
C78 C79 1.382(6) . ?
C79 C80 1.380(7) . ?
C80 C81 1.383(5) . ?
C83 C84 1.522(5) . ?
C83 C90 1.528(5) . ?
C84 C89 1.379(5) . ?
C84 C85 1.380(5) . ?
C85 C86 1.385(7) . ?
C86 C87 1.381(8) . ?
C87 C88 1.370(7) . ?
C88 C89 1.383(5) . ?
C90 C95 1.381(6) . ?
C90 C91 1.395(6) . ?
C91 C92 1.383(7) . ?
C92 C93 1.355(9) . ?
C93 C94 1.377(9) . ?
C94 C95 1.402(6) . ?
C101 Cl1 1.726(8) . ?
C101 Cl3 1.745(8) . ?
C101 Cl2 1.763(8) . ?
C102 Cl6 1.719(9) . ?
C102 Cl4 1.746(7) . ?
C102 Cl5 1.764(8) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1N N2 0.92(4) 1.94(5) 2.676(4) 136(4) . yes
N3 H3N N4 0.89(5) 1.96(5) 2.665(4) 135(4) . yes
