# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

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

data_I
_database_code_depnum_ccdc_archive 'CCDC 1054267'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_audit_creation_date             2015-03-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H48 O8, C5 H5 N O, 3(H2 O)'
_chemical_formula_sum            'C45 H59 N O12'
_chemical_formula_weight         805.93
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.163(2)
_cell_length_b                   12.581(3)
_cell_length_c                   15.876(3)
_cell_angle_alpha                71.47(3)
_cell_angle_beta                 73.69(3)
_cell_angle_gamma                69.55(3)
_cell_volume                     2118.4(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    170
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0884 before and 0.0708 after correction.
The Ratio of minimum to maximum transmission is 0.7259.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19133
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.092
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4264
_reflns_number_total             7571
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         7571
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1700
_refine_ls_R_factor_gt           0.0980
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0692P)²+7.5823P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2383
_refine_ls_wR_factor_ref         0.2734
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O12(0.5) O13(0.5)
3.a Riding coordinates:
 O6(H6A), O2(H2), O10(H10D,H10E), O7(H7), O1(H1), O11(H11A,H11B), O3(H3),
 O8(H8A), O4(H4), O5(H5), O13(H12A,H12B)
3.b Ternary CH refined with riding coordinates:
 C8(H8), C18(H18), C28(H28), C38(H38)
3.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C19(H19A,H19B), C29(H29A,H29B), C39(H39A,H39B)
3.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C26(H26), C36(H36), C41(H41), C42(H42), C43(H43), C44(H44),
 C45(H45)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C20(H20A,H20B,
 H20C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C40(H40A,
 H40B,H40C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9051(5) 0.0429(5) 0.1477(4) 0.0332(13) Uani 1 1 d . . . . .
C2 C 0.9484(5) -0.0621(5) 0.2104(4) 0.0331(13) Uani 1 1 d . . . . .
C3 C 0.8755(5) -0.1329(5) 0.2643(4) 0.0344(13) Uani 1 1 d . . . . .
C4 C 0.7561(5) -0.0960(5) 0.2564(4) 0.0337(13) Uani 1 1 d . . . . .
C5 C 0.7084(5) 0.0083(5) 0.1951(4) 0.0327(13) Uani 1 1 d . . . . .
C6 C 0.7844(5) 0.0753(5) 0.1444(4) 0.0343(13) Uani 1 1 d . . . . .
H6 H 0.7523 0.1478 0.1049 0.041 Uiso 1 1 calc R . . . .
C7 C 0.9263(5) -0.2468(5) 0.3292(4) 0.0421(15) Uani 1 1 d . . . . .
H7A H 0.9984 -0.2936 0.2968 0.063 Uiso 1 1 calc GR . . . .
H7B H 0.8668 -0.2903 0.3547 0.063 Uiso 1 1 calc GR . . . .
H7C H 0.9466 -0.2299 0.3782 0.063 Uiso 1 1 calc GR . . . .
C8 C 0.5779(5) 0.0460(5) 0.1873(4) 0.0341(13) Uani 1 1 d . . . . .
H8 H 0.5501 -0.0258 0.2116 0.041 Uiso 1 1 calc R . . . .
C9 C 0.5605(5) 0.0950(5) 0.0883(4) 0.0445(15) Uani 1 1 d . . . . .
H9A H 0.4744 0.1170 0.0872 0.053 Uiso 1 1 calc R . . . .
H9B H 0.5869 0.1668 0.0621 0.053 Uiso 1 1 calc R . . . .
C10 C 0.6293(6) 0.0087(6) 0.0296(5) 0.062(2) Uani 1 1 d . . . . .
H10A H 0.6113 0.0429 -0.0314 0.093 Uiso 1 1 calc GR . . . .
H10B H 0.6057 -0.0637 0.0562 0.093 Uiso 1 1 calc GR . . . .
H10C H 0.7153 -0.0087 0.0264 0.093 Uiso 1 1 calc GR . . . .
C11 C 0.5022(5) 0.1298(5) 0.2473(4) 0.0326(13) Uani 1 1 d . . . . .
C12 C 0.4489(5) 0.0892(5) 0.3357(4) 0.0356(13) Uani 1 1 d . . . . .
C13 C 0.3807(5) 0.1637(5) 0.3938(4) 0.0350(13) Uani 1 1 d . . . . .
C14 C 0.3663(5) 0.2832(5) 0.3577(4) 0.0331(13) Uani 1 1 d . . . . .
C15 C 0.4168(5) 0.3288(5) 0.2690(4) 0.0331(13) Uani 1 1 d . . . . .
C16 C 0.4865(5) 0.2503(5) 0.2157(4) 0.0339(13) Uani 1 1 d . . . . .
H16 H 0.5245 0.2799 0.1560 0.041 Uiso 1 1 calc R . . . .
C17 C 0.3209(5) 0.1181(5) 0.4872(4) 0.0460(15) Uani 1 1 d . . . . .
H17A H 0.3205 0.1642 0.5268 0.069 Uiso 1 1 calc GR . . . .
H17B H 0.3642 0.0360 0.5094 0.069 Uiso 1 1 calc GR . . . .
H17C H 0.2384 0.1239 0.4871 0.069 Uiso 1 1 calc GR . . . .
C18 C 0.3932(5) 0.4605(5) 0.2301(4) 0.0366(13) Uani 1 1 d . . . . .
H18 H 0.3151 0.4982 0.2657 0.044 Uiso 1 1 calc R . . . .
C19 C 0.3786(6) 0.4992(5) 0.1313(4) 0.0447(15) Uani 1 1 d . . . . .
H19A H 0.4562 0.4685 0.0931 0.054 Uiso 1 1 calc R . . . .
H19B H 0.3203 0.4648 0.1252 0.054 Uiso 1 1 calc R . . . .
C20 C 0.3364(7) 0.6312(6) 0.0972(5) 0.065(2) Uani 1 1 d . . . . .
H20A H 0.3227 0.6510 0.0354 0.097 Uiso 1 1 calc GR . . . .
H20B H 0.3974 0.6652 0.0975 0.097 Uiso 1 1 calc GR . . . .
H20C H 0.2617 0.6626 0.1366 0.097 Uiso 1 1 calc GR . . . .
C21 C 0.4861(5) 0.5037(4) 0.2446(4) 0.0332(13) Uani 1 1 d . . . . .
C22 C 0.4668(5) 0.5506(5) 0.3192(4) 0.0340(13) Uani 1 1 d . . . . .
C23 C 0.5513(5) 0.5916(5) 0.3319(4) 0.0358(13) Uani 1 1 d . . . . .
C24 C 0.6593(5) 0.5820(5) 0.2723(4) 0.0368(14) Uani 1 1 d . . . . .
C25 C 0.6835(5) 0.5374(4) 0.1967(4) 0.0336(13) Uani 1 1 d . . . . .
C26 C 0.5961(5) 0.4975(5) 0.1863(4) 0.0353(13) Uani 1 1 d . . . . .
H26 H 0.6126 0.4641 0.1366 0.042 Uiso 1 1 calc R . . . .
C27 C 0.5266(6) 0.6419(6) 0.4140(4) 0.0477(16) Uani 1 1 d . . . . .
H27A H 0.4803 0.7245 0.4000 0.072 Uiso 1 1 calc GR . . . .
H27B H 0.6026 0.6351 0.4281 0.072 Uiso 1 1 calc GR . . . .
H27C H 0.4811 0.5983 0.4663 0.072 Uiso 1 1 calc GR . . . .
C28 C 0.8015(5) 0.5312(5) 0.1301(4) 0.0352(13) Uani 1 1 d . . . . .
H28 H 0.8348 0.5892 0.1377 0.042 Uiso 1 1 calc R . . . .
C29 C 0.7865(5) 0.5684(5) 0.0304(4) 0.0441(15) Uani 1 1 d . . . . .
H29A H 0.8663 0.5604 -0.0094 0.053 Uiso 1 1 calc R . . . .
H29B H 0.7503 0.5150 0.0207 0.053 Uiso 1 1 calc R . . . .
C30 C 0.7089(6) 0.6935(5) 0.0034(5) 0.0542(18) Uani 1 1 d . . . . .
H30A H 0.6996 0.7111 -0.0594 0.081 Uiso 1 1 calc GR . . . .
H30B H 0.7470 0.7474 0.0088 0.081 Uiso 1 1 calc GR . . . .
H30C H 0.6302 0.7026 0.0433 0.081 Uiso 1 1 calc GR . . . .
C31 C 0.8927(5) 0.4127(5) 0.1509(4) 0.0322(12) Uani 1 1 d . . . . .
C32 C 0.9760(5) 0.3893(5) 0.2039(4) 0.0344(13) Uani 1 1 d . . . . .
C33 C 1.0648(5) 0.2820(5) 0.2190(4) 0.0329(13) Uani 1 1 d . . . . .
C34 C 1.0639(5) 0.1939(4) 0.1826(4) 0.0322(13) Uani 1 1 d . . . . .
C35 C 0.9813(5) 0.2125(4) 0.1308(4) 0.0309(12) Uani 1 1 d . . . . .
C36 C 0.8966(5) 0.3212(5) 0.1165(4) 0.0331(13) Uani 1 1 d . . . . .
H36 H 0.8389 0.3342 0.0819 0.040 Uiso 1 1 calc R . . . .
C37 C 1.1592(5) 0.2624(5) 0.2703(4) 0.0431(15) Uani 1 1 d . . . . .
H37A H 1.1667 0.3379 0.2691 0.065 Uiso 1 1 calc GR . . . .
H37B H 1.2358 0.2158 0.2422 0.065 Uiso 1 1 calc GR . . . .
H37C H 1.1370 0.2205 0.3331 0.065 Uiso 1 1 calc GR . . . .
C38 C 0.9841(5) 0.1188(5) 0.0873(4) 0.0321(12) Uani 1 1 d . . . . .
H38 H 1.0680 0.0665 0.0804 0.039 Uiso 1 1 calc R . . . .
C39 C 0.9544(5) 0.1709(5) -0.0081(4) 0.0380(14) Uani 1 1 d . . . . .
H39A H 0.9585 0.1067 -0.0332 0.046 Uiso 1 1 calc R . . . .
H39B H 0.8716 0.2231 -0.0037 0.046 Uiso 1 1 calc R . . . .
C40 C 1.0383(6) 0.2391(5) -0.0719(4) 0.0480(16) Uani 1 1 d . . . . .
H40A H 1.0164 0.2690 -0.1318 0.072 Uiso 1 1 calc GR . . . .
H40B H 1.1205 0.1877 -0.0768 0.072 Uiso 1 1 calc GR . . . .
H40C H 1.0323 0.3047 -0.0487 0.072 Uiso 1 1 calc GR . . . .
O9 O 0.9448(4) 0.2576(5) 0.4853(3) 0.0670(14) Uani 1 1 d . . . . .
N1 N 0.8853(5) 0.2301(5) 0.4394(4) 0.0504(14) Uani 1 1 d . . . . .
C41 C 0.9334(7) 0.1260(6) 0.4173(5) 0.0609(19) Uani 1 1 d . . . . .
H41 H 1.0084 0.0759 0.4314 0.073 Uiso 1 1 calc R . . . .
C42 C 0.8715(9) 0.0947(8) 0.3741(6) 0.077(2) Uani 1 1 d . . . . .
H42 H 0.9037 0.0215 0.3585 0.092 Uiso 1 1 calc R . . . .
C43 C 0.7642(9) 0.1665(9) 0.3530(5) 0.078(3) Uani 1 1 d . . . . .
H43 H 0.7212 0.1433 0.3238 0.094 Uiso 1 1 calc R . . . .
C44 C 0.7194(8) 0.2728(7) 0.3746(5) 0.072(2) Uani 1 1 d . . . . .
H44 H 0.6458 0.3249 0.3590 0.086 Uiso 1 1 calc R . . . .
C45 C 0.7812(6) 0.3037(6) 0.4190(5) 0.0587(19) Uani 1 1 d . . . . .
H45 H 0.7502 0.3767 0.4349 0.070 Uiso 1 1 calc R . . . .
O6 O 0.7448(4) 0.6182(4) 0.2885(3) 0.0531(12) Uani 1 1 d . . . . .
H6A H 0.8204 0.5819 0.2747 0.064 Uiso 1 1 d R . . . .
O2 O 0.6829(3) -0.1651(3) 0.3098(3) 0.0431(10) Uani 1 1 d . . . . .
H2 H 0.6144 -0.1255 0.3267 0.052 Uiso 1 1 d R . . . .
O10 O 0.1911(4) 0.7654(4) 0.3521(3) 0.0499(11) Uani 1 1 d . . . . .
H10D H 0.1364 0.7565 0.4010 0.060 Uiso 1 1 d R . . . .
H10E H 0.2469 0.7006 0.3576 0.060 Uiso 1 1 d R . . . .
O7 O 0.9726(3) 0.4763(3) 0.2414(3) 0.0438(10) Uani 1 1 d . . . . .
H7 H 0.9870 0.4595 0.2954 0.053 Uiso 1 1 d R . . . .
O1 O 1.0670(3) -0.0957(3) 0.2148(3) 0.0424(10) Uani 1 1 d . . . . .
H1 H 1.1111 -0.1504 0.2491 0.051 Uiso 1 1 d R . . . .
O11 O 0.7585(4) 0.0384(4) 0.6430(4) 0.0699(15) Uani 1 1 d . . . . .
H11A H 0.7649 0.1055 0.6539 0.084 Uiso 1 1 d R . . . .
H11B H 0.7753 -0.0177 0.6983 0.084 Uiso 1 1 d R . . . .
O3 O 0.4605(3) -0.0301(3) 0.3714(3) 0.0417(10) Uani 1 1 d . . . . .
H3 H 0.3953 -0.0445 0.3728 0.050 Uiso 1 1 d R . . . .
O8 O 1.1502(3) 0.0888(3) 0.1985(3) 0.0452(11) Uani 1 1 d . . . . .
H8A H 1.1306 0.0277 0.1976 0.054 Uiso 1 1 d R . . . .
O4 O 0.2989(4) 0.3584(3) 0.4132(3) 0.0451(10) Uani 1 1 d . . . . .
H4 H 0.2312 0.3806 0.4431 0.054 Uiso 1 1 d R . . . .
O5 O 0.3593(3) 0.5574(3) 0.3809(3) 0.0415(10) Uani 1 1 d . . . . .
H5 H 0.3365 0.4988 0.3913 0.050 Uiso 1 1 d R . . . .
O12 O 0.0363(8) 0.4349(9) 0.4060(8) 0.053(3) Uani 0.5 1 d . . P A 2
O13 O 0.0740(11) 0.4251(11) 0.4483(9) 0.079(4) Uani 0.5 1 d . . P B 1
H12A H 0.0440 0.3670 0.4454 0.095 Uiso 1 1 d R . . . .
H12B H -0.0124 0.4789 0.4411 0.095 Uiso 1 1 d R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.409(8) . ?
C1 C6 1.392(7) . ?
C1 C38 1.515(8) . ?
C2 C3 1.398(8) . ?
C2 O1 1.370(6) . ?
C3 C4 1.390(7) . ?
C3 C7 1.516(8) . ?
C4 C5 1.406(7) . ?
C4 O2 1.385(7) . ?
C5 C6 1.381(8) . ?
C5 C8 1.519(7) . ?
C8 C9 1.540(8) . ?
C8 C11 1.527(7) . ?
C9 C10 1.522(9) . ?
C11 C12 1.384(8) . ?
C11 C16 1.399(7) . ?
C12 C13 1.412(8) . ?
C12 O3 1.397(6) . ?
C13 C14 1.395(8) . ?
C13 C17 1.484(8) . ?
C14 C15 1.391(8) . ?
C14 O4 1.389(6) . ?
C15 C16 1.397(7) . ?
C15 C18 1.525(8) . ?
C18 C19 1.530(8) . ?
C18 C21 1.509(7) . ?
C19 C20 1.518(9) . ?
C21 C22 1.412(8) . ?
C21 C26 1.390(8) . ?
C22 C23 1.384(7) . ?
C22 O5 1.390(6) . ?
C23 C24 1.379(8) . ?
C23 C27 1.538(8) . ?
C24 C25 1.399(8) . ?
C24 O6 1.382(6) . ?
C25 C26 1.389(7) . ?
C25 C28 1.518(8) . ?
C28 C29 1.546(8) . ?
C28 C31 1.517(7) . ?
C29 C30 1.520(8) . ?
C31 C32 1.390(7) . ?
C31 C36 1.404(7) . ?
C32 C33 1.403(7) . ?
C32 O7 1.386(6) . ?
C33 C34 1.407(7) . ?
C33 C37 1.497(7) . ?
C34 C35 1.384(7) . ?
C34 O8 1.372(6) . ?
C35 C36 1.390(7) . ?
C35 C38 1.532(7) . ?
C38 C39 1.537(8) . ?
C39 C40 1.510(8) . ?
O9 N1 1.342(7) . ?
N1 C41 1.350(8) . ?
N1 C45 1.337(8) . ?
C41 C42 1.365(11) . ?
C42 C43 1.364(12) . ?
C43 C44 1.372(11) . ?
C44 C45 1.374(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C38 122.5(5) . . ?
C6 C1 C2 116.6(5) . . ?
C6 C1 C38 120.9(5) . . ?
C3 C2 C1 122.0(5) . . ?
O1 C2 C1 117.6(5) . . ?
O1 C2 C3 120.3(5) . . ?
C2 C3 C7 120.4(5) . . ?
C4 C3 C2 118.2(5) . . ?
C4 C3 C7 121.4(5) . . ?
C3 C4 C5 122.0(5) . . ?
O2 C4 C3 118.7(5) . . ?
O2 C4 C5 119.3(5) . . ?
C4 C5 C8 120.9(5) . . ?
C6 C5 C4 117.2(5) . . ?
C6 C5 C8 121.9(5) . . ?
C5 C6 C1 123.9(5) . . ?
C5 C8 C9 112.4(5) . . ?
C5 C8 C11 110.6(4) . . ?
C11 C8 C9 113.0(4) . . ?
C10 C9 C8 113.2(5) . . ?
C12 C11 C8 121.4(5) . . ?
C12 C11 C16 117.3(5) . . ?
C16 C11 C8 121.3(5) . . ?
C11 C12 C13 123.0(5) . . ?
C11 C12 O3 120.3(5) . . ?
O3 C12 C13 116.7(5) . . ?
C12 C13 C17 121.7(5) . . ?
C14 C13 C12 116.9(5) . . ?
C14 C13 C17 121.3(5) . . ?
C15 C14 C13 122.5(5) . . ?
O4 C14 C13 118.0(5) . . ?
O4 C14 C15 119.4(5) . . ?
C14 C15 C16 117.9(5) . . ?
C14 C15 C18 121.1(5) . . ?
C16 C15 C18 121.0(5) . . ?
C15 C16 C11 122.4(5) . . ?
C15 C18 C19 112.9(5) . . ?
C21 C18 C15 111.3(4) . . ?
C21 C18 C19 112.5(5) . . ?
C20 C19 C18 112.8(5) . . ?
C22 C21 C18 121.8(5) . . ?
C26 C21 C18 121.9(5) . . ?
C26 C21 C22 116.3(5) . . ?
C23 C22 C21 121.9(5) . . ?
C23 C22 O5 119.0(5) . . ?
O5 C22 C21 119.1(5) . . ?
C22 C23 C27 120.2(5) . . ?
C24 C23 C22 119.1(5) . . ?
C24 C23 C27 120.7(5) . . ?
C23 C24 C25 121.7(5) . . ?
C23 C24 O6 118.3(5) . . ?
O6 C24 C25 120.0(5) . . ?
C24 C25 C28 120.9(5) . . ?
C26 C25 C24 117.2(5) . . ?
C26 C25 C28 121.9(5) . . ?
C25 C26 C21 123.7(5) . . ?
C25 C28 C29 112.9(5) . . ?
C31 C28 C25 112.4(5) . . ?
C31 C28 C29 111.5(5) . . ?
C30 C29 C28 113.0(5) . . ?
C32 C31 C28 122.3(5) . . ?
C32 C31 C36 117.0(5) . . ?
C36 C31 C28 120.8(5) . . ?
C31 C32 C33 122.4(5) . . ?
O7 C32 C31 118.7(5) . . ?
O7 C32 C33 118.9(5) . . ?
C32 C33 C34 117.8(5) . . ?
C32 C33 C37 121.3(5) . . ?
C34 C33 C37 120.9(5) . . ?
C35 C34 C33 121.8(5) . . ?
O8 C34 C33 117.5(5) . . ?
O8 C34 C35 120.7(5) . . ?
C34 C35 C36 118.1(5) . . ?
C34 C35 C38 121.8(5) . . ?
C36 C35 C38 120.1(5) . . ?
C35 C36 C31 122.9(5) . . ?
C1 C38 C35 111.8(4) . . ?
C1 C38 C39 111.7(4) . . ?
C35 C38 C39 112.4(4) . . ?
C40 C39 C38 112.8(5) . . ?
O9 N1 C41 117.6(6) . . ?
C45 N1 O9 120.0(6) . . ?
C45 N1 C41 122.4(6) . . ?
N1 C41 C42 118.2(7) . . ?
C43 C42 C41 121.3(8) . . ?
C42 C43 C44 118.9(8) . . ?
C43 C44 C45 119.8(8) . . ?
N1 C45 C44 119.4(7) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_II
_database_code_depnum_ccdc_archive 'CCDC 1054268'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_audit_creation_date             2015-03-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C40 H48 O8, C6 H5 N O3, 3(O)'
_chemical_formula_sum            'C46 H53 N O14'
_chemical_formula_weight         843.89
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C26 H17 O8 N2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4574(6)
_cell_length_b                   11.5478(6)
_cell_length_c                   17.0220(8)
_cell_angle_alpha                77.408(4)
_cell_angle_beta                 87.270(4)
_cell_angle_gamma                74.490(5)
_cell_volume                     2117.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5449
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.2020
_cell_measurement_theta_min      3.9850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.1527
_exptl_crystal_size_min          0.1224
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13282
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.733
_diffrn_reflns_theta_min         4.004
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    3.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -43.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000   30.0000 32

