# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_q6_mgcl2_ephedr_2
_database_code_depnum_ccdc_archive 'CCDC 1868756'
_audit_update_record             
;
2018-11-05 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'cucurbit[6]uril/(-)-ephedrine complex'
_chemical_melting_point          ?
_chemical_formula_moiety         (C36H36N24O12).2(C10H16NO)+.2Cl-.8.6(H2O)
_chemical_formula_sum            'C56 H85 Cl2 N26 O22.6'
_chemical_formula_weight         1555.3

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   12.4801(1)
_cell_length_b                   23.2176(2)
_cell_length_c                   23.4275(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6788.3(1)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    9214
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_F_000             3252
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.194
_shelx_estimated_absorpt_T_min   0.845
_shelx_estimated_absorpt_T_max   0.953
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaApexII
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            44488
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         2.385
_diffrn_reflns_theta_max         28.619
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             17148
_reflns_number_gt                15484
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_max     0.975
_reflns_Friedel_fraction_full    0.998

_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.
;

_computing_data_collection       
'Collect data collection software (Nonius B.V., 1998)'
_computing_cell_refinement       'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0417P)²+9.6497P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 6367 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(4)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         17148
_refine_ls_number_parameters     1026
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1284
_refine_ls_wR_factor_gt          0.1211
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.94596(9) 0.81826(5) 0.49658(5) 0.0304(2) Uani 1 1 d . . . . .
Cl4 Cl 0.78689(10) 0.64102(5) 0.56167(5) 0.0337(2) Uani 1 1 d . . . . .
O7 O 0.9056(2) 0.87757(12) 0.24143(11) 0.0193(5) Uani 1 1 d . . . . .
O9 O 0.8992(2) 1.02192(11) 0.05998(12) 0.0194(5) Uani 1 1 d . . . . .
O8 O 1.0396(2) 0.92475(11) 0.12455(11) 0.0183(5) Uani 1 1 d . . . . .
N17 N 1.0589(3) 1.07143(13) 0.07106(13) 0.0171(6) Uani 1 1 d . . . . .
O10 O 0.6272(2) 1.07128(12) 0.10928(12) 0.0210(6) Uani 1 1 d . . . . .
O2 O 1.2307(2) 1.10871(12) 0.28055(12) 0.0226(6) Uani 1 1 d . . . . .
O11 O 0.4939(2) 1.01948(11) 0.22488(11) 0.0200(5) Uani 1 1 d . . . . .
O6 O 0.8768(2) 1.09269(12) 0.44104(12) 0.0218(6) Uani 1 1 d . . . . .
N21 N 0.5149(3) 1.11671(14) 0.24326(13) 0.0176(6) Uani 1 1 d . . . . .
N18 N 0.9070(3) 1.12086(13) 0.07168(13) 0.0179(6) Uani 1 1 d . . . . .
O1 O 1.1257(2) 1.04343(12) 0.40462(12) 0.0219(6) Uani 1 1 d . . . . .
O4 O 0.8497(2) 1.25871(12) 0.24396(11) 0.0203(6) Uani 1 1 d . . . . .
N14 N 1.0734(3) 0.89829(14) 0.27869(13) 0.0182(6) Uani 1 1 d . . . . .
C14 C 1.1204(3) 0.90962(15) 0.33380(15) 0.0158(7) Uani 1 1 d . . . . .
H14 H 1.1776 0.8810 0.3433 0.019 Uiso 1 1 calc R U . . .
C17 C 1.0936(3) 1.13019(16) 0.07922(15) 0.0169(7) Uani 1 1 d . . . . .
H17 H 1.1504 1.1414 0.0513 0.020 Uiso 1 1 calc R U . . .
N6 N 0.9880(3) 1.20366(13) 0.11961(13) 0.0179(6) Uani 1 1 d . . . . .
N12 N 0.8480(3) 0.99427(13) 0.43563(15) 0.0189(6) Uani 1 1 d . . . . .
N10 N 0.6171(3) 1.12523(13) 0.36958(13) 0.0173(6) Uani 1 1 d . . . . .
N9 N 0.5979(3) 1.19175(13) 0.30223(13) 0.0172(6) Uani 1 1 d . . . . .
N16 N 1.1607(3) 1.00049(13) 0.12417(13) 0.0169(6) Uani 1 1 d . . . . .
O5 O 0.7440(2) 1.19746(11) 0.36227(12) 0.0204(5) Uani 1 1 d . . . . .
N23 N 0.6198(3) 0.98511(13) 0.36407(13) 0.0167(6) Uani 1 1 d . . . . .
O3 O 1.0853(2) 1.21771(12) 0.20212(12) 0.0226(6) Uani 1 1 d . . . . .
N1 N 1.0216(3) 0.96155(13) 0.40227(14) 0.0184(6) Uani 1 1 d . . . . .
C25 C 0.9655(3) 0.88887(15) 0.28159(15) 0.0163(7) Uani 1 1 d . . . . .
C18 C 0.9895(3) 1.16552(16) 0.07061(16) 0.0178(7) Uani 1 1 d . . . . .
H18 H 0.9899 1.1872 0.0338 0.021 Uiso 1 1 calc R U . . .
N2 N 1.1574(3) 0.96827(14) 0.34183(14) 0.0181(6) Uani 1 1 d . . . . .
C36 C 0.8281(3) 0.87822(15) 0.35721(16) 0.0162(7) Uani 1 1 d . . . . .
H36A H 0.7924 0.8549 0.3274 0.019 Uiso 1 1 calc R U . . .
H36B H 0.8344 0.8541 0.3919 0.019 Uiso 1 1 calc R U . . .
C4 C 1.2296(3) 1.13041(16) 0.15992(16) 0.0183(7) Uani 1 1 d . . . . .
H4A H 1.2817 1.1308 0.1280 0.022 Uiso 1 1 calc R U . . .
H4B H 1.2515 1.1605 0.1875 0.022 Uiso 1 1 calc R U . . .
N15 N 1.1638(3) 0.93849(13) 0.19606(13) 0.0175(6) Uani 1 1 d . . . . .
N20 N 0.5849(3) 1.15643(14) 0.15497(13) 0.0177(6) Uani 1 1 d . . . . .
