# 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. 
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data_SH3880
_database_code_depnum_ccdc_archive 'CCDC 1835293'
loop_
_audit_author_name
_audit_author_address
'Carola Schulzke'
;Ernst-Moritz-Arndt-Universit?t Greifswald
Germany
;
_audit_update_record             
;
2018-04-06 deposited with the CCDC.	2020-01-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT220_shelx               
;
PROBLEM: Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 4.9 Ratio
RESPONSE: This is the structure of a compound plus five molecules of dmf
solvent comprising 146 non-hydrogen atoms with very different 
moieties like isopropyl groups and phenyl rings. it is not surprising
that the carbon atoms behave distinctly. 
;
_vrf_PLAT222_shelx               
;
PROBLEM: Non-Solvent Resd 1 H Uiso(max)/Uiso(min) Range 7.8 Ratio
RESPONSE: This is the structure of a cod plus five molecules of dmf
solvent comprising 146 non-hydrogen atoms with very different 
moieties like isopropyl groups and phenyl rings. it is not surprising
that the carbon atoms behave distinctly as do the hydrogen atoms
calculated into idealised postions with Ueq depending on the parent atom.
;
_vrf_PLAT241_shelx               
;
PROBLEM: High ?MainMol? Ueq as Compared to Neighbors of O24 Check
RESPONSE: This is the oxygen atom of one dmf solvent molecule pointing 
directly towards the complex potentially involved in a hydrogen bond
with the apical OH of that compIn vicinity of the complex with low Ueq
that of the solvent appears to be high.
;
_vrf_PLAT242_shelx               
;
PROBLEM: Low ?MainMol? Ueq as Compared to Neighbors of C8 Check
RESPONSE: This is the methine C atom of an isopropyl moiety with methyl 
groups of much higher flexibility.
;
_vrf_PLAT309_shelx               
;
PROBLEM: Single Bonded Oxygen (C-O > 1.3 Ang) ........... O25 Check
RESPONSE: This is the oxygen atom of a dmf solvent molecule. It should be 
in a double bond. A tautomeric ol-form can neither be excluded nor 
modeled sufficiently well.
;
_vrf_PLAT341_shelx               
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.00723 Ang.
RESPONSE: ...
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 274 Report
RESPONSE: ...
;
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Residual Density 0.09A From N17 1.81 eA-3
RESPONSE: An overlooked atom site or wring assignment can be excluded.
This is undoubtedly the nitrogen of a dmf solvent molecule.
;
_vrf_PLAT975_shelx               
;
PROBLEM: Check Calcd Residual Density 0.90A From O2 0.74 eA-3
RESPONSE: This residual density is due to a slight disorder of the
respective Cu-O-Cu moiety, the modeling of which did not improve
the refinement at all. The presence of a hydrogen can be excluded.
;
_vrf_PLAT978_shelx               
;
PROBLEM: Number C-C Bonds with Positive Residual Density. 0 Info
RESPONSE: ...
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C75 H111 Cu9 N15 O23 P4, 4 (C3 H7 N O)'
_chemical_formula_sum            'C87 H139 Cu9 N19 O27 P4'
_chemical_formula_weight         2578.90

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'
P P 0.1023 0.0942 '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                   11.159(3)
_cell_length_b                   22.849(6)
_cell_length_c                   23.684(7)
_cell_angle_alpha                111.619(11)
_cell_angle_beta                 97.083(12)
_cell_angle_gamma                91.352(13)
_cell_volume                     5555(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    152(2)
_cell_measurement_reflns_used    9896
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      29.73

_exptl_crystal_description       platelet
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_F_000             2662
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.672
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.822
_shelx_estimated_absorpt_T_min   0.374
_shelx_estimated_absorpt_T_max   0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6215
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      152(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            76022
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.572
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             21551
_reflns_number_gt                17169
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'