#__ type_ start__ end____ width___ exp.time_
  3 omega  -49.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000 -120.0000 81

#__ type_ start__ end____ width___ exp.time_
  4 omega  -96.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  125.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega -115.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -57.0000   90.0000 100

#__ type_ start__ end____ width___ exp.time_
  6 omega   80.00  171.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   30.0000  -60.0000 91

#__ type_ start__ end____ width___ exp.time_
  7 omega  111.00  178.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   61.0000  -30.0000 67

#__ type_ start__ end____ width___ exp.time_
  8 omega   53.00  144.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   15.0000   90.0000 91

#__ type_ start__ end____ width___ exp.time_
  9 omega   40.00  109.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -94.0000  -60.0000 69

#__ type_ start__ end____ width___ exp.time_
 10 omega   36.00   98.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -45.0000  -90.0000 62

#__ type_ start__ end____ width___ exp.time_
 11 omega   35.00   87.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -45.0000 -180.0000 52

#__ type_ start__ end____ width___ exp.time_
 12 omega   25.00  109.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -94.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
 13 omega   31.00   91.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -30.0000   30.0000 60

#__ type_ start__ end____ width___ exp.time_
 14 omega   30.00  131.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -77.0000   30.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0822138000
_diffrn_orient_matrix_UB_12      -0.0756418000
_diffrn_orient_matrix_UB_13      -0.0203508000
_diffrn_orient_matrix_UB_21      0.0464136000
_diffrn_orient_matrix_UB_22      0.0164825000
_diffrn_orient_matrix_UB_23      -0.0871040000
_diffrn_orient_matrix_UB_31      0.1027664000
_diffrn_orient_matrix_UB_32      -0.1186939000
_diffrn_orient_matrix_UB_33      0.0244866000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5956
_reflns_number_total             7430
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         7430
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0520
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0853P)²+0.7245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1558
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.02
3. Others
 Sof(O14)=1-FVAR(1)
 Sof(O15)=FVAR(1)
 Fixed Sof: O12(0.5) O13(0.5) O19(0.45) O18(0.3) O16(0.15) O17(0.1)
4.a Riding coordinates:
 O1(H1)
4.b Ternary CH refined with riding coordinates:
 C18(H18), C8(H8A), C38(H38), C28(H28)
4.c Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C9(H9A,H9B), C29(H29A,H29B), C19(H19A,H19B)
4.d Aromatic/amide H refined with riding coordinates:
 C16(H16), C5(H5A), C36(H36), C26(H26), C44(H44), C42(H42), C41(H41), C43(H43)
4.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C40(H40A,H40B,H40C), C17(H17A,H17B,
 H17C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C37(H37A,
 H37B,H37C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
O8 O 0.37517(14) 0.64246(14) 0.28891(10) 0.0270(3) Uani 1 1 d D . . . .
H8 H 0.331(2) 0.7133(18) 0.2788(17) 0.032 Uiso 1 1 d DR . . . .
O2 O 0.52903(13) 1.08794(14) 0.37198(9) 0.0225(3) Uani 1 1 d . . . . .
O4 O 1.11159(13) 0.68067(15) 0.33142(10) 0.0276(3) Uani 1 1 d . . . . .
O5 O 1.21847(13) 0.50528(15) 0.23553(10) 0.0278(3) Uani 1 1 d . . . . .
O3 O 0.76898(15) 0.97445(16) 0.40559(9) 0.0304(4) Uani 1 1 d . . . . .
O7 O 0.72972(14) 0.35006(14) 0.23776(10) 0.0281(3) Uani 1 1 d . . . . .
O6 O 0.95505(14) 0.28911(14) 0.16104(11) 0.0300(4) Uani 1 1 d . . . . .
O11 O 0.57517(16) 0.81322(16) 0.50319(10) 0.0358(4) Uani 1 1 d . . . . .
O9 O 0.86345(16) 0.51783(16) 0.54172(10) 0.0379(4) Uani 1 1 d . . . . .
C23 C 1.09105(18) 0.39744(19) 0.19788(13) 0.0227(4) Uani 1 1 d . . . . .
O10 O 0.71901(16) 0.68708(16) 0.58726(9) 0.0344(4) Uani 1 1 d . . . . .
C16 C 0.86456(18) 0.89896(18) 0.20988(12) 0.0185(4) Uani 1 1 d . . . . .
H16 H 0.8403 0.9227 0.1561 0.022 Uiso 1 1 calc R . . . .
C5 C 0.53558(17) 0.94392(17) 0.20276(12) 0.0180(4) Uani 1 1 d . . . . .
H5A H 0.5866 0.9274 0.1601 0.022 Uiso 1 1 calc R . . . .
C2 C 0.38658(18) 0.98723(18) 0.33371(12) 0.0201(4) Uani 1 1 d . . . . .
C36 C 0.58852(18) 0.66121(19) 0.12246(12) 0.0204(4) Uani 1 1 d . . . . .
H36 H 0.5999 0.7162 0.0758 0.024 Uiso 1 1 calc R . . . .
C18 C 1.04971(18) 0.74683(18) 0.16792(12) 0.0195(4) Uani 1 1 d . . . . .
H18 H 1.1343 0.7313 0.1843 0.023 Uiso 1 1 calc R . . . .
N1 N 0.81694(18) 0.56257(18) 0.46672(11) 0.0280(4) Uani 1 1 d . . . . .
C4 C 0.56547(17) 1.01082(17) 0.25389(12) 0.0176(4) Uani 1 1 d . . . . .
C8 C 0.67699(17) 1.06030(18) 0.23905(12) 0.0176(4) Uani 1 1 d . . . . .
H8A H 0.6700 1.1196 0.2735 0.021 Uiso 1 1 calc R . . . .
C12 C 0.83076(19) 0.9199(2) 0.34581(12) 0.0225(4) Uani 1 1 d . . . . .
C26 C 0.92273(18) 0.61644(18) 0.13207(12) 0.0195(4) Uani 1 1 d . . . . .
H26 H 0.8665 0.6897 0.1101 0.023 Uiso 1 1 calc R . . . .
C1 C 0.35869(17) 0.92492(18) 0.27820(13) 0.0200(4) Uani 1 1 d . . . . .
C11 C 0.79199(17) 0.95802(18) 0.26520(12) 0.0181(4) Uani 1 1 d . . . . .
C38 C 0.40378(17) 0.82830(18) 0.15429(12) 0.0193(4) Uani 1 1 d . . . . .
H38 H 0.3217 0.8194 0.1663 0.023 Uiso 1 1 calc R . . . .
C21 C 1.02804(18) 0.62235(18) 0.16683(12) 0.0193(4) Uani 1 1 d . . . . .
C6 C 0.43231(17) 0.90060(17) 0.21281(12) 0.0182(4) Uani 1 1 d . . . . .
C13 C 0.93788(19) 0.8290(2) 0.37002(12) 0.0241(4) Uani 1 1 d . . . . .
C3 C 0.49066(18) 1.02989(18) 0.31972(12) 0.0186(4) Uani 1 1 d . . . . .
C44 C 0.67462(19) 0.70628(19) 0.37313(13) 0.0237(4) Uani 1 1 d . . . . .
H44 H 0.6067 0.7731 0.3620 0.028 Uiso 1 1 calc R . . . .
C39 C 0.40227(18) 0.89773(19) 0.06666(12) 0.0221(4) Uani 1 1 d . . . . .
H39A H 0.3873 0.8471 0.0317 0.026 Uiso 1 1 calc R . . . .
H39B H 0.4811 0.9126 0.0536 0.026 Uiso 1 1 calc R . . . .
C35 C 0.48949(18) 0.69828(18) 0.17079(12) 0.0189(4) Uani 1 1 d . . . . .
C24 C 0.98346(19) 0.39716(19) 0.16289(13) 0.0229(4) Uani 1 1 d . . . . .
C42 C 0.8296(2) 0.5509(2) 0.32965(13) 0.0270(5) Uani 1 1 d . . . . .
H42 H 0.8682 0.5131 0.2890 0.032 Uiso 1 1 calc R . . . .
C15 C 0.97120(18) 0.80655(18) 0.23068(12) 0.0177(4) Uani 1 1 d . . . . .
C32 C 0.65060(19) 0.46465(19) 0.21109(13) 0.0224(4) Uani 1 1 d . . . . .
C34 C 0.47160(18) 0.61242(19) 0.23891(13) 0.0212(4) Uani 1 1 d . . . . .
C25 C 0.89754(18) 0.50604(19) 0.12864(12) 0.0208(4) Uani 1 1 d . . . . .
C9 C 0.68229(18) 1.13032(18) 0.15192(12) 0.0200(4) Uani 1 1 d . . . . .
H9A H 0.7536 1.1615 0.1458 0.024 Uiso 1 1 calc R . . . .
H9B H 0.6903 1.0738 0.1162 0.024 Uiso 1 1 calc R . . . .
C14 C 1.00520(18) 0.77135(19) 0.31219(13) 0.0213(4) Uani 1 1 d . . . . .
C33 C 0.5494(2) 0.49445(19) 0.25906(13) 0.0249(5) Uani 1 1 d . . . . .
C45 C 0.71934(19) 0.6624(2) 0.45103(13) 0.0243(4) Uani 1 1 d . . . . .
C28 C 0.78138(18) 0.50398(19) 0.08972(13) 0.0227(4) Uani 1 1 d . . . . .
H28 H 0.7883 0.4174 0.0900 0.027 Uiso 1 1 calc R . . . .
C31 C 0.67141(18) 0.54525(19) 0.14099(13) 0.0209(4) Uani 1 1 d . . . . .
C22 C 1.11140(18) 0.51102(19) 0.20020(12) 0.0213(4) Uani 1 1 d . . . . .
C41 C 0.8714(2) 0.5070(2) 0.40730(14) 0.0319(5) Uani 1 1 d . . . . .
H41 H 0.9376 0.4386 0.4193 0.038 Uiso 1 1 calc R . . . .
C7 C 0.3103(2) 1.0038(2) 0.40722(14) 0.0273(5) Uani 1 1 d . . . . .
H7A H 0.2605 1.0869 0.3991 0.041 Uiso 1 1 calc GR . . . .
H7B H 0.3621 0.9870 0.4533 0.041 Uiso 1 1 calc GR . . . .
H7C H 0.2597 0.9481 0.4161 0.041 Uiso 1 1 calc GR . . . .
C10 C 0.5705(2) 1.2372(2) 0.12725(13) 0.0266(5) Uani 1 1 d . . . . .
H10A H 0.5842 1.2865 0.0762 0.040 Uiso 1 1 calc GR . . . .
H10B H 0.5549 1.2867 0.1671 0.040 Uiso 1 1 calc GR . . . .
H10C H 0.5021 1.2059 0.1228 0.040 Uiso 1 1 calc GR . . . .
C46 C 0.6645(2) 0.7264(2) 0.51704(13) 0.0279(5) Uani 1 1 d . . . . .
C29 C 0.7702(2) 0.5704(2) 0.00142(13) 0.0274(5) Uani 1 1 d . . . . .
H29A H 0.8472 0.5460 -0.0247 0.033 Uiso 1 1 calc R . . . .
H29B H 0.7511 0.6584 -0.0020 0.033 Uiso 1 1 calc R . . . .
C40 C 0.3050(2) 1.0209(2) 0.05089(14) 0.0310(5) Uani 1 1 d . . . . .
H40A H 0.3047 1.0597 -0.0051 0.046 Uiso 1 1 calc GR . . . .
H40B H 0.3225 1.0734 0.0829 0.046 Uiso 1 1 calc GR . . . .
H40C H 0.2271 1.0069 0.0650 0.046 Uiso 1 1 calc GR . . . .
C43 C 0.7302(2) 0.6515(2) 0.31161(13) 0.0245(4) Uani 1 1 d . . . . .
H43 H 0.7011 0.6818 0.2590 0.029 Uiso 1 1 calc R . . . .
C19 C 1.0335(2) 0.83287(19) 0.08369(13) 0.0241(4) Uani 1 1 d . . . . .
H19A H 0.9517 0.8459 0.0644 0.029 Uiso 1 1 calc R . . . .
H19B H 1.0434 0.9120 0.0881 0.029 Uiso 1 1 calc R . . . .
C17 C 0.9810(2) 0.7996(3) 0.45657(14) 0.0398(6) Uani 1 1 d . . . . .
H17A H 0.9638 0.8741 0.4763 0.060 Uiso 1 1 calc GR . . . .
H17B H 1.0666 0.7621 0.4594 0.060 Uiso 1 1 calc GR . . . .
H17C H 0.9397 0.7440 0.4888 0.060 Uiso 1 1 calc GR . . . .
C20 C 1.1229(2) 0.7823(2) 0.02255(14) 0.0331(5) Uani 1 1 d . . . . .
H20A H 1.1119 0.8415 -0.0276 0.050 Uiso 1 1 calc GR . . . .
H20B H 1.1090 0.7073 0.0146 0.050 Uiso 1 1 calc GR . . . .
H20C H 1.2040 0.7664 0.0422 0.050 Uiso 1 1 calc GR . . . .
C27 C 1.1843(2) 0.2782(2) 0.23169(16) 0.0321(5) Uani 1 1 d . . . . .
H27A H 1.1531 0.2351 0.2792 0.048 Uiso 1 1 calc GR . . . .
H27B H 1.2572 0.2959 0.2451 0.048 Uiso 1 1 calc GR . . . .
H27C H 1.2016 0.2280 0.1922 0.048 Uiso 1 1 calc GR . . . .
C30 C 0.6717(2) 0.5413(2) -0.04276(15) 0.0356(6) Uani 1 1 d . . . . .
H30A H 0.6645 0.5877 -0.0973 0.053 Uiso 1 1 calc GR . . . .
H30B H 0.5958 0.5630 -0.0160 0.053 Uiso 1 1 calc GR . . . .
H30C H 0.6930 0.4550 -0.0427 0.053 Uiso 1 1 calc GR . . . .
C37 C 0.5239(3) 0.4017(2) 0.32968(17) 0.0446(7) Uani 1 1 d . . . . .
H37A H 0.5622 0.3203 0.3219 0.067 Uiso 1 1 calc GR . . . .
H37B H 0.4381 0.4123 0.3344 0.067 Uiso 1 1 calc GR . . . .
H37C H 0.5552 0.4131 0.3779 0.067 Uiso 1 1 calc GR . . . .
O14 O 1.0384(2) 1.0645(2) 0.2666(5) 0.0427(15) Uani 0.825(18) 1 d . . P A 2
H10 H 0.785(3) 0.612(3) 0.586(2) 0.050(9) Uiso 1 1 d . . . . .
H7 H 0.789(3) 0.336(3) 0.203(2) 0.051(9) Uiso 1 1 d . . . . .
H2 H 0.476(3) 1.112(3) 0.409(2) 0.062(10) Uiso 1 1 d . . . . .
H5 H 1.213(3) 0.573(3) 0.252(2) 0.059(10) Uiso 1 1 d . . . . .
H3 H 0.694(3) 1.012(3) 0.3920(19) 0.045(8) Uiso 1 1 d . . . . .
H4 H 1.121(3) 0.640(3) 0.382(2) 0.050(9) Uiso 1 1 d . . . . .
H6 H 1.009(3) 0.229(4) 0.192(2) 0.064(11) Uiso 1 1 d . . . . .
O15 O 1.0563(12) 1.0565(10) 0.2164(19) 0.034(6) Uani 0.175(18) 1 d . . P A 1
O12 O 0.3826(7) 0.5809(9) 0.4744(4) 0.070(2) Uani 0.5 1 d . . P B 1
O1 O 0.25570(13) 0.88217(14) 0.29115(10) 0.0275(3) Uani 1 1 d . . . . .
H1 H 0.1832 0.9377 0.2877 0.033 Uiso 1 1 d R . . . .
O13 O 0.4087(7) 0.5891(9) 0.4471(4) 0.077(3) Uani 0.5 1 d . . P C 2
O19 O 0.8803(4) 1.1876(4) 0.3689(2) 0.0451(10) Uani 0.45 1 d . . P D 1
O18 O 0.7788(6) 1.2543(8) 0.4210(4) 0.0541(19) Uani 0.3 1 d . . P E 2
O16 O 0.9282(12) 1.0690(12) 0.4334(9) 0.048(3) Uani 0.15 1 d . . P F 3
O17 O 0.7204(19) 1.2408(15) 0.4818(13) 0.047(5) Uani 0.1 1 d . . P G 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O8 H8 0.825(17) . ?
O8 C34 1.378(2) . ?
O2 C3 1.374(2) . ?
O2 H2 0.90(4) . ?
O4 C14 1.377(3) . ?
O4 H4 0.89(4) . ?
O5 C22 1.371(3) . ?
O5 H5 0.87(4) . ?
O3 C12 1.380(3) . ?
O3 H3 0.87(3) . ?
O7 C32 1.384(3) . ?
O7 H7 0.89(4) . ?
O6 C24 1.378(3) . ?
O6 H6 0.89(4) . ?
O11 C46 1.216(3) . ?
O9 N1 1.346(2) . ?
C23 C24 1.395(3) . ?
C23 C22 1.401(3) . ?
C23 C27 1.515(3) . ?
O10 C46 1.307(3) . ?
O10 H10 0.99(3) . ?
C16 H16 0.9300 . ?
C16 C11 1.395(3) . ?
C16 C15 1.391(3) . ?
C5 H5A 0.9300 . ?
C5 C4 1.391(3) . ?
C5 C6 1.393(3) . ?
C2 C1 1.400(3) . ?
C2 C3 1.399(3) . ?
C2 C7 1.509(3) . ?
C36 H36 0.9300 . ?
C36 C35 1.397(3) . ?
C36 C31 1.400(3) . ?
C18 H18 0.9800 . ?
C18 C21 1.527(3) . ?
C18 C15 1.524(3) . ?
C18 C19 1.544(3) . ?
N1 C45 1.362(3) . ?
N1 C41 1.354(3) . ?
C4 C8 1.523(3) . ?
C4 C3 1.398(3) . ?
C8 H8A 0.9800 . ?
C8 C11 1.524(3) . ?
C8 C9 1.534(3) . ?
C12 C11 1.401(3) . ?
C12 C13 1.396(3) . ?
C26 H26 0.9300 . ?
C26 C21 1.393(3) . ?
C26 C25 1.394(3) . ?
C1 C6 1.396(3) . ?
C1 O1 1.387(2) . ?
C38 H38 0.9800 . ?
C38 C6 1.528(3) . ?
C38 C39 1.530(3) . ?
C38 C35 1.533(3) . ?
C21 C22 1.401(3) . ?
C13 C14 1.395(3) . ?
C13 C17 1.514(3) . ?
C44 H44 0.9300 . ?
C44 C45 1.382(3) . ?
C44 C43 1.383(3) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.534(3) . ?
C35 C34 1.398(3) . ?
C24 C25 1.401(3) . ?
C42 H42 0.9300 . ?
C42 C41 1.368(3) . ?
C42 C43 1.383(3) . ?
C15 C14 1.401(3) . ?
C32 C33 1.396(3) . ?
C32 C31 1.398(3) . ?
C34 C33 1.394(3) . ?
C25 C28 1.523(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.523(3) . ?
C33 C37 1.500(3) . ?
C45 C46 1.500(3) . ?
C28 H28 0.9800 . ?
C28 C31 1.527(3) . ?
C28 C29 1.525(3) . ?
C41 H41 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.531(3) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C43 H43 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.522(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
O1 H1 0.8991 . ?

