# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1973478'
loop_
_audit_author_name
_audit_author_address
'Dr Manjit K. Bhattacharyya'
;Cotton University
India
;
_audit_update_record             
;
2019-12-21 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C96 H84 Cu6 N16 O40'
_chemical_formula_sum            'C96 H84 Cu6 N16 O40'
_chemical_formula_weight         2483.03

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'
Cu Cu 0.3201 1.2651 '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      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                   12.317(5)
_cell_length_b                   14.999(7)
_cell_length_c                   17.394(8)
_cell_angle_alpha                79.894(9)
_cell_angle_beta                 84.538(9)
_cell_angle_gamma                71.908(9)
_cell_volume                     3004(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4277
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      18.01

_exptl_crystal_description       Block
_exptl_crystal_colour            'Dark Blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_F_000             1266
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    1.127
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53096
_diffrn_reflns_av_unetI/netI     0.1356
_diffrn_reflns_av_R_equivalents  0.1565
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.868
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10550
_reflns_number_gt                5663
_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 (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)+(0.1461P)²+5.1959P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10550
_refine_ls_number_parameters     712
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.0866
_refine_ls_wR_factor_ref         0.2998
_refine_ls_wR_factor_gt          0.2340
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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 0.72504(8) 0.16465(7) 0.45875(6) 0.0510(3) Uani 1 1 d . . . . .
Cu2 Cu 0.73312(8) 0.42102(7) 0.31701(6) 0.0511(3) Uani 1 1 d . . . . .
Cu3 Cu 0.69724(9) 0.56057(8) 0.16365(6) 0.0594(4) Uani 1 1 d . . . . .
O3 O 0.6929(5) 0.2504(4) 0.5385(3) 0.0536(14) Uani 1 1 d . . . . .
O4 O 0.7016(5) 0.3329(4) 0.4232(4) 0.0591(15) Uani 1 1 d . . . . .
O2 O 0.5634(5) 0.1808(4) 0.4542(4) 0.0613(15) Uani 1 1 d . . . . .
O5 O 0.5796(5) 0.4389(4) 0.2862(4) 0.0639(16) Uani 1 1 d . . . . .
O7 O 0.6895(5) 0.5453(4) 0.3519(4) 0.0612(15) Uani 1 1 d . . . . .
O8 O 0.6901(6) 0.6433(4) 0.2397(4) 0.0686(17) Uani 1 1 d . . . . .
O6 O 0.5374(5) 0.5645(5) 0.1896(4) 0.0674(16) Uani 1 1 d . . . . .
O1 O 0.6113(6) 0.0672(5) 0.5559(4) 0.0771(19) Uani 1 1 d . . . . .
N2 N 0.8941(5) 0.1413(4) 0.4591(4) 0.0493(16) Uani 1 1 d . . . . .
N1 N 0.7730(6) 0.0751(5) 0.3809(4) 0.0537(17) Uani 1 1 d . . . . .
N3 N 0.7988(6) 0.3112(5) 0.2569(4) 0.0538(17) Uani 1 1 d . . . . .
N4 N 0.9001(6) 0.3968(5) 0.3354(4) 0.0541(17) Uani 1 1 d . . . . .
N6 N 0.8682(6) 0.5234(6) 0.1529(4) 0.0619(19) Uani 1 1 d . . . . .
N5 N 0.7202(7) 0.4678(5) 0.0890(4) 0.0613(19) Uani 1 1 d . . . . .
C41 C 0.6895(6) 0.3301(6) 0.4956(5) 0.0488(19) Uani 1 1 d . . . . .
O9 O 0.6581(7) 0.6832(5) 0.0720(5) 0.102(3) Uani 1 1 d . . . . .
C47 C 0.6833(7) 0.6262(6) 0.3124(6) 0.054(2) Uani 1 1 d . . . . .
C11 C 0.9535(7) 0.0807(5) 0.4111(5) 0.0487(19) Uani 1 1 d . . . . .
C42 C 0.6770(8) 0.4153(6) 0.5325(6) 0.063(2) Uani 1 1 d . . . . .
H42A H 0.622493 0.468947 0.503432 0.075 Uiso 1 1 calc R U . . .
H42B H 0.749963 0.428227 0.526600 0.075 Uiso 1 1 calc R U . . .
C37 C 0.5380(8) 0.1266(6) 0.5150(6) 0.057(2) Uani 1 1 d . . . . .
C45 C 0.5119(8) 0.5051(7) 0.2442(6) 0.058(2) Uani 1 1 d . . . . .
C44 C 0.6498(8) 0.4936(7) 0.6534(6) 0.066(3) Uani 1 1 d . . . . .
H44A H 0.601649 0.552598 0.626059 0.080 Uiso 1 1 calc R U . . .
H44B H 0.728327 0.495209 0.646038 0.080 Uiso 1 1 calc R U . . .
C24 C 0.9170(8) 0.2811(6) 0.2551(5) 0.058(2) Uani 1 1 d . . . . .
C7 C 1.0734(7) 0.0541(6) 0.4004(5) 0.059(2) Uani 1 1 d . . . . .
C4 C 0.9444(8) -0.0243(6) 0.3184(5) 0.062(2) Uani 1 1 d . . . . .
C43 C 0.6387(8) 0.4107(6) 0.6183(5) 0.059(2) Uani 1 1 d . . . . .
H43A H 0.684437 0.351700 0.647191 0.071 Uiso 1 1 calc R U . . .
H43B H 0.559617 0.410732 0.623958 0.071 Uiso 1 1 calc R U . . .
C23 C 0.9697(7) 0.3291(6) 0.2970(5) 0.058(2) Uani 1 1 d . . . . .
C12 C 0.8885(7) 0.0435(6) 0.3685(5) 0.054(2) Uani 1 1 d . . . . .
C22 C 0.9482(8) 0.4388(7) 0.3768(5) 0.066(2) Uani 1 1 d . . . . .
H22 H 0.902436 0.486863 0.403335 0.079 Uiso 1 1 calc R U . . .
C10 C 0.9516(7) 0.1788(6) 0.5000(5) 0.059(2) Uani 1 1 d . . . . .
H10 H 0.911094 0.219926 0.534251 0.071 Uiso 1 1 calc R U . . .
C46 C 0.3846(7) 0.5140(7) 0.2589(6) 0.069(3) Uani 1 1 d . . . . .
H46A H 0.367916 0.464246 0.237655 0.083 Uiso 1 1 calc R U . . .
H46B H 0.339584 0.574607 0.231931 0.083 Uiso 1 1 calc R U . . .
C13 C 0.7461(9) 0.2678(6) 0.2193(5) 0.066(2) Uani 1 1 d . . . . .