N4 N 1.2334(3) 1.07491(13) 0.18766(14) 0.0185(6) Uani 1 1 d . . . . .
C34 C 0.5125(3) 1.00108(16) 0.34663(16) 0.0183(7) Uani 1 1 d . . . . .
H34A H 0.4663 1.0033 0.3809 0.022 Uiso 1 1 calc R U . . .
H34B H 0.4834 0.9705 0.3216 0.022 Uiso 1 1 calc R U . . .
C7 C 0.7881(3) 1.24103(15) 0.20670(16) 0.0178(7) Uani 1 1 d . . . . .
C3 C 1.2343(3) 1.06906(16) 0.24646(15) 0.0168(7) Uani 1 1 d . . . . .
N5 N 1.1240(3) 1.14431(14) 0.13788(13) 0.0172(6) Uani 1 1 d . . . . .
C10 C 0.6487(3) 1.10621(15) 0.42622(15) 0.0166(7) Uani 1 1 d . . . . .
H10A H 0.6919 1.1369 0.4444 0.020 Uiso 1 1 calc R U . . .
H10B H 0.5834 1.1008 0.4496 0.020 Uiso 1 1 calc R U . . .
C5 C 1.0678(3) 1.19111(16) 0.15776(15) 0.0177(7) Uani 1 1 d . . . . .
C27 C 1.1142(3) 0.95226(15) 0.14631(16) 0.0160(7) Uani 1 1 d . . . . .
C13 C 1.0239(3) 0.90509(16) 0.37567(15) 0.0165(7) Uani 1 1 d . . . . .
H13 H 1.0343 0.8737 0.4044 0.020 Uiso 1 1 calc R U . . .
N8 N 0.6849(3) 1.22380(14) 0.21487(13) 0.0181(6) Uani 1 1 d . . . . .
C19 C 0.7234(3) 1.21310(16) 0.11733(15) 0.0182(7) Uani 1 1 d . . . . .
H19 H 0.7071 1.2370 0.0829 0.022 Uiso 1 1 calc R U . . .
N3 N 1.2414(3) 1.01152(13) 0.25875(13) 0.0181(6) Uani 1 1 d . . . . .
N11 N 0.7100(3) 1.05321(13) 0.42675(13) 0.0175(6) Uani 1 1 d . . . . .
O12 O 0.6492(3) 0.92036(15) 0.29197(14) 0.0364(8) Uani 1 1 d . . . . .
C31 C 0.6462(3) 1.12131(16) 0.12110(15) 0.0174(7) Uani 1 1 d . . . . .
C16 C 1.2503(3) 1.02061(15) 0.15822(16) 0.0173(7) Uani 1 1 d . . . . .
H16 H 1.3184 1.0209 0.1357 0.021 Uiso 1 1 calc R U . . .
C26 C 1.1375(3) 0.88734(16) 0.22822(16) 0.0181(7) Uani 1 1 d . . . . .
H26A H 1.2048 0.8681 0.2399 0.022 Uiso 1 1 calc R U . . .
H26B H 1.0979 0.8605 0.2031 0.022 Uiso 1 1 calc R U . . .
C15 C 1.2550(3) 0.97610(16) 0.20834(16) 0.0173(7) Uani 1 1 d . . . . .
H15 H 1.3243 0.9545 0.2090 0.021 Uiso 1 1 calc R U . . .
N7 N 0.8119(3) 1.23651(13) 0.15001(13) 0.0173(6) Uani 1 1 d . . . . .
C6 C 0.9155(3) 1.25148(15) 0.12665(16) 0.0181(7) Uani 1 1 d . . . . .
H6A H 0.9047 1.2700 0.0890 0.022 Uiso 1 1 calc R U . . .
H6B H 0.9496 1.2802 0.1520 0.022 Uiso 1 1 calc R U . . .
C2 C 1.2549(3) 0.99025(16) 0.31650(16) 0.0189(7) Uani 1 1 d . . . . .
H2A H 1.3093 0.9592 0.3162 0.023 Uiso 1 1 calc R U . . .
H2B H 1.2828 1.0219 0.3407 0.023 Uiso 1 1 calc R U . . .
C12 C 0.9551(3) 0.97591(16) 0.45082(15) 0.0184(7) Uani 1 1 d . . . . .
H12A H 0.9903 1.0071 0.4728 0.022 Uiso 1 1 calc R U . . .
H12B H 0.9499 0.9418 0.4760 0.022 Uiso 1 1 calc R U . . .
C23 C 0.6614(3) 0.99679(15) 0.42051(15) 0.0159(7) Uani 1 1 d . . . . .
H23 H 0.6070 0.9891 0.4509 0.019 Uiso 1 1 calc R U . . .
N24 N 0.7618(3) 0.92748(14) 0.37007(13) 0.0178(6) Uani 1 1 d . . . . .
N19 N 0.7337(3) 1.15259(13) 0.10333(13) 0.0166(6) Uani 1 1 d . . . . .
C33 C 0.5051(3) 1.05915(16) 0.25788(15) 0.0168(7) Uani 1 1 d . . . . .
N13 N 0.9347(3) 0.89315(14) 0.33771(13) 0.0180(6) Uani 1 1 d . . . . .
C32 C 0.4925(3) 1.13628(16) 0.18551(15) 0.0182(7) Uani 1 1 d . . . . .
H32A H 0.4599 1.1041 0.1638 0.022 Uiso 1 1 calc R U . . .
H32B H 0.4392 1.1678 0.1873 0.022 Uiso 1 1 calc R U . . .
C1 C 1.1041(3) 0.99590(16) 0.38494(15) 0.0176(7) Uani 1 1 d . . . . .
C29 C 0.9501(3) 1.06656(16) 0.06670(15) 0.0164(7) Uani 1 1 d . . . . .
N22 N 0.5076(3) 1.05574(13) 0.31661(13) 0.0175(6) Uani 1 1 d . . . . .
C28 C 1.1315(3) 1.02309(16) 0.06851(16) 0.0186(7) Uani 1 1 d . . . . .
H28A H 1.1975 1.0351 0.0483 0.022 Uiso 1 1 calc R U . . .
H28B H 1.0978 0.9919 0.0459 0.022 Uiso 1 1 calc R U . . .