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
C34 O8 H8 118(2) . . ?
C3 O2 H2 116(2) . . ?
C14 O4 H4 116(2) . . ?
C22 O5 H5 110(2) . . ?
C12 O3 H3 112(2) . . ?
C32 O7 H7 110(2) . . ?
C24 O6 H6 107(2) . . ?
C24 C23 C22 118.30(19) . . ?
C24 C23 C27 120.96(19) . . ?
C22 C23 C27 120.74(19) . . ?
C46 O10 H10 109.0(19) . . ?
C11 C16 H16 118.2 . . ?
C15 C16 H16 118.2 . . ?
C15 C16 C11 123.66(18) . . ?
C4 C5 H5A 118.7 . . ?
C4 C5 C6 122.67(18) . . ?
C6 C5 H5A 118.7 . . ?
C1 C2 C7 121.50(18) . . ?
C3 C2 C1 117.23(18) . . ?
C3 C2 C7 121.23(18) . . ?
C35 C36 H36 118.5 . . ?
C35 C36 C31 123.06(19) . . ?
C31 C36 H36 118.5 . . ?
C21 C18 H18 107.1 . . ?
C21 C18 C19 112.11(17) . . ?
C15 C18 H18 107.1 . . ?
C15 C18 C21 111.08(16) . . ?
C15 C18 C19 112.08(16) . . ?
C19 C18 H18 107.1 . . ?
O9 N1 C45 120.77(18) . . ?
O9 N1 C41 118.07(19) . . ?
C41 N1 C45 121.14(19) . . ?
C5 C4 C8 120.97(17) . . ?
C5 C4 C3 117.85(18) . . ?
C3 C4 C8 121.18(17) . . ?
C4 C8 H8A 106.9 . . ?
C4 C8 C11 110.84(15) . . ?
C4 C8 C9 112.12(16) . . ?
C11 C8 H8A 106.9 . . ?
C11 C8 C9 112.67(16) . . ?
C9 C8 H8A 106.9 . . ?
O3 C12 C11 122.13(19) . . ?
O3 C12 C13 115.71(18) . . ?
C13 C12 C11 122.08(19) . . ?
C21 C26 H26 118.4 . . ?
C21 C26 C25 123.20(19) . . ?
C25 C26 H26 118.4 . . ?
C6 C1 C2 122.74(18) . . ?
O1 C1 C2 117.95(18) . . ?
O1 C1 C6 119.27(18) . . ?
C16 C11 C8 121.59(17) . . ?
C16 C11 C12 116.78(18) . . ?
C12 C11 C8 121.62(18) . . ?
C6 C38 H38 106.9 . . ?
C6 C38 C39 112.03(16) . . ?
C6 C38 C35 109.67(16) . . ?
C39 C38 H38 106.9 . . ?
C39 C38 C35 114.02(17) . . ?
C35 C38 H38 106.9 . . ?
C26 C21 C18 120.23(18) . . ?
C26 C21 C22 117.64(18) . . ?
C22 C21 C18 122.13(18) . . ?
C5 C6 C1 117.28(18) . . ?
C5 C6 C38 120.27(17) . . ?
C1 C6 C38 122.44(18) . . ?
C12 C13 C17 119.71(19) . . ?
C14 C13 C12 118.46(19) . . ?
C14 C13 C17 121.8(2) . . ?
O2 C3 C2 122.06(18) . . ?
O2 C3 C4 115.72(17) . . ?
C4 C3 C2 122.15(18) . . ?
C45 C44 H44 119.8 . . ?
C45 C44 C43 120.4(2) . . ?
C43 C44 H44 119.8 . . ?
C38 C39 H39A 109.2 . . ?
C38 C39 H39B 109.2 . . ?
C38 C39 C40 112.15(17) . . ?
H39A C39 H39B 107.9 . . ?
C40 C39 H39A 109.2 . . ?
C40 C39 H39B 109.2 . . ?
C36 C35 C38 123.34(18) . . ?
C36 C35 C34 117.41(18) . . ?
C34 C35 C38 119.21(18) . . ?
O6 C24 C23 121.64(19) . . ?
O6 C24 C25 116.14(18) . . ?
C23 C24 C25 122.22(19) . . ?
C41 C42 H42 120.0 . . ?
C41 C42 C43 120.0(2) . . ?
C43 C42 H42 120.0 . . ?
C16 C15 C18 121.96(18) . . ?
C16 C15 C14 117.18(18) . . ?
C14 C15 C18 120.85(18) . . ?
O7 C32 C33 115.56(19) . . ?
O7 C32 C31 122.04(19) . . ?
C33 C32 C31 122.40(19) . . ?
O8 C34 C35 120.49(18) . . ?
O8 C34 C33 117.55(19) . . ?
C33 C34 C35 121.96(19) . . ?
C26 C25 C24 117.10(18) . . ?
C26 C25 C28 121.40(18) . . ?
C24 C25 C28 121.50(18) . . ?
C8 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 C8 112.73(16) . . ?
C10 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
O4 C14 C13 121.88(19) . . ?
O4 C14 C15 116.28(18) . . ?
C13 C14 C15 121.78(19) . . ?
C32 C33 C37 121.0(2) . . ?
C34 C33 C32 118.2(2) . . ?
C34 C33 C37 120.8(2) . . ?
N1 C45 C44 119.1(2) . . ?
N1 C45 C46 120.2(2) . . ?
C44 C45 C46 120.6(2) . . ?
C25 C28 H28 106.0 . . ?
C25 C28 C31 111.10(17) . . ?
C25 C28 C29 112.08(18) . . ?
C31 C28 H28 106.0 . . ?
C29 C28 H28 106.0 . . ?
C29 C28 C31 115.00(17) . . ?
C36 C31 C28 123.80(19) . . ?
C32 C31 C36 116.84(19) . . ?
C32 C31 C28 119.36(18) . . ?
O5 C22 C23 115.56(18) . . ?
O5 C22 C21 122.89(19) . . ?
C23 C22 C21 121.53(19) . . ?
N1 C41 C42 120.4(2) . . ?
N1 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O11 C46 O10 123.0(2) . . ?
O11 C46 C45 119.9(2) . . ?
O10 C46 C45 117.1(2) . . ?
C28 C29 H29A 109.3 . . ?
C28 C29 H29B 109.3 . . ?
C28 C29 C30 111.82(19) . . ?
H29A C29 H29B 107.9 . . ?
C30 C29 H29A 109.3 . . ?
C30 C29 H29B 109.3 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C44 C43 C42 118.9(2) . . ?
C44 C43 H43 120.6 . . ?
C42 C43 H43 120.6 . . ?
C18 C19 H19A 109.0 . . ?
C18 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C20 C19 C18 113.03(18) . . ?
C20 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C1 O1 H1 118.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O8 C34 C33 C32 -177.06(18) . . . . ?
O8 C34 C33 C37 3.8(3) . . . . ?
O3 C12 C11 C16 177.61(18) . . . . ?
O3 C12 C11 C8 -1.6(3) . . . . ?
O3 C12 C13 C14 -179.29(19) . . . . ?
O3 C12 C13 C17 -2.1(3) . . . . ?
O7 C32 C33 C34 174.87(18) . . . . ?
O7 C32 C33 C37 -6.0(3) . . . . ?
O7 C32 C31 C36 -176.59(18) . . . . ?
O7 C32 C31 C28 3.0(3) . . . . ?
O6 C24 C25 C26 178.08(18) . . . . ?
O6 C24 C25 C28 -1.6(3) . . . . ?
O9 N1 C45 C44 179.5(2) . . . . ?
O9 N1 C45 C46 1.9(3) . . . . ?
O9 N1 C41 C42 -178.3(2) . . . . ?
C23 C24 C25 C26 -1.1(3) . . . . ?
C23 C24 C25 C28 179.18(19) . . . . ?
C16 C15 C14 O4 -179.36(17) . . . . ?
C16 C15 C14 C13 -2.2(3) . . . . ?
C5 C4 C8 C11 -76.9(2) . . . . ?
C5 C4 C8 C9 50.0(2) . . . . ?
C5 C4 C3 O2 175.05(17) . . . . ?
C5 C4 C3 C2 -1.9(3) . . . . ?
C2 C1 C6 C5 -1.6(3) . . . . ?
C2 C1 C6 C38 177.63(18) . . . . ?
C36 C35 C34 O8 -179.49(18) . . . . ?
C36 C35 C34 C33 0.6(3) . . . . ?
C18 C21 C22 O5 -0.5(3) . . . . ?
C18 C21 C22 C23 -179.19(18) . . . . ?
C18 C15 C14 O4 -0.4(3) . . . . ?
C18 C15 C14 C13 176.77(18) . . . . ?
N1 C45 C46 O11 -177.8(2) . . . . ?
N1 C45 C46 O10 4.3(3) . . . . ?
C4 C5 C6 C1 -1.1(3) . . . . ?
C4 C5 C6 C38 179.58(17) . . . . ?
C4 C8 C11 C16 98.9(2) . . . . ?
C4 C8 C11 C12 -82.0(2) . . . . ?
C4 C8 C9 C10 57.4(2) . . . . ?
C8 C4 C3 O2 -4.2(3) . . . . ?
C8 C4 C3 C2 178.82(18) . . . . ?
C12 C13 C14 O4 -179.83(19) . . . . ?
C12 C13 C14 C15 3.2(3) . . . . ?
C26 C21 C22 O5 179.56(18) . . . . ?
C26 C21 C22 C23 0.9(3) . . . . ?
C26 C25 C28 C31 -70.8(2) . . . . ?
C26 C25 C28 C29 59.4(2) . . . . ?
C1 C2 C3 O2 -177.43(17) . . . . ?
C1 C2 C3 C4 -0.7(3) . . . . ?
C11 C16 C15 C18 -178.27(18) . . . . ?
C11 C16 C15 C14 0.7(3) . . . . ?
C11 C8 C9 C10 -176.69(17) . . . . ?
C11 C12 C13 C14 -2.7(3) . . . . ?
C11 C12 C13 C17 174.5(2) . . . . ?
C38 C35 C34 O8 2.7(3) . . . . ?
C38 C35 C34 C33 -177.24(18) . . . . ?
C21 C18 C15 C16 -100.6(2) . . . . ?
C21 C18 C15 C14 80.5(2) . . . . ?
C21 C18 C19 C20 -62.0(2) . . . . ?
C21 C26 C25 C24 0.5(3) . . . . ?
C21 C26 C25 C28 -179.75(18) . . . . ?
C6 C5 C4 C8 -177.87(18) . . . . ?
C6 C5 C4 C3 2.8(3) . . . . ?
C6 C38 C39 C40 -61.3(2) . . . . ?
C6 C38 C35 C36 -103.7(2) . . . . ?
C6 C38 C35 C34 74.0(2) . . . . ?
C13 C12 C11 C16 1.2(3) . . . . ?
C13 C12 C11 C8 -177.97(19) . . . . ?
C3 C2 C1 C6 2.5(3) . . . . ?
C3 C2 C1 O1 -179.92(17) . . . . ?
C3 C4 C8 C11 102.4(2) . . . . ?
C3 C4 C8 C9 -130.77(19) . . . . ?
C44 C45 C46 O11 4.6(3) . . . . ?
C44 C45 C46 O10 -173.3(2) . . . . ?
C39 C38 C6 C5 -53.6(2) . . . . ?
C39 C38 C6 C1 127.2(2) . . . . ?
C39 C38 C35 C36 22.9(3) . . . . ?
C39 C38 C35 C34 -159.42(18) . . . . ?
C35 C36 C31 C32 0.7(3) . . . . ?
C35 C36 C31 C28 -178.85(18) . . . . ?
C35 C38 C6 C5 74.1(2) . . . . ?
C35 C38 C6 C1 -105.1(2) . . . . ?
C35 C38 C39 C40 173.42(17) . . . . ?
C35 C34 C33 C32 2.9(3) . . . . ?
C35 C34 C33 C37 -176.3(2) . . . . ?
C24 C23 C22 O5 179.80(18) . . . . ?
C24 C23 C22 C21 -1.5(3) . . . . ?
C24 C25 C28 C31 108.9(2) . . . . ?
C24 C25 C28 C29 -120.9(2) . . . . ?
C15 C16 C11 C8 178.97(17) . . . . ?
C15 C16 C11 C12 -0.2(3) . . . . ?
C15 C18 C21 C26 75.0(2) . . . . ?
C15 C18 C21 C22 -104.9(2) . . . . ?
C15 C18 C19 C20 172.30(18) . . . . ?
C25 C26 C21 C18 179.65(18) . . . . ?
C25 C26 C21 C22 -0.5(3) . . . . ?
C25 C28 C31 C36 104.1(2) . . . . ?
C25 C28 C31 C32 -75.5(2) . . . . ?
C25 C28 C29 C30 165.78(18) . . . . ?
C9 C8 C11 C16 -27.6(2) . . . . ?
C9 C8 C11 C12 151.49(18) . . . . ?
C33 C32 C31 C36 3.0(3) . . . . ?
C33 C32 C31 C28 -177.42(19) . . . . ?
C45 N1 C41 C42 0.5(4) . . . . ?
C45 C44 C43 C42 1.2(3) . . . . ?
C31 C36 C35 C38 175.28(18) . . . . ?
C31 C36 C35 C34 -2.5(3) . . . . ?
C31 C32 C33 C34 -4.7(3) . . . . ?
C31 C32 C33 C37 174.4(2) . . . . ?
C31 C28 C29 C30 -66.1(2) . . . . ?
C22 C23 C24 O6 -177.58(19) . . . . ?
C22 C23 C24 C25 1.6(3) . . . . ?
C41 N1 C45 C44 0.8(3) . . . . ?
C41 N1 C45 C46 -176.8(2) . . . . ?
C41 C42 C43 C44 0.1(3) . . . . ?
C7 C2 C1 C6 -175.35(19) . . . . ?
C7 C2 C1 O1 2.2(3) . . . . ?
C7 C2 C3 O2 0.4(3) . . . . ?
C7 C2 C3 C4 177.19(19) . . . . ?
C29 C28 C31 C36 -24.6(3) . . . . ?
C29 C28 C31 C32 155.87(19) . . . . ?
C43 C44 C45 N1 -1.7(3) . . . . ?
C43 C44 C45 C46 176.0(2) . . . . ?
C43 C42 C41 N1 -0.9(4) . . . . ?
C19 C18 C21 C26 -51.3(2) . . . . ?
C19 C18 C21 C22 128.8(2) . . . . ?
C19 C18 C15 C16 25.7(3) . . . . ?
C19 C18 C15 C14 -153.25(19) . . . . ?
C17 C13 C14 O4 3.0(3) . . . . ?
C17 C13 C14 C15 -173.9(2) . . . . ?
C27 C23 C24 O6 3.1(3) . . . . ?
C27 C23 C24 C25 -177.7(2) . . . . ?
C27 C23 C22 O5 -0.9(3) . . . . ?
C27 C23 C22 C21 177.9(2) . . . . ?
O1 C1 C6 C5 -179.19(17) . . . . ?
O1 C1 C6 C38 0.1(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4 -3 -9 0.0829 -4.0000 -3.0000 -9.0000 0.7389 0.5488 -0.2754
4 4 9 0.0663 4.0000 4.0000 9.0000 -0.8146 -0.5324 0.1567
3 -6 -2 0.1203 3.0000 -6.0000 -2.0000 0.2479 0.2146 0.9715
-4 5 -1 0.1084 -4.0000 5.0000 -1.0000 -0.0290 -0.0161 -1.0290
-6 -3 6 0.0592 -6.0000 -3.0000 6.0000 0.5981 -0.8506 -0.1136
6 2 -6 0.0489 6.0000 2.0000 -6.0000 -0.5225 0.8341 0.2323
3 -1 -10 0.0402 3.0000 -1.0000 -10.0000 0.0325 0.9938 0.1821
-2 0 10 0.0612 -2.0000 -0.0000 10.0000 -0.0391 -0.9639 0.0393
2 0 10 0.0742 2.0000 -0.0000 10.0000 -0.3679 -0.7782 0.4504
5 0 8 0.0672 5.0000 -0.0000 8.0000 -0.5739 -0.4648 0.7097
-4 -7 -5 0.0863 -4.0000 -7.0000 -5.0000 0.9601 0.1345 0.2974
4 7 4 0.0736 4.0000 7.0000 4.0000 -0.9398 -0.0474 -0.3218