_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)+(0.0534P)²+12.8551P] 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         21551
_refine_ls_number_parameters     1261
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.1216
_refine_ls_wR_factor_gt          0.1105
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_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 0.47246(4) 0.30328(2) 0.72985(2) 0.02246(11) Uani 1 1 d . . . . .
Cu2 Cu 0.48479(4) 0.32924(2) 0.59938(2) 0.02276(11) Uani 1 1 d . . . . .
Cu3 Cu 0.54446(4) 0.44941(2) 0.73683(2) 0.02274(11) Uani 1 1 d . . . . .
Cu4 Cu 0.63191(5) 0.11924(2) 0.65595(2) 0.02636(11) Uani 1 1 d . . . . .
Cu5 Cu 0.68052(4) 0.21694(2) 0.58299(2) 0.02369(11) Uani 1 1 d . . . . .
Cu6 Cu 0.76676(4) 0.41259(2) 0.52551(2) 0.02424(11) Uani 1 1 d . . . . .
Cu7 Cu 0.80418(4) 0.46762(2) 0.67724(2) 0.02255(11) Uani 1 1 d . . . . .
Cu8 Cu 0.81274(4) 0.49732(2) 0.90790(2) 0.02552(11) Uani 1 1 d . . . . .
Cu9 Cu 0.74680(4) 0.34273(2) 0.83041(2) 0.02161(10) Uani 1 1 d . . . . .
P1 P 0.59529(9) 0.21188(4) 0.79124(4) 0.0227(2) Uani 1 1 d . . . . .
P2 P 0.62161(9) 0.27580(4) 0.48328(4) 0.0223(2) Uani 1 1 d . . . . .
P3 P 0.74792(10) 0.55985(4) 0.80640(4) 0.0254(2) Uani 1 1 d . . . . .
P4 P 0.76863(9) 0.34109(4) 0.69608(4) 0.01977(19) Uani 1 1 d . . . . .
O1 O 0.4630(2) 0.36449(11) 0.68862(11) 0.0216(5) Uani 1 1 d . . . . .
H1O H 0.392(4) 0.369(2) 0.682(2) 0.026 Uiso 1 1 d . U . . .
O2 O 0.6658(3) 0.19736(12) 0.65284(13) 0.0329(7) Uani 1 1 d D . . . .
H2O H 0.688(4) 0.2270(14) 0.6853(11) 0.039 Uiso 1 1 d D U . . .
O3 O 0.7920(3) 0.40020(12) 0.59976(12) 0.0282(6) Uani 1 1 d D . . . .
H3O H 0.753(4) 0.3696(15) 0.599(2) 0.034 Uiso 1 1 d D U . . .
O4 O 0.8021(3) 0.42429(12) 0.83781(12) 0.0283(6) Uani 1 1 d D . . . .
H4O H 0.788(4) 0.4324(19) 0.8068(11) 0.034 Uiso 1 1 d D U . . .
O5 O 0.4912(2) 0.24267(12) 0.76918(12) 0.0269(6) Uani 1 1 d . . . . .
O6 O 0.7061(2) 0.25668(12) 0.82237(12) 0.0276(6) Uani 1 1 d . . . . .
O7 O 0.5476(3) 0.19477(12) 0.84583(12) 0.0278(6) Uani 1 1 d . . . . .
O8 O 0.6218(3) 0.14984(12) 0.74352(12) 0.0288(6) Uani 1 1 d . . . . .
O9 O 0.6000(3) 0.03266(13) 0.64912(14) 0.0408(8) Uani 1 1 d . . . . .
O10 O 0.6976(2) 0.23666(12) 0.51125(12) 0.0270(6) Uani 1 1 d . . . . .
O11 O 0.5713(3) 0.22633(12) 0.41476(12) 0.0280(6) Uani 1 1 d . . . . .
O12 O 0.5092(2) 0.29601(12) 0.51310(12) 0.0262(6) Uani 1 1 d . . . . .
O13 O 0.6939(3) 0.32809(12) 0.47500(12) 0.0268(6) Uani 1 1 d . . . . .
O14 O 0.7503(3) 0.43745(13) 0.45527(13) 0.0370(7) Uani 1 1 d . . . . .
O15 O 0.8260(3) 0.53788(12) 0.75572(12) 0.0303(6) Uani 1 1 d . . . . .
O16 O 0.7371(3) 0.63414(12) 0.82025(12) 0.0321(7) Uani 1 1 d . . . . .
O17 O 0.8064(3) 0.55591(12) 0.86612(12) 0.0312(6) Uani 1 1 d . . . . .
O18 O 0.6183(3) 0.53283(12) 0.78654(13) 0.0296(6) Uani 1 1 d . . . . .
O19 O 0.8586(3) 0.56735(13) 0.98695(13) 0.0377(7) Uani 1 1 d . . . . .
O20 O 0.7502(2) 0.41138(11) 0.71723(11) 0.0222(5) Uani 1 1 d . . . . .
O21 O 0.7371(3) 0.31301(12) 0.74152(12) 0.0285(6) Uani 1 1 d . . . . .
O22 O 0.6973(2) 0.30687(11) 0.63270(11) 0.0232(5) Uani 1 1 d . . . . .
O23 O 0.9064(2) 0.33226(13) 0.68528(13) 0.0313(6) Uani 1 1 d . . . . .
N1 N 0.4163(3) 0.23815(14) 0.65002(15) 0.0258(7) Uani 1 1 d . . . . .
N2 N 0.4301(3) 0.24671(14) 0.59682(14) 0.0240(7) Uani 1 1 d . . . . .
N3 N 0.5115(3) 0.41518(14) 0.60493(14) 0.0249(7) Uani 1 1 d . . . . .
N4 N 0.5400(3) 0.46419(14) 0.65996(15) 0.0249(7) Uani 1 1 d . . . . .
N5 N 0.5135(3) 0.43443(14) 0.81012(14) 0.0255(7) Uani 1 1 d . . . . .
N6 N 0.5002(3) 0.37454(14) 0.80890(14) 0.0234(7) Uani 1 1 d . . . . .
N7 N 0.5979(4) -0.04741(16) 0.68175(18) 0.0403(9) Uani 1 1 d . . . . .
N8 N 0.6545(3) 0.08644(15) 0.56813(15) 0.0293(7) Uani 1 1 d . . . . .
N9 N 0.6780(3) 0.12667(14) 0.53987(14) 0.0267(7) Uani 1 1 d . . . . .
N10 N 0.7242(3) 0.43045(16) 0.35791(16) 0.0334(8) Uani 1 1 d . . . . .
N11 N 0.8533(3) 0.49581(14) 0.57293(14) 0.0256(7) Uani 1 1 d . . . . .
N12 N 0.8672(3) 0.51810(14) 0.63519(14) 0.0262(7) Uani 1 1 d . . . . .
N13 N 0.9422(4) 0.66367(16) 1.04593(17) 0.0378(9) Uani 1 1 d . . . . .
N14 N 0.7942(3) 0.44009(15) 0.95129(15) 0.0303(8) Uani 1 1 d . . . . .
N15 N 0.7631(3) 0.37737(15) 0.91962(14) 0.0264(7) Uani 1 1 d . . . . .
C1 C 0.7710(4) 0.68658(17) 0.87392(19) 0.0326(10) Uani 1 1 d . . . . .
C2 C 0.6985(4) 0.7030(2) 0.9202(2) 0.0386(11) Uani 1 1 d . . . . .
C3 C 0.7279(5) 0.7606(2) 0.9689(2) 0.0497(13) Uani 1 1 d . . . . .
H3A H 0.680283 0.772919 1.001385 0.060 Uiso 1 1 calc R U . . .
C4 C 0.8246(6) 0.7998(2) 0.9708(2) 0.0544(14) Uani 1 1 d . . . . .
H4A H 0.841663 0.839435 1.003837 0.065 Uiso 1 1 calc R U . . .
C5 C 0.8963(5) 0.7822(2) 0.9256(2) 0.0523(14) Uani 1 1 d . . . . .
H5 H 0.964053 0.809403 0.928158 0.063 Uiso 1 1 calc R U . . .
C6 C 0.8719(5) 0.7243(2) 0.8752(2) 0.0415(11) Uani 1 1 d . . . . .
C7 C 0.5667(6) 0.6617(4) 0.9798(3) 0.080(2) Uani 1 1 d . . . . .
H7A H 0.641212 0.652995 1.000945 0.121 Uiso 1 1 calc R U . . .
H7B H 0.502460 0.629150 0.974041 0.121 Uiso 1 1 calc R U . . .
H7C H 0.541911 0.703157 1.004425 0.121 Uiso 1 1 calc R U . . .
C8 C 0.5891(5) 0.6612(2) 0.9177(2) 0.0466(12) Uani 1 1 d . . . . .
H8 H 0.606211 0.616981 0.892958 0.056 Uiso 1 1 calc R U . . .
C9 C 0.4782(6) 0.6754(4) 0.8836(4) 0.098(3) Uani 1 1 d . . . . .
H9A H 0.455573 0.717813 0.907035 0.146 Uiso 1 1 calc R U . . .
H9B H 0.411408 0.644334 0.878143 0.146 Uiso 1 1 calc R U . . .
H9C H 0.495257 0.673390 0.843314 0.146 Uiso 1 1 calc R U . . .
C10 C 1.0510(7) 0.6675(3) 0.8439(4) 0.087(2) Uani 1 1 d . . . . .
H10A H 1.107383 0.696345 0.878587 0.130 Uiso 1 1 calc R U . . .
H10B H 1.094730 0.647611 0.808962 0.130 Uiso 1 1 calc R U . . .
H10C H 1.015132 0.634832 0.855593 0.130 Uiso 1 1 calc R U . . .
C11 C 0.9537(5) 0.7033(2) 0.8263(2) 0.0570(15) Uani 1 1 d . . . . .
H11 H 0.903214 0.672971 0.788476 0.068 Uiso 1 1 calc R U . . .
C12 C 1.0058(7) 0.7550(4) 0.8088(4) 0.091(2) Uani 1 1 d . . . . .
H12A H 0.941721 0.782020 0.803646 0.136 Uiso 1 1 calc R U . . .
H12B H 1.039032 0.736082 0.770216 0.136 Uiso 1 1 calc R U . . .
H12C H 1.070231 0.780469 0.841240 0.136 Uiso 1 1 calc R U . . .
C13 C 0.5054(4) 0.47418(19) 0.86698(19) 0.0332(9) Uani 1 1 d . . . . .
H13 H 0.512408 0.518913 0.880354 0.040 Uiso 1 1 calc R U . . .
C14 C 0.4853(4) 0.4407(2) 0.90376(19) 0.0354(10) Uani 1 1 d . . . . .
H14 H 0.474915 0.456911 0.945843 0.043 Uiso 1 1 calc R U . . .
C15 C 0.4840(4) 0.37851(19) 0.86525(18) 0.0287(9) Uani 1 1 d . . . . .
H15 H 0.473116 0.343391 0.876935 0.034 Uiso 1 1 calc R U . . .
C16 C 0.3716(4) 0.17880(18) 0.63468(19) 0.0318(9) Uani 1 1 d . . . . .
H16 H 0.353719 0.160317 0.662925 0.038 Uiso 1 1 calc R U . . .
C17 C 0.3551(4) 0.14830(19) 0.5718(2) 0.0349(10) Uani 1 1 d . . . . .
H17 H 0.324308 0.105936 0.548608 0.042 Uiso 1 1 calc R U . . .
C18 C 0.3933(4) 0.19296(18) 0.54973(19) 0.0306(9) Uani 1 1 d . . . . .
H18 H 0.393233 0.186283 0.507693 0.037 Uiso 1 1 calc R U . . .
C19 C 0.5126(4) 0.43771(18) 0.56010(19) 0.0289(9) Uani 1 1 d . . . . .
H19 H 0.494369 0.413306 0.517422 0.035 Uiso 1 1 calc R U . . .
C20 C 0.5441(4) 0.50153(19) 0.5854(2) 0.0343(10) Uani 1 1 d . . . . .
H20 H 0.552212 0.529405 0.564399 0.041 Uiso 1 1 calc R U . . .
C21 C 0.5613(4) 0.51630(18) 0.6482(2) 0.0310(9) Uani 1 1 d . . . . .
H21 H 0.584676 0.557180 0.678433 0.037 Uiso 1 1 calc R U . . .
C22 C 0.9254(4) 0.57541(18) 0.65658(19) 0.0303(9) Uani 1 1 d . . . . .
H22 H 0.945412 0.601565 0.698731 0.036 Uiso 1 1 calc R U . . .
C23 C 0.9522(4) 0.59088(19) 0.6083(2) 0.0332(10) Uani 1 1 d . . . . .
H23 H 0.994419 0.628331 0.610231 0.040 Uiso 1 1 calc R U . . .
C24 C 0.9042(4) 0.53997(18) 0.55643(19) 0.0296(9) Uani 1 1 d . . . . .
H24 H 0.906635 0.536600 0.515397 0.036 Uiso 1 1 calc R U . . .
C25 C 0.5735(4) 0.23178(18) 0.35833(18) 0.0290(9) Uani 1 1 d . . . . .
C26 C 0.6736(4) 0.2116(2) 0.3279(2) 0.0384(10) Uani 1 1 d . . . . .
C27 C 0.6688(6) 0.2120(3) 0.2686(2) 0.0551(14) Uani 1 1 d . . . . .
H27 H 0.735179 0.198320 0.246655 0.066 Uiso 1 1 calc R U . . .
C28 C 0.5713(6) 0.2316(3) 0.2417(2) 0.0642(17) Uani 1 1 d . . . . .
H28 H 0.570820 0.231937 0.201641 0.077 Uiso 1 1 calc R U . . .
C29 C 0.4737(6) 0.2508(3) 0.2721(2) 0.0564(15) Uani 1 1 d . . . . .
H29 H 0.406285 0.264340 0.252676 0.068 Uiso 1 1 calc R U . . .
C30 C 0.4711(4) 0.2509(2) 0.3318(2) 0.0387(11) Uani 1 1 d . . . . .
C31 C 0.7663(6) 0.1152(2) 0.3307(3) 0.0598(15) Uani 1 1 d . . . . .
H31A H 0.691523 0.100930 0.341088 0.090 Uiso 1 1 calc R U . . .
H31B H 0.835830 0.099596 0.349014 0.090 Uiso 1 1 calc R U . . .
H31C H 0.763473 0.098940 0.286062 0.090 Uiso 1 1 calc R U . . .
C32 C 0.7791(4) 0.1871(2) 0.3557(2) 0.0441(11) Uani 1 1 d . . . . .
H32 H 0.777273 0.202456 0.400969 0.053 Uiso 1 1 calc R U . . .
C33 C 0.9018(6) 0.2114(3) 0.3456(4) 0.0759(19) Uani 1 1 d . . . . .
H33A H 0.906735 0.196221 0.301529 0.114 Uiso 1 1 calc R U . . .
H33B H 0.967876 0.195817 0.366150 0.114 Uiso 1 1 calc R U . . .
H33C H 0.908592 0.257698 0.362631 0.114 Uiso 1 1 calc R U . . .
C34 C 0.2428(6) 0.2432(3) 0.3263(3) 0.0756(19) Uani 1 1 d . . . . .
H34A H 0.230789 0.255535 0.290683 0.113 Uiso 1 1 calc R U . . .
H34B H 0.177581 0.257918 0.351164 0.113 Uiso 1 1 calc R U . . .
H34C H 0.242029 0.197098 0.312399 0.113 Uiso 1 1 calc R U . . .
C35 C 0.3642(4) 0.2727(2) 0.3649(2) 0.0437(11) Uani 1 1 d . . . . .
H35 H 0.372848 0.260304 0.401400 0.052 Uiso 1 1 calc R U . . .
C36 C 0.3663(6) 0.3443(2) 0.3881(3) 0.0616(15) Uani 1 1 d . . . . .
H36A H 0.446262 0.362611 0.410942 0.092 Uiso 1 1 calc R U . . .
H36B H 0.304482 0.358731 0.415252 0.092 Uiso 1 1 calc R U . . .
H36C H 0.349427 0.357609 0.353276 0.092 Uiso 1 1 calc R U . . .
C37 C 0.6901(4) 0.0929(2) 0.48152(19) 0.0376(10) Uani 1 1 d . . . . .
H37 H 0.707179 0.110014 0.452125 0.045 Uiso 1 1 calc R U . . .
C38 C 0.6741(6) 0.0300(2) 0.4708(2) 0.0535(14) Uani 1 1 d . . . . .
H38 H 0.677680 -0.004706 0.433517 0.064 Uiso 1 1 calc R U . . .
C39 C 0.6516(5) 0.02801(19) 0.5263(2) 0.0448(12) Uani 1 1 d . . . . .
H39 H 0.636226 -0.009510 0.533532 0.054 Uiso 1 1 calc R U . . .
C40 C 0.5294(4) 0.13525(18) 0.84788(18) 0.0278(9) Uani 1 1 d . . . . .
C41 C 0.4165(4) 0.1026(2) 0.8253(2) 0.0326(9) Uani 1 1 d . . . . .
C42 C 0.3970(4) 0.0463(2) 0.8341(2) 0.0434(11) Uani 1 1 d . . . . .
H42 H 0.320787 0.022849 0.818694 0.052 Uiso 1 1 calc R U . . .
C43 C 0.4864(5) 0.0241(2) 0.8648(2) 0.0472(12) Uani 1 1 d . . . . .
H43 H 0.470847 -0.013740 0.871393 0.057 Uiso 1 1 calc R U . . .
C44 C 0.5974(5) 0.0566(2) 0.8858(2) 0.0442(12) Uani 1 1 d . . . . .
H44 H 0.658941 0.040417 0.906176 0.053 Uiso 1 1 calc R U . . .
C45 C 0.6226(4) 0.1131(2) 0.8781(2) 0.0373(10) Uani 1 1 d . . . . .
C46 C 0.2647(6) 0.0789(3) 0.7311(3) 0.0635(16) Uani 1 1 d . . . . .
H46A H 0.330929 0.064201 0.706961 0.095 Uiso 1 1 calc R U . . .
H46B H 0.206503 0.097913 0.709705 0.095 Uiso 1 1 calc R U . . .
H46C H 0.223946 0.043127 0.736244 0.095 Uiso 1 1 calc R U . . .
C47 C 0.3150(4) 0.1274(2) 0.7932(2) 0.0383(10) Uani 1 1 d . . . . .
H47 H 0.349262 0.165089 0.786960 0.046 Uiso 1 1 calc R U . . .
C48 C 0.2161(6) 0.1487(4) 0.8338(3) 0.084(2) Uani 1 1 d . . . . .
H48A H 0.188160 0.113880 0.844783 0.127 Uiso 1 1 calc R U . . .
H48B H 0.148050 0.161324 0.811523 0.127 Uiso 1 1 calc R U . . .
H48C H 0.248470 0.184691 0.871155 0.127 Uiso 1 1 calc R U . . .
C49 C 0.8380(7) 0.1120(4) 0.8623(5) 0.124(4) Uani 1 1 d . U . . .
H49A H 0.847775 0.071780 0.867665 0.186 Uiso 1 1 calc R U . . .
H49B H 0.916049 0.136939 0.874524 0.186 Uiso 1 1 calc R U . . .
H49C H 0.809056 0.103833 0.819070 0.186 Uiso 1 1 calc R U . . .
C50 C 0.7460(5) 0.1485(3) 0.9021(3) 0.0555(14) Uani 1 1 d . U . . .
H50 H 0.741072 0.190033 0.897088 0.067 Uiso 1 1 calc R U . . .
C51 C 0.7798(8) 0.1619(5) 0.9688(4) 0.136(4) Uani 1 1 d . U . . .
H51A H 0.724596 0.190975 0.992137 0.204 Uiso 1 1 calc R U . . .
H51B H 0.863043 0.181009 0.982174 0.204 Uiso 1 1 calc R U . . .
H51C H 0.774021 0.122328 0.975926 0.204 Uiso 1 1 calc R U . . .
C52 C 0.7392(4) 0.3523(2) 0.96008(19) 0.0329(9) Uani 1 1 d . . . . .
H52 H 0.714179 0.309180 0.949935 0.040 Uiso 1 1 calc R U . . .
C53 C 0.7559(5) 0.3975(2) 1.0186(2) 0.0437(12) Uani 1 1 d . . . . .
H53 H 0.746062 0.392265 1.055751 0.052 Uiso 1 1 calc R U . . .
C54 C 0.7902(5) 0.4522(2) 1.01093(19) 0.0412(11) Uani 1 1 d . . . . .
H54 H 0.808274 0.492373 1.043070 0.049 Uiso 1 1 calc R U . . .
C55 C 1.0075(4) 0.3214(2) 0.72001(19) 0.0316(9) Uani 1 1 d . . . . .
C56 C 1.0356(4) 0.2588(2) 0.7076(2) 0.0344(10) Uani 1 1 d . . . . .
C57 C 1.1474(4) 0.2510(2) 0.7374(2) 0.0383(10) Uani 1 1 d . . . . .
H57 H 1.169680 0.209326 0.730677 0.046 Uiso 1 1 calc R U . . .
C58 C 1.2252(4) 0.3003(2) 0.7754(2) 0.0350(10) Uani 1 1 d . . . . .
H58 H 1.301016 0.292885 0.793742 0.042 Uiso 1 1 calc R U . . .
C59 C 1.1930(4) 0.3616(2) 0.7873(2) 0.0361(10) Uani 1 1 d . . . . .
H59 H 1.246730 0.395995 0.814589 0.043 Uiso 1 1 calc R U . . .
C60 C 1.0838(4) 0.3739(2) 0.76000(19) 0.0304(9) Uani 1 1 d . . . . .
C61 C 1.0168(6) 0.1676(3) 0.6077(3) 0.085(2) Uani 1 1 d . . . . .
H61A H 1.031341 0.195544 0.585927 0.128 Uiso 1 1 calc R U . . .
H61B H 0.963165 0.130872 0.580474 0.128 Uiso 1 1 calc R U . . .
H61C H 1.094009 0.153419 0.620575 0.128 Uiso 1 1 calc R U . . .
C62 C 0.9567(4) 0.2037(2) 0.6649(3) 0.0471(12) Uani 1 1 d . . . . .
H62 H 0.880153 0.219357 0.650845 0.057 Uiso 1 1 calc R U . . .
C63 C 0.9237(5) 0.1597(3) 0.6970(3) 0.0700(19) Uani 1 1 d . . . . .
H63A H 0.997365 0.143207 0.710629 0.105 Uiso 1 1 calc R U . . .
H63B H 0.868142 0.124550 0.668442 0.105 Uiso 1 1 calc R U . . .
H63C H 0.884425 0.183212 0.732662 0.105 Uiso 1 1 calc R U . . .
C64 C 1.1049(5) 0.4668(3) 0.7293(3) 0.0534(13) Uani 1 1 d . . . . .
H64A H 1.193169 0.465306 0.734949 0.080 Uiso 1 1 calc R U . . .
H64B H 1.084593 0.510511 0.738627 0.080 Uiso 1 1 calc R U . . .
H64C H 1.071859 0.441007 0.686723 0.080 Uiso 1 1 calc R U . . .
C65 C 1.0511(4) 0.4411(2) 0.7721(2) 0.0337(9) Uani 1 1 d . . . . .
H65 H 0.960966 0.440374 0.763364 0.040 Uiso 1 1 calc R U . . .
C66 C 1.0897(5) 0.4845(2) 0.8377(2) 0.0480(12) Uani 1 1 d . . . . .
H66A H 1.064128 0.464774 0.865094 0.072 Uiso 1 1 calc R U . . .
H66B H 1.052161 0.524539 0.845435 0.072 Uiso 1 1 calc R U . . .
H66C H 1.178056 0.492393 0.845304 0.072 Uiso 1 1 calc R U . . .
C67 C 0.7228(4) 0.40515(19) 0.39931(19) 0.0311(9) Uani 1 1 d . . . . .
H67 H 0.700424 0.361335 0.386540 0.037 Uiso 1 1 calc R U . . .
C68 C 0.7588(5) 0.4973(2) 0.3767(2) 0.0421(11) Uani 1 1 d . . . . .
H68A H 0.739446 0.519921 0.418138 0.063 Uiso 1 1 calc R U . . .
H68B H 0.714310 0.513739 0.348096 0.063 Uiso 1 1 calc R U . . .
H68C H 0.846002 0.503339 0.376581 0.063 Uiso 1 1 calc R U . . .
C69 C 0.6962(6) 0.3938(3) 0.2925(2) 0.0611(16) Uani 1 1 d . . . . .
H69A H 0.768748 0.393750 0.272936 0.092 Uiso 1 1 calc R U . . .
H69B H 0.631668 0.412663 0.274468 0.092 Uiso 1 1 calc R U . . .
H69C H 0.669431 0.350354 0.285877 0.092 Uiso 1 1 calc R U . . .
C70 C 0.6037(4) 0.01258(19) 0.6912(2) 0.0368(10) Uani 1 1 d . . . . .
H70 H 0.611108 0.042234 0.732217 0.044 Uiso 1 1 calc R U . . .
C71 C 0.5909(6) -0.0945(2) 0.6199(2) 0.0566(15) Uani 1 1 d . . . . .
H71A H 0.527874 -0.127772 0.613634 0.085 Uiso 1 1 calc R U . . .
H71B H 0.669045 -0.112885 0.614364 0.085 Uiso 1 1 calc R U . . .
H71C H 0.570880 -0.074481 0.590119 0.085 Uiso 1 1 calc R U . . .
C72 C 0.6092(6) -0.0700(3) 0.7323(3) 0.0645(17) Uani 1 1 d . . . . .
H72A H 0.686561 -0.089029 0.734415 0.097 Uiso 1 1 calc R U . . .
H72B H 0.542493 -0.101638 0.725402 0.097 Uiso 1 1 calc R U . . .
H72C H 0.605985 -0.034481 0.770970 0.097 Uiso 1 1 calc R U . . .
C73 C 0.9113(4) 0.6182(2) 0.9926(2) 0.0357(10) Uani 1 1 d . . . . .
H73 H 0.929619 0.624066 0.956809 0.043 Uiso 1 1 calc R U . . .
C74 C 1.0022(5) 0.7233(2) 1.0517(3) 0.0506(13) Uani 1 1 d . . . . .
H74A H 1.018533 0.721106 1.011292 0.076 Uiso 1 1 calc R U . . .
H74B H 1.078686 0.731471 1.079526 0.076 Uiso 1 1 calc R U . . .
H74C H 0.949692 0.757548 1.068249 0.076 Uiso 1 1 calc R U . . .
C75 C 0.9155(6) 0.6566(3) 1.1013(2) 0.0673(18) Uani 1 1 d . . . . .
H75A H 0.839813 0.630156 1.092284 0.101 Uiso 1 1 calc R U . . .
H75B H 0.906810 0.698246 1.132272 0.101 Uiso 1 1 calc R U . . .
H75C H 0.981594 0.636670 1.116812 0.101 Uiso 1 1 calc R U . . .
O24 O 0.2537(3) 0.35727(19) 0.61762(18) 0.0592(6) Uani 1 1 d . . . . .
N16 N 0.1025(4) 0.3102(2) 0.5397(2) 0.0592(6) Uani 1 1 d . . . . .
C76 C 0.1505(5) 0.3334(3) 0.5969(3) 0.0592(6) Uani 1 1 d . . . . .
H76 H 0.100062 0.331725 0.625881 0.071 Uiso 1 1 calc R U . . .
C77 C 0.1796(5) 0.3074(3) 0.4921(3) 0.0592(6) Uani 1 1 d . . . . .
H77A H 0.147366 0.333314 0.469489 0.089 Uiso 1 1 calc R U . . .
H77B H 0.179600 0.263600 0.463560 0.089 Uiso 1 1 calc R U . . .
H77C H 0.262520 0.323544 0.511690 0.089 Uiso 1 1 calc R U . . .
C78 C -0.0224(5) 0.2853(3) 0.5207(3) 0.0592(6) Uani 1 1 d . . . . .
H78A H -0.057455 0.284013 0.556235 0.089 Uiso 1 1 calc R U . . .
H78B H -0.026480 0.242583 0.489504 0.089 Uiso 1 1 calc R U . . .
H78C H -0.067942 0.312549 0.503574 0.089 Uiso 1 1 calc R U . . .
O25 O 1.1157(6) 0.0658(3) 0.3166(3) 0.1283(13) Uani 1 1 d . . . . .
N17 N 1.0646(8) 0.0542(5) 0.4008(4) 0.1283(13) Uani 1 1 d . . . . .
C79 C 1.0781(10) 0.0262(6) 0.3417(5) 0.1283(13) Uani 1 1 d . . . . .
H79 H 1.062502 -0.017953 0.319566 0.154 Uiso 1 1 calc R U . . .
C80 C 1.0925(10) 0.1194(5) 0.4354(5) 0.1283(13) Uani 1 1 d . . . . .
H80A H 1.126632 0.139245 0.410016 0.192 Uiso 1 1 calc R U . . .
H80B H 1.151605 0.124930 0.471512 0.192 Uiso 1 1 calc R U . . .
H80C H 1.018548 0.139248 0.448595 0.192 Uiso 1 1 calc R U . . .
C81 C 1.0189(9) 0.0145(5) 0.4304(5) 0.1283(13) Uani 1 1 d . . . . .
H81A H 0.931922 0.018756 0.431518 0.192 Uiso 1 1 calc R U . . .
H81B H 1.061350 0.027598 0.472394 0.192 Uiso 1 1 calc R U . . .
H81C H 1.032550 -0.029607 0.407310 0.192 Uiso 1 1 calc R U . . .
O26 O 0.7458(7) 0.0916(3) 0.1547(3) 0.1356(15) Uani 1 1 d . . . . .
N18 N 0.9277(9) 0.0583(4) 0.1311(4) 0.1356(15) Uani 1 1 d . . . . .
C82 C 0.8162(10) 0.0774(5) 0.1189(5) 0.1356(15) Uani 1 1 d . . . . .
H82 H 0.793345 0.079398 0.079705 0.163 Uiso 1 1 calc R U . . .
C83 C 1.0071(10) 0.0437(5) 0.0848(5) 0.1356(15) Uani 1 1 d . . . . .
H83A H 1.009675 -0.002198 0.065481 0.203 Uiso 1 1 calc R U . . .
H83B H 1.088811 0.062883 0.103839 0.203 Uiso 1 1 calc R U . . .
H83C H 0.976889 0.060489 0.053594 0.203 Uiso 1 1 calc R U . . .
C84 C 0.9751(10) 0.0561(5) 0.1894(5) 0.1356(15) Uani 1 1 d . . . . .
H84A H 0.917767 0.073067 0.218577 0.203 Uiso 1 1 calc R U . . .
H84B H 1.052701 0.081376 0.204865 0.203 Uiso 1 1 calc R U . . .
H84C H 0.987223 0.012223 0.184608 0.203 Uiso 1 1 calc R U . . .
O27 O 0.7527(5) -0.0173(2) -0.0228(2) 0.0944(9) Uani 1 1 d . . . . .
