# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# 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_AS3
_database_code_depnum_ccdc_archive 'CCDC 1587847'
_audit_update_record             
;
2018-01-23 deposited with the CCDC.
2018-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H33 Cu N4 O2'
_chemical_formula_sum            'C46 H33 Cu N4 O2'
_chemical_formula_weight         737.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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                   13.6770(4)
_cell_length_b                   25.6111(9)
_cell_length_c                   26.6282(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.512(2)
_cell_angle_gamma                90
_cell_volume                     9309.9(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    90.0(5)
_cell_measurement_reflns_used    9934
_cell_measurement_theta_min      3.45
_cell_measurement_theta_max      52.69

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_F_000             3056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.939
_shelx_estimated_absorpt_T_min   0.813
_shelx_estimated_absorpt_T_max   0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90.0(5)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'I\mS microfocus'
_diffrn_radiation_monochromator  'QUAZAR multilayer optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61957
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.396
_diffrn_reflns_theta_max         53.694
_diffrn_reflns_theta_full        53.694
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             10888
_reflns_number_gt                7285
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1067P)²+11.8983P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10888
_refine_ls_number_parameters     961
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0710
_refine_ls_wR_factor_ref         0.2179
_refine_ls_wR_factor_gt          0.1903
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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
Cu1 Cu 0.37113(5) 0.52385(3) 0.37942(3) 0.0655(3) Uani 1 1 d . . . . .
O1 O 0.4061(3) 0.3041(2) 0.6900(2) 0.1112(16) Uani 1 1 d . . . . .
O2 O 0.3894(3) 0.4957(2) 0.71003(18) 0.0968(14) Uani 1 1 d . . . . .
N1 N 0.3608(3) 0.4893(2) 0.44115(18) 0.0620(12) Uani 1 1 d . . . . .
N2 N 0.3927(3) 0.45972(19) 0.34600(19) 0.0682(13) Uani 1 1 d . . . . .
N3 N 0.3544(3) 0.5657(2) 0.32187(19) 0.0677(13) Uani 1 1 d . . . . .
N4 N 0.3744(3) 0.58264(19) 0.42145(18) 0.0628(12) Uani 1 1 d . . . . .
C1 C 0.3666(3) 0.5187(3) 0.4826(2) 0.0627(16) Uani 1 1 d . . . . .
C2 C 0.3854(3) 0.4877(3) 0.5269(2) 0.0624(15) Uani 1 1 d . . . . .
C3 C 0.3997(4) 0.4376(2) 0.5082(2) 0.0638(15) Uani 1 1 d . . . . .
H3 H 0.416220 0.407707 0.528023 0.077 Uiso 1 1 calc R U . . .
C4 C 0.3862(4) 0.4383(3) 0.4558(2) 0.0621(15) Uani 1 1 d . . . . .
C5 C 0.3952(4) 0.4001(2) 0.4195(2) 0.0683(16) Uani 1 1 d . . . . .
C6 C 0.3890(4) 0.4101(3) 0.3670(2) 0.0705(16) Uani 1 1 d . . . . .
C7 C 0.3725(5) 0.3737(3) 0.3272(3) 0.0810(18) Uani 1 1 d . . . . .
H7 H 0.365969 0.337015 0.331144 0.097 Uiso 1 1 calc R U . . .
C8 C 0.3674(5) 0.3994(3) 0.2832(3) 0.0858(19) Uani 1 1 d . . . . .
H8 H 0.357477 0.384440 0.250619 0.103 Uiso 1 1 calc R U . . .
C9 C 0.3799(4) 0.4540(3) 0.2948(3) 0.0751(17) Uani 1 1 d . . . . .
C10 C 0.3775(4) 0.4955(3) 0.2598(2) 0.0739(17) Uani 1 1 d . . . . .
C11 C 0.3705(4) 0.5480(3) 0.2736(3) 0.0727(17) Uani 1 1 d . . . . .
C12 C 0.3849(5) 0.5926(3) 0.2413(3) 0.0843(19) Uani 1 1 d . . . . .
H12 H 0.396076 0.591681 0.206458 0.101 Uiso 1 1 calc R U . . .
C13 C 0.3796(5) 0.6351(3) 0.2699(3) 0.0841(19) Uani 1 1 d . . . . .
H13 H 0.386819 0.669973 0.258617 0.101 Uiso 1 1 calc R U . . .
C14 C 0.3612(4) 0.6200(3) 0.3204(3) 0.0729(17) Uani 1 1 d . . . . .
C15 C 0.3547(4) 0.6536(3) 0.3619(3) 0.0720(17) Uani 1 1 d . . . . .
C16 C 0.3570(4) 0.6352(3) 0.4113(3) 0.0692(16) Uani 1 1 d . . . . .
C17 C 0.3393(4) 0.6588(3) 0.4577(3) 0.0785(18) Uani 1 1 d . . . . .
H17 H 0.327894 0.695034 0.462472 0.094 Uiso 1 1 calc R U . . .
C18 C 0.3408(4) 0.6220(3) 0.4949(3) 0.0773(18) Uani 1 1 d . . . . .
H18 H 0.331411 0.627482 0.529566 0.093 Uiso 1 1 calc R U . . .
C19 C 0.3594(4) 0.5737(3) 0.4708(2) 0.0669(16) Uani 1 1 d . . . . .
C20 C 0.4164(5) 0.3448(3) 0.4375(2) 0.0757(17) Uani 1 1 d . . . . .
C21 C 0.3622(5) 0.3232(3) 0.4758(3) 0.090(2) Uani 1 1 d . . . . .
H21 H 0.309230 0.341713 0.488910 0.108 Uiso 1 1 calc R U . . .
C22 C 0.3893(7) 0.2730(3) 0.4943(3) 0.105(3) Uani 1 1 d . . . . .
H22 H 0.355480 0.258403 0.521102 0.126 Uiso 1 1 calc R U . . .
C23 C 0.4636(8) 0.2447(3) 0.4743(4) 0.116(3) Uani 1 1 d . . . . .
C24 C 0.5113(7) 0.2665(3) 0.4374(4) 0.118(3) Uani 1 1 d . . . . .
H24 H 0.562609 0.247129 0.423651 0.142 Uiso 1 1 calc R U . . .
C25 C 0.4905(6) 0.3151(3) 0.4181(3) 0.093(2) Uani 1 1 d . . . . .
H25 H 0.526574 0.328539 0.391533 0.112 Uiso 1 1 calc R U . . .
C26 C 0.4891(9) 0.1907(3) 0.4958(4) 0.156(4) Uani 1 1 d . . . . .
H26A H 0.551743 0.192358 0.515615 0.234 Uiso 1 1 calc R U . . .
H26B H 0.494183 0.165782 0.468112 0.234 Uiso 1 1 calc R U . . .
H26C H 0.437587 0.179264 0.517340 0.234 Uiso 1 1 calc R U . . .
C27 C 0.3858(6) 0.4829(3) 0.2062(3) 0.090(2) Uani 1 1 d . . . . .
C28 C 0.4617(7) 0.4531(4) 0.1909(3) 0.123(3) Uani 1 1 d . . . . .
H28 H 0.508936 0.439669 0.215238 0.147 Uiso 1 1 calc R U . . .
C29 C 0.4703(9) 0.4423(5) 0.1404(4) 0.175(5) Uani 1 1 d . . . . .
H29 H 0.522515 0.420949 0.130455 0.210 Uiso 1 1 calc R U . . .
C30 C 0.4039(9) 0.4623(5) 0.1042(3) 0.153(4) Uani 1 1 d . . . . .
C31 C 0.3237(8) 0.4910(4) 0.1188(3) 0.134(3) Uani 1 1 d . . . . .
H31 H 0.276292 0.503661 0.094124 0.161 Uiso 1 1 calc R U . . .
C32 C 0.3133(6) 0.5012(3) 0.1698(3) 0.099(2) Uani 1 1 d . . . . .
H32 H 0.258277 0.520095 0.180117 0.119 Uiso 1 1 calc R U . . .
C33 C 0.4169(11) 0.4514(6) 0.0477(4) 0.233(7) Uani 1 1 d . . . . .
H33A H 0.352441 0.450243 0.029474 0.349 Uiso 1 1 calc R U . . .
H33B H 0.450157 0.417889 0.044125 0.349 Uiso 1 1 calc R U . . .
H33C H 0.456176 0.479328 0.033800 0.349 Uiso 1 1 calc R U . . .
C34 C 0.3480(5) 0.7111(3) 0.3532(3) 0.0810(18) Uani 1 1 d . . . . .
C35 C 0.4118(5) 0.7460(3) 0.3779(3) 0.091(2) Uani 1 1 d . . . . .
H35 H 0.460087 0.733388 0.402075 0.109 Uiso 1 1 calc R U . . .
C36 C 0.4063(7) 0.7991(3) 0.3680(3) 0.121(3) Uani 1 1 d . . . . .
H36 H 0.450398 0.822284 0.385650 0.145 Uiso 1 1 calc R U . . .
C37 C 0.3377(7) 0.8188(3) 0.3326(4) 0.123(3) Uani 1 1 d . . . . .
C38 C 0.2720(6) 0.7845(3) 0.3083(3) 0.109(2) Uani 1 1 d . . . . .
H38 H 0.222940 0.797524 0.284792 0.131 Uiso 1 1 calc R U . . .
C39 C 0.2774(5) 0.7316(3) 0.3180(3) 0.097(2) Uani 1 1 d . . . . .
H39 H 0.232615 0.708647 0.300490 0.116 Uiso 1 1 calc R U . . .
C40 C 0.3338(8) 0.8769(3) 0.3219(4) 0.160(4) Uani 1 1 d . . . . .
H40A H 0.274625 0.891726 0.335272 0.240 Uiso 1 1 calc R U . . .
H40B H 0.332307 0.882679 0.285495 0.240 Uiso 1 1 calc R U . . .
H40C H 0.391774 0.893823 0.338038 0.240 Uiso 1 1 calc R U . . .
C41 C 0.3865(4) 0.5064(2) 0.5767(2) 0.0669(16) Uani 1 1 d . . . . .
H41 H 0.389522 0.543260 0.579972 0.080 Uiso 1 1 calc R U . . .
C42 C 0.3839(4) 0.4792(3) 0.6214(2) 0.0687(16) Uani 1 1 d . . . . .
C43 C 0.3731(4) 0.4226(3) 0.6239(2) 0.0710(16) Uani 1 1 d . . . . .
H43 H 0.345721 0.405683 0.594592 0.085 Uiso 1 1 calc R U . . .
C44 C 0.3979(4) 0.3924(3) 0.6633(3) 0.0760(17) Uani 1 1 d . . . . .
H44 H 0.423378 0.406803 0.694310 0.091 Uiso 1 1 calc R U . . .
C45 C 0.3847(4) 0.3368(4) 0.6571(3) 0.094(2) Uani 1 1 d . . . . .
H45 H 0.357481 0.324620 0.625617 0.112 Uiso 1 1 calc R U . . .
C46 C 0.3885(4) 0.5106(3) 0.6675(3) 0.0799(18) Uani 1 1 d . . . . .
H46 H 0.390950 0.547406 0.662932 0.096 Uiso 1 1 calc R U . . .