C22 C 0.5140(3) 1.11140(16) 0.34401(15) 0.0165(7) Uani 1 1 d . . . . .
H22 H 0.4538 1.1173 0.3716 0.020 Uiso 1 1 calc R U . . .
C30 C 0.7975(3) 1.13242(16) 0.05584(15) 0.0178(7) Uani 1 1 d . . . . .
H30A H 0.7650 1.0968 0.0404 0.021 Uiso 1 1 calc R U . . .
H30B H 0.7965 1.1618 0.0252 0.021 Uiso 1 1 calc R U . . .
C11 C 0.8172(3) 1.05086(16) 0.43446(15) 0.0169(7) Uani 1 1 d . . . . .
N1X N 0.9579(3) 1.18621(14) 0.32234(15) 0.0221(7) Uani 1 1 d . . . . .
H1X1 H 0.9052 1.1879 0.3539 0.027 Uiso 1 1 calc R U . . .
H1X2 H 0.9310 1.2113 0.2913 0.027 Uiso 1 1 calc R U . . .
N1Y N 0.8198(3) 0.94794(14) 0.15043(14) 0.0181(6) Uani 1 1 d . . . . .
H1Y1 H 0.8360 0.9133 0.1734 0.022 Uiso 1 1 calc R U . . .
H1Y2 H 0.8802 0.9537 0.1236 0.022 Uiso 1 1 calc R U . . .
C1X C 0.9620(4) 1.12598(17) 0.30075(18) 0.0251(8) Uani 1 1 d . . . . .
H1X6 H 1.0153 1.1232 0.2701 0.038 Uiso 1 1 calc R U . . .
H1X7 H 0.8915 1.1150 0.2859 0.038 Uiso 1 1 calc R U . . .
H1X3 H 0.9820 1.1000 0.3320 0.038 Uiso 1 1 calc R U . . .
C1Y C 0.8150(3) 0.99870(18) 0.18961(18) 0.0241(8) Uani 1 1 d . . . . .
H1Y5 H 0.7887 1.0323 0.1686 0.036 Uiso 1 1 calc R U . . .
H1Y6 H 0.8868 1.0068 0.2046 0.036 Uiso 1 1 calc R U . . .
H1Y3 H 0.7663 0.9903 0.2214 0.036 Uiso 1 1 calc R U . . .
C9 C 0.6619(3) 1.17333(15) 0.34600(15) 0.0167(7) Uani 1 1 d . . . . .
O2W O 1.0512(3) 0.86948(15) 0.01828(13) 0.0282(7) Uani 1 1 d . . . . .
H2W1 H 1.048(5) 0.883(3) 0.054(3) 0.042 Uiso 1 1 d . U . . .
H2W2 H 1.063(5) 0.834(3) 0.021(3) 0.042 Uiso 1 1 d . U . . .
O1X O 1.0102(3) 1.18494(14) 0.43808(13) 0.0302(7) Uani 1 1 d . . . . .
H1X H 0.9745 1.1543 0.4389 0.045 Uiso 1 1 calc R U . . .
C24 C 0.7594(3) 0.95574(15) 0.42526(15) 0.0160(7) Uani 1 1 d . . . . .
H24 H 0.7504 0.9274 0.4571 0.019 Uiso 1 1 calc R U . . .
C21 C 0.5069(3) 1.15418(16) 0.29270(15) 0.0165(7) Uani 1 1 d . . . . .
H21 H 0.4379 1.1761 0.2929 0.020 Uiso 1 1 calc R U . . .
O1W O 1.1548(3) 0.94424(15) -0.05840(14) 0.0303(7) Uani 1 1 d . . . . .
H1W1 H 1.144(5) 0.919(3) -0.035(3) 0.045 Uiso 1 1 d . U . . .
H1W2 H 1.229(5) 0.939(3) -0.063(3) 0.045 Uiso 1 1 d . U . . .
O3W O 0.5438(4) 0.88239(18) 0.43942(17) 0.0432(9) Uani 1 1 d . . . . .
H3W1 H 0.476(6) 0.881(3) 0.435(3) 0.065 Uiso 1 1 d . U . . .
H3W2 H 0.561(6) 0.849(3) 0.426(3) 0.065 Uiso 1 1 d . U . . .
C20 C 0.6299(3) 1.21335(16) 0.16062(15) 0.0179(7) Uani 1 1 d . . . . .
H20 H 0.5762 1.2441 0.1519 0.022 Uiso 1 1 calc R U . . .
O1Y O 0.6656(2) 0.87117(11) 0.18990(11) 0.0189(5) Uani 1 1 d . . . . .
H1Y H 0.6639 0.8792 0.2249 0.028 Uiso 1 1 calc R U . . .
C3Y C 0.7459(3) 0.88949(17) 0.07338(16) 0.0211(8) Uani 1 1 d . . . . .
H3Y1 H 0.8118 0.8996 0.0529 0.032 Uiso 1 1 calc R U . . .
H3Y2 H 0.6869 0.8856 0.0461 0.032 Uiso 1 1 calc R U . . .
H3Y3 H 0.7563 0.8529 0.0935 0.032 Uiso 1 1 calc R U . . .
C4Y C 0.6297(3) 0.91976(15) 0.15759(15) 0.0166(7) Uani 1 1 d . . . . .
H4Y H 0.6176 0.9526 0.1844 0.020 Uiso 1 1 calc R U . . .
C6Y C 0.4816(3) 0.94834(16) 0.08986(16) 0.0191(7) Uani 1 1 d . . . . .
H6Y H 0.5177 0.9839 0.0841 0.023 Uiso 1 1 calc R U . . .
C8 C 0.6260(3) 1.23997(16) 0.26612(15) 0.0190(7) Uani 1 1 d . . . . .
H8A H 0.6700 1.2674 0.2885 0.023 Uiso 1 1 calc R U . . .
H8B H 0.5595 1.2602 0.2547 0.023 Uiso 1 1 calc R U . . .
C35 C 0.6748(3) 0.94197(17) 0.33758(16) 0.0195(7) Uani 1 1 d . . . . .
C5Y C 0.5253(3) 0.90731(16) 0.12666(15) 0.0157(7) Uani 1 1 d . . . . .
C2Y C 0.7195(3) 0.93645(16) 0.11610(15) 0.0173(7) Uani 1 1 d . . . . .
