# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_sanj_a
_database_code_depnum_ccdc_archive 'CCDC 2000071'
loop_
_audit_author_name
_audit_author_address
'vsvsnswamy swamysaivarre'
;National Chemical Laboratory
India
;
_audit_update_record             
;
2020-04-29 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'Al(III) compound'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H30 Al Cl2 N3, 2(C6 H6)'
_chemical_formula_sum            'C35 H42 Al Cl2 N3'
_chemical_formula_weight         602.59

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

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

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

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

_cell_length_a                   17.2631(13)
_cell_length_b                   10.6231(7)
_cell_length_c                   18.1589(13)
_cell_angle_alpha                90
_cell_angle_beta                 103.330(3)
_cell_angle_gamma                90
_cell_volume                     3240.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9114
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      28.27

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_F_000             1280
_exptl_transmission_factor_min   0.921
_exptl_transmission_factor_max   0.970
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.256
_shelx_estimated_absorpt_T_min   0.923
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (BRUKER, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            140823
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.305
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5699
_reflns_number_gt                4941
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0331P)²+2.9606P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5699
_refine_ls_number_parameters     377
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0862
_refine_ls_wR_factor_gt          0.0793
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cl1 Cl 0.34777(3) 0.54518(4) 0.52679(3) 0.02092(12) Uani 1 1 d . . . . .
Cl2 Cl 0.32492(2) 0.79332(4) 0.38140(2) 0.01873(11) Uani 1 1 d . . . . .
Al1 Al 0.32019(3) 0.74272(5) 0.49749(3) 0.01227(12) Uani 1 1 d . . . . .
N2 N 0.32036(8) 0.84778(13) 0.58283(8) 0.0139(3) Uani 1 1 d . . . . .
N1 N 0.20263(8) 0.73191(12) 0.47324(8) 0.0124(3) Uani 1 1 d . . . . .
N3 N 0.43927(8) 0.78995(13) 0.52839(8) 0.0150(3) Uani 1 1 d . . . . .
C3 C 0.26853(10) 0.83250(15) 0.62679(9) 0.0152(4) Uani 1 1 d . . . . .
C1 C 0.16314(10) 0.72859(15) 0.52841(10) 0.0148(4) Uani 1 1 d . . . . .
C13 C 0.13707(10) 0.60923(16) 0.35915(9) 0.0135(3) Uani 1 1 d . . . . .
C12 C 0.15500(10) 0.72515(16) 0.39611(9) 0.0130(3) Uani 1 1 d . . . . .
C6 C 0.38945(10) 0.92999(16) 0.60995(10) 0.0173(4) Uani 1 1 d . . . . .
H6A H 0.4055 0.9271 0.6659 0.021 Uiso 1 1 calc R U . . .
H6B H 0.3755 1.0180 0.5944 0.021 Uiso 1 1 calc R U . . .
C7 C 0.45697(10) 0.88613(16) 0.57695(9) 0.0150(4) Uani 1 1 d . . . . .
C16 C 0.08435(10) 0.83411(16) 0.28424(10) 0.0165(4) Uani 1 1 d . . . . .
H16 H 0.0663 0.9102 0.2585 0.020 Uiso 1 1 calc R U . . .
C2 C 0.19805(11) 0.76459(16) 0.60301(10) 0.0177(4) Uani 1 1 d . . . . .
H2 H 0.1711 0.7404 0.6409 0.021 Uiso 1 1 calc R U . . .
C15 C 0.06664(10) 0.72026(17) 0.24692(10) 0.0170(4) Uani 1 1 d . . . . .
H15 H 0.0368 0.7185 0.1960 0.020 Uiso 1 1 calc R U . . .
C21 C 0.16431(10) 0.48446(16) 0.39709(10) 0.0161(4) Uani 1 1 d . . . . .
H21 H 0.1885 0.5012 0.4517 0.019 Uiso 1 1 calc R U . . .
C17 C 0.12828(10) 0.83882(16) 0.35896(10) 0.0152(4) Uani 1 1 d . . . . .
C5 C 0.28353(11) 0.89123(17) 0.70437(10) 0.0200(4) Uani 1 1 d . . . . .
H5A H 0.3341 0.8600 0.7353 0.030 Uiso 1 1 calc R U . . .
H5B H 0.2402 0.8689 0.7285 0.030 Uiso 1 1 calc R U . . .
H5C H 0.2861 0.9830 0.6998 0.030 Uiso 1 1 calc R U . . .
C8 C 0.53249(11) 0.93932(17) 0.59584(10) 0.0193(4) Uani 1 1 d . . . . .
H8 H 0.5432 1.0094 0.6291 0.023 Uiso 1 1 calc R U . . .
C11 C 0.49767(11) 0.73946(17) 0.49954(10) 0.0189(4) Uani 1 1 d . . . . .
H11 H 0.4855 0.6697 0.4661 0.023 Uiso 1 1 calc R U . . .
C14 C 0.09265(10) 0.60929(16) 0.28419(10) 0.0158(4) Uani 1 1 d . . . . .
H14 H 0.0801 0.5315 0.2584 0.019 Uiso 1 1 calc R U . . .
C23 C 0.22842(11) 0.42555(17) 0.36188(11) 0.0208(4) Uani 1 1 d . . . . .
H23A H 0.2048 0.4014 0.3094 0.031 Uiso 1 1 calc R U . . .
H23B H 0.2504 0.3508 0.3909 0.031 Uiso 1 1 calc R U . . .
H23C H 0.2711 0.4868 0.3628 0.031 Uiso 1 1 calc R U . . .
C18 C 0.14447(11) 0.96553(16) 0.39864(10) 0.0193(4) Uani 1 1 d . . . . .
H18 H 0.1868 0.9529 0.4459 0.023 Uiso 1 1 calc R U . . .
C4 C 0.07730(10) 0.68715(18) 0.51266(10) 0.0200(4) Uani 1 1 d . . . . .
H4A H 0.0466 0.7327 0.4686 0.030 Uiso 1 1 calc R U . . .
H4B H 0.0555 0.7053 0.5568 0.030 Uiso 1 1 calc R U . . .
H4C H 0.0741 0.5965 0.5024 0.030 Uiso 1 1 calc R U . . .
C10 C 0.57412(11) 0.78551(18) 0.51682(11) 0.0224(4) Uani 1 1 d . . . . .
H10 H 0.6143 0.7479 0.4961 0.027 Uiso 1 1 calc R U . . .
C9 C 0.59145(11) 0.88840(18) 0.56532(11) 0.0229(4) Uani 1 1 d . . . . .
H9 H 0.6435 0.9232 0.5773 0.027 Uiso 1 1 calc R U . . .
C22 C 0.09444(11) 0.39334(17) 0.39249(11) 0.0230(4) Uani 1 1 d . . . . .
H22A H 0.0514 0.4362 0.4095 0.034 Uiso 1 1 calc R U . . .
H22B H 0.1122 0.3203 0.4250 0.034 Uiso 1 1 calc R U . . .
H22C H 0.0751 0.3652 0.3401 0.034 Uiso 1 1 calc R U . . .
C29 C 0.46534(12) 0.6693(2) 0.73928(12) 0.0306(5) Uani 1 1 d . . . . .
H29 H 0.4111 0.6469 0.7341 0.037 Uiso 1 1 calc R U . . .
C20 C 0.06964(12) 1.01330(18) 0.42169(11) 0.0247(4) Uani 1 1 d . . . . .
H20A H 0.0262 1.0222 0.3765 0.037 Uiso 1 1 calc R U . . .
H20B H 0.0808 1.0952 0.4467 0.037 Uiso 1 1 calc R U . . .
H20C H 0.0541 0.9531 0.4566 0.037 Uiso 1 1 calc R U . . .
C24 C 0.50046(13) 0.7565(2) 0.79294(12) 0.0317(5) Uani 1 1 d . . . . .
H24 H 0.4703 0.7943 0.8246 0.038 Uiso 1 1 calc R U . . .
C31 C 0.79950(12) 0.66647(19) 0.91863(11) 0.0281(4) Uani 1 1 d . . . . .
H31 H 0.7743 0.5998 0.9391 0.034 Uiso 1 1 calc R U . . .
C30 C 0.77639(12) 0.78916(19) 0.92573(11) 0.0275(4) Uani 1 1 d . . . . .
H30 H 0.7356 0.8069 0.9515 0.033 Uiso 1 1 calc R U . . .
C19 C 0.17443(12) 1.06386(17) 0.35050(12) 0.0282(5) Uani 1 1 d . . . . .
H19A H 0.2173 1.0276 0.3300 0.042 Uiso 1 1 calc R U . . .
H19B H 0.1947 1.1372 0.3818 0.042 Uiso 1 1 calc R U . . .
H19C H 0.1306 1.0899 0.3087 0.042 Uiso 1 1 calc R U . . .
C28 C 0.50915(13) 0.61468(19) 0.69304(12) 0.0306(5) Uani 1 1 d . . . . .
H28 H 0.4851 0.5551 0.6558 0.037 Uiso 1 1 calc R U . . .
C25 C 0.57967(13) 0.7890(2) 0.80075(12) 0.0323(5) Uani 1 1 d . . . . .
H25 H 0.6036 0.8493 0.8376 0.039 Uiso 1 1 calc R U . . .
C27 C 0.58829(13) 0.6472(2) 0.70127(12) 0.0325(5) Uani 1 1 d . . . . .
H27 H 0.6185 0.6096 0.6695 0.039 Uiso 1 1 calc R U . . .
C26 C 0.62368(13) 0.7337(2) 0.75509(12) 0.0329(5) Uani 1 1 d . . . . .
H26 H 0.6782 0.7551 0.7607 0.039 Uiso 1 1 calc R U . . .
C32 C 0.85925(13) 0.6404(2) 0.88179(12) 0.0339(5) Uani 1 1 d . . . . .
H32 H 0.8751 0.5558 0.8769 0.041 Uiso 1 1 calc R U . . .
C35 C 0.81217(13) 0.8864(2) 0.89561(12) 0.0318(5) Uani 1 1 d . . . . .
H35 H 0.7955 0.9708 0.8998 0.038 Uiso 1 1 calc R U . . .
C33 C 0.89577(13) 0.7366(2) 0.85221(13) 0.0393(6) Uani 1 1 d . . . . .
H33 H 0.9369 0.7187 0.8269 0.047 Uiso 1 1 calc R U . . .
C34 C 0.87222(14) 0.8605(2) 0.85938(12) 0.0385(6) Uani 1 1 d . . . . .
H34 H 0.8976 0.9273 0.8393 0.046 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 Al1 2.1901(7) . ?
Cl2 Al1 2.1953(7) . ?
Al1 N2 1.9092(15) . ?
Al1 N1 1.9783(15) . ?
Al1 N3 2.0641(15) . ?
N2 C3 1.339(2) . ?
N2 C6 1.469(2) . ?
N1 C1 1.336(2) . ?
N1 C12 1.453(2) . ?
N3 C7 1.338(2) . ?
N3 C11 1.350(2) . ?
C3 C2 1.395(2) . ?
C3 C5 1.508(2) . ?
C1 C2 1.403(2) . ?
C1 C4 1.509(2) . ?
C13 C14 1.400(2) . ?
C13 C12 1.402(2) . ?
C13 C21 1.518(2) . ?
C12 C17 1.408(2) . ?
C6 C7 1.502(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.389(2) . ?
C16 C15 1.386(2) . ?
C16 C17 1.394(2) . ?
C16 H16 0.9500 . ?
C2 H2 0.9500 . ?
C15 C14 1.382(2) . ?
C15 H15 0.9500 . ?
C21 C23 1.533(2) . ?
C21 C22 1.534(2) . ?
C21 H21 1.0000 . ?
C17 C18 1.522(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C8 C9 1.377(3) . ?
C8 H8 0.9500 . ?
C11 C10 1.374(3) . ?
C11 H11 0.9500 . ?
C14 H14 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C18 C19 1.527(3) . ?
C18 C20 1.533(3) . ?
C18 H18 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C10 C9 1.392(3) . ?
C10 H10 0.9500 . ?
C9 H9 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C29 C24 1.379(3) . ?
C29 C28 1.381(3) . ?
C29 H29 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C24 C25 1.385(3) . ?
C24 H24 0.9500 . ?
C31 C30 1.378(3) . ?
C31 C32 1.381(3) . ?
C31 H31 0.9500 . ?
C30 C35 1.380(3) . ?
C30 H30 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C28 C27 1.384(3) . ?
C28 H28 0.9500 . ?
C25 C26 1.378(3) . ?
C25 H25 0.9500 . ?
C27 C26 1.377(3) . ?
C27 H27 0.9500 . ?
C26 H26 0.9500 . ?
C32 C33 1.373(3) . ?
C32 H32 0.9500 . ?
C35 C34 1.377(3) . ?
C35 H35 0.9500 . ?
C33 C34 1.392(3) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Al1 N1 91.38(6) . . ?
N2 Al1 N3 79.76(6) . . ?
N1 Al1 N3 168.78(6) . . ?
N2 Al1 Cl1 113.79(5) . . ?
N1 Al1 Cl1 98.79(4) . . ?
N3 Al1 Cl1 91.13(4) . . ?
N2 Al1 Cl2 130.01(5) . . ?
N1 Al1 Cl2 93.66(5) . . ?
N3 Al1 Cl2 86.92(4) . . ?
Cl1 Al1 Cl2 114.44(3) . . ?
C3 N2 C6 118.34(14) . . ?
C3 N2 Al1 122.46(11) . . ?
C6 N2 Al1 117.97(11) . . ?
C1 N1 C12 116.63(14) . . ?
C1 N1 Al1 120.62(11) . . ?
C12 N1 Al1 122.74(11) . . ?
C7 N3 C11 118.79(15) . . ?
C7 N3 Al1 115.25(11) . . ?
C11 N3 Al1 125.73(12) . . ?
N2 C3 C2 122.23(15) . . ?
N2 C3 C5 120.82(15) . . ?
C2 C3 C5 116.94(15) . . ?
N1 C1 C2 122.48(16) . . ?
N1 C1 C4 120.96(15) . . ?
C2 C1 C4 116.55(15) . . ?
C14 C13 C12 118.42(15) . . ?
C14 C13 C21 119.00(15) . . ?
C12 C13 C21 122.58(15) . . ?
C13 C12 C17 120.80(15) . . ?
C13 C12 N1 121.20(14) . . ?
C17 C12 N1 117.99(14) . . ?
N2 C6 C7 109.06(14) . . ?
N2 C6 H6A 109.9 . . ?
C7 C6 H6A 109.9 . . ?
N2 C6 H6B 109.9 . . ?
C7 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N3 C7 C8 122.14(16) . . ?
N3 C7 C6 114.80(15) . . ?
C8 C7 C6 123.06(15) . . ?
C15 C16 C17 121.10(16) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C3 C2 C1 126.15(16) . . ?
C3 C2 H2 116.9 . . ?
C1 C2 H2 116.9 . . ?
C14 C15 C16 119.67(16) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C13 C21 C23 110.18(14) . . ?
C13 C21 C22 111.65(14) . . ?
C23 C21 C22 110.72(15) . . ?
C13 C21 H21 108.1 . . ?
C23 C21 H21 108.1 . . ?
C22 C21 H21 108.1 . . ?
C16 C17 C12 118.68(15) . . ?
C16 C17 C18 119.46(15) . . ?
C12 C17 C18 121.84(15) . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C9 C8 C7 118.65(17) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
N3 C11 C10 122.26(17) . . ?
N3 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C15 C14 C13 121.33(16) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C17 C18 C19 112.56(15) . . ?
C17 C18 C20 110.34(15) . . ?
C19 C18 C20 110.35(15) . . ?
C17 C18 H18 107.8 . . ?
C19 C18 H18 107.8 . . ?
C20 C18 H18 107.8 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C11 C10 C9 118.62(17) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C8 C9 C10 119.47(17) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C29 C28 119.9(2) . . ?
C24 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C29 C24 C25 120.2(2) . . ?
C29 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C30 C31 C32 120.0(2) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C30 C35 120.4(2) . . ?
C31 C30 H30 119.8 . . ?
C35 C30 H30 119.8 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C29 C28 C27 119.7(2) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C26 C25 C24 120.0(2) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C27 C28 120.6(2) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C26 C25 119.7(2) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C33 C32 C31 120.1(2) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C34 C35 C30 119.7(2) . . ?
C34 C35 H35 120.2 . . ?
C30 C35 H35 120.2 . . ?
C32 C33 C34 119.8(2) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C35 C34 C33 120.1(2) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?

