# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_dv217
_database_code_depnum_ccdc_archive 'CCDC 1471555'
_audit_update_record             
;
2016-03-31 deposited with the CCDC.
2016-12-13 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H134 Al2 F12 N4 O19 S4'
_chemical_formula_iupac          ?
_chemical_formula_weight         2058.26

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.7628(8)
_cell_length_b                   27.367(2)
_cell_length_c                   19.2292(14)
_cell_angle_alpha                90
_cell_angle_beta                 101.133(3)
_cell_angle_gamma                90
_cell_volume                     5040.9(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3929
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      21.49
_cell_measurement_temperature    153.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2176

_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.97

_exptl_special_details           
;
;

_diffrn_ambient_temperature      153.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            60773
_diffrn_reflns_av_R_equivalents  0.1503
_diffrn_reflns_av_unetI/netI     0.1278
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_full        26.48
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24

_refine_special_details          
;
;

_reflns_number_total             10354
_reflns_number_gt                5464
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1876
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.039
_refine_ls_number_reflns         10354
_refine_ls_number_parameters     648
_refine_ls_number_restraints     155
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0729P)²+3.1400P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.537
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2014)'
_computing_structure_solution    'SHELXT (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al Al1 0.84143(12) 0.17706(4) 0.67995(6) 0.0182(3) Uani d . . . 1 . .
C C1 0.6978(4) 0.15050(14) 0.59633(19) 0.0202(9) Uani d . . . 1 . .
C C2 0.6262(4) 0.18957(13) 0.5570(2) 0.0204(9) Uani d . . . 1 . .
C C3 0.5272(4) 0.18357(14) 0.49515(19) 0.0243(9) Uani d . . . 1 . .
H H3 0.4823 0.2111 0.4707 0.029 Uiso calc U . R 1 . .
C C4 0.4947(4) 0.13660(14) 0.4696(2) 0.0264(10) Uani d . . . 1 . .
H H4 0.4299 0.1317 0.4265 0.032 Uiso calc U . R 1 . .
C C5 0.5575(4) 0.09767(14) 0.5074(2) 0.0252(9) Uani d . . . 1 . .
H H5 0.534 0.0656 0.4904 0.03 Uiso calc U . R 1 . .
C C6 0.6552(4) 0.10365(13) 0.57019(19) 0.0200(9) Uani d . . . 1 . .
C C7 0.6577(4) 0.23843(14) 0.5856(2) 0.0228(9) Uani d . . . 1 . .
H H7 0.6114 0.2659 0.5616 0.027 Uiso calc U . R 1 . .
C C8 0.7702(4) 0.29505(14) 0.6677(2) 0.0239(9) Uani d . . . 1 . .
C C9 0.7008(4) 0.31173(14) 0.7210(2) 0.0268(10) Uani d . . . 1 . .
C C10 0.5949(5) 0.28011(15) 0.7486(2) 0.0304(10) Uani d . . . 1 . .
H H10 0.6243 0.2452 0.7462 0.037 Uiso calc U . R 1 . .
C C11 0.5850(5) 0.29120(17) 0.8254(2) 0.0398(12) Uani d . . . 1 . .
H H11A 0.5442 0.3237 0.8281 0.06 Uiso calc U . R 1 . .
H H11B 0.6785 0.2904 0.8552 0.06 Uiso calc U . R 1 . .
H H11C 0.5259 0.2667 0.8422 0.06 Uiso calc U . R 1 . .
C C12 0.4497(5) 0.28568(17) 0.7009(3) 0.0420(12) Uani d . . . 1 . .
H H12A 0.3825 0.265 0.719 0.063 Uiso calc U . R 1 . .
H H12B 0.4542 0.2757 0.6524 0.063 Uiso calc U . R 1 . .
H H12C 0.42 0.3199 0.7008 0.063 Uiso calc U . R 1 . .
C C13 0.7249(5) 0.35953(15) 0.7442(2) 0.0343(11) Uani d . . . 1 . .
H H13 0.679 0.3717 0.7799 0.041 Uiso calc U . R 1 . .
C C14 0.8144(5) 0.38975(16) 0.7165(2) 0.0388(12) Uani d . . . 1 . .
H H14 0.8309 0.4221 0.734 0.047 Uiso calc U . R 1 . .
C C15 0.8794(5) 0.37315(15) 0.6639(2) 0.0343(11) Uani d . . . 1 . .
H H15 0.9383 0.3946 0.6443 0.041 Uiso calc U . R 1 . .
C C16 0.8607(4) 0.32520(14) 0.6384(2) 0.0268(10) Uani d . . . 1 . .
C C17 0.9325(5) 0.30853(15) 0.5792(2) 0.0308(10) Uani d . . . 1 . .
H H17 0.9355 0.272 0.5804 0.037 Uiso calc U . R 1 . .
C C18 0.8513(5) 0.32366(18) 0.5070(2) 0.0461(13) Uani d . . . 1 . .
H H18A 0.755 0.3118 0.5013 0.069 Uiso calc U . R 1 . .
H H18B 0.8952 0.3095 0.4699 0.069 Uiso calc U . R 1 . .
H H18C 0.8511 0.3594 0.5032 0.069 Uiso calc U . R 1 . .
C C19 1.0836(5) 0.32687(16) 0.5886(2) 0.0368(11) Uani d . . . 1 . .
H H19A 1.0836 0.362 0.5789 0.055 Uiso calc U . R 1 . .
H H19B 1.1314 0.3096 0.5555 0.055 Uiso calc U . R 1 . .
H H19C 1.1323 0.3207 0.6373 0.055 Uiso calc U . R 1 . .
C C20 0.7033(4) 0.05967(14) 0.6123(2) 0.0204(9) Uani d . . . 1 . .
H H20 0.772 0.0632 0.6543 0.024 Uiso calc U . R 1 . .
C C21 0.7002(4) -0.02331(13) 0.6403(2) 0.0232(9) Uani d . . . 1 . .
C C22 0.6272(4) -0.03372(14) 0.6953(2) 0.0254(9) Uani d . . . 1 . .
C C23 0.5082(4) -0.00092(15) 0.7083(2) 0.0300(10) Uani d . . . 1 . .
H H23 0.5322 0.0335 0.6978 0.036 Uiso calc U . R 1 . .
C C24 0.3750(5) -0.01419(18) 0.6583(2) 0.0438(13) Uani d . . . 1 . .
H H24A 0.3892 -0.0118 0.6093 0.066 Uiso calc U . R 1 . .
H H24B 0.3006 0.0083 0.6652 0.066 Uiso calc U . R 1 . .
H H24C 0.3486 -0.0477 0.6678 0.066 Uiso calc U . R 1 . .
C C25 0.4863(5) -0.00260(18) 0.7854(2) 0.0440(13) Uani d . . . 1 . .
H H25A 0.4196 0.0228 0.7925 0.066 Uiso calc U . R 1 . .
H H25B 0.5756 0.0031 0.8176 0.066 Uiso calc U . R 1 . .
H H25C 0.4498 -0.0347 0.795 0.066 Uiso calc U . R 1 . .
C C26 0.6644(4) -0.07548(15) 0.7348(2) 0.0304(10) Uani d . . . 1 . .
H H26 0.6165 -0.0833 0.7719 0.036 Uiso calc U . R 1 . .
C C27 0.7685(4) -0.10617(15) 0.7221(2) 0.0322(11) Uani d . . . 1 . .
H H27 0.7905 -0.135 0.7495 0.039 Uiso calc U . R 1 . .
C C28 0.8410(4) -0.09457(14) 0.6690(2) 0.0268(10) Uani d . . . 1 . .
H H28 0.9138 -0.1155 0.6608 0.032 Uiso calc U . R 1 . .
C C29 0.8097(4) -0.05305(14) 0.6274(2) 0.0232(9) Uani d . . . 1 . .
C C30 0.8870(4) -0.04059(15) 0.5683(2) 0.0277(10) Uani d . . . 1 . .
H H30 0.8968 -0.0042 0.5676 0.033 Uiso calc U . R 1 . .
C C31 1.0341(5) -0.06217(16) 0.5793(2) 0.0352(11) Uani d . . . 1 . .
H H31A 1.085 -0.054 0.6269 0.053 Uiso calc U . R 1 . .
H H31B 1.0836 -0.0486 0.5439 0.053 Uiso calc U . R 1 . .
H H31C 1.0281 -0.0978 0.574 0.053 Uiso calc U . R 1 . .
C C32 0.8008(5) -0.05577(17) 0.4967(2) 0.0370(11) Uani d . . . 1 . .
H H32A 0.7861 -0.0912 0.4962 0.056 Uiso calc U . R 1 . .
H H32B 0.8506 -0.0468 0.459 0.056 Uiso calc U . R 1 . .
H H32C 0.7103 -0.0391 0.4891 0.056 Uiso calc U . R 1 . .
C C33 1.1565(5) 0.21816(16) 0.8586(2) 0.0329(11) Uani d . . . 1 . .
C C34 1.0280(5) 0.04648(16) 0.7960(2) 0.0365(11) Uani d . . . 1 . .
C C35 0.9723(5) 0.16689(16) 0.54805(19) 0.0287(10) Uani d . . . 1 . .
H H35A 0.883 0.1773 0.5181 0.034 Uiso calc U . R 1 . .
H H35B 0.9777 0.1308 0.5476 0.034 Uiso calc U . R 1 . .
C C36 1.0946(5) 0.18934(16) 0.5227(2) 0.0332(11) Uani d . . . 1 . .
H H36A 1.0738 0.2232 0.506 0.04 Uiso calc U . R 1 . .
H H36B 1.121 0.1698 0.484 0.04 Uiso calc U . R 1 . .
C C37 1.2081(5) 0.18819(17) 0.5884(2) 0.0368(12) Uani d . . . 1 . .
H H37A 1.2822 0.2123 0.5852 0.044 Uiso calc U . R 1 . .
H H37B 1.2505 0.1553 0.596 0.044 Uiso calc U . R 1 . .
C C38 1.1308(4) 0.20147(15) 0.6475(2) 0.0271(10) Uani d . . . 1 . .
H H38A 1.1716 0.1842 0.6919 0.033 Uiso calc U . R 1 . .
H H38B 1.1351 0.2371 0.6565 0.033 Uiso calc U . R 1 . .
C C39 0.5683(4) 0.14937(15) 0.7256(2) 0.0251(9) Uani d . . . 1 . .
H H39A 0.5607 0.118 0.6994 0.03 Uiso calc U . R 1 . .
H H39B 0.5127 0.1744 0.6954 0.03 Uiso calc U . R 1 . .
C C40 0.5191(5) 0.14381(18) 0.7943(2) 0.0363(11) Uani d . . . 1 . .
H H40A 0.4432 0.1194 0.7903 0.044 Uiso calc U . R 1 . .
H H40B 0.4858 0.1753 0.8101 0.044 Uiso calc U . R 1 . .
C C41 0.6496(4) 0.12646(18) 0.8445(2) 0.0362(11) Uani d . . . 1 . .
H H41A 0.6423 0.1317 0.8946 0.043 Uiso calc U . R 1 . .
H H41B 0.668 0.0915 0.8371 0.043 Uiso calc U . R 1 . .