H2Y H 0.6986 0.9723 0.0951 0.021 Uiso 1 1 calc R U . . .
C7Y C 0.3857(3) 0.93762(17) 0.06145(17) 0.0208(7) Uani 1 1 d . . . . .
H7Y H 0.3574 0.9655 0.0359 0.025 Uiso 1 1 calc R U . . .
C10Y C 0.4696(3) 0.85627(17) 0.13598(16) 0.0210(8) Uani 1 1 d . . . . .
H10Y H 0.4974 0.8283 0.1616 0.025 Uiso 1 1 calc R U . . .
C3X C 1.0952(3) 1.17924(16) 0.39810(16) 0.0180(7) Uani 1 1 d . . . . .
H3X H 1.1069 1.1375 0.3895 0.022 Uiso 1 1 calc R U . . .
C2X C 1.0620(3) 1.21062(16) 0.34341(17) 0.0200(7) Uani 1 1 d . . . . .
H2X H 1.1183 1.2046 0.3137 0.024 Uiso 1 1 calc R U . . .
C9Y C 0.3732(3) 0.84602(18) 0.10786(18) 0.0244(8) Uani 1 1 d . . . . .
H9Y H 0.3357 0.8110 0.1145 0.029 Uiso 1 1 calc R U . . .
C8Y C 0.3313(3) 0.88636(18) 0.07027(18) 0.0233(8) Uani 1 1 d . . . . .
H8Y H 0.2660 0.8789 0.0508 0.028 Uiso 1 1 calc R U . . .
C4X C 1.0442(4) 1.27492(19) 0.3516(2) 0.0387(12) Uani 1 1 d . . . . .
H4X1 H 1.0251 1.2925 0.3149 0.058 Uiso 1 1 calc R U . . .
H4X2 H 1.1100 1.2927 0.3661 0.058 Uiso 1 1 calc R U . . .
H4X3 H 0.9859 1.2811 0.3790 0.058 Uiso 1 1 calc R U . . .
O5W O 0.6325(3) 0.59355(17) 0.46132(18) 0.0413(9) Uani 1 1 d . . . . .
H5W1 H 0.573(6) 0.615(3) 0.468(3) 0.062 Uiso 1 1 d . U . . .
H5W2 H 0.668(6) 0.605(3) 0.491(3) 0.062 Uiso 1 1 d . U . . .
C5X C 1.1979(3) 1.20505(15) 0.42135(15) 0.0161(7) Uani 1 1 d . . . . .
O6W O 0.7665(4) 0.73568(17) 0.4622(2) 0.0557(12) Uani 1 1 d . . . . .
H6W1 H 0.828(7) 0.765(4) 0.467(3) 0.084 Uiso 1 1 d . U . . .
H6W2 H 0.757(7) 0.713(4) 0.489(4) 0.084 Uiso 1 1 d . U . . .
C6X C 1.2027(3) 1.23036(17) 0.47550(16) 0.0201(7) Uani 1 1 d . . . . .
H6X H 1.1407 1.2307 0.4990 0.024 Uiso 1 1 calc R U . . .
O7W O 0.8868(3) 0.63902(15) 0.69086(17) 0.0373(8) Uani 1 1 d . . . . .
H7W1 H 0.953(6) 0.642(3) 0.691(3) 0.056 Uiso 1 1 d . U . . .
H7W2 H 0.876(6) 0.642(3) 0.653(3) 0.056 Uiso 1 1 d . U . . .
C7X C 1.2971(3) 1.25500(17) 0.49520(17) 0.0215(8) Uani 1 1 d . . . . .
H7X H 1.2996 1.2716 0.5323 0.026 Uiso 1 1 calc R U . . .
C8X C 1.3878(3) 1.25550(17) 0.46089(17) 0.0228(8) Uani 1 1 d . . . . .
H8X H 1.4521 1.2730 0.4741 0.027 Uiso 1 1 calc R U . . .
C10X C 1.2900(3) 1.20479(17) 0.38801(17) 0.0212(8) Uani 1 1 d . . . . .
H10X H 1.2887 1.1869 0.3516 0.025 Uiso 1 1 calc R U . . .
C9X C 1.3839(3) 1.23025(17) 0.40710(18) 0.0227(8) Uani 1 1 d . . . . .
H9X H 1.4457 1.2304 0.3834 0.027 Uiso 1 1 calc R U . . .
O9W O 1.4284(5) 1.2930(3) 0.1885(3) 0.050(2) Uani 0.621(9) 1 d . . P A 1
O4W O 0.5818(5) 0.7653(3) 0.4250(3) 0.0451(18) Uani 0.621(9) 1 d . . P A 1
O8W O 1.2597(10) 1.2677(7) 0.2546(6) 0.045(3) Uani 0.621(9) 1 d . . P A 1
O9WA O 1.3900(8) 1.2783(5) 0.1332(5) 0.050(3) Uani 0.379(9) 1 d . . P A 2
O8WA O 1.2946(14) 1.2630(10) 0.2440(9) 0.032(3) Uani 0.379(9) 1 d . . P 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
O7 C25 1.230(5) . ?
O9 C29 1.226(4) . ?
O8 C27 1.239(4) . ?
N17 C29 1.365(5) . ?
N17 C28 1.444(5) . ?
N17 C17 1.444(5) . ?
O10 C31 1.218(5) . ?
O2 C3 1.219(5) . ?
O11 C33 1.210(5) . ?
O6 C11 1.233(4) . ?
N21 C33 1.385(5) . ?
N21 C21 1.452(5) . ?
N21 C32 1.454(5) . ?
N18 C29 1.376(5) . ?
N18 C30 1.441(5) . ?
N18 C18 1.462(5) . ?
O1 C1 1.226(5) . ?
O4 C7 1.233(5) . ?
N14 C25 1.366(5) . ?
N14 C14 1.442(5) . ?
N14 C26 1.450(5) . ?
C14 N2 1.450(5) . ?
C14 C13 1.556(5) . ?
C14 H14 1.0000 . ?
C17 N5 1.463(5) . ?
C17 C18 1.549(5) . ?
C17 H17 1.0000 . ?
N6 C5 1.369(5) . ?
N6 C6 1.442(5) . ?