Cu2 Cu 0.13008(5) 0.43750(4) 0.59912(3) 0.0768(3) Uani 1 1 d . . . . .
O3 O 0.1070(5) 0.4985(3) 0.2258(3) 0.155(3) Uani 1 1 d . . . . .
O4 O 0.1037(3) 0.6505(2) 0.3393(2) 0.1181(18) Uani 1 1 d . . . . .
N5 N 0.1250(3) 0.5104(2) 0.6060(2) 0.0785(15) Uani 1 1 d . . . . .
N6 N 0.1461(3) 0.4293(2) 0.6685(2) 0.0753(14) Uani 1 1 d . . . . .
N7 N 0.1119(3) 0.3664(2) 0.5818(2) 0.0777(14) Uani 1 1 d . . . . .
N8 N 0.1393(3) 0.4553(2) 0.5319(2) 0.0761(14) Uani 1 1 d . . . . .
C47 C 0.1319(3) 0.5065(3) 0.5202(3) 0.0734(18) Uani 1 1 d . . . . .
C48 C 0.1150(4) 0.5136(3) 0.4671(3) 0.0769(18) Uani 1 1 d . . . . .
C49 C 0.1016(4) 0.4636(3) 0.4475(3) 0.0763(18) Uani 1 1 d . . . . .
H49 H 0.084943 0.455110 0.413306 0.092 Uiso 1 1 calc R U . . .
C50 C 0.1173(4) 0.4275(3) 0.4877(3) 0.0788(19) Uani 1 1 d . . . . .
C51 C 0.1058(4) 0.3720(3) 0.4886(3) 0.0809(19) Uani 1 1 d . . . . .
C52 C 0.1134(4) 0.3448(3) 0.5348(3) 0.0821(19) Uani 1 1 d . . . . .
C53 C 0.1289(6) 0.2893(3) 0.5405(3) 0.104(2) Uani 1 1 d . . . . .
H53 H 0.132360 0.264583 0.514045 0.124 Uiso 1 1 calc R U . . .
C54 C 0.1374(5) 0.2790(3) 0.5901(3) 0.099(2) Uani 1 1 d . . . . .
H54 H 0.147955 0.245449 0.604627 0.119 Uiso 1 1 calc R U . . .
C55 C 0.1281(5) 0.3268(3) 0.6177(3) 0.086(2) Uani 1 1 d . . . . .
C56 C 0.1324(4) 0.3333(3) 0.6693(3) 0.0785(18) Uani 1 1 d . . . . .
C57 C 0.1350(4) 0.3817(3) 0.6935(3) 0.0785(18) Uani 1 1 d . . . . .
C58 C 0.1244(4) 0.3912(3) 0.7458(3) 0.0858(19) Uani 1 1 d . . . . .
H58 H 0.117602 0.365357 0.770915 0.103 Uiso 1 1 calc R U . . .
C59 C 0.1258(5) 0.4429(3) 0.7532(3) 0.089(2) Uani 1 1 d . . . . .
H59 H 0.118718 0.460514 0.784122 0.107 Uiso 1 1 calc R U . . .
C60 C 0.1398(4) 0.4663(3) 0.7056(3) 0.0801(18) Uani 1 1 d . . . . .
C61 C 0.1411(4) 0.5222(3) 0.6958(3) 0.0829(19) Uani 1 1 d . . . . .
C62 C 0.1368(4) 0.5424(3) 0.6472(3) 0.0782(18) Uani 1 1 d . . . . .
C63 C 0.1509(5) 0.5944(3) 0.6282(3) 0.092(2) Uani 1 1 d . . . . .
H63 H 0.158101 0.625266 0.647788 0.111 Uiso 1 1 calc R U . . .
C64 C 0.1520(4) 0.5915(3) 0.5775(3) 0.086(2) Uani 1 1 d . . . . .
H64 H 0.160939 0.619820 0.555266 0.104 Uiso 1 1 calc R U . . .
C65 C 0.1373(4) 0.5386(3) 0.5638(3) 0.0779(19) Uani 1 1 d . . . . .
C66 C 0.0874(6) 0.3440(3) 0.4410(3) 0.089(2) Uani 1 1 d . . . . .
C67 C 0.1377(5) 0.3541(3) 0.3985(3) 0.098(2) Uani 1 1 d . . . . .
H67 H 0.187454 0.380099 0.400016 0.117 Uiso 1 1 calc R U . . .
C68 C 0.1177(6) 0.3277(4) 0.3540(3) 0.109(3) Uani 1 1 d . . . . .
H68 H 0.155537 0.335131 0.326092 0.131 Uiso 1 1 calc R U . . .
C69 C 0.0440(8) 0.2904(4) 0.3485(3) 0.115(3) Uani 1 1 d . . . . .
C70 C -0.0053(6) 0.2805(3) 0.3915(4) 0.109(2) Uani 1 1 d . . . . .
H70 H -0.055890 0.254983 0.389877 0.131 Uiso 1 1 calc R U . . .
C71 C 0.0158(7) 0.3060(3) 0.4366(3) 0.100(2) Uani 1 1 d . . . . .
H71 H -0.019607 0.297301 0.465097 0.121 Uiso 1 1 calc R U . . .
C72 C 0.0228(8) 0.2616(4) 0.3001(3) 0.141(3) Uani 1 1 d . . . . .
H72A H 0.068796 0.272753 0.275447 0.211 Uiso 1 1 calc R U . . .
H72B H -0.044357 0.269067 0.287191 0.211 Uiso 1 1 calc R U . . .
H72C H 0.030059 0.223956 0.306085 0.211 Uiso 1 1 calc R U . . .
C73 C 0.1309(5) 0.2857(3) 0.7009(3) 0.0846(19) Uani 1 1 d . . . . .
C74 C 0.0573(6) 0.2488(3) 0.6943(3) 0.102(2) Uani 1 1 d . . . . .
H74 H 0.006460 0.253695 0.668804 0.122 Uiso 1 1 calc R U . . .
C75 C 0.0572(6) 0.2047(3) 0.7249(3) 0.108(2) Uani 1 1 d . . . . .
H75 H 0.004231 0.180803 0.720508 0.130 Uiso 1 1 calc R U . . .
C76 C 0.1302(6) 0.1945(3) 0.7609(3) 0.091(2) Uani 1 1 d . . . . .
C77 C 0.2037(6) 0.2321(4) 0.7676(3) 0.113(3) Uani 1 1 d . . . . .
H77 H 0.254571 0.226973 0.793051 0.136 Uiso 1 1 calc R U . . .
C78 C 0.2044(6) 0.2769(3) 0.7380(3) 0.111(3) Uani 1 1 d . . . . .
H78 H 0.255708 0.301679 0.743296 0.133 Uiso 1 1 calc R U . . .
C79 C 0.1319(6) 0.1458(3) 0.7927(3) 0.104(2) Uani 1 1 d . . . . .
H79A H 0.175453 0.119971 0.778704 0.156 Uiso 1 1 calc R U . . .
H79B H 0.065570 0.131455 0.793038 0.156 Uiso 1 1 calc R U . . .
H79C H 0.155852 0.154480 0.827172 0.156 Uiso 1 1 calc R U . . .
C80 C 0.1490(5) 0.5584(3) 0.7391(3) 0.089(2) Uani 1 1 d . . . . .
C81 C 0.0861(5) 0.6013(3) 0.7423(3) 0.104(2) Uani 1 1 d . . . . .
H81 H 0.034150 0.605829 0.717350 0.125 Uiso 1 1 calc R U . . .
C82 C 0.0977(7) 0.6374(3) 0.7811(4) 0.117(3) Uani 1 1 d . . . . .
H82 H 0.054030 0.666150 0.782204 0.141 Uiso 1 1 calc R U . . .
C83 C 0.1719(7) 0.6318(4) 0.8180(3) 0.114(3) Uani 1 1 d . . . . .
C84 C 0.2346(6) 0.5894(4) 0.8156(3) 0.105(2) Uani 1 1 d . . . . .
H84 H 0.286556 0.584988 0.840577 0.126 Uiso 1 1 calc R U . . .
C85 C 0.2214(5) 0.5528(3) 0.7763(3) 0.096(2) Uani 1 1 d . . . . .
H85 H 0.263992 0.523552 0.775666 0.116 Uiso 1 1 calc R U . . .
C86 C 0.1879(7) 0.6736(4) 0.8591(4) 0.149(4) Uani 1 1 d . . . . .
H86A H 0.142937 0.667307 0.885711 0.223 Uiso 1 1 calc R U . . .
H86B H 0.175371 0.708210 0.844450 0.223 Uiso 1 1 calc R U . . .
H86C H 0.255639 0.671806 0.873293 0.223 Uiso 1 1 calc R U . . .
C87 C 0.1097(4) 0.5639(3) 0.4429(3) 0.086(2) Uani 1 1 d . . . . .
H87 H 0.102787 0.592875 0.464667 0.103 Uiso 1 1 calc R U . . .
C88 C 0.1132(4) 0.5756(3) 0.3929(3) 0.086(2) Uani 1 1 d . . . . .
C89 C 0.1258(4) 0.5384(3) 0.3544(3) 0.091(2) Uani 1 1 d . . . . .
H89 H 0.152015 0.505888 0.365883 0.109 Uiso 1 1 calc R U . . .
C90 C 0.1070(4) 0.5416(3) 0.3047(4) 0.094(2) Uani 1 1 d . . . . .
H90 H 0.081654 0.573401 0.290839 0.113 Uiso 1 1 calc R U . . .
C91 C 0.1236(6) 0.4986(4) 0.2710(5) 0.123(3) Uani 1 1 d . . . . .
H91 H 0.150031 0.467439 0.285744 0.148 Uiso 1 1 calc R U . . .
C92 C 0.1055(4) 0.6327(3) 0.3815(4) 0.106(3) Uani 1 1 d . . . . .
H92 H 0.101685 0.656300 0.408820 0.127 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
Cu1 N3 1.873(5) . ?
Cu1 N4 1.875(5) . ?
Cu1 N1 1.880(5) . ?
Cu1 N2 1.899(5) . ?
O1 C45 1.234(8) . ?
O2 C46 1.196(7) . ?
N1 C1 1.335(7) . ?
N1 C4 1.401(7) . ?
N2 C9 1.371(8) . ?
N2 C6 1.389(7) . ?
N3 C11 1.393(8) . ?
N3 C14 1.393(8) . ?
N4 C19 1.362(7) . ?
N4 C16 1.390(7) . ?
C1 C2 1.433(8) . ?
C1 C19 1.446(8) . ?
C2 C3 1.393(8) . ?
C2 C41 1.407(8) . ?
C3 C4 1.395(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(8) . ?
C5 C6 1.420(8) . ?
C5 C20 1.516(9) . ?
C6 C7 1.419(8) . ?
C7 C8 1.343(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.441(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.412(9) . ?
C10 C11 1.398(9) . ?
C10 C27 1.476(9) . ?
C11 C12 1.451(9) . ?
C12 C13 1.333(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.437(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.407(9) . ?
C15 C16 1.396(9) . ?
C15 C34 1.492(9) . ?
C16 C17 1.412(9) . ?