H13 H 0.666570 0.286784 0.220784 0.080 Uiso 1 1 calc R U . . .
C9 C 1.0681(8) 0.1582(7) 0.4925(6) 0.071(3) Uani 1 1 d . . . . .
H9 H 1.105458 0.186905 0.520070 0.085 Uiso 1 1 calc R U . . .
C36 C 0.8315(9) 0.4285(7) 0.0707(5) 0.064(2) Uani 1 1 d . . . . .
C1 C 0.7079(9) 0.0414(7) 0.3426(6) 0.072(3) Uani 1 1 d . . . . .
H1 H 0.628657 0.062698 0.348985 0.087 Uiso 1 1 calc R U . . .
C48 C 0.6683(9) 0.7069(6) 0.3567(5) 0.067(2) Uani 1 1 d . . . . .
H48A H 0.604882 0.759595 0.335311 0.080 Uiso 1 1 calc R U . . .
H48B H 0.736408 0.727289 0.347047 0.080 Uiso 1 1 calc R U . . .
C40 C 0.3537(8) 0.3128(6) 0.5552(6) 0.065(2) Uani 1 1 d . . . . .
H40A H 0.432210 0.313481 0.544243 0.079 Uiso 1 1 calc R U . . .
H40B H 0.304111 0.375061 0.534798 0.079 Uiso 1 1 calc R U . . .
C19 C 1.0891(8) 0.3027(7) 0.2972(6) 0.072(3) Uani 1 1 d . . . . .
C35 C 0.9115(8) 0.4577(7) 0.1043(5) 0.066(2) Uani 1 1 d . . . . .
C6 C 1.1286(8) -0.0121(7) 0.3512(6) 0.073(3) Uani 1 1 d . . . . .
H6 H 1.207918 -0.030885 0.345451 0.088 Uiso 1 1 calc R U . . .
C38 C 0.4107(7) 0.1390(6) 0.5340(6) 0.069(3) Uani 1 1 d . . . . .
H38A H 0.387617 0.097421 0.506500 0.083 Uiso 1 1 calc R U . . .
H38B H 0.400486 0.118402 0.589578 0.083 Uiso 1 1 calc R U . . .
C8 C 1.1301(8) 0.0948(7) 0.4441(6) 0.073(3) Uani 1 1 d . . . . .
H8 H 1.209470 0.079080 0.440405 0.088 Uiso 1 1 calc R U . . .
C15 C 0.9209(11) 0.1678(7) 0.1742(6) 0.079(3) Uani 1 1 d . . . . .
H15 H 0.960129 0.120211 0.145154 0.095 Uiso 1 1 calc R U . . .
C20 C 1.1371(9) 0.3479(9) 0.3424(7) 0.081(3) Uani 1 1 d . . . . .
H20 H 1.215991 0.332998 0.344615 0.098 Uiso 1 1 calc R U . . .
C39 C 0.3325(8) 0.2383(7) 0.5136(6) 0.072(3) Uani 1 1 d . . . . .
H39A H 0.254256 0.237412 0.525780 0.086 Uiso 1 1 calc R U . . .
H39B H 0.339910 0.257755 0.457609 0.086 Uiso 1 1 calc R U . . .
O20 O 0.4312(8) 0.2266(8) 0.3179(5) 0.136(4) Uani 1 1 d . . . . .
C14 C 0.8057(11) 0.1953(7) 0.1780(6) 0.079(3) Uani 1 1 d . . . . .
H14 H 0.766369 0.165558 0.153015 0.095 Uiso 1 1 calc R U . . .
N8 N 0.9976(11) 0.3287(9) 0.6348(10) 0.111(4) Uani 1 1 d . . . . .
C25 C 0.6416(10) 0.4419(8) 0.0575(6) 0.078(3) Uani 1 1 d . . . . .
H25 H 0.564409 0.468337 0.070057 0.093 Uiso 1 1 calc R U . . .
C33 C 1.0595(10) 0.5226(10) 0.1703(7) 0.093(4) Uani 1 1 d . . . . .
H33 H 1.107654 0.546643 0.192993 0.111 Uiso 1 1 calc R U . . .
C16 C 0.9840(9) 0.2095(6) 0.2132(6) 0.068(3) Uani 1 1 d . . . . .
C3 C 0.8741(10) -0.0565(8) 0.2802(6) 0.081(3) Uani 1 1 d . . . . .
H3 H 0.906697 -0.099188 0.245537 0.097 Uiso 1 1 calc R U . . .
C18 C 1.1529(9) 0.2292(9) 0.2518(7) 0.088(4) Uani 1 1 d . . . . .
H18 H 1.232359 0.211087 0.250530 0.105 Uiso 1 1 calc R U . . .
C2 C 0.7615(11) -0.0283(8) 0.2915(6) 0.085(3) Uani 1 1 d . . . . .
H2 H 0.716676 -0.053248 0.266524 0.102 Uiso 1 1 calc R U . . .
C31 C 1.0307(10) 0.4199(8) 0.0887(6) 0.083(3) Uani 1 1 d . . . . .
C34 C 0.9407(9) 0.5566(8) 0.1848(6) 0.079(3) Uani 1 1 d . . . . .
H34 H 0.911531 0.602658 0.217078 0.095 Uiso 1 1 calc R U . . .
C17 C 1.1027(10) 0.1877(8) 0.2129(7) 0.079(3) Uani 1 1 d . . . . .
H17 H 1.147582 0.141947 0.183861 0.095 Uiso 1 1 calc R U . . .
C28 C 0.8701(12) 0.3590(8) 0.0175(6) 0.087(3) Uani 1 1 d . . . . .
C5 C 1.0665(9) -0.0501(7) 0.3109(6) 0.079(3) Uani 1 1 d . . . . .
H5 H 1.105213 -0.093633 0.278100 0.095 Uiso 1 1 calc R U . . .
C29 C 0.9908(14) 0.3223(9) 0.0030(7) 0.100(4) Uani 1 1 d . . . . .
H29 H 1.017596 0.277195 -0.030394 0.120 Uiso 1 1 calc R U . . .
C30 C 1.0666(12) 0.3501(9) 0.0354(8) 0.098(4) Uani 1 1 d . . . . .
H30 H 1.144186 0.324286 0.023610 0.118 Uiso 1 1 calc R U . . .
C21 C 1.0688(11) 0.4117(10) 0.3815(7) 0.089(4) Uani 1 1 d . . . . .
H21 H 1.100025 0.440132 0.413423 0.107 Uiso 1 1 calc R U . . .
N7 N 0.4326(13) 0.3107(12) 0.1169(8) 0.125(5) Uani 1 1 d . . . . .