N6 C18 1.450(5) . ?
N12 C11 1.369(5) . ?
N12 C24 1.443(5) . ?
N12 C12 1.447(5) . ?
N10 C9 1.366(5) . ?
N10 C10 1.453(5) . ?
N10 C22 1.455(5) . ?
N9 C9 1.368(5) . ?
N9 C8 1.446(5) . ?
N9 C21 1.450(5) . ?
N16 C27 1.364(5) . ?
N16 C16 1.451(5) . ?
N16 C28 1.452(5) . ?
O5 C9 1.229(5) . ?
N23 C35 1.364(5) . ?
N23 C23 1.446(5) . ?
N23 C34 1.448(5) . ?
O3 C5 1.228(5) . ?
N1 C1 1.365(5) . ?
N1 C12 1.447(5) . ?
N1 C13 1.452(5) . ?
C25 N13 1.373(5) . ?
C18 H18 1.0000 . ?
N2 C1 1.369(5) . ?
N2 C2 1.447(5) . ?
C36 N24 1.444(5) . ?
C36 N13 1.449(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C4 N4 1.444(5) . ?
C4 N5 1.452(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N15 C27 1.358(5) . ?
N15 C26 1.444(5) . ?
N15 C15 1.463(5) . ?
N20 C31 1.371(5) . ?
N20 C32 1.435(5) . ?
N20 C20 1.442(5) . ?
N4 C3 1.384(5) . ?
N4 C16 1.452(5) . ?
C34 N22 1.452(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C7 N8 1.363(5) . ?
C7 N7 1.365(5) . ?
C3 N3 1.370(5) . ?
N5 C5 1.374(5) . ?
C10 N11 1.449(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C13 N13 1.451(5) . ?
C13 H13 1.0000 . ?
N8 C8 1.457(5) . ?
N8 C20 1.465(5) . ?
C19 N19 1.448(5) . ?
C19 N7 1.450(5) . ?
C19 C20 1.546(5) . ?
C19 H19 1.0000 . ?
N3 C15 1.449(5) . ?
N3 C2 1.450(5) . ?
N11 C11 1.351(5) . ?
N11 C23 1.451(5) . ?
O12 C35 1.223(5) . ?
C31 N19 1.375(5) . ?
C16 C15 1.565(5) . ?
C16 H16 1.0000 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C15 H15 1.0000 . ?
N7 C6 1.447(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C23 C24 1.554(5) . ?
C23 H23 1.0000 . ?
N24 C35 1.368(5) . ?
N24 C24 1.450(4) . ?
N19 C30 1.446(5) . ?
C33 N22 1.379(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
N22 C22 1.445(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C22 C21 1.562(5) . ?
C22 H22 1.0000 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
N1X C1X 1.488(5) . ?
N1X C2X 1.500(5) . ?
N1X H1X1 0.9900 . ?
N1X H1X2 0.9900 . ?
N1Y C1Y 1.495(5) . ?
N1Y C2Y 1.512(5) . ?
N1Y H1Y1 0.9900 . ?
N1Y H1Y2 0.9900 . ?
C1X H1X6 0.9800 . ?
C1X H1X7 0.9800 . ?
C1X H1X3 0.9800 . ?
C1Y H1Y5 0.9800 . ?
C1Y H1Y6 0.9800 . ?
C1Y H1Y3 0.9800 . ?
O2W H2W1 0.89(6) . ?
O2W H2W2 0.84(6) . ?
O1X C3X 1.421(5) . ?
O1X H1X 0.8400 . ?
C24 H24 1.0000 . ?
C21 H21 1.0000 . ?
O1W H1W1 0.81(7) . ?
O1W H1W2 0.94(7) . ?
O3W H3W1 0.85(8) . ?
O3W H3W2 0.86(8) . ?
C20 H20 1.0000 . ?
O1Y C4Y 1.431(4) . ?
O1Y H1Y 0.8400 . ?
C3Y C2Y 1.516(5) . ?
C3Y H3Y1 0.9800 . ?
C3Y H3Y2 0.9800 . ?
C3Y H3Y3 0.9800 . ?
C4Y C5Y 1.519(5) . ?
C4Y C2Y 1.534(5) . ?
C4Y H4Y 1.0000 . ?
C6Y C7Y 1.393(5) . ?
C6Y C5Y 1.395(5) . ?
C6Y H6Y 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C5Y C10Y 1.391(5) . ?
C2Y H2Y 1.0000 . ?
C7Y C8Y 1.385(6) . ?
C7Y H7Y 0.9500 . ?
C10Y C9Y 1.392(5) . ?
C10Y H10Y 0.9500 . ?
C3X C5X 1.516(5) . ?
C3X C2X 1.531(5) . ?
C3X H3X 1.0000 . ?
C2X C4X 1.521(6) . ?
C2X H2X 1.0000 . ?
C9Y C8Y 1.388(6) . ?
C9Y H9Y 0.9500 . ?
C8Y H8Y 0.9500 . ?
C4X H4X1 0.9800 . ?
C4X H4X2 0.9800 . ?
C4X H4X3 0.9800 . ?
O5W H5W1 0.90(8) . ?
O5W H5W2 0.87(8) . ?
C5X C10X 1.390(5) . ?
C5X C6X 1.399(5) . ?
O6W H6W1 1.04(9) . ?
O6W H6W2 0.82(9) . ?
C6X C7X 1.389(6) . ?
C6X H6X 0.9500 . ?
O7W H7W1 0.83(7) . ?
O7W H7W2 0.90(7) . ?
C7X C8X 1.388(6) . ?
C7X H7X 0.9500 . ?
C8X C9X 1.391(6) . ?
C8X H8X 0.9500 . ?
C10X C9X 1.386(6) . ?
C10X H10X 0.9500 . ?
C9X H9X 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
C29 N17 C28 123.8(3) . . ?
C29 N17 C17 112.7(3) . . ?
C28 N17 C17 123.5(3) . . ?
C33 N21 C21 112.0(3) . . ?
C33 N21 C32 121.0(3) . . ?
C21 N21 C32 122.8(3) . . ?
C29 N18 C30 121.3(3) . . ?
C29 N18 C18 111.9(3) . . ?
C30 N18 C18 122.1(3) . . ?
C25 N14 C14 112.7(3) . . ?