_refine_diff_density_max         0.856
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.047



####################################################################### 
# 
# 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_sp__a
_database_code_depnum_ccdc_archive 'CCDC 2000154'
loop_
_audit_author_name
_audit_author_address
'vsvsnswamy swamysaivarre'
;National Chemical Laboratory
India
;
_audit_update_record             
;
2020-04-29 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_space_group_name_Hall           '-P 1'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
_cell_length_a                   7.9051(3)
_cell_length_b                   8.8862(4)
_cell_length_c                   9.0373(4)
_cell_angle_alpha                67.589(2)
_cell_angle_beta                 74.175(2)
_cell_angle_gamma                77.444(2)
_cell_volume                     560.036
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Ge1 Ge 0.16967(2) 0.33139(2) 0.33140(2)
Cl1 Cl 0.46073(5) 0.22028(4) 0.26271(5)
N2 N 0.17105(16) 0.28619(15) 0.55875(15)
N1 N 0.24696(15) 0.54361(14) 0.31300(15)
C5 C 0.26019(18) 0.55236(17) 0.45705(18)
C6 C 0.20987(18) 0.41041(18) 0.59646(18)
C7 C 0.19994(19) 0.3589(2) 0.76464(19)
C9 C 0.13763(19) 0.15617(19) 0.70070(19)
C1 C 0.29128(19) 0.66613(18) 0.17059(18)
H1 H 0.2791 0.6585 0.0732
C4 C 0.32223(19) 0.68821(19) 0.4562(2)
H4 H 0.3313 0.6960 0.5546
C2 C 0.3534(2) 0.80086(19) 0.1637(2)
H2 H 0.3841 0.8848 0.0631
C3 C 0.3703(2) 0.81155(19) 0.3082(2)
H3 H 0.4145 0.9027 0.3056
C11 C 0.0964(2) 0.00021(19) 0.7004(2)
H11A H -0.0227 0.0165 0.6822
H11B H 0.1044 -0.0854 0.8050
H11C H 0.1805 -0.0318 0.6137
C8 C 0.1540(2) 0.1984(2) 0.82757(19)
H8 H 0.1373 0.1308 0.9383
C10 C 0.2326(2) 0.4520(2) 0.8599(2)
H10A H 0.3494 0.4874 0.8140
H10B H 0.2260 0.3816 0.9734
H10C H 0.1437 0.5472 0.8540

#END
####################################################################### 
# 
# 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_sen02_a
_database_code_depnum_ccdc_archive 'CCDC 2000072'
loop_
_audit_author_name
_audit_author_address
'vsvsnswamy swamysaivarre'
;National Chemical Laboratory
India
;
_audit_update_record             
;
2020-04-29 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H30 Cl Ge N3'
_chemical_formula_sum            'C23 H30 Cl Ge N3'
_chemical_formula_weight         456.54

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.7669(4)
_cell_length_b                   11.2877(4)
_cell_length_c                   18.6038(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.881(2)
_cell_angle_gamma                90
_cell_volume                     2244.70(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    105(2)
_cell_measurement_reflns_used    9897
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      28.15