C17 C18 1.366(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.423(8) . ?
C18 H18 0.9500 . ?
C20 C25 1.391(9) . ?
C20 C21 1.412(9) . ?
C21 C22 1.418(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.380(12) . ?
C22 H22 0.9500 . ?
C23 C24 1.336(12) . ?
C23 C26 1.529(11) . ?
C24 C25 1.371(10) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.370(10) . ?
C27 C32 1.422(10) . ?
C28 C29 1.387(11) . ?
C28 H28 0.9500 . ?
C29 C30 1.381(13) . ?
C29 H29 0.9500 . ?
C30 C31 1.395(13) . ?
C30 C33 1.551(13) . ?
C31 C32 1.400(11) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.387(9) . ?
C34 C39 1.407(9) . ?
C35 C36 1.386(10) . ?
C35 H35 0.9500 . ?
C36 C37 1.383(11) . ?
C36 H36 0.9500 . ?
C37 C38 1.389(10) . ?
C37 C40 1.514(11) . ?
C38 C39 1.379(9) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.383(8) . ?
C41 H41 0.9500 . ?
C42 C43 1.459(9) . ?
C42 C46 1.464(9) . ?
C43 C44 1.331(8) . ?
C43 H43 0.9500 . ?
C44 C45 1.442(10) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
Cu2 N6 1.858(6) . ?
Cu2 N8 1.858(6) . ?
Cu2 N5 1.879(6) . ?
Cu2 N7 1.891(6) . ?
O3 C91 1.211(10) . ?
O4 C92 1.211(8) . ?
N5 C65 1.354(8) . ?
N5 C62 1.370(8) . ?
N6 C60 1.376(8) . ?
N6 C57 1.403(8) . ?
N7 C52 1.370(8) . ?
N7 C55 1.403(8) . ?
N8 C47 1.350(8) . ?
N8 C50 1.394(8) . ?
C47 C65 1.420(9) . ?
C47 C48 1.432(9) . ?
C48 C49 1.391(9) . ?
C48 C87 1.438(9) . ?
C49 C50 1.421(9) . ?
C49 H49 0.9500 . ?
C50 C51 1.430(10) . ?
C51 C52 1.410(9) . ?
C51 C66 1.466(10) . ?
C52 C53 1.445(9) . ?
C53 C54 1.346(9) . ?
C53 H53 0.9500 . ?
C54 C55 1.437(10) . ?
C54 H54 0.9500 . ?
C55 C56 1.380(9) . ?
C56 C57 1.395(9) . ?
C56 C73 1.484(9) . ?
C57 C58 1.431(9) . ?
C58 C59 1.337(9) . ?
C58 H58 0.9500 . ?
C59 C60 1.425(9) . ?
C59 H59 0.9500 . ?
C60 C61 1.455(9) . ?
C61 C62 1.393(9) . ?
C61 C80 1.478(10) . ?
C62 C63 1.442(9) . ?
C63 C64 1.351(9) . ?
C63 H63 0.9500 . ?
C64 C65 1.415(10) . ?
C64 H64 0.9500 . ?
C66 C71 1.380(10) . ?
C66 C67 1.386(9) . ?
C67 C68 1.378(11) . ?
C67 H67 0.9500 . ?
C68 C69 1.388(12) . ?
C68 H68 0.9500 . ?
C69 C70 1.389(11) . ?
C69 C72 1.498(11) . ?
C70 C71 1.383(10) . ?
C70 H70 0.9500 . ?
C71 H71 0.9500 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 C78 1.382(10) . ?
C73 C74 1.384(10) . ?
C74 C75 1.392(10) . ?
C74 H74 0.9500 . ?
C75 C76 1.368(10) . ?
C75 H75 0.9500 . ?
C76 C77 1.396(10) . ?
C76 C79 1.506(9) . ?
C77 C78 1.394(10) . ?
C77 H77 0.9500 . ?
C78 H78 0.9500 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 C85 1.364(9) . ?
C80 C81 1.403(10) . ?
C81 C82 1.386(11) . ?
C81 H81 0.9500 . ?
C82 C83 1.376(11) . ?
C82 H82 0.9500 . ?
C83 C84 1.388(11) . ?
C83 C86 1.537(11) . ?
C84 C85 1.407(10) . ?
C84 H84 0.9500 . ?
C85 H85 0.9500 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 C88 1.369(9) . ?
C87 H87 0.9500 . ?
C88 C89 1.417(10) . ?
C88 C92 1.496(11) . ?
C89 C90 1.337(10) . ?
C89 H89 0.9500 . ?
C90 C91 1.448(12) . ?
C90 H90 0.9500 . ?
C91 H91 0.9500 . ?
C92 H92 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
N3 Cu1 N4 91.5(2) . . ?
N3 Cu1 N1 166.7(2) . . ?
N4 Cu1 N1 81.7(2) . . ?
N3 Cu1 N2 97.3(2) . . ?
N4 Cu1 N2 167.2(2) . . ?
N1 Cu1 N2 91.4(2) . . ?
C1 N1 C4 107.1(5) . . ?
C1 N1 Cu1 117.0(4) . . ?
C4 N1 Cu1 130.7(4) . . ?
C9 N2 C6 107.3(5) . . ?
C9 N2 Cu1 122.9(4) . . ?
C6 N2 Cu1 126.3(4) . . ?
C11 N3 C14 106.6(5) . . ?
C11 N3 Cu1 123.3(4) . . ?
C14 N3 Cu1 126.1(4) . . ?
C19 N4 C16 108.4(5) . . ?
C19 N4 Cu1 116.2(4) . . ?
C16 N4 Cu1 131.6(4) . . ?
N1 C1 C2 111.5(6) . . ?
N1 C1 C19 111.7(5) . . ?
C2 C1 C19 136.6(6) . . ?
C3 C2 C41 131.0(6) . . ?
C3 C2 C1 103.8(5) . . ?
C41 C2 C1 125.2(6) . . ?
C2 C3 C4 109.5(5) . . ?
C2 C3 H3 125.2 . . ?
C4 C3 H3 125.2 . . ?
C5 C4 C3 132.6(6) . . ?
C5 C4 N1 119.6(5) . . ?
C3 C4 N1 107.8(5) . . ?
C4 C5 C6 123.9(6) . . ?
C4 C5 C20 117.5(6) . . ?
C6 C5 C20 118.6(6) . . ?
N2 C6 C7 108.0(5) . . ?
N2 C6 C5 124.0(6) . . ?
C7 C6 C5 127.8(6) . . ?
C8 C7 C6 109.1(6) . . ?
C8 C7 H7 125.5 . . ?
C6 C7 H7 125.5 . . ?
C7 C8 C9 106.8(6) . . ?
C7 C8 H8 126.6 . . ?
C9 C8 H8 126.6 . . ?
N2 C9 C10 124.9(6) . . ?
N2 C9 C8 108.8(6) . . ?
C10 C9 C8 126.2(7) . . ?
C11 C10 C9 123.3(6) . . ?
C11 C10 C27 118.4(6) . . ?
C9 C10 C27 118.3(7) . . ?
N3 C11 C10 125.0(6) . . ?
N3 C11 C12 109.0(6) . . ?
C10 C11 C12 126.0(7) . . ?
C13 C12 C11 106.9(6) . . ?
C13 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
C12 C13 C14 109.5(6) . . ?
C12 C13 H13 125.2 . . ?
C14 C13 H13 125.2 . . ?
N3 C14 C15 125.5(6) . . ?
N3 C14 C13 108.1(6) . . ?
C15 C14 C13 126.3(7) . . ?
C16 C15 C14 122.2(6) . . ?
C16 C15 C34 118.5(6) . . ?
C14 C15 C34 119.3(6) . . ?
N4 C16 C15 120.3(6) . . ?
N4 C16 C17 106.3(6) . . ?
C15 C16 C17 133.3(6) . . ?
C18 C17 C16 110.1(6) . . ?
C18 C17 H17 125.0 . . ?
C16 C17 H17 125.0 . . ?
C17 C18 C19 105.6(6) . . ?
C17 C18 H18 127.2 . . ?
C19 C18 H18 127.2 . . ?
N4 C19 C18 109.3(6) . . ?
N4 C19 C1 111.2(5) . . ?
C18 C19 C1 139.5(6) . . ?
C25 C20 C21 118.7(7) . . ?
C25 C20 C5 121.5(6) . . ?
C21 C20 C5 119.7(6) . . ?
C20 C21 C22 118.0(8) . . ?
C20 C21 H21 121.0 . . ?
C22 C21 H21 121.0 . . ?
C23 C22 C21 121.7(8) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C24 C23 C22 118.0(8) . . ?
C24 C23 C26 122.9(11) . . ?
C22 C23 C26 119.1(10) . . ?
C23 C24 C25 123.8(9) . . ?
C23 C24 H24 118.1 . . ?
C25 C24 H24 118.1 . . ?
C24 C25 C20 119.8(8) . . ?
C24 C25 H25 120.1 . . ?
C20 C25 H25 120.1 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C32 119.4(7) . . ?
C28 C27 C10 120.9(7) . . ?
C32 C27 C10 119.7(7) . . ?
C27 C28 C29 120.6(9) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C30 C29 C28 120.8(10) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C31 119.8(9) . . ?
C29 C30 C33 120.0(11) . . ?
C31 C30 C33 120.2(10) . . ?
C30 C31 C32 119.7(9) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C31 C32 C27 119.5(8) . . ?
C31 C32 H32 120.2 . . ?
C27 C32 H32 120.2 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C39 117.5(6) . . ?
C35 C34 C15 122.2(6) . . ?
C39 C34 C15 120.3(6) . . ?
C36 C35 C34 121.1(7) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C37 C36 C35 121.0(8) . . ?
C37 C36 H36 119.5 . . ?
C35 C36 H36 119.5 . . ?
C36 C37 C38 118.6(7) . . ?
C36 C37 C40 120.1(8) . . ?
C38 C37 C40 121.3(8) . . ?
C39 C38 C37 120.6(7) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C38 C39 C34 121.2(7) . . ?
C38 C39 H39 119.4 . . ?
C34 C39 H39 119.4 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C2 129.8(6) . . ?
C42 C41 H41 115.1 . . ?
C2 C41 H41 115.1 . . ?
C41 C42 C43 123.2(6) . . ?
C41 C42 C46 116.3(6) . . ?
C43 C42 C46 120.5(6) . . ?
C44 C43 C42 126.3(6) . . ?
C44 C43 H43 116.8 . . ?
C42 C43 H43 116.8 . . ?
C43 C44 C45 117.3(7) . . ?
C43 C44 H44 121.3 . . ?
C45 C44 H44 121.3 . . ?
O1 C45 C44 124.5(8) . . ?
O1 C45 H45 117.7 . . ?
C44 C45 H45 117.7 . . ?
O2 C46 C42 127.9(7) . . ?
O2 C46 H46 116.0 . . ?
C42 C46 H46 116.0 . . ?
N6 Cu2 N8 166.9(2) . . ?
N6 Cu2 N5 91.0(3) . . ?
N8 Cu2 N5 81.7(3) . . ?
N6 Cu2 N7 98.0(3) . . ?
N8 Cu2 N7 91.0(3) . . ?