C C42 0.7608(4) 0.15866(16) 0.82355(19) 0.0280(10) Uani d . . . 1 . .
H H42A 0.7655 0.1906 0.848 0.034 Uiso calc U . R 1 . .
H H42B 0.8536 0.1428 0.8351 0.034 Uiso calc U . R 1 . .
F F1 1.2223(3) 0.24749(11) 0.91076(14) 0.0532(8) Uani d . . . 1 . .
F F2 1.2518(3) 0.20244(10) 0.82335(13) 0.0435(7) Uani d . . . 1 . .
F F3 1.1076(3) 0.18019(10) 0.88897(13) 0.0491(7) Uani d . . . 1 . .
F F4 1.1227(3) 0.01135(9) 0.80758(16) 0.0570(8) Uani d . . . 1 . .
F F5 1.0383(3) 0.07175(10) 0.85603(13) 0.0527(8) Uani d . . . 1 . .
F F6 0.9030(3) 0.02622(10) 0.78306(14) 0.0488(7) Uani d . . . 1 . .
N N1 0.7476(3) 0.24459(11) 0.64314(16) 0.0213(7) Uani d . . . 1 . .
N N2 0.6562(3) 0.01732(11) 0.59433(16) 0.0242(8) Uani d . . . 1 . .
O O1 0.9560(3) 0.21233(9) 0.75289(12) 0.0195(6) Uani d . . . 1 . .
O O2 1.0893(3) 0.28763(10) 0.76840(16) 0.0407(8) Uani d . . . 1 . .
O O3 0.9295(3) 0.26664(11) 0.84905(15) 0.0395(8) Uani d . . . 1 . .
O O4 0.9376(3) 0.11956(9) 0.72059(13) 0.0205(6) Uani d . . . 1 . .
O O5 1.1889(3) 0.10720(11) 0.74921(18) 0.0430(8) Uani d . . . 1 . .
O O6 1.0420(3) 0.05459(11) 0.66375(15) 0.0399(8) Uani d . . . 1 . .
O O7 0.9852(3) 0.18559(9) 0.62124(12) 0.0217(6) Uani d . . . 1 . .
O O8 0.7157(3) 0.16470(9) 0.74612(12) 0.0204(6) Uani d . . . 1 . .
S S1 1.01778(11) 0.25156(4) 0.80199(5) 0.0283(3) Uani d . . . 1 . .
S S2 1.05605(11) 0.08557(4) 0.72356(6) 0.0267(3) Uani d . . . 1 . .
O O9 0.4832(8) 0.14952(19) 0.0135(3) 0.132(2) Uani d U . D 1 . .
C C43 0.5070(10) 0.1129(3) 0.0668(4) 0.109(3) Uani d U . D 1 . .
H H43A 0.5984 0.1188 0.0983 0.131 Uiso calc U . R 1 . .
H H43B 0.4338 0.1151 0.0959 0.131 Uiso calc U . R 1 . .
C C44 0.5057(11) 0.0674(3) 0.0381(4) 0.134(3) Uani d U . D 1 . .
H H44A 0.4577 0.044 0.0645 0.161 Uiso calc U . R 1 . .
H H44B 0.6021 0.0557 0.0391 0.161 Uiso calc U . R 1 . .
C C45 0.4272(10) 0.0729(3) -0.0374(4) 0.126(3) Uani d U . D 1 . .
H H45A 0.4893 0.0685 -0.072 0.152 Uiso calc U . R 1 . .
H H45B 0.348 0.0498 -0.0484 0.152 Uiso calc U . R 1 . .
C C46 0.3791(9) 0.1241(4) -0.0355(4) 0.131(3) Uani d U . D 1 . .
H H46A 0.3677 0.139 -0.0831 0.157 Uiso calc U . R 1 . .
H H46B 0.2883 0.1253 -0.0199 0.157 Uiso calc U . R 1 . .
O O10 -0.086(2) 1.0218(7) 1.0058(11) 0.144(5) Uani d U P D 0.5 A -1
C C47 -0.098(2) 0.9782(9) 0.9651(14) 0.122(5) Uani d U P D 0.5 A -1
H H47A -0.164 0.9836 0.9198 0.146 Uiso calc U P R 0.5 A -1
H H47B -0.1357 0.9519 0.9912 0.146 Uiso calc U P R 0.5 A -1
C C48 0.034(2) 0.9633(6) 0.9506(8) 0.107(5) Uani d U P D 0.5 A -1
H H48A 0.0565 0.9802 0.9085 0.128 Uiso calc U P R 0.5 A -1
H H48B 0.0392 0.9275 0.9441 0.128 Uiso calc U P R 0.5 A -1
C C49 0.131(2) 0.9804(8) 1.0201(11) 0.114(5) Uani d U P D 0.5 A -1
H H49A 0.2274 0.9866 1.0131 0.136 Uiso calc U P R 0.5 A -1
H H49B 0.1334 0.9564 1.0588 0.136 Uiso calc U P R 0.5 A -1
C C50 0.055(2) 1.0286(8) 1.0342(13) 0.106(5) Uani d U P D 0.5 A -1
H H50A 0.0688 1.0351 1.0857 0.128 Uiso calc U P R 0.5 A -1
H H50B 0.0925 1.0567 1.0112 0.128 Uiso calc U P R 0.5 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 O1 . 1.882(3) ?
Al1 O4 . 1.920(3) ?
Al1 O8 . 1.960(3) ?
Al1 O7 . 1.977(3) ?
Al1 C1 . 2.052(4) ?
Al1 N1 . 2.122(3) ?
C1 C6 . 1.410(5) ?
C1 C2 . 1.414(5) ?
C2 C3 . 1.389(5) ?
C2 C7 . 1.457(5) ?
C3 C4 . 1.391(5) ?
C4 C5 . 1.366(5) ?
C5 C6 . 1.397(5) ?
C6 C20 . 1.476(5) ?
C7 N1 . 1.283(5) ?
C8 C16 . 1.404(5) ?
C8 C9 . 1.409(5) ?
C8 N1 . 1.462(5) ?
C9 C13 . 1.388(5) ?
C9 C10 . 1.520(6) ?
C10 C11 . 1.530(6) ?
C10 C12 . 1.540(6) ?
C13 C14 . 1.382(6) ?
C14 C15 . 1.371(6) ?
C15 C16 . 1.400(6) ?
C16 C17 . 1.518(6) ?
C17 C18 . 1.518(6) ?
C17 C19 . 1.536(6) ?
C20 N2 . 1.270(5) ?
C21 C29 . 1.404(5) ?
C21 C22 . 1.413(5) ?
C21 N2 . 1.434(5) ?
C22 C26 . 1.381(5) ?
C22 C23 . 1.527(6) ?
C23 C24 . 1.505(6) ?
C23 C25 . 1.537(6) ?
C26 C27 . 1.376(6) ?
C27 C28 . 1.387(6) ?
C28 C29 . 1.389(5) ?
C29 C30 . 1.519(5) ?
C30 C32 . 1.525(6) ?
C30 C31 . 1.530(6) ?
C33 F2 . 1.324(4) ?
C33 F3 . 1.325(5) ?
C33 F1 . 1.347(5) ?
C33 S1 . 1.812(5) ?
C34 F6 . 1.320(5) ?
C34 F4 . 1.323(5) ?
C34 F5 . 1.333(5) ?
C34 S2 . 1.818(5) ?
C35 O7 . 1.480(4) ?
C35 C36 . 1.505(6) ?
C36 C37 . 1.512(6) ?
C37 C38 . 1.524(5) ?
C38 O7 . 1.480(5) ?
C39 O8 . 1.478(4) ?
C39 C40 . 1.498(5) ?
C40 C41 . 1.518(6) ?
C41 C42 . 1.513(6) ?
C42 O8 . 1.478(4) ?
O1 S1 . 1.479(3) ?
O2 S1 . 1.433(3) ?
O3 S1 . 1.426(3) ?
O4 S2 . 1.477(3) ?
O5 S2 . 1.424(3) ?
O6 S2 . 1.414(3) ?
O9 C43 . 1.419(8) ?
O9 C46 . 1.427(10) ?
C43 C44 . 1.362(9) ?
C44 C45 . 1.514(10) ?
C45 C46 . 1.480(11) ?
O10 C50 . 1.391(9) ?
O10 C47 . 1.419(9) ?
C47 C48 . 1.431(13) ?
C48 C49 . 1.550(13) ?
C49 C50 . 1.564(13) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Al1 O4 . . 86.76(12) ?
O1 Al1 O8 . . 87.78(11) ?
O4 Al1 O8 . . 84.97(11) ?
O1 Al1 O7 . . 88.84(11) ?
O4 Al1 O7 . . 89.09(11) ?
O8 Al1 O7 . . 173.33(12) ?
O1 Al1 C1 . . 169.54(14) ?
O4 Al1 C1 . . 103.60(14) ?
O8 Al1 C1 . . 91.64(13) ?
O7 Al1 C1 . . 92.72(13) ?
O1 Al1 N1 . . 87.61(12) ?
O4 Al1 N1 . . 174.36(13) ?
O8 Al1 N1 . . 94.74(12) ?
O7 Al1 N1 . . 90.87(12) ?
C1 Al1 N1 . . 82.03(14) ?
C6 C1 C2 . . 114.5(3) ?
C6 C1 Al1 . . 135.3(3) ?
C2 C1 Al1 . . 110.1(3) ?
C3 C2 C1 . . 124.0(3) ?
C3 C2 C7 . . 119.6(4) ?
C1 C2 C7 . . 116.4(3) ?
C2 C3 C4 . . 119.0(4) ?
C5 C4 C3 . . 119.0(4) ?
C4 C5 C6 . . 122.0(4) ?
C5 C6 C1 . . 121.3(3) ?
C5 C6 C20 . . 118.1(3) ?
C1 C6 C20 . . 120.3(3) ?
N1 C7 C2 . . 120.4(4) ?
C16 C8 C9 . . 121.9(4) ?
C16 C8 N1 . . 119.6(3) ?
C9 C8 N1 . . 118.5(3) ?
C13 C9 C8 . . 117.6(4) ?
C13 C9 C10 . . 120.6(4) ?
C8 C9 C10 . . 121.6(3) ?
C9 C10 C11 . . 113.5(4) ?
C9 C10 C12 . . 110.2(4) ?
C11 C10 C12 . . 109.4(4) ?
C14 C13 C9 . . 121.4(4) ?
C15 C14 C13 . . 120.2(4) ?
C14 C15 C16 . . 121.4(4) ?
C15 C16 C8 . . 117.4(4) ?
C15 C16 C17 . . 119.8(4) ?
C8 C16 C17 . . 122.8(4) ?
C18 C17 C16 . . 111.6(4) ?
C18 C17 C19 . . 109.8(3) ?
C16 C17 C19 . . 112.7(3) ?
N2 C20 C6 . . 122.3(4) ?
C29 C21 C22 . . 121.8(4) ?
C29 C21 N2 . . 119.2(3) ?
C22 C21 N2 . . 118.9(3) ?
C26 C22 C21 . . 117.4(4) ?
C26 C22 C23 . . 121.6(4) ?
C21 C22 C23 . . 120.9(3) ?
C24 C23 C22 . . 110.1(3) ?
C24 C23 C25 . . 110.2(4) ?
C22 C23 C25 . . 113.1(4) ?
C27 C26 C22 . . 122.2(4) ?
C26 C27 C28 . . 119.3(4) ?
C27 C28 C29 . . 121.6(4) ?
C28 C29 C21 . . 117.5(4) ?
C28 C29 C30 . . 121.9(4) ?
C21 C29 C30 . . 120.5(3) ?
C29 C30 C32 . . 110.3(3) ?
C29 C30 C31 . . 113.5(3) ?
C32 C30 C31 . . 111.1(3) ?
F2 C33 F3 . . 108.6(4) ?
F2 C33 F1 . . 107.1(3) ?
F3 C33 F1 . . 107.4(3) ?
F2 C33 S1 . . 111.9(3) ?
F3 C33 S1 . . 111.7(3) ?
F1 C33 S1 . . 109.9(3) ?
F6 C34 F4 . . 108.5(4) ?
F6 C34 F5 . . 107.1(4) ?
F4 C34 F5 . . 107.3(4) ?
F6 C34 S2 . . 111.9(3) ?
F4 C34 S2 . . 110.7(3) ?
F5 C34 S2 . . 111.2(3) ?
O7 C35 C36 . . 103.9(3) ?
C35 C36 C37 . . 102.7(3) ?
C36 C37 C38 . . 103.3(3) ?
O7 C38 C37 . . 104.9(3) ?
O8 C39 C40 . . 104.8(3) ?
C39 C40 C41 . . 102.7(3) ?
C42 C41 C40 . . 101.9(3) ?
O8 C42 C41 . . 104.1(3) ?
C7 N1 C8 . . 115.9(3) ?
C7 N1 Al1 . . 110.6(3) ?
C8 N1 Al1 . . 133.3(3) ?
C20 N2 C21 . . 119.3(3) ?
S1 O1 Al1 . . 163.34(18) ?
S2 O4 Al1 . . 148.19(17) ?
C38 O7 C35 . . 109.0(3) ?
C38 O7 Al1 . . 125.5(2) ?
C35 O7 Al1 . . 124.3(2) ?
C39 O8 C42 . . 108.8(3) ?
C39 O8 Al1 . . 125.1(2) ?
C42 O8 Al1 . . 124.8(2) ?
O3 S1 O2 . . 119.58(19) ?
O3 S1 O1 . . 113.16(17) ?
O2 S1 O1 . . 112.72(16) ?
O3 S1 C33 . . 103.75(18) ?
O2 S1 C33 . . 104.2(2) ?
O1 S1 C33 . . 100.52(18) ?
O6 S2 O5 . . 118.0(2) ?
O6 S2 O4 . . 113.22(17) ?
O5 S2 O4 . . 113.92(17) ?
O6 S2 C34 . . 105.4(2) ?
O5 S2 C34 . . 103.9(2) ?
O4 S2 C34 . . 99.65(18) ?
C43 O9 C46 . . 97.4(6) ?
C44 C43 O9 . . 111.5(7) ?
C43 C44 C45 . . 105.1(7) ?
C46 C45 C44 . . 100.1(7) ?
O9 C46 C45 . . 106.8(7) ?
C50 O10 C47 . . 107.5(11) ?
O10 C47 C48 . . 111.4(13) ?
C47 C48 C49 . . 99.7(14) ?
C48 C49 C50 . . 100.0(13) ?
O10 C50 C49 . . 106.5(11) ?