N19 N 0.6000(7) -0.0926(3) -0.0612(3) 0.0944(9) Uani 1 1 d . . . . .
C85 C 0.6611(8) -0.0448(4) -0.0169(4) 0.0944(9) Uani 1 1 d . . . . .
H85 H 0.633779 -0.030369 0.021993 0.113 Uiso 1 1 calc R U . . .
C86 C 0.4937(8) -0.1221(4) -0.0516(4) 0.0944(9) Uani 1 1 d . . . . .
H86A H 0.485404 -0.104846 -0.007888 0.142 Uiso 1 1 calc R U . . .
H86B H 0.500708 -0.167701 -0.065066 0.142 Uiso 1 1 calc R U . . .
H86C H 0.422338 -0.113754 -0.075281 0.142 Uiso 1 1 calc R U . . .
C87 C 0.6405(8) -0.1194(4) -0.1207(4) 0.0944(9) Uani 1 1 d . . . . .
H87A H 0.709147 -0.092732 -0.122240 0.142 Uiso 1 1 calc R U . . .
H87B H 0.574101 -0.121570 -0.152766 0.142 Uiso 1 1 calc R U . . .
H87C H 0.665625 -0.161938 -0.127271 0.142 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 O5 1.935(3) . ?
Cu1 N1 1.942(3) . ?
Cu1 N6 1.959(3) . ?
Cu1 O1 1.977(3) . ?
Cu2 N3 1.933(3) . ?
Cu2 N2 1.945(3) . ?
Cu2 O12 1.957(3) . ?
Cu2 O1 2.014(3) . ?
Cu3 O18 1.932(3) . ?
Cu3 N5 1.957(3) . ?
Cu3 N4 1.966(3) . ?
Cu3 O1 1.981(3) . ?
Cu4 O2 1.846(3) . ?
Cu4 O9 1.945(3) . ?
Cu4 O8 1.948(3) . ?
Cu4 N8 1.985(3) . ?
Cu5 O2 1.890(3) . ?
Cu5 N9 1.933(3) . ?
Cu5 O10 1.941(3) . ?
Cu5 O22 1.946(2) . ?
Cu6 O3 1.871(3) . ?
Cu6 O14 1.936(3) . ?
Cu6 O13 1.950(3) . ?
Cu6 N11 1.970(3) . ?
Cu7 O3 1.898(3) . ?
Cu7 O15 1.940(3) . ?
Cu7 N12 1.949(3) . ?
Cu7 O20 1.978(3) . ?
Cu8 O4 1.859(3) . ?
Cu8 O17 1.934(3) . ?
Cu8 N14 1.959(3) . ?
Cu8 O19 1.961(3) . ?
Cu9 O4 1.887(3) . ?
Cu9 O6 1.941(3) . ?
Cu9 N15 1.947(3) . ?
Cu9 O21 1.947(3) . ?
P1 O5 1.509(3) . ?
P1 O6 1.510(3) . ?
P1 O8 1.515(3) . ?
P1 O7 1.625(3) . ?
P2 O13 1.511(3) . ?
P2 O12 1.513(3) . ?
P2 O10 1.514(3) . ?
P2 O11 1.619(3) . ?
P3 O18 1.507(3) . ?
P3 O15 1.512(3) . ?
P3 O17 1.518(3) . ?
P3 O16 1.616(3) . ?
P4 O21 1.512(3) . ?
P4 O22 1.520(3) . ?
P4 O20 1.523(3) . ?
P4 O23 1.595(3) . ?
O1 H1O 0.80(4) . ?
O2 H2O 0.820(2) . ?
O3 H3O 0.803(19) . ?
O4 H4O 0.820(2) . ?
O7 C40 1.390(4) . ?
O9 C70 1.238(5) . ?
O11 C25 1.390(5) . ?
O14 C67 1.251(5) . ?
O16 C1 1.390(5) . ?
O19 C73 1.244(5) . ?
O23 C55 1.394(5) . ?
N1 C16 1.334(5) . ?
N1 N2 1.370(4) . ?
N2 C18 1.332(5) . ?
N3 C19 1.341(5) . ?
N3 N4 1.364(4) . ?
N4 C21 1.341(5) . ?
N5 C13 1.334(5) . ?
N5 N6 1.362(4) . ?
N6 C15 1.339(5) . ?
N7 C70 1.304(5) . ?
N7 C71 1.454(6) . ?
N7 C72 1.462(6) . ?
N8 C39 1.334(5) . ?
N8 N9 1.359(4) . ?
N9 C37 1.337(5) . ?
N10 C67 1.310(5) . ?
N10 C68 1.452(6) . ?
N10 C69 1.454(6) . ?
N11 C24 1.346(5) . ?
N11 N12 1.358(4) . ?
N12 C22 1.335(5) . ?
N13 C73 1.306(5) . ?
N13 C75 1.443(7) . ?
N13 C74 1.456(6) . ?
N14 C54 1.343(5) . ?
N14 N15 1.363(4) . ?
N15 C52 1.333(5) . ?
C1 C2 1.388(6) . ?
C1 C6 1.392(7) . ?
C2 C3 1.391(6) . ?
C2 C8 1.514(7) . ?
C3 C4 1.371(8) . ?
C3 H3A 0.9500 . ?
C4 C5 1.362(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.410(6) . ?
C5 H5 0.9500 . ?
C6 C11 1.509(7) . ?
C7 C8 1.518(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.502(8) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.485(9) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.514(8) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.389(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.375(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.378(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.374(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.387(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.379(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.380(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.394(6) . ?
C25 C26 1.398(6) . ?
C26 C27 1.404(7) . ?
C26 C32 1.498(7) . ?
C27 C28 1.361(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.372(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.417(7) . ?
C29 H29 0.9500 . ?
C30 C35 1.502(7) . ?
C31 C32 1.523(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.544(7) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.523(7) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.520(7) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.369(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.385(7) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.387(6) . ?
C40 C45 1.399(6) . ?
C41 C42 1.394(6) . ?
C41 C47 1.523(6) . ?
C42 C43 1.377(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.366(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.395(6) . ?
C44 H44 0.9500 . ?
C45 C50 1.513(7) . ?
C46 C47 1.507(7) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.524(8) . ?
C47 H47 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.529(10) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.492(9) . ?
C50 H50 1.0000 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.376(6) . ?
C52 H52 0.9500 . ?
C53 C54 1.378(6) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.403(6) . ?
C55 C60 1.405(6) . ?
C56 C57 1.404(6) . ?
C56 C62 1.475(6) . ?
C57 C58 1.359(6) . ?
C57 H57 0.9500 . ?
C58 C59 1.390(6) . ?
C58 H58 0.9500 . ?
C59 C60 1.391(6) . ?
C59 H59 0.9500 . ?
C60 C65 1.517(6) . ?
C61 C62 1.546(8) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C63 1.530(8) . ?
C62 H62 1.0000 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 C65 1.517(6) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 C66 1.504(6) . ?
C65 H65 1.0000 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67 0.9500 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70 0.9500 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73 0.9500 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
O24 C76 1.224(6) . ?
N16 C76 1.296(7) . ?
N16 C78 1.445(7) . ?
N16 C77 1.485(7) . ?
C76 H76 0.9500 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
O25 C79 1.339(12) . ?
N17 C79 1.337(13) . ?
N17 C80 1.415(12) . ?
N17 C81 1.452(12) . ?
C79 H79 0.9500 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
O26 C82 1.190(10) . ?
N18 C82 1.361(13) . ?
N18 C84 1.437(13) . ?
N18 C83 1.443(11) . ?
C82 H82 0.9500 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
O27 C85 1.236(9) . ?
N19 C85 1.304(10) . ?
N19 C86 1.433(10) . ?
N19 C87 1.448(10) . ?
C85 H85 0.9500 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 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
O5 Cu1 N1 92.71(12) . . ?
O5 Cu1 N6 91.99(12) . . ?
N1 Cu1 N6 169.71(14) . . ?
O5 Cu1 O1 176.70(12) . . ?
N1 Cu1 O1 87.21(12) . . ?
N6 Cu1 O1 88.62(12) . . ?
N3 Cu2 N2 170.11(14) . . ?
N3 Cu2 O12 91.51(12) . . ?
N2 Cu2 O12 92.99(12) . . ?
N3 Cu2 O1 87.78(12) . . ?
N2 Cu2 O1 87.86(12) . . ?
O12 Cu2 O1 178.80(12) . . ?
O18 Cu3 N5 91.03(13) . . ?
O18 Cu3 N4 93.33(12) . . ?
N5 Cu3 N4 168.49(14) . . ?
O18 Cu3 O1 177.25(12) . . ?
N5 Cu3 O1 86.81(12) . . ?
N4 Cu3 O1 88.48(12) . . ?
O2 Cu4 O9 173.15(13) . . ?
O2 Cu4 O8 96.25(12) . . ?
O9 Cu4 O8 90.54(12) . . ?
O2 Cu4 N8 84.47(13) . . ?
O9 Cu4 N8 88.70(13) . . ?
O8 Cu4 N8 175.79(13) . . ?
O2 Cu5 N9 85.24(13) . . ?
O2 Cu5 O10 179.29(13) . . ?
N9 Cu5 O10 94.49(12) . . ?
O2 Cu5 O22 91.01(11) . . ?
N9 Cu5 O22 173.79(13) . . ?
O10 Cu5 O22 89.20(11) . . ?
O3 Cu6 O14 171.91(12) . . ?
O3 Cu6 O13 96.84(11) . . ?
O14 Cu6 O13 91.25(11) . . ?
O3 Cu6 N11 84.71(12) . . ?
O14 Cu6 N11 87.24(12) . . ?
O13 Cu6 N11 174.89(13) . . ?
O3 Cu7 O15 176.65(13) . . ?
O3 Cu7 N12 84.71(12) . . ?
O15 Cu7 N12 92.94(13) . . ?
O3 Cu7 O20 92.36(11) . . ?
O15 Cu7 O20 89.84(11) . . ?
N12 Cu7 O20 175.27(12) . . ?
O4 Cu8 O17 96.39(12) . . ?
O4 Cu8 N14 85.38(13) . . ?
O17 Cu8 N14 171.59(14) . . ?
O4 Cu8 O19 167.07(14) . . ?
O17 Cu8 O19 90.33(12) . . ?
N14 Cu8 O19 89.58(13) . . ?
O4 Cu9 O6 174.43(13) . . ?
O4 Cu9 N15 85.77(12) . . ?
O6 Cu9 N15 94.78(12) . . ?
O4 Cu9 O21 90.54(11) . . ?
O6 Cu9 O21 88.79(11) . . ?
N15 Cu9 O21 176.18(12) . . ?
O5 P1 O6 113.33(15) . . ?
O5 P1 O8 113.64(16) . . ?
O6 P1 O8 113.93(16) . . ?
O5 P1 O7 104.03(15) . . ?
O6 P1 O7 104.42(15) . . ?
O8 P1 O7 106.24(15) . . ?
O13 P2 O12 114.55(16) . . ?
O13 P2 O10 113.78(16) . . ?
O12 P2 O10 113.02(15) . . ?
O13 P2 O11 105.84(14) . . ?
O12 P2 O11 104.73(15) . . ?
O10 P2 O11 103.53(15) . . ?
O18 P3 O15 113.64(16) . . ?
O18 P3 O17 114.56(17) . . ?
O15 P3 O17 113.33(17) . . ?
O18 P3 O16 103.09(16) . . ?
O15 P3 O16 104.90(16) . . ?
O17 P3 O16 105.92(15) . . ?
O21 P4 O22 111.89(15) . . ?
O21 P4 O20 112.42(15) . . ?
O22 P4 O20 109.55(14) . . ?
O21 P4 O23 110.91(16) . . ?
O22 P4 O23 103.94(15) . . ?
O20 P4 O23 107.73(15) . . ?
Cu1 O1 Cu3 115.91(13) . . ?
Cu1 O1 Cu2 115.31(12) . . ?
Cu3 O1 Cu2 115.16(13) . . ?
Cu1 O1 H1O 105(3) . . ?
Cu3 O1 H1O 107(3) . . ?
Cu2 O1 H1O 95(3) . . ?
Cu4 O2 Cu5 128.04(15) . . ?
Cu4 O2 H2O 118(3) . . ?
Cu5 O2 H2O 113(3) . . ?
Cu6 O3 Cu7 122.71(14) . . ?
Cu6 O3 H3O 113(3) . . ?
Cu7 O3 H3O 112(3) . . ?
Cu8 O4 Cu9 126.11(14) . . ?
Cu8 O4 H4O 111(3) . . ?
Cu9 O4 H4O 116(3) . . ?
P1 O5 Cu1 136.17(17) . . ?
P1 O6 Cu9 132.23(17) . . ?
C40 O7 P1 127.5(2) . . ?
P1 O8 Cu4 135.19(17) . . ?
C70 O9 Cu4 127.7(3) . . ?
P2 O10 Cu5 129.77(17) . . ?
C25 O11 P2 130.0(2) . . ?
P2 O12 Cu2 131.33(17) . . ?
P2 O13 Cu6 137.77(17) . . ?
C67 O14 Cu6 130.6(3) . . ?
P3 O15 Cu7 132.07(17) . . ?
C1 O16 P3 130.4(3) . . ?
P3 O17 Cu8 139.32(17) . . ?
P3 O18 Cu3 133.10(17) . . ?
C73 O19 Cu8 123.5(3) . . ?
P4 O20 Cu7 124.60(15) . . ?
P4 O21 Cu9 135.63(16) . . ?
P4 O22 Cu5 128.85(15) . . ?
C55 O23 P4 132.6(3) . . ?
C16 N1 N2 107.5(3) . . ?
C16 N1 Cu1 130.7(3) . . ?
N2 N1 Cu1 121.4(2) . . ?
C18 N2 N1 108.4(3) . . ?
C18 N2 Cu2 131.2(3) . . ?
N1 N2 Cu2 120.2(2) . . ?
C19 N3 N4 108.4(3) . . ?
C19 N3 Cu2 129.6(3) . . ?
N4 N3 Cu2 121.9(2) . . ?
C21 N4 N3 107.4(3) . . ?
C21 N4 Cu3 132.5(3) . . ?
N3 N4 Cu3 120.1(2) . . ?
C13 N5 N6 107.8(3) . . ?
C13 N5 Cu3 131.5(3) . . ?
N6 N5 Cu3 120.6(2) . . ?
C15 N6 N5 107.8(3) . . ?
C15 N6 Cu1 131.1(3) . . ?
N5 N6 Cu1 119.5(2) . . ?
C70 N7 C71 120.4(4) . . ?
C70 N7 C72 122.0(4) . . ?
C71 N7 C72 117.3(4) . . ?
C39 N8 N9 106.9(3) . . ?
C39 N8 Cu4 132.4(3) . . ?
N9 N8 Cu4 120.7(2) . . ?
C37 N9 N8 108.9(3) . . ?
C37 N9 Cu5 130.4(3) . . ?
N8 N9 Cu5 120.6(2) . . ?
C67 N10 C68 119.9(4) . . ?
C67 N10 C69 122.7(4) . . ?
C68 N10 C69 117.3(4) . . ?
C24 N11 N12 107.7(3) . . ?
C24 N11 Cu6 132.9(3) . . ?
N12 N11 Cu6 119.4(2) . . ?
C22 N12 N11 108.3(3) . . ?
C22 N12 Cu7 131.5(3) . . ?
N11 N12 Cu7 120.2(2) . . ?
C73 N13 C75 120.6(4) . . ?
C73 N13 C74 121.6(4) . . ?
C75 N13 C74 117.8(4) . . ?
C54 N14 N15 107.8(3) . . ?
C54 N14 Cu8 130.8(3) . . ?
N15 N14 Cu8 120.7(2) . . ?
C52 N15 N14 107.5(3) . . ?
C52 N15 Cu9 132.2(3) . . ?
N14 N15 Cu9 120.0(2) . . ?
C2 C1 O16 120.3(4) . . ?
C2 C1 C6 122.9(4) . . ?
O16 C1 C6 116.4(4) . . ?
C1 C2 C3 117.6(5) . . ?
C1 C2 C8 121.8(4) . . ?
C3 C2 C8 120.6(5) . . ?
C4 C3 C2 121.2(5) . . ?
C4 C3 H3A 119.4 . . ?
C2 C3 H3A 119.4 . . ?
C5 C4 C3 120.4(4) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C4 C5 C6 121.3(5) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 116.6(5) . . ?
C1 C6 C11 121.7(4) . . ?
C5 C6 C11 121.6(5) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C2 111.2(5) . . ?
C9 C8 C7 111.8(5) . . ?
C2 C8 C7 114.1(5) . . ?
C9 C8 H8 106.4 . . ?
C2 C8 H8 106.4 . . ?
C7 C8 H8 106.4 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C10 C11 C6 109.9(5) . . ?
C10 C11 C12 111.1(6) . . ?
C6 C11 C12 115.6(5) . . ?
C10 C11 H11 106.6 . . ?
C6 C11 H11 106.6 . . ?
C12 C11 H11 106.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 C14 110.1(4) . . ?
N5 C13 H13 125.0 . . ?
C14 C13 H13 125.0 . . ?
C15 C14 C13 104.0(4) . . ?
C15 C14 H14 128.0 . . ?
C13 C14 H14 128.0 . . ?
N6 C15 C14 110.3(4) . . ?
N6 C15 H15 124.9 . . ?
C14 C15 H15 124.9 . . ?
N1 C16 C17 109.9(4) . . ?
N1 C16 H16 125.0 . . ?
C17 C16 H16 125.0 . . ?
C16 C17 C18 104.9(4) . . ?
C16 C17 H17 127.5 . . ?
C18 C17 H17 127.5 . . ?
N2 C18 C17 109.2(4) . . ?
N2 C18 H18 125.4 . . ?
C17 C18 H18 125.4 . . ?
N3 C19 C20 109.5(4) . . ?
N3 C19 H19 125.2 . . ?
C20 C19 H19 125.2 . . ?
C19 C20 C21 104.9(4) . . ?
C19 C20 H20 127.6 . . ?
C21 C20 H20 127.6 . . ?
N4 C21 C20 109.8(4) . . ?
N4 C21 H21 125.1 . . ?
C20 C21 H21 125.1 . . ?
N12 C22 C23 109.7(4) . . ?
N12 C22 H22 125.1 . . ?
C23 C22 H22 125.1 . . ?
C22 C23 C24 104.8(3) . . ?
C22 C23 H23 127.6 . . ?
C24 C23 H23 127.6 . . ?
N11 C24 C23 109.5(4) . . ?
N11 C24 H24 125.2 . . ?
C23 C24 H24 125.2 . . ?
O11 C25 C30 118.6(4) . . ?
O11 C25 C26 118.3(4) . . ?
C30 C25 C26 122.7(4) . . ?
C25 C26 C27 117.3(5) . . ?
C25 C26 C32 121.8(4) . . ?
C27 C26 C32 120.9(5) . . ?
C28 C27 C26 121.6(5) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C27 C28 C29 120.3(5) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C28 C29 C30 121.5(5) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C25 C30 C29 116.6(5) . . ?
C25 C30 C35 122.4(4) . . ?
C29 C30 C35 121.0(5) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C26 C32 C31 110.0(4) . . ?
C26 C32 C33 112.4(5) . . ?
C31 C32 C33 110.9(5) . . ?
C26 C32 H32 107.8 . . ?
C31 C32 H32 107.8 . . ?
C33 C32 H32 107.8 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C30 C35 C36 109.7(4) . . ?
C30 C35 C34 113.7(5) . . ?
C36 C35 C34 110.3(5) . . ?
C30 C35 H35 107.6 . . ?
C36 C35 H35 107.6 . . ?
C34 C35 H35 107.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N9 C37 C38 109.4(4) . . ?
N9 C37 H37 125.3 . . ?
C38 C37 H37 125.3 . . ?
C37 C38 C39 104.6(4) . . ?
C37 C38 H38 127.7 . . ?
C39 C38 H38 127.7 . . ?
N8 C39 C38 110.2(4) . . ?
N8 C39 H39 124.9 . . ?
C38 C39 H39 124.9 . . ?
C41 C40 O7 119.2(4) . . ?
C41 C40 C45 122.2(4) . . ?
O7 C40 C45 118.3(4) . . ?
C40 C41 C42 117.8(4) . . ?
C40 C41 C47 122.0(4) . . ?
C42 C41 C47 120.2(4) . . ?
C43 C42 C41 121.1(4) . . ?
C43 C42 H42 119.4 . . ?
C41 C42 H42 119.4 . . ?
C44 C43 C42 120.0(4) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C45 121.5(4) . . ?
C43 C44 H44 119.2 . . ?
C45 C44 H44 119.2 . . ?
C44 C45 C40 117.3(4) . . ?
C44 C45 C50 120.6(4) . . ?
C40 C45 C50 122.1(4) . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C46 C47 C41 111.5(4) . . ?
C46 C47 C48 111.3(5) . . ?
C41 C47 C48 109.9(4) . . ?
C46 C47 H47 108.0 . . ?
C41 C47 H47 108.0 . . ?
C48 C47 H47 108.0 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 H49A 109.5 . . ?
C50 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C50 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 C45 111.2(5) . . ?
C51 C50 C49 113.8(7) . . ?
C45 C50 C49 109.0(5) . . ?
C51 C50 H50 107.5 . . ?
C45 C50 H50 107.5 . . ?
C49 C50 H50 107.5 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N15 C52 C53 110.6(4) . . ?
N15 C52 H52 124.7 . . ?
C53 C52 H52 124.7 . . ?
C52 C53 C54 104.2(4) . . ?
C52 C53 H53 127.9 . . ?
C54 C53 H53 127.9 . . ?
N14 C54 C53 109.9(4) . . ?
N14 C54 H54 125.1 . . ?
C53 C54 H54 125.1 . . ?
O23 C55 C56 118.2(4) . . ?
O23 C55 C60 118.0(4) . . ?
C56 C55 C60 123.3(4) . . ?
C55 C56 C57 115.7(4) . . ?
C55 C56 C62 123.4(4) . . ?
C57 C56 C62 120.9(4) . . ?
C58 C57 C56 123.0(4) . . ?
C58 C57 H57 118.5 . . ?
C56 C57 H57 118.5 . . ?
C57 C58 C59 119.4(4) . . ?
C57 C58 H58 120.3 . . ?
C59 C58 H58 120.3 . . ?
C58 C59 C60 121.5(4) . . ?
C58 C59 H59 119.2 . . ?
C60 C59 H59 119.2 . . ?
C59 C60 C55 117.0(4) . . ?
C59 C60 C65 121.0(4) . . ?
C55 C60 C65 122.0(4) . . ?
C62 C61 H61A 109.5 . . ?
C62 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C62 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C56 C62 C63 110.8(5) . . ?
C56 C62 C61 111.2(4) . . ?
C63 C62 C61 110.7(5) . . ?
C56 C62 H62 108.0 . . ?
C63 C62 H62 108.0 . . ?
C61 C62 H62 108.0 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C65 C64 H64A 109.5 . . ?
C65 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C65 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C66 C65 C64 110.0(4) . . ?
C66 C65 C60 112.5(4) . . ?
C64 C65 C60 110.8(4) . . ?
C66 C65 H65 107.8 . . ?
C64 C65 H65 107.8 . . ?
C60 C65 H65 107.8 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O14 C67 N10 121.4(4) . . ?
O14 C67 H67 119.3 . . ?
N10 C67 H67 119.3 . . ?
N10 C68 H68A 109.5 . . ?
N10 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
N10 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
N10 C69 H69A 109.5 . . ?
N10 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
N10 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
O9 C70 N7 123.0(4) . . ?
O9 C70 H70 118.5 . . ?
N7 C70 H70 118.5 . . ?
N7 C71 H71A 109.5 . . ?
N7 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
N7 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
N7 C72 H72A 109.5 . . ?
N7 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
N7 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O19 C73 N13 122.2(4) . . ?
O19 C73 H73 118.9 . . ?
N13 C73 H73 118.9 . . ?
N13 C74 H74A 109.5 . . ?
N13 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
N13 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
N13 C75 H75A 109.5 . . ?
N13 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
N13 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C76 N16 C78 122.2(5) . . ?
C76 N16 C77 118.9(5) . . ?
C78 N16 C77 118.9(5) . . ?
O24 C76 N16 127.0(6) . . ?
O24 C76 H76 116.5 . . ?
N16 C76 H76 116.5 . . ?
N16 C77 H77A 109.5 . . ?
N16 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
N16 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
N16 C78 H78A 109.5 . . ?
N16 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
N16 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C79 N17 C80 123.8(11) . . ?
C79 N17 C81 117.1(10) . . ?
C80 N17 C81 119.1(9) . . ?
N17 C79 O25 114.1(11) . . ?
N17 C79 H79 123.0 . . ?
O25 C79 H79 123.0 . . ?
N17 C80 H80A 109.5 . . ?
N17 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
N17 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
N17 C81 H81A 109.5 . . ?
N17 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
N17 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C82 N18 C84 123.6(9) . . ?
C82 N18 C83 118.8(10) . . ?
C84 N18 C83 117.4(9) . . ?
O26 C82 N18 123.5(12) . . ?
O26 C82 H82 118.2 . . ?
N18 C82 H82 118.2 . . ?
N18 C83 H83A 109.5 . . ?
N18 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
N18 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
N18 C84 H84A 109.5 . . ?
N18 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
N18 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C85 N19 C86 121.0(8) . . ?
C85 N19 C87 121.1(8) . . ?
C86 N19 C87 117.9(7) . . ?
O27 C85 N19 123.7(9) . . ?
O27 C85 H85 118.2 . . ?
N19 C85 H85 118.2 . . ?
N19 C86 H86A 109.5 . . ?
N19 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
N19 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
N19 C87 H87A 109.5 . . ?
N19 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
N19 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 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
O3 H3O O22 0.803(19) 2.01(3) 2.756(4) 155(5) .
O1 H1O O24 0.80(4) 1.98(5) 2.668(5) 144(4) .
O4 H4O O20 0.820(2) 1.981(17) 2.746(4) 155(4) .
O2 H2O O21 0.820(2) 1.943(17) 2.725(4) 159(5) .