C25 N14 C26 123.8(3) . . ?
C14 N14 C26 122.6(3) . . ?
N14 C14 N2 114.6(3) . . ?
N14 C14 C13 103.8(3) . . ?
N2 C14 C13 103.2(3) . . ?
N14 C14 H14 111.6 . . ?
N2 C14 H14 111.6 . . ?
C13 C14 H14 111.6 . . ?
N17 C17 N5 114.5(3) . . ?
N17 C17 C18 103.4(3) . . ?
N5 C17 C18 102.8(3) . . ?
N17 C17 H17 111.8 . . ?
N5 C17 H17 111.8 . . ?
C18 C17 H17 111.8 . . ?
C5 N6 C6 123.1(3) . . ?
C5 N6 C18 112.2(3) . . ?
C6 N6 C18 124.7(3) . . ?
C11 N12 C24 112.1(3) . . ?
C11 N12 C12 123.2(3) . . ?
C24 N12 C12 124.5(3) . . ?
C9 N10 C10 120.4(3) . . ?
C9 N10 C22 112.1(3) . . ?
C10 N10 C22 123.3(3) . . ?
C9 N9 C8 122.6(3) . . ?
C9 N9 C21 112.6(3) . . ?
C8 N9 C21 124.4(3) . . ?
C27 N16 C16 112.5(3) . . ?
C27 N16 C28 122.1(3) . . ?
C16 N16 C28 124.8(3) . . ?
C35 N23 C23 111.9(3) . . ?
C35 N23 C34 121.7(3) . . ?
C23 N23 C34 122.8(3) . . ?
C1 N1 C12 122.2(3) . . ?
C1 N1 C13 112.6(3) . . ?
C12 N1 C13 123.8(3) . . ?
O7 C25 N14 126.5(4) . . ?
O7 C25 N13 125.3(4) . . ?
N14 C25 N13 108.2(3) . . ?
N6 C18 N18 114.2(3) . . ?
N6 C18 C17 103.4(3) . . ?
N18 C18 C17 102.3(3) . . ?
N6 C18 H18 112.1 . . ?
N18 C18 H18 112.1 . . ?
C17 C18 H18 112.1 . . ?
C1 N2 C2 123.1(3) . . ?
C1 N2 C14 112.4(3) . . ?
C2 N2 C14 123.1(3) . . ?
N24 C36 N13 113.8(3) . . ?
N24 C36 H36A 108.8 . . ?
N13 C36 H36A 108.8 . . ?
N24 C36 H36B 108.8 . . ?
N13 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?
N4 C4 N5 112.8(3) . . ?
N4 C4 H4A 109.0 . . ?
N5 C4 H4A 109.0 . . ?
N4 C4 H4B 109.0 . . ?
N5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C27 N15 C26 122.5(3) . . ?
C27 N15 C15 112.5(3) . . ?
C26 N15 C15 124.4(3) . . ?
C31 N20 C32 122.9(3) . . ?
C31 N20 C20 112.4(3) . . ?
C32 N20 C20 124.4(3) . . ?
C3 N4 C4 122.4(3) . . ?
C3 N4 C16 112.7(3) . . ?
C4 N4 C16 124.4(3) . . ?
N23 C34 N22 113.6(3) . . ?
N23 C34 H34A 108.9 . . ?
N22 C34 H34A 108.9 . . ?
N23 C34 H34B 108.9 . . ?
N22 C34 H34B 108.9 . . ?
H34A C34 H34B 107.7 . . ?
O4 C7 N8 126.0(4) . . ?
O4 C7 N7 125.4(4) . . ?
N8 C7 N7 108.6(3) . . ?
O2 C3 N3 126.9(3) . . ?
O2 C3 N4 125.3(4) . . ?
N3 C3 N4 107.8(3) . . ?
C5 N5 C4 121.2(3) . . ?
C5 N5 C17 111.3(3) . . ?
C4 N5 C17 121.3(3) . . ?
N11 C10 N10 114.2(3) . . ?
N11 C10 H10A 108.7 . . ?
N10 C10 H10A 108.7 . . ?
N11 C10 H10B 108.7 . . ?
N10 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
O3 C5 N6 125.0(4) . . ?
O3 C5 N5 126.4(4) . . ?
N6 C5 N5 108.6(3) . . ?
O8 C27 N15 125.1(3) . . ?
O8 C27 N16 125.9(3) . . ?
N15 C27 N16 109.0(3) . . ?
N13 C13 N1 114.9(3) . . ?
N13 C13 C14 102.7(3) . . ?
N1 C13 C14 103.0(3) . . ?
N13 C13 H13 111.9 . . ?
N1 C13 H13 111.9 . . ?
C14 C13 H13 111.9 . . ?
C7 N8 C8 121.1(3) . . ?
C7 N8 C20 111.7(3) . . ?
C8 N8 C20 121.4(3) . . ?
N19 C19 N7 114.6(3) . . ?
N19 C19 C20 102.6(3) . . ?
N7 C19 C20 103.1(3) . . ?
N19 C19 H19 111.9 . . ?
N7 C19 H19 111.9 . . ?
C20 C19 H19 111.9 . . ?
C3 N3 C15 113.0(3) . . ?
C3 N3 C2 122.4(3) . . ?
C15 N3 C2 123.6(3) . . ?
C11 N11 C10 123.9(3) . . ?
C11 N11 C23 113.0(3) . . ?
C10 N11 C23 123.1(3) . . ?
O10 C31 N20 126.1(4) . . ?
O10 C31 N19 126.2(4) . . ?
N20 C31 N19 107.7(3) . . ?
N16 C16 N4 115.4(3) . . ?
N16 C16 C15 103.2(3) . . ?
N4 C16 C15 102.8(3) . . ?
N16 C16 H16 111.6 . . ?
N4 C16 H16 111.6 . . ?
C15 C16 H16 111.6 . . ?
N15 C26 N14 114.0(3) . . ?
N15 C26 H26A 108.7 . . ?
N14 C26 H26A 108.7 . . ?
N15 C26 H26B 108.7 . . ?
N14 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
N3 C15 N15 114.0(3) . . ?
N3 C15 C16 103.4(3) . . ?
N15 C15 C16 102.5(3) . . ?