N5 Cu2 N7 167.4(2) . . ?
C65 N5 C62 109.4(6) . . ?
C65 N5 Cu2 116.2(5) . . ?
C62 N5 Cu2 131.9(5) . . ?
C60 N6 C57 104.1(6) . . ?
C60 N6 Cu2 128.9(5) . . ?
C57 N6 Cu2 124.0(5) . . ?
C52 N7 C55 108.7(6) . . ?
C52 N7 Cu2 127.0(5) . . ?
C55 N7 Cu2 121.1(5) . . ?
C47 N8 C50 107.0(6) . . ?
C47 N8 Cu2 116.9(5) . . ?
C50 N8 Cu2 131.7(5) . . ?
N8 C47 C65 112.0(6) . . ?
N8 C47 C48 111.0(7) . . ?
C65 C47 C48 136.9(7) . . ?
C49 C48 C47 105.2(6) . . ?
C49 C48 C87 130.9(7) . . ?
C47 C48 C87 123.9(8) . . ?
C48 C49 C50 107.9(7) . . ?
C48 C49 H49 126.0 . . ?
C50 C49 H49 126.0 . . ?
N8 C50 C49 108.6(7) . . ?
N8 C50 C51 120.7(6) . . ?
C49 C50 C51 130.5(8) . . ?
C52 C51 C50 120.2(7) . . ?
C52 C51 C66 120.8(7) . . ?
C50 C51 C66 119.0(6) . . ?
N7 C52 C51 126.4(7) . . ?
N7 C52 C53 108.1(6) . . ?
C51 C52 C53 125.4(7) . . ?
C54 C53 C52 107.4(7) . . ?
C54 C53 H53 126.3 . . ?
C52 C53 H53 126.3 . . ?
C53 C54 C55 109.3(7) . . ?
C53 C54 H54 125.3 . . ?
C55 C54 H54 125.3 . . ?
C56 C55 N7 125.8(7) . . ?
C56 C55 C54 127.8(7) . . ?
N7 C55 C54 106.4(7) . . ?
C55 C56 C57 124.4(7) . . ?
C55 C56 C73 117.6(7) . . ?
C57 C56 C73 118.0(7) . . ?
C56 C57 N6 123.6(7) . . ?
C56 C57 C58 126.8(7) . . ?
N6 C57 C58 109.5(7) . . ?
C59 C58 C57 108.1(7) . . ?
C59 C58 H58 126.0 . . ?
C57 C58 H58 126.0 . . ?
C58 C59 C60 106.7(7) . . ?
C58 C59 H59 126.6 . . ?
C60 C59 H59 126.6 . . ?
N6 C60 C59 111.5(6) . . ?
N6 C60 C61 123.1(7) . . ?
C59 C60 C61 125.3(8) . . ?
C62 C61 C60 122.1(7) . . ?
C62 C61 C80 119.3(7) . . ?
C60 C61 C80 118.5(7) . . ?
N5 C62 C61 121.3(7) . . ?
N5 C62 C63 106.4(6) . . ?
C61 C62 C63 132.1(8) . . ?
C64 C63 C62 108.0(7) . . ?
C64 C63 H63 126.0 . . ?
C62 C63 H63 126.0 . . ?
C63 C64 C65 107.5(6) . . ?
C63 C64 H64 126.2 . . ?
C65 C64 H64 126.2 . . ?
N5 C65 C64 108.5(7) . . ?
N5 C65 C47 111.5(7) . . ?
C64 C65 C47 140.0(7) . . ?
C71 C66 C67 116.7(8) . . ?
C71 C66 C51 120.0(7) . . ?
C67 C66 C51 123.2(8) . . ?
C68 C67 C66 121.8(8) . . ?
C68 C67 H67 119.1 . . ?
C66 C67 H67 119.1 . . ?
C67 C68 C69 122.2(8) . . ?
C67 C68 H68 118.9 . . ?
C69 C68 H68 118.9 . . ?
C68 C69 C70 115.2(8) . . ?
C68 C69 C72 122.0(9) . . ?
C70 C69 C72 122.7(11) . . ?
C71 C70 C69 123.0(9) . . ?
C71 C70 H70 118.5 . . ?
C69 C70 H70 118.5 . . ?
C66 C71 C70 121.0(8) . . ?
C66 C71 H71 119.5 . . ?
C70 C71 H71 119.5 . . ?
C69 C72 H72A 109.5 . . ?
C69 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C69 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C78 C73 C74 118.1(7) . . ?
C78 C73 C56 120.3(7) . . ?
C74 C73 C56 121.6(7) . . ?
C73 C74 C75 120.4(7) . . ?
C73 C74 H74 119.8 . . ?
C75 C74 H74 119.8 . . ?
C76 C75 C74 122.6(8) . . ?
C76 C75 H75 118.7 . . ?
C74 C75 H75 118.7 . . ?
C75 C76 C77 116.5(7) . . ?
C75 C76 C79 122.7(8) . . ?
C77 C76 C79 120.8(7) . . ?
C78 C77 C76 121.7(8) . . ?
C78 C77 H77 119.1 . . ?
C76 C77 H77 119.1 . . ?
C73 C78 C77 120.5(8) . . ?
C73 C78 H78 119.7 . . ?
C77 C78 H78 119.7 . . ?
C76 C79 H79A 109.5 . . ?
C76 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C76 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C85 C80 C81 117.3(8) . . ?
C85 C80 C61 121.0(7) . . ?
C81 C80 C61 121.6(7) . . ?
C82 C81 C80 121.7(8) . . ?
C82 C81 H81 119.2 . . ?
C80 C81 H81 119.2 . . ?
C83 C82 C81 120.5(8) . . ?
C83 C82 H82 119.7 . . ?
C81 C82 H82 119.7 . . ?
C82 C83 C84 118.7(8) . . ?
C82 C83 C86 120.2(9) . . ?
C84 C83 C86 121.0(9) . . ?
C83 C84 C85 120.2(8) . . ?
C83 C84 H84 119.9 . . ?
C85 C84 H84 119.9 . . ?
C80 C85 C84 121.6(8) . . ?
C80 C85 H85 119.2 . . ?
C84 C85 H85 119.2 . . ?
C83 C86 H86A 109.5 . . ?
C83 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C83 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C88 C87 C48 128.9(8) . . ?
C88 C87 H87 115.6 . . ?
C48 C87 H87 115.6 . . ?
C87 C88 C89 124.7(7) . . ?
C87 C88 C92 114.0(8) . . ?
C89 C88 C92 121.3(7) . . ?
C90 C89 C88 130.6(8) . . ?
C90 C89 H89 114.7 . . ?
C88 C89 H89 114.7 . . ?
C89 C90 C91 122.6(9) . . ?
C89 C90 H90 118.7 . . ?
C91 C90 H90 118.7 . . ?
O3 C91 C90 126.1(10) . . ?
O3 C91 H91 116.9 . . ?
C90 C91 H91 116.9 . . ?
O4 C92 C88 123.6(9) . . ?
O4 C92 H92 118.2 . . ?
C88 C92 H92 118.2 . . ?

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
N3 Cu1 N1 C1 -64.0(10) . . . . ?
N4 Cu1 N1 C1 -4.0(4) . . . . ?
N2 Cu1 N1 C1 165.2(4) . . . . ?
N3 Cu1 N1 C4 145.1(8) . . . . ?
N4 Cu1 N1 C4 -154.9(5) . . . . ?
N2 Cu1 N1 C4 14.3(5) . . . . ?
N3 Cu1 N2 C9 -8.7(4) . . . . ?
N4 Cu1 N2 C9 -141.6(9) . . . . ?
N1 Cu1 N2 C9 161.1(4) . . . . ?
N3 Cu1 N2 C6 -164.8(4) . . . . ?
N4 Cu1 N2 C6 62.3(11) . . . . ?
N1 Cu1 N2 C6 5.0(5) . . . . ?
N4 Cu1 N3 C11 163.1(4) . . . . ?
N1 Cu1 N3 C11 -137.9(9) . . . . ?
N2 Cu1 N3 C11 -7.6(4) . . . . ?
N4 Cu1 N3 C14 8.8(4) . . . . ?
N1 Cu1 N3 C14 67.8(11) . . . . ?
N2 Cu1 N3 C14 -161.9(4) . . . . ?
N3 Cu1 N4 C19 162.7(4) . . . . ?
N1 Cu1 N4 C19 -5.8(3) . . . . ?
N2 Cu1 N4 C19 -64.0(10) . . . . ?
N3 Cu1 N4 C16 7.5(5) . . . . ?
N1 Cu1 N4 C16 -161.0(5) . . . . ?
N2 Cu1 N4 C16 140.8(9) . . . . ?
C4 N1 C1 C2 -6.3(5) . . . . ?
Cu1 N1 C1 C2 -163.7(3) . . . . ?
C4 N1 C1 C19 169.4(4) . . . . ?
Cu1 N1 C1 C19 12.1(5) . . . . ?
N1 C1 C2 C3 5.5(5) . . . . ?
C19 C1 C2 C3 -168.7(6) . . . . ?
N1 C1 C2 C41 -173.8(5) . . . . ?
C19 C1 C2 C41 12.0(9) . . . . ?
C41 C2 C3 C4 176.9(5) . . . . ?
C1 C2 C3 C4 -2.4(5) . . . . ?
C2 C3 C4 C5 177.3(5) . . . . ?
C2 C3 C4 N1 -1.2(5) . . . . ?
C1 N1 C4 C5 -174.1(4) . . . . ?
Cu1 N1 C4 C5 -21.1(7) . . . . ?
C1 N1 C4 C3 4.6(5) . . . . ?
Cu1 N1 C4 C3 157.7(4) . . . . ?
C3 C4 C5 C6 -172.4(5) . . . . ?
N1 C4 C5 C6 6.0(8) . . . . ?
C3 C4 C5 C20 5.5(8) . . . . ?
N1 C4 C5 C20 -176.2(5) . . . . ?
C9 N2 C6 C7 -0.7(6) . . . . ?
Cu1 N2 C6 C7 158.4(4) . . . . ?
C9 N2 C6 C5 -177.2(5) . . . . ?
Cu1 N2 C6 C5 -18.1(8) . . . . ?
C4 C5 C6 N2 13.3(8) . . . . ?
C20 C5 C6 N2 -164.6(5) . . . . ?
C4 C5 C6 C7 -162.6(6) . . . . ?
C20 C5 C6 C7 19.6(9) . . . . ?
N2 C6 C7 C8 0.9(7) . . . . ?
C5 C6 C7 C8 177.2(6) . . . . ?
C6 C7 C8 C9 -0.7(7) . . . . ?
C6 N2 C9 C10 179.1(5) . . . . ?
Cu1 N2 C9 C10 19.1(8) . . . . ?
C6 N2 C9 C8 0.3(6) . . . . ?
Cu1 N2 C9 C8 -159.7(4) . . . . ?
C7 C8 C9 N2 0.2(7) . . . . ?
C7 C8 C9 C10 -178.5(6) . . . . ?
N2 C9 C10 C11 -11.9(9) . . . . ?
C8 C9 C10 C11 166.7(6) . . . . ?
N2 C9 C10 C27 166.3(6) . . . . ?