_refine_diff_density_max         1.815
_refine_diff_density_min         -1.535
_refine_diff_density_rms         0.096

####################################################################### 
# 
# 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_BS-187
_database_code_depnum_ccdc_archive 'CCDC 1835296'
loop_
_audit_author_name
_audit_author_address
'Carola Schulzke'
;Ernst-Moritz-Arndt-Universit?t Greifswald
Germany
;
_audit_update_record             
;
2018-04-06 deposited with the CCDC.	2020-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C167 H167 Cu9 N15 O23 P4'
_chemical_formula_weight         3447.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c :H'
_space_group_name_Hall           'R 3 -2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-y+2/3, -x+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-y+1/3, -x+2/3, z+7/6'

_cell_length_a                   31.5291(7)
_cell_length_b                   31.5291(7)
_cell_length_c                   28.0882(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     24181.2(14)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7947
_cell_measurement_theta_min      3.4110
_cell_measurement_theta_max      28.3540

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_F_000             10674
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.274
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150.01(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21569
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.262
_diffrn_reflns_theta_max         29.120
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.742
_diffrn_reflns_point_group_measured_fraction_full 0.870
_reflns_number_total             10717
_reflns_number_gt                8742
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.656
_reflns_Friedel_fraction_max     0.588
_reflns_Friedel_fraction_full    0.743

_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.