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_III
_database_code_depnum_ccdc_archive 'CCDC 1054269'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_audit_creation_date             2015-03-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C5 H5 Cl2 Cu N O'
_chemical_formula_sum            'C5 H5 Cl2 Cu N O'
_chemical_formula_weight         229.54
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   5.8340(12)
_cell_length_b                   13.603(3)
_cell_length_c                   9.863(2)
_cell_angle_alpha                90
_cell_angle_beta                 105.34(3)
_cell_angle_gamma                90
_cell_volume                     754.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1896
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.700
_cell_measurement_theta_min      0.407
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.523
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0874 before and 0.0656 after correction.
The Ratio of minimum to maximum transmission is 0.7174.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.37
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6631
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         2.613
_diffrn_ambient_temperature      123.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1099
_reflns_number_total             1361
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0381
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0227P)²+1.4129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0758
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.26933(9) 0.51673(4) 0.09510(5) 0.01779(17) Uani 1 1 d . . . . .
Cl1 Cl 0.59211(18) 0.42289(8) 0.14135(10) 0.0204(3) Uani 1 1 d . . . . .
Cl2 Cl 0.36427(19) 0.61561(8) 0.28003(10) 0.0222(3) Uani 1 1 d . . . . .
O1 O 0.0349(5) 0.4159(2) -0.0107(3) 0.0197(7) Uani 1 1 d . . . . .
N1 N 0.0786(6) 0.3210(3) -0.0385(3) 0.0160(8) Uani 1 1 d . . . . .
C1 C 0.2243(8) 0.3036(4) -0.1206(4) 0.0207(10) Uani 1 1 d . . . . .
H1 H 0.2900 0.3567 -0.1604 0.025 Uiso 1 1 calc R . . . .
C2 C 0.2775(8) 0.2085(3) -0.1467(4) 0.0213(10) Uani 1 1 d . . . . .
H2 H 0.3849 0.1951 -0.2018 0.026 Uiso 1 1 calc R . . . .
C3 C 0.1726(8) 0.1322(4) -0.0915(4) 0.0262(11) Uani 1 1 d . . . . .
H3 H 0.2074 0.0658 -0.1087 0.031 Uiso 1 1 calc R . . . .
C4 C 0.0169(8) 0.1532(4) -0.0113(4) 0.0251(11) Uani 1 1 d . . . . .
H4 H -0.0570 0.1014 0.0261 0.030 Uiso 1 1 calc R . . . .
C5 C -0.0301(8) 0.2487(3) 0.0141(4) 0.0200(10) Uani 1 1 d . . . . .
H5 H -0.1382 0.2640 0.0681 0.024 Uiso 1 1 calc R . . . .