C8 C9 C10 C27 -15.1(9) . . . . ?
C14 N3 C11 C10 174.7(5) . . . . ?
Cu1 N3 C11 C10 16.1(7) . . . . ?
C14 N3 C11 C12 -1.6(6) . . . . ?
Cu1 N3 C11 C12 -160.1(4) . . . . ?
C9 C10 C11 N3 -7.3(9) . . . . ?
C27 C10 C11 N3 174.6(5) . . . . ?
C9 C10 C11 C12 168.4(6) . . . . ?
C27 C10 C11 C12 -9.8(9) . . . . ?
N3 C11 C12 C13 1.2(7) . . . . ?
C10 C11 C12 C13 -175.0(6) . . . . ?
C11 C12 C13 C14 -0.4(7) . . . . ?
C11 N3 C14 C15 -176.6(5) . . . . ?
Cu1 N3 C14 C15 -18.8(8) . . . . ?
C11 N3 C14 C13 1.3(6) . . . . ?
Cu1 N3 C14 C13 159.1(4) . . . . ?
C12 C13 C14 N3 -0.6(7) . . . . ?
C12 C13 C14 C15 177.3(6) . . . . ?
N3 C14 C15 C16 11.1(9) . . . . ?
C13 C14 C15 C16 -166.4(5) . . . . ?
N3 C14 C15 C34 -170.6(5) . . . . ?
C13 C14 C15 C34 11.9(9) . . . . ?
C19 N4 C16 C15 -171.7(5) . . . . ?
Cu1 N4 C16 C15 -15.1(8) . . . . ?
C19 N4 C16 C17 5.1(6) . . . . ?
Cu1 N4 C16 C17 161.7(4) . . . . ?
C14 C15 C16 N4 5.6(8) . . . . ?
C34 C15 C16 N4 -172.7(5) . . . . ?
C14 C15 C16 C17 -170.2(6) . . . . ?
C34 C15 C16 C17 11.6(9) . . . . ?
N4 C16 C17 C18 -2.9(6) . . . . ?
C15 C16 C17 C18 173.4(6) . . . . ?
C16 C17 C18 C19 -0.4(6) . . . . ?
C16 N4 C19 C18 -5.5(6) . . . . ?
Cu1 N4 C19 C18 -166.2(3) . . . . ?
C16 N4 C19 C1 174.1(4) . . . . ?
Cu1 N4 C19 C1 13.4(5) . . . . ?
C17 C18 C19 N4 3.7(6) . . . . ?
C17 C18 C19 C1 -175.8(6) . . . . ?
N1 C1 C19 N4 -16.0(6) . . . . ?
C2 C1 C19 N4 158.2(5) . . . . ?
N1 C1 C19 C18 163.5(6) . . . . ?
C2 C1 C19 C18 -22.3(11) . . . . ?
C4 C5 C20 C25 -131.5(6) . . . . ?
C6 C5 C20 C25 46.4(8) . . . . ?
C4 C5 C20 C21 46.5(7) . . . . ?
C6 C5 C20 C21 -135.6(6) . . . . ?
C25 C20 C21 C22 2.8(9) . . . . ?
C5 C20 C21 C22 -175.2(5) . . . . ?
C20 C21 C22 C23 -2.6(10) . . . . ?
C21 C22 C23 C24 1.3(12) . . . . ?
C21 C22 C23 C26 -179.8(7) . . . . ?
C22 C23 C24 C25 -0.2(14) . . . . ?
C26 C23 C24 C25 -179.1(8) . . . . ?
C23 C24 C25 C20 0.5(13) . . . . ?
C21 C20 C25 C24 -1.9(10) . . . . ?
C5 C20 C25 C24 176.1(6) . . . . ?
C11 C10 C27 C28 125.2(8) . . . . ?
C9 C10 C27 C28 -53.1(9) . . . . ?
C11 C10 C27 C32 -55.8(8) . . . . ?
C9 C10 C27 C32 126.0(7) . . . . ?
C32 C27 C28 C29 2.4(14) . . . . ?
C10 C27 C28 C29 -178.5(9) . . . . ?
C27 C28 C29 C30 1.5(18) . . . . ?
C28 C29 C30 C31 -4(2) . . . . ?
C28 C29 C30 C33 177.9(12) . . . . ?
C29 C30 C31 C32 2.6(18) . . . . ?
C33 C30 C31 C32 -179.3(11) . . . . ?
C30 C31 C32 C27 1.2(14) . . . . ?
C28 C27 C32 C31 -3.7(12) . . . . ?
C10 C27 C32 C31 177.2(7) . . . . ?
C16 C15 C34 C35 51.9(9) . . . . ?
C14 C15 C34 C35 -126.4(7) . . . . ?
C16 C15 C34 C39 -130.2(7) . . . . ?
C14 C15 C34 C39 51.5(8) . . . . ?
C39 C34 C35 C36 -0.3(11) . . . . ?
C15 C34 C35 C36 177.7(7) . . . . ?
C34 C35 C36 C37 -0.7(13) . . . . ?
C35 C36 C37 C38 2.0(15) . . . . ?
C35 C36 C37 C40 -179.3(9) . . . . ?
C36 C37 C38 C39 -2.2(14) . . . . ?
C40 C37 C38 C39 179.1(9) . . . . ?
C37 C38 C39 C34 1.2(13) . . . . ?
C35 C34 C39 C38 0.1(11) . . . . ?
C15 C34 C39 C38 -177.9(7) . . . . ?
C3 C2 C41 C42 -13.8(9) . . . . ?
C1 C2 C41 C42 165.3(5) . . . . ?
C2 C41 C42 C43 -3.9(9) . . . . ?
C2 C41 C42 C46 178.6(5) . . . . ?
C41 C42 C43 C44 158.9(6) . . . . ?
C46 C42 C43 C44 -23.6(8) . . . . ?
C42 C43 C44 C45 -177.6(5) . . . . ?
C43 C44 C45 O1 178.5(6) . . . . ?
C41 C42 C46 O2 -178.2(6) . . . . ?
C43 C42 C46 O2 4.2(9) . . . . ?
N6 Cu2 N5 C65 164.2(4) . . . . ?
N8 Cu2 N5 C65 -4.8(4) . . . . ?
N7 Cu2 N5 C65 -59.3(12) . . . . ?
N6 Cu2 N5 C62 4.3(5) . . . . ?
N8 Cu2 N5 C62 -164.7(5) . . . . ?
N7 Cu2 N5 C62 140.7(10) . . . . ?
N8 Cu2 N6 C60 64.1(12) . . . . ?
N5 Cu2 N6 C60 8.2(5) . . . . ?
N7 Cu2 N6 C60 -163.1(5) . . . . ?
N8 Cu2 N6 C57 -138.3(10) . . . . ?
N5 Cu2 N6 C57 165.8(4) . . . . ?
N7 Cu2 N6 C57 -5.5(4) . . . . ?
N6 Cu2 N7 C52 -167.4(5) . . . . ?
N8 Cu2 N7 C52 3.0(5) . . . . ?
N5 Cu2 N7 C52 56.7(12) . . . . ?
N6 Cu2 N7 C55 -9.6(5) . . . . ?
N8 Cu2 N7 C55 160.8(4) . . . . ?
N5 Cu2 N7 C55 -145.5(10) . . . . ?
N6 Cu2 N8 C47 -60.8(11) . . . . ?
N5 Cu2 N8 C47 -4.0(4) . . . . ?
N7 Cu2 N8 C47 165.8(4) . . . . ?
N6 Cu2 N8 C50 146.3(9) . . . . ?
N5 Cu2 N8 C50 -156.9(5) . . . . ?
N7 Cu2 N8 C50 12.9(5) . . . . ?
C50 N8 C47 C65 170.6(4) . . . . ?
Cu2 N8 C47 C65 11.4(5) . . . . ?
C50 N8 C47 C48 -6.0(6) . . . . ?
Cu2 N8 C47 C48 -165.2(3) . . . . ?
N8 C47 C48 C49 6.4(6) . . . . ?
C65 C47 C48 C49 -169.0(6) . . . . ?
N8 C47 C48 C87 -176.3(5) . . . . ?
C65 C47 C48 C87 8.3(9) . . . . ?
C47 C48 C49 C50 -4.1(6) . . . . ?
C87 C48 C49 C50 178.8(5) . . . . ?
C47 N8 C50 C49 3.3(6) . . . . ?
Cu2 N8 C50 C49 158.1(4) . . . . ?
C47 N8 C50 C51 -171.6(5) . . . . ?
Cu2 N8 C50 C51 -16.8(8) . . . . ?
C48 C49 C50 N8 0.6(6) . . . . ?
C48 C49 C50 C51 174.9(5) . . . . ?
N8 C50 C51 C52 2.0(8) . . . . ?
C49 C50 C51 C52 -171.6(5) . . . . ?
N8 C50 C51 C66 -177.1(5) . . . . ?
C49 C50 C51 C66 9.3(9) . . . . ?
C55 N7 C52 C51 -176.0(6) . . . . ?
Cu2 N7 C52 C51 -16.0(9) . . . . ?
C55 N7 C52 C53 1.3(7) . . . . ?
Cu2 N7 C52 C53 161.3(5) . . . . ?
C50 C51 C52 N7 14.0(9) . . . . ?
C66 C51 C52 N7 -166.8(6) . . . . ?
C50 C51 C52 C53 -162.9(6) . . . . ?
C66 C51 C52 C53 16.3(10) . . . . ?
N7 C52 C53 C54 -0.8(8) . . . . ?
C51 C52 C53 C54 176.6(6) . . . . ?
C52 C53 C54 C55 -0.1(8) . . . . ?
C52 N7 C55 C56 179.6(6) . . . . ?
Cu2 N7 C55 C56 18.2(8) . . . . ?
C52 N7 C55 C54 -1.4(7) . . . . ?
Cu2 N7 C55 C54 -162.8(4) . . . . ?
C53 C54 C55 C56 179.9(7) . . . . ?
C53 C54 C55 N7 0.9(8) . . . . ?
N7 C55 C56 C57 -9.6(10) . . . . ?
C54 C55 C56 C57 171.5(6) . . . . ?
N7 C55 C56 C73 168.5(6) . . . . ?
C54 C55 C56 C73 -10.4(10) . . . . ?
C55 C56 C57 N6 -8.4(9) . . . . ?
C73 C56 C57 N6 173.6(5) . . . . ?
C55 C56 C57 C58 169.7(6) . . . . ?
C73 C56 C57 C58 -8.3(9) . . . . ?
C60 N6 C57 C56 177.0(5) . . . . ?
Cu2 N6 C57 C56 14.9(7) . . . . ?
C60 N6 C57 C58 -1.3(6) . . . . ?
Cu2 N6 C57 C58 -163.5(4) . . . . ?
C56 C57 C58 C59 -176.5(6) . . . . ?
N6 C57 C58 C59 1.8(7) . . . . ?
C57 C58 C59 C60 -1.5(7) . . . . ?
C57 N6 C60 C59 0.4(6) . . . . ?
Cu2 N6 C60 C59 161.4(4) . . . . ?
C57 N6 C60 C61 -175.9(5) . . . . ?