C26 C 0.6743(13) 0.3762(9) 0.0063(7) 0.099(4) Uani 1 1 d . . . . .
H26 H 0.618426 0.358669 -0.014491 0.118 Uiso 1 1 calc R U . . .
C32 C 1.1047(9) 0.4558(9) 0.1240(7) 0.087(3) Uani 1 1 d . . . . .
H32 H 1.183440 0.433396 0.115213 0.104 Uiso 1 1 calc R U . . .
C27 C 0.7874(14) 0.3361(8) -0.0146(7) 0.099(4) Uani 1 1 d . . . . .
H27 H 0.807283 0.293684 -0.050333 0.119 Uiso 1 1 calc R U . . .
O17 O 0.6283(12) 0.2509(10) 0.8411(9) 0.197(6) Uani 1 1 d . . . . .
O15 O 0.4876(14) 0.2992(14) 0.1657(9) 0.234(9) Uani 1 1 d . . . . .
O16 O 0.5693(11) 0.9620(12) 0.6953(8) 0.216(7) Uani 1 1 d . . . . .
O18 O 0.6221(12) 0.1805(9) 0.7019(8) 0.181(5) Uani 1 1 d . . . . .
O10 O 0.9198(13) 0.2954(12) 0.6483(9) 0.204(6) Uani 1 1 d . . . . .
O19 O 0.8593(12) 0.2457(11) 0.8099(8) 0.199(6) Uani 1 1 d . . . . .
O12 O 1.0142(14) 0.3627(9) 0.5689(8) 0.191(7) Uani 1 1 d . . . . .
O14 O 0.4043(15) 0.3716(15) 0.0652(10) 0.219(8) Uani 1 1 d . . . . .
O11 O 1.0487(18) 0.3229(15) 0.6847(12) 0.270(10) Uani 1 1 d . . . . .
O13 O 0.381(3) 0.2621(17) 0.1198(15) 0.330(14) Uani 1 1 d . . . . .
H9B H 0.595302 0.673100 0.051002 0.080 Uiso 1 1 d . U . . .
H9A H 0.655400 0.725700 0.072800 0.080 Uiso 1 1 d . 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 O2 1.937(6) . ?
Cu1 O3 1.985(5) . ?
Cu1 N1 1.995(7) . ?
Cu1 N2 2.002(6) . ?
Cu1 O4 2.423(6) . ?
Cu2 O5 1.940(6) . ?
Cu2 O7 1.961(6) . ?
Cu2 N3 2.020(7) . ?
Cu2 N4 2.021(7) . ?
Cu2 O4 2.153(6) . ?
Cu3 O8 1.945(6) . ?
Cu3 O6 1.963(6) . ?
Cu3 N6 2.003(8) . ?
Cu3 N5 2.006(7) . ?
Cu3 O9 2.173(7) . ?
O3 C41 1.284(9) . ?
O4 C41 1.248(10) . ?
O2 C37 1.293(11) . ?
O5 C45 1.250(11) . ?
O7 C47 1.269(10) . ?
O8 C47 1.245(10) . ?
O6 C45 1.270(10) . ?
O1 C37 1.230(11) . ?
N2 C11 1.340(10) . ?
N2 C10 1.345(10) . ?
N1 C1 1.346(10) . ?
N1 C12 1.362(10) . ?
N3 C13 1.329(11) . ?
N3 C24 1.382(11) . ?
N4 C22 1.319(11) . ?
N4 C23 1.342(11) . ?
N6 C34 1.349(12) . ?
N6 C35 1.359(12) . ?
N5 C25 1.341(12) . ?
N5 C36 1.346(11) . ?
C41 C42 1.489(11) . ?
O9 H9B 0.949(8) . ?
O9 H9A 0.630(7) . ?
C47 C48 1.501(11) . ?
C11 C7 1.408(11) . ?
C11 C12 1.427(11) . ?
C42 C43 1.518(12) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C37 C38 1.531(12) . ?
C45 C46 1.532(12) . ?
C44 C43 1.525(11) . ?
C44 C46 1.538(13) 2_666 ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C24 C16 1.404(12) . ?
C24 C23 1.427(12) . ?
C7 C6 1.397(13) . ?
C7 C8 1.402(13) . ?
C4 C3 1.380(13) . ?
C4 C12 1.426(11) . ?
C4 C5 1.431(13) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C23 C19 1.401(12) . ?
C22 C21 1.419(14) . ?
C22 H22 0.9300 . ?
C10 C9 1.370(12) . ?
C10 H10 0.9300 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C13 C14 1.384(13) . ?
C13 H13 0.9300 . ?
C9 C8 1.380(14) . ?
C9 H9 0.9300 . ?
C36 C35 1.405(13) . ?
C36 C28 1.453(13) . ?
C1 C2 1.451(13) . ?
C1 H1 0.9300 . ?
C48 C40 1.524(13) 2_666 ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C40 C39 1.531(11) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C19 C20 1.398(15) . ?
C19 C18 1.451(16) . ?
C35 C31 1.419(14) . ?
C6 C5 1.383(14) . ?
C6 H6 0.9300 . ?
C38 C39 1.504(13) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C8 H8 0.9300 . ?
C15 C14 1.348(15) . ?
C15 C16 1.416(14) . ?
C15 H15 0.9300 . ?
C20 C21 1.305(15) . ?
C20 H20 0.9300 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C14 H14 0.9300 . ?
N8 O11 1.096(17) . ?
N8 O12 1.197(15) . ?
N8 O10 1.198(15) . ?
C25 C26 1.386(15) . ?
C25 H25 0.9300 . ?
C33 C32 1.346(16) . ?
C33 C34 1.406(15) . ?
C33 H33 0.9300 . ?
C16 C17 1.396(14) . ?
C3 C2 1.323(14) . ?
C3 H3 0.9300 . ?
C18 C17 1.301(15) . ?
C18 H18 0.9300 . ?
C2 H2 0.9300 . ?
C31 C32 1.424(16) . ?
C31 C30 1.458(17) . ?
C34 H34 0.9300 . ?
C17 H17 0.9300 . ?
C28 C27 1.365(17) . ?
C28 C29 1.430(17) . ?
C5 H5 0.9300 . ?
C29 C30 1.338(18) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C21 H21 0.9300 . ?
N7 O15 1.093(14) . ?
N7 O13 1.098(19) . ?
N7 O14 1.157(17) . ?
C26 C27 1.376(17) . ?
C26 H26 0.9300 . ?
C32 H32 0.9300 . ?
C27 H27 0.9300 . ?

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
O2 Cu1 O3 90.8(2) . . ?
O2 Cu1 N1 94.5(3) . . ?
O3 Cu1 N1 174.6(2) . . ?