The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 5984.0Å³ and 1656 e, respectively. Six voids were found 
per unit cell with 276 electrons per void. Void and electrons are 
due to a unrefineable rotating substituent with a twofold symmetry 
at best sitting on an otherwise threefold symmetric molecule axis in 
a trigonal space group. It was impossible to model the disorder or to 
assign atoms to positions making chemical sense. Therefore, the apical
substituent was removed from the refinement. Neither refining in lower
symmetry space groups (including P1) nor a combination of lower symmetry 
and application of twin laws led to an improvement of the electron density 
pattern. It was, hence, concluded that R3c is indeed the appropriate 
space group and the substituent turning almost freely around the 3fold
symmetry axis.
The disordered substituent has been treated as a diffuse contribution 
to the overall scattering without specific atom positions.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016 (Sheldrick, 2016)'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_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)+(0.0483P)²] 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_abs_structure_details 
;
 Flack x determined using 2929 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10717
_refine_ls_number_parameters     556
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.1002
_refine_ls_wR_factor_gt          0.0935
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_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 0.46070(2) 0.61904(2) 0.51550(3) 0.02987(17) Uani 1 1 d . . . . .
Cu2 Cu 0.35030(2) 0.61610(2) 0.41813(2) 0.02577(15) Uani 1 1 d . . . . .
Cu3 Cu 0.44824(2) 0.71862(2) 0.51298(3) 0.02705(15) Uani 1 1 d . . . . .
P1 P 0.35933(5) 0.53679(5) 0.48030(6) 0.0281(3) Uani 1 1 d . . . . .
P2 P 0.333333 0.666667 0.53136(9) 0.0240(5) Uani 1 3 d S T P . .
O1 O 0.34808(12) 0.48509(12) 0.45744(16) 0.0338(10) Uani 1 1 d . . . . .
O2 O 0.36880(13) 0.56961(13) 0.43780(15) 0.0327(9) Uani 1 1 d . . . . .
O3 O 0.47505(13) 0.78910(12) 0.50797(16) 0.0353(10) Uani 1 1 d . . . . .
O4 O 0.40436(13) 0.55347(13) 0.51068(16) 0.0342(9) Uani 1 1 d . . . . .
O5 O 0.50447(14) 0.59082(14) 0.51853(16) 0.0393(10) Uani 1 1 d . . . . .
O6 O 0.32651(13) 0.61768(14) 0.51500(18) 0.0417(11) Uani 1 1 d . . . . .
O7 O 0.333333 0.666667 0.5875(3) 0.061(2) Uani 1 3 d S T P . .
O8 O 0.42473(14) 0.65109(13) 0.52282(16) 0.0320(9) Uani 1 1 d D . . . .
H8O H 0.3955(10) 0.634(2) 0.522(3) 0.05(2) Uiso 1 1 d D . . . .
O9 O 0.333333 0.666667 0.4033(2) 0.0254(13) Uani 1 3 d DS T P . .
H9O H 0.333333 0.666667 0.3734(10) 0.04(3) Uiso 1 3 d DS . P . .
N1 N 0.51777(17) 0.68460(17) 0.5136(2) 0.0417(13) Uani 1 1 d . . . . .
N2 N 0.51221(16) 0.72441(16) 0.5122(2) 0.0423(14) Uani 1 1 d . . . . .
N3 N 0.41851(16) 0.66612(17) 0.40925(17) 0.0293(11) Uani 1 1 d . . . . .
N4 N 0.28129(16) 0.56748(16) 0.40976(17) 0.0305(11) Uani 1 1 d . . . . .
N5 N 0.52218(17) 0.53337(17) 0.54200(18) 0.0358(12) Uani 1 1 d . . . . .
C1 C 0.3799(2) 0.46622(19) 0.4589(2) 0.0328(13) Uani 1 1 d . . . . .
C2 C 0.37207(19) 0.43184(19) 0.4937(2) 0.0317(13) Uani 1 1 d . . . . .
C3 C 0.4025(2) 0.4115(2) 0.4940(2) 0.0385(15) Uani 1 1 d . . . . .
H3 H 0.398124 0.388548 0.518086 0.046 Uiso 1 1 calc R U . . .
C4 C 0.4388(2) 0.4236(2) 0.4605(2) 0.0361(14) Uani 1 1 d . . . . .
C5 C 0.44437(19) 0.4576(2) 0.4252(2) 0.0361(14) Uani 1 1 d . . . . .
H5 H 0.468520 0.465729 0.401242 0.043 Uiso 1 1 calc R U . . .
C6 C 0.4157(2) 0.47979(19) 0.4241(2) 0.0347(14) Uani 1 1 d . . . . .
C7 C 0.3300(2) 0.4154(2) 0.5290(2) 0.0379(15) Uani 1 1 d . . . . .
H7 H 0.320534 0.441313 0.528877 0.045 Uiso 1 1 calc R U . . .
C8 C 0.3473(2) 0.4140(3) 0.5793(3) 0.0492(17) Uani 1 1 d . . . . .
C9 C 0.3404(3) 0.3717(3) 0.6005(3) 0.070(2) Uani 1 1 d . . . . .
H9 H 0.323756 0.341860 0.583209 0.084 Uiso 1 1 calc R U . . .
C10 C 0.3563(4) 0.3711(5) 0.6450(4) 0.104(4) Uani 1 1 d . . . . .
H10 H 0.350599 0.341125 0.658832 0.125 Uiso 1 1 calc R U . . .
C11 C 0.3811(4) 0.4144(7) 0.6703(4) 0.122(6) Uani 1 1 d . . . . .
H11 H 0.392397 0.414032 0.701576 0.146 Uiso 1 1 calc R U . . .
C12 C 0.3891(3) 0.4560(6) 0.6516(4) 0.109(5) Uani 1 1 d . . . . .
H12 H 0.406122 0.485372 0.669575 0.130 Uiso 1 1 calc R U . . .
C13 C 0.3723(2) 0.4576(4) 0.6043(3) 0.084(3) Uani 1 1 d . . . . .
H13 H 0.378223 0.487618 0.590694 0.100 Uiso 1 1 calc R U . . .
C14 C 0.2842(2) 0.3677(2) 0.5146(2) 0.0361(14) Uani 1 1 d . . . . .
C15 C 0.2840(2) 0.3368(2) 0.4804(3) 0.0455(16) Uani 1 1 d . . . . .
H15 H 0.313623 0.345570 0.463991 0.055 Uiso 1 1 calc R U . . .
C16 C 0.2422(3) 0.2930(2) 0.4687(3) 0.059(2) Uani 1 1 d . . . . .
H16 H 0.243128 0.272169 0.444819 0.071 Uiso 1 1 calc R U . . .
C17 C 0.1995(3) 0.2806(3) 0.4926(3) 0.062(2) Uani 1 1 d . . . . .
H17 H 0.170457 0.250979 0.484940 0.075 Uiso 1 1 calc R U . . .
C18 C 0.1983(2) 0.3099(3) 0.5268(3) 0.058(2) Uani 1 1 d . . . . .
H18 H 0.168479 0.301062 0.542854 0.070 Uiso 1 1 calc R U . . .
C19 C 0.2409(2) 0.3533(2) 0.5387(2) 0.0433(15) Uani 1 1 d . . . . .
H19 H 0.240125 0.373213 0.563724 0.052 Uiso 1 1 calc R U . . .
C20 C 0.4691(2) 0.3981(2) 0.4595(3) 0.0454(16) Uani 1 1 d . . . . .
H20 H 0.466254 0.382803 0.491469 0.054 Uiso 1 1 calc R U . . .
C21 C 0.4477(3) 0.3576(3) 0.4231(4) 0.077(3) Uani 1 1 d . . . . .
H21A H 0.412886 0.335691 0.429948 0.116 Uiso 1 1 calc R U . . .
H21B H 0.451180 0.371824 0.391259 0.116 Uiso 1 1 calc R U . . .
H21C H 0.465006 0.339105 0.424219 0.116 Uiso 1 1 calc R U . . .
C22 C 0.5227(2) 0.4324(3) 0.4498(3) 0.058(2) Uani 1 1 d . . . . .
H22A H 0.536064 0.458444 0.473786 0.087 Uiso 1 1 calc R U . . .
H22B H 0.540389 0.414221 0.451037 0.087 Uiso 1 1 calc R U . . .
H22C H 0.526563 0.446941 0.418078 0.087 Uiso 1 1 calc R U . . .
C23 C 0.4217(2) 0.5157(2) 0.3853(2) 0.0409(15) Uani 1 1 d . . . . .
H23 H 0.415343 0.540579 0.400868 0.049 Uiso 1 1 calc R U . . .
C24 C 0.4747(2) 0.5443(2) 0.3667(2) 0.0373(14) Uani 1 1 d . . . . .
C25 C 0.5110(2) 0.5773(2) 0.3972(3) 0.0491(17) Uani 1 1 d . . . . .
H25 H 0.502058 0.582449 0.428066 0.059 Uiso 1 1 calc R U . . .
C26 C 0.5592(3) 0.6026(3) 0.3840(4) 0.070(2) Uani 1 1 d . . . . .
H26 H 0.583247 0.624531 0.405800 0.084 Uiso 1 1 calc R U . . .
C27 C 0.5726(3) 0.5964(4) 0.3409(4) 0.096(3) Uani 1 1 d . . . . .
H27 H 0.606279 0.612827 0.332377 0.116 Uiso 1 1 calc R U . . .
C28 C 0.5380(4) 0.5665(5) 0.3087(4) 0.129(5) Uani 1 1 d . . . . .
H28 H 0.547493 0.563630 0.277377 0.155 Uiso 1 1 calc R U . . .
C29 C 0.4880(3) 0.5398(3) 0.3219(3) 0.080(3) Uani 1 1 d . . . . .
H29 H 0.463920 0.518994 0.299550 0.096 Uiso 1 1 calc R U . . .
C30 C 0.3840(2) 0.4927(2) 0.3464(3) 0.0466(16) Uani 1 1 d . . . . .
C31 C 0.3755(2) 0.4506(3) 0.3246(3) 0.0571(19) Uani 1 1 d . . . . .
H31 H 0.392620 0.434574 0.334853 0.069 Uiso 1 1 calc R U . . .
C32 C 0.3411(3) 0.4303(3) 0.2868(3) 0.069(2) Uani 1 1 d . . . . .
H32 H 0.335730 0.401015 0.271712 0.083 Uiso 1 1 calc R U . . .
C33 C 0.3157(3) 0.4527(4) 0.2718(3) 0.078(3) Uani 1 1 d . . . . .
H33 H 0.293660 0.439812 0.245719 0.093 Uiso 1 1 calc R U . . .
C34 C 0.3224(3) 0.4936(4) 0.2949(3) 0.077(3) Uani 1 1 d . . . . .
H34 H 0.303656 0.508390 0.286190 0.092 Uiso 1 1 calc R U . . .
C35 C 0.3575(3) 0.5140(3) 0.3317(3) 0.061(2) Uani 1 1 d . . . . .
H35 H 0.362791 0.543213 0.346745 0.073 Uiso 1 1 calc R U . . .
C36 C 0.4924(2) 0.5508(2) 0.5382(2) 0.0340(13) Uani 1 1 d . . . . .
H36 H 0.460306 0.532336 0.550910 0.041 Uiso 1 1 calc R U . . .
C37 C 0.5091(3) 0.4900(2) 0.5714(3) 0.0489(17) Uani 1 1 d . . . . .
H37A H 0.535486 0.482229 0.570121 0.073 Uiso 1 1 calc R U . . .
H37B H 0.504244 0.496757 0.604450 0.073 Uiso 1 1 calc R U . . .
H37C H 0.478740 0.462195 0.559371 0.073 Uiso 1 1 calc R U . . .
C38 C 0.5714(2) 0.5598(3) 0.5242(3) 0.0551(19) Uani 1 1 d . . . . .
H38A H 0.587882 0.540978 0.530288 0.083 Uiso 1 1 calc R U . . .
H38B H 0.570767 0.564943 0.489832 0.083 Uiso 1 1 calc R U . . .
H38C H 0.589213 0.591607 0.540244 0.083 Uiso 1 1 calc R U . . .
C39 C 0.5656(2) 0.6999(2) 0.5094(3) 0.055(2) Uani 1 1 d . . . . .
H39 H 0.579395 0.679157 0.508313 0.066 Uiso 1 1 calc R U . . .
C40 C 0.5920(2) 0.7505(2) 0.5070(3) 0.063(2) Uani 1 1 d . . . . .
H40 H 0.626599 0.771208 0.505773 0.076 Uiso 1 1 calc R U . . .
C41 C 0.5570(2) 0.7639(2) 0.5066(3) 0.058(2) Uani 1 1 d . . . . .
H41 H 0.563338 0.796562 0.502913 0.069 Uiso 1 1 calc R U . . .
C42 C 0.4580(2) 0.6618(2) 0.4006(2) 0.0402(15) Uani 1 1 d . . . . .
H42 H 0.458256 0.631870 0.399014 0.048 Uiso 1 1 calc R U . . .
C43 C 0.4981(2) 0.7077(2) 0.3945(3) 0.0497(18) Uani 1 1 d . . . . .
H43 H 0.530708 0.715625 0.387241 0.060 Uiso 1 1 calc R U . . .
C44 C 0.2585(2) 0.5191(2) 0.4011(2) 0.0392(15) Uani 1 1 d . . . . .
H44 H 0.273917 0.499898 0.399677 0.047 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 O8 1.870(4) . ?
Cu1 O4 1.943(4) . ?
Cu1 N1 1.948(5) . ?
Cu1 O5 1.983(4) . ?
Cu2 O2 1.910(4) . ?
Cu2 N3 1.945(4) . ?
Cu2 N4 1.950(4) . ?
Cu2 O9 1.9630(16) . ?
Cu3 O8 1.892(4) . ?
Cu3 N2 1.932(5) . ?
Cu3 O6 1.943(4) 2_665 ?
Cu3 O3 1.948(3) . ?
P1 O3 1.499(4) 3_565 ?
P1 O4 1.508(4) . ?
P1 O2 1.509(4) . ?
P1 O1 1.618(4) . ?
P2 O6 1.520(4) 3_565 ?
P2 O6 1.520(4) 2_665 ?
P2 O6 1.520(4) . ?
P2 O7 1.577(9) . ?
O1 C1 1.400(6) . ?
O5 C36 1.249(7) . ?
N1 C39 1.340(8) . ?
N1 N2 1.352(6) . ?
N2 C41 1.346(8) . ?
N3 N4 1.339(6) 2_665 ?
N3 C42 1.340(7) . ?
N4 C44 1.343(7) . ?
N5 C36 1.308(7) . ?
N5 C38 1.436(8) . ?
N5 C37 1.468(7) . ?
C1 C2 1.385(8) . ?
C1 C6 1.391(8) . ?
C2 C3 1.396(7) . ?
C2 C7 1.525(8) . ?
C3 C4 1.380(8) . ?
C4 C5 1.405(9) . ?
C4 C20 1.527(7) . ?
C5 C6 1.393(7) . ?
C6 C23 1.513(9) . ?
C7 C8 1.523(10) . ?
C7 C14 1.529(8) . ?
C8 C9 1.375(10) . ?
C8 C13 1.385(11) . ?
C9 C10 1.353(13) . ?
C10 C11 1.382(18) . ?
C11 C12 1.316(18) . ?
C12 C13 1.440(16) . ?
C14 C15 1.366(9) . ?
C14 C19 1.381(8) . ?
C15 C16 1.389(9) . ?
C16 C17 1.376(11) . ?
C17 C18 1.346(11) . ?
C18 C19 1.397(9) . ?
C20 C21 1.507(10) . ?
C20 C22 1.508(9) . ?
C23 C30 1.508(10) . ?
C23 C24 1.541(8) . ?
C24 C29 1.354(10) . ?
C24 C25 1.392(9) . ?
C25 C26 1.368(10) . ?
C26 C27 1.329(13) . ?
C27 C28 1.366(14) . ?
C28 C29 1.416(11) . ?
C30 C31 1.363(9) . ?
C30 C35 1.370(9) . ?
C31 C32 1.421(11) . ?
C32 C33 1.373(12) . ?
C33 C34 1.362(13) . ?
C34 C35 1.412(12) . ?
C39 C40 1.384(9) . ?
C40 C41 1.366(9) . ?
C42 C43 1.375(9) . ?
C43 C44 1.367(8) 2_665 ?

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
O8 Cu1 O4 95.96(16) . . ?
O8 Cu1 N1 85.27(18) . . ?
O4 Cu1 N1 174.4(2) . . ?
O8 Cu1 O5 169.79(19) . . ?
O4 Cu1 O5 89.81(15) . . ?
N1 Cu1 O5 89.79(17) . . ?
O2 Cu2 N3 91.21(16) . . ?
O2 Cu2 N4 94.61(17) . . ?
N3 Cu2 N4 165.6(2) . . ?
O2 Cu2 O9 175.0(2) . . ?
N3 Cu2 O9 87.37(13) . . ?
N4 Cu2 O9 87.88(14) . . ?
O8 Cu3 N2 84.90(17) . . ?
O8 Cu3 O6 91.77(16) . 2_665 ?
N2 Cu3 O6 176.63(17) . 2_665 ?
O8 Cu3 O3 175.26(19) . . ?
N2 Cu3 O3 93.11(17) . . ?
O6 Cu3 O3 90.17(15) 2_665 . ?
O3 P1 O4 114.0(3) 3_565 . ?
O3 P1 O2 114.7(2) 3_565 . ?
O4 P1 O2 112.3(2) . . ?
O3 P1 O1 104.7(2) 3_565 . ?
O4 P1 O1 105.7(2) . . ?
O2 P1 O1 104.2(2) . . ?
O6 P2 O6 111.3(2) 3_565 2_665 ?
O6 P2 O6 111.3(2) 3_565 . ?
O6 P2 O6 111.3(2) 2_665 . ?
O6 P2 O7 107.6(2) 3_565 . ?
O6 P2 O7 107.6(2) 2_665 . ?
O6 P2 O7 107.6(2) . . ?
C1 O1 P1 125.0(3) . . ?
P1 O2 Cu2 136.3(2) . . ?
P1 O3 Cu3 136.1(2) 2_665 . ?
P1 O4 Cu1 127.7(2) . . ?
C36 O5 Cu1 122.9(4) . . ?
P2 O6 Cu3 133.3(2) . 3_565 ?
Cu1 O8 Cu3 126.1(2) . . ?
Cu2 O9 Cu2 115.64(14) . 3_565 ?
Cu2 O9 Cu2 115.64(14) . 2_665 ?
Cu2 O9 Cu2 115.64(14) 3_565 2_665 ?
C39 N1 N2 107.9(5) . . ?
C39 N1 Cu1 131.4(4) . . ?
N2 N1 Cu1 120.4(3) . . ?
C41 N2 N1 107.5(5) . . ?
C41 N2 Cu3 130.6(4) . . ?
N1 N2 Cu3 121.7(3) . . ?
N4 N3 C42 108.3(5) 2_665 . ?
N4 N3 Cu2 121.3(3) 2_665 . ?
C42 N3 Cu2 130.4(4) . . ?
N3 N4 C44 108.0(4) 3_565 . ?
N3 N4 Cu2 119.9(3) 3_565 . ?
C44 N4 Cu2 131.9(4) . . ?
C36 N5 C38 121.4(5) . . ?
C36 N5 C37 120.7(5) . . ?
C38 N5 C37 117.1(5) . . ?
C2 C1 C6 122.5(5) . . ?
C2 C1 O1 117.9(5) . . ?
C6 C1 O1 119.5(5) . . ?
C1 C2 C3 117.9(5) . . ?
C1 C2 C7 120.6(5) . . ?
C3 C2 C7 121.4(5) . . ?
C4 C3 C2 122.4(6) . . ?
C3 C4 C5 117.5(5) . . ?
C3 C4 C20 121.1(6) . . ?
C5 C4 C20 121.2(6) . . ?
C6 C5 C4 122.3(5) . . ?
C1 C6 C5 117.4(5) . . ?
C1 C6 C23 121.0(5) . . ?
C5 C6 C23 121.6(6) . . ?
C8 C7 C2 110.4(5) . . ?
C8 C7 C14 113.1(5) . . ?
C2 C7 C14 113.3(5) . . ?
C9 C8 C13 118.5(8) . . ?
C9 C8 C7 122.9(7) . . ?
C13 C8 C7 118.6(7) . . ?
C10 C9 C8 122.4(10) . . ?
C9 C10 C11 119.4(12) . . ?
C12 C11 C10 120.9(12) . . ?
C11 C12 C13 120.8(12) . . ?
C8 C13 C12 118.1(11) . . ?
C15 C14 C19 117.4(6) . . ?
C15 C14 C7 123.5(5) . . ?
C19 C14 C7 119.0(6) . . ?
C14 C15 C16 122.6(7) . . ?
C17 C16 C15 118.3(8) . . ?
C18 C17 C16 120.8(7) . . ?
C17 C18 C19 120.0(7) . . ?
C14 C19 C18 120.8(7) . . ?
C21 C20 C22 110.6(6) . . ?
C21 C20 C4 108.9(6) . . ?
C22 C20 C4 113.3(5) . . ?
C30 C23 C6 112.8(5) . . ?
C30 C23 C24 113.4(6) . . ?
C6 C23 C24 112.0(5) . . ?
C29 C24 C25 118.0(6) . . ?
C29 C24 C23 123.8(6) . . ?
C25 C24 C23 118.2(6) . . ?
C26 C25 C24 121.8(7) . . ?
C27 C26 C25 120.2(9) . . ?
C26 C27 C28 120.0(9) . . ?
C27 C28 C29 120.4(10) . . ?
C24 C29 C28 119.4(9) . . ?
C31 C30 C35 118.1(7) . . ?
C31 C30 C23 121.2(6) . . ?
C35 C30 C23 120.7(6) . . ?
C30 C31 C32 120.6(7) . . ?
C33 C32 C31 120.5(8) . . ?
C34 C33 C32 119.2(9) . . ?
C33 C34 C35 119.7(8) . . ?
C30 C35 C34 121.9(8) . . ?
O5 C36 N5 122.8(6) . . ?
N1 C39 C40 109.9(6) . . ?
C41 C40 C39 104.1(6) . . ?
N2 C41 C40 110.4(6) . . ?
N3 C42 C43 109.2(5) . . ?
C44 C43 C42 104.9(5) 2_665 . ?
N4 C44 C43 109.5(5) . 3_565 ?