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   0.578
_exptl_transmission_factor_max   0.787
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.497
_shelx_estimated_absorpt_T_min   0.615
_shelx_estimated_absorpt_T_max   0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (BRUKER, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      105(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33365
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.084
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3954
_reflns_number_gt                3576
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0254P)²+1.7847P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3954
_refine_ls_number_parameters     260
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0595
_refine_ls_wR_factor_gt          0.0574
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ge1 Ge 0.68799(2) 0.59972(2) 0.65837(2) 0.01503(8) Uani 1 1 d . . . . .
Cl1 Cl 0.88813(4) 0.66736(4) 0.70510(3) 0.02131(12) Uani 1 1 d . . . . .
N1 N 0.63982(14) 0.74900(13) 0.60964(8) 0.0130(3) Uani 1 1 d . . . . .
N2 N 0.61493(14) 0.65163(14) 0.74460(8) 0.0170(3) Uani 1 1 d . . . . .
N3 N 0.35732(16) 0.62464(17) 0.74597(11) 0.0330(5) Uani 1 1 d . . . . .
C12 C 0.60955(18) 0.74246(16) 0.53160(10) 0.0156(4) Uani 1 1 d . . . . .
C3 C 0.60792(17) 0.76433(18) 0.76456(10) 0.0179(4) Uani 1 1 d . . . . .
C1 C 0.63026(17) 0.85188(17) 0.64421(10) 0.0161(4) Uani 1 1 d . . . . .
C17 C 0.48488(18) 0.72225(17) 0.50319(10) 0.0183(4) Uani 1 1 d . . . . .
C7 C 0.42936(18) 0.53607(17) 0.77481(10) 0.0182(4) Uani 1 1 d . . . . .
C13 C 0.70565(19) 0.75143(17) 0.48712(11) 0.0205(4) Uani 1 1 d . . . . .
C2 C 0.62944(17) 0.85863(17) 0.71879(10) 0.0175(4) Uani 1 1 d . . . . .
H2 H 0.6449 0.9341 0.7407 0.021 Uiso 1 1 calc R U . . .
C18 C 0.38072(18) 0.70693(18) 0.55134(11) 0.0211(4) Uani 1 1 d . . . . .
H18 H 0.4187 0.7143 0.6029 0.025 Uiso 1 1 calc R U . . .
C6 C 0.56955(18) 0.55544(19) 0.78788(11) 0.0223(4) Uani 1 1 d . . . . .
H6A H 0.5932 0.5733 0.8398 0.027 Uiso 1 1 calc R U . . .
H6B H 0.6121 0.4810 0.7769 0.027 Uiso 1 1 calc R U . . .
C21 C 0.84174(19) 0.76810(18) 0.51784(11) 0.0227(4) Uani 1 1 d . . . . .
H21 H 0.8444 0.7848 0.5708 0.027 Uiso 1 1 calc R U . . .
C4 C 0.61507(20) 0.96508(17) 0.60128(11) 0.0238(5) Uani 1 1 d . . . . .
H4A H 0.6800 0.9697 0.5687 0.036 Uiso 1 1 calc R U . . .
H4B H 0.6230 1.0329 0.6344 0.036 Uiso 1 1 calc R U . . .
H4C H 0.5324 0.9664 0.5728 0.036 Uiso 1 1 calc R U . . .
C10 C 0.17664(19) 0.50392(19) 0.75474(12) 0.0287(5) Uani 1 1 d . . . . .
H10 H 0.0883 0.4956 0.7469 0.034 Uiso 1 1 calc R U . . .
C16 C 0.4572(2) 0.71400(19) 0.42807(11) 0.0257(5) Uani 1 1 d . . . . .
H16 H 0.3732 0.7011 0.4075 0.031 Uiso 1 1 calc R U . . .
C5 C 0.5712(2) 0.7960(2) 0.83781(11) 0.0279(5) Uani 1 1 d . . . . .
H5A H 0.4825 0.7778 0.8390 0.042 Uiso 1 1 calc R U . . .
H5B H 0.5855 0.8807 0.8468 0.042 Uiso 1 1 calc R U . . .
H5C H 0.6218 0.7500 0.8752 0.042 Uiso 1 1 calc R U . . .
C14 C 0.6724(2) 0.7418(2) 0.41232(11) 0.0287(5) Uani 1 1 d . . . . .
H14 H 0.7355 0.7474 0.3809 0.034 Uiso 1 1 calc R U . . .
C8 C 0.3794(2) 0.43016(18) 0.79475(12) 0.0279(5) Uani 1 1 d . . . . .
H8 H 0.4326 0.3687 0.8152 0.033 Uiso 1 1 calc R U . . .
C15 C 0.5497(2) 0.7243(2) 0.38340(11) 0.0305(5) Uani 1 1 d . . . . .
H15 H 0.5289 0.7193 0.3324 0.037 Uiso 1 1 calc R U . . .
C23 C 0.9166(2) 0.65456(19) 0.50928(12) 0.0283(5) Uani 1 1 d . . . . .
H23A H 0.8814 0.5897 0.5354 0.042 Uiso 1 1 calc R U . . .
H23B H 1.0041 0.6672 0.5291 0.042 Uiso 1 1 calc R U . . .
H23C H 0.9122 0.6342 0.4578 0.042 Uiso 1 1 calc R U . . .
C9 C 0.2508(2) 0.4141(2) 0.78478(13) 0.0327(5) Uani 1 1 d . . . . .
H9 H 0.2148 0.3420 0.7986 0.039 Uiso 1 1 calc R U . . .
C22 C 0.9014(2) 0.8737(2) 0.48293(14) 0.0341(5) Uani 1 1 d . . . . .
H22A H 0.9010 0.8590 0.4310 0.051 Uiso 1 1 calc R U . . .
H22B H 0.9878 0.8838 0.5055 0.051 Uiso 1 1 calc R U . . .
H22C H 0.8535 0.9457 0.4900 0.051 Uiso 1 1 calc R U . . .
C19 C 0.2809(2) 0.8037(2) 0.53671(13) 0.0347(6) Uani 1 1 d . . . . .
H19A H 0.3195 0.8816 0.5463 0.052 Uiso 1 1 calc R U . . .
H19B H 0.2156 0.7918 0.5685 0.052 Uiso 1 1 calc R U . . .
H19C H 0.2437 0.7995 0.4860 0.052 Uiso 1 1 calc R U . . .
C11 C 0.2334(2) 0.6059(2) 0.73640(15) 0.0382(6) Uani 1 1 d . . . . .
H11 H 0.1815 0.6680 0.7154 0.046 Uiso 1 1 calc R U . . .
C20 C 0.3222(2) 0.5846(2) 0.54143(15) 0.0411(6) Uani 1 1 d . . . . .
H20A H 0.2852 0.5749 0.4910 0.062 Uiso 1 1 calc R U . . .
H20B H 0.2569 0.5760 0.5735 0.062 Uiso 1 1 calc R U . . .
H20C H 0.3866 0.5241 0.5533 0.062 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.9539(15) . ?
Ge1 N2 1.9591(16) . ?
Ge1 Cl1 2.3523(5) . ?
N1 C1 1.337(2) . ?
N1 C12 1.451(2) . ?
N2 C3 1.330(3) . ?
N2 C6 1.470(2) . ?
N3 C7 1.338(3) . ?
N3 C11 1.341(3) . ?
C12 C17 1.401(3) . ?
C12 C13 1.404(3) . ?
C3 C2 1.400(3) . ?
C3 C5 1.507(3) . ?
C1 C2 1.391(3) . ?
C1 C4 1.505(3) . ?
C17 C16 1.397(3) . ?
C17 C18 1.527(3) . ?
C7 C8 1.380(3) . ?
C7 C6 1.516(3) . ?
C13 C14 1.399(3) . ?
C13 C21 1.519(3) . ?
C2 H2 0.9500 . ?
C18 C20 1.520(3) . ?
C18 C19 1.534(3) . ?
C18 H18 1.0000 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C21 C23 1.532(3) . ?
C21 C22 1.534(3) . ?
C21 H21 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C10 C11 1.366(3) . ?
C10 C9 1.367(3) . ?
C10 H10 0.9500 . ?
C16 C15 1.376(3) . ?
C16 H16 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C14 C15 1.381(3) . ?
C14 H14 0.9500 . ?
C8 C9 1.387(3) . ?
C8 H8 0.9500 . ?
C15 H15 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C9 H9 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C11 H11 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 N2 90.67(6) . . ?
N1 Ge1 Cl1 94.13(5) . . ?
N2 Ge1 Cl1 92.30(5) . . ?
C1 N1 C12 120.29(15) . . ?
C1 N1 Ge1 123.85(12) . . ?
C12 N1 Ge1 115.82(11) . . ?
C3 N2 C6 121.33(17) . . ?
C3 N2 Ge1 123.82(13) . . ?
C6 N2 Ge1 114.84(13) . . ?
C7 N3 C11 117.09(19) . . ?
C17 C12 C13 122.00(17) . . ?
C17 C12 N1 118.41(16) . . ?
C13 C12 N1 119.54(17) . . ?
N2 C3 C2 122.59(17) . . ?
N2 C3 C5 120.61(18) . . ?
C2 C3 C5 116.77(18) . . ?
N1 C1 C2 122.51(17) . . ?
N1 C1 C4 119.44(17) . . ?
C2 C1 C4 118.01(17) . . ?
C16 C17 C12 117.94(18) . . ?
C16 C17 C18 119.71(18) . . ?
C12 C17 C18 122.35(17) . . ?
N3 C7 C8 121.95(19) . . ?
N3 C7 C6 118.36(17) . . ?
C8 C7 C6 119.66(18) . . ?
C14 C13 C12 117.53(19) . . ?
C14 C13 C21 120.25(18) . . ?
C12 C13 C21 122.21(17) . . ?
C1 C2 C3 125.91(18) . . ?
C1 C2 H2 117.0 . . ?
C3 C2 H2 117.0 . . ?
C20 C18 C17 110.79(17) . . ?
C20 C18 C19 110.71(18) . . ?
C17 C18 C19 111.33(17) . . ?
C20 C18 H18 108.0 . . ?
C17 C18 H18 108.0 . . ?
C19 C18 H18 108.0 . . ?
N2 C6 C7 114.13(16) . . ?
N2 C6 H6A 108.7 . . ?
C7 C6 H6A 108.7 . . ?
N2 C6 H6B 108.7 . . ?
C7 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
C13 C21 C23 110.66(17) . . ?
C13 C21 C22 111.77(17) . . ?
C23 C21 C22 110.70(17) . . ?
C13 C21 H21 107.8 . . ?
C23 C21 H21 107.8 . . ?
C22 C21 H21 107.8 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C11 C10 C9 118.0(2) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
C15 C16 C17 121.0(2) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C15 C14 C13 121.2(2) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C7 C8 C9 119.51(19) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C16 C15 C14 120.35(19) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C10 C9 C8 118.8(2) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C11 C10 124.6(2) . . ?
N3 C11 H11 117.7 . . ?
C10 C11 H11 117.7 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_refine_diff_density_max         0.370
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.052