N3 C15 H15 112.0 . . ?
N15 C15 H15 112.0 . . ?
C16 C15 H15 112.0 . . ?
C7 N7 C6 122.9(3) . . ?
C7 N7 C19 112.2(3) . . ?
C6 N7 C19 124.9(3) . . ?
N6 C6 N7 114.8(3) . . ?
N6 C6 H6A 108.6 . . ?
N7 C6 H6A 108.6 . . ?
N6 C6 H6B 108.6 . . ?
N7 C6 H6B 108.6 . . ?
H6A C6 H6B 107.5 . . ?
N2 C2 N3 113.8(3) . . ?
N2 C2 H2A 108.8 . . ?
N3 C2 H2A 108.8 . . ?
N2 C2 H2B 108.8 . . ?
N3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
N1 C12 N12 113.8(3) . . ?
N1 C12 H12A 108.8 . . ?
N12 C12 H12A 108.8 . . ?
N1 C12 H12B 108.8 . . ?
N12 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
N23 C23 N11 114.3(3) . . ?
N23 C23 C24 103.5(3) . . ?
N11 C23 C24 102.6(3) . . ?
N23 C23 H23 111.9 . . ?
N11 C23 H23 111.9 . . ?
C24 C23 H23 111.9 . . ?
C35 N24 C36 122.3(3) . . ?
C35 N24 C24 111.6(3) . . ?
C36 N24 C24 123.8(3) . . ?
C31 N19 C30 119.9(3) . . ?
C31 N19 C19 111.9(3) . . ?
C30 N19 C19 122.5(3) . . ?
O11 C33 N22 126.6(4) . . ?
O11 C33 N21 125.9(3) . . ?
N22 C33 N21 107.5(3) . . ?
C25 N13 C36 122.8(3) . . ?
C25 N13 C13 112.7(3) . . ?
C36 N13 C13 123.8(3) . . ?
N20 C32 N21 114.3(3) . . ?
N20 C32 H32A 108.7 . . ?
N21 C32 H32A 108.7 . . ?
N20 C32 H32B 108.7 . . ?
N21 C32 H32B 108.7 . . ?
H32A C32 H32B 107.6 . . ?
O1 C1 N1 125.4(4) . . ?
O1 C1 N2 126.4(4) . . ?
N1 C1 N2 108.2(3) . . ?
O9 C29 N17 126.5(4) . . ?
O9 C29 N18 125.6(3) . . ?
N17 C29 N18 107.9(3) . . ?
C33 N22 C22 113.2(3) . . ?
C33 N22 C34 122.3(3) . . ?
C22 N22 C34 124.3(3) . . ?
N17 C28 N16 113.7(3) . . ?
N17 C28 H28A 108.8 . . ?
N16 C28 H28A 108.8 . . ?
N17 C28 H28B 108.8 . . ?
N16 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
N22 C22 N10 115.4(3) . . ?
N22 C22 C21 102.9(3) . . ?
N10 C22 C21 103.1(3) . . ?
N22 C22 H22 111.6 . . ?
N10 C22 H22 111.6 . . ?
C21 C22 H22 111.6 . . ?
N18 C30 N19 112.6(3) . . ?
N18 C30 H30A 109.1 . . ?
N19 C30 H30A 109.1 . . ?
N18 C30 H30B 109.1 . . ?
N19 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
O6 C11 N11 125.6(4) . . ?
O6 C11 N12 125.7(4) . . ?
N11 C11 N12 108.6(3) . . ?
C1X N1X C2X 115.9(3) . . ?
C1X N1X H1X1 108.3 . . ?
C2X N1X H1X1 108.3 . . ?
C1X N1X H1X2 108.3 . . ?
C2X N1X H1X2 108.3 . . ?
H1X1 N1X H1X2 107.4 . . ?
C1Y N1Y C2Y 115.6(3) . . ?
C1Y N1Y H1Y1 108.4 . . ?
C2Y N1Y H1Y1 108.4 . . ?
C1Y N1Y H1Y2 108.4 . . ?
C2Y N1Y H1Y2 108.4 . . ?
H1Y1 N1Y H1Y2 107.4 . . ?
N1X C1X H1X6 109.5 . . ?
N1X C1X H1X7 109.5 . . ?
H1X6 C1X H1X7 109.5 . . ?
N1X C1X H1X3 109.5 . . ?
H1X6 C1X H1X3 109.5 . . ?
H1X7 C1X H1X3 109.5 . . ?
N1Y C1Y H1Y5 109.5 . . ?
N1Y C1Y H1Y6 109.5 . . ?
H1Y5 C1Y H1Y6 109.5 . . ?
N1Y C1Y H1Y3 109.5 . . ?
H1Y5 C1Y H1Y3 109.5 . . ?
H1Y6 C1Y H1Y3 109.5 . . ?
O5 C9 N10 126.1(3) . . ?
O5 C9 N9 125.2(3) . . ?
N10 C9 N9 108.7(3) . . ?
H2W1 O2W H2W2 106(6) . . ?
C3X O1X H1X 109.5 . . ?
N12 C24 N24 114.5(3) . . ?
N12 C24 C23 103.6(3) . . ?
N24 C24 C23 103.3(3) . . ?
N12 C24 H24 111.6 . . ?
N24 C24 H24 111.6 . . ?
C23 C24 H24 111.6 . . ?
N9 C21 N21 115.4(3) . . ?
N9 C21 C22 102.7(3) . . ?
N21 C21 C22 103.2(3) . . ?
N9 C21 H21 111.6 . . ?
N21 C21 H21 111.6 . . ?
C22 C21 H21 111.6 . . ?
H1W1 O1W H1W2 99(6) . . ?
H3W1 O3W H3W2 100(7) . . ?
N20 C20 N8 114.4(3) . . ?
N20 C20 C19 103.3(3) . . ?
N8 C20 C19 102.5(3) . . ?
N20 C20 H20 112.0 . . ?
N8 C20 H20 112.0 . . ?
C19 C20 H20 112.0 . . ?
C4Y O1Y H1Y 109.5 . . ?
C2Y C3Y H3Y1 109.5 . . ?
C2Y C3Y H3Y2 109.5 . . ?
H3Y1 C3Y H3Y2 109.5 . . ?
C2Y C3Y H3Y3 109.5 . . ?