# start Validation Reply Form
_vrf_PLAT411_dv217               
;
PROBLEM: Short Inter H...H Contact  H15    ..  H48B    ..       1.97 Ang.  
RESPONSE: This is due to disorder of the solvent molecule.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1471553'
_audit_update_record             
;
2016-03-31 deposited with the CCDC.
2016-12-13 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H39 Al Cl2 N2'
_chemical_formula_iupac          ?
_chemical_formula_weight         549.53

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_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                   9.5076(11)
_cell_length_b                   25.913(3)
_cell_length_c                   12.6579(12)
_cell_angle_alpha                90
_cell_angle_beta                 98.541(4)
_cell_angle_gamma                90
_cell_volume                     3083.9(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6751
_cell_measurement_theta_min      2.2623
_cell_measurement_theta_max      23.1226
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168

_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_T_max  0.95

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            53249
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_full        26.48
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15

_refine_special_details          
;
;

_reflns_number_total             6341
_reflns_number_gt                4631
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0928
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_number_reflns         6341
_refine_ls_number_parameters     342
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0296P)²+1.9767P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.325
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'XT, VERSION 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al Al1 0.53264(6) 0.69549(2) 0.38963(4) 0.01745(14) Uani d . . . 1 . .
C C1 0.64592(19) 0.66058(7) 0.50910(14) 0.0153(4) Uani d . . . 1 . .
C C2 0.6297(2) 0.60932(7) 0.53654(15) 0.0184(4) Uani d . . . 1 . .
C C3 0.7111(2) 0.58828(8) 0.62769(16) 0.0232(5) Uani d . . . 1 . .
H H3 0.6997 0.5531 0.6458 0.028 Uiso calc U . R 1 . .
C C4 0.8085(2) 0.61917(8) 0.69143(16) 0.0234(5) Uani d . . . 1 . .
H H4 0.8639 0.6049 0.7532 0.028 Uiso calc U . R 1 . .
C C5 0.8258(2) 0.67060(8) 0.66590(15) 0.0205(4) Uani d . . . 1 . .
H H5 0.8919 0.6918 0.7099 0.025 Uiso calc U . R 1 . .
C C6 0.7440(2) 0.69080(7) 0.57408(14) 0.0159(4) Uani d . . . 1 . .
C C7 0.7480(2) 0.74461(7) 0.53877(15) 0.0170(4) Uani d . . . 1 . .
H H7 0.8136 0.7685 0.5756 0.02 Uiso calc U . R 1 . .
C C8 0.66149(19) 0.81220(7) 0.42377(14) 0.0150(4) Uani d . . . 1 . .
C C9 0.7505(2) 0.82750(7) 0.35083(15) 0.0174(4) Uani d . . . 1 . .
C C10 0.8540(2) 0.79132(8) 0.30808(16) 0.0246(5) Uani d . . . 1 . .
H H10 0.8269 0.7551 0.3239 0.029 Uiso calc U . R 1 . .
C C11 1.0045(2) 0.80100(10) 0.3657(2) 0.0433(6) Uani d . . . 1 . .
H H11A 1.0313 0.8369 0.3548 0.065 Uiso calc U . R 1 . .
H H11B 1.071 0.7778 0.3371 0.065 Uiso calc U . R 1 . .
H H11C 1.0077 0.7945 0.4423 0.065 Uiso calc U . R 1 . .
C C12 0.8488(3) 0.79628(9) 0.18700(18) 0.0377(6) Uani d . . . 1 . .
H H12A 0.7509 0.7913 0.1516 0.057 Uiso calc U . R 1 . .
H H12B 0.9105 0.7701 0.162 0.057 Uiso calc U . R 1 . .
H H12C 0.8818 0.8307 0.1699 0.057 Uiso calc U . R 1 . .
C C13 0.7482(2) 0.87951(8) 0.32197(16) 0.0205(4) Uani d . . . 1 . .
H H13 0.8071 0.8912 0.2724 0.025 Uiso calc U . R 1 . .
C C14 0.6618(2) 0.91425(8) 0.36411(16) 0.0209(4) Uani d . . . 1 . .
H H14 0.6621 0.9495 0.3437 0.025 Uiso calc U . R 1 . .
C C15 0.5749(2) 0.89805(7) 0.43591(15) 0.0178(4) Uani d . . . 1 . .
H H15 0.5161 0.9225 0.4644 0.021 Uiso calc U . R 1 . .
C C16 0.57183(19) 0.84674(7) 0.46714(14) 0.0155(4) Uani d . . . 1 . .
C C17 0.4790(2) 0.82921(7) 0.54821(15) 0.0197(4) Uani d . . . 1 . .
H H17 0.4578 0.7918 0.5352 0.024 Uiso calc U . R 1 . .
C C18 0.5579(3) 0.83456(8) 0.66193(16) 0.0298(5) Uani d . . . 1 . .
H H18A 0.6435 0.813 0.6702 0.045 Uiso calc U . R 1 . .
H H18B 0.4958 0.8234 0.7128 0.045 Uiso calc U . R 1 . .
H H18C 0.585 0.8707 0.6757 0.045 Uiso calc U . R 1 . .
C C19 0.3376(2) 0.85768(9) 0.53707(19) 0.0346(6) Uani d . . . 1 . .
H H19A 0.3541 0.8937 0.559 0.052 Uiso calc U . R 1 . .
H H19B 0.2757 0.8412 0.5826 0.052 Uiso calc U . R 1 . .
H H19C 0.2918 0.8565 0.4624 0.052 Uiso calc U . R 1 . .
C C20 0.5192(2) 0.58138(7) 0.46612(15) 0.0209(4) Uani d . . . 1 . .
H H20 0.5002 0.5463 0.4802 0.025 Uiso calc U . R 1 . .
C C21 0.3352(2) 0.57560(7) 0.32346(15) 0.0200(4) Uani d . . . 1 . .
C C22 0.3585(2) 0.55595(7) 0.22403(16) 0.0222(4) Uani d . . . 1 . .
C C23 0.4986(2) 0.56404(8) 0.18362(17) 0.0282(5) Uani d . . . 1 . .
H H23 0.5484 0.5934 0.2248 0.034 Uiso calc U . R 1 . .
C C24 0.5931(3) 0.51658(11) 0.2046(2) 0.0618(9) Uani d . . . 1 . .
H H24A 0.6111 0.5096 0.2815 0.093 Uiso calc U . R 1 . .
H H24B 0.6836 0.5228 0.1784 0.093 Uiso calc U . R 1 . .
H H24C 0.5453 0.4868 0.1673 0.093 Uiso calc U . R 1 . .
C C25 0.4793(3) 0.57856(10) 0.06531(18) 0.0397(6) Uani d . . . 1 . .
H H25A 0.4359 0.5496 0.0225 0.06 Uiso calc U . R 1 . .
H H25B 0.5721 0.5865 0.0445 0.06 Uiso calc U . R 1 . .
H H25C 0.4174 0.6089 0.0532 0.06 Uiso calc U . R 1 . .
C C26 0.2495(2) 0.52747(8) 0.16529(17) 0.0284(5) Uani d . . . 1 . .
H H26 0.2627 0.5136 0.098 0.034 Uiso calc U . R 1 . .
C C27 0.1230(3) 0.51920(8) 0.20327(17) 0.0326(6) Uani d . . . 1 . .
H H27 0.0505 0.4992 0.1627 0.039 Uiso calc U . R 1 . .
C C28 0.1010(2) 0.53985(8) 0.30005(17) 0.0308(5) Uani d . . . 1 . .
H H28 0.0127 0.5343 0.3247 0.037 Uiso calc U . R 1 . .
C C29 0.2064(2) 0.56885(8) 0.36256(16) 0.0246(5) Uani d . . . 1 . .
C C30 0.1779(2) 0.59178(9) 0.46817(17) 0.0309(5) Uani d . . . 1 . .
H H30 0.2588 0.6154 0.4947 0.037 Uiso calc U . R 1 . .
C C31 0.1748(4) 0.54896(12) 0.5513(2) 0.0623(9) Uani d . . . 1 . .
H H31A 0.1028 0.5233 0.524 0.093 Uiso calc U . R 1 . .
H H31B 0.1513 0.5639 0.6176 0.093 Uiso calc U . R 1 . .
H H31C 0.2683 0.5324 0.5654 0.093 Uiso calc U . R 1 . .
C C32 0.0417(3) 0.62341(13) 0.4562(2) 0.0542(8) Uani d . . . 1 . .
H H32A 0.047 0.6511 0.4042 0.081 Uiso calc U . R 1 . .
H H32B 0.03 0.6385 0.5254 0.081 Uiso calc U . R 1 . .
H H32C -0.0396 0.6011 0.4313 0.081 Uiso calc U . R 1 . .
Cl Cl1 0.32266(5) 0.72220(2) 0.39377(4) 0.02340(12) Uani d . . . 1 . .
Cl Cl2 0.57859(6) 0.69832(2) 0.22942(4) 0.02661(13) Uani d . . . 1 . .
N N1 0.65996(16) 0.75855(6) 0.45630(12) 0.0154(3) Uani d . . . 1 . .
N N2 0.44857(17) 0.60410(6) 0.38589(12) 0.0173(4) Uani d . . . 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 C1 . 1.9446(19) ?
Al1 Cl1 . 2.1208(8) ?
Al1 N1 . 2.1317(16) ?
Al1 Cl2 . 2.1382(7) ?
C1 C2 . 1.387(3) ?
C1 C6 . 1.390(3) ?
C2 C3 . 1.401(3) ?
C2 C20 . 1.464(3) ?
C3 C4 . 1.388(3) ?
C4 C5 . 1.387(3) ?
C5 C6 . 1.400(3) ?
C6 C7 . 1.467(3) ?
C7 N1 . 1.289(2) ?
C8 C9 . 1.399(3) ?
C8 C16 . 1.403(3) ?
C8 N1 . 1.450(2) ?
C9 C13 . 1.396(3) ?
C9 C10 . 1.516(3) ?
C10 C11 . 1.527(3) ?
C10 C12 . 1.531(3) ?
C13 C14 . 1.378(3) ?
C14 C15 . 1.382(3) ?
C15 C16 . 1.388(3) ?
C16 C17 . 1.519(3) ?
C17 C19 . 1.522(3) ?
C17 C18 . 1.528(3) ?
C20 N2 . 1.276(2) ?
C21 C29 . 1.398(3) ?
C21 C22 . 1.405(3) ?
C21 N2 . 1.442(2) ?
C22 C26 . 1.394(3) ?
C22 C23 . 1.511(3) ?
C23 C24 . 1.523(3) ?
C23 C25 . 1.528(3) ?
C26 C27 . 1.377(3) ?
C27 C28 . 1.381(3) ?
C28 C29 . 1.400(3) ?
C29 C30 . 1.524(3) ?
C30 C32 . 1.521(3) ?
C30 C31 . 1.532(3) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Al1 Cl1 . . 123.18(6) ?
C1 Al1 N1 . . 80.35(7) ?
Cl1 Al1 N1 . . 102.79(5) ?
C1 Al1 Cl2 . . 125.86(6) ?
Cl1 Al1 Cl2 . . 109.75(3) ?
N1 Al1 Cl2 . . 99.50(5) ?
C2 C1 C6 . . 118.75(17) ?
C2 C1 Al1 . . 124.81(14) ?
C6 C1 Al1 . . 116.33(14) ?
C1 C2 C3 . . 120.70(18) ?
C1 C2 C20 . . 114.68(17) ?
C3 C2 C20 . . 124.58(18) ?
C4 C3 C2 . . 119.58(18) ?
C5 C4 C3 . . 120.69(18) ?
C4 C5 C6 . . 118.84(18) ?
C1 C6 C5 . . 121.44(18) ?
C1 C6 C7 . . 113.63(16) ?
C5 C6 C7 . . 124.90(17) ?
N1 C7 C6 . . 118.05(17) ?
C9 C8 C16 . . 122.65(17) ?
C9 C8 N1 . . 119.43(16) ?
C16 C8 N1 . . 117.91(16) ?
C13 C9 C8 . . 117.31(17) ?
C13 C9 C10 . . 119.32(17) ?
C8 C9 C10 . . 123.26(17) ?
C9 C10 C11 . . 109.84(17) ?
C9 C10 C12 . . 112.29(17) ?
C11 C10 C12 . . 110.65(19) ?
C14 C13 C9 . . 121.10(18) ?
C13 C14 C15 . . 120.35(18) ?
C14 C15 C16 . . 121.19(18) ?
C15 C16 C8 . . 117.39(17) ?
C15 C16 C17 . . 121.15(17) ?
C8 C16 C17 . . 121.42(17) ?
C16 C17 C19 . . 112.74(16) ?
C16 C17 C18 . . 110.86(16) ?
C19 C17 C18 . . 110.30(17) ?
N2 C20 C2 . . 120.12(18) ?
C29 C21 C22 . . 122.34(18) ?
C29 C21 N2 . . 119.52(17) ?
C22 C21 N2 . . 118.14(18) ?
C26 C22 C21 . . 117.7(2) ?
C26 C22 C23 . . 121.08(19) ?
C21 C22 C23 . . 121.16(18) ?
C22 C23 C24 . . 110.8(2) ?
C22 C23 C25 . . 112.46(18) ?
C24 C23 C25 . . 110.6(2) ?
C27 C26 C22 . . 121.0(2) ?
C26 C27 C28 . . 120.3(2) ?
C27 C28 C29 . . 121.3(2) ?
C21 C29 C28 . . 117.2(2) ?
C21 C29 C30 . . 122.76(18) ?
C28 C29 C30 . . 120.0(2) ?
C32 C30 C29 . . 112.48(18) ?
C32 C30 C31 . . 110.8(2) ?
C29 C30 C31 . . 110.1(2) ?
C7 N1 C8 . . 117.76(15) ?
C7 N1 Al1 . . 111.60(12) ?
C8 N1 Al1 . . 130.64(12) ?
C20 N2 C21 . . 117.54(16) ?