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

data_mo_SWAMY_01_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2000073'
loop_
_audit_author_name
_audit_author_address
'vsvsnswamy swamysaivarre'
;National Chemical Laboratory
India
;
_audit_update_record             
;
2020-04-29 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H19 Cl2 Ge N'
_chemical_formula_sum            'C12 H19 Cl2 Ge N'
_chemical_formula_weight         320.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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'

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

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

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

_cell_length_a                   8.8999(6)
_cell_length_b                   9.3908(7)
_cell_length_c                   9.8279(7)
_cell_angle_alpha                91.216(2)
_cell_angle_beta                 109.977(2)
_cell_angle_gamma                110.198(2)
_cell_volume                     715.42(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9842
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      28.35

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_F_000             328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    2.490
_shelx_estimated_absorpt_T_min   0.451
_shelx_estimated_absorpt_T_max   0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_T_max  0.671
_exptl_absorpt_process_details   'SADABS (BRUKER, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26002
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.233
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2523
_reflns_number_gt                2355
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0143P)²+0.3674P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0023(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2523
_refine_ls_number_parameters     222
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0169
_refine_ls_wR_factor_ref         0.0399
_refine_ls_wR_factor_gt          0.0383
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.30271(19) 0.57650(18) 0.73068(16) 0.0090(3) Uani 1 1 d . . . . .
C2 C 0.3220(2) 0.73081(18) 0.74842(17) 0.0103(3) Uani 1 1 d . . . . .
C3 C 0.2596(2) 0.77676(19) 0.84704(18) 0.0128(3) Uani 1 1 d . . . . .
C4 C 0.1830(2) 0.67442(19) 0.92458(18) 0.0141(4) Uani 1 1 d . . . . .
C5 C 0.1637(2) 0.52214(19) 0.90341(18) 0.0131(3) Uani 1 1 d . . . . .
C6 C 0.2207(2) 0.46897(18) 0.80505(17) 0.0100(3) Uani 1 1 d . . . . .
C7 C 0.2035(2) 0.30152(18) 0.78634(18) 0.0121(3) Uani 1 1 d . . . . .
C8 C 0.0524(2) 0.1913(2) 0.8194(2) 0.0197(4) Uani 1 1 d . . . . .
C9 C 0.3714(2) 0.2864(2) 0.8836(2) 0.0181(4) Uani 1 1 d . . . . .
C10 C 0.4078(2) 0.85086(18) 0.66910(18) 0.0132(3) Uani 1 1 d . . . . .
C11 C 0.5732(2) 0.9729(2) 0.7777(2) 0.0196(4) Uani 1 1 d . . . . .
C12 C 0.2844(3) 0.9232(2) 0.5785(2) 0.0231(4) Uani 1 1 d . . . . .
Cl1 Cl 0.31592(5) 0.61980(5) 0.31179(4) 0.01603(10) Uani 1 1 d . . . . .
Cl2 Cl 0.23261(5) 0.25040(5) 0.36568(5) 0.01789(10) Uani 1 1 d . . . . .
Ge1 Ge 0.15095(2) 0.44561(2) 0.41112(2) 0.01150(7) Uani 1 1 d . . . . .
H1 H 0.388(2) 0.447(2) 0.6456(19) 0.013(5) Uiso 1 1 d . . . . .
H2 H 0.441(2) 0.590(2) 0.6152(19) 0.010(5) Uiso 1 1 d . . . . .
H3 H 0.274(2) 0.879(2) 0.8630(18) 0.011(4) Uiso 1 1 d . . . . .
H4 H 0.146(2) 0.7082(19) 0.9931(19) 0.010(4) Uiso 1 1 d . . . . .
H5 H 0.114(2) 0.452(2) 0.9581(19) 0.011(4) Uiso 1 1 d . . . . .
H6 H 0.437(2) 0.8035(19) 0.6011(18) 0.006(4) Uiso 1 1 d . . . . .
H7 H 0.182(2) 0.273(2) 0.685(2) 0.014(4) Uiso 1 1 d . . . . .
H8 H 0.627(3) 1.048(2) 0.729(2) 0.025(5) Uiso 1 1 d . . . . .
H9 H 0.551(3) 1.031(2) 0.849(2) 0.029(5) Uiso 1 1 d . . . . .
H10 H 0.654(2) 0.926(2) 0.832(2) 0.022(5) Uiso 1 1 d . . . . .
H11 H 0.343(3) 0.998(2) 0.530(2) 0.030(6) Uiso 1 1 d . . . . .
H12 H 0.180(3) 0.849(2) 0.510(2) 0.032(6) Uiso 1 1 d . . . . .
H13 H 0.249(3) 0.973(2) 0.638(2) 0.029(6) Uiso 1 1 d . . . . .
H14 H 0.472(3) 0.351(2) 0.865(2) 0.028(5) Uiso 1 1 d . . . . .
H15 H 0.362(2) 0.181(2) 0.872(2) 0.023(5) Uiso 1 1 d . . . . .
H16 H 0.391(2) 0.316(2) 0.985(2) 0.024(5) Uiso 1 1 d . . . . .
H17 H -0.052(3) 0.211(2) 0.771(2) 0.024(5) Uiso 1 1 d . . . . .
H18 H 0.033(2) 0.087(2) 0.787(2) 0.025(5) Uiso 1 1 d . . . . .
H19 H 0.079(3) 0.201(2) 0.925(2) 0.028(5) Uiso 1 1 d . . . . .
N1 N 0.35884(18) 0.52215(18) 0.62428(15) 0.0098(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.399(2) . ?
C1 C6 1.405(2) . ?
C1 N1 1.454(2) . ?
C2 C3 1.396(2) . ?
C2 C10 1.520(2) . ?
C3 C4 1.380(2) . ?
C3 H3 0.926(18) . ?
C4 C5 1.383(2) . ?
C4 H4 0.938(17) . ?
C5 C6 1.390(2) . ?
C5 H5 0.948(18) . ?
C6 C7 1.527(2) . ?
C7 C8 1.528(2) . ?
C7 C9 1.531(2) . ?
C7 H7 0.963(18) . ?
C8 H17 0.97(2) . ?
C8 H18 0.96(2) . ?
C8 H19 0.98(2) . ?
C9 H14 0.97(2) . ?
C9 H15 0.96(2) . ?
C9 H16 0.97(2) . ?
C10 C11 1.526(2) . ?
C10 C12 1.527(2) . ?
C10 H6 0.948(17) . ?
C11 H8 0.95(2) . ?
C11 H9 0.99(2) . ?
C11 H10 0.98(2) . ?
C12 H11 0.96(2) . ?
C12 H12 0.95(2) . ?
C12 H13 0.94(2) . ?
Cl1 Ge1 2.2744(4) . ?
Cl2 Ge1 2.2793(4) . ?
Ge1 N1 2.1674(14) . ?
N1 H1 0.84(2) . ?
N1 H2 0.823(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 122.45(14) . . ?
C2 C1 N1 119.14(14) . . ?
C6 C1 N1 118.28(14) . . ?
C3 C2 C1 117.31(14) . . ?
C3 C2 C10 118.34(14) . . ?
C1 C2 C10 124.35(14) . . ?
C4 C3 C2 121.39(15) . . ?
C4 C3 H3 119.7(10) . . ?
C2 C3 H3 118.9(11) . . ?
C3 C4 C5 120.02(15) . . ?
C3 C4 H4 120.2(10) . . ?
C5 C4 H4 119.8(10) . . ?
C4 C5 C6 121.26(15) . . ?
C4 C5 H5 120.5(10) . . ?
C6 C5 H5 118.2(10) . . ?
C5 C6 C1 117.53(14) . . ?
C5 C6 C7 120.63(14) . . ?
C1 C6 C7 121.75(14) . . ?
C6 C7 C8 113.43(14) . . ?
C6 C7 C9 109.94(14) . . ?
C8 C7 C9 109.68(14) . . ?
C6 C7 H7 106.5(10) . . ?
C8 C7 H7 107.5(10) . . ?
C9 C7 H7 109.7(10) . . ?
C7 C8 H17 111.1(11) . . ?
C7 C8 H18 109.8(11) . . ?
H17 C8 H18 109.5(16) . . ?
C7 C8 H19 110.6(12) . . ?
H17 C8 H19 109.2(16) . . ?
H18 C8 H19 106.6(16) . . ?
C7 C9 H14 113.7(12) . . ?
C7 C9 H15 110.3(12) . . ?
H14 C9 H15 108.8(16) . . ?
C7 C9 H16 108.4(11) . . ?
H14 C9 H16 107.9(16) . . ?
H15 C9 H16 107.4(16) . . ?
C2 C10 C11 110.59(14) . . ?
C2 C10 C12 111.26(14) . . ?
C11 C10 C12 111.25(15) . . ?
C2 C10 H6 109.7(10) . . ?
C11 C10 H6 108.1(10) . . ?
C12 C10 H6 105.8(10) . . ?
C10 C11 H8 111.0(12) . . ?
C10 C11 H9 112.2(12) . . ?
H8 C11 H9 105.3(16) . . ?
C10 C11 H10 110.8(11) . . ?
H8 C11 H10 108.7(16) . . ?
H9 C11 H10 108.7(16) . . ?
C10 C12 H11 108.9(12) . . ?
C10 C12 H12 112.4(13) . . ?
H11 C12 H12 111.1(17) . . ?
C10 C12 H13 111.4(12) . . ?
H11 C12 H13 108.1(17) . . ?
H12 C12 H13 104.8(17) . . ?
N1 Ge1 Cl1 90.63(4) . . ?
N1 Ge1 Cl2 90.78(4) . . ?
Cl1 Ge1 Cl2 95.903(16) . . ?
C1 N1 Ge1 110.22(10) . . ?
C1 N1 H1 113.4(12) . . ?
Ge1 N1 H1 106.3(12) . . ?
C1 N1 H2 111.7(12) . . ?
Ge1 N1 H2 107.8(12) . . ?
H1 N1 H2 107.2(17) . . ?