O2 Cu1 N2 176.2(3) . . ?
O3 Cu1 N2 92.9(2) . . ?
N1 Cu1 N2 81.7(3) . . ?
O2 Cu1 O4 93.5(2) . . ?
O3 Cu1 O4 58.1(2) . . ?
N1 Cu1 O4 122.4(2) . . ?
N2 Cu1 O4 88.9(2) . . ?
O5 Cu2 O7 92.6(2) . . ?
O5 Cu2 N3 91.8(3) . . ?
O7 Cu2 N3 164.4(3) . . ?
O5 Cu2 N4 172.5(3) . . ?
O7 Cu2 N4 92.4(3) . . ?
N3 Cu2 N4 81.8(3) . . ?
O5 Cu2 O4 89.6(2) . . ?
O7 Cu2 O4 100.8(2) . . ?
N3 Cu2 O4 94.1(2) . . ?
N4 Cu2 O4 94.9(2) . . ?
O8 Cu3 O6 90.8(3) . . ?
O8 Cu3 N6 93.0(3) . . ?
O6 Cu3 N6 165.4(3) . . ?
O8 Cu3 N5 174.3(3) . . ?
O6 Cu3 N5 93.5(3) . . ?
N6 Cu3 N5 81.9(3) . . ?
O8 Cu3 O9 89.8(3) . . ?
O6 Cu3 O9 95.3(3) . . ?
N6 Cu3 O9 98.8(3) . . ?
N5 Cu3 O9 93.5(3) . . ?
C41 O3 Cu1 101.3(5) . . ?
C41 O4 Cu2 142.4(5) . . ?
C41 O4 Cu1 82.0(5) . . ?
Cu2 O4 Cu1 133.9(3) . . ?
C37 O2 Cu1 105.7(5) . . ?
C45 O5 Cu2 132.2(6) . . ?
C47 O7 Cu2 129.3(6) . . ?
C47 O8 Cu3 129.2(6) . . ?
C45 O6 Cu3 121.0(6) . . ?
C11 N2 C10 118.6(7) . . ?
C11 N2 Cu1 113.2(5) . . ?
C10 N2 Cu1 128.2(6) . . ?
C1 N1 C12 118.1(8) . . ?
C1 N1 Cu1 129.0(6) . . ?
C12 N1 Cu1 112.8(5) . . ?
C13 N3 C24 118.2(8) . . ?
C13 N3 Cu2 129.9(6) . . ?
C24 N3 Cu2 111.9(6) . . ?
C22 N4 C23 117.4(8) . . ?
C22 N4 Cu2 129.7(7) . . ?
C23 N4 Cu2 112.8(6) . . ?
C34 N6 C35 118.9(9) . . ?
C34 N6 Cu3 128.8(8) . . ?
C35 N6 Cu3 112.2(6) . . ?
C25 N5 C36 119.1(8) . . ?
C25 N5 Cu3 128.9(7) . . ?
C36 N5 Cu3 112.0(6) . . ?
O4 C41 O3 118.5(7) . . ?
O4 C41 C42 121.5(8) . . ?
O3 C41 C42 119.9(8) . . ?
Cu3 O9 H9B 98.8(5) . . ?
Cu3 O9 H9A 130.1(8) . . ?
H9B O9 H9A 116.6(10) . . ?
O8 C47 O7 124.8(8) . . ?
O8 C47 C48 117.7(8) . . ?
O7 C47 C48 117.5(8) . . ?
N2 C11 C7 123.8(8) . . ?
N2 C11 C12 116.4(7) . . ?
C7 C11 C12 119.8(8) . . ?
C41 C42 C43 117.4(7) . . ?
C41 C42 H42A 108.0 . . ?
C43 C42 H42A 108.0 . . ?
C41 C42 H42B 108.0 . . ?
C43 C42 H42B 108.0 . . ?
H42A C42 H42B 107.2 . . ?
O1 C37 O2 122.6(8) . . ?
O1 C37 C38 120.8(9) . . ?
O2 C37 C38 116.6(9) . . ?
O5 C45 O6 127.0(8) . . ?
O5 C45 C46 116.4(9) . . ?
O6 C45 C46 116.6(9) . . ?
C43 C44 C46 112.0(7) . 2_666 ?
C43 C44 H44A 109.2 . . ?
C46 C44 H44A 109.2 2_666 . ?
C43 C44 H44B 109.2 . . ?
C46 C44 H44B 109.2 2_666 . ?
H44A C44 H44B 107.9 . . ?
N3 C24 C16 123.4(9) . . ?
N3 C24 C23 116.1(8) . . ?
C16 C24 C23 120.5(9) . . ?
C6 C7 C8 124.2(9) . . ?
C6 C7 C11 119.8(9) . . ?
C8 C7 C11 115.9(8) . . ?
C3 C4 C12 116.1(9) . . ?
C3 C4 C5 126.7(9) . . ?
C12 C4 C5 117.2(9) . . ?
C42 C43 C44 112.5(7) . . ?
C42 C43 H43A 109.1 . . ?
C44 C43 H43A 109.1 . . ?
C42 C43 H43B 109.1 . . ?
C44 C43 H43B 109.1 . . ?
H43A C43 H43B 107.8 . . ?
N4 C23 C19 123.7(9) . . ?
N4 C23 C24 117.1(8) . . ?
C19 C23 C24 119.2(9) . . ?
N1 C12 C4 123.7(8) . . ?
N1 C12 C11 115.8(7) . . ?
C4 C12 C11 120.5(8) . . ?
N4 C22 C21 120.9(10) . . ?
N4 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
N2 C10 C9 121.7(9) . . ?
N2 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C45 C46 C44 111.7(8) . 2_666 ?
C45 C46 H46A 109.3 . . ?
C44 C46 H46A 109.3 2_666 . ?
C45 C46 H46B 109.3 . . ?
C44 C46 H46B 109.3 2_666 . ?
H46A C46 H46B 107.9 . . ?
N3 C13 C14 122.1(10) . . ?
N3 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C10 C9 C8 120.1(9) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
N5 C36 C35 117.5(8) . . ?
N5 C36 C28 122.4(10) . . ?
C35 C36 C28 120.1(10) . . ?
N1 C1 C2 119.9(9) . . ?
N1 C1 H1 120.1 . . ?
C2 C1 H1 120.1 . . ?
C47 C48 C40 116.7(7) . 2_666 ?
C47 C48 H48A 108.1 . . ?
C40 C48 H48A 108.1 2_666 . ?
C47 C48 H48B 108.1 . . ?
C40 C48 H48B 108.1 2_666 . ?
H48A C48 H48B 107.3 . . ?
C48 C40 C39 111.9(8) 2_666 . ?