_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 Cl1 2.2202(12) . ?
Cu1 Cl2 2.2155(12) . ?
Cu1 O1 2.021(3) . ?
Cu1 O1 1.975(3) 3_565 ?
O1 Cu1 1.975(3) 3_565 ?
O1 N1 1.358(4) . ?
N1 C1 1.341(5) . ?
N1 C5 1.346(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.370(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.388(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.364(6) . ?
C5 H5 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Cu1 Cl1 99.57(5) . . ?
O1 Cu1 Cl1 166.43(9) 3_565 . ?
O1 Cu1 Cl1 97.90(9) . . ?
O1 Cu1 Cl2 93.81(9) 3_565 . ?
O1 Cu1 Cl2 145.55(8) . . ?
O1 Cu1 O1 71.76(14) 3_565 . ?
Cu1 O1 Cu1 108.24(14) 3_565 . ?
N1 O1 Cu1 123.5(2) . 3_565 ?
N1 O1 Cu1 127.7(2) . . ?
C1 N1 O1 118.2(3) . . ?
C1 N1 C5 122.8(4) . . ?
C5 N1 O1 119.0(3) . . ?
N1 C1 H1 120.3 . . ?
N1 C1 C2 119.4(4) . . ?
C2 C1 H1 120.3 . . ?
C1 C2 H2 120.4 . . ?
C1 C2 C3 119.2(4) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.6(4) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 119.1(4) . . ?
N1 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_IV
_database_code_depnum_ccdc_archive 'CCDC 1054270'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_audit_creation_date             2015-03-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C10 H10 Cl2 Cu N2 O2, 2(C40 H48 O8), 2(C H4 O), 2(C H3 O)'
_chemical_formula_sum            'C94 H120 Cl2 Cu N2 O22'
_chemical_formula_weight         1764.35
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.163(2)
_cell_length_b                   12.630(3)
_cell_length_c                   16.953(3)
_cell_angle_alpha                105.26(3)
_cell_angle_beta                 101.94(3)
_cell_angle_gamma                97.56(3)
_cell_volume                     2410.0(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0832 before and 0.0714 after correction.
The Ratio of minimum to maximum transmission is 0.8369.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             937
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_unetI/netI     0.1546
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30183
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         2.502
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5243
_reflns_number_total             8720
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         8720
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0765
_refine_ls_restrained_S_all      2.442
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1028P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1979
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H3 of O3, H5 of O5, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H8 of O8, H4 of O4, H15 of O15, All C(H,H,H,H,H,H)
  groups, All Cl(H) groups
2. Restrained distances
 O15-H15
 0.85 with sigma of 0.02
 O5-O6
 0.85 with sigma of 0.02
 H5-O5
 0.85 with sigma of 0.02
 O3-H3
 0.85 with sigma of 0.02
 O10-C47
 1.47 with sigma of 0.02
 H7-O7
 0.85 with sigma of 0.02
 O6-H6
 0.85 with sigma of 0.02
 H8-O8
 0.85 with sigma of 0.02
 H2-O2
 0.85 with sigma of 0.02
 H5-O5
 0.85 with sigma of 0.02
 O11-C47
 1.45 with sigma of 0.02
 O10-C47
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O11) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: O10(0.85) O11(0.15) H47A(0.85) H47B(0.85) H47C(0.85) H47D(0.15)
 H47E(0.15) H47F(0.15)
5.a Me refined with riding coordinates:
 C47(H47A,H47B,H47C), C47(H47D,H47E,H47F)
5.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C46(H46A,H46B,H46C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.0000 1.0000 0.0000 0.0291(2) Uani 1 2 d S T P . .
Cl1 Cl 0.11554(10) 1.03194(11) -0.08128(7) 0.0379(3) Uani 1 1 d . . . . .
H1 H -0.085(5) 1.050(5) 0.225(4) 0.057 Uiso 1 1 d R . . . .
O3 O -0.1715(2) 0.5319(3) 0.3297(2) 0.0311(8) Uani 1 1 d D . . . .
H3 H -0.218(3) 0.477(3) 0.297(3) 0.037 Uiso 1 1 d DR . . . .
O6 O 0.4195(3) 0.8418(3) 0.10996(18) 0.0304(7) Uani 1 1 d D . . . .
O2 O -0.2111(3) 0.7314(3) 0.30118(19) 0.0296(7) Uani 1 1 d D . . . .
H2 H -0.196(4) 0.678(3) 0.319(3) 0.035 Uiso 1 1 d DR . . . .
H6 H 0.373(3) 0.858(4) 0.073(2) 0.035 Uiso 1 1 d DR . . . .
O1 O -0.0481(3) 1.0806(3) 0.2768(2) 0.0287(7) Uani 1 1 d . . . . .
O8 O 0.1380(3) 1.2133(3) 0.26355(19) 0.0289(7) Uani 1 1 d D . . . .
H8 H 0.077(3) 1.185(4) 0.273(3) 0.043 Uiso 1 1 d DR . . . .
O4 O 0.1016(3) 0.3720(3) 0.18967(18) 0.0249(7) Uani 1 1 d . . . . .
H4 H 0.108(4) 0.322(4) 0.207(3) 0.037 Uiso 1 1 d R . . . .
O9 O 0.0875(3) 0.8869(3) 0.0173(2) 0.0378(8) Uani 1 1 d . . . . .
C29 C 0.5411(4) 0.9583(4) 0.3757(3) 0.0235(10) Uani 1 1 d . . . . .
H29A H 0.504(4) 0.941(4) 0.411(3) 0.028 Uiso 1 1 d R . . . .
H29B H 0.592(4) 0.908(4) 0.375(2) 0.028 Uiso 1 1 d R . . . .
C30 C 0.6060(5) 1.0768(5) 0.4151(3) 0.0362(12) Uani 1 1 d . . . . .
H30A H 0.653(5) 1.096(5) 0.384(3) 0.054 Uiso 1 1 d R . . . .
H30B H 0.650(5) 1.092(4) 0.476(4) 0.054 Uiso 1 1 d R . . . .
H30C H 0.558(5) 1.129(5) 0.415(3) 0.054 Uiso 1 1 d R . . . .
C40 C 0.3157(4) 1.2462(4) 0.5146(3) 0.0317(11) Uani 1 1 d . . . . .
H40A H 0.368(4) 1.248(4) 0.481(3) 0.048 Uiso 1 1 d R . . . .
H40B H 0.365(4) 1.270(4) 0.583(3) 0.048 Uiso 1 1 d R . . . .
H40C H 0.269(5) 1.295(5) 0.510(3) 0.048 Uiso 1 1 d R . . . .
C20 C 0.3415(4) 0.4813(4) 0.4193(3) 0.0378(12) Uani 1 1 d . . . . .
H20A H 0.3477 0.4100 0.3817 0.057 Uiso 1 1 calc GR . . . .
H20B H 0.2634 0.4767 0.4268 0.057 Uiso 1 1 calc GR . . . .
H20C H 0.3960 0.4970 0.4743 0.057 Uiso 1 1 calc GR . . . .
C27 C 0.2882(4) 0.6215(4) 0.0132(3) 0.0379(12) Uani 1 1 d . . . . .
H27A H 0.2077 0.6236 -0.0087 0.057 Uiso 1 1 calc GR . . . .
H27B H 0.2996 0.5442 -0.0044 0.057 Uiso 1 1 calc GR . . . .
H27C H 0.3369 0.6683 -0.0091 0.057 Uiso 1 1 calc GR . . . .
C19 C 0.3685(4) 0.5751(4) 0.3807(3) 0.0270(10) Uani 1 1 d . . . . .
H19A H 0.455(4) 0.584(4) 0.374(3) 0.032 Uiso 1 1 d R . . . .
H19B H 0.360(4) 0.640(4) 0.416(3) 0.032 Uiso 1 1 d R . . . .
N1 N 0.0628(3) 0.8189(3) 0.0633(2) 0.0281(9) Uani 1 1 d . . . . .
C46 C 0.3542(5) 0.9027(5) -0.0786(4) 0.0540(16) Uani 1 1 d . . . . .
H46A H 0.3078 0.8825 -0.1370 0.081 Uiso 1 1 calc GR . . . .
H46B H 0.4248 0.8729 -0.0779 0.081 Uiso 1 1 calc GR . . . .
H46C H 0.3736 0.9843 -0.0548 0.081 Uiso 1 1 calc GR . . . .
C10 C 0.0632(5) 0.6702(5) 0.5582(3) 0.0344(12) Uani 1 1 d . . . . .
H10A H 0.073(4) 0.600(5) 0.527(3) 0.052 Uiso 1 1 d R . . . .
H10B H -0.018(5) 0.652(4) 0.564(3) 0.052 Uiso 1 1 d R . . . .
H10C H 0.118(4) 0.695(4) 0.615(3) 0.052 Uiso 1 1 d R . . . .
C17 C -0.1284(4) 0.3453(4) 0.2051(3) 0.0280(11) Uani 1 1 d . . . . .
H17A H -0.145(4) 0.302(4) 0.237(3) 0.042 Uiso 1 1 d R . . . .
H17B H -0.105(4) 0.308(4) 0.166(3) 0.042 Uiso 1 1 d R . . . .
H17C H -0.197(4) 0.379(4) 0.183(3) 0.042 Uiso 1 1 d R . . . .
C7 C -0.2445(4) 0.9033(5) 0.2331(3) 0.0359(12) Uani 1 1 d . . . . .
H7A H -0.259(5) 0.972(5) 0.242(3) 0.054 Uiso 1 1 d R . . . .
H7B H -0.306(5) 0.855(5) 0.242(3) 0.054 Uiso 1 1 d R . . . .
H7C H -0.251(4) 0.873(4) 0.174(4) 0.054 Uiso 1 1 d R . . . .
C26 C 0.3794(3) 0.7418(4) 0.2849(3) 0.0196(9) Uani 1 1 d . . . . .
H26 H 0.402(3) 0.769(3) 0.345(3) 0.024 Uiso 1 1 d R . . . .
C9 C 0.0729(4) 0.7613(4) 0.5150(3) 0.0241(10) Uani 1 1 d . . . . .
H9A H 0.144(4) 0.781(4) 0.516(3) 0.029 Uiso 1 1 d R . . . .
H9B H 0.067(4) 0.839(4) 0.553(3) 0.029 Uiso 1 1 d R . . . .
C3 C -0.1323(4) 0.9056(4) 0.2915(2) 0.0234(10) Uani 1 1 d . . . . .
C39 C 0.2337(4) 1.1334(4) 0.4870(3) 0.0249(10) Uani 1 1 d . . . . .
H39A H 0.275(4) 1.073(4) 0.488(3) 0.030 Uiso 1 1 d R . . . .
H39B H 0.184(4) 1.137(4) 0.524(3) 0.030 Uiso 1 1 d R . . . .
C18 C 0.2864(4) 0.5535(4) 0.2932(3) 0.0226(10) Uani 1 1 d . . . . .
H18 H 0.290(4) 0.483(4) 0.264(3) 0.027 Uiso 1 1 d R . . . .
C24 C 0.3818(4) 0.7728(4) 0.1529(3) 0.0230(10) Uani 1 1 d . . . . .
C28 C 0.4706(3) 0.9360(4) 0.2848(3) 0.0213(9) Uani 1 1 d . . . . .
H28 H 0.533(4) 0.955(4) 0.258(2) 0.026 Uiso 1 1 d R . . . .
C4 C -0.0394(4) 0.9949(4) 0.3142(2) 0.0226(10) Uani 1 1 d . . . . .
C25 C 0.4107(3) 0.8142(4) 0.2409(2) 0.0211(10) Uani 1 1 d . . . . .
C23 C 0.3202(4) 0.6657(4) 0.1096(3) 0.0251(10) Uani 1 1 d . . . . .
C1 C -0.0195(3) 0.8231(3) 0.3879(2) 0.0188(9) Uani 1 1 d . . . . .
C13 C -0.0378(4) 0.4451(4) 0.2585(3) 0.0243(10) Uani 1 1 d . . . . .
C16 C 0.1303(4) 0.6336(4) 0.3546(2) 0.0191(9) Uani 1 1 d . . . . .
H16 H 0.186(4) 0.692(4) 0.386(3) 0.023 Uiso 1 1 d R . . . .
C12 C -0.0623(3) 0.5335(4) 0.3176(3) 0.0233(10) Uani 1 1 d . . . . .
C8 C -0.0088(4) 0.7273(4) 0.4267(3) 0.0221(10) Uani 1 1 d . . . . .
H8A H -0.071(4) 0.707(4) 0.436(3) 0.027 Uiso 1 1 d R . . . .
C15 C 0.1614(4) 0.5465(3) 0.2990(2) 0.0199(9) Uani 1 1 d . . . . .
C33 C 0.2898(4) 1.1396(4) 0.2148(2) 0.0238(10) Uani 1 1 d . . . . .
C2 C -0.1185(3) 0.8180(4) 0.3275(2) 0.0219(10) Uani 1 1 d . . . . .
C14 C 0.0757(4) 0.4552(4) 0.2515(2) 0.0207(9) Uani 1 1 d . . . . .
C31 C 0.3830(3) 1.0123(3) 0.2794(2) 0.0193(9) Uani 1 1 d . . . . .
C42 C -0.0322(5) 0.6465(5) 0.0685(3) 0.0395(13) Uani 1 1 d . . . . .
H42 H -0.070(4) 0.572(5) 0.037(3) 0.047 Uiso 1 1 d R . . . .
C43 C 0.0128(4) 0.6795(4) 0.1552(3) 0.0318(12) Uani 1 1 d . . . . .
H43 H 0.000(4) 0.647(4) 0.187(3) 0.038 Uiso 1 1 d R . . . .
C38 C 0.1583(4) 1.1053(4) 0.3973(2) 0.0202(9) Uani 1 1 d . . . . .
H38 H 0.118(3) 1.165(4) 0.398(2) 0.024 Uiso 1 1 d R . . . .
C11 C 0.0193(3) 0.6293(3) 0.3652(2) 0.0184(9) Uani 1 1 d . . . . .
C21 C 0.3181(3) 0.6319(4) 0.2446(2) 0.0198(9) Uani 1 1 d . . . . .
C41 C -0.0052(5) 0.7178(4) 0.0239(3) 0.0375(12) Uani 1 1 d . . . . .
H41 H -0.038(4) 0.699(4) -0.036(3) 0.045 Uiso 1 1 d R . . . .
C35 C 0.2297(3) 1.0906(3) 0.3320(2) 0.0197(9) Uani 1 1 d . . . . .
C6 C 0.0669(4) 0.9169(3) 0.4103(3) 0.0180(9) Uani 1 1 d . . . . .
H6A H 0.130(4) 0.926(3) 0.453(3) 0.022 Uiso 1 1 d R . . . .
C36 C 0.3094(3) 1.0222(4) 0.3329(3) 0.0207(9) Uani 1 1 d . . . . .
H36 H 0.316(3) 0.979(4) 0.372(3) 0.025 Uiso 1 1 d R . . . .
C22 C 0.2874(4) 0.5977(4) 0.1568(3) 0.0259(10) Uani 1 1 d . . . . .
C5 C 0.0614(3) 1.0036(4) 0.3740(2) 0.0188(9) Uani 1 1 d . . . . .
C44 C 0.0828(4) 0.7827(4) 0.1938(3) 0.0275(11) Uani 1 1 d . . . . .
H44 H 0.117(4) 0.801(4) 0.249(3) 0.033 Uiso 1 1 d R . . . .
C37 C 0.2777(5) 1.1994(5) 0.1490(3) 0.0335(12) Uani 1 1 d . . . . .
H37A H 0.197(5) 1.195(4) 0.124(3) 0.050 Uiso 1 1 d R . . . .
H37B H 0.302(4) 1.166(4) 0.103(3) 0.050 Uiso 1 1 d R . . . .
H37C H 0.310(4) 1.281(5) 0.172(3) 0.050 Uiso 1 1 d R . . . .
C34 C 0.2205(3) 1.1478(3) 0.2711(2) 0.0207(9) Uani 1 1 d . . . . .
C32 C 0.3731(3) 1.0729(3) 0.2212(2) 0.0211(9) Uani 1 1 d . . . . .
C45 C 0.1072(4) 0.8519(4) 0.1474(3) 0.0301(11) Uani 1 1 d . . . . .
H45 H 0.151(4) 0.914(4) 0.165(3) 0.036 Uiso 1 1 d R . . . .
O7 O 0.4440(3) 1.0705(3) 0.16811(19) 0.0300(7) Uani 1 1 d D . . . .
H7 H 0.457(4) 1.007(2) 0.152(3) 0.025(13) Uiso 1 1 d D . . . .
O5 O 0.2245(3) 0.4947(3) 0.11058(18) 0.0333(8) Uani 1 1 d D . . . .
H5 H 0.203(4) 0.453(3) 0.137(3) 0.040 Uiso 1 1 d DR . . . .
O10 O 0.3372(5) 0.6451(5) 0.7141(4) 0.0781(17) Uani 0.85 1 d D . . A 1
O15 O 0.2912(3) 0.8567(3) -0.0299(2) 0.0422(9) Uani 1 1 d D . . . .
H15 H 0.234(4) 0.890(5) -0.027(4) 0.063 Uiso 1 1 d DR . . . .
O11 O 0.411(3) 0.712(3) 0.7478(14) 0.104(13) Uani 0.15 1 d D U . A 2
C47 C 0.3987(7) 0.6538(8) 0.6551(5) 0.099(3) Uani 1 1 d D . . . .
H47A H 0.3485 0.6193 0.5980 0.148 Uiso 0.85 1 calc R . . A 1
H47B H 0.4632 0.6152 0.6626 0.148 Uiso 0.85 1 calc R . . A 1
H47C H 0.4277 0.7329 0.6628 0.148 Uiso 0.85 1 calc R . . A 1
H47D H 0.3466 0.6865 0.6204 0.148 Uiso 0.15 1 calc R . . A 2
H47E H 0.3675 0.5738 0.6422 0.148 Uiso 0.15 1 calc R . . A 2
H47F H 0.4739 0.6634 0.6427 0.148 Uiso 0.15 1 calc R . . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cl1 2.2317(12) 2_575 ?
Cu1 Cl1 2.2317(12) . ?
Cu1 O9 1.937(3) . ?
Cu1 O9 1.937(3) 2_575 ?
O3 H3 0.820(19) . ?
O3 C12 1.383(5) . ?
O6 H6 0.839(19) . ?
O6 C24 1.366(5) . ?
O2 H2 0.830(19) . ?
O2 C2 1.369(5) . ?
O1 H1 0.85(6) . ?
O1 C4 1.397(5) . ?
O8 H8 0.84(2) . ?
O8 C34 1.389(5) . ?
O4 H4 0.77(5) . ?
O4 C14 1.395(5) . ?
O9 N1 1.348(5) . ?
C29 H29A 0.88(5) . ?
C29 H29B 0.94(4) . ?
C29 C30 1.501(7) . ?
C29 C28 1.533(6) . ?
C30 H30A 0.90(6) . ?
C30 H30B 1.01(6) . ?
C30 H30C 0.94(5) . ?
C40 H40A 0.93(5) . ?
C40 H40B 1.14(5) . ?
C40 H40C 0.90(5) . ?
C40 C39 1.526(7) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 C19 1.528(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C27 C23 1.527(6) . ?
C19 H19A 1.08(4) . ?
C19 H19B 0.92(4) . ?
C19 C18 1.541(6) . ?
N1 C41 1.343(6) . ?
N1 C45 1.344(6) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C46 O15 1.416(6) . ?
C10 H10A 0.94(5) . ?
C10 H10B 1.02(6) . ?
C10 H10C 0.99(5) . ?
C10 C9 1.523(6) . ?
C17 H17A 0.90(5) . ?
C17 H17B 0.82(5) . ?
C17 H17C 1.04(5) . ?
C17 C13 1.498(6) . ?
C7 H7A 0.89(6) . ?
C7 H7B 0.97(6) . ?
C7 H7C 0.96(5) . ?
C7 C3 1.502(6) . ?
C26 H26 0.96(4) . ?
C26 C25 1.387(6) . ?
C26 C21 1.402(6) . ?
C9 H9A 0.86(5) . ?
C9 H9B 1.04(4) . ?
C9 C8 1.532(6) . ?
C3 C4 1.397(6) . ?
C3 C2 1.410(6) . ?
C39 H39A 0.97(4) . ?
C39 H39B 0.95(4) . ?
C39 C38 1.527(6) . ?
C18 H18 0.91(4) . ?
C18 C15 1.536(6) . ?
C18 C21 1.506(6) . ?
C24 C25 1.396(6) . ?
C24 C23 1.383(6) . ?
C28 H28 1.00(4) . ?
C28 C25 1.525(6) . ?
C28 C31 1.533(5) . ?
C4 C5 1.392(6) . ?
C23 C22 1.393(6) . ?
C1 C8 1.528(6) . ?
C1 C2 1.392(6) . ?
C1 C6 1.387(6) . ?
C13 C12 1.400(6) . ?
C13 C14 1.403(6) . ?
C16 H16 0.89(5) . ?
C16 C15 1.397(5) . ?
C16 C11 1.394(5) . ?
C12 C11 1.392(6) . ?
C8 H8A 0.82(5) . ?
C8 C11 1.522(5) . ?
C15 C14 1.383(6) . ?
C33 C37 1.497(6) . ?
C33 C34 1.391(6) . ?
C33 C32 1.405(6) . ?
C31 C36 1.394(6) . ?
C31 C32 1.394(6) . ?
C42 H42 0.95(5) . ?
C42 C43 1.384(7) . ?
C42 C41 1.369(7) . ?
C43 H43 0.79(5) . ?
C43 C44 1.371(7) . ?
C38 H38 0.95(4) . ?
C38 C35 1.533(5) . ?
C38 C5 1.529(6) . ?
C21 C22 1.391(6) . ?
C41 H41 0.96(5) . ?
C35 C36 1.382(5) . ?
C35 C34 1.401(6) . ?
C6 H6A 0.91(4) . ?
C6 C5 1.392(6) . ?
C36 H36 0.97(4) . ?
C22 O5 1.358(5) . ?
C44 H44 0.90(5) . ?
C44 C45 1.364(7) . ?
C37 H37A 0.98(5) . ?
C37 H37B 0.91(5) . ?
C37 H37C 0.99(6) . ?
C32 O7 1.367(5) . ?
C45 H45 0.83(5) . ?
O7 H7 0.819(19) . ?
O5 H5 0.825(14) . ?
O10 C47 1.385(7) . ?
O15 H15 0.86(2) . ?
O11 C47 1.517(18) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C47 H47D 0.9800 . ?
C47 H47E 0.9800 . ?
C47 H47F 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
Cl1 Cu1 Cl1 180.0 . 2_575 ?
O9 Cu1 Cl1 95.21(10) . 2_575 ?
O9 Cu1 Cl1 95.21(10) 2_575 . ?
O9 Cu1 Cl1 84.79(10) . . ?
O9 Cu1 Cl1 84.79(10) 2_575 2_575 ?
O9 Cu1 O9 180.0 2_575 . ?
C12 O3 H3 113(3) . . ?
C24 O6 H6 121(4) . . ?
C2 O2 H2 111(4) . . ?
C4 O1 H1 107(4) . . ?
C34 O8 H8 112(4) . . ?
C14 O4 H4 107(4) . . ?
N1 O9 Cu1 122.6(2) . . ?
H29A C29 H29B 100(4) . . ?
C30 C29 H29A 108(3) . . ?
C30 C29 H29B 110(3) . . ?
C30 C29 C28 113.1(4) . . ?
C28 C29 H29A 117(3) . . ?
C28 C29 H29B 108(2) . . ?
C29 C30 H30A 111(4) . . ?
C29 C30 H30B 113(3) . . ?
C29 C30 H30C 112(3) . . ?
H30A C30 H30B 111(5) . . ?
H30A C30 H30C 102(5) . . ?
H30B C30 H30C 107(4) . . ?
H40A C40 H40B 109(4) . . ?
H40A C40 H40C 112(5) . . ?
H40B C40 H40C 108(4) . . ?
C39 C40 H40A 112(3) . . ?
C39 C40 H40B 112(3) . . ?
C39 C40 H40C 104(4) . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
C20 C19 H19A 111(2) . . ?
C20 C19 H19B 108(3) . . ?
C20 C19 C18 111.6(4) . . ?
H19A C19 H19B 109(4) . . ?
C18 C19 H19A 109(2) . . ?
C18 C19 H19B 109(3) . . ?
C41 N1 O9 119.2(4) . . ?
C41 N1 C45 120.8(4) . . ?
C45 N1 O9 120.0(4) . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O15 C46 H46A 109.5 . . ?
O15 C46 H46B 109.5 . . ?
O15 C46 H46C 109.5 . . ?
H10A C10 H10B 102(4) . . ?
H10A C10 H10C 109(4) . . ?
H10B C10 H10C 109(4) . . ?
C9 C10 H10A 115(3) . . ?
C9 C10 H10B 110(3) . . ?
C9 C10 H10C 111(3) . . ?
H17A C17 H17B 108(5) . . ?
H17A C17 H17C 113(4) . . ?
H17B C17 H17C 112(4) . . ?
C13 C17 H17A 109(3) . . ?
C13 C17 H17B 110(4) . . ?
C13 C17 H17C 104(3) . . ?
H7A C7 H7B 110(5) . . ?
H7A C7 H7C 108(5) . . ?
H7B C7 H7C 102(5) . . ?
C3 C7 H7A 110(4) . . ?
C3 C7 H7B 111(3) . . ?
C3 C7 H7C 116(3) . . ?
C25 C26 H26 118(3) . . ?
C25 C26 C21 122.8(4) . . ?
C21 C26 H26 119(3) . . ?
C10 C9 H9A 108(3) . . ?
C10 C9 H9B 112(2) . . ?
C10 C9 C8 112.7(4) . . ?
H9A C9 H9B 95(4) . . ?
C8 C9 H9A 115(3) . . ?
C8 C9 H9B 113(2) . . ?
C4 C3 C7 122.0(4) . . ?
C4 C3 C2 117.4(4) . . ?
C2 C3 C7 120.5(4) . . ?
C40 C39 H39A 111(3) . . ?
C40 C39 H39B 108(3) . . ?
C40 C39 C38 112.7(4) . . ?
H39A C39 H39B 111(4) . . ?
C38 C39 H39A 107(2) . . ?
C38 C39 H39B 107(3) . . ?
C19 C18 H18 104(3) . . ?
C15 C18 C19 111.2(3) . . ?
C15 C18 H18 105(3) . . ?
C21 C18 C19 115.1(4) . . ?
C21 C18 H18 109(3) . . ?
C21 C18 C15 111.9(3) . . ?
O6 C24 C25 117.2(4) . . ?
O6 C24 C23 120.3(4) . . ?
C23 C24 C25 122.5(4) . . ?
C29 C28 H28 99(2) . . ?
C25 C28 C29 114.2(4) . . ?
C25 C28 H28 109(2) . . ?
C25 C28 C31 109.7(3) . . ?
C31 C28 C29 112.0(3) . . ?
C31 C28 H28 112(2) . . ?
O1 C4 C3 119.0(4) . . ?
C5 C4 O1 118.1(4) . . ?
C5 C4 C3 122.9(4) . . ?
C26 C25 C24 117.3(4) . . ?
C26 C25 C28 122.6(4) . . ?
C24 C25 C28 120.0(4) . . ?
C24 C23 C27 122.1(4) . . ?
C24 C23 C22 117.8(4) . . ?
C22 C23 C27 120.1(4) . . ?
C2 C1 C8 120.1(4) . . ?
C6 C1 C8 122.4(4) . . ?
C6 C1 C2 117.5(4) . . ?
C12 C13 C17 121.7(4) . . ?
C12 C13 C14 116.6(4) . . ?
C14 C13 C17 121.7(4) . . ?
C15 C16 H16 117(3) . . ?
C11 C16 H16 120(3) . . ?
C11 C16 C15 122.6(4) . . ?
O3 C12 C13 121.3(4) . . ?
O3 C12 C11 116.0(3) . . ?
C11 C12 C13 122.7(4) . . ?
C9 C8 H8A 103(3) . . ?
C1 C8 C9 114.5(4) . . ?
C1 C8 H8A 108(3) . . ?
C11 C8 C9 112.5(3) . . ?
C11 C8 C1 110.0(3) . . ?
C11 C8 H8A 109(3) . . ?
C16 C15 C18 120.3(4) . . ?
C14 C15 C18 122.5(3) . . ?
C14 C15 C16 117.2(4) . . ?
C34 C33 C37 121.9(4) . . ?
C34 C33 C32 117.9(4) . . ?
C32 C33 C37 120.1(4) . . ?
O2 C2 C3 114.9(4) . . ?
O2 C2 C1 123.4(4) . . ?
C1 C2 C3 121.7(4) . . ?
O4 C14 C13 118.1(4) . . ?
C15 C14 O4 118.4(3) . . ?
C15 C14 C13 123.4(4) . . ?
C36 C31 C28 120.3(4) . . ?
C36 C31 C32 117.9(3) . . ?
C32 C31 C28 121.8(3) . . ?
C43 C42 H42 123(3) . . ?
C41 C42 H42 117(3) . . ?
C41 C42 C43 119.0(5) . . ?
C42 C43 H43 127(4) . . ?
C44 C43 C42 119.1(5) . . ?
C44 C43 H43 114(4) . . ?
C39 C38 H38 106(2) . . ?
C39 C38 C35 111.5(3) . . ?
C39 C38 C5 113.5(3) . . ?
C35 C38 H38 113(2) . . ?
C5 C38 H38 102(3) . . ?
C5 C38 C35 110.6(3) . . ?
C16 C11 C8 120.0(4) . . ?
C12 C11 C16 117.5(4) . . ?
C12 C11 C8 122.5(3) . . ?
C26 C21 C18 122.2(4) . . ?
C22 C21 C26 116.8(4) . . ?
C22 C21 C18 120.9(4) . . ?
N1 C41 C42 120.8(5) . . ?
N1 C41 H41 118(3) . . ?
C42 C41 H41 121(3) . . ?
C36 C35 C38 120.5(4) . . ?
C36 C35 C34 117.1(4) . . ?
C34 C35 C38 122.3(3) . . ?
C1 C6 H6A 120(3) . . ?
C1 C6 C5 123.8(4) . . ?
C5 C6 H6A 117(3) . . ?
C31 C36 H36 117(2) . . ?
C35 C36 C31 123.1(4) . . ?
C35 C36 H36 119(2) . . ?
C21 C22 C23 122.6(4) . . ?
O5 C22 C23 115.0(4) . . ?
O5 C22 C21 122.4(4) . . ?
C4 C5 C38 119.9(4) . . ?
C4 C5 C6 116.5(4) . . ?
C6 C5 C38 123.5(4) . . ?
C43 C44 H44 118(3) . . ?
C45 C44 C43 120.4(5) . . ?
C45 C44 H44 121(3) . . ?
C33 C37 H37A 110(3) . . ?
C33 C37 H37B 114(3) . . ?
C33 C37 H37C 114(3) . . ?
H37A C37 H37B 102(4) . . ?
H37A C37 H37C 104(4) . . ?
H37B C37 H37C 112(5) . . ?
O8 C34 C33 117.3(4) . . ?
O8 C34 C35 120.2(3) . . ?
C33 C34 C35 122.5(3) . . ?
C31 C32 C33 121.4(3) . . ?
O7 C32 C33 116.9(4) . . ?
O7 C32 C31 121.7(3) . . ?
N1 C45 C44 119.9(5) . . ?
N1 C45 H45 113(4) . . ?
C44 C45 H45 127(4) . . ?
C32 O7 H7 110(3) . . ?
C22 O5 H5 117(4) . . ?
C46 O15 H15 107(4) . . ?
O10 C47 H47A 109.5 . . ?
O10 C47 H47B 109.5 . . ?
O10 C47 H47C 109.5 . . ?
O11 C47 H47D 109.5 . . ?
O11 C47 H47E 109.5 . . ?
O11 C47 H47F 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
H47D C47 H47E 109.5 . . ?
H47D C47 H47F 109.5 . . ?
H47E C47 H47F 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.500 0.000 276.6 88.1 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_V
_database_code_depnum_ccdc_archive 'CCDC 1054271'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_audit_creation_date             2015-03-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C12 H8 Cu N2 O6'
_chemical_formula_sum            'C12 H8 Cu N2 O6'
_chemical_formula_weight         339.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C7 H7 N1 O3 Cu1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   3.6410(6)
_cell_length_b                   12.6301(17)
_cell_length_c                   12.1194(13)
_cell_angle_alpha                90
_cell_angle_beta                 94.057(13)
_cell_angle_gamma                90
_cell_volume                     555.93(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    440
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      71.8850
_cell_measurement_theta_min      4.9870
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.139
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.1174
_exptl_crystal_size_mid          0.0289
_exptl_crystal_size_min          0.0247
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.1155
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1617
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         66.725
_diffrn_reflns_theta_min         5.064
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -38.00  -11.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.8676   37.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega   -2.00   29.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.8676   37.0000  -90.0000 31