_refine_diff_density_max         1.066
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.069

####################################################################### 
# 
# 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_BS-212
_database_code_depnum_ccdc_archive 'CCDC 1835295'
loop_
_audit_author_name
_audit_author_address
'Carola Schulzke'
;Ernst-Moritz-Arndt-Universit?t Greifswald
Germany
;
_audit_update_record             
;
2018-04-06 deposited with the CCDC.	2020-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C159 H150.67 Cu9 N15 O23 P4'
_chemical_formula_weight         3335.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c :H'
_space_group_name_Hall           'R 3 -2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   31.198(4)
_cell_length_b                   31.198(4)
_cell_length_c                   27.045(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     22796(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    63703
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      52.9

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_F_000             10288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.406
_exptl_crystal_size_min          0.380
_exptl_absorpt_coefficient_mu    1.348
_shelx_estimated_absorpt_T_min   0.562
_shelx_estimated_absorpt_T_max   0.628
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6778
_exptl_absorpt_correction_T_max  0.9455
_exptl_absorpt_process_details   'face indexed'

_exptl_special_details           
;
programs X-Red32 and X-Shape by STOE & Cie GmbH 2010
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            61838
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.684
_diffrn_reflns_theta_max         26.464
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             9916
_reflns_number_gt                7175
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_max     0.903
_reflns_Friedel_fraction_full    0.922

_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.

The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 5652.0Å³ and 1933 e, respectively. Six voids were found 
per unit cell with 322 electrons per void. Void and electrons are 
due to a unrefineable rotating substituent with a twofold symmetry 
at best sitting on an otherwise threefold symmetric molecule axis in 
a trigonal space group. It was impossible to model the disorder or to 
assign atoms to positions making chemical sense. Therefore, the apical
substituent was removed from the refinement. Neither refining in lower
symmetry space groups (including P1) nor a combination of lower symmetry 
and application of twin laws led to an improvement of the electron density 
pattern. It was, hence, concluded that R3c is indeed the appropriate 
space group and the substituent turning almost freely around the 3fold
symmetry axis.
The disordered substituent has been treated as a diffuse contribution 
to the overall scattering without specific atom positions.
;

_computing_data_collection       'X-Area by STOE & Cie GmbH 2010'
_computing_cell_refinement       'X-Area by STOE & Cie GmbH 2010'
_computing_data_reduction        'X-Area by STOE & Cie GmbH 2010'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016 (Sheldrick, 2016)'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_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)+(0.0488P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.000017(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 2862 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9916
_refine_ls_number_parameters     541
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0864
_refine_ls_wR_factor_gt          0.0821
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_restrained_S_all      0.888
_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 0.79058(3) 0.51121(3) 0.61021(3) 0.04606(19) Uani 1 1 d . . . . .
Cu2 Cu 0.78268(3) 0.40028(3) 0.60928(3) 0.04383(18) Uani 1 1 d . . . . .
Cu3 Cu 0.68122(2) 0.40053(2) 0.51184(3) 0.04013(17) Uani 1 1 d . . . . .
P1 P 0.68736(5) 0.48839(5) 0.57601(6) 0.0427(3) Uani 1 1 d . . . . .
P2 P 0.666667 0.333333 0.62997(11) 0.0400(6) Uani 1 3 d S T P . .
O1 O 0.67523(14) 0.52800(13) 0.55062(16) 0.0466(10) Uani 1 1 d . . . . .
O2 O 0.73228(15) 0.51767(14) 0.60861(18) 0.0488(10) Uani 1 1 d . . . . .
O3 O 0.69822(14) 0.46522(14) 0.53244(16) 0.0473(10) Uani 1 1 d . . . . .
O4 O 0.81263(15) 0.35826(15) 0.60414(16) 0.0487(10) Uani 1 1 d . . . . .
O5 O 0.65818(16) 0.37471(15) 0.61296(19) 0.0549(11) Uani 1 1 d . . . . .
O6 O 0.666667 0.333333 0.6876(3) 0.0531(18) Uani 1 3 d S T P . .
O7 O 0.75674(15) 0.44268(16) 0.61917(17) 0.0502(11) Uani 1 1 d . . . . .
H7O H 0.726233 0.426(2) 0.616(3) 0.052(19) Uiso 1 1 d . . . . .
O8 O 0.666667 0.333333 0.4964(3) 0.0433(16) Uani 1 3 d DS T P . .
H8O H 0.666667 0.333333 0.4657(6) 0.03(3) Uiso 1 3 d DS . P . .
O9 O 0.83260(16) 0.58407(16) 0.61013(19) 0.0608(12) Uani 1 1 d . . . . .
N1 N 0.84629(19) 0.46045(19) 0.6066(2) 0.0552(14) Uani 1 1 d . . . . .
N2 N 0.84969(19) 0.50578(19) 0.6063(2) 0.0558(14) Uani 1 1 d . . . . .
N3 N 0.75018(17) 0.42145(17) 0.49989(19) 0.0430(12) Uani 1 1 d . . . . .
N4 N 0.61150(19) 0.37815(18) 0.50377(19) 0.0446(12) Uani 1 1 d . . . . .
N5 N 0.8484(2) 0.66005(19) 0.6322(2) 0.0665(16) Uani 1 1 d . . . . .
C1 C 0.7068(2) 0.5791(2) 0.5498(2) 0.0471(14) Uani 1 1 d . . . . .
C2 C 0.7415(2) 0.6007(2) 0.5122(2) 0.0486(15) Uani 1 1 d . . . . .
C3 C 0.7698(3) 0.6524(2) 0.5112(3) 0.0569(17) Uani 1 1 d . . . . .
H3 H 0.793444 0.667944 0.485569 0.068 Uiso 1 1 calc R U . . .
C4 C 0.7645(3) 0.6814(2) 0.5466(3) 0.0573(17) Uani 1 1 d . . . . .
C5 C 0.7298(3) 0.6584(2) 0.5837(3) 0.0590(17) Uani 1 1 d . . . . .
H5 H 0.726187 0.677943 0.608397 0.071 Uiso 1 1 calc R U . . .
C6 C 0.7003(2) 0.6073(2) 0.5854(2) 0.0480(15) Uani 1 1 d . . . . .
C7 C 0.7465(2) 0.5690(2) 0.4734(3) 0.0572(17) Uani 1 1 d . . . . .
H7 H 0.740352 0.538211 0.491028 0.069 Uiso 1 1 calc R U . . .
C8 C 0.8004(2) 0.5929(2) 0.4540(3) 0.0521(15) Uani 1 1 d . . . . .
C9 C 0.8377(3) 0.6003(3) 0.4862(3) 0.072(2) Uani 1 1 d . . . . .
H9 H 0.829999 0.590768 0.519882 0.086 Uiso 1 1 calc R U . . .
C10 C 0.8851(3) 0.6209(3) 0.4706(4) 0.078(2) Uani 1 1 d . . . . .
H10 H 0.910124 0.626045 0.493781 0.094 Uiso 1 1 calc R U . . .
C11 C 0.8977(3) 0.6340(4) 0.4237(4) 0.094(3) Uani 1 1 d . . . . .
H11 H 0.931426 0.649754 0.413951 0.112 Uiso 1 1 calc R U . . .
C12 C 0.8624(4) 0.6250(6) 0.3906(4) 0.138(5) Uani 1 1 d . . . . .
H12 H 0.871219 0.633323 0.356891 0.166 Uiso 1 1 calc R U . . .
C13 C 0.8123(3) 0.6032(4) 0.4046(3) 0.092(3) Uani 1 1 d . . . . .
H13 H 0.787279 0.595779 0.380676 0.111 Uiso 1 1 calc R U . . .
C14 C 0.7079(2) 0.5518(2) 0.4330(3) 0.0579(17) Uani 1 1 d . . . . .
C15 C 0.7011(3) 0.5836(3) 0.4043(3) 0.077(2) Uani 1 1 d . . . . .
H15 H 0.721914 0.618296 0.408584 0.093 Uiso 1 1 calc R U . . .
C16 C 0.6633(4) 0.5656(4) 0.3684(4) 0.096(3) Uani 1 1 d . . . . .
H16 H 0.658388 0.588669 0.349957 0.116 Uiso 1 1 calc R U . . .
C17 C 0.6340(3) 0.5170(3) 0.3593(3) 0.080(2) Uani 1 1 d . . . . .
H17 H 0.611122 0.505477 0.332631 0.096 Uiso 1 1 calc R U . . .
C18 C 0.6389(3) 0.4843(3) 0.3907(3) 0.083(2) Uani 1 1 d . . . . .
H18 H 0.616228 0.449786 0.388776 0.099 Uiso 1 1 calc R U . . .
C19 C 0.6770(3) 0.5027(3) 0.4248(3) 0.077(2) Uani 1 1 d . . . . .
H19 H 0.681784 0.479695 0.443550 0.092 Uiso 1 1 calc R U . . .
C20 C 0.7966(3) 0.7378(2) 0.5434(3) 0.078(2) Uani 1 1 d . . . . .
H20A H 0.800442 0.748073 0.508678 0.117 Uiso 1 1 calc R U . . .
H20B H 0.829248 0.748219 0.557697 0.117 Uiso 1 1 calc R U . . .
H20C H 0.780726 0.753168 0.561744 0.117 Uiso 1 1 calc R U . . .
C21 C 0.6581(2) 0.5821(2) 0.6226(2) 0.0516(16) Uani 1 1 d . . . . .
H21 H 0.649233 0.546510 0.623633 0.062 Uiso 1 1 calc R U . . .
C22 C 0.6742(2) 0.6021(2) 0.6753(3) 0.0538(16) Uani 1 1 d . . . . .
C23 C 0.6972(3) 0.5826(3) 0.7047(3) 0.069(2) Uani 1 1 d . . . . .
H23 H 0.704385 0.558745 0.691400 0.083 Uiso 1 1 calc R U . . .
C24 C 0.7095(3) 0.5980(4) 0.7534(3) 0.086(3) Uani 1 1 d . . . . .
H24 H 0.725373 0.585142 0.773463 0.103 Uiso 1 1 calc R U . . .
C25 C 0.6984(3) 0.6320(4) 0.7719(3) 0.085(3) Uani 1 1 d . . . . .
H25 H 0.705675 0.641839 0.805475 0.103 Uiso 1 1 calc R U . . .
C26 C 0.6773(3) 0.6521(3) 0.7431(3) 0.080(2) Uani 1 1 d . . . . .
H26 H 0.670703 0.676451 0.756263 0.096 Uiso 1 1 calc R U . . .
C27 C 0.6658(3) 0.6372(3) 0.6959(3) 0.070(2) Uani 1 1 d . . . . .
H27 H 0.651200 0.651729 0.676140 0.084 Uiso 1 1 calc R U . . .
C28 C 0.6112(2) 0.5824(2) 0.6067(3) 0.0551(16) Uani 1 1 d . . . . .
C29 C 0.6110(3) 0.6123(3) 0.5703(3) 0.080(2) Uani 1 1 d . . . . .
H29 H 0.640927 0.634534 0.553865 0.096 Uiso 1 1 calc R U . . .
C30 C 0.5669(4) 0.6104(4) 0.5572(4) 0.095(3) Uani 1 1 d . . . . .
H30 H 0.566737 0.631410 0.531842 0.114 Uiso 1 1 calc R U . . .
C31 C 0.5236(4) 0.5780(4) 0.5810(4) 0.097(3) Uani 1 1 d . . . . .
H31 H 0.493368 0.576297 0.571999 0.116 Uiso 1 1 calc R U . . .
C32 C 0.5247(3) 0.5493(4) 0.6165(4) 0.085(3) Uani 1 1 d . . . . .
H32 H 0.494660 0.527009 0.632773 0.102 Uiso 1 1 calc R U . . .
C33 C 0.5672(3) 0.5506(3) 0.6306(3) 0.071(2) Uani 1 1 d . . . . .
H33 H 0.566714 0.529860 0.656538 0.085 Uiso 1 1 calc R U . . .
C34 C 0.8919(2) 0.4675(3) 0.6012(3) 0.0630(19) Uani 1 1 d . . . . .
H34 H 0.899635 0.441738 0.599582 0.076 Uiso 1 1 calc R U . . .
C35 C 0.9263(3) 0.5175(3) 0.5983(4) 0.081(3) Uani 1 1 d . . . . .
H35 H 0.961242 0.532791 0.595103 0.097 Uiso 1 1 calc R U . . .
C36 C 0.8977(2) 0.5401(3) 0.6011(3) 0.071(2) Uani 1 1 d . . . . .
H36 H 0.910257 0.574768 0.599601 0.085 Uiso 1 1 calc R U . . .
C37 C 0.7887(2) 0.4658(2) 0.4883(3) 0.0503(15) Uani 1 1 d . . . . .
H37 H 0.787268 0.495302 0.483869 0.060 Uiso 1 1 calc R U . . .
C38 C 0.8301(2) 0.4620(2) 0.4840(3) 0.0594(18) Uani 1 1 d . . . . .
H38 H 0.862423 0.487595 0.475584 0.071 Uiso 1 1 calc R U . . .
C39 C 0.5865(2) 0.4021(2) 0.4941(3) 0.0568(17) Uani 1 1 d . . . . .
H39 H 0.600333 0.436987 0.494368 0.068 Uiso 1 1 calc R U . . .
C40 C 0.8197(2) 0.6119(2) 0.6299(3) 0.0557(16) Uani 1 1 d . . . . .
H40 H 0.787519 0.597538 0.643951 0.067 Uiso 1 1 calc R U . . .
C41 C 0.8969(4) 0.6845(3) 0.6117(4) 0.104(3) Uani 1 1 d . . . . .
H41A H 0.897812 0.666178 0.582687 0.155 Uiso 1 1 calc R U . . .
H41B H 0.920530 0.686011 0.636454 0.155 Uiso 1 1 calc R U . . .
H41C H 0.905628 0.718136 0.601875 0.155 Uiso 1 1 calc R U . . .
C42 C 0.8335(4) 0.6901(3) 0.6591(4) 0.091(3) Uani 1 1 d . . . . .
H42A H 0.798909 0.669720 0.669479 0.137 Uiso 1 1 calc R U . . .
H42B H 0.836730 0.717002 0.637812 0.137 Uiso 1 1 calc R U . . .
H42C H 0.854560 0.704061 0.688296 0.137 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 O7 1.867(4) . ?
Cu1 O2 1.928(4) . ?
Cu1 N2 1.937(5) . ?
Cu1 O9 1.976(4) . ?
Cu2 O7 1.883(4) . ?
Cu2 N1 1.934(5) . ?
Cu2 O5 1.957(4) 3_665 ?
Cu2 O4 1.959(4) . ?
Cu3 O3 1.896(4) . ?
Cu3 N4 1.936(5) . ?
Cu3 N3 1.938(5) . ?
Cu3 O8 1.9558(18) . ?
P1 O4 1.490(4) 2_655 ?
P1 O3 1.507(4) . ?
P1 O2 1.515(4) . ?
P1 O1 1.616(4) . ?
P2 O5 1.513(4) 3_665 ?
P2 O5 1.513(4) 2_655 ?
P2 O5 1.513(4) . ?
P2 O6 1.557(8) . ?
O1 C1 1.395(6) . ?
O7 H7O 0.831(9) . ?
O8 H8O 0.829(14) . ?
O9 C40 1.245(8) . ?
N1 C34 1.333(8) . ?
N1 N2 1.364(7) . ?
N2 C36 1.344(8) . ?
N3 C37 1.339(7) . ?
N3 N4 1.364(7) 3_665 ?
N4 C39 1.346(7) . ?
N5 C40 1.311(8) . ?
N5 C41 1.420(11) . ?
N5 C42 1.437(10) . ?
C1 C6 1.385(9) . ?
C1 C2 1.387(9) . ?
C2 C3 1.397(8) . ?
C2 C7 1.506(9) . ?
C3 C4 1.383(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(9) . ?
C4 C20 1.532(9) . ?
C5 C6 1.386(8) . ?
C5 H5 0.9500 . ?
C6 C21 1.527(9) . ?
C7 C14 1.513(10) . ?
C7 C8 1.550(9) . ?
C7 H7 1.0000 . ?
C8 C9 1.378(10) . ?
C8 C13 1.380(11) . ?
C9 C10 1.352(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.330(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.336(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.409(12) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.358(10) . ?
C14 C19 1.359(10) . ?
C15 C16 1.409(13) . ?
C15 H15 0.9500 . ?
C16 C17 1.346(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(13) . ?
C17 H17 0.9500 . ?
C18 C19 1.381(12) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C28 1.531(9) . ?
C21 C22 1.535(10) . ?
C21 H21 1.0000 . ?
C22 C27 1.368(10) . ?
C22 C23 1.398(10) . ?
C23 C24 1.387(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.363(13) . ?
C24 H24 0.9500 . ?
C25 C26 1.359(13) . ?
C25 H25 0.9500 . ?
C26 C27 1.343(11) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.358(11) . ?
C28 C33 1.388(10) . ?
C29 C30 1.393(12) . ?
C29 H29 0.9500 . ?
C30 C31 1.376(14) . ?
C30 H30 0.9500 . ?
C31 C32 1.326(14) . ?
C31 H31 0.9500 . ?
C32 C33 1.360(12) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.386(10) . ?
C34 H34 0.9500 . ?
C35 C36 1.387(10) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.361(9) . ?
C37 H37 0.9500 . ?
C38 C39 1.373(9) 3_665 ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 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
O7 Cu1 O2 95.72(17) . . ?
O7 Cu1 N2 85.7(2) . . ?
O2 Cu1 N2 175.5(2) . . ?
O7 Cu1 O9 170.8(2) . . ?
O2 Cu1 O9 89.86(18) . . ?
N2 Cu1 O9 89.3(2) . . ?
O7 Cu2 N1 85.2(2) . . ?
O7 Cu2 O5 91.38(18) . 3_665 ?
N1 Cu2 O5 176.6(2) . 3_665 ?
O7 Cu2 O4 175.26(19) . . ?
N1 Cu2 O4 92.61(19) . . ?
O5 Cu2 O4 90.77(17) 3_665 . ?
O3 Cu3 N4 94.77(19) . . ?
O3 Cu3 N3 91.02(18) . . ?
N4 Cu3 N3 163.9(2) . . ?
O3 Cu3 O8 174.6(2) . . ?
N4 Cu3 O8 88.42(14) . . ?
N3 Cu3 O8 87.06(15) . . ?
O4 P1 O3 114.9(2) 2_655 . ?
O4 P1 O2 113.5(3) 2_655 . ?
O3 P1 O2 112.5(2) . . ?
O4 P1 O1 104.8(2) 2_655 . ?
O3 P1 O1 103.3(2) . . ?
O2 P1 O1 106.6(2) . . ?
O5 P2 O5 111.2(2) 3_665 2_655 ?
O5 P2 O5 111.2(2) 3_665 . ?
O5 P2 O5 111.2(2) 2_655 . ?
O5 P2 O6 107.7(2) 3_665 . ?
O5 P2 O6 107.7(2) 2_655 . ?
O5 P2 O6 107.7(2) . . ?
C1 O1 P1 125.5(4) . . ?
P1 O2 Cu1 125.9(3) . . ?
P1 O3 Cu3 136.9(3) . . ?
P1 O4 Cu2 134.9(3) 3_665 . ?
P2 O5 Cu2 133.7(3) . 2_655 ?
Cu1 O7 Cu2 126.2(2) . . ?
Cu1 O7 H7O 121(4) . . ?
Cu2 O7 H7O 108(4) . . ?
Cu3 O8 Cu3 115.54(16) 3_665 2_655 ?
Cu3 O8 Cu3 115.54(16) 3_665 . ?
Cu3 O8 Cu3 115.54(16) 2_655 . ?
Cu3 O8 H8O 102.4(2) 3_665 . ?
Cu3 O8 H8O 102.4(2) 2_655 . ?
Cu3 O8 H8O 102.4(2) . . ?
C40 O9 Cu1 122.8(4) . . ?
C34 N1 N2 107.7(5) . . ?
C34 N1 Cu2 131.0(4) . . ?
N2 N1 Cu2 121.1(4) . . ?
C36 N2 N1 107.7(5) . . ?
C36 N2 Cu1 131.8(5) . . ?
N1 N2 Cu1 120.4(4) . . ?
C37 N3 N4 108.4(5) . 3_665 ?
C37 N3 Cu3 131.1(4) . . ?
N4 N3 Cu3 120.4(3) 3_665 . ?
C39 N4 N3 107.1(5) . 2_655 ?
C39 N4 Cu3 132.7(4) . . ?
N3 N4 Cu3 119.5(3) 2_655 . ?
C40 N5 C41 122.1(7) . . ?
C40 N5 C42 120.8(7) . . ?
C41 N5 C42 116.9(7) . . ?
C6 C1 C2 121.7(5) . . ?
C6 C1 O1 118.1(5) . . ?
C2 C1 O1 120.1(5) . . ?
C1 C2 C3 117.7(6) . . ?
C1 C2 C7 120.2(5) . . ?
C3 C2 C7 122.0(6) . . ?
C4 C3 C2 121.8(6) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C5 C4 C3 118.7(6) . . ?
C5 C4 C20 122.0(6) . . ?
C3 C4 C20 119.3(6) . . ?
C4 C5 C6 121.2(6) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 118.8(6) . . ?
C1 C6 C21 119.5(5) . . ?
C5 C6 C21 121.4(6) . . ?
C2 C7 C14 114.3(6) . . ?
C2 C7 C8 111.4(5) . . ?
C14 C7 C8 113.9(6) . . ?
C2 C7 H7 105.4 . . ?
C14 C7 H7 105.4 . . ?
C8 C7 H7 105.4 . . ?
C9 C8 C13 117.8(7) . . ?
C9 C8 C7 119.2(6) . . ?
C13 C8 C7 122.7(7) . . ?
C10 C9 C8 120.9(8) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11 C10 C9 121.9(9) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C10 C11 C12 119.3(9) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C13 121.2(9) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C8 C13 C12 118.5(8) . . ?
C8 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C15 C14 C19 116.6(7) . . ?
C15 C14 C7 122.7(7) . . ?
C19 C14 C7 120.6(6) . . ?
C14 C15 C16 120.5(8) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 122.5(9) . . ?
C17 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C16 C17 C18 116.8(9) . . ?
C16 C17 H17 121.6 . . ?
C18 C17 H17 121.6 . . ?
C19 C18 C17 119.3(8) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C14 C19 C18 123.7(8) . . ?
C14 C19 H19 118.1 . . ?
C18 C19 H19 118.1 . . ?
C4 C20 H20A 109.5 . . ?
C4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C6 C21 C28 113.1(5) . . ?
C6 C21 C22 112.4(5) . . ?
C28 C21 C22 112.1(5) . . ?
C6 C21 H21 106.2 . . ?
C28 C21 H21 106.2 . . ?
C22 C21 H21 106.2 . . ?
C27 C22 C23 117.5(7) . . ?
C27 C22 C21 123.4(6) . . ?
C23 C22 C21 119.1(6) . . ?
C24 C23 C22 120.2(8) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 118.9(9) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C26 C25 C24 121.2(9) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C27 C26 C25 119.5(9) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C26 C27 C22 122.6(8) . . ?
C26 C27 H27 118.7 . . ?
C22 C27 H27 118.7 . . ?
C29 C28 C33 119.0(7) . . ?
C29 C28 C21 122.8(7) . . ?
C33 C28 C21 118.2(7) . . ?
C28 C29 C30 120.0(9) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C31 C30 C29 119.9(10) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C32 C31 C30 119.2(9) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
C31 C32 C33 122.4(9) . . ?
C31 C32 H32 118.8 . . ?
C33 C32 H32 118.8 . . ?
C32 C33 C28 119.6(9) . . ?
C32 C33 H33 120.2 . . ?
C28 C33 H33 120.2 . . ?
N1 C34 C35 110.8(6) . . ?
N1 C34 H34 124.6 . . ?
C35 C34 H34 124.6 . . ?
C34 C35 C36 103.5(6) . . ?
C34 C35 H35 128.2 . . ?
C36 C35 H35 128.2 . . ?
N2 C36 C35 110.2(6) . . ?
N2 C36 H36 124.9 . . ?
C35 C36 H36 124.9 . . ?
N3 C37 C38 109.2(5) . . ?
N3 C37 H37 125.4 . . ?
C38 C37 H37 125.4 . . ?
C37 C38 C39 106.0(5) . 3_665 ?
C37 C38 H38 127.0 . . ?
C39 C38 H38 127.0 3_665 . ?
N4 C39 C38 109.3(6) . 2_655 ?
N4 C39 H39 125.4 . . ?
C38 C39 H39 125.4 2_655 . ?
O9 C40 N5 123.0(7) . . ?
O9 C40 H40 118.5 . . ?
N5 C40 H40 118.5 . . ?
N5 C41 H41A 109.5 . . ?
N5 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N5 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N5 C42 H42A 109.5 . . ?
N5 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N5 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