Cu2 N6 C60 C61 -14.9(8) . . . . ?
C58 C59 C60 N6 0.7(7) . . . . ?
C58 C59 C60 C61 176.9(6) . . . . ?
N6 C60 C61 C62 8.1(9) . . . . ?
C59 C60 C61 C62 -167.7(6) . . . . ?
N6 C60 C61 C80 -170.9(5) . . . . ?
C59 C60 C61 C80 13.4(9) . . . . ?
C65 N5 C62 C61 -171.2(5) . . . . ?
Cu2 N5 C62 C61 -10.3(8) . . . . ?
C65 N5 C62 C63 4.0(6) . . . . ?
Cu2 N5 C62 C63 165.0(4) . . . . ?
C60 C61 C62 N5 4.1(9) . . . . ?
C80 C61 C62 N5 -177.0(5) . . . . ?
C60 C61 C62 C63 -169.8(6) . . . . ?
C80 C61 C62 C63 9.2(10) . . . . ?
N5 C62 C63 C64 -3.0(7) . . . . ?
C61 C62 C63 C64 171.5(6) . . . . ?
C62 C63 C64 C65 0.9(7) . . . . ?
C62 N5 C65 C64 -3.6(6) . . . . ?
Cu2 N5 C65 C64 -167.9(4) . . . . ?
C62 N5 C65 C47 176.3(5) . . . . ?
Cu2 N5 C65 C47 12.0(6) . . . . ?
C63 C64 C65 N5 1.6(7) . . . . ?
C63 C64 C65 C47 -178.2(7) . . . . ?
N8 C47 C65 N5 -14.7(6) . . . . ?
C48 C47 C65 N5 160.7(6) . . . . ?
N8 C47 C65 C64 165.1(7) . . . . ?
C48 C47 C65 C64 -19.5(12) . . . . ?
C52 C51 C66 C71 46.0(9) . . . . ?
C50 C51 C66 C71 -134.9(7) . . . . ?
C52 C51 C66 C67 -135.2(7) . . . . ?
C50 C51 C66 C67 43.9(9) . . . . ?
C71 C66 C67 C68 -0.2(10) . . . . ?
C51 C66 C67 C68 -179.0(6) . . . . ?
C66 C67 C68 C69 2.0(12) . . . . ?
C67 C68 C69 C70 -2.3(12) . . . . ?
C67 C68 C69 C72 -179.7(7) . . . . ?
C68 C69 C70 C71 0.8(12) . . . . ?
C72 C69 C70 C71 178.2(8) . . . . ?
C67 C66 C71 C70 -1.3(11) . . . . ?
C51 C66 C71 C70 177.6(6) . . . . ?
C69 C70 C71 C66 1.0(12) . . . . ?
C55 C56 C73 C78 125.2(7) . . . . ?
C57 C56 C73 C78 -56.7(8) . . . . ?
C55 C56 C73 C74 -54.6(9) . . . . ?
C57 C56 C73 C74 123.6(7) . . . . ?
C78 C73 C74 C75 0.9(11) . . . . ?
C56 C73 C74 C75 -179.4(7) . . . . ?
C73 C74 C75 C76 -2.7(12) . . . . ?
C74 C75 C76 C77 3.2(12) . . . . ?
C74 C75 C76 C79 -177.9(7) . . . . ?
C75 C76 C77 C78 -2.1(12) . . . . ?
C79 C76 C77 C78 178.9(7) . . . . ?
C74 C73 C78 C77 0.1(11) . . . . ?
C56 C73 C78 C77 -179.6(7) . . . . ?
C76 C77 C78 C73 0.5(12) . . . . ?
C62 C61 C80 C85 -126.9(7) . . . . ?
C60 C61 C80 C85 52.0(9) . . . . ?
C62 C61 C80 C81 49.5(9) . . . . ?
C60 C61 C80 C81 -131.5(7) . . . . ?
C85 C80 C81 C82 1.2(11) . . . . ?
C61 C80 C81 C82 -175.4(7) . . . . ?
C80 C81 C82 C83 -0.3(13) . . . . ?
C81 C82 C83 C84 -0.1(13) . . . . ?
C81 C82 C83 C86 176.5(8) . . . . ?
C82 C83 C84 C85 -0.4(12) . . . . ?
C86 C83 C84 C85 -177.0(8) . . . . ?
C81 C80 C85 C84 -1.8(11) . . . . ?
C61 C80 C85 C84 174.8(7) . . . . ?
C83 C84 C85 C80 1.5(12) . . . . ?
C49 C48 C87 C88 -17.5(10) . . . . ?
C47 C48 C87 C88 165.9(5) . . . . ?
C48 C87 C88 C89 -1.7(9) . . . . ?
C48 C87 C88 C92 -180.0(5) . . . . ?
C87 C88 C89 C90 161.3(6) . . . . ?
C92 C88 C89 C90 -20.6(10) . . . . ?
C88 C89 C90 C91 -179.0(6) . . . . ?
C89 C90 C91 O3 179.0(8) . . . . ?
C87 C88 C92 O4 -177.3(6) . . . . ?
C89 C88 C92 O4 4.4(9) . . . . ?

_refine_diff_density_max         0.568
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.066



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane/dichloromethane'
####################################################################### 
# 
# 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_AS3_2016
_database_code_depnum_ccdc_archive 'CCDC 1587848'
_audit_update_record             
;
2018-03-01 deposited with the CCDC.
2018-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H45 Ga N4 O5, 0.65(C H2 Cl2)'
_chemical_formula_sum            'C52.70 H46.40 Cl1.40 Ga N4 O5'
_chemical_formula_weight         934.48

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'
Ga Ga 0.2307 1.6083 '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'

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

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

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

_cell_length_a                   36.7663(9)
_cell_length_b                   17.2278(4)
_cell_length_c                   14.6878(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.4310(10)
_cell_angle_gamma                90
_cell_volume                     9118.7(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    90.0(5)
_cell_measurement_reflns_used    5512
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      23.38
_exptl_crystal_description       needle
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_F_000             3881
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.739
_shelx_estimated_absorpt_T_min   0.854
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90.0(5)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'TRIUMPH curved graphite'
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33613
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.844
_diffrn_reflns_theta_max         26.751
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9678
_reflns_number_gt                6080
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0524P)²+0.8008P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9678
_refine_ls_number_parameters     594
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1184
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
Ga1 Ga 0.68121(2) 0.74394(2) 0.22366(2) 0.02323(10) Uani 1 1 d . . . . .
O1B O 0.81397(15) 0.8756(3) 0.6756(4) 0.0208(11) Uani 0.7 1 d D . P A 1
O2B O 0.7927(3) 1.0036(4) 0.6663(5) 0.0259(16) Uani 0.7 1 d D . P A 1
O3 O 0.62799(6) 1.04831(10) 0.67269(13) 0.0306(5) Uani 1 1 d . . . . .
O4 O 0.92606(7) 0.82580(16) 0.40861(18) 0.0628(8) Uani 1 1 d . . . . .
O5 O 0.67833(6) 0.84380(11) 0.14407(13) 0.0263(5) Uani 1 1 d D . . . .
H5O H 0.6653(8) 0.8796(14) 0.157(2) 0.039 Uiso 1 1 d D U . . .
N1 N 0.67506(7) 0.80026(12) 0.33341(15) 0.0219(5) Uani 1 1 d . . . . .
N2 N 0.62932(7) 0.72482(12) 0.19139(15) 0.0226(6) Uani 1 1 d . . . . .
N3 N 0.69469(7) 0.67559(12) 0.13377(15) 0.0216(5) Uani 1 1 d . . . . .
N4 N 0.73287(7) 0.75772(12) 0.28071(15) 0.0235(5) Uani 1 1 d . . . . .
C1 C 0.70684(9) 0.82370(15) 0.39182(18) 0.0241(7) Uani 1 1 d . . . . .
C2 C 0.69696(9) 0.86260(15) 0.46797(19) 0.0259(7) Uani 1 1 d . . . . .
H2 H 0.713401 0.884776 0.519469 0.031 Uiso 0.3 1 calc R U P B 2
C3 C 0.65768(9) 0.86204(15) 0.45244(18) 0.0259(7) Uani 1 1 d . . . . .
C4 C 0.64456(9) 0.82163(15) 0.36601(19) 0.0234(7) Uani 1 1 d . . . . .
C5 C 0.60872(8) 0.80386(15) 0.31422(18) 0.0217(7) Uani 1 1 d . . . . .
C6 C 0.60214(8) 0.75921(15) 0.23213(19) 0.0226(6) Uani 1 1 d . . . . .
C7 C 0.56707(9) 0.73911(15) 0.17674(19) 0.0266(7) Uani 1 1 d . . . . .
H7 H 0.543572 0.754989 0.187721 0.032 Uiso 1 1 calc R U . . .
C8 C 0.57283(9) 0.69355(16) 0.1058(2) 0.0287(7) Uani 1 1 d . . . . .
H8 H 0.554171 0.672262 0.058282 0.034 Uiso 1 1 calc R U . . .
C9 C 0.61199(9) 0.68318(15) 0.11510(19) 0.0235(7) Uani 1 1 d . . . . .
C10 C 0.63097(9) 0.63869(15) 0.05798(18) 0.0231(7) Uani 1 1 d . . . . .
C11 C 0.66972(9) 0.63504(14) 0.06874(19) 0.0219(7) Uani 1 1 d . . . . .
C12 C 0.69076(9) 0.59020(15) 0.01417(19) 0.0255(7) Uani 1 1 d . . . . .
H12 H 0.680763 0.556736 -0.035979 0.031 Uiso 1 1 calc R U . . .
C13 C 0.72712(9) 0.60416(15) 0.04690(19) 0.0254(7) Uani 1 1 d . . . . .
H13 H 0.747131 0.582197 0.023515 0.030 Uiso 1 1 calc R U . . .
C14 C 0.73048(9) 0.65762(15) 0.12278(19) 0.0241(7) Uani 1 1 d . . . . .
C15 C 0.76357(9) 0.68603(15) 0.17706(19) 0.0247(7) Uani 1 1 d . . . . .
C16 C 0.76505(8) 0.73419(15) 0.25629(19) 0.0234(7) Uani 1 1 d . . . . .
C17 C 0.79511(9) 0.76522(15) 0.3249(2) 0.0276(7) Uani 1 1 d . . . . .
C18 C 0.77880(9) 0.80537(15) 0.3901(2) 0.0278(7) Uani 1 1 d . . . . .
H18 H 0.791653 0.831608 0.443809 0.033 Uiso 0.7 1 calc R U P C 1
C19 C 0.74034(9) 0.79967(15) 0.36152(19) 0.0240(7) Uani 1 1 d . . . . .