#__ type_ start__ end____ width___ exp.time_
  3 omega   26.00   51.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.8676   77.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
  4 omega   53.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.8676   77.0000    0.0000 40

#__ type_ start__ end____ width___ exp.time_
  5 omega   77.00  161.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   30.0000  -60.0000 84

#__ type_ start__ end____ width___ exp.time_
  6 omega  109.00  171.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  125.0000 -150.0000 62

#__ type_ start__ end____ width___ exp.time_
  7 omega   79.00  176.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   61.0000 -180.0000 97

#__ type_ start__ end____ width___ exp.time_
  8 omega   45.00   95.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -45.0000   60.0000 50

#__ type_ start__ end____ width___ exp.time_
  9 omega   50.00   90.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -30.0000  150.0000 40

#__ type_ start__ end____ width___ exp.time_
 10 omega   23.00   97.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.8676 -125.0000 -120.0000 74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0971907000
_diffrn_orient_matrix_UB_12      0.0053690000
_diffrn_orient_matrix_UB_13      -0.1255046000
_diffrn_orient_matrix_UB_21      -0.2250104000
_diffrn_orient_matrix_UB_22      -0.1029744000
_diffrn_orient_matrix_UB_23      0.0063320000
_diffrn_orient_matrix_UB_31      -0.3462702000
_diffrn_orient_matrix_UB_32      0.0653143000
_diffrn_orient_matrix_UB_33      0.0204008000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                700
_reflns_number_total             975
_reflns_odcompleteness_completeness 98.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         975
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0826
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1256P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2050
_refine_ls_wR_factor_ref         0.2401
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 1.0000 1.0000 0.5000 0.0189(6) Uani 1 2 d S T P . .
O1 O 0.6212(14) 0.8918(4) 0.4752(4) 0.0214(11) Uani 1 1 d . . . . .
O2 O 1.0668(13) 0.9660(4) 0.6520(4) 0.0206(11) Uani 1 1 d . . . . .
O3 O 0.9286(14) 0.8899(4) 0.8083(4) 0.0230(12) Uani 1 1 d . . . . .
N1 N 0.6048(15) 0.8042(5) 0.5385(5) 0.0174(13) Uani 1 1 d . . . . .
C1 C 0.7315(19) 0.8007(6) 0.6470(6) 0.0198(15) Uani 1 1 d . . . . .
C2 C 0.6923(18) 0.7043(6) 0.7031(6) 0.0176(14) Uani 1 1 d . . . . .
H2 H 0.7825 0.6991 0.7766 0.021 Uiso 1 1 calc R . . . .
C3 C 0.5232(19) 0.6166(6) 0.6522(6) 0.0218(16) Uani 1 1 d . . . . .
H3 H 0.5012 0.5531 0.6900 0.026 Uiso 1 1 calc R . . . .
C4 C 0.3890(19) 0.6273(6) 0.5431(6) 0.0236(16) Uani 1 1 d . . . . .
H4 H 0.2698 0.5707 0.5069 0.028 Uiso 1 1 calc R . . . .
C5 C 0.4305(18) 0.7202(6) 0.4885(6) 0.0192(15) Uani 1 1 d . . . . .
H5 H 0.3373 0.7263 0.4153 0.023 Uiso 1 1 calc R . . . .
C6 C 0.9219(17) 0.8928(6) 0.7072(6) 0.0168(15) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.950(5) . ?
Cu1 O1 1.950(5) 3_776 ?
Cu1 O2 1.891(5) . ?
Cu1 O2 1.891(5) 3_776 ?
O1 N1 1.350(7) . ?
O2 C6 1.277(9) . ?
O3 C6 1.224(9) . ?
N1 C1 1.364(8) . ?
N1 C5 1.356(10) . ?
C1 C2 1.406(9) . ?
C1 C6 1.514(10) . ?
C2 H2 0.9300 . ?
C2 C3 1.391(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.383(11) . ?
C4 H4 0.9300 . ?
C4 C5 1.362(11) . ?
C5 H5 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 . 3_776 ?
O2 Cu1 O1 88.2(2) 3_776 . ?
O2 Cu1 O1 88.2(2) . 3_776 ?
O2 Cu1 O1 91.8(2) 3_776 3_776 ?
O2 Cu1 O1 91.8(2) . . ?
O2 Cu1 O2 180.0 . 3_776 ?
N1 O1 Cu1 123.1(4) . . ?
C6 O2 Cu1 130.2(4) . . ?
O1 N1 C1 123.3(6) . . ?
O1 N1 C5 115.1(5) . . ?
C5 N1 C1 121.5(6) . . ?
N1 C1 C2 117.0(7) . . ?
N1 C1 C6 123.5(6) . . ?
C2 C1 C6 119.4(6) . . ?
C1 C2 H2 118.9 . . ?
C3 C2 C1 122.2(6) . . ?
C3 C2 H2 118.9 . . ?
C2 C3 H3 121.3 . . ?
C4 C3 C2 117.5(7) . . ?
C4 C3 H3 121.3 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.4(7) . . ?
C5 C4 H4 119.8 . . ?
N1 C5 C4 121.4(6) . . ?
N1 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
O2 C6 C1 119.7(6) . . ?
O3 C6 O2 124.5(7) . . ?
O3 C6 C1 115.8(6) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -8 -2 0.0110 0.0021 -8.0081 -1.9847 0.2059 0.8116 -0.5643
0 8 3 0.0164 -0.0016 8.0073 2.9857 -0.3316 -0.8053 0.5844
-2 0 0 0.0518 -1.9975 0.0125 0.0068 0.1934 0.4482 0.6926
2 0 0 0.0636 1.9975 -0.0125 -0.0068 -0.1934 -0.4482 -0.6926
0 3 -7 0.0116 -0.0053 3.0093 -7.0134 0.8969 -0.3531 0.0553
0 -3 7 0.0131 0.0053 -3.0093 7.0134 -0.8969 0.3531 -0.0553
2 -4 -2 0.0459 1.9980 -4.0158 -2.0001 0.0353 -0.0487 -0.9949

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_VI
_database_code_depnum_ccdc_archive 'CCDC 1054272'
_audit_update_record             
;
2015-03-16 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_VI                  
;
PROBLEM: Short Inter D...A Contact  O11    ..  O13     ..       2.70 Ang.  
RESPONSE: Due to disordered oxygens
;
_vrf_PLAT910_VI                  
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         14 Report
RESPONSE: These reflections are affected by the beamstopper
;
# end Validation Reply Form
_audit_creation_date             2015-03-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C40 H48 O8), C12 H8 Cu N2 O6, 4(H2 O), 2(O)'
_chemical_formula_sum            'C92 H112 Cu N2 O28'
_chemical_formula_weight         1757.37
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H20 N1 O9'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.1909(7)
_cell_length_b                   12.7422(6)
_cell_length_c                   15.5226(9)
_cell_angle_alpha                81.845(4)
_cell_angle_beta                 73.601(5)
_cell_angle_gamma                69.069(5)
_cell_volume                     2158.3(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3760
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.7680
_cell_measurement_theta_min      3.4160
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             931
_exptl_crystal_size_max          0.1543
_exptl_crystal_size_mid          0.1409
_exptl_crystal_size_min          0.0854
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14471
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         3.048
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -90.00   13.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2930  -19.0000   30.0000 103

#__ type_ start__ end____ width___ exp.time_
  2 omega  -86.00   12.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2930  -77.0000 -150.0000 98

#__ type_ start__ end____ width___ exp.time_
  3 omega  -28.00    1.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2930  -57.0000  -30.0000 29

#__ type_ start__ end____ width___ exp.time_
  4 omega  -47.00   50.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2930   77.0000  -30.0000 97

#__ type_ start__ end____ width___ exp.time_
  5 omega   15.00   61.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5430  -99.0000  120.0000 46