_refine_diff_density_max         0.542
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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_BS-92
_database_code_depnum_ccdc_archive 'CCDC 1835294'
loop_
_audit_author_name
_audit_author_address
'Carola Schulzke'
;Ernst-Moritz-Arndt-Universit?t Greifswald
Germany
;
_audit_update_record             
;
2018-04-06 deposited with the CCDC.	2020-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C163 H159 Cu9 N15 O23 P4'
_chemical_formula_weight         3391.78

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c :H'
_space_group_name_Hall           'R 3 -2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   31.380(4)
_cell_length_b                   31.380(4)
_cell_length_c                   27.242(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     23232(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    71105
_cell_measurement_theta_min      5.0
_cell_measurement_theta_max      55.0

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_F_000             10482
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.119
_exptl_absorpt_coefficient_mu    1.324
_shelx_estimated_absorpt_T_min   0.764
_shelx_estimated_absorpt_T_max   0.858
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7835
_exptl_absorpt_correction_T_max  0.8799
_exptl_absorpt_process_details   'face indexed'

_exptl_special_details           
;
programs X-Red32 and X-Shape by STOE & Cie GmbH 2010
;


_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            68936
_diffrn_reflns_av_unetI/netI     0.1179
_diffrn_reflns_av_R_equivalents  0.1296
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.483
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11745
_reflns_number_gt                6141
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_max     0.987
_reflns_Friedel_fraction_full    0.999

_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.

The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 5607.0Å³ and 1656 e, respectively. Six voids were found 
per unit cell with 276 electrons per void. Void and electrons are 
due to a unrefineable rotating substituent with a twofold symmetry 
at best sitting on an otherwise threefold symmetric molecule axis in 
a trigonal space group. It was impossible to model the disorder or to 
assign atoms to positions making chemical sense. Therefore, the apical
substituent was removed from the refinement. Neither refining in lower
symmetry space groups (including P1) nor a combination of lower symmetry 
and application of twin laws led to an improvement of the electron density 
pattern. It was, hence, concluded that R3c is indeed the appropriate 
space group and the substituent turning almost freely around the 3fold
symmetry axis.
The disordered substituent has been treated as a diffuse contribution 
to the overall scattering without specific atom positions.

The hydroxide protons were not actually located. Very weak electron 
density was used to fix them into idealised position (DFIX) and Ueq was
set to 1.5 times of that of the respective oxygen atom (O4, O7).
This assumption (hydoxides instead of oxides is based on a very similar 
structure and the sum of the charges present.
;