C48 C40 H40A 109.2 2_666 . ?
C39 C40 H40A 109.2 . . ?
C48 C40 H40B 109.2 2_666 . ?
C39 C40 H40B 109.2 . . ?
H40A C40 H40B 107.9 . . ?
C20 C19 C23 117.3(10) . . ?
C20 C19 C18 125.4(10) . . ?
C23 C19 C18 117.3(10) . . ?
N6 C35 C36 116.3(9) . . ?
N6 C35 C31 122.3(10) . . ?
C36 C35 C31 121.4(10) . . ?
C5 C6 C7 120.7(9) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C39 C38 C37 115.4(8) . . ?
C39 C38 H38A 108.4 . . ?
C37 C38 H38A 108.4 . . ?
C39 C38 H38B 108.4 . . ?
C37 C38 H38B 108.4 . . ?
H38A C38 H38B 107.5 . . ?
C9 C8 C7 119.9(8) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C14 C15 C16 121.8(9) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C21 C20 C19 118.6(10) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
C38 C39 C40 115.3(8) . . ?
C38 C39 H39A 108.4 . . ?
C40 C39 H39A 108.4 . . ?
C38 C39 H39B 108.4 . . ?
C40 C39 H39B 108.4 . . ?
H39A C39 H39B 107.5 . . ?
C15 C14 C13 119.8(10) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
O11 N8 O12 126.1(18) . . ?
O11 N8 O10 116(2) . . ?
O12 N8 O10 118.0(16) . . ?
N5 C25 C26 120.6(11) . . ?
N5 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C32 C33 C34 121.0(11) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C17 C16 C24 118.4(10) . . ?
C17 C16 C15 126.9(10) . . ?
C24 C16 C15 114.7(9) . . ?
C2 C3 C4 121.9(9) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C17 C18 C19 122.3(10) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C3 C2 C1 120.3(9) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C35 C31 C32 117.2(11) . . ?
C35 C31 C30 117.1(12) . . ?
C32 C31 C30 125.6(12) . . ?
N6 C34 C33 121.1(11) . . ?
N6 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C18 C17 C16 122.3(10) . . ?
C18 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
C27 C28 C29 126.2(12) . . ?
C27 C28 C36 116.7(12) . . ?
C29 C28 C36 117.1(12) . . ?
C6 C5 C4 121.8(9) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C30 C29 C28 122.6(12) . . ?
C30 C29 H29 118.7 . . ?
C28 C29 H29 118.7 . . ?
C29 C30 C31 121.6(12) . . ?
C29 C30 H30 119.2 . . ?
C31 C30 H30 119.2 . . ?
C20 C21 C22 122.0(11) . . ?
C20 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
O15 N7 O13 117(2) . . ?
O15 N7 O14 133.3(18) . . ?
O13 N7 O14 109(2) . . ?
C27 C26 C25 121.6(11) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C33 C32 C31 119.4(11) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C28 C27 C26 119.6(11) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?

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
Cu2 O4 C41 O3 -166.7(6) . . . . ?
Cu1 O4 C41 O3 -1.9(6) . . . . ?
Cu2 O4 C41 C42 10.4(13) . . . . ?
Cu1 O4 C41 C42 175.1(7) . . . . ?
Cu1 O3 C41 O4 2.4(8) . . . . ?
Cu1 O3 C41 C42 -174.7(6) . . . . ?
Cu3 O8 C47 O7 6.3(13) . . . . ?
Cu3 O8 C47 C48 -174.5(6) . . . . ?
Cu2 O7 C47 O8 10.2(12) . . . . ?
Cu2 O7 C47 C48 -169.0(6) . . . . ?
C10 N2 C11 C7 -0.3(12) . . . . ?
Cu1 N2 C11 C7 179.1(6) . . . . ?
C10 N2 C11 C12 -179.5(7) . . . . ?
Cu1 N2 C11 C12 0.0(9) . . . . ?
O4 C41 C42 C43 167.8(8) . . . . ?
O3 C41 C42 C43 -15.2(12) . . . . ?
Cu1 O2 C37 O1 -11.1(9) . . . . ?
Cu1 O2 C37 C38 169.2(5) . . . . ?
Cu2 O5 C45 O6 25.6(13) . . . . ?
Cu2 O5 C45 C46 -156.0(6) . . . . ?
Cu3 O6 C45 O5 -0.9(12) . . . . ?
Cu3 O6 C45 C46 -179.3(5) . . . . ?
C13 N3 C24 C16 2.4(12) . . . . ?
Cu2 N3 C24 C16 -176.1(7) . . . . ?
C13 N3 C24 C23 -179.3(7) . . . . ?
Cu2 N3 C24 C23 2.1(9) . . . . ?
N2 C11 C7 C6 177.8(8) . . . . ?
C12 C11 C7 C6 -3.1(12) . . . . ?
N2 C11 C7 C8 0.3(12) . . . . ?
C12 C11 C7 C8 179.4(8) . . . . ?
C41 C42 C43 C44 169.5(8) . . . . ?
C46 C44 C43 C42 -177.7(8) 2_666 . . . ?
C22 N4 C23 C19 -1.6(12) . . . . ?
Cu2 N4 C23 C19 176.8(7) . . . . ?
C22 N4 C23 C24 177.3(7) . . . . ?
Cu2 N4 C23 C24 -4.3(9) . . . . ?
N3 C24 C23 N4 1.5(11) . . . . ?
C16 C24 C23 N4 179.8(8) . . . . ?
N3 C24 C23 C19 -179.6(7) . . . . ?
C16 C24 C23 C19 -1.3(12) . . . . ?
C1 N1 C12 C4 -1.1(12) . . . . ?
Cu1 N1 C12 C4 177.0(6) . . . . ?
C1 N1 C12 C11 -179.4(7) . . . . ?
Cu1 N1 C12 C11 -1.3(9) . . . . ?
C3 C4 C12 N1 1.3(13) . . . . ?
C5 C4 C12 N1 179.7(8) . . . . ?
C3 C4 C12 C11 179.6(8) . . . . ?
C5 C4 C12 C11 -2.1(12) . . . . ?
N2 C11 C12 N1 0.9(11) . . . . ?
C7 C11 C12 N1 -178.3(7) . . . . ?
N2 C11 C12 C4 -177.5(7) . . . . ?
C7 C11 C12 C4 3.4(12) . . . . ?
C23 N4 C22 C21 -1.2(12) . . . . ?
Cu2 N4 C22 C21 -179.2(7) . . . . ?
C11 N2 C10 C9 1.3(12) . . . . ?
Cu1 N2 C10 C9 -178.0(7) . . . . ?