####################################################################### 
# 
# 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_dv340
_database_code_depnum_ccdc_archive 'CCDC 1471554'
_audit_update_record             
;
2016-12-06 deposited with the CCDC.
2016-12-13 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C90.80 H95.60 Al2 B Cl17.60 N4 Na'
_chemical_formula_iupac          ?
_chemical_formula_weight         1954.59

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.9979(7)
_cell_length_b                   27.9699(11)
_cell_length_c                   20.6231(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.6642(16)
_cell_angle_gamma                90
_cell_volume                     9794.2(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.3786
_cell_measurement_theta_max      26.2602
_cell_measurement_temperature    153.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.220
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4038

_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_T_max  0.89

_exptl_special_details           
;
;

_diffrn_ambient_temperature      153.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            31319
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0998
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         29.19
_diffrn_reflns_theta_full        29.19
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       14

_refine_special_details          
;
;

_reflns_number_total             13106
_reflns_number_gt                8442
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1686
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.043
_refine_ls_number_reflns         13106
_refine_ls_number_parameters     585
_refine_ls_number_restraints     116
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0583P)²+14.2122P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.667
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
B B 0.0013 0.0007 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'XS, VERSION 2013/1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na Na1 1.0122(6) 0.0055(4) 0.9979(7) 0.0422(17) Uani d . P . 0.5 A -1
Al Al1 0.87647(5) 0.08879(3) 0.92355(4) 0.01799(18) Uani d . . . 1 . .
B B1 0.5 0.21856(14) 0.75 0.0152(8) Uani d T P S 1 . .
C C1 0.85821(15) 0.14866(9) 0.87855(13) 0.0181(5) Uani d . . . 1 . .
C C2 0.91997(16) 0.17924(10) 0.86669(14) 0.0220(6) Uani d . . . 1 . .
C C3 0.90625(19) 0.22250(11) 0.83442(17) 0.0347(8) Uani d . . . 1 . .
H H3 0.9485 0.2435 0.8261 0.042 Uiso calc U . R 1 . .
C C4 0.8289(2) 0.23426(12) 0.81461(19) 0.0411(9) Uani d . . . 1 . .
H H4 0.8188 0.2637 0.7929 0.049 Uiso calc U . R 1 . .
C C5 0.76656(18) 0.20386(10) 0.82596(16) 0.0300(7) Uani d . . . 1 . .
H H5 0.7143 0.2122 0.8119 0.036 Uiso calc U . R 1 . .
C C6 0.78176(16) 0.16094(9) 0.85824(13) 0.0200(6) Uani d . . . 1 . .
C C7 0.99653(16) 0.16097(10) 0.89192(14) 0.0228(6) Uani d . . . 1 . .
H H7 1.0436 0.1788 0.8875 0.027 Uiso calc U . R 1 . .
C C8 1.07116(15) 0.10009(9) 0.94487(13) 0.0194(5) Uani d . . . 1 . .
C C9 1.11249(16) 0.07009(10) 0.90373(14) 0.0235(6) Uani d . . . 1 . .
C C10 1.08828(18) 0.06297(12) 0.83297(14) 0.0295(7) Uani d . . . 1 . .
H H10 1.0316 0.0723 0.8269 0.035 Uiso calc U . R 1 . .
C C11 1.0957(2) 0.01085(13) 0.81145(18) 0.0424(9) Uani d . . . 1 . .
H H11A 1.1509 0.0009 0.8162 0.064 Uiso calc U . R 1 . .
H H11B 1.0773 0.0078 0.7659 0.064 Uiso calc U . R 1 . .
H H11C 1.0636 -0.0095 0.8384 0.064 Uiso calc U . R 1 . .
C C12 1.1361(2) 0.09599(15) 0.79015(17) 0.0483(10) Uani d . . . 1 . .
H H12A 1.1271 0.1294 0.8022 0.073 Uiso calc U . R 1 . .
H H12B 1.1194 0.0912 0.7445 0.073 Uiso calc U . R 1 . .
H H12C 1.1922 0.0885 0.7964 0.073 Uiso calc U . R 1 . .
C C13 1.18125(17) 0.04908(11) 0.93029(15) 0.0295(7) Uani d . . . 1 . .
H H13 1.2114 0.029 0.9038 0.035 Uiso calc U . R 1 . .
C C14 1.20653(17) 0.05675(11) 0.99390(16) 0.0309(7) Uani d . . . 1 . .
H H14 1.2527 0.0413 1.0111 0.037 Uiso calc U . R 1 . .
C C15 1.16472(17) 0.08694(11) 1.03276(15) 0.0275(7) Uani d . . . 1 . .
H H15 1.1832 0.0925 1.0763 0.033 Uiso calc U . R 1 . .
C C16 1.09588(16) 0.10938(10) 1.00907(14) 0.0217(6) Uani d . . . 1 . .
C C17 1.05440(17) 0.14469(11) 1.05174(15) 0.0283(7) Uani d . . . 1 . .
H H17 1.0004 0.1503 1.0318 0.034 Uiso calc U . R 1 . .
C C18 1.0984(2) 0.19259(12) 1.0527(2) 0.0516(11) Uani d . . . 1 . .
H H18A 1.1509 0.1883 1.0734 0.077 Uiso calc U . R 1 . .
H H18B 1.069 0.2161 1.0772 0.077 Uiso calc U . R 1 . .
H H18C 1.1033 0.2039 1.0081 0.077 Uiso calc U . R 1 . .
C C19 1.0453(2) 0.12632(14) 1.12118(16) 0.0423(9) Uani d . . . 1 . .
H H19A 1.0216 0.0944 1.1196 0.063 Uiso calc U . R 1 . .
H H19B 1.0112 0.1481 1.1443 0.063 Uiso calc U . R 1 . .
H H19C 1.0971 0.1248 1.1439 0.063 Uiso calc U . R 1 . .
C C20 0.72423(16) 0.12421(9) 0.87451(13) 0.0201(6) Uani d . . . 1 . .
H H20 0.6698 0.1282 0.8633 0.024 Uiso calc U . R 1 . .
C C21 0.69356(15) 0.04966(9) 0.91993(13) 0.0186(5) Uani d . . . 1 . .
C C22 0.67689(15) 0.01338(9) 0.87444(13) 0.0189(5) Uani d . . . 1 . .
C C23 0.70885(17) 0.01381(10) 0.80686(14) 0.0227(6) Uani d . . . 1 . .
H H23 0.7568 0.0346 0.8083 0.027 Uiso calc U . R 1 . .
C C24 0.7333(2) -0.03557(11) 0.78429(16) 0.0340(7) Uani d . . . 1 . .
H H24A 0.6868 -0.0562 0.7797 0.051 Uiso calc U . R 1 . .
H H24B 0.7712 -0.0494 0.8163 0.051 Uiso calc U . R 1 . .
H H24C 0.7577 -0.0329 0.7423 0.051 Uiso calc U . R 1 . .
C C25 0.6490(2) 0.03594(14) 0.75836(16) 0.0431(9) Uani d . . . 1 . .
H H25A 0.5999 0.0176 0.7581 0.065 Uiso calc U . R 1 . .
H H25B 0.67 0.0353 0.7149 0.065 Uiso calc U . R 1 . .
H H25C 0.6388 0.0691 0.7708 0.065 Uiso calc U . R 1 . .
C C26 0.62583(16) -0.02318(10) 0.89214(14) 0.0221(6) Uani d . . . 1 . .
H H26 0.6132 -0.0482 0.8623 0.026 Uiso calc U . R 1 . .
C C27 0.59364(16) -0.02335(10) 0.95253(15) 0.0243(6) Uani d . . . 1 . .
H H27 0.5599 -0.0487 0.9642 0.029 Uiso calc U . R 1 . .
C C28 0.61048(16) 0.01335(10) 0.99596(14) 0.0235(6) Uani d . . . 1 . .
H H28 0.5875 0.013 1.0371 0.028 Uiso calc U . R 1 . .
C C29 0.66019(15) 0.05074(10) 0.98090(14) 0.0214(6) Uani d . . . 1 . .
C C30 0.67292(18) 0.09209(11) 1.02723(14) 0.0282(7) Uani d . . . 1 . .
H H30 0.7223 0.1088 1.0156 0.034 Uiso calc U . R 1 . .
C C31 0.6050(2) 0.12778(12) 1.0187(2) 0.0445(9) Uani d . . . 1 . .
H H31A 0.6022 0.1397 0.974 0.067 Uiso calc U . R 1 . .
H H31B 0.6138 0.1546 1.0487 0.067 Uiso calc U . R 1 . .
H H31C 0.5553 0.1119 1.0279 0.067 Uiso calc U . R 1 . .
C C32 0.6831(2) 0.07638(15) 1.09779(17) 0.0490(10) Uani d . . . 1 . .
H H32A 0.6358 0.0594 1.1103 0.074 Uiso calc U . R 1 . .
H H32B 0.6915 0.1045 1.1255 0.074 Uiso calc U . R 1 . .
H H32C 0.7288 0.0551 1.1029 0.074 Uiso calc U . R 1 . .
C C33 0.44555(15) 0.18558(9) 0.79600(12) 0.0169(5) Uani d . . . 1 . .
C C34 0.47436(16) 0.14204(9) 0.82090(13) 0.0184(5) Uani d . . . 1 . .
H H34 0.5241 0.1309 0.808 0.022 Uiso calc U . R 1 . .
C C35 0.43332(17) 0.11489(9) 0.86332(13) 0.0223(6) Uani d . . . 1 . .