#__ type_ start__ end____ width___ exp.time_
  6 omega   41.00   66.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5430 -107.0000  121.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0331426000
_diffrn_orient_matrix_UB_12      0.0066792000
_diffrn_orient_matrix_UB_13      0.0456293000
_diffrn_orient_matrix_UB_21      -0.0397659000
_diffrn_orient_matrix_UB_22      -0.0249892000
_diffrn_orient_matrix_UB_23      -0.0075509000
_diffrn_orient_matrix_UB_31      0.0382176000
_diffrn_orient_matrix_UB_32      -0.0537618000
_diffrn_orient_matrix_UB_33      0.0115997000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5613
_reflns_number_total             7807
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.839
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0755
_refine_ls_restrained_S_all      1.189
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1057P)²+3.7171P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2229
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H3-O3
 0.85 with sigma of 0.02
 H2-O2
 0.85 with sigma of 0.02
 O4-H4
 0.85 with sigma of 0.02
 O5-H5
 0.85 with sigma of 0.02
 H1-O1
 0.85 with sigma of 0.02
 H8-O8
 0.85 with sigma of 0.02
 O6-H6
 0.85 with sigma of 0.02
 O15-H15A
 0.85 with sigma of 0.02
 H15B-O15
 0.85 with sigma of 0.02
 H14A-H14B
 0.85 with sigma of 0.02
 H14B-H14A
 0.85 with sigma of 0.02
 H14A-O14
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: O12(0.5) O13(0.5)
4.a Riding coordinates:
 O14(H14A,H14B)
4.b Ternary CH refined with riding coordinates:
 C8(H8A), C18(H18), C28(H28), C38(H38)
4.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C19(H19A,H19B), C29(H29A,H29B), C39(H39A,H39B)
4.d Aromatic/amide H refined with riding coordinates:
 C6(H6A), C16(H16), C26(H26), C36(H36), C41(H41), C42(H42), C43(H43), C44(H44)
4.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C20(H20A,H20B,
 H20C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C40(H40A,
 H40B,H40C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
O1 O 0.2925(3) -0.1963(2) 0.2155(2) 0.0237(7) Uani 1 1 d D . . . .
H1 H 0.222(3) -0.152(4) 0.234(4) 0.053(18) Uiso 1 1 d D . . . .
O2 O 0.6860(3) -0.1614(2) 0.1382(2) 0.0240(7) Uani 1 1 d D . . . .
H2 H 0.735(6) -0.228(3) 0.138(6) 0.10(3) Uiso 1 1 d D . . . .
O3 O 0.7335(3) 0.0378(2) 0.0948(2) 0.0238(7) Uani 1 1 d D . . . .
H3 H 0.721(5) -0.022(3) 0.115(4) 0.051(18) Uiso 1 1 d D . . . .
O4 O 0.5526(3) 0.4289(2) 0.1297(2) 0.0235(7) Uani 1 1 d D . . . .
H4 H 0.496(5) 0.482(4) 0.157(4) 0.07(2) Uiso 1 1 d D . . . .
O5 O 0.3353(3) 0.5844(2) 0.1993(2) 0.0227(7) Uani 1 1 d D . . . .
H5 H 0.310(5) 0.648(3) 0.221(4) 0.055(19) Uiso 1 1 d D . . . .
O6 O -0.0559(3) 0.5417(2) 0.2848(2) 0.0226(7) Uani 1 1 d D . . . .
H6 H -0.080(4) 0.488(3) 0.296(4) 0.034(15) Uiso 1 1 d D . . . .
O7 O -0.1306(3) 0.3567(2) 0.3008(2) 0.0228(7) Uani 1 1 d . . . . .
H7 H -0.161(5) 0.359(4) 0.265(4) 0.024(15) Uiso 1 1 d . . . . .
O8 O 0.0620(3) -0.0431(2) 0.2574(2) 0.0216(7) Uani 1 1 d D . . . .
H8 H 0.036(4) -0.038(4) 0.213(2) 0.032(15) Uiso 1 1 d D . . . .
C1 C 0.3377(4) -0.0888(3) 0.3090(3) 0.0154(9) Uani 1 1 d . . . . .
C2 C 0.3735(4) -0.1562(3) 0.2359(3) 0.0165(9) Uani 1 1 d . . . . .
C3 C 0.4903(4) -0.1840(3) 0.1788(3) 0.0194(9) Uani 1 1 d . . . . .
C4 C 0.5706(4) -0.1398(3) 0.1960(3) 0.0179(9) Uani 1 1 d . . . . .
C5 C 0.5381(4) -0.0680(3) 0.2658(3) 0.0169(9) Uani 1 1 d . . . . .
C6 C 0.4207(4) -0.0442(3) 0.3210(3) 0.0166(9) Uani 1 1 d . . . . .
H6A H 0.3965 0.0047 0.3688 0.020 Uiso 1 1 calc R . . . .
C7 C 0.5276(4) -0.2564(4) 0.0992(3) 0.0289(11) Uani 1 1 d . . . . .
H7A H 0.5754 -0.3334 0.1143 0.043 Uiso 1 1 calc GR . . . .
H7B H 0.5765 -0.2257 0.0474 0.043 Uiso 1 1 calc GR . . . .
H7C H 0.4549 -0.2571 0.0841 0.043 Uiso 1 1 calc GR . . . .
C8 C 0.6267(4) -0.0180(3) 0.2813(3) 0.0170(9) Uani 1 1 d . . . . .
H8A H 0.7092 -0.0639 0.2474 0.020 Uiso 1 1 calc R . . . .
C9 C 0.6304(4) -0.0277(3) 0.3799(3) 0.0217(9) Uani 1 1 d . . . . .
H9A H 0.6864 0.0094 0.3861 0.026 Uiso 1 1 calc R . . . .
H9B H 0.5486 0.0124 0.4167 0.026 Uiso 1 1 calc R . . . .
C10 C 0.6717(4) -0.1494(4) 0.4157(3) 0.0307(11) Uani 1 1 d . . . . .
H10A H 0.7516 -0.1901 0.3783 0.046 Uiso 1 1 calc GR . . . .
H10B H 0.6132 -0.1850 0.4139 0.046 Uiso 1 1 calc GR . . . .
H10C H 0.6767 -0.1512 0.4778 0.046 Uiso 1 1 calc GR . . . .
C11 C 0.6042(3) 0.1023(3) 0.2405(3) 0.0156(9) Uani 1 1 d . . . . .
C12 C 0.6577(4) 0.1228(3) 0.1513(3) 0.0190(9) Uani 1 1 d . . . . .
C13 C 0.6397(4) 0.2328(3) 0.1137(3) 0.0195(9) Uani 1 1 d . . . . .
C14 C 0.5640(4) 0.3220(3) 0.1692(3) 0.0189(9) Uani 1 1 d . . . . .
C15 C 0.5103(3) 0.3053(3) 0.2585(3) 0.0158(9) Uani 1 1 d . . . . .
C16 C 0.5301(3) 0.1941(3) 0.2931(3) 0.0164(9) Uani 1 1 d . . . . .
H16 H 0.4919 0.1808 0.3540 0.020 Uiso 1 1 calc R . . . .
C17 C 0.7046(4) 0.2537(4) 0.0181(3) 0.0259(10) Uani 1 1 d . . . . .
H17A H 0.6577 0.3263 -0.0055 0.039 Uiso 1 1 calc GR . . . .
H17B H 0.7130 0.1937 -0.0190 0.039 Uiso 1 1 calc GR . . . .
H17C H 0.7852 0.2546 0.0165 0.039 Uiso 1 1 calc GR . . . .
C18 C 0.4304(4) 0.4053(3) 0.3176(3) 0.0182(9) Uani 1 1 d . . . . .
H18 H 0.4608 0.4693 0.2923 0.022 Uiso 1 1 calc R . . . .
C19 C 0.4383(4) 0.3849(3) 0.4151(3) 0.0224(10) Uani 1 1 d . . . . .
H19A H 0.4073 0.3227 0.4427 0.027 Uiso 1 1 calc R . . . .
H19B H 0.5245 0.3610 0.4166 0.027 Uiso 1 1 calc R . . . .
C20 C 0.3669(5) 0.4882(4) 0.4710(4) 0.0357(12) Uani 1 1 d . . . . .
H20A H 0.3958 0.5507 0.4434 0.054 Uiso 1 1 calc GR . . . .
H20B H 0.3786 0.4710 0.5321 0.054 Uiso 1 1 calc GR . . . .
H20C H 0.2806 0.5092 0.4736 0.054 Uiso 1 1 calc GR . . . .
C21 C 0.2999(4) 0.4416(3) 0.3087(3) 0.0162(9) Uani 1 1 d . . . . .
C22 C 0.2549(4) 0.5330(3) 0.2527(3) 0.0186(9) Uani 1 1 d . . . . .
C23 C 0.1356(4) 0.5681(3) 0.2443(3) 0.0169(9) Uani 1 1 d . . . . .
C24 C 0.0615(3) 0.5073(3) 0.2939(3) 0.0154(8) Uani 1 1 d . . . . .
C25 C 0.1023(4) 0.4157(3) 0.3527(3) 0.0158(9) Uani 1 1 d . . . . .
C26 C 0.2215(3) 0.3850(3) 0.3573(3) 0.0156(9) Uani 1 1 d . . . . .
H26 H 0.2512 0.3222 0.3954 0.019 Uiso 1 1 calc R . . . .
C27 C 0.0870(4) 0.6669(3) 0.1835(3) 0.0212(9) Uani 1 1 d . . . . .
H27A H 0.0838 0.6396 0.1287 0.032 Uiso 1 1 calc GR . . . .
H27B H 0.1404 0.7125 0.1678 0.032 Uiso 1 1 calc GR . . . .
H27C H 0.0053 0.7129 0.2146 0.032 Uiso 1 1 calc GR . . . .
C28 C 0.0190(3) 0.3547(3) 0.4117(3) 0.0146(8) Uani 1 1 d . . . . .
H28 H -0.0659 0.4073 0.4172 0.018 Uiso 1 1 calc R . . . .
C29 C 0.0373(4) 0.3290(3) 0.5073(3) 0.0184(9) Uani 1 1 d . . . . .
H29A H 0.1220 0.2795 0.5039 0.022 Uiso 1 1 calc R . . . .
H29B H 0.0258 0.4002 0.5328 0.022 Uiso 1 1 calc R . . . .
C30 C -0.0478(4) 0.2728(4) 0.5710(3) 0.0243(10) Uani 1 1 d . . . . .
H30A H -0.0360 0.2013 0.5472 0.036 Uiso 1 1 calc GR . . . .
H30B H -0.1320 0.3222 0.5767 0.036 Uiso 1 1 calc GR . . . .
H30C H -0.0301 0.2588 0.6302 0.036 Uiso 1 1 calc GR . . . .
C31 C 0.0297(4) 0.2506(3) 0.3675(3) 0.0160(9) Uani 1 1 d . . . . .
C32 C -0.0463(4) 0.2529(3) 0.3152(3) 0.0167(9) Uani 1 1 d . . . . .
C33 C -0.0413(4) 0.1571(3) 0.2782(3) 0.0181(9) Uani 1 1 d . . . . .
C34 C 0.0479(4) 0.0552(3) 0.2942(3) 0.0175(9) Uani 1 1 d . . . . .
C35 C 0.1236(3) 0.0474(3) 0.3489(3) 0.0148(8) Uani 1 1 d . . . . .
C36 C 0.1134(3) 0.1464(3) 0.3837(3) 0.0159(9) Uani 1 1 d . . . . .
H36 H 0.1658 0.1428 0.4200 0.019 Uiso 1 1 calc R . . . .
C37 C -0.1318(4) 0.1607(4) 0.2285(3) 0.0238(10) Uani 1 1 d . . . . .
H37A H -0.1035 0.1814 0.1650 0.036 Uiso 1 1 calc GR . . . .
H37B H -0.2102 0.2166 0.2544 0.036 Uiso 1 1 calc GR . . . .
H37C H -0.1409 0.0865 0.2337 0.036 Uiso 1 1 calc GR . . . .
C38 C 0.2123(3) -0.0650(3) 0.3731(3) 0.0145(8) Uani 1 1 d . . . . .
H38 H 0.1811 -0.1245 0.3647 0.017 Uiso 1 1 calc R . . . .
C39 C 0.2143(4) -0.0748(3) 0.4723(3) 0.0195(9) Uani 1 1 d . . . . .
H39A H 0.2466 -0.0181 0.4831 0.023 Uiso 1 1 calc R . . . .
H39B H 0.1301 -0.0575 0.5100 0.023 Uiso 1 1 calc R . . . .
C40 C 0.2905(4) -0.1905(4) 0.5012(3) 0.0260(10) Uani 1 1 d . . . . .
H40A H 0.3751 -0.2064 0.4669 0.039 Uiso 1 1 calc GR . . . .
H40B H 0.2599 -0.2474 0.4898 0.039 Uiso 1 1 calc GR . . . .
H40C H 0.2855 -0.1925 0.5655 0.039 Uiso 1 1 calc GR . . . .
Cu1 Cu 0.0000 0.5000 0.0000 0.0333(3) Uani 1 2 d S T P . .
O9 O 0.1196(3) 0.4428(3) 0.0670(3) 0.0428(10) Uani 1 1 d . . . . .
O10 O -0.0370(3) 0.3625(3) 0.0224(2) 0.0306(8) Uani 1 1 d . . . . .
O11 O 0.0383(3) 0.1806(3) -0.0028(3) 0.0447(10) Uani 1 1 d . . . . .
N1 N 0.1733(3) 0.3336(3) 0.0866(3) 0.0290(9) Uani 1 1 d . . . . .
C41 C 0.2615(4) 0.3149(4) 0.1299(3) 0.0299(11) Uani 1 1 d . . . . .
H41 H 0.2768 0.3768 0.1457 0.036 Uiso 1 1 calc R . . . .
C42 C 0.3284(4) 0.2076(4) 0.1509(3) 0.0300(11) Uani 1 1 d . . . . .
H42 H 0.3889 0.1953 0.1822 0.036 Uiso 1 1 calc R . . . .
C43 C 0.3084(4) 0.1178(4) 0.1269(3) 0.0310(11) Uani 1 1 d . . . . .
H43 H 0.3564 0.0429 0.1393 0.037 Uiso 1 1 calc R . . . .
C44 C 0.2176(4) 0.1385(4) 0.0845(3) 0.0286(11) Uani 1 1 d . . . . .
H44 H 0.2019 0.0769 0.0686 0.034 Uiso 1 1 calc R . . . .
C45 C 0.1478(4) 0.2477(4) 0.0643(3) 0.0254(10) Uani 1 1 d . . . . .
C46 C 0.0435(4) 0.2650(4) 0.0228(3) 0.0305(11) Uani 1 1 d . . . . .
O14 O 0.7611(3) 0.4383(3) 0.1589(3) 0.0400(9) Uani 1 1 d D . . . .
H14A H 0.8153 0.4037 0.1130 0.8(3) Uiso 1 1 d DR . . . .
H14B H 0.6914 0.4407 0.1516 0.22(6) Uiso 1 1 d DR . . . .
O15 O -0.1683(3) 0.6215(3) 0.1402(2) 0.0314(8) Uani 1 1 d D . . . .
H15A H -0.210(5) 0.576(4) 0.159(4) 0.053(19) Uiso 1 1 d D . . . .
H15B H -0.132(5) 0.612(5) 0.182(3) 0.043(17) Uiso 1 1 d D . . . .
O12 O 0.0490(11) -0.0522(10) 0.0904(11) 0.059(4) Uani 0.5 1 d . . . A 1
O13 O -0.0109(11) -0.0442(13) 0.1071(11) 0.066(4) Uani 0.5 1 d . . . B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.84(2) . ?
O1 C2 1.386(5) . ?
O2 H2 0.85(2) . ?
O2 C4 1.393(5) . ?
O3 H3 0.83(2) . ?
O3 C12 1.376(5) . ?
O4 H4 0.83(2) . ?
O4 C14 1.387(5) . ?
O5 H5 0.84(2) . ?
O5 C22 1.385(5) . ?
O6 H6 0.809(19) . ?
O6 C24 1.381(5) . ?
O7 H7 0.74(5) . ?
O7 C32 1.389(5) . ?
O8 H8 0.83(2) . ?
O8 C34 1.385(5) . ?
C1 C2 1.396(6) . ?
C1 C6 1.389(6) . ?
C1 C38 1.521(5) . ?
C2 C3 1.398(6) . ?
C3 C4 1.391(6) . ?
C3 C7 1.514(6) . ?
C4 C5 1.395(6) . ?
C5 C6 1.394(6) . ?
C5 C8 1.522(5) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 1.0000 . ?
C8 C9 1.529(6) . ?
C8 C11 1.532(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.523(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.386(6) . ?
C11 C16 1.396(6) . ?
C12 C13 1.405(6) . ?
C13 C14 1.403(6) . ?
C13 C17 1.508(6) . ?
C14 C15 1.378(6) . ?
C15 C16 1.403(5) . ?
C15 C18 1.534(5) . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 1.0000 . ?
C18 C19 1.525(6) . ?
C18 C21 1.531(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.523(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.393(6) . ?
C21 C26 1.390(6) . ?
C22 C23 1.400(6) . ?
C23 C24 1.396(6) . ?
C23 C27 1.507(6) . ?