_computing_data_collection       'X-Area by STOE & Cie GmbH 2010'
_computing_cell_refinement       'X-Area by STOE & Cie GmbH 2010'
_computing_data_reduction        'X-Area by STOE & Cie GmbH 2010'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016 (Sheldrick, 2016)'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_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)+(0.0592P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.000106(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 2265 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11745
_refine_ls_number_parameters     546
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1214
_refine_ls_wR_factor_gt          0.1025
_refine_ls_goodness_of_fit_ref   0.825
_refine_ls_restrained_S_all      0.825
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.40040(4) 0.68138(4) 0.54081(4) 0.0357(3) Uani 1 1 d . . . . .
Cu2 Cu 0.38271(4) 0.60040(4) 0.44457(4) 0.0376(3) Uani 1 1 d . . . . .
Cu3 Cu 0.28049(4) 0.48969(4) 0.44332(4) 0.0404(3) Uani 1 1 d . . . . .
P1 P 0.48821(8) 0.68796(9) 0.47734(9) 0.0369(5) Uani 1 1 d . . . . .
P2 P 0.333333 0.666667 0.42507(14) 0.0332(8) Uani 1 3 d S T P . .
O1 O 0.5279(2) 0.6762(2) 0.5016(2) 0.0396(14) Uani 1 1 d . . . . .
O2 O 0.4652(2) 0.6983(2) 0.52102(19) 0.0393(14) Uani 1 1 d . . . . .
O3 O 0.4537(2) 0.6423(2) 0.4496(2) 0.0429(16) Uani 1 1 d . . . . .
O4 O 0.333333 0.666667 0.5553(4) 0.042(3) Uani 1 3 d DS T P . .
H4O H 0.333333 0.666667 0.5858(12) 0.063 Uiso 1 3 d DS U P . .
O5 O 0.3747(2) 0.6583(2) 0.4420(3) 0.0459(16) Uani 1 1 d . . . . .
O6 O 0.333333 0.666667 0.3673(4) 0.055(3) Uani 1 3 d S T P . .
O7 O 0.3146(2) 0.5581(3) 0.4351(2) 0.0474(16) Uani 1 1 d D . . . .
H7O H 0.299(4) 0.573(4) 0.435(4) 0.071 Uiso 1 1 d D U . . .
O8 O 0.2504(3) 0.4170(2) 0.4420(2) 0.0520(17) Uani 1 1 d . . . . .
O9 O 0.5171(2) 0.7326(2) 0.4454(3) 0.0454(15) Uani 1 1 d . . . . .
N1 N 0.3783(3) 0.6122(3) 0.5491(2) 0.0373(17) Uani 1 1 d . . . . .
N2 N 0.4206(3) 0.7494(3) 0.5526(3) 0.0399(18) Uani 1 1 d . . . . .
N3 N 0.3865(3) 0.5408(3) 0.4473(3) 0.049(2) Uani 1 1 d . . . . .
N4 N 0.3447(3) 0.4948(3) 0.4468(3) 0.050(2) Uani 1 1 d . . . . .
N5 N 0.1906(3) 0.3412(3) 0.4193(3) 0.052(2) Uani 1 1 d . . . . .
C1 C 0.5783(3) 0.7064(3) 0.5018(3) 0.041(2) Uani 1 1 d . . . . .
C2 C 0.6004(3) 0.7412(4) 0.5388(3) 0.043(2) Uani 1 1 d . . . . .
C3 C 0.6522(4) 0.7703(4) 0.5401(4) 0.060(3) Uani 1 1 d . . . . .
H3 H 0.667648 0.794585 0.564826 0.072 Uiso 1 1 calc R U . . .
C4 C 0.6808(3) 0.7636(4) 0.5056(4) 0.058(3) Uani 1 1 d . . . . .
C5 C 0.6570(3) 0.7288(4) 0.4688(4) 0.053(3) Uani 1 1 d . . . . .
H5 H 0.676150 0.725034 0.444015 0.064 Uiso 1 1 calc R U . . .
C6 C 0.6067(3) 0.6998(3) 0.4672(3) 0.041(2) Uani 1 1 d . . . . .
C7 C 0.5695(3) 0.7478(4) 0.5776(3) 0.045(2) Uani 1 1 d . . . . .
H7 H 0.538765 0.741895 0.560545 0.054 Uiso 1 1 calc R U . . .
C8 C 0.5529(3) 0.7093(4) 0.6178(3) 0.048(2) Uani 1 1 d . . . . .
C9 C 0.5042(4) 0.6811(4) 0.6279(4) 0.059(3) Uani 1 1 d . . . . .
H9 H 0.481688 0.686869 0.609813 0.070 Uiso 1 1 calc R U . . .
C10 C 0.4858(4) 0.6446(5) 0.6630(4) 0.068(3) Uani 1 1 d . . . . .
H10 H 0.451286 0.624542 0.667792 0.081 Uiso 1 1 calc R U . . .
C11 C 0.5187(5) 0.6378(4) 0.6911(4) 0.073(3) Uani 1 1 d . . . . .
H11 H 0.507375 0.613711 0.716399 0.088 Uiso 1 1 calc R U . . .
C12 C 0.5682(5) 0.6669(5) 0.6815(5) 0.081(4) Uani 1 1 d . . . . .
H12 H 0.591142 0.662593 0.700554 0.097 Uiso 1 1 calc R U . . .
C13 C 0.5854(4) 0.7022(4) 0.6447(4) 0.066(3) Uani 1 1 d . . . . .
H13 H 0.619737 0.721280 0.638353 0.080 Uiso 1 1 calc R U . . .
C14 C 0.5946(3) 0.8016(3) 0.5963(3) 0.044(2) Uani 1 1 d . . . . .
C15 C 0.6099(6) 0.8141(4) 0.6443(4) 0.085(4) Uani 1 1 d . . . . .
H15 H 0.605091 0.789559 0.667534 0.102 Uiso 1 1 calc R U . . .
C16 C 0.6326(6) 0.8639(5) 0.6581(5) 0.096(5) Uani 1 1 d . . . . .
H16 H 0.644439 0.872934 0.690765 0.116 Uiso 1 1 calc R U . . .
C17 C 0.6380(5) 0.8987(4) 0.6264(5) 0.077(4) Uani 1 1 d . . . . .
H17 H 0.653769 0.932198 0.636276 0.093 Uiso 1 1 calc R U . . .
C18 C 0.6213(5) 0.8860(4) 0.5811(5) 0.072(4) Uani 1 1 d . . . . .
H18 H 0.623927 0.910756 0.559092 0.086 Uiso 1 1 calc R U . . .
C19 C 0.6001(5) 0.8382(4) 0.5648(4) 0.071(3) Uani 1 1 d . . . . .
H19 H 0.589246 0.830470 0.531756 0.085 Uiso 1 1 calc R U . . .
C20 C 0.7375(4) 0.7915(5) 0.5088(5) 0.078(4) Uani 1 1 d . . . . .
H20A H 0.747588 0.775307 0.533684 0.094 Uiso 1 1 calc R U . . .
H20B H 0.750949 0.788911 0.476736 0.094 Uiso 1 1 calc R U . . .
C21 C 0.7589(6) 0.8433(6) 0.5214(7) 0.133(7) Uani 1 1 d . . . . .
H21A H 0.794815 0.858595 0.522807 0.200 Uiso 1 1 calc R U . . .
H21B H 0.749848 0.859823 0.496489 0.200 Uiso 1 1 calc R U . . .
H21C H 0.746483 0.846204 0.553503 0.200 Uiso 1 1 calc R U . . .
C22 C 0.5813(4) 0.6589(4) 0.4298(3) 0.045(2) Uani 1 1 d . . . . .
H22 H 0.545997 0.650239 0.429127 0.055 Uiso 1 1 calc R U . . .
C23 C 0.6011(4) 0.6749(4) 0.3777(3) 0.048(2) Uani 1 1 d . . . . .
C24 C 0.6361(4) 0.6659(4) 0.3565(4) 0.062(3) Uani 1 1 d . . . . .
H24 H 0.649225 0.649708 0.375406 0.075 Uiso 1 1 calc R U . . .
C25 C 0.6520(5) 0.6792(5) 0.3105(4) 0.078(4) Uani 1 1 d . . . . .
H25 H 0.676561 0.672879 0.297907 0.093 Uiso 1 1 calc R U . . .
C26 C 0.6335(6) 0.7017(5) 0.2812(5) 0.093(5) Uani 1 1 d . . . . .
H26 H 0.643924 0.709693 0.248018 0.112 Uiso 1 1 calc R U . . .
C27 C 0.5995(6) 0.7125(5) 0.3009(5) 0.085(4) Uani 1 1 d . . . . .
H27 H 0.587714 0.729829 0.281747 0.102 Uiso 1 1 calc R U . . .
C28 C 0.5820(5) 0.6982(4) 0.3491(4) 0.071(3) Uani 1 1 d . . . . .
H28 H 0.557505 0.704460 0.361995 0.085 Uiso 1 1 calc R U . . .
C29 C 0.5819(4) 0.6121(4) 0.4452(4) 0.049(2) Uani 1 1 d . . . . .
C30 C 0.5496(4) 0.5676(4) 0.4219(4) 0.064(3) Uani 1 1 d . . . . .
H30 H 0.528503 0.567175 0.396738 0.076 Uiso 1 1 calc R U . . .
C31 C 0.5482(5) 0.5246(4) 0.4350(4) 0.072(4) Uani 1 1 d . . . . .
H31 H 0.525385 0.494542 0.419556 0.086 Uiso 1 1 calc R U . . .
C32 C 0.5797(6) 0.5250(5) 0.4703(5) 0.082(4) Uani 1 1 d . . . . .
H32 H 0.579150 0.495390 0.478620 0.099 Uiso 1 1 calc R U . . .
C33 C 0.6121(5) 0.5684(5) 0.4937(5) 0.072(3) Uani 1 1 d . . . . .
H33 H 0.633747 0.568981 0.518412 0.087 Uiso 1 1 calc R U . . .
C34 C 0.6121(4) 0.6109(5) 0.4802(4) 0.063(3) Uani 1 1 d . . . . .
H34 H 0.634456 0.640752 0.496179 0.076 Uiso 1 1 calc R U . . .
C35 C 0.4024(4) 0.5877(4) 0.5587(3) 0.044(2) Uani 1 1 d . . . . .
H35 H 0.437172 0.601722 0.558349 0.053 Uiso 1 1 calc R U . . .
C36 C 0.3688(4) 0.5390(4) 0.5693(4) 0.055(3) Uani 1 1 d . . . . .
H36 H 0.375758 0.513809 0.578303 0.065 Uiso 1 1 calc R U . . .
C37 C 0.4653(3) 0.7885(3) 0.5641(3) 0.042(2) Uani 1 1 d . . . . .
H37 H 0.494808 0.787443 0.567934 0.050 Uiso 1 1 calc R U . . .
C38 C 0.4253(4) 0.5350(4) 0.4519(4) 0.055(3) Uani 1 1 d . . . . .
H38 H 0.458525 0.561052 0.453183 0.066 Uiso 1 1 calc R U . . .
C39 C 0.4104(4) 0.4856(4) 0.4544(5) 0.071(4) Uani 1 1 d . . . . .
H39 H 0.430541 0.471026 0.457314 0.085 Uiso 1 1 calc R U . . .
C40 C 0.3577(4) 0.4610(4) 0.4516(5) 0.059(3) Uani 1 1 d . . . . .
H40 H 0.335974 0.426399 0.453041 0.071 Uiso 1 1 calc R U . . .
C41 C 0.2103(4) 0.3894(4) 0.4229(4) 0.049(2) Uani 1 1 d . . . . .
H41 H 0.192305 0.403800 0.409786 0.059 Uiso 1 1 calc R U . . .
C42 C 0.2154(5) 0.3178(4) 0.4388(5) 0.078(4) Uani 1 1 d . . . . .
H42A H 0.195756 0.282290 0.432935 0.117 Uiso 1 1 calc R U . . .
H42B H 0.247491 0.330834 0.422689 0.117 Uiso 1 1 calc R U . . .
H42C H 0.220189 0.324072 0.474129 0.117 Uiso 1 1 calc R U . . .
C43 C 0.1468(4) 0.3120(4) 0.3914(5) 0.075(4) Uani 1 1 d . . . . .
H43A H 0.137901 0.277369 0.393105 0.113 Uiso 1 1 calc R U . . .
H43B H 0.119890 0.315821 0.404927 0.113 Uiso 1 1 calc R U . . .
H43C H 0.152441 0.322934 0.357124 0.113 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 O2 1.905(6) . ?
Cu1 N2 1.927(8) . ?
Cu1 N1 1.932(8) . ?
Cu1 O4 1.956(2) . ?
Cu2 O7 1.886(7) . ?
Cu2 N3 1.933(8) . ?
Cu2 O3 1.944(6) . ?
Cu2 O5 1.956(7) . ?
Cu3 O7 1.871(7) . ?
Cu3 N4 1.941(8) . ?
Cu3 O9 1.943(7) 3_565 ?
Cu3 O8 1.985(7) . ?
P1 O3 1.500(6) . ?
P1 O9 1.507(7) . ?
P1 O2 1.508(6) . ?
P1 O1 1.609(6) . ?
P2 O5 1.520(6) 3_565 ?
P2 O5 1.520(6) . ?
P2 O5 1.520(6) 2_665 ?
P2 O6 1.573(11) . ?
O1 C1 1.378(10) . ?
O4 H4O 0.83(3) . ?
O7 H7O 0.83(3) . ?
O8 C41 1.232(11) . ?
N1 C35 1.348(11) . ?
N1 N2 1.372(10) 3_565 ?
N2 C37 1.358(11) . ?
N3 C38 1.324(12) . ?
N3 N4 1.383(11) . ?
N4 C40 1.323(12) . ?
N5 C41 1.322(12) . ?
N5 C42 1.413(14) . ?
N5 C43 1.432(13) . ?
C1 C6 1.383(12) . ?
C1 C2 1.390(12) . ?
C2 C3 1.412(13) . ?
C2 C7 1.519(12) . ?
C3 C4 1.384(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(13) . ?
C4 C20 1.543(14) . ?
C5 C6 1.372(13) . ?
C5 H5 0.9500 . ?
C6 C22 1.516(12) . ?
C7 C8 1.516(14) . ?
C7 C14 1.549(13) . ?
C7 H7 1.0000 . ?
C8 C9 1.357(13) . ?
C8 C13 1.364(14) . ?
C9 C10 1.379(15) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(17) . ?
C10 H10 0.9500 . ?
C11 C12 1.378(18) . ?
C11 H11 0.9500 . ?
C12 C13 1.387(17) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.375(15) . ?
C14 C15 1.379(13) . ?
C15 C16 1.405(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.336(18) . ?
C16 H16 0.9500 . ?
C17 C18 1.323(16) . ?
C17 H17 0.9500 . ?
C18 C19 1.377(15) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.455(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.530(13) . ?
C22 C29 1.537(14) . ?
C22 H22 1.0000 . ?
C23 C24 1.390(14) . ?
C23 C28 1.393(15) . ?
C24 C25 1.334(15) . ?
C24 H24 0.9500 . ?
C25 C26 1.37(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.38(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.406(17) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.359(15) . ?
C29 C30 1.401(15) . ?
C30 C31 1.374(16) . ?
C30 H30 0.9500 . ?
C31 C32 1.374(19) . ?
C31 H31 0.9500 . ?
C32 C33 1.382(18) . ?
C32 H32 0.9500 . ?
C33 C34 1.383(16) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.387(14) . ?
C35 H35 0.9500 . ?
C36 C37 1.376(13) 3_565 ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.381(15) . ?
C38 H38 0.9500 . ?
C39 C40 1.435(15) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 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
O2 Cu1 N2 91.4(3) . . ?
O2 Cu1 N1 94.6(3) . . ?
N2 Cu1 N1 163.6(3) . . ?
O2 Cu1 O4 174.6(3) . . ?
N2 Cu1 O4 87.0(2) . . ?
N1 Cu1 O4 88.3(2) . . ?
O7 Cu2 N3 85.4(3) . . ?
O7 Cu2 O3 175.7(3) . . ?
N3 Cu2 O3 92.7(3) . . ?
O7 Cu2 O5 91.3(3) . . ?
N3 Cu2 O5 176.7(3) . . ?
O3 Cu2 O5 90.6(3) . . ?
O7 Cu3 N4 86.3(3) . . ?
O7 Cu3 O9 95.6(3) . 3_565 ?
N4 Cu3 O9 175.3(4) . 3_565 ?
O7 Cu3 O8 170.3(3) . . ?
N4 Cu3 O8 88.5(3) . . ?
O9 Cu3 O8 90.2(3) 3_565 . ?
O3 P1 O9 114.1(4) . . ?
O3 P1 O2 114.1(4) . . ?
O9 P1 O2 112.7(4) . . ?
O3 P1 O1 105.1(3) . . ?
O9 P1 O1 106.0(4) . . ?
O2 P1 O1 103.5(4) . . ?
O5 P2 O5 111.2(3) 3_565 . ?
O5 P2 O5 111.2(3) 3_565 2_665 ?
O5 P2 O5 111.2(3) . 2_665 ?
O5 P2 O6 107.7(3) 3_565 . ?
O5 P2 O6 107.7(3) . . ?
O5 P2 O6 107.7(3) 2_665 . ?
C1 O1 P1 126.6(6) . . ?
P1 O2 Cu1 136.2(4) . . ?
P1 O3 Cu2 135.9(4) . . ?
Cu1 O4 Cu1 116.03(19) 2_665 3_565 ?
Cu1 O4 Cu1 116.03(19) 2_665 . ?
Cu1 O4 Cu1 116.03(19) 3_565 . ?
Cu1 O4 H4O 101.6(3) 2_665 . ?
Cu1 O4 H4O 101.6(3) 3_565 . ?
Cu1 O4 H4O 101.7(3) . . ?
P2 O5 Cu2 133.5(4) . . ?
Cu2 O7 Cu3 126.1(4) . . ?
Cu2 O7 H7O 113(8) . . ?
Cu3 O7 H7O 119(8) . . ?
C41 O8 Cu3 123.1(7) . . ?
P1 O9 Cu3 126.3(4) . 2_665 ?
C35 N1 N2 107.8(8) . 3_565 ?
C35 N1 Cu1 132.4(6) . . ?
N2 N1 Cu1 119.3(5) 3_565 . ?
C37 N2 N1 107.8(7) . 2_665 ?
C37 N2 Cu1 131.2(7) . . ?
N1 N2 Cu1 121.0(5) 2_665 . ?
C38 N3 N4 108.4(8) . . ?
C38 N3 Cu2 130.0(7) . . ?
N4 N3 Cu2 121.6(6) . . ?
C40 N4 N3 108.9(8) . . ?
C40 N4 Cu3 131.5(7) . . ?
N3 N4 Cu3 119.5(6) . . ?
C41 N5 C42 120.3(9) . . ?
C41 N5 C43 121.4(10) . . ?
C42 N5 C43 118.0(9) . . ?
O1 C1 C6 120.0(8) . . ?
O1 C1 C2 119.6(7) . . ?
C6 C1 C2 120.3(8) . . ?
C1 C2 C3 119.2(8) . . ?
C1 C2 C7 120.6(8) . . ?
C3 C2 C7 120.2(8) . . ?
C4 C3 C2 120.6(9) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 118.2(9) . . ?
C3 C4 C20 121.7(9) . . ?
C5 C4 C20 120.0(9) . . ?
C6 C5 C4 122.1(9) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C5 C6 C1 119.5(8) . . ?
C5 C6 C22 121.8(8) . . ?
C1 C6 C22 118.6(8) . . ?
C8 C7 C2 112.5(8) . . ?
C8 C7 C14 114.5(8) . . ?
C2 C7 C14 111.4(8) . . ?
C8 C7 H7 105.9 . . ?
C2 C7 H7 105.9 . . ?
C14 C7 H7 105.9 . . ?
C9 C8 C13 118.4(10) . . ?
C9 C8 C7 119.4(9) . . ?
C13 C8 C7 122.2(9) . . ?
C8 C9 C10 123.4(11) . . ?
C8 C9 H9 118.3 . . ?
C10 C9 H9 118.3 . . ?
C9 C10 C11 118.4(11) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
C12 C11 C10 118.3(11) . . ?
C12 C11 H11 120.9 . . ?
C10 C11 H11 120.9 . . ?
C11 C12 C13 121.8(12) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C8 C13 C12 119.6(11) . . ?
C8 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C19 C14 C15 118.2(10) . . ?
C19 C14 C7 119.2(8) . . ?
C15 C14 C7 122.6(9) . . ?
C14 C15 C16 118.9(11) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C17 C16 C15 121.4(12) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C18 C17 C16 119.3(12) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 122.1(12) . . ?
C17 C18 H18 119.0 . . ?
C19 C18 H18 119.0 . . ?
C14 C19 C18 120.0(11) . . ?
C14 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C4 113.8(12) . . ?
C21 C20 H20A 108.8 . . ?
C4 C20 H20A 108.8 . . ?
C21 C20 H20B 108.8 . . ?
C4 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C6 C22 C23 113.1(8) . . ?
C6 C22 C29 111.8(8) . . ?
C23 C22 C29 111.8(8) . . ?
C6 C22 H22 106.6 . . ?
C23 C22 H22 106.6 . . ?
C29 C22 H22 106.6 . . ?
C24 C23 C28 117.8(10) . . ?
C24 C23 C22 123.5(10) . . ?
C28 C23 C22 118.7(9) . . ?
C25 C24 C23 122.5(12) . . ?
C25 C24 H24 118.8 . . ?
C23 C24 H24 118.8 . . ?
C24 C25 C26 121.2(14) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C25 C26 C27 118.5(12) . . ?
C25 C26 H26 120.7 . . ?
C27 C26 H26 120.7 . . ?
C26 C27 C28 120.7(13) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C23 C28 C27 119.2(13) . . ?
C23 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C34 C29 C30 117.1(11) . . ?
C34 C29 C22 124.1(10) . . ?
C30 C29 C22 118.8(9) . . ?
C31 C30 C29 121.0(12) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C32 C31 C30 120.0(13) . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C32 C33 120.3(13) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C32 C33 C34 118.1(12) . . ?
C32 C33 H33 120.9 . . ?
C34 C33 H33 120.9 . . ?
C29 C34 C33 123.4(12) . . ?
C29 C34 H34 118.3 . . ?
C33 C34 H34 118.3 . . ?
N1 C35 C36 109.6(9) . . ?
N1 C35 H35 125.2 . . ?
C36 C35 H35 125.2 . . ?
C37 C36 C35 105.4(8) 3_565 . ?
C37 C36 H36 127.3 3_565 . ?
C35 C36 H36 127.3 . . ?
N2 C37 C36 109.5(8) . 2_665 ?
N2 C37 H37 125.3 . . ?
C36 C37 H37 125.3 2_665 . ?
N3 C38 C39 109.9(9) . . ?
N3 C38 H38 125.0 . . ?
C39 C38 H38 125.0 . . ?
C38 C39 C40 104.7(9) . . ?
C38 C39 H39 127.6 . . ?
C40 C39 H39 127.6 . . ?
N4 C40 C39 108.0(10) . . ?
N4 C40 H40 126.0 . . ?
C39 C40 H40 126.0 . . ?
O8 C41 N5 124.3(10) . . ?
O8 C41 H41 117.9 . . ?
N5 C41 H41 117.9 . . ?
N5 C42 H42A 109.5 . . ?
N5 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N5 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C43 H43A 109.5 . . ?
N5 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N5 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?

_refine_diff_density_max         0.696
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.084