C C36 0.36154(18) 0.12928(11) 0.88548(15) 0.0284(7) Uani d . . . 1 . .
H H36 0.3333 0.1105 0.915 0.034 Uiso calc U . R 1 . .
C C37 0.33331(17) 0.17267(11) 0.86204(15) 0.0271(6) Uani d . . . 1 . .
C C38 0.37286(16) 0.20019(10) 0.81832(14) 0.0224(6) Uani d . . . 1 . .
H H38 0.3503 0.2294 0.8032 0.027 Uiso calc U . R 1 . .
C C39 0.55555(15) 0.25275(9) 0.79823(13) 0.0166(5) Uani d . . . 1 . .
C C40 0.56848(16) 0.24433(9) 0.86460(13) 0.0192(5) Uani d . . . 1 . .
H H40 0.5434 0.218 0.884 0.023 Uiso calc U . R 1 . .
C C41 0.61750(17) 0.27388(10) 0.90285(14) 0.0253(6) Uani d . . . 1 . .
C C42 0.65671(19) 0.31194(10) 0.87751(16) 0.0313(7) Uani d . . . 1 . .
H H42 0.6912 0.3314 0.9038 0.038 Uiso calc U . R 1 . .
C C43 0.64370(19) 0.32064(10) 0.81203(16) 0.0309(7) Uani d . . . 1 . .
C C44 0.59461(17) 0.29217(9) 0.77290(14) 0.0240(6) Uani d . . . 1 . .
H H44 0.5873 0.2995 0.728 0.029 Uiso calc U . R 1 . .
C C45 0.3384(4) 0.1743(3) 0.0644(3) 0.111(3) Uani d . P . 0.9 B 1
H H45A 0.3361 0.1433 0.0414 0.133 Uiso calc U P R 0.9 B 1
H H45B 0.2992 0.1958 0.0425 0.133 Uiso calc U P R 0.9 B 1
Cl Cl7 0.31131(10) 0.16525(6) 0.14385(8) 0.0844(5) Uani d . P D 0.9 B 1
Cl Cl8 0.42926(11) 0.19814(8) 0.05716(12) 0.1254(8) Uani d . P D 0.9 B 1
Cl Cl1 0.88331(4) 0.07534(3) 1.02630(3) 0.02539(16) Uani d . . . 1 . .
Cl Cl2 0.90713(4) 0.02057(2) 0.88273(3) 0.02364(15) Uani d . . . 1 . .
Cl Cl3 0.47347(5) 0.06077(3) 0.88964(4) 0.0354(2) Uani d . . . 1 . .
Cl Cl4 0.24390(5) 0.19376(4) 0.89091(5) 0.0513(3) Uani d . . . 1 . .
Cl Cl5 0.62981(6) 0.26291(3) 0.98594(4) 0.0454(2) Uani d . . . 1 . .
Cl Cl6 0.69066(7) 0.36874(4) 0.77693(5) 0.0664(4) Uani d . . . 1 . .
N N1 0.99725(12) 0.12022(8) 0.92001(11) 0.0187(5) Uani d . . . 1 . .
N N2 0.74933(12) 0.08658(8) 0.90420(11) 0.0179(5) Uani d . . . 1 . .
C C47 0.5146(18) 0.1523(4) 0.2380(15) 0.132(4) Uani d U P D 0.4 C -1
H H47A 0.5628 0.1672 0.2578 0.159 Uiso calc U P R 0.4 C -1
H H47B 0.4935 0.1722 0.2014 0.159 Uiso calc U P R 0.4 C -1
Cl Cl9 0.5302(5) 0.0896(4) 0.2141(5) 0.209(4) Uani d U P D 0.4 C -1
Cl Cl10 0.4402(3) 0.1399(2) 0.2980(2) 0.1180(15) Uani d U P D 0.4 C -1
C C47A 0.511(5) 0.1304(8) 0.3078(13) 0.107(5) Uani d U P D 0.1 D -2
H H47C 0.4695 0.1383 0.3384 0.128 Uiso calc U P R 0.1 D -2
H H47D 0.5625 0.1289 0.3318 0.128 Uiso calc U P R 0.1 D -2
Cl Cl11 0.512(2) 0.1736(4) 0.2408(17) 0.106(5) Uani d U P D 0.1 D -2
Cl Cl12 0.4884(7) 0.0740(3) 0.2642(8) 0.050(3) Uani d U P D 0.1 D -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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Na1 Cl2 . 2.934(13) ?
Na1 Cl1 . 3.013(13) ?
Na1 Al1 . 3.573(13) ?
Al1 C1 . 1.933(3) ?
Al1 Cl1 . 2.1501(10) ?
Al1 Cl2 . 2.1592(10) ?
Al1 N2 . 2.180(2) ?
Al1 N1 . 2.238(2) ?
B1 C33 2_656 1.640(3) ?
B1 C33 . 1.640(3) ?
B1 C39 2_656 1.646(3) ?
B1 C39 . 1.646(3) ?
C1 C2 . 1.385(4) ?
C1 C6 . 1.390(4) ?
C2 C3 . 1.395(4) ?
C2 C7 . 1.470(4) ?
C3 C4 . 1.398(4) ?
C4 C5 . 1.387(4) ?
C5 C6 . 1.391(4) ?
C6 C20 . 1.468(4) ?
C7 N1 . 1.278(3) ?
C8 C16 . 1.395(4) ?
C8 C9 . 1.405(4) ?
C8 N1 . 1.449(3) ?
C9 C13 . 1.397(4) ?
C9 C10 . 1.511(4) ?
C10 C11 . 1.531(5) ?
C10 C12 . 1.536(5) ?
C13 C14 . 1.378(4) ?
C14 C15 . 1.383(4) ?
C15 C16 . 1.396(4) ?
C16 C17 . 1.518(4) ?
C17 C18 . 1.534(4) ?
C17 C19 . 1.536(5) ?
C20 N2 . 1.281(3) ?
C21 C22 . 1.402(4) ?
C21 C29 . 1.404(4) ?
C21 N2 . 1.449(3) ?
C22 C26 . 1.401(4) ?
C22 C23 . 1.519(4) ?
C23 C24 . 1.521(4) ?
C23 C25 . 1.524(4) ?
C26 C27 . 1.383(4) ?
C27 C28 . 1.383(4) ?
C28 C29 . 1.389(4) ?
C29 C30 . 1.509(4) ?
C30 C32 . 1.522(4) ?
C30 C31 . 1.531(4) ?
C33 C38 . 1.399(4) ?
C33 C34 . 1.401(3) ?
C34 C35 . 1.373(4) ?
C35 C36 . 1.383(4) ?
C35 Cl3 . 1.737(3) ?
C36 C37 . 1.384(4) ?
C37 C38 . 1.383(4) ?
C37 Cl4 . 1.760(3) ?
C39 C40 . 1.396(4) ?
C39 C44 . 1.401(4) ?
C40 C41 . 1.392(4) ?
C41 C42 . 1.372(4) ?
C41 Cl5 . 1.744(3) ?
C42 C43 . 1.380(4) ?
C43 C44 . 1.385(4) ?
C43 Cl6 . 1.739(3) ?
C45 Cl8 . 1.695(6) ?
C45 Cl7 . 1.740(6) ?
C47 Cl10 . 1.842(9) ?
C47 Cl9 . 1.845(9) ?
C47A Cl11 . 1.836(10) ?
C47A Cl12 . 1.846(10) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl2 Na1 Cl1 . . 69.1(3) ?
Cl2 Na1 Al1 . . 37.15(15) ?
Cl1 Na1 Al1 . . 36.89(14) ?
C1 Al1 Cl1 . . 128.68(9) ?
C1 Al1 Cl2 . . 127.94(9) ?
Cl1 Al1 Cl2 . . 103.10(4) ?
C1 Al1 N2 . . 78.52(10) ?
Cl1 Al1 N2 . . 100.55(7) ?
Cl2 Al1 N2 . . 99.13(7) ?
C1 Al1 N1 . . 76.76(10) ?
Cl1 Al1 N1 . . 95.35(7) ?
Cl2 Al1 N1 . . 95.51(7) ?
N2 Al1 N1 . . 155.28(9) ?
C1 Al1 Na1 . . 148.96(13) ?
Cl1 Al1 Na1 . . 57.2(2) ?
Cl2 Al1 Na1 . . 55.1(2) ?
N2 Al1 Na1 . . 132.44(12) ?
N1 Al1 Na1 . . 72.24(11) ?
C33 B1 C33 2_656 . 111.5(3) ?
C33 B1 C39 2_656 2_656 107.49(13) ?
C33 B1 C39 . 2_656 110.68(13) ?
C33 B1 C39 2_656 . 110.67(13) ?
C33 B1 C39 . . 107.49(13) ?
C39 B1 C39 2_656 . 109.0(3) ?
C2 C1 C6 . . 120.0(2) ?
C2 C1 Al1 . . 120.92(19) ?
C6 C1 Al1 . . 119.1(2) ?
C1 C2 C3 . . 120.6(3) ?
C1 C2 C7 . . 112.9(2) ?
C3 C2 C7 . . 126.6(3) ?
C2 C3 C4 . . 118.5(3) ?
C5 C4 C3 . . 121.4(3) ?
C4 C5 C6 . . 118.9(3) ?
C1 C6 C5 . . 120.5(3) ?
C1 C6 C20 . . 112.4(2) ?
C5 C6 C20 . . 127.0(2) ?
N1 C7 C2 . . 117.4(2) ?
C16 C8 C9 . . 123.2(2) ?
C16 C8 N1 . . 118.8(2) ?
C9 C8 N1 . . 117.9(2) ?
C13 C9 C8 . . 116.6(3) ?
C13 C9 C10 . . 120.6(3) ?
C8 C9 C10 . . 122.7(2) ?
C9 C10 C11 . . 112.5(3) ?
C9 C10 C12 . . 110.4(3) ?
C11 C10 C12 . . 110.7(3) ?
C14 C13 C9 . . 121.7(3) ?
C13 C14 C15 . . 120.0(3) ?
C14 C15 C16 . . 121.1(3) ?
C8 C16 C15 . . 117.3(3) ?
C8 C16 C17 . . 123.0(2) ?
C15 C16 C17 . . 119.6(3) ?
C16 C17 C18 . . 109.7(3) ?
C16 C17 C19 . . 113.1(3) ?
C18 C17 C19 . . 110.5(3) ?
N2 C20 C6 . . 118.3(2) ?
C22 C21 C29 . . 122.5(2) ?
C22 C21 N2 . . 118.7(2) ?
C29 C21 N2 . . 118.8(2) ?
C26 C22 C21 . . 117.5(3) ?
C26 C22 C23 . . 119.8(2) ?
C21 C22 C23 . . 122.6(2) ?
C22 C23 C24 . . 112.8(2) ?
C22 C23 C25 . . 110.4(2) ?
C24 C23 C25 . . 110.5(3) ?
C27 C26 C22 . . 120.9(3) ?
C26 C27 C28 . . 120.1(3) ?
C27 C28 C29 . . 121.6(3) ?
C28 C29 C21 . . 117.3(3) ?
C28 C29 C30 . . 120.4(3) ?
C21 C29 C30 . . 122.1(3) ?
C29 C30 C32 . . 113.0(3) ?
C29 C30 C31 . . 110.0(2) ?
C32 C30 C31 . . 110.5(3) ?
C38 C33 C34 . . 115.6(2) ?
C38 C33 B1 . . 123.8(2) ?
C34 C33 B1 . . 120.3(2) ?
C35 C34 C33 . . 122.3(3) ?
C34 C35 C36 . . 122.1(3) ?
C34 C35 Cl3 . . 118.5(2) ?
C36 C35 Cl3 . . 119.4(2) ?
C35 C36 C37 . . 115.9(3) ?
C38 C37 C36 . . 123.0(3) ?
C38 C37 Cl4 . . 119.2(2) ?
C36 C37 Cl4 . . 117.8(2) ?
C37 C38 C33 . . 121.0(3) ?
C40 C39 C44 . . 116.3(2) ?
C40 C39 B1 . . 123.7(2) ?
C44 C39 B1 . . 120.0(2) ?
C41 C40 C39 . . 121.2(3) ?
C42 C41 C40 . . 122.2(3) ?
C42 C41 Cl5 . . 118.2(2) ?
C40 C41 Cl5 . . 119.6(2) ?
C41 C42 C43 . . 116.8(3) ?
C42 C43 C44 . . 122.2(3) ?
C42 C43 Cl6 . . 119.2(2) ?
C44 C43 Cl6 . . 118.5(2) ?
C43 C44 C39 . . 121.2(3) ?
Cl8 C45 Cl7 . . 115.0(3) ?
Al1 Cl1 Na1 . . 85.9(3) ?
Al1 Cl2 Na1 . . 87.7(3) ?
C7 N1 C8 . . 119.8(2) ?
C7 N1 Al1 . . 112.06(18) ?
C8 N1 Al1 . . 128.16(17) ?
C20 N2 C21 . . 119.1(2) ?
C20 N2 Al1 . . 111.69(18) ?
C21 N2 Al1 . . 129.24(16) ?
Cl10 C47 Cl9 . . 96.4(6) ?
Cl11 C47A Cl12 . . 101.8(8) ?