C20 C 0.72450(12) 0.8858(2) 0.5539(3) 0.0202(9) Uani 0.7 1 d . . P A 1
H20 H 0.716077 0.878974 0.610449 0.024 Uiso 0.7 1 calc R U P A 1
C21 C 0.75844(12) 0.9139(2) 0.5633(3) 0.0196(9) Uani 0.7 1 d . . P A 1
H21 H 0.768075 0.926634 0.509779 0.024 Uiso 0.7 1 calc R U P A 1
C22B C 0.78177(14) 0.9260(3) 0.6577(4) 0.0217(12) Uani 0.7 1 d D . P A 1
H22B H 0.766277 0.914780 0.704970 0.026 Uiso 0.7 1 calc R U P A 1
C20A C 0.7918(3) 0.8376(5) 0.4921(6) 0.022(2) Uiso 0.3 1 d . . P D 2
H20A H 0.811553 0.809069 0.528720 0.026 Uiso 0.3 1 calc R U P D 2
C21A C 0.7803(3) 0.8964(5) 0.5353(6) 0.022(2) Uiso 0.3 1 d . . P D 2
H21A H 0.763691 0.932183 0.499389 0.027 Uiso 0.3 1 calc R U P D 2
C23B C 0.84157(14) 0.8907(3) 0.6231(3) 0.0296(11) Uani 0.7 1 d . . P A 1
H23A H 0.861992 0.853688 0.640435 0.044 Uiso 0.7 1 calc R U P A 1
H23B H 0.830838 0.885332 0.556779 0.044 Uiso 0.7 1 calc R U P A 1
H23C H 0.850991 0.943684 0.635641 0.044 Uiso 0.7 1 calc R U P A 1
C24B C 0.7975(5) 1.0131(10) 0.7507(12) 0.036(5) Uiso 0.3 1 d D . P D 2
H24A H 0.799162 1.069632 0.757643 0.054 Uiso 0.3 1 calc R U P D 2
H24B H 0.775561 0.994280 0.772524 0.054 Uiso 0.3 1 calc R U P D 2
H24C H 0.819810 0.989112 0.787519 0.054 Uiso 0.3 1 calc R U P D 2
C25 C 0.63541(9) 0.89679(15) 0.51216(19) 0.0284(7) Uani 1 1 d . . . . .
H25 H 0.611040 0.876967 0.508314 0.034 Uiso 1 1 calc R U . . .
C26 C 0.64619(9) 0.95494(16) 0.57293(19) 0.0281(7) Uani 1 1 d . . . . .
H26 H 0.670918 0.973700 0.580897 0.034 Uiso 1 1 calc R U . . .
C27 C 0.62175(9) 0.98925(16) 0.62567(19) 0.0289(7) Uani 1 1 d . . . . .
H27 H 0.598626 0.964178 0.624228 0.035 Uiso 1 1 calc R U . . .
C28 C 0.57520(8) 0.83261(16) 0.34656(19) 0.0247(7) Uani 1 1 d . . . . .
C29 C 0.56241(8) 0.90805(16) 0.3260(2) 0.0280(7) Uani 1 1 d . . . . .
H29 H 0.575220 0.941190 0.291279 0.034 Uiso 1 1 calc R U . . .
C30 C 0.53127(9) 0.93511(17) 0.3555(2) 0.0330(8) Uani 1 1 d . . . . .
H30 H 0.523152 0.986798 0.340995 0.040 Uiso 1 1 calc R U . . .
C31 C 0.51166(9) 0.88867(19) 0.4059(2) 0.0368(8) Uani 1 1 d . . . . .
C32 C 0.52485(10) 0.81364(19) 0.4273(2) 0.0396(9) Uani 1 1 d . . . . .
H32 H 0.512227 0.780862 0.462842 0.047 Uiso 1 1 calc R U . . .
C33 C 0.55585(9) 0.78597(17) 0.3980(2) 0.0331(8) Uani 1 1 d . . . . .
H33 H 0.564071 0.734435 0.413145 0.040 Uiso 1 1 calc R U . . .
C34 C 0.47674(9) 0.9167(2) 0.4346(3) 0.0496(10) Uani 1 1 d . . . . .
H34A H 0.455074 0.894159 0.393378 0.074 Uiso 1 1 calc R U . . .
H34B H 0.475483 0.973437 0.430285 0.074 Uiso 1 1 calc R U . . .
H34C H 0.476969 0.900718 0.498720 0.074 Uiso 1 1 calc R U . . .
C35 C 0.60863(9) 0.59084(17) -0.0179(2) 0.0287(7) Uani 1 1 d . . . . .
C36 C 0.60758(11) 0.6085(2) -0.1106(2) 0.0489(10) Uani 1 1 d . . . . .
H36 H 0.620651 0.652509 -0.126257 0.059 Uiso 1 1 calc R U . . .
C37 C 0.58775(12) 0.5627(2) -0.1804(2) 0.0588(11) Uani 1 1 d . . . . .
H37 H 0.586733 0.576889 -0.243379 0.071 Uiso 1 1 calc R U . . .
C38 C 0.56950(11) 0.4973(2) -0.1608(3) 0.0524(10) Uani 1 1 d . . . . .
C39 C 0.57136(12) 0.4789(2) -0.0685(3) 0.0607(12) Uani 1 1 d . . . . .
H39 H 0.559157 0.433562 -0.053063 0.073 Uiso 1 1 calc R U . . .
C40 C 0.59049(10) 0.52469(19) 0.0012(2) 0.0456(9) Uani 1 1 d . . . . .
H40 H 0.591250 0.510470 0.064077 0.055 Uiso 1 1 calc R U . . .
C41 C 0.54943(13) 0.4464(3) -0.2392(3) 0.0902(17) Uani 1 1 d . . . . .
H41A H 0.532242 0.478261 -0.283546 0.135 Uiso 1 1 calc R U . . .
H41B H 0.535526 0.406038 -0.213871 0.135 Uiso 1 1 calc R U . . .
H41C H 0.567576 0.422153 -0.270981 0.135 Uiso 1 1 calc R U . . .
C42 C 0.79904(8) 0.66302(16) 0.14913(19) 0.0252(7) Uani 1 1 d . . . . .
C43 C 0.81675(9) 0.71507(17) 0.1005(2) 0.0306(7) Uani 1 1 d . . . . .
H43 H 0.806013 0.764578 0.084266 0.037 Uiso 1 1 calc R U . . .
C44 C 0.84995(9) 0.69553(17) 0.0753(2) 0.0306(7) Uani 1 1 d . . . . .
H44 H 0.861769 0.732167 0.042453 0.037 Uiso 1 1 calc R U . . .
C45 C 0.86626(9) 0.62370(16) 0.0969(2) 0.0287(7) Uani 1 1 d . . . . .
C46 C 0.84791(9) 0.57053(17) 0.1430(2) 0.0322(8) Uani 1 1 d . . . . .
H46 H 0.858246 0.520436 0.157504 0.039 Uiso 1 1 calc R U . . .
C47 C 0.81460(9) 0.59006(16) 0.1681(2) 0.0300(7) Uani 1 1 d . . . . .
H47 H 0.802257 0.552792 0.198815 0.036 Uiso 1 1 calc R U . . .
C48 C 0.90291(9) 0.60560(18) 0.0704(2) 0.0394(8) Uani 1 1 d . . . . .
H48A H 0.902692 0.624739 0.007494 0.059 Uiso 1 1 calc R U . . .
H48B H 0.906903 0.549335 0.072372 0.059 Uiso 1 1 calc R U . . .
H48C H 0.922972 0.630978 0.114210 0.059 Uiso 1 1 calc R U . . .
C49 C 0.83441(9) 0.75760(17) 0.3276(2) 0.0346(8) Uani 1 1 d . . . . .
H49 H 0.841608 0.718238 0.289462 0.042 Uiso 1 1 calc R U . . .
C50 C 0.86199(10) 0.79987(19) 0.3780(2) 0.0382(8) Uani 1 1 d . . . . .
H50 H 0.856456 0.838494 0.419327 0.046 Uiso 1 1 calc R U . . .
C51 C 0.89959(11) 0.7870(2) 0.3696(3) 0.0476(10) Uani 1 1 d . . . . .
H51 H 0.904388 0.745465 0.331066 0.057 Uiso 1 1 calc R U . . .
C52 C 0.71018(9) 0.87781(18) 0.1182(2) 0.0382(8) Uani 1 1 d . . . . .
H52A H 0.722842 0.911305 0.168595 0.057 Uiso 1 1 calc R U . . .
H52B H 0.702450 0.908776 0.061734 0.057 Uiso 1 1 calc R U . . .
H52C H 0.727123 0.836727 0.106614 0.057 Uiso 1 1 calc R U . . .
C22A C 0.7920(4) 0.9117(8) 0.6417(9) 0.024(4) Uiso 0.3 1 d D . P D 2
H22A H 0.771413 0.892924 0.671449 0.029 Uiso 0.3 1 calc R U P D 2
C23A C 0.8576(3) 0.9012(7) 0.6558(8) 0.029(3) Uiso 0.3 1 d . . P D 2
H23D H 0.879290 0.871385 0.686295 0.044 Uiso 0.3 1 calc R U P D 2
H23E H 0.854813 0.896715 0.588232 0.044 Uiso 0.3 1 calc R U P D 2
H23F H 0.860864 0.955858 0.673931 0.044 Uiso 0.3 1 calc R U P D 2
O1A O 0.8247(3) 0.8710(9) 0.6836(12) 0.026(4) Uiso 0.3 1 d D . P D 2
O2A O 0.7945(7) 0.9928(9) 0.6541(13) 0.030(5) Uiso 0.3 1 d D . P D 2
C24A C 0.8104(2) 1.0246(3) 0.7594(4) 0.0291(14) Uani 0.7 1 d D . P A 1
H24D H 0.817426 1.079574 0.760949 0.044 Uiso 0.7 1 calc R U P A 1
H24E H 0.793150 1.015947 0.801386 0.044 Uiso 0.7 1 calc R U P A 1
H24F H 0.832633 0.992772 0.779162 0.044 Uiso 0.7 1 calc R U P A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga1 N2 1.901(2) . ?
Ga1 N3 1.906(2) . ?
Ga1 N1 1.933(2) . ?
Ga1 N4 1.933(2) . ?
Ga1 O5 2.0709(19) . ?
O1B C23B 1.415(7) . ?
O1B C22B 1.449(6) . ?
O2B C22B 1.395(7) . ?
O2B C24A 1.440(7) . ?
O3 C27 1.226(3) . ?
O4 C51 1.225(4) . ?
O5 C52 1.427(3) . ?
O5 H5O 0.826(17) . ?
N1 C4 1.354(3) . ?
N1 C1 1.367(3) . ?
N2 C9 1.376(3) . ?
N2 C6 1.394(3) . ?
N3 C11 1.377(3) . ?
N3 C14 1.392(4) . ?
N4 C16 1.364(4) . ?
N4 C19 1.370(3) . ?
C1 C2 1.412(4) . ?
C1 C19 1.450(4) . ?
C2 C3 1.416(4) . ?
C2 C20 1.507(5) . ?
C2 H2 0.9500 . ?
C3 C25 1.443(4) . ?
C3 C4 1.444(4) . ?
C4 C5 1.418(4) . ?
C5 C6 1.410(4) . ?
C5 C28 1.491(4) . ?
C6 C7 1.424(4) . ?
C7 C8 1.354(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.430(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.418(4) . ?
C10 C11 1.404(4) . ?
C10 C35 1.494(4) . ?
C11 C12 1.443(4) . ?
C12 C13 1.350(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.432(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.404(4) . ?
C15 C16 1.421(4) . ?