O5 C45 C46 C44 46.5(11) . . . 2_666 ?
O6 C45 C46 C44 -134.9(8) . . . 2_666 ?
C24 N3 C13 C14 -1.0(13) . . . . ?
Cu2 N3 C13 C14 177.3(7) . . . . ?
N2 C10 C9 C8 -2.3(14) . . . . ?
C25 N5 C36 C35 179.6(8) . . . . ?
Cu3 N5 C36 C35 -0.8(10) . . . . ?
C25 N5 C36 C28 0.4(13) . . . . ?
Cu3 N5 C36 C28 -180.0(7) . . . . ?
C12 N1 C1 C2 1.5(13) . . . . ?
Cu1 N1 C1 C2 -176.3(7) . . . . ?
O8 C47 C48 C40 173.1(8) . . . 2_666 ?
O7 C47 C48 C40 -7.7(12) . . . 2_666 ?
N4 C23 C19 C20 2.3(13) . . . . ?
C24 C23 C19 C20 -176.6(8) . . . . ?
N4 C23 C19 C18 -179.0(8) . . . . ?
C24 C23 C19 C18 2.1(12) . . . . ?
C34 N6 C35 C36 -177.8(8) . . . . ?
Cu3 N6 C35 C36 0.4(10) . . . . ?
C34 N6 C35 C31 2.7(13) . . . . ?
Cu3 N6 C35 C31 -179.1(7) . . . . ?
N5 C36 C35 N6 0.3(12) . . . . ?
C28 C36 C35 N6 179.5(8) . . . . ?
N5 C36 C35 C31 179.8(8) . . . . ?
C28 C36 C35 C31 -1.0(14) . . . . ?
C8 C7 C6 C5 179.0(9) . . . . ?
C11 C7 C6 C5 1.8(14) . . . . ?
O1 C37 C38 C39 147.7(9) . . . . ?
O2 C37 C38 C39 -32.7(11) . . . . ?
C10 C9 C8 C7 2.3(15) . . . . ?
C6 C7 C8 C9 -178.6(9) . . . . ?
C11 C7 C8 C9 -1.3(13) . . . . ?
C23 C19 C20 C21 0.0(15) . . . . ?
C18 C19 C20 C21 -178.6(10) . . . . ?
C37 C38 C39 C40 -60.8(12) . . . . ?
C48 C40 C39 C38 -64.0(11) 2_666 . . . ?
C16 C15 C14 C13 1.7(15) . . . . ?
N3 C13 C14 C15 -1.0(15) . . . . ?
C36 N5 C25 C26 -0.5(14) . . . . ?
Cu3 N5 C25 C26 179.8(8) . . . . ?
N3 C24 C16 C17 177.3(8) . . . . ?
C23 C24 C16 C17 -0.9(13) . . . . ?
N3 C24 C16 C15 -1.7(13) . . . . ?
C23 C24 C16 C15 -179.9(8) . . . . ?
C14 C15 C16 C17 -179.3(10) . . . . ?
C14 C15 C16 C24 -0.4(14) . . . . ?
C12 C4 C3 C2 -2.1(15) . . . . ?
C5 C4 C3 C2 179.7(10) . . . . ?
C20 C19 C18 C17 177.7(10) . . . . ?
C23 C19 C18 C17 -0.9(15) . . . . ?
C4 C3 C2 C1 2.6(17) . . . . ?
N1 C1 C2 C3 -2.3(16) . . . . ?
N6 C35 C31 C32 -2.1(14) . . . . ?
C36 C35 C31 C32 178.5(9) . . . . ?
N6 C35 C31 C30 -179.8(8) . . . . ?
C36 C35 C31 C30 0.7(14) . . . . ?
C35 N6 C34 C33 -1.6(14) . . . . ?
Cu3 N6 C34 C33 -179.5(7) . . . . ?
C32 C33 C34 N6 -0.1(16) . . . . ?
C19 C18 C17 C16 -1.3(17) . . . . ?
C24 C16 C17 C18 2.2(15) . . . . ?
C15 C16 C17 C18 -178.9(10) . . . . ?
N5 C36 C28 C27 1.0(14) . . . . ?
C35 C36 C28 C27 -178.2(9) . . . . ?
N5 C36 C28 C29 -179.9(9) . . . . ?
C35 C36 C28 C29 1.0(14) . . . . ?
C7 C6 C5 C4 -0.6(15) . . . . ?
C3 C4 C5 C6 178.9(10) . . . . ?
C12 C4 C5 C6 0.8(14) . . . . ?
C27 C28 C29 C30 178.3(12) . . . . ?
C36 C28 C29 C30 -0.7(17) . . . . ?
C28 C29 C30 C31 0.5(18) . . . . ?
C35 C31 C30 C29 -0.5(16) . . . . ?
C32 C31 C30 C29 -178.0(11) . . . . ?
C19 C20 C21 C22 -2.7(16) . . . . ?
N4 C22 C21 C20 3.4(15) . . . . ?
N5 C25 C26 C27 -0.7(18) . . . . ?
C34 C33 C32 C31 0.7(16) . . . . ?
C35 C31 C32 C33 0.4(15) . . . . ?
C30 C31 C32 C33 177.9(10) . . . . ?
C29 C28 C27 C26 178.8(11) . . . . ?
C36 C28 C27 C26 -2.2(17) . . . . ?
C25 C26 C27 C28 2.1(19) . . . . ?

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
C10 H10 O3 0.93 2.58 3.078(11) 114.1 . yes
C10 H10 O10 0.93 2.48 3.291(17) 146.3 . yes
C13 H13 O5 0.93 2.61 3.078(11) 111.7 . yes
C13 H13 O15 0.93 2.43 3.272(18) 150.8 . yes
C48 H48B O11 0.97 2.55 3.40(2) 145.8 2_766 yes
C34 H34 O8 0.93 2.61 3.084(13) 112.2 . yes
C34 H34 O11 0.93 2.36 3.17(2) 146.0 2_766 yes
C10 H10 O3 0.93 2.58 3.078(11) 114.1 . yes
C10 H10 O10 0.93 2.48 3.291(17) 146.3 . yes
C13 H13 O5 0.93 2.61 3.078(11) 111.7 . yes
C13 H13 O15 0.93 2.43 3.272(18) 150.8 . yes
C48 H48B O11 0.97 2.55 3.40(2) 145.8 2_766 yes
C34 H34 O8 0.93 2.61 3.084(13) 112.2 . yes
C34 H34 O11 0.93 2.36 3.17(2) 146.0 2_766 yes

_refine_diff_density_max         0.955
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.115

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1973479'
loop_
_audit_author_name
_audit_author_address
'Dr Manjit K. Bhattacharyya'
;Cotton University
India
;
_audit_update_record             
;
2019-12-21 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H18 Co O9'
_chemical_formula_weight         293.13

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'
Co Co 0.3494 0.9721 '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'
H H 0.0000 0.0000 '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                   8.0383(7)
_cell_length_b                   15.1299(14)
_cell_length_c                   12.5637(11)
_cell_angle_alpha                90
_cell_angle_beta                 129.548(6)
_cell_angle_gamma                90
_cell_volume                     1178.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3035
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      24.46

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_F_000             612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    1.488
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13558
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.496
_diffrn_reflns_theta_max         26.538
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             2363
_reflns_number_gt                1727
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2363
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1674
_refine_ls_R_factor_gt           0.1461
_refine_ls_wR_factor_ref         0.4594
_refine_ls_wR_factor_gt          0.4470
_refine_ls_goodness_of_fit_ref   1.823
_refine_ls_restrained_S_all      1.823
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.004

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
Co1 Co 1.500000 0.000000 0.500000 0.0273(8) Uani 1 2 d S . P . .