_refine_diff_density_max         0.338
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.048



####################################################################### 
# 
# 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_mo_sanj_28_1_2020_0m_a_sqd
_database_code_depnum_ccdc_archive 'CCDC 2002736'
loop_
_audit_author_name
_audit_author_address
'Dr. Rajesh G. Gonnade'
;CSIR NATIONAL CHEMICAL LABORATORY PUNE INDIA
India
;
_audit_update_record             
;
2020-05-08 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT990_mo_sanj_28_1_2020_0m_a_sqd 
;
PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE Job ... ! Note
RESPONSE: The lattice contain the highly disordered THF molecules,
which have been treated as a diffuse contribution to the overall 
scattering without specific atomic positions by Squeeze/Platon.
The squeeze was run in platon having 3013 version of 
Shelx. CIF was selected for squeeze job and the files created 
were _sq.ins and _sq.hkl. However, refining the structure with 
these as input files didn't show the squeezing effect. Hence, the 
squeeze was run with .ins file which gave _sqd.ins and _sqd.hkl 
files. Refining the structure with these files removed the 
contribution of solvent from the diffraction data.
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H58 Al2 N6, 0.75(C4 H8 O)'
_chemical_formula_sum            'C49 H64 Al2 N6 O(0.75)'
_chemical_formula_weight         803.02

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.8257(6)
_cell_length_b                   15.7134(10)
_cell_length_c                   17.6385(11)
_cell_angle_alpha                82.476(2)
_cell_angle_beta                 76.292(2)
_cell_angle_gamma                75.862(2)
_cell_volume                     2297.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9967
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      25.56