####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1471556'
_audit_update_record             
;
2016-03-31 deposited with the CCDC.
2016-12-13 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64.36 H68.91 Al B Cl11.82 N2 O'
_chemical_formula_iupac          ?
_chemical_formula_weight         1343.31

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_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                   14.2999(7)
_cell_length_b                   16.7422(9)
_cell_length_c                   17.0542(9)
_cell_angle_alpha                118.9176(18)
_cell_angle_beta                 104.6772(19)
_cell_angle_gamma                98.331(2)
_cell_volume                     3280.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9970
_cell_measurement_theta_min      2.4328
_cell_measurement_theta_max      26.1161
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.390
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392

_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_T_max  0.81

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            106602
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_full        27.13
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21

_refine_special_details          
;
;

_reflns_number_total             14392
_reflns_number_gt                10643
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1380
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.062
_refine_ls_number_reflns         14392
_refine_ls_number_parameters     892
_refine_ls_number_restraints     561
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0492P)²+6.5342P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.628
_refine_diff_density_min         -0.817
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
B B 0.0013 0.0007 '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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'XT, VERSION 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al Al1 0.47196(6) 0.69927(6) 0.47886(6) 0.01882(18) Uani d . . . 1.0 . .
B B1 0.7855(2) 0.7725(2) 0.1987(2) 0.0156(6) Uani d . . . 1.0 . .
C C1 0.4757(2) 0.78546(19) 0.4341(2) 0.0186(6) Uani d . . . 1.0 . .
C C2 0.3927(2) 0.8162(2) 0.4158(2) 0.0185(6) Uani d . . . 1.0 . .
C C3 0.3961(2) 0.8807(2) 0.3862(2) 0.0198(6) Uani d . . . 1.0 . .
H H3 0.3397 0.9028 0.3746 0.024 Uiso calc U . R 1.0 . .
C C4 0.4839(2) 0.9120(2) 0.3740(2) 0.0211(6) Uani d . . . 1.0 . .
H H4 0.4862 0.9547 0.3524 0.025 Uiso calc U . R 1.0 . .
C C5 0.5684(2) 0.8822(2) 0.3928(2) 0.0192(6) Uani d . . . 1.0 . .
H H5 0.6281 0.9048 0.3851 0.023 Uiso calc U . R 1.0 . .
C C6 0.5632(2) 0.81830(19) 0.4233(2) 0.0187(6) Uani d . . . 1.0 . .
C C7 0.6470(2) 0.78649(19) 0.4561(2) 0.0185(6) Uani d . . . 1.0 . .
H H7 0.7117 0.8048 0.4536 0.022 Uiso calc U . R 1.0 . .
C C8 0.7152(2) 0.71872(19) 0.5409(2) 0.0183(6) Uani d . . . 1.0 . .
C C9 0.7484(2) 0.6403(2) 0.4933(2) 0.0205(6) Uani d . . . 1.0 . .
C C10 0.7016(2) 0.5672(2) 0.3852(2) 0.0215(6) Uani d . . . 1.0 . .
H H10 0.6524 0.5911 0.3559 0.026 Uiso calc U . R 1.0 . .
C C11 0.7818(3) 0.5548(3) 0.3383(3) 0.0381(8) Uani d . . . 1.0 . .
H H11A 0.8196 0.6173 0.3533 0.057 Uiso calc U . R 1.0 . .
H H11B 0.7478 0.5106 0.2681 0.057 Uiso calc U . R 1.0 . .
H H11C 0.8292 0.5285 0.3635 0.057 Uiso calc U . R 1.0 . .
C C12 0.6424(3) 0.4707(2) 0.3626(3) 0.0369(8) Uani d . . . 1.0 . .
H H12A 0.689 0.4454 0.3902 0.055 Uiso calc U . R 1.0 . .
H H12B 0.6101 0.4254 0.2925 0.055 Uiso calc U . R 1.0 . .
H H12C 0.5898 0.479 0.3906 0.055 Uiso calc U . R 1.0 . .
C C13 0.8296(2) 0.6302(2) 0.5502(2) 0.0279(7) Uani d . . . 1.0 . .
H H13 0.8533 0.577 0.5205 0.033 Uiso calc U . R 1.0 . .
C C14 0.8758(2) 0.6960(3) 0.6485(3) 0.0328(8) Uani d . . . 1.0 . .
H H14 0.9315 0.6883 0.6855 0.039 Uiso calc U . R 1.0 . .
C C15 0.8416(2) 0.7731(3) 0.6935(2) 0.0312(7) Uani d . . . 1.0 . .
H H15 0.8743 0.8179 0.7613 0.037 Uiso calc U . R 1.0 . .
C C16 0.7606(2) 0.7860(2) 0.6416(2) 0.0242(6) Uani d . . . 1.0 . .
C C17 0.7266(3) 0.8735(2) 0.6925(2) 0.0291(7) Uani d . . . 1.0 . .
H H17 0.6557 0.8594 0.6502 0.035 Uiso calc U . R 1.0 . .
C C18 0.7245(3) 0.8951(3) 0.7901(3) 0.0472(10) Uani d . . . 1.0 . .
H H18A 0.6816 0.8377 0.7811 0.071 Uiso calc U . R 1.0 . .
H H18B 0.6966 0.9482 0.8171 0.071 Uiso calc U . R 1.0 . .
H H18C 0.7938 0.9132 0.8346 0.071 Uiso calc U . R 1.0 . .
C C19 0.7950(3) 0.9611(2) 0.7043(3) 0.0420(9) Uani d . . . 1.0 . .
H H19A 0.8662 0.9722 0.7398 0.063 Uiso calc U . R 1.0 . .
H H19B 0.7752 1.0178 0.7403 0.063 Uiso calc U . R 1.0 . .
H H19C 0.7873 0.9492 0.6405 0.063 Uiso calc U . R 1.0 . .
C C20 0.2443(2) 0.6916(2) 0.4970(2) 0.0250(7) Uani d . . . 1.0 . .
C C21 0.1569(2) 0.6139(2) 0.4260(3) 0.0292(7) Uani d . . . 1.0 . .
C C22 0.1316(2) 0.5697(2) 0.3190(3) 0.0311(7) Uani d . . . 1.0 . .
H H22 0.196 0.5873 0.3097 0.037 Uiso calc U . R 1.0 . .
C C23 0.0569(3) 0.6135(3) 0.2829(3) 0.0344(8) Uani d . . . 1.0 . .
H H23A -0.0063 0.5984 0.2927 0.052 Uiso calc U . R 1.0 . .
H H23B 0.0418 0.5863 0.214 0.052 Uiso calc U . R 1.0 . .
H H23C 0.0879 0.6834 0.3191 0.052 Uiso calc U . R 1.0 . .
C C24 0.0862(3) 0.4599(3) 0.2575(3) 0.0423(9) Uani d . . . 1.0 . .
H H24A 0.1332 0.432 0.2807 0.063 Uiso calc U . R 1.0 . .
H H24B 0.0756 0.4364 0.19 0.063 Uiso calc U . R 1.0 . .
H H24C 0.0209 0.441 0.2625 0.063 Uiso calc U . R 1.0 . .
C C25 0.0867(3) 0.5821(3) 0.4570(3) 0.0358(8) Uani d . . . 1.0 . .
H H25 0.0271 0.5287 0.4108 0.043 Uiso calc U . R 1.0 . .
C C26 0.1027(3) 0.6270(3) 0.5534(3) 0.0418(10) Uani d . . . 1.0 . .
H H26 0.0548 0.6034 0.573 0.05 Uiso calc U . R 1.0 . .
C C27 0.1873(3) 0.7058(3) 0.6223(3) 0.0371(9) Uani d . . . 1.0 . .
H H27 0.196 0.7369 0.6884 0.044 Uiso calc U . R 1.0 . .
C C28 0.2610(2) 0.7406(3) 0.5954(3) 0.0302(7) Uani d . . . 1.0 . .
C C29 0.3491(3) 0.8324(3) 0.6689(2) 0.0328(8) Uani d . . . 1.0 . .
H H29 0.4059 0.8286 0.6444 0.039 Uiso calc U . R 1.0 . .
C C30 0.3183(3) 0.9199(3) 0.6776(3) 0.0385(8) Uani d . . . 1.0 . .
H H30A 0.3007 0.9138 0.6151 0.058 Uiso calc U . R 1.0 . .
H H30B 0.3753 0.9789 0.7263 0.058 Uiso calc U . R 1.0 . .
H H30C 0.2592 0.9227 0.6969 0.058 Uiso calc U . R 1.0 . .
C C31 0.3895(3) 0.8463(3) 0.7682(3) 0.0519(11) Uani d . . . 1.0 . .
H H31A 0.3391 0.8604 0.7984 0.078 Uiso calc U . R 1.0 . .
H H31B 0.4533 0.9 0.8089 0.078 Uiso calc U . R 1.0 . .
H H31C 0.4019 0.7874 0.7608 0.078 Uiso calc U . R 1.0 . .
C C32 0.3718(2) 0.4893(2) 0.3817(2) 0.0254(6) Uani d . . . 1.0 . .