Co2 Co 1.000000 0.000000 0.500000 0.0272(8) Uani 1 2 d S . P . .
O1 O 0.8911(10) 0.0467(5) 0.3108(7) 0.0404(18) Uani 1 1 d . . . . .
O2 O 0.5548(12) 0.0801(6) 0.2091(8) 0.050(2) Uani 1 1 d . . . . .
O3 O 0.1651(10) 0.1157(5) -0.4113(8) 0.0420(19) Uani 1 1 d . . . . .
O4 O -0.0298(11) 0.1764(5) -0.3573(8) 0.0451(19) Uani 1 1 d . . . . .
C5 C 0.3118(15) 0.2370(6) -0.2540(10) 0.039(2) Uani 1 1 d . . . . .
H5A H 0.261526 0.280493 -0.223461 0.046 Uiso 1 1 calc R U . . .
H5B H 0.351221 0.267657 -0.302885 0.046 Uiso 1 1 calc R U . . .
O8 O 1.2879(9) -0.0539(4) 0.5342(7) 0.0317(15) Uani 1 1 d . . . . .
O9 O 1.2243(11) 0.0362(6) 0.3113(8) 0.052(2) Uani 1 1 d . . . . .
O31 O 1.4960(11) 0.1183(5) 0.5853(8) 0.047(2) Uani 1 1 d . . . . .
C6 C 0.1338(15) 0.1713(6) -0.3495(10) 0.038(3) Uani 1 1 d . . . . .
C1 C 0.7123(14) 0.0762(6) 0.2098(10) 0.033(2) Uani 1 1 d . . . . .
C2 C 0.6931(16) 0.1078(7) 0.0896(10) 0.040(2) Uani 1 1 d . . . . .
H2A H 0.810811 0.148682 0.124639 0.048 Uiso 1 1 calc R U . . .
H2B H 0.716101 0.057269 0.052757 0.048 Uiso 1 1 calc R U . . .
C3 C 0.4903(15) 0.1517(7) -0.0277(12) 0.038(2) Uani 1 1 d . . . . .
H3A H 0.373254 0.109220 -0.073457 0.046 Uiso 1 1 calc R U . . .
H3B H 0.455732 0.198903 0.007711 0.046 Uiso 1 1 calc R U . . .
C4 C 0.5078(16) 0.1889(7) -0.1295(11) 0.041(3) Uani 1 1 d . . . . .
H4A H 0.542969 0.140888 -0.163317 0.049 Uiso 1 1 calc R U . . .
H4B H 0.628577 0.229674 -0.081195 0.049 Uiso 1 1 calc R U . . .
O32 O 0.1165(12) 0.0771(5) 0.0509(8) 0.052(2) Uani 1 1 d . . . . .
O37 O 0.8860(18) 0.2986(7) 0.3185(12) 0.079(3) Uani 1 1 d . . . . .
H31A H 1.340000 0.128339 0.517200 0.080 Uiso 1 1 d . U . . .
H9A H 1.248302 0.083100 0.343102 0.080 Uiso 1 1 d . U . . .
H37B H 0.983700 0.278900 0.293900 0.080 Uiso 1 1 d . U . . .
H37A H 0.919700 0.359900 0.301805 0.080 Uiso 1 1 d . U . . .
H32B H 0.236865 0.043000 0.062800 0.080 Uiso 1 1 d . U . . .
H32C H 0.075700 0.132600 0.022202 0.080 Uiso 1 1 d . U . . .
H31D H 1.602400 0.108809 0.641400 0.080 Uiso 1 1 d . U . . .
H9D H 1.181314 0.060400 0.213500 0.080 Uiso 1 1 d . U . . .
H8A H 1.182899 -0.077700 0.497800 0.080 Uiso 1 1 d . U . . .
H8B H 1.275490 0.003000 0.546700 0.080 Uiso 1 1 d . 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
Co1 O9 2.035(7) 3_856 ?
Co1 O9 2.035(7) . ?
Co1 O31 2.097(7) 3_856 ?
Co1 O31 2.097(7) . ?
Co1 O8 2.166(6) 3_856 ?
Co1 O8 2.166(6) . ?
Co2 O3 2.046(7) 3_655 ?
Co2 O3 2.046(7) 1_656 ?
Co2 O1 2.065(7) . ?
Co2 O1 2.065(7) 3_756 ?
Co2 O8 2.222(6) . ?
Co2 O8 2.222(6) 3_756 ?
Co2 H8A 1.89632(13) . ?
Co2 H8B 1.8962(2) . ?
O1 C1 1.246(11) . ?
O2 C1 1.261(13) . ?
O3 C6 1.274(13) . ?
O4 C6 1.257(13) . ?
C5 C6 1.513(13) . ?
C5 C4 1.523(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
O8 H8A 0.748(6) . ?
O8 H8B 0.892(6) . ?
O9 H9A 0.776(10) . ?
O9 H9D 1.106(8) . ?
O31 H31A 0.981(7) . ?
O31 H31D 0.693(7) . ?
C1 C2 1.496(15) . ?
C2 C3 1.487(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.484(15) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
O32 H32B 1.020(8) . ?
O32 H32C 0.890(8) . ?
O37 H37B 1.054(10) . ?
O37 H37A 1.025(10) . ?

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
O9 Co1 O9 180.0(5) 3_856 . ?
O9 Co1 O31 90.4(3) 3_856 3_856 ?
O9 Co1 O31 89.6(3) . 3_856 ?
O9 Co1 O31 89.6(3) 3_856 . ?
O9 Co1 O31 90.4(3) . . ?
O31 Co1 O31 180.0 3_856 . ?