_exptl_crystal_description       PLATE
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_F_000             868
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.105
_shelx_estimated_absorpt_T_min   0.978
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'Photon II CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            95322
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.494
_diffrn_reflns_theta_max         25.618
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8597
_reflns_number_gt                7467
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0453P)²+1.6661P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0064(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8597
_refine_ls_number_parameters     626
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1165
_refine_ls_wR_factor_gt          0.1112
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
N5B N 0.6549(5) 0.4674(3) 0.1417(3) 0.0149(9) Uani 0.5 1 d . . P A 1
C37B C 0.5571(6) 0.4112(3) 0.1755(3) 0.0142(10) Uani 0.5 1 d . . P A 1
C38B C 0.4867(6) 0.3736(3) 0.1273(2) 0.0218(8) Uani 0.5 1 d . . P A 1
H38B H 0.4165 0.3356 0.1499 0.026 Uiso 0.5 1 calc R U P A 1
C39B C 0.5211(5) 0.3928(3) 0.0482(2) 0.0293(9) Uani 0.5 1 d . . P A 1
H39B H 0.4742 0.3681 0.0156 0.035 Uiso 0.5 1 calc R U P A 1
C40B C 0.6248(6) 0.4487(3) 0.0147(2) 0.0312(10) Uani 0.5 1 d . . P A 1
H40B H 0.6495 0.4622 -0.0403 0.037 Uiso 0.5 1 calc R U P A 1
C41B C 0.6894(6) 0.4832(2) 0.0636(2) 0.0215(8) Uani 0.5 1 d . . P A 1
H41B H 0.7620 0.5200 0.0412 0.026 Uiso 0.5 1 calc R U P A 1
N5A N 0.7241(5) 0.4518(3) 0.1277(3) 0.0175(10) Uani 0.5 1 d . . P A 2
C37A C 0.6239(6) 0.3964(3) 0.1544(3) 0.0162(10) Uani 0.5 1 d . . P A 2
C38A C 0.5918(6) 0.3463(3) 0.1020(2) 0.0246(9) Uani 0.5 1 d . . P A 2
H38A H 0.5179 0.3094 0.1199 0.029 Uiso 0.5 1 calc R U P A 2
C39A C 0.6684(6) 0.3516(3) 0.0249(2) 0.0354(11) Uani 0.5 1 d . . P A 2
H39A H 0.6479 0.3176 -0.0108 0.043 Uiso 0.5 1 calc R U P A 2
C40A C 0.7761(6) 0.4061(3) -0.0017(2) 0.0340(10) Uani 0.5 1 d . . P A 2
H40A H 0.8316 0.4087 -0.0549 0.041 Uiso 0.5 1 calc R U P A 2
C41A C 0.7997(6) 0.4560(3) 0.0510(2) 0.0245(8) Uani 0.5 1 d . . P A 2
H41A H 0.8708 0.4947 0.0334 0.029 Uiso 0.5 1 calc R U P A 2
C36 C 0.2807(3) 0.21841(14) 0.30583(14) 0.0361(5) Uani 1 1 d . . . . .
H36A H 0.3613 0.2253 0.2579 0.054 Uiso 1 1 calc R U . . .
H36B H 0.2030 0.2745 0.3146 0.054 Uiso 1 1 calc R U . . .
H36C H 0.2255 0.1732 0.3003 0.054 Uiso 1 1 calc R U . . .
N6A N 0.9417(6) 0.2802(4) 0.1784(3) 0.0156(10) Uani 0.5 1 d . . P B 1
C46A C 1.0122(7) 0.3445(4) 0.1886(4) 0.0157(13) Uani 0.5 1 d . . P B 1
C45A C 1.1448(5) 0.3626(2) 0.1316(3) 0.0220(8) Uani 0.5 1 d . . P B 1
H45A H 1.1960 0.4068 0.1386 0.026 Uiso 0.5 1 calc R U P B 1
C44A C 1.1992(5) 0.3167(3) 0.0668(2) 0.0295(9) Uani 0.5 1 d . . P B 1
H44A H 1.2898 0.3281 0.0290 0.035 Uiso 0.5 1 calc R U P B 1
C43A C 1.1225(6) 0.2528(3) 0.0556(2) 0.0316(10) Uani 0.5 1 d . . P B 1
H43A H 1.1577 0.2214 0.0098 0.038 Uiso 0.5 1 calc R U P B 1
C42A C 0.9942(6) 0.2368(2) 0.1131(2) 0.0218(8) Uani 0.5 1 d . . P B 1
H42A H 0.9410 0.1935 0.1062 0.026 Uiso 0.5 1 calc R U P B 1
C46B C 0.9655(7) 0.3454(4) 0.1711(3) 0.0134(11) Uani 0.5 1 d . . P B 2
N6B N 0.8838(6) 0.2843(4) 0.1684(4) 0.0162(11) Uani 0.5 1 d . . P B 2
C42B C 0.9021(6) 0.2476(2) 0.1003(2) 0.0218(8) Uani 0.5 1 d . . P B 2
H42B H 0.8429 0.2049 0.0993 0.026 Uiso 0.5 1 calc R U P B 2
C43B C 1.0036(6) 0.2703(3) 0.0330(2) 0.0300(9) Uani 0.5 1 d . . P B 2
H43B H 1.0136 0.2446 -0.0143 0.036 Uiso 0.5 1 calc R U P B 2
C44B C 1.0921(5) 0.3322(3) 0.0356(2) 0.0304(10) Uani 0.5 1 d . . P B 2
H44B H 1.1657 0.3477 -0.0098 0.037 Uiso 0.5 1 calc R U P B 2
C45B C 1.0724(5) 0.3705(2) 0.1041(3) 0.0214(8) Uani 0.5 1 d . . P B 2
H45B H 1.1304 0.4134 0.1060 0.026 Uiso 0.5 1 calc R U P B 2
Al2 Al 0.76617(6) 0.50676(3) 0.21589(3) 0.01632(13) Uani 1 1 d . . . . .
Al3 Al 0.73258(7) 0.26779(3) 0.26473(3) 0.01856(14) Uani 1 1 d . . . . .
N1 N 0.58228(18) 0.46286(9) 0.28249(10) 0.0219(4) Uani 1 1 d . . . . .
N2 N 0.84968(16) 0.33250(9) 0.31106(8) 0.0157(3) Uani 1 1 d . . . . .
N3 N 0.71030(17) 0.60835(9) 0.27587(9) 0.0178(3) Uani 1 1 d . . . . .
N4 N 0.70274(16) 0.19205(9) 0.35960(8) 0.0133(3) Uani 1 1 d . . . . .
C1 C 0.5564(3) 0.38873(12) 0.24944(13) 0.0292(5) Uani 1 1 d . . . . .
C2 C 0.9290(2) 0.39050(11) 0.25143(11) 0.0225(4) Uani 1 1 d . . . . .
C3 C 0.5095(2) 0.48238(12) 0.35401(13) 0.0271(5) Uani 1 1 d . . . . .
C4 C 0.5304(2) 0.55523(12) 0.38681(14) 0.0333(5) Uani 1 1 d . . . . .
H4 H 0.4785 0.5631 0.4399 0.040 Uiso 1 1 calc R U . . .
C5 C 0.6185(2) 0.61590(12) 0.34929(12) 0.0279(5) Uani 1 1 d . . . . .
C6 C 0.3982(2) 0.42820(13) 0.40430(16) 0.0391(6) Uani 1 1 d . . . . .
H6A H 0.3117 0.4285 0.3781 0.059 Uiso 1 1 calc R U . . .
H6B H 0.3529 0.4533 0.4550 0.059 Uiso 1 1 calc R U . . .
H6C H 0.4578 0.3676 0.4125 0.059 Uiso 1 1 calc R U . . .
C7 C 0.6109(4) 0.69416(15) 0.39234(15) 0.0536(8) Uani 1 1 d . . . . .
H7A H 0.7194 0.6977 0.3938 0.080 Uiso 1 1 calc R U . . .
H7B H 0.5487 0.6876 0.4459 0.080 Uiso 1 1 calc R U . . .
H7C H 0.5594 0.7481 0.3653 0.080 Uiso 1 1 calc R U . . .
C8 C 0.7741(2) 0.68394(11) 0.23961(10) 0.0157(4) Uani 1 1 d . . . . .
C9 C 0.6794(2) 0.75239(11) 0.19985(10) 0.0177(4) Uani 1 1 d . . . . .
C10 C 0.7448(2) 0.82213(12) 0.16114(11) 0.0204(4) Uani 1 1 d . . . . .
H10 H 0.6821 0.8684 0.1340 0.024 Uiso 1 1 calc R U . . .
C11 C 0.8998(2) 0.82532(12) 0.16143(11) 0.0223(4) Uani 1 1 d . . . . .
H11 H 0.9432 0.8732 0.1343 0.027 Uiso 1 1 calc R U . . .
C12 C 0.9915(2) 0.75871(12) 0.20131(11) 0.0196(4) Uani 1 1 d . . . . .
H12 H 1.0977 0.7615 0.2014 0.024 Uiso 1 1 calc R U . . .
C13 C 0.9312(2) 0.68739(11) 0.24139(10) 0.0168(4) Uani 1 1 d . . . . .
C14 C 0.5085(2) 0.75025(12) 0.19748(12) 0.0231(4) Uani 1 1 d . . . . .
H14 H 0.4863 0.6994 0.2354 0.028 Uiso 1 1 calc R U . C 1
C15 C 0.5037(3) 0.72104(16) 0.11987(12) 0.0351(5) Uani 1 1 d . U . . .
H15A H 0.5419 0.7625 0.0774 0.053 Uiso 1 1 calc R U . . .
H15B H 0.3936 0.7195 0.1193 0.053 Uiso 1 1 calc R U . . .
H15C H 0.5724 0.6622 0.1126 0.053 Uiso 1 1 calc R U . . .
C16 C 0.3882(6) 0.8286(4) 0.2342(4) 0.0312(12) Uani 0.5 1 d . U P D 1
H16A H 0.4087 0.8831 0.2038 0.047 Uiso 0.5 1 calc R U P D 1
H16B H 0.3988 0.8300 0.2881 0.047 Uiso 0.5 1 calc R U P D 1
H16C H 0.2797 0.8234 0.2344 0.047 Uiso 0.5 1 calc R U P D 1
C16' C 0.3983(6) 0.8473(3) 0.1924(4) 0.0292(11) Uani 0.5 1 d . . P D 2
H16D H 0.4386 0.8792 0.1431 0.044 Uiso 0.5 1 calc R U P D 2
H16E H 0.4006 0.8787 0.2365 0.044 Uiso 0.5 1 calc R U P D 2
H16F H 0.2881 0.8435 0.1946 0.044 Uiso 0.5 1 calc R U P D 2
C17 C 1.0368(2) 0.61626(12) 0.28494(11) 0.0213(4) Uani 1 1 d . . . . .
H17 H 0.9729 0.5721 0.3115 0.026 Uiso 1 1 calc R U . . .
C18 C 1.1833(2) 0.56859(14) 0.22903(12) 0.0299(5) Uani 1 1 d . . . . .
H18A H 1.1492 0.5462 0.1880 0.045 Uiso 1 1 calc R U . . .
H18B H 1.2428 0.5194 0.2580 0.045 Uiso 1 1 calc R U . . .
H18C H 1.2521 0.6096 0.2051 0.045 Uiso 1 1 calc R U . . .
C19 C 1.0894(3) 0.65374(16) 0.34775(14) 0.0429(6) Uani 1 1 d . . . . .
H19A H 1.1535 0.6059 0.3760 0.064 Uiso 1 1 calc R U . . .
H19B H 0.9948 0.6826 0.3846 0.064 Uiso 1 1 calc R U . . .
H19C H 1.1536 0.6967 0.3230 0.064 Uiso 1 1 calc R U . . .
C20 C 0.8415(2) 0.33693(11) 0.38581(11) 0.0179(4) Uani 1 1 d . . . . .
C21 C 0.7749(2) 0.27713(11) 0.44368(10) 0.0188(4) Uani 1 1 d . . . . .
H21 H 0.7678 0.2865 0.4966 0.023 Uiso 1 1 calc R U . . .
C22 C 0.7193(2) 0.20640(11) 0.43090(10) 0.0151(3) Uani 1 1 d . . . . .
C23 C 0.9067(2) 0.40521(13) 0.41300(12) 0.0277(4) Uani 1 1 d . . . . .
H23A H 1.0214 0.3970 0.3902 0.042 Uiso 1 1 calc R U . . .
H23B H 0.8898 0.3988 0.4702 0.042 Uiso 1 1 calc R U . . .
H23C H 0.8512 0.4642 0.3963 0.042 Uiso 1 1 calc R U . . .
C24 C 0.6774(2) 0.14242(12) 0.49947(10) 0.0212(4) Uani 1 1 d . . . . .
H24A H 0.5655 0.1391 0.5062 0.032 Uiso 1 1 calc R U . . .
H24B H 0.6927 0.1624 0.5469 0.032 Uiso 1 1 calc R U . . .
H24C H 0.7468 0.0841 0.4899 0.032 Uiso 1 1 calc R U . . .
C25 C 0.6578(2) 0.11078(11) 0.35367(9) 0.0145(3) Uani 1 1 d . . . . .