C24 C25 1.408(6) . ?
C25 C26 1.383(5) . ?
C25 C28 1.520(5) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28 1.0000 . ?
C28 C29 1.535(6) . ?
C28 C31 1.527(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.522(6) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.384(6) . ?
C31 C36 1.397(5) . ?
C32 C33 1.395(6) . ?
C33 C34 1.408(6) . ?
C33 C37 1.500(6) . ?
C34 C35 1.392(6) . ?
C35 C36 1.393(6) . ?
C35 C38 1.527(5) . ?
C36 H36 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38 1.0000 . ?
C38 C39 1.533(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.519(6) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
Cu1 O9 1.903(3) . ?
Cu1 O9 1.903(3) 2_565 ?
Cu1 O10 1.923(3) . ?
Cu1 O10 1.923(3) 2_565 ?
O9 N1 1.342(5) . ?
O10 C46 1.279(6) . ?
O11 C46 1.225(6) . ?
N1 C41 1.358(6) . ?
N1 C45 1.352(6) . ?
C41 H41 0.9500 . ?
C41 C42 1.367(6) . ?
C42 H42 0.9500 . ?
C42 C43 1.371(7) . ?
C43 H43 0.9500 . ?
C43 C44 1.372(7) . ?
C44 H44 0.9500 . ?
C44 C45 1.393(6) . ?
C45 C46 1.518(6) . ?
O14 H14A 0.8681 . ?
O14 H14B 0.8781 . ?
O15 H15A 0.87(2) . ?
O15 H15B 0.86(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O1 H1 109(4) . . ?
C4 O2 H2 118(6) . . ?
C12 O3 H3 110(4) . . ?
C14 O4 H4 116(5) . . ?
C22 O5 H5 103(4) . . ?
C24 O6 H6 109(4) . . ?
C32 O7 H7 115(4) . . ?
C34 O8 H8 118(4) . . ?
C2 C1 C38 121.2(4) . . ?
C6 C1 C2 117.5(4) . . ?
C6 C1 C38 121.3(4) . . ?
O1 C2 C1 120.8(4) . . ?
O1 C2 C3 117.0(4) . . ?
C1 C2 C3 122.2(4) . . ?
C2 C3 C7 121.6(4) . . ?
C4 C3 C2 117.5(4) . . ?
C4 C3 C7 120.8(4) . . ?
O2 C4 C5 118.0(4) . . ?
C3 C4 O2 119.2(4) . . ?
C3 C4 C5 122.7(4) . . ?
C4 C5 C8 121.5(4) . . ?
C6 C5 C4 117.2(4) . . ?
C6 C5 C8 121.3(4) . . ?
C1 C6 C5 122.8(4) . . ?
C1 C6 H6A 118.6 . . ?
C5 C6 H6A 118.6 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 106.4 . . ?
C5 C8 C9 112.9(3) . . ?
C5 C8 C11 111.1(3) . . ?
C9 C8 H8A 106.4 . . ?
C9 C8 C11 113.1(3) . . ?
C11 C8 H8A 106.4 . . ?
C8 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 C8 112.6(4) . . ?
C10 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C8 121.1(4) . . ?
C12 C11 C16 118.4(4) . . ?
C16 C11 C8 120.5(4) . . ?
O3 C12 C11 122.5(4) . . ?
O3 C12 C13 115.9(4) . . ?
C11 C12 C13 121.6(4) . . ?
C12 C13 C17 120.8(4) . . ?
C14 C13 C12 117.8(4) . . ?
C14 C13 C17 121.3(4) . . ?
O4 C14 C13 115.5(4) . . ?
C15 C14 O4 122.0(4) . . ?
C15 C14 C13 122.5(4) . . ?
C14 C15 C16 117.8(4) . . ?
C14 C15 C18 120.9(3) . . ?
C16 C15 C18 121.3(4) . . ?
C11 C16 C15 121.9(4) . . ?
C11 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18 106.7 . . ?
C19 C18 C15 113.9(3) . . ?
C19 C18 H18 106.7 . . ?
C19 C18 C21 112.6(4) . . ?
C21 C18 C15 109.6(3) . . ?
C21 C18 H18 106.7 . . ?
C18 C19 H19A 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 C18 113.2(4) . . ?
C20 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C18 121.4(4) . . ?
C26 C21 C18 121.1(3) . . ?
C26 C21 C22 117.6(4) . . ?
O5 C22 C21 117.6(4) . . ?
O5 C22 C23 120.0(4) . . ?
C21 C22 C23 122.2(4) . . ?
C22 C23 C27 122.2(4) . . ?
C24 C23 C22 117.6(4) . . ?
C24 C23 C27 120.1(4) . . ?
O6 C24 C23 117.4(3) . . ?
O6 C24 C25 120.4(4) . . ?
C23 C24 C25 122.1(4) . . ?
C24 C25 C28 122.1(3) . . ?
C26 C25 C24 117.2(4) . . ?
C26 C25 C28 120.7(3) . . ?
C21 C26 H26 118.4 . . ?
C25 C26 C21 123.2(4) . . ?
C25 C26 H26 118.4 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28 106.7 . . ?
C25 C28 C29 111.9(3) . . ?
C25 C28 C31 111.5(3) . . ?
C29 C28 H28 106.7 . . ?
C31 C28 H28 106.7 . . ?
C31 C28 C29 112.9(3) . . ?
C28 C29 H29A 108.7 . . ?
C28 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C30 C29 C28 114.4(3) . . ?
C30 C29 H29A 108.7 . . ?
C30 C29 H29B 108.7 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C28 122.6(3) . . ?
C32 C31 C36 117.2(4) . . ?
C36 C31 C28 120.1(4) . . ?
O7 C32 C33 120.3(4) . . ?
C31 C32 O7 116.7(3) . . ?
C31 C32 C33 123.0(4) . . ?
C32 C33 C34 117.2(4) . . ?
C32 C33 C37 121.6(4) . . ?
C34 C33 C37 121.1(4) . . ?
O8 C34 C33 121.0(4) . . ?
O8 C34 C35 116.9(3) . . ?
C35 C34 C33 122.1(4) . . ?
C34 C35 C36 117.5(4) . . ?
C34 C35 C38 122.1(3) . . ?
C36 C35 C38 120.4(4) . . ?
C31 C36 H36 118.6 . . ?
C35 C36 C31 122.9(4) . . ?
C35 C36 H36 118.6 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C1 C38 C35 111.7(3) . . ?
C1 C38 H38 106.5 . . ?
C1 C38 C39 113.2(3) . . ?
C35 C38 H38 106.5 . . ?
C35 C38 C39 112.0(3) . . ?
C39 C38 H38 106.5 . . ?
C38 C39 H39A 108.9 . . ?
C38 C39 H39B 108.9 . . ?
H39A C39 H39B 107.7 . . ?
C40 C39 C38 113.3(4) . . ?
C40 C39 H39A 108.9 . . ?
C40 C39 H39B 108.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O9 Cu1 O9 180.00(18) . 2_565 ?
O9 Cu1 O10 91.55(14) . . ?
O9 Cu1 O10 88.45(14) . 2_565 ?
O9 Cu1 O10 91.55(14) 2_565 2_565 ?
O9 Cu1 O10 88.45(14) 2_565 . ?
O10 Cu1 O10 180.0 . 2_565 ?
N1 O9 Cu1 125.2(3) . . ?
C46 O10 Cu1 123.4(3) . . ?
O9 N1 C41 113.4(4) . . ?
O9 N1 C45 125.1(4) . . ?
C45 N1 C41 121.4(4) . . ?
N1 C41 H41 119.8 . . ?
N1 C41 C42 120.4(4) . . ?
C42 C41 H41 119.8 . . ?
C41 C42 H42 119.9 . . ?
C41 C42 C43 120.2(4) . . ?
C43 C42 H42 119.9 . . ?
C42 C43 H43 120.8 . . ?
C42 C43 C44 118.5(4) . . ?
C44 C43 H43 120.8 . . ?
C43 C44 H44 119.2 . . ?
C43 C44 C45 121.6(4) . . ?
C45 C44 H44 119.2 . . ?
N1 C45 C44 117.9(4) . . ?
N1 C45 C46 123.1(4) . . ?
C44 C45 C46 118.9(4) . . ?
O10 C46 C45 119.3(4) . . ?
O11 C46 O10 124.2(4) . . ?
O11 C46 C45 116.2(4) . . ?
H14A O14 H14B 105.1 . . ?
H15A O15 H15B 101(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C4 177.1(4) . . . . ?
O1 C2 C3 C7 -1.0(6) . . . . ?
O2 C4 C5 C6 177.7(3) . . . . ?
O2 C4 C5 C8 -2.4(6) . . . . ?
O3 C12 C13 C14 -179.3(3) . . . . ?
O3 C12 C13 C17 -2.3(6) . . . . ?
O4 C14 C15 C16 -178.1(3) . . . . ?
O4 C14 C15 C18 2.5(6) . . . . ?
O5 C22 C23 C24 174.6(4) . . . . ?
O5 C22 C23 C27 -4.7(6) . . . . ?
O6 C24 C25 C26 179.0(4) . . . . ?
O6 C24 C25 C28 -3.1(6) . . . . ?
O7 C32 C33 C34 178.9(4) . . . . ?
O7 C32 C33 C37 -5.0(6) . . . . ?
O8 C34 C35 C36 177.8(4) . . . . ?
O8 C34 C35 C38 -4.1(6) . . . . ?
C1 C2 C3 C4 -1.4(6) . . . . ?
C1 C2 C3 C7 -179.5(4) . . . . ?
C1 C38 C39 C40 -59.3(4) . . . . ?
C2 C1 C6 C5 -2.9(6) . . . . ?
C2 C1 C38 C35 -96.6(4) . . . . ?
C2 C1 C38 C39 135.8(4) . . . . ?
C2 C3 C4 O2 -177.1(4) . . . . ?
C2 C3 C4 C5 -1.5(6) . . . . ?
C3 C4 C5 C6 2.1(6) . . . . ?
C3 C4 C5 C8 -178.0(4) . . . . ?
C4 C5 C6 C1 0.2(6) . . . . ?
C4 C5 C8 C9 -133.1(4) . . . . ?
C4 C5 C8 C11 98.6(4) . . . . ?
C5 C8 C9 C10 61.5(5) . . . . ?
C5 C8 C11 C12 -86.6(5) . . . . ?
C5 C8 C11 C16 94.2(4) . . . . ?
C6 C1 C2 O1 -174.9(4) . . . . ?
C6 C1 C2 C3 3.5(6) . . . . ?
C6 C1 C38 C35 83.2(5) . . . . ?
C6 C1 C38 C39 -44.3(5) . . . . ?
C6 C5 C8 C9 46.8(5) . . . . ?
C6 C5 C8 C11 -81.5(5) . . . . ?
C7 C3 C4 O2 1.1(6) . . . . ?
C7 C3 C4 C5 176.6(4) . . . . ?
C8 C5 C6 C1 -179.7(4) . . . . ?
C8 C11 C12 O3 -0.3(6) . . . . ?
C8 C11 C12 C13 -178.7(4) . . . . ?
C8 C11 C16 C15 178.2(3) . . . . ?
C9 C8 C11 C12 145.3(4) . . . . ?
C9 C8 C11 C16 -34.0(5) . . . . ?
C11 C8 C9 C10 -171.3(4) . . . . ?
C11 C12 C13 C14 -0.8(6) . . . . ?
C11 C12 C13 C17 176.3(4) . . . . ?
C12 C11 C16 C15 -1.0(6) . . . . ?
C12 C13 C14 O4 177.9(3) . . . . ?
C12 C13 C14 C15 1.5(6) . . . . ?
C13 C14 C15 C16 -2.0(6) . . . . ?
C13 C14 C15 C18 178.6(4) . . . . ?
C14 C15 C16 C11 1.7(6) . . . . ?
C14 C15 C18 C19 -146.1(4) . . . . ?
C14 C15 C18 C21 86.7(4) . . . . ?
C15 C18 C19 C20 175.1(4) . . . . ?
C15 C18 C21 C22 -99.5(4) . . . . ?
C15 C18 C21 C26 81.2(5) . . . . ?
C16 C11 C12 O3 179.0(4) . . . . ?
C16 C11 C12 C13 0.6(6) . . . . ?
C16 C15 C18 C19 34.5(5) . . . . ?
C16 C15 C18 C21 -92.7(4) . . . . ?
C17 C13 C14 O4 0.8(6) . . . . ?
C17 C13 C14 C15 -175.5(4) . . . . ?
C18 C15 C16 C11 -178.9(3) . . . . ?
C18 C21 C22 O5 5.3(6) . . . . ?
C18 C21 C22 C23 -179.5(4) . . . . ?
C18 C21 C26 C25 178.9(4) . . . . ?
C19 C18 C21 C22 132.6(4) . . . . ?
C19 C18 C21 C26 -46.7(5) . . . . ?
C21 C18 C19 C20 -59.2(5) . . . . ?
C21 C22 C23 C24 -0.5(6) . . . . ?
C21 C22 C23 C27 -179.9(4) . . . . ?
C22 C21 C26 C25 -0.4(6) . . . . ?
C22 C23 C24 O6 -179.4(4) . . . . ?
C22 C23 C24 C25 1.8(6) . . . . ?
C23 C24 C25 C26 -2.2(6) . . . . ?
C23 C24 C25 C28 175.6(4) . . . . ?
C24 C25 C26 C21 1.6(6) . . . . ?
C24 C25 C28 C29 -137.2(4) . . . . ?
C24 C25 C28 C31 95.3(4) . . . . ?
C25 C28 C29 C30 177.2(3) . . . . ?
C25 C28 C31 C32 -93.2(4) . . . . ?
C25 C28 C31 C36 90.9(4) . . . . ?
C26 C21 C22 O5 -175.4(4) . . . . ?
C26 C21 C22 C23 -0.1(6) . . . . ?
C26 C25 C28 C29 40.6(5) . . . . ?
C26 C25 C28 C31 -86.9(5) . . . . ?
C27 C23 C24 O6 -0.1(6) . . . . ?
C27 C23 C24 C25 -178.9(4) . . . . ?
C28 C25 C26 C21 -176.3(4) . . . . ?
C28 C31 C32 O7 2.9(6) . . . . ?
C28 C31 C32 C33 -176.7(4) . . . . ?
C28 C31 C36 C35 176.9(4) . . . . ?
C29 C28 C31 C32 139.8(4) . . . . ?
C29 C28 C31 C36 -36.1(5) . . . . ?
C31 C28 C29 C30 -56.0(5) . . . . ?
C31 C32 C33 C34 -1.5(6) . . . . ?
C31 C32 C33 C37 174.7(4) . . . . ?
C32 C31 C36 C35 0.8(6) . . . . ?
C32 C33 C34 O8 -177.8(4) . . . . ?
C32 C33 C34 C35 3.9(6) . . . . ?
C33 C34 C35 C36 -3.9(6) . . . . ?
C33 C34 C35 C38 174.3(4) . . . . ?
C34 C35 C36 C31 1.5(6) . . . . ?
C34 C35 C38 C1 93.8(4) . . . . ?
C34 C35 C38 C39 -138.0(4) . . . . ?
C35 C38 C39 C40 173.3(3) . . . . ?
C36 C31 C32 O7 178.9(4) . . . . ?
C36 C31 C32 C33 -0.7(6) . . . . ?
C36 C35 C38 C1 -88.1(5) . . . . ?
C36 C35 C38 C39 40.1(5) . . . . ?
C37 C33 C34 O8 6.0(6) . . . . ?
C37 C33 C34 C35 -172.3(4) . . . . ?
C38 C1 C2 O1 5.0(6) . . . . ?
C38 C1 C2 C3 -176.6(4) . . . . ?
C38 C1 C6 C5 177.2(4) . . . . ?
C38 C35 C36 C31 -176.7(4) . . . . ?
Cu1 O9 N1 C41 175.7(3) . . . . ?
Cu1 O9 N1 C45 -2.3(7) . . . . ?
Cu1 O10 C46 O11 -145.9(4) . . . . ?
Cu1 O10 C46 C45 39.5(6) . . . . ?
O9 N1 C41 C42 -177.1(5) . . . . ?
O9 N1 C45 C44 175.8(4) . . . . ?
O9 N1 C45 C46 -7.2(7) . . . . ?
N1 C41 C42 C43 1.2(8) . . . . ?
N1 C45 C46 O10 -12.4(7) . . . . ?
N1 C45 C46 O11 172.6(5) . . . . ?
C41 N1 C45 C44 -2.1(7) . . . . ?
C41 N1 C45 C46 174.9(5) . . . . ?
C41 C42 C43 C44 -2.3(8) . . . . ?
C42 C43 C44 C45 1.2(8) . . . . ?
C43 C44 C45 N1 0.9(7) . . . . ?
C43 C44 C45 C46 -176.1(5) . . . . ?
C44 C45 C46 O10 164.4(4) . . . . ?
C44 C45 C46 O11 -10.6(7) . . . . ?
C45 N1 C41 C42 1.0(7) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5 -18 -1 0.0640 -5.0000 -18.0000 -1.0000 -0.0001 0.6562 0.7650
6 18 1 0.0846 6.0000 18.0000 1.0000 -0.0330 -0.6960 -0.7268
16 0 11 0.0638 16.0000 0.0000 11.0000 -0.0284 -0.7193 0.7391
-16 -2 -11 0.0827 -16.0000 -2.0000 -11.0000 0.0150 0.7693 -0.6316
-4 2 18 0.0263 -4.0000 2.0000 18.0000 0.9673 -0.0268 -0.0516
4 -2 -18 0.0591 4.0000 -2.0000 -18.0000 -0.9673 0.0268 0.0516
-11 5 -15 0.0765 -11.0000 5.0000 -15.0000 -0.2865 0.4257 -0.8632
4 18 2 0.0689 4.0000 18.0000 2.0000 0.0789 -0.6240 -0.7916
-2 -1 20 0.0084 -2.0000 -1.0000 20.0000 0.9722 -0.0465 0.2093
-3 -16 -11 0.0702 -3.0000 -16.0000 -11.0000 -0.5094 0.6022 0.6179

_olex2_submission_special_instructions 'No special instructions were received'