O9 Co1 O8 85.5(3) 3_856 3_856 ?
O9 Co1 O8 94.5(3) . 3_856 ?
O31 Co1 O8 87.1(3) 3_856 3_856 ?
O31 Co1 O8 92.9(3) . 3_856 ?
O9 Co1 O8 94.5(3) 3_856 . ?
O9 Co1 O8 85.5(3) . . ?
O31 Co1 O8 92.9(3) 3_856 . ?
O31 Co1 O8 87.1(3) . . ?
O8 Co1 O8 180.0 3_856 . ?
O3 Co2 O3 180.0 3_655 1_656 ?
O3 Co2 O1 90.8(3) 3_655 . ?
O3 Co2 O1 89.2(3) 1_656 . ?
O3 Co2 O1 89.2(3) 3_655 3_756 ?
O3 Co2 O1 90.8(3) 1_656 3_756 ?
O1 Co2 O1 180.0 . 3_756 ?
O3 Co2 O8 91.5(2) 3_655 . ?
O3 Co2 O8 88.5(2) 1_656 . ?
O1 Co2 O8 88.5(2) . . ?
O1 Co2 O8 91.5(2) 3_756 . ?
O3 Co2 O8 88.5(2) 3_655 3_756 ?
O3 Co2 O8 91.5(2) 1_656 3_756 ?
O1 Co2 O8 91.5(2) . 3_756 ?
O1 Co2 O8 88.5(2) 3_756 3_756 ?
O8 Co2 O8 180.0 . 3_756 ?
O3 Co2 H8A 72.63(19) 3_655 . ?
O3 Co2 H8A 107.37(19) 1_656 . ?
O1 Co2 H8A 87.67(18) . . ?
O1 Co2 H8A 92.33(18) 3_756 . ?
O8 Co2 H8A 18.87(16) . . ?
O8 Co2 H8A 161.13(16) 3_756 . ?
O3 Co2 H8B 114.44(19) 3_655 . ?
O3 Co2 H8B 65.56(19) 1_656 . ?
O1 Co2 H8B 84.46(17) . . ?
O1 Co2 H8B 95.54(17) 3_756 . ?
O8 Co2 H8B 23.34(16) . . ?
O8 Co2 H8B 156.66(16) 3_756 . ?
H8A Co2 H8B 41.913(4) . . ?
C1 O1 Co2 131.5(6) . . ?
C6 O3 Co2 125.8(6) . 1_454 ?
C6 C5 C4 109.8(8) . . ?
C6 C5 H5A 109.7 . . ?
C4 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
C4 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
Co1 O8 Co2 132.7(3) . . ?
Co1 O8 H8A 141.6(7) . . ?
Co2 O8 H8A 55.1(4) . . ?
Co1 O8 H8B 82.0(4) . . ?
Co2 O8 H8B 57.4(3) . . ?
H8A O8 H8B 111.3(7) . . ?
Co1 O9 H9A 85.2(6) . . ?
Co1 O9 H9D 136.1(5) . . ?
H9A O9 H9D 93.9(8) . . ?
Co1 O31 H31A 96.5(5) . . ?
Co1 O31 H31D 86.2(6) . . ?
H31A O31 H31D 169.5(12) . . ?
O4 C6 O3 126.6(8) . . ?
O4 C6 C5 115.9(9) . . ?
O3 C6 C5 117.6(9) . . ?
O1 C1 O2 121.7(9) . . ?
O1 C1 C2 116.9(8) . . ?
O2 C1 C2 121.4(8) . . ?
C3 C2 C1 119.1(9) . . ?
C3 C2 H2A 107.6 . . ?
C1 C2 H2A 107.6 . . ?
C3 C2 H2B 107.5 . . ?
C1 C2 H2B 107.5 . . ?
H2A C2 H2B 107.0 . . ?
C4 C3 C2 112.2(8) . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 C5 117.5(9) . . ?
C3 C4 H4A 107.9 . . ?
C5 C4 H4A 107.9 . . ?
C3 C4 H4B 107.9 . . ?
C5 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
H32B O32 H32C 127.3(9) . . ?
H37B O37 H37A 81.5(7) . . ?

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
Co2 O3 C6 O4 -17.0(15) 1_454 . . . ?
Co2 O3 C6 C5 161.4(6) 1_454 . . . ?
C4 C5 C6 O4 111.4(10) . . . . ?
C4 C5 C6 O3 -67.2(13) . . . . ?
Co2 O1 C1 O2 -1.8(15) . . . . ?
Co2 O1 C1 C2 177.7(7) . . . . ?
O1 C1 C2 C3 -174.0(9) . . . . ?
O2 C1 C2 C3 5.4(15) . . . . ?
C1 C2 C3 C4 172.8(9) . . . . ?
C2 C3 C4 C5 -179.2(9) . . . . ?
C6 C5 C4 C3 -70.2(13) . . . . ?

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
O31 H31A O3 0.981(7) 2.104(8) 2.688(10) 116.4(5) 1_656 yes
O9 H9A O31 0.776(10) 2.407(8) 2.931(11) 125.9(6) . yes
O37 H37B O4 1.054(10) 1.953(8) 2.717(12) 126.7(6) 4_666 yes
O32 H32B O2 1.020(8) 2.060(7) 2.729(10) 121.0(5) . yes
O32 H32C O37 0.890(8) 2.233(12) 2.934(14) 135.3(6) 4_465 yes
O31 H31D O9 0.693(7) 2.460(9) 2.912(11) 124.9(6) 3_856 yes
O31 H31D O37 0.693(7) 2.377(12) 2.880(14) 131.1(7) 4_666 yes
O9 H9D O32 1.106(8) 1.775(8) 2.869(12) 168.7(6) 1_655 yes
O31 H31A O3 0.981(7) 2.104(8) 2.688(10) 116.4(5) 1_656 yes
O9 H9A O31 0.776(10) 2.407(8) 2.931(11) 125.9(6) . yes
O37 H37B O4 1.054(10) 1.953(8) 2.717(12) 126.7(6) 4_666 yes
O32 H32B O2 1.020(8) 2.060(7) 2.729(10) 121.0(5) . yes
O32 H32C O37 0.890(8) 2.233(12) 2.934(14) 135.3(6) 4_465 yes
O31 H31D O9 0.693(7) 2.460(9) 2.912(11) 124.9(6) 3_856 yes
O31 H31D O37 0.693(7) 2.377(12) 2.880(14) 131.1(7) 4_666 yes
O9 H9D O32 1.106(8) 1.775(8) 2.869(12) 168.7(6) 1_655 yes

_refine_diff_density_max         1.501
_refine_diff_density_min         -1.562
_refine_diff_density_rms         0.265