C26 C 0.7783(2) 0.03370(11) 0.33938(10) 0.0179(4) Uani 1 1 d . . . . .
C27 C 0.7350(2) -0.04302(12) 0.32982(11) 0.0243(4) Uani 1 1 d . . . . .
H27 H 0.8153 -0.0952 0.3196 0.029 Uiso 1 1 calc R U . . .
C28 C 0.5774(3) -0.04442(13) 0.33499(12) 0.0285(5) Uani 1 1 d . . . . .
H28 H 0.5498 -0.0973 0.3282 0.034 Uiso 1 1 calc R U . . .
C29 C 0.4597(2) 0.03100(12) 0.35004(12) 0.0264(4) Uani 1 1 d . . . . .
H29 H 0.3512 0.0293 0.3538 0.032 Uiso 1 1 calc R U . . .
C30 C 0.4969(2) 0.10955(11) 0.35976(11) 0.0192(4) Uani 1 1 d . . . . .
C31 C 0.9539(2) 0.03312(12) 0.33193(11) 0.0223(4) Uani 1 1 d . . . . .
H31 H 0.9597 0.0880 0.3530 0.027 Uiso 1 1 calc R U . . .
C32 C 1.0401(3) 0.03422(14) 0.24602(13) 0.0355(5) Uani 1 1 d . . . . .
H32A H 1.0370 -0.0194 0.2242 0.053 Uiso 1 1 calc R U . . .
H32B H 1.1517 0.0368 0.2418 0.053 Uiso 1 1 calc R U . . .
H32C H 0.9872 0.0859 0.2169 0.053 Uiso 1 1 calc R U . . .
C33 C 1.0367(2) -0.04545(15) 0.37927(15) 0.0396(6) Uani 1 1 d . . . . .
H33A H 0.9778 -0.0461 0.4339 0.059 Uiso 1 1 calc R U . . .
H33B H 1.1463 -0.0406 0.3769 0.059 Uiso 1 1 calc R U . . .
H33C H 1.0390 -0.1001 0.3574 0.059 Uiso 1 1 calc R U . . .
C34 C 0.3622(2) 0.19073(12) 0.37523(12) 0.0243(4) Uani 1 1 d . . . . .
H34 H 0.4104 0.2399 0.3818 0.029 Uiso 1 1 calc R U . . .
C35 C 0.2393(3) 0.17714(17) 0.45052(14) 0.0401(6) Uani 1 1 d . . . . .
H35A H 0.1842 0.1322 0.4443 0.060 Uiso 1 1 calc R U . . .
H35B H 0.1611 0.2327 0.4613 0.060 Uiso 1 1 calc R U . . .
H35C H 0.2938 0.1579 0.4942 0.060 Uiso 1 1 calc R U . . .
H2 H 0.885(2) 0.5479(14) 0.1494(12) 0.029(6) Uiso 1 1 d . . . . .
H1 H 0.672(3) 0.2098(15) 0.2187(13) 0.038(6) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N5B C41B 1.343(6) . ?
N5B C37B 1.368(8) . ?
N5B Al2 2.043(5) . ?
C37B C1 1.305(6) . ?
C37B C38B 1.420(6) . ?
C38B C39B 1.366(6) . ?
C38B H38B 0.9500 . ?
C39B C40B 1.399(6) . ?
C39B H39B 0.9500 . ?
C40B C41B 1.367(6) . ?
C40B H40B 0.9500 . ?
C41B H41B 0.9500 . ?
N5A C37A 1.353(8) . ?
N5A C41A 1.360(6) . ?
N5A Al2 2.022(5) . ?
C37A C38A 1.406(6) . ?
C37A C1 1.639(5) . ?
C38A C39A 1.370(6) . ?
C38A H38A 0.9500 . ?
C39A C40A 1.393(6) . ?
C39A H39A 0.9500 . ?
C40A C41A 1.374(6) . ?
C40A H40A 0.9500 . ?
C41A H41A 0.9500 . ?
C36 C34 1.526(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N6A C42A 1.344(7) . ?
N6A C46A 1.360(9) . ?
N6A Al3 2.128(6) . ?
C46A C2 1.362(7) . ?
C46A C45A 1.411(8) . ?
C45A C44A 1.358(6) . ?
C45A H45A 0.9500 . ?
C44A C43A 1.398(6) . ?
C44A H44A 0.9500 . ?
C43A C42A 1.379(6) . ?
C43A H43A 0.9500 . ?
C42A H42A 0.9500 . ?
C46B N6B 1.346(9) . ?
C46B C45B 1.404(7) . ?
C46B C2 1.596(6) . ?
N6B C42B 1.359(7) . ?
N6B Al3 1.927(6) . ?
C42B C43B 1.372(6) . ?
C42B H42B 0.9500 . ?
C43B C44B 1.399(6) . ?
C43B H43B 0.9500 . ?
C44B C45B 1.375(6) . ?
C44B H44B 0.9500 . ?
C45B H45B 0.9500 . ?
Al2 N3 1.9290(15) . ?
Al2 N1 1.9801(17) . ?
Al2 C2 2.1542(18) . ?
Al2 H2 1.56(2) . ?
Al3 N4 1.9259(15) . ?
Al3 N2 1.9750(16) . ?
Al3 C1 2.1733(19) . ?
Al3 H1 1.55(2) . ?
N1 C3 1.311(3) . ?
N1 C1 1.456(2) . ?
N2 C20 1.313(2) . ?
N2 C2 1.462(2) . ?
N3 C5 1.358(2) . ?
N3 C8 1.447(2) . ?
N4 C22 1.353(2) . ?
N4 C25 1.449(2) . ?
C3 C4 1.416(3) . ?
C3 C6 1.508(3) . ?
C4 C5 1.380(3) . ?
C4 H4 0.9500 . ?
C5 C7 1.508(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C13 1.409(2) . ?
C8 C9 1.410(2) . ?
C9 C10 1.388(3) . ?
C9 C14 1.527(2) . ?
C10 C11 1.383(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.394(2) . ?
C12 H12 0.9500 . ?
C13 C17 1.521(2) . ?
C14 C15 1.513(3) . ?
C14 C16 1.519(5) . ?
C14 C16' 1.600(5) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16' H16D 0.9800 . ?
C16' H16E 0.9800 . ?
C16' H16F 0.9800 . ?
C17 C18 1.523(3) . ?
C17 C19 1.529(3) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.416(2) . ?
C20 C23 1.510(3) . ?
C21 C22 1.383(2) . ?
C21 H21 0.9500 . ?
C22 C24 1.504(2) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C30 1.404(2) . ?
C25 C26 1.409(2) . ?
C26 C27 1.392(3) . ?
C26 C31 1.522(3) . ?
C27 C28 1.377(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.393(3) . ?
C29 H29 0.9500 . ?
C30 C34 1.520(2) . ?
C31 C32 1.526(3) . ?
C31 C33 1.528(3) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.530(3) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C41B N5B C37B 119.9(5) . . ?
C41B N5B Al2 124.2(4) . . ?
C37B N5B Al2 115.2(4) . . ?
C1 C37B N5B 113.9(4) . . ?
C1 C37B C38B 126.2(4) . . ?
N5B C37B C38B 119.3(5) . . ?
C39B C38B C37B 119.3(4) . . ?
C39B C38B H38B 120.4 . . ?
C37B C38B H38B 120.4 . . ?
C38B C39B C40B 120.5(4) . . ?
C38B C39B H39B 119.7 . . ?
C40B C39B H39B 119.7 . . ?
C41B C40B C39B 118.0(4) . . ?
C41B C40B H40B 121.0 . . ?
C39B C40B H40B 121.0 . . ?
N5B C41B C40B 123.0(4) . . ?
N5B C41B H41B 118.5 . . ?
C40B C41B H41B 118.5 . . ?
C37A N5A C41A 120.2(5) . . ?
C37A N5A Al2 111.9(4) . . ?
C41A N5A Al2 127.2(4) . . ?
N5A C37A C38A 119.9(5) . . ?
N5A C37A C1 115.6(4) . . ?
C38A C37A C1 124.4(4) . . ?
C39A C38A C37A 119.2(4) . . ?
C39A C38A H38A 120.4 . . ?
C37A C38A H38A 120.4 . . ?
C38A C39A C40A 120.7(4) . . ?
C38A C39A H39A 119.7 . . ?
C40A C39A H39A 119.7 . . ?
C41A C40A C39A 118.1(4) . . ?
C41A C40A H40A 121.0 . . ?
C39A C40A H40A 121.0 . . ?
N5A C41A C40A 121.9(4) . . ?
N5A C41A H41A 119.1 . . ?
C40A C41A H41A 119.1 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C42A N6A C46A 120.1(6) . . ?
C42A N6A Al3 124.7(4) . . ?
C46A N6A Al3 114.8(5) . . ?
N6A C46A C2 112.1(5) . . ?
N6A C46A C45A 119.4(6) . . ?
C2 C46A C45A 128.1(5) . . ?
C44A C45A C46A 119.9(4) . . ?
C44A C45A H45A 120.1 . . ?
C46A C45A H45A 120.1 . . ?
C45A C44A C43A 120.3(4) . . ?
C45A C44A H44A 119.9 . . ?
C43A C44A H44A 119.9 . . ?
C42A C43A C44A 117.9(4) . . ?
C42A C43A H43A 121.1 . . ?
C44A C43A H43A 121.1 . . ?
N6A C42A C43A 122.4(5) . . ?
N6A C42A H42A 118.8 . . ?
C43A C42A H42A 118.8 . . ?
N6B C46B C45B 120.3(6) . . ?
N6B C46B C2 117.3(5) . . ?
C45B C46B C2 122.3(5) . . ?
C46B N6B C42B 120.1(6) . . ?
C46B N6B Al3 112.8(5) . . ?
C42B N6B Al3 126.9(4) . . ?
N6B C42B C43B 122.0(4) . . ?
N6B C42B H42B 119.0 . . ?
C43B C42B H42B 119.0 . . ?
C42B C43B C44B 118.4(4) . . ?
C42B C43B H43B 120.8 . . ?
C44B C43B H43B 120.8 . . ?
C45B C44B C43B 119.8(4) . . ?
C45B C44B H44B 120.1 . . ?
C43B C44B H44B 120.1 . . ?
C44B C45B C46B 119.4(4) . . ?
C44B C45B H45B 120.3 . . ?
C46B C45B H45B 120.3 . . ?
N3 Al2 N1 90.03(7) . . ?
N3 Al2 N5A 146.16(14) . . ?
N1 Al2 N5A 86.00(15) . . ?
N3 Al2 N5B 132.20(13) . . ?
N1 Al2 N5B 73.54(14) . . ?
N3 Al2 C2 119.03(8) . . ?
N1 Al2 C2 90.44(7) . . ?
N5A Al2 C2 94.63(14) . . ?
N5B Al2 C2 105.96(14) . . ?
N3 Al2 H2 92.8(8) . . ?
N1 Al2 H2 166.6(8) . . ?
N5A Al2 H2 84.3(8) . . ?
N5B Al2 H2 95.0(8) . . ?
C2 Al2 H2 99.6(8) . . ?
N4 Al3 N6B 142.68(17) . . ?
N4 Al3 N2 90.40(6) . . ?
N6B Al3 N2 85.53(16) . . ?
N4 Al3 N6A 131.37(15) . . ?
N2 Al3 N6A 73.81(16) . . ?
N4 Al3 C1 120.35(8) . . ?
N6B Al3 C1 96.76(18) . . ?
N2 Al3 C1 90.02(7) . . ?
N6A Al3 C1 105.66(17) . . ?
N4 Al3 H1 92.9(8) . . ?
N6B Al3 H1 85.5(9) . . ?
N2 Al3 H1 169.1(8) . . ?
N6A Al3 H1 96.3(9) . . ?
C1 Al3 H1 97.2(8) . . ?
C3 N1 C1 120.74(17) . . ?
C3 N1 Al2 127.17(13) . . ?
C1 N1 Al2 110.80(14) . . ?
C20 N2 C2 121.14(15) . . ?
C20 N2 Al3 127.11(12) . . ?
C2 N2 Al3 110.90(12) . . ?
C5 N3 C8 116.45(14) . . ?
C5 N3 Al2 126.60(12) . . ?
C8 N3 Al2 116.94(11) . . ?
C22 N4 C25 116.65(13) . . ?
C22 N4 Al3 127.14(12) . . ?
C25 N4 Al3 116.21(10) . . ?
C37B C1 N1 107.4(3) . . ?
N1 C1 C37A 109.1(2) . . ?
C37B C1 Al3 111.2(2) . . ?
N1 C1 Al3 113.05(12) . . ?
C37A C1 Al3 92.3(2) . . ?
C46A C2 N2 109.4(3) . . ?
N2 C2 C46B 105.8(3) . . ?
C46A C2 Al2 110.7(3) . . ?
N2 C2 Al2 113.14(11) . . ?
C46B C2 Al2 95.4(2) . . ?
N1 C3 C4 121.72(17) . . ?
N1 C3 C6 120.89(18) . . ?
C4 C3 C6 117.4(2) . . ?
C5 C4 C3 126.5(2) . . ?
C5 C4 H4 116.7 . . ?
C3 C4 H4 116.7 . . ?
N3 C5 C4 123.08(18) . . ?
N3 C5 C7 119.01(17) . . ?
C4 C5 C7 117.91(18) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C13 C8 C9 120.46(16) . . ?
C13 C8 N3 120.34(15) . . ?
C9 C8 N3 119.15(15) . . ?
C10 C9 C8 118.86(16) . . ?
C10 C9 C14 119.77(16) . . ?
C8 C9 C14 121.36(16) . . ?