C15 C42 1.496(4) . ?
C16 C17 1.442(4) . ?
C17 C18 1.408(4) . ?
C17 C49 1.443(4) . ?
C18 C19 1.396(4) . ?
C18 C20A 1.580(9) . ?
C18 H18 0.9500 . ?
C20 C21 1.320(5) . ?
C20 H20 0.9500 . ?
C21 C22B 1.493(6) . ?
C21 H21 0.9500 . ?
C22B H22B 1.0000 . ?
C20A C21A 1.311(12) . ?
C20A H20A 0.9500 . ?
C21A C22A 1.560(16) . ?
C21A H21A 0.9500 . ?
C23B H23A 0.9800 . ?
C23B H23B 0.9800 . ?
C23B H23C 0.9800 . ?
C24B O2A 1.445(14) . ?
C24B H24A 0.9800 . ?
C24B H24B 0.9800 . ?
C24B H24C 0.9800 . ?
C25 C26 1.348(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.426(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C33 1.391(4) . ?
C28 C29 1.395(4) . ?
C29 C30 1.383(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.385(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.394(4) . ?
C31 C34 1.508(4) . ?
C32 C33 1.381(4) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C40 1.377(4) . ?
C35 C36 1.389(4) . ?
C36 C37 1.381(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.371(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.380(5) . ?
C38 C41 1.518(5) . ?
C39 C40 1.372(4) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C47 1.386(4) . ?
C42 C43 1.387(4) . ?
C43 C44 1.386(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.384(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.391(4) . ?
C45 C48 1.508(4) . ?
C46 C47 1.388(4) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.345(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.429(5) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C22A O2A 1.410(14) . ?
C22A O1A 1.422(13) . ?
C22A H22A 1.0000 . ?
C23A O1A 1.447(19) . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 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
N2 Ga1 N3 96.09(10) . . ?
N2 Ga1 N1 91.00(10) . . ?
N3 Ga1 N1 167.71(10) . . ?
N2 Ga1 N4 168.75(9) . . ?
N3 Ga1 N4 90.47(10) . . ?
N1 Ga1 N4 81.03(10) . . ?
N2 Ga1 O5 93.82(9) . . ?
N3 Ga1 O5 96.51(8) . . ?
N1 Ga1 O5 93.01(8) . . ?
N4 Ga1 O5 94.50(9) . . ?
C23B O1B C22B 116.1(5) . . ?
C22B O2B C24A 113.3(5) . . ?
C52 O5 Ga1 122.59(18) . . ?
C52 O5 H5O 107(2) . . ?
Ga1 O5 H5O 117(2) . . ?
C4 N1 C1 111.3(2) . . ?
C4 N1 Ga1 132.3(2) . . ?
C1 N1 Ga1 116.43(19) . . ?
C9 N2 C6 108.4(2) . . ?
C9 N2 Ga1 124.97(19) . . ?
C6 N2 Ga1 126.04(19) . . ?
C11 N3 C14 108.8(2) . . ?
C11 N3 Ga1 124.39(19) . . ?
C14 N3 Ga1 126.80(19) . . ?
C16 N4 C19 110.4(2) . . ?
C16 N4 Ga1 132.73(19) . . ?
C19 N4 Ga1 116.8(2) . . ?
N1 C1 C2 108.4(3) . . ?
N1 C1 C19 113.3(2) . . ?
C2 C1 C19 138.3(3) . . ?
C1 C2 C3 106.5(3) . . ?
C1 C2 C20 123.6(3) . . ?
C3 C2 C20 129.1(3) . . ?
C1 C2 H2 126.8 . . ?
C3 C2 H2 126.8 . . ?
C2 C3 C25 125.6(3) . . ?
C2 C3 C4 107.3(2) . . ?
C25 C3 C4 127.1(3) . . ?
N1 C4 C5 119.9(2) . . ?
N1 C4 C3 106.6(3) . . ?
C5 C4 C3 133.5(3) . . ?
C6 C5 C4 124.1(3) . . ?
C6 C5 C28 116.2(3) . . ?
C4 C5 C28 119.8(2) . . ?
N2 C6 C5 125.6(3) . . ?
N2 C6 C7 107.2(2) . . ?
C5 C6 C7 127.1(3) . . ?
C8 C7 C6 108.6(3) . . ?
C8 C7 H7 125.7 . . ?
C6 C7 H7 125.7 . . ?
C7 C8 C9 107.9(3) . . ?
C7 C8 H8 126.1 . . ?
C9 C8 H8 126.1 . . ?
N2 C9 C10 124.1(3) . . ?
N2 C9 C8 107.9(2) . . ?
C10 C9 C8 128.0(3) . . ?
C11 C10 C9 124.4(3) . . ?
C11 C10 C35 117.1(2) . . ?
C9 C10 C35 118.5(3) . . ?
N3 C11 C10 125.3(2) . . ?
N3 C11 C12 107.5(3) . . ?
C10 C11 C12 127.2(3) . . ?
C13 C12 C11 108.0(3) . . ?
C13 C12 H12 126.0 . . ?
C11 C12 H12 126.0 . . ?
C12 C13 C14 108.6(3) . . ?
C12 C13 H13 125.7 . . ?
C14 C13 H13 125.7 . . ?
N3 C14 C15 126.1(3) . . ?
N3 C14 C13 107.2(3) . . ?
C15 C14 C13 126.7(3) . . ?
C14 C15 C16 123.8(3) . . ?
C14 C15 C42 117.1(3) . . ?
C16 C15 C42 119.0(3) . . ?
N4 C16 C15 119.6(3) . . ?
N4 C16 C17 106.9(2) . . ?
C15 C16 C17 133.5(3) . . ?
C18 C17 C16 106.7(3) . . ?
C18 C17 C49 125.8(3) . . ?
C16 C17 C49 127.6(3) . . ?
C19 C18 C17 107.7(3) . . ?
C19 C18 C20A 114.1(4) . . ?
C17 C18 C20A 136.7(4) . . ?
C19 C18 H18 126.2 . . ?
C17 C18 H18 126.2 . . ?
N4 C19 C18 108.3(3) . . ?
N4 C19 C1 112.3(3) . . ?
C18 C19 C1 139.3(3) . . ?
C21 C20 C2 130.5(3) . . ?
C21 C20 H20 114.7 . . ?
C2 C20 H20 114.7 . . ?
C20 C21 C22B 120.4(4) . . ?
C20 C21 H21 119.8 . . ?
C22B C21 H21 119.8 . . ?
O2B C22B O1B 110.3(6) . . ?
O2B C22B C21 108.6(4) . . ?
O1B C22B C21 112.6(5) . . ?
O2B C22B H22B 108.4 . . ?
O1B C22B H22B 108.4 . . ?
C21 C22B H22B 108.4 . . ?
C21A C20A C18 131.7(8) . . ?
C21A C20A H20A 114.2 . . ?
C18 C20A H20A 114.2 . . ?
C20A C21A C22A 124.4(10) . . ?
C20A C21A H21A 117.8 . . ?
C22A C21A H21A 117.8 . . ?
O1B C23B H23A 109.5 . . ?
O1B C23B H23B 109.5 . . ?
H23A C23B H23B 109.5 . . ?
O1B C23B H23C 109.5 . . ?
H23A C23B H23C 109.5 . . ?
H23B C23B H23C 109.5 . . ?
O2A C24B H24A 109.5 . . ?
O2A C24B H24B 109.5 . . ?
H24A C24B H24B 109.5 . . ?
O2A C24B H24C 109.5 . . ?
H24A C24B H24C 109.5 . . ?
H24B C24B H24C 109.5 . . ?
C26 C25 C3 125.7(3) . . ?
C26 C25 H25 117.2 . . ?
C3 C25 H25 117.2 . . ?
C25 C26 C27 122.2(3) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
O3 C27 C26 125.6(3) . . ?
O3 C27 H27 117.2 . . ?
C26 C27 H27 117.2 . . ?
C33 C28 C29 118.0(3) . . ?
C33 C28 C5 121.7(3) . . ?
C29 C28 C5 120.3(2) . . ?
C30 C29 C28 120.7(3) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C29 C30 C31 121.6(3) . . ?
C29 C30 H30 119.2 . . ?
C31 C30 H30 119.2 . . ?
C30 C31 C32 117.5(3) . . ?
C30 C31 C34 121.8(3) . . ?
C32 C31 C34 120.7(3) . . ?
C33 C32 C31 121.4(3) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C32 C33 C28 120.8(3) . . ?
C32 C33 H33 119.6 . . ?
C28 C33 H33 119.6 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C40 C35 C36 117.4(3) . . ?
C40 C35 C10 121.4(3) . . ?
C36 C35 C10 121.0(3) . . ?
C37 C36 C35 120.7(3) . . ?
C37 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
C38 C37 C36 121.4(3) . . ?
C38 C37 H37 119.3 . . ?
C36 C37 H37 119.3 . . ?
C37 C38 C39 117.7(3) . . ?
C37 C38 C41 120.0(4) . . ?
C39 C38 C41 122.3(4) . . ?
C40 C39 C38 121.3(3) . . ?
C40 C39 H39 119.4 . . ?
C38 C39 H39 119.4 . . ?
C39 C40 C35 121.4(3) . . ?
C39 C40 H40 119.3 . . ?
C35 C40 H40 119.3 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C47 C42 C43 118.2(3) . . ?
C47 C42 C15 122.2(3) . . ?
C43 C42 C15 119.6(3) . . ?
C44 C43 C42 120.6(3) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C45 C44 C43 121.3(3) . . ?
C45 C44 H44 119.3 . . ?
C43 C44 H44 119.3 . . ?
C44 C45 C46 118.1(3) . . ?
C44 C45 C48 119.6(3) . . ?
C46 C45 C48 122.3(3) . . ?
C47 C46 C45 120.5(3) . . ?
C47 C46 H46 119.7 . . ?
C45 C46 H46 119.7 . . ?
C42 C47 C46 121.1(3) . . ?
C42 C47 H47 119.4 . . ?
C46 C47 H47 119.4 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 C17 127.4(3) . . ?
C50 C49 H49 116.3 . . ?
C17 C49 H49 116.3 . . ?
C49 C50 C51 120.4(3) . . ?
C49 C50 H50 119.8 . . ?
C51 C50 H50 119.8 . . ?
O4 C51 C50 124.5(4) . . ?
O4 C51 H51 117.7 . . ?
C50 C51 H51 117.7 . . ?
O5 C52 H52A 109.5 . . ?
O5 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
O5 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O2A C22A O1A 114.0(16) . . ?
O2A C22A C21A 107.1(12) . . ?
O1A C22A C21A 113.1(12) . . ?
O2A C22A H22A 107.5 . . ?
O1A C22A H22A 107.5 . . ?
C21A C22A H22A 107.5 . . ?
O1A C23A H23D 109.5 . . ?
O1A C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
O1A C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C22A O1A C23A 112.5(13) . . ?
C22A O2A C24B 110.9(15) . . ?
O2B C24A H24D 109.5 . . ?
O2B C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
O2B C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O5 H5O O3 0.826(17) 1.898(18) 2.714(3) 170(3) 6_575 yes

_refine_diff_density_max         0.359
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.066