H H32A 0.3089 0.4957 0.3951 0.03 Uiso calc U . R 1.0 . .
H H32B 0.4188 0.4846 0.4319 0.03 Uiso calc U . R 1.0 . .
C C33 0.3478(3) 0.4028(2) 0.2823(2) 0.0336(7) Uani d . . . 1.0 . .
H H33A 0.2858 0.352 0.263 0.04 Uiso calc U . R 1.0 . .
H H33B 0.4052 0.3762 0.2804 0.04 Uiso calc U . R 1.0 . .
C C34 0.3307(3) 0.4399(2) 0.2160(2) 0.0330(7) Uani d . . . 1.0 . .
H H34A 0.2604 0.4427 0.1973 0.04 Uiso calc U . R 1.0 . .
H H34B 0.3435 0.3988 0.157 0.04 Uiso calc U . R 1.0 . .
C C35 0.4082(2) 0.5401(2) 0.2776(2) 0.0247(6) Uani d . . . 1.0 . .
H H35A 0.4737 0.5381 0.2684 0.03 Uiso calc U . R 1.0 . .
H H35B 0.3828 0.584 0.2608 0.03 Uiso calc U . R 1.0 . .
C C36 0.6748(2) 0.7007(2) 0.17215(18) 0.0185(6) Uani d . . . 1.0 . .
C C37 0.6610(2) 0.6081(2) 0.1543(2) 0.0224(6) Uani d . . . 1.0 . .
H H37 0.7173 0.5843 0.1579 0.027 Uiso calc U . R 1.0 . .
C C38 0.5655(2) 0.5508(2) 0.1313(2) 0.0273(7) Uani d . . . 1.0 . .
C C39 0.4804(2) 0.5811(2) 0.1252(2) 0.0297(7) Uani d . . . 1.0 . .
H H39 0.4151 0.5402 0.1072 0.036 Uiso calc U . R 1.0 . .
C C40 0.4950(2) 0.6737(2) 0.1466(2) 0.0284(7) Uani d . . . 1.0 . .
C C41 0.5895(2) 0.7328(2) 0.1698(2) 0.0236(6) Uani d . . . 1.0 . .
H H41 0.5965 0.7963 0.1843 0.028 Uiso calc U . R 1.0 . .
C C42 0.7693(2) 0.83997(19) 0.15495(19) 0.0169(5) Uani d . . . 1.0 . .
C C43 0.6939(2) 0.8001(2) 0.0637(2) 0.0223(6) Uani d . . . 1.0 . .
H H43 0.6486 0.7367 0.0312 0.027 Uiso calc U . R 1.0 . .
C C44 0.6844(2) 0.8517(2) 0.0203(2) 0.0265(7) Uani d . . . 1.0 . .
C C45 0.7474(2) 0.9442(2) 0.0633(2) 0.0247(6) Uani d . . . 1.0 . .
H H45 0.7398 0.9792 0.033 0.03 Uiso calc U . R 1.0 . .
C C46 0.8222(2) 0.9830(2) 0.1528(2) 0.0234(6) Uani d . . . 1.0 . .
C C47 0.8340(2) 0.9327(2) 0.1980(2) 0.0192(6) Uani d . . . 1.0 . .
H H47 0.887 0.9621 0.2593 0.023 Uiso calc U . R 1.0 . .
C C48 0.8572(2) 0.71429(19) 0.14601(19) 0.0158(5) Uani d . . . 1.0 . .
C C49 0.8159(2) 0.6274(2) 0.05679(19) 0.0189(6) Uani d . . . 1.0 . .
H H49 0.7442 0.5971 0.0276 0.023 Uiso calc U . R 1.0 . .
C C50 0.8773(2) 0.5842(2) 0.00962(19) 0.0200(6) Uani d . . . 1.0 . .
C C51 0.9820(2) 0.6249(2) 0.0465(2) 0.0210(6) Uani d . . . 1.0 . .
H H51 1.0233 0.5949 0.0134 0.025 Uiso calc U . R 1.0 . .
C C52 1.0228(2) 0.7121(2) 0.1348(2) 0.0198(6) Uani d . . . 1.0 . .
C C53 0.9634(2) 0.75614(19) 0.1844(2) 0.0187(6) Uani d . . . 1.0 . .
H H53 0.995 0.8155 0.2452 0.022 Uiso calc U . R 1.0 . .
C C54 0.83966(19) 0.83254(19) 0.31672(19) 0.0149(5) Uani d . . . 1.0 . .
C C55 0.8986(2) 0.79544(19) 0.36189(19) 0.0159(5) Uani d . . . 1.0 . .
H H55 0.912 0.7379 0.3232 0.019 Uiso calc U . R 1.0 . .
C C56 0.93754(19) 0.84063(19) 0.4613(2) 0.0162(5) Uani d . . . 1.0 . .
C C57 0.91941(19) 0.92404(19) 0.52172(19) 0.0148(5) Uani d . . . 1.0 . .
H H57 0.946 0.9548 0.5899 0.018 Uiso calc U . R 1.0 . .
C C58 0.86043(19) 0.96000(18) 0.47709(19) 0.0146(5) Uani d . . . 1.0 . .
C C59 0.82148(18) 0.91695(18) 0.37777(18) 0.0133(5) Uani d . . . 1.0 . .
H H59 0.7821 0.9449 0.3508 0.016 Uiso calc U . R 1.0 . .
C C69 0.3099(2) 0.7788(2) 0.4376(2) 0.0207(6) Uani d . . . 1.0 . .
H H69 0.2485 0.7945 0.4282 0.025 Uiso calc U . R 1.0 . .
C C61 0.9778(19) 0.8591(10) 0.0314(12) 0.045(3) Uani d U P D 0.392(5) A -1
H H61A 0.9433 0.873 0.0779 0.054 Uiso calc U P R 0.392(5) A -1
H H61B 1.042 0.8486 0.0569 0.054 Uiso calc U P R 0.392(5) A -1
Cl Cl10 0.8986(6) 0.7541(4) -0.0812(6) 0.082(2) Uani d U P D 0.392(5) A -1
Cl Cl11 1.0055(3) 0.9563(2) 0.0201(2) 0.0587(13) Uani d U P D 0.392(5) A -1
C C61A 0.9647(13) 0.8460(14) 0.0239(15) 0.054(3) Uani d U P D 0.393(5) B 2
H H61C 0.9538 0.8174 0.0611 0.065 Uiso calc U P R 0.393(5) B 2
H H61D 0.9668 0.914 0.0611 0.065 Uiso calc U P R 0.393(5) B 2
Cl Cl1A 1.0818(3) 0.8423(3) 0.0109(4) 0.101(2) Uani d U P D 0.393(5) B 2
Cl Cl2A 0.8672(3) 0.7872(4) -0.0822(5) 0.0731(13) Uani d U P . 0.393(5) B 2
C C61B 0.89(2) 0.866(12) 0.048(18) 0.056(5) Uani d U P D 0.0102(19) C 3
H H61E 0.9225 0.907 0.1192 0.067 Uiso calc U P R 0.0102(19) C 3
H H61F 0.8128 0.8516 0.0328 0.067 Uiso calc U P R 0.0102(19) C 3
Cl Cl1B 0.925(5) 0.927(6) -0.004(7) 0.061(6) Uani d U P D 0.0102(19) C 3
Cl Cl2B 0.918(10) 0.759(5) 0.002(8) 0.061(7) Uani d U P D 0.0102(19) C 3
C C61C -0.010(3) -0.136(3) 0.0349(16) 0.060(7) Uani d U P D 0.204(6) D 4
H H61G -0.0303 -0.0824 0.0791 0.072 Uiso calc U P R 0.204(6) D 4
H H61H 0.0359 -0.1534 0.0735 0.072 Uiso calc U P R 0.204(6) D 4
Cl Cl1C 0.0513(8) -0.1000(9) -0.0242(6) 0.121(6) Uani d U P D 0.204(6) D 4
Cl Cl2C -0.1192(6) -0.2356(8) -0.0534(7) 0.041(2) Uani d U P D 0.204(6) D 4
Cl Cl1 0.50141(5) 0.69019(5) 0.60198(5) 0.02262(15) Uani d . . . 1.0 . .
Cl Cl2 0.54891(7) 0.43419(6) 0.10626(6) 0.0375(2) Uani d . . . 1.0 . .
Cl Cl3 0.39009(6) 0.71577(8) 0.14146(7) 0.0462(2) Uani d . . . 1.0 . .
Cl Cl4 0.58940(7) 0.79790(7) -0.09395(6) 0.0440(2) Uani d . . . 1.0 . .
Cl Cl5 0.90484(7) 1.09916(6) 0.21086(6) 0.0393(2) Uani d . . . 1.0 . .
Cl Cl6 0.82111(6) 0.47159(5) -0.09936(5) 0.03008(18) Uani d . . . 1.0 . .
Cl Cl7 1.15526(5) 0.76570(5) 0.18679(6) 0.03281(19) Uani d . . . 1.0 . .
Cl Cl8 1.01232(6) 0.79333(5) 0.51421(5) 0.02505(16) Uani d . . . 1.0 . .
Cl Cl9 0.83396(5) 1.06356(5) 0.55138(5) 0.01960(14) Uani d . . . 1.0 . .
C C62 0.172(2) 0.6912(13) 0.9267(17) 0.091(4) Uani d U P D 0.262(4) E 1
H H62A 0.1014 0.6949 0.9131 0.109 Uiso calc U P R 0.262(4) E 1
H H62B 0.2143 0.7432 0.9944 0.109 Uiso calc U P R 0.262(4) E 1
Cl Cl12 0.2203(6) 0.7026(5) 0.8487(5) 0.0765(18) Uani d U P D 0.262(4) E 1
Cl Cl13 0.1719(3) 0.5738(4) 0.9075(3) 0.0562(14) Uani d U P D 0.262(4) E 1
C C68 0.450(3) 0.887(3) 1.073(2) 0.070(4) Uani d U P D 0.150(3) F 2
H H68A 0.5249 0.9089 1.1075 0.084 Uiso calc U P R 0.150(3) F 2
H H68B 0.4268 0.8162 1.03 0.084 Uiso calc U P R 0.150(3) F 2
Cl Cl15 0.3916(8) 0.9208(7) 1.1561(7) 0.079(3) Uani d U P D 0.150(3) F 2
Cl Cl14 0.4226(10) 0.9361(8) 1.0061(6) 0.094(4) Uani d U P D 0.150(3) F 2
C C63 0.4072(9) 0.8979(5) 1.0392(7) 0.089(3) Uani d U P D 0.591(5) G 3
H H63A 0.3584 0.9338 1.0421 0.134 Uiso calc U P R 0.591(5) G 3
H H63B 0.4605 0.9214 1.022 0.134 Uiso calc U P R 0.591(5) G 3
H H63C 0.4382 0.9069 1.1024 0.134 Uiso calc U P R 0.591(5) G 3
C C64 0.3562(7) 0.7994(7) 0.9691(7) 0.082(2) Uani d U P D 0.591(5) G 3
H H64A 0.3822 0.7582 0.9896 0.099 Uiso calc U P R 0.591(5) G 3
H H64B 0.3603 0.7808 0.9057 0.099 Uiso calc U P R 0.591(5) G 3
C C65 0.2477(8) 0.7967(7) 0.9674(9) 0.110(3) Uani d U P D 0.591(5) G 3
H H65A 0.2376 0.7965 1.0227 0.132 Uiso calc U P R 0.591(5) G 3
H H65B 0.2276 0.8493 0.9638 0.132 Uiso calc U P R 0.591(5) G 3