C11 C10 C9 121.07(17) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C12 C11 C10 119.85(17) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 121.35(17) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C12 C13 C8 118.38(16) . . ?
C12 C13 C17 119.18(16) . . ?
C8 C13 C17 122.45(16) . . ?
C15 C14 C16 122.2(3) . . ?
C15 C14 C9 110.37(16) . . ?
C16 C14 C9 111.7(2) . . ?
C15 C14 C16' 99.4(3) . . ?
C9 C14 C16' 111.6(2) . . ?
C15 C14 H14 103.4 . . ?
C16 C14 H14 103.4 . . ?
C9 C14 H14 103.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C16' H16D 109.5 . . ?
C14 C16' H16E 109.5 . . ?
H16D C16' H16E 109.5 . . ?
C14 C16' H16F 109.5 . . ?
H16D C16' H16F 109.5 . . ?
H16E C16' H16F 109.5 . . ?
C13 C17 C18 111.46(15) . . ?
C13 C17 C19 111.67(16) . . ?
C18 C17 C19 109.73(17) . . ?
C13 C17 H17 107.9 . . ?
C18 C17 H17 107.9 . . ?
C19 C17 H17 107.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 C21 121.64(16) . . ?
N2 C20 C23 120.88(16) . . ?
C21 C20 C23 117.46(16) . . ?
C22 C21 C20 126.59(16) . . ?
C22 C21 H21 116.7 . . ?
C20 C21 H21 116.7 . . ?
N4 C22 C21 122.89(15) . . ?
N4 C22 C24 118.99(15) . . ?
C21 C22 C24 118.11(15) . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 120.48(16) . . ?
C30 C25 N4 120.38(15) . . ?
C26 C25 N4 119.12(15) . . ?
C27 C26 C25 118.76(17) . . ?
C27 C26 C31 119.53(16) . . ?
C25 C26 C31 121.69(16) . . ?
C28 C27 C26 121.02(17) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 119.97(18) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 121.23(18) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 H29 119.4 . . ?
C29 C30 C25 118.53(17) . . ?
C29 C30 C34 118.81(16) . . ?
C25 C30 C34 122.65(16) . . ?
C26 C31 C32 110.28(16) . . ?
C26 C31 C33 111.94(16) . . ?
C32 C31 C33 110.64(17) . . ?
C26 C31 H31 107.9 . . ?
C32 C31 H31 107.9 . . ?
C33 C31 H31 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 C36 111.08(17) . . ?
C30 C34 C35 112.05(16) . . ?
C36 C34 C35 110.51(17) . . ?
C30 C34 H34 107.7 . . ?
C36 C34 H34 107.7 . . ?
C35 C34 H34 107.7 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C41B N5B C37B C1 168.0(4) . . . . ?
Al2 N5B C37B C1 -2.9(5) . . . . ?
C41B N5B C37B C38B -3.1(7) . . . . ?
Al2 N5B C37B C38B -174.0(3) . . . . ?
C1 C37B C38B C39B -168.5(4) . . . . ?
N5B C37B C38B C39B 1.5(7) . . . . ?
C37B C38B C39B C40B 0.2(7) . . . . ?
C38B C39B C40B C41B -0.2(6) . . . . ?
C37B N5B C41B C40B 3.2(7) . . . . ?
Al2 N5B C41B C40B 173.2(3) . . . . ?
C39B C40B C41B N5B -1.5(7) . . . . ?
C41A N5A C37A C38A -3.1(7) . . . . ?
Al2 N5A C37A C38A -174.6(4) . . . . ?
C41A N5A C37A C1 173.2(4) . . . . ?
Al2 N5A C37A C1 1.8(5) . . . . ?
N5A C37A C38A C39A 2.9(7) . . . . ?
C1 C37A C38A C39A -173.1(4) . . . . ?
C37A C38A C39A C40A -0.4(7) . . . . ?
C38A C39A C40A C41A -1.7(7) . . . . ?
C37A N5A C41A C40A 0.9(7) . . . . ?
Al2 N5A C41A C40A 170.9(4) . . . . ?
C39A C40A C41A N5A 1.5(7) . . . . ?
C42A N6A C46A C2 170.4(4) . . . . ?
Al3 N6A C46A C2 -2.4(6) . . . . ?
C42A N6A C46A C45A -2.6(8) . . . . ?
Al3 N6A C46A C45A -175.4(4) . . . . ?
N6A C46A C45A C44A 1.0(8) . . . . ?
C2 C46A C45A C44A -170.8(4) . . . . ?
C46A C45A C44A C43A 1.2(7) . . . . ?
C45A C44A C43A C42A -1.7(7) . . . . ?
C46A N6A C42A C43A 2.2(8) . . . . ?
Al3 N6A C42A C43A 174.2(4) . . . . ?
C44A C43A C42A N6A 0.0(7) . . . . ?
C45B C46B N6B C42B -1.1(8) . . . . ?
C2 C46B N6B C42B 175.9(4) . . . . ?
C45B C46B N6B Al3 -175.3(4) . . . . ?
C2 C46B N6B Al3 1.7(6) . . . . ?
C46B N6B C42B C43B 0.5(8) . . . . ?
Al3 N6B C42B C43B 173.8(4) . . . . ?
N6B C42B C43B C44B 1.1(7) . . . . ?
C42B C43B C44B C45B -1.9(7) . . . . ?
C43B C44B C45B C46B 1.3(7) . . . . ?
N6B C46B C45B C44B 0.2(7) . . . . ?
C2 C46B C45B C44B -176.6(4) . . . . ?
N5B C37B C1 N1 31.7(4) . . . . ?
C38B C37B C1 N1 -158.0(4) . . . . ?
N5B C37B C1 Al3 -92.5(4) . . . . ?
C38B C37B C1 Al3 77.9(5) . . . . ?
C3 N1 C1 C37B 143.5(3) . . . . ?
Al2 N1 C1 C37B -48.6(3) . . . . ?
C3 N1 C1 C37A 165.4(2) . . . . ?
Al2 N1 C1 C37A -26.7(2) . . . . ?
C3 N1 C1 Al3 -93.45(19) . . . . ?
Al2 N1 C1 Al3 74.48(14) . . . . ?
N5A C37A C1 N1 16.6(5) . . . . ?
C38A C37A C1 N1 -167.3(4) . . . . ?
N5A C37A C1 Al3 -98.8(4) . . . . ?
C38A C37A C1 Al3 77.4(4) . . . . ?
N6A C46A C2 N2 31.3(5) . . . . ?
C45A C46A C2 N2 -156.4(5) . . . . ?
N6A C46A C2 Al2 -94.0(4) . . . . ?
C45A C46A C2 Al2 78.3(5) . . . . ?
C20 N2 C2 C46A 140.8(3) . . . . ?
Al3 N2 C2 C46A -49.0(3) . . . . ?
C20 N2 C2 C46B 161.6(2) . . . . ?
Al3 N2 C2 C46B -28.2(2) . . . . ?
C20 N2 C2 Al2 -95.31(17) . . . . ?
Al3 N2 C2 Al2 74.90(13) . . . . ?
N6B C46B C2 N2 17.9(5) . . . . ?
C45B C46B C2 N2 -165.1(4) . . . . ?
N6B C46B C2 Al2 -98.0(4) . . . . ?
C45B C46B C2 Al2 79.0(5) . . . . ?
C1 N1 C3 C4 -178.70(18) . . . . ?
Al2 N1 C3 C4 15.5(3) . . . . ?
C1 N1 C3 C6 0.6(3) . . . . ?
Al2 N1 C3 C6 -165.23(14) . . . . ?
N1 C3 C4 C5 3.5(3) . . . . ?
C6 C3 C4 C5 -175.8(2) . . . . ?
C8 N3 C5 C4 170.07(19) . . . . ?
Al2 N3 C5 C4 -10.8(3) . . . . ?
C8 N3 C5 C7 -9.6(3) . . . . ?
Al2 N3 C5 C7 169.51(18) . . . . ?
C3 C4 C5 N3 -6.1(4) . . . . ?
C3 C4 C5 C7 173.6(2) . . . . ?
C5 N3 C8 C13 97.3(2) . . . . ?
Al2 N3 C8 C13 -81.93(18) . . . . ?
C5 N3 C8 C9 -85.2(2) . . . . ?
Al2 N3 C8 C9 95.59(16) . . . . ?
C13 C8 C9 C10 1.4(2) . . . . ?
N3 C8 C9 C10 -176.11(15) . . . . ?
C13 C8 C9 C14 -179.70(15) . . . . ?
N3 C8 C9 C14 2.8(2) . . . . ?
C8 C9 C10 C11 -0.3(3) . . . . ?
C14 C9 C10 C11 -179.19(16) . . . . ?
C9 C10 C11 C12 -0.6(3) . . . . ?
C10 C11 C12 C13 0.3(3) . . . . ?
C11 C12 C13 C8 0.8(3) . . . . ?
C11 C12 C13 C17 -179.47(16) . . . . ?
C9 C8 C13 C12 -1.7(2) . . . . ?
N3 C8 C13 C12 175.83(15) . . . . ?
C9 C8 C13 C17 178.63(16) . . . . ?
N3 C8 C13 C17 -3.9(2) . . . . ?
C10 C9 C14 C15 77.9(2) . . . . ?
C8 C9 C14 C15 -101.0(2) . . . . ?
C10 C9 C14 C16 -61.4(3) . . . . ?
C8 C9 C14 C16 119.7(3) . . . . ?
C10 C9 C14 C16' -31.6(3) . . . . ?
C8 C9 C14 C16' 149.5(3) . . . . ?
C12 C13 C17 C18 -63.7(2) . . . . ?
C8 C13 C17 C18 115.99(19) . . . . ?
C12 C13 C17 C19 59.4(2) . . . . ?
C8 C13 C17 C19 -120.9(2) . . . . ?
C2 N2 C20 C21 -175.54(15) . . . . ?
Al3 N2 C20 C21 16.0(2) . . . . ?
C2 N2 C20 C23 3.1(2) . . . . ?
Al3 N2 C20 C23 -165.45(13) . . . . ?
N2 C20 C21 C22 3.4(3) . . . . ?
C23 C20 C21 C22 -175.24(17) . . . . ?
C25 N4 C22 C21 174.21(16) . . . . ?
Al3 N4 C22 C21 -5.7(2) . . . . ?
C25 N4 C22 C24 -5.0(2) . . . . ?
Al3 N4 C22 C24 175.03(12) . . . . ?
C20 C21 C22 N4 -8.9(3) . . . . ?
C20 C21 C22 C24 170.37(17) . . . . ?
C22 N4 C25 C30 95.66(19) . . . . ?
Al3 N4 C25 C30 -84.41(17) . . . . ?
C22 N4 C25 C26 -86.24(19) . . . . ?
Al3 N4 C25 C26 93.69(16) . . . . ?
C30 C25 C26 C27 1.3(3) . . . . ?
N4 C25 C26 C27 -176.79(15) . . . . ?
C30 C25 C26 C31 179.57(16) . . . . ?
N4 C25 C26 C31 1.5(2) . . . . ?
C25 C26 C27 C28 -0.7(3) . . . . ?
C31 C26 C27 C28 -178.99(17) . . . . ?
C26 C27 C28 C29 -0.2(3) . . . . ?
C27 C28 C29 C30 0.4(3) . . . . ?
C28 C29 C30 C25 0.2(3) . . . . ?
C28 C29 C30 C34 179.26(18) . . . . ?
C26 C25 C30 C29 -1.1(3) . . . . ?
N4 C25 C30 C29 177.01(16) . . . . ?
C26 C25 C30 C34 179.91(16) . . . . ?
N4 C25 C30 C34 -2.0(3) . . . . ?
C27 C26 C31 C32 75.8(2) . . . . ?
C25 C26 C31 C32 -102.48(19) . . . . ?
C27 C26 C31 C33 -47.9(2) . . . . ?
C25 C26 C31 C33 133.88(19) . . . . ?
C29 C30 C34 C36 -63.6(2) . . . . ?
C25 C30 C34 C36 115.4(2) . . . . ?
C29 C30 C34 C35 60.5(2) . . . . ?
C25 C30 C34 C35 -120.5(2) . . . . ?

# SQUEEZE RESULTS (Version = 120716)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.028 0.000 0.000 281 59 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
PLATON/SQUEEZE was used to correct the diffraction data for the 
contribution from disordered lattice solvent (THF) molecules. 
The solvent accessible void volume per unit cell was 281 A3 (12%) 
and Electron Count/unit Cell was 59 e/A-3, estimated by PLATON. 
This electron count corresponds to one and half (1.5) disordered 
THF molecules present in the unit cell (0.75 occupancy in the 
asymmetric unit). However, they have been included in SFAC and UNIT 
instructions to get the correct molecular formula of the asymmetruc 
unit and formula weight. 
;


_refine_diff_density_max         0.681
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.045