C C66 0.1946(10) 0.6993(9) 0.8727(9) 0.100(3) Uani d U P D 0.591(5) G 3
H H66A 0.2356 0.6852 0.8316 0.119 Uiso calc U P R 0.591(5) G 3
H H66B 0.1262 0.6954 0.8364 0.119 Uiso calc U P R 0.591(5) G 3
C C67 0.1877(8) 0.6313(8) 0.9097(7) 0.081(3) Uani d U P D 0.591(5) G 3
H H67A 0.136 0.5692 0.8588 0.122 Uiso calc U P R 0.591(5) G 3
H H67B 0.1689 0.66 0.9665 0.122 Uiso calc U P R 0.591(5) G 3
H H67C 0.2539 0.6216 0.9273 0.122 Uiso calc U P R 0.591(5) G 3
N N1 0.62923(17) 0.73278(16) 0.48855(17) 0.0177(5) Uani d . . . 1.0 . .
N N2 0.32286(18) 0.72424(17) 0.46986(18) 0.0208(5) Uani d . . . 1.0 . .
O O1 0.42087(15) 0.57187(14) 0.37835(14) 0.0205(4) Uani d . . . 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 O1 . 1.844(2) ?
Al1 C1 . 1.932(3) ?
Al1 Cl1 . 2.1185(11) ?
Al1 N1 . 2.181(2) ?
Al1 N2 . 2.213(2) ?
B1 C54 . 1.639(4) ?
B1 C42 . 1.640(4) ?
B1 C36 . 1.647(4) ?
B1 C48 . 1.649(4) ?
C1 C2 . 1.384(4) ?
C1 C6 . 1.385(4) ?
C2 C3 . 1.395(4) ?
C2 C69 . 1.471(4) ?
C3 C4 . 1.394(4) ?
C4 C5 . 1.395(4) ?
C5 C6 . 1.398(4) ?
C6 C7 . 1.472(4) ?
C7 N1 . 1.290(3) ?
C8 C9 . 1.399(4) ?
C8 C16 . 1.411(4) ?
C8 N1 . 1.447(3) ?
C9 C13 . 1.401(4) ?
C9 C10 . 1.516(4) ?
C10 C12 . 1.522(4) ?
C10 C11 . 1.541(4) ?
C13 C14 . 1.380(5) ?
C14 C15 . 1.381(5) ?
C15 C16 . 1.383(4) ?
C16 C17 . 1.525(4) ?
C17 C19 . 1.532(4) ?
C17 C18 . 1.533(5) ?
C20 C21 . 1.399(5) ?
C20 C28 . 1.399(5) ?
C20 N2 . 1.451(4) ?
C21 C25 . 1.400(4) ?
C21 C22 . 1.513(5) ?
C22 C24 . 1.531(5) ?
C22 C23 . 1.545(4) ?
C25 C26 . 1.372(6) ?
C26 C27 . 1.379(6) ?
C27 C28 . 1.407(4) ?
C28 C29 . 1.516(5) ?
C29 C31 . 1.529(5) ?
C29 C30 . 1.540(4) ?
C32 O1 . 1.492(3) ?
C32 C33 . 1.509(5) ?
C33 C34 . 1.518(5) ?
C34 C35 . 1.521(4) ?
C35 O1 . 1.483(3) ?
C36 C37 . 1.399(4) ?
C36 C41 . 1.402(4) ?
C37 C38 . 1.387(4) ?
C38 C39 . 1.384(5) ?
C38 Cl2 . 1.749(3) ?
C39 C40 . 1.377(5) ?
C40 C41 . 1.387(4) ?
C40 Cl3 . 1.749(3) ?
C42 C47 . 1.394(4) ?
C42 C43 . 1.402(4) ?
C43 C44 . 1.384(4) ?
C44 C45 . 1.383(4) ?
C44 Cl4 . 1.750(3) ?
C45 C46 . 1.381(4) ?
C46 C47 . 1.390(4) ?
C46 Cl5 . 1.744(3) ?
C48 C49 . 1.391(4) ?
C48 C53 . 1.404(4) ?
C49 C50 . 1.385(4) ?
C50 C51 . 1.383(4) ?
C50 Cl6 . 1.752(3) ?
C51 C52 . 1.385(4) ?
C52 C53 . 1.387(4) ?
C52 Cl7 . 1.751(3) ?
C54 C59 . 1.403(4) ?
C54 C55 . 1.405(4) ?
C55 C56 . 1.385(4) ?
C56 C57 . 1.388(4) ?
C56 Cl8 . 1.741(3) ?
C57 C58 . 1.385(4) ?
C58 C59 . 1.387(4) ?
C58 Cl9 . 1.750(3) ?
C69 N2 . 1.285(4) ?
C61 Cl11 . 1.732(15) ?
C61 Cl10 . 1.765(13) ?
C61A Cl2A . 1.67(2) ?
C61A Cl1A . 1.750(15) ?
C61B Cl2B . 1.750(17) ?
C61B Cl1B . 1.750(17) ?
C61C Cl1C . 1.741(16) ?
C61C Cl2C . 1.765(15) ?
C62 Cl12 . 1.723(14) ?
C62 Cl13 . 1.831(15) ?
C68 Cl14 . 1.704(15) ?
C68 Cl15 . 1.729(16) ?
C63 C64 . 1.407(10) ?
C64 C65 . 1.539(12) ?
C65 C66 . 1.522(13) ?
C66 C67 . 1.549(14) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Al1 C1 . . 112.23(11) ?
O1 Al1 Cl1 . . 102.68(7) ?
C1 Al1 Cl1 . . 145.07(10) ?
O1 Al1 N1 . . 100.40(9) ?
C1 Al1 N1 . . 78.32(10) ?
Cl1 Al1 N1 . . 96.81(7) ?
O1 Al1 N2 . . 96.36(10) ?
C1 Al1 N2 . . 77.83(10) ?
Cl1 Al1 N2 . . 97.86(7) ?
N1 Al1 N2 . . 154.69(9) ?
C54 B1 C42 . . 114.4(2) ?
C54 B1 C36 . . 104.9(2) ?
C42 B1 C36 . . 110.5(2) ?
C54 B1 C48 . . 111.6(2) ?
C42 B1 C48 . . 102.5(2) ?
C36 B1 C48 . . 113.1(2) ?
C2 C1 C6 . . 120.5(2) ?
C2 C1 Al1 . . 120.1(2) ?
C6 C1 Al1 . . 119.3(2) ?
C1 C2 C3 . . 120.4(3) ?
C1 C2 C69 . . 112.5(2) ?
C3 C2 C69 . . 127.0(2) ?
C4 C3 C2 . . 118.7(3) ?
C3 C4 C5 . . 121.5(3) ?
C4 C5 C6 . . 118.6(3) ?
C1 C6 C5 . . 120.3(3) ?
C1 C6 C7 . . 112.7(2) ?
C5 C6 C7 . . 126.7(2) ?
N1 C7 C6 . . 117.4(2) ?
C9 C8 C16 . . 122.5(3) ?
C9 C8 N1 . . 120.8(3) ?
C16 C8 N1 . . 116.6(2) ?
C8 C9 C13 . . 117.0(3) ?
C8 C9 C10 . . 123.6(2) ?
C13 C9 C10 . . 119.4(3) ?
C9 C10 C12 . . 110.8(3) ?
C9 C10 C11 . . 112.2(3) ?
C12 C10 C11 . . 110.1(3) ?
C14 C13 C9 . . 121.3(3) ?
C13 C14 C15 . . 120.4(3) ?
C14 C15 C16 . . 121.1(3) ?
C15 C16 C8 . . 117.7(3) ?
C15 C16 C17 . . 120.0(3) ?
C8 C16 C17 . . 122.2(3) ?
C16 C17 C19 . . 109.9(3) ?
C16 C17 C18 . . 112.8(3) ?
C19 C17 C18 . . 110.8(3) ?
C21 C20 C28 . . 122.9(3) ?
C21 C20 N2 . . 120.1(3) ?
C28 C20 N2 . . 117.0(3) ?
C20 C21 C25 . . 117.4(3) ?
C20 C21 C22 . . 122.9(3) ?
C25 C21 C22 . . 119.4(3) ?
C21 C22 C24 . . 114.2(3) ?
C21 C22 C23 . . 109.2(3) ?
C24 C22 C23 . . 109.3(3) ?
C26 C25 C21 . . 120.8(4) ?
C25 C26 C27 . . 121.1(3) ?
C26 C27 C28 . . 120.7(3) ?
C20 C28 C27 . . 117.1(3) ?
C20 C28 C29 . . 121.4(3) ?
C27 C28 C29 . . 121.3(3) ?
C28 C29 C31 . . 113.2(3) ?
C28 C29 C30 . . 110.2(3) ?
C31 C29 C30 . . 110.4(3) ?
O1 C32 C33 . . 103.9(2) ?
C32 C33 C34 . . 105.1(3) ?
C33 C34 C35 . . 103.3(3) ?
O1 C35 C34 . . 104.7(2) ?
C37 C36 C41 . . 116.8(3) ?
C37 C36 B1 . . 123.3(2) ?
C41 C36 B1 . . 119.9(3) ?
C38 C37 C36 . . 120.4(3) ?
C39 C38 C37 . . 122.7(3) ?
C39 C38 Cl2 . . 117.5(2) ?
C37 C38 Cl2 . . 119.8(3) ?
C40 C39 C38 . . 116.7(3) ?
C39 C40 C41 . . 122.0(3) ?
C39 C40 Cl3 . . 118.4(2) ?
C41 C40 Cl3 . . 119.6(3) ?
C40 C41 C36 . . 121.2(3) ?
C47 C42 C43 . . 116.6(2) ?
C47 C42 B1 . . 123.7(2) ?
C43 C42 B1 . . 119.3(2) ?
C44 C43 C42 . . 120.9(3) ?
C45 C44 C43 . . 122.8(3) ?
C45 C44 Cl4 . . 118.3(2) ?
C43 C44 Cl4 . . 118.9(2) ?
C46 C45 C44 . . 116.1(3) ?
C45 C46 C47 . . 122.5(3) ?
C45 C46 Cl5 . . 118.6(2) ?
C47 C46 Cl5 . . 118.9(2) ?
C46 C47 C42 . . 121.1(3) ?
C49 C48 C53 . . 116.5(2) ?
C49 C48 B1 . . 122.3(2) ?
C53 C48 B1 . . 120.8(2) ?
C50 C49 C48 . . 121.3(3) ?
C51 C50 C49 . . 122.7(3) ?
C51 C50 Cl6 . . 118.3(2) ?
C49 C50 Cl6 . . 119.0(2) ?
C50 C51 C52 . . 115.9(2) ?
C51 C52 C53 . . 122.6(3) ?
C51 C52 Cl7 . . 118.1(2) ?
C53 C52 Cl7 . . 119.2(2) ?
C52 C53 C48 . . 120.9(3) ?
C59 C54 C55 . . 116.4(2) ?
C59 C54 B1 . . 122.6(2) ?
C55 C54 B1 . . 120.7(2) ?
C56 C55 C54 . . 121.6(2) ?
C55 C56 C57 . . 122.0(2) ?
C55 C56 Cl8 . . 120.0(2) ?
C57 C56 Cl8 . . 118.0(2) ?
C58 C57 C56 . . 116.3(2) ?
C57 C58 C59 . . 122.9(2) ?
C57 C58 Cl9 . . 117.3(2) ?
C59 C58 Cl9 . . 119.8(2) ?
C58 C59 C54 . . 120.7(2) ?
N2 C69 C2 . . 118.3(2) ?
Cl11 C61 Cl10 . . 110.8(10) ?
Cl2A C61A Cl1A . . 112.5(10) ?
Cl2B C61B Cl1B . . 108.6(15) ?
Cl1C C61C Cl2C . . 107.9(12) ?
Cl12 C62 Cl13 . . 106.9(10) ?
Cl14 C68 Cl15 . . 110.8(12) ?
C63 C64 C65 . . 99.1(8) ?
C66 C65 C64 . . 95.6(9) ?
C65 C66 C67 . . 101.1(9) ?
C7 N1 C8 . . 118.1(2) ?
C7 N1 Al1 . . 112.01(18) ?
C8 N1 Al1 . . 128.68(17) ?
C69 N2 C20 . . 118.7(2) ?
C69 N2 Al1 . . 111.18(18) ?
C20 N2 Al1 . . 130.04(17) ?
C35 O1 C32 . . 110.2(2) ?
C35 O1 Al1 . . 123.02(17) ?
C32 O1 Al1 . . 126.08(17) ?