H3Y1 C3Y H3Y3 109.5 . . ?
H3Y2 C3Y H3Y3 109.5 . . ?
O1Y C4Y C5Y 111.8(3) . . ?
O1Y C4Y C2Y 107.8(3) . . ?
C5Y C4Y C2Y 111.9(3) . . ?
O1Y C4Y H4Y 108.4 . . ?
C5Y C4Y H4Y 108.4 . . ?
C2Y C4Y H4Y 108.4 . . ?
C7Y C6Y C5Y 120.6(4) . . ?
C7Y C6Y H6Y 119.7 . . ?
C5Y C6Y H6Y 119.7 . . ?
N9 C8 N8 113.9(3) . . ?
N9 C8 H8A 108.8 . . ?
N8 C8 H8A 108.8 . . ?
N9 C8 H8B 108.8 . . ?
N8 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
O12 C35 N23 124.6(4) . . ?
O12 C35 N24 126.4(4) . . ?
N23 C35 N24 109.1(3) . . ?
C10Y C5Y C6Y 118.9(3) . . ?
C10Y C5Y C4Y 121.1(3) . . ?
C6Y C5Y C4Y 120.0(3) . . ?
N1Y C2Y C3Y 107.3(3) . . ?
N1Y C2Y C4Y 108.2(3) . . ?
C3Y C2Y C4Y 113.3(3) . . ?
N1Y C2Y H2Y 109.3 . . ?
C3Y C2Y H2Y 109.3 . . ?
C4Y C2Y H2Y 109.3 . . ?
C8Y C7Y C6Y 120.2(4) . . ?
C8Y C7Y H7Y 119.9 . . ?
C6Y C7Y H7Y 119.9 . . ?
C5Y C10Y C9Y 120.2(4) . . ?
C5Y C10Y H10Y 119.9 . . ?
C9Y C10Y H10Y 119.9 . . ?
O1X C3X C5X 110.9(3) . . ?
O1X C3X C2X 107.7(3) . . ?
C5X C3X C2X 110.0(3) . . ?
O1X C3X H3X 109.4 . . ?
C5X C3X H3X 109.4 . . ?
C2X C3X H3X 109.4 . . ?
N1X C2X C4X 106.6(3) . . ?
N1X C2X C3X 109.3(3) . . ?
C4X C2X C3X 113.7(4) . . ?
N1X C2X H2X 109.1 . . ?
C4X C2X H2X 109.1 . . ?
C3X C2X H2X 109.1 . . ?
C8Y C9Y C10Y 120.7(4) . . ?
C8Y C9Y H9Y 119.7 . . ?
C10Y C9Y H9Y 119.7 . . ?
C7Y C8Y C9Y 119.3(4) . . ?
C7Y C8Y H8Y 120.3 . . ?
C9Y C8Y H8Y 120.3 . . ?
C2X C4X H4X1 109.5 . . ?
C2X C4X H4X2 109.5 . . ?
H4X1 C4X H4X2 109.5 . . ?
C2X C4X H4X3 109.5 . . ?
H4X1 C4X H4X3 109.5 . . ?
H4X2 C4X H4X3 109.5 . . ?
H5W1 O5W H5W2 96(6) . . ?
C10X C5X C6X 118.4(4) . . ?
C10X C5X C3X 119.7(3) . . ?
C6X C5X C3X 121.8(3) . . ?
H6W1 O6W H6W2 116(8) . . ?
C7X C6X C5X 120.7(4) . . ?
C7X C6X H6X 119.7 . . ?
C5X C6X H6X 119.7 . . ?
H7W1 O7W H7W2 99(6) . . ?
C8X C7X C6X 120.2(4) . . ?
C8X C7X H7X 119.9 . . ?
C6X C7X H7X 119.9 . . ?
C7X C8X C9X 119.5(4) . . ?
C7X C8X H8X 120.3 . . ?
C9X C8X H8X 120.3 . . ?
C9X C10X C5X 121.1(4) . . ?
C9X C10X H10X 119.5 . . ?
C5X C10X H10X 119.5 . . ?
C10X C9X C8X 120.1(4) . . ?
C10X C9X H9X 119.9 . . ?
C8X C9X H9X 119.9 . . ?

_refine_diff_density_max         0.576
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.061

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_q6_syn_noHCl
_database_code_depnum_ccdc_archive 'CCDC 1868759'
_audit_update_record             
;
2018-11-05 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'cucurbit[6]uril/(+-)-synephrine complex'
_chemical_melting_point          ?
_chemical_formula_moiety         (C36H36N24O12).2(C9H14NO2)+.2Cl-.14(H2O)
_chemical_formula_sum            'C54 H92 Cl2 N26 O30'
_chemical_formula_weight         1656.27

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.3239(7)
_cell_length_b                   20.8368(7)
_cell_length_c                   12.9299(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.378(5)
_cell_angle_gamma                90
_cell_volume                     3662.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    7789
_cell_measurement_theta_min      3.60
_cell_measurement_theta_max      71.02

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_F_000             1704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.693
_shelx_estimated_absorpt_T_min   0.728
_shelx_estimated_absorpt_T_max   0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           ?

_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3
_diffrn_reflns_number            13625
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.883
_diffrn_reflns_theta_max         71.194
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6953
_reflns_number_gt                6529
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1056P)²+5.6628P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6953
_refine_ls_number_parameters     577
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0692
_refine_ls_wR_factor_ref         0.1933
_refine_ls_wR_factor_gt          0.1907
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1X N -0.05549(17) 0.45246(11) 0.2306(2) 0.0296(5) Uani 1 1 d . . . . .
H1X1 H -0.0134 0.4843 0.2810 0.035 Uiso 1 1 calc R U . . .
H1X2 H -0.0231 0.4101 0.2482 0.035 Uiso 1 1 calc R U . . .
C8X C -0.15254(19) 0.44971(13) 0.2502(2) 0.0282(6) Uani 1 1 d . . . . .
H8X1 H -0.1951 0.4174 0.2015 0.034 Uiso 1 1 calc R U . . .
H8X2 H -0.1856 0.4920 0.2340 0.034 Uiso 1 1 calc R U . . .
C9X C -0.0616(2) 0.46969(15) 0.1179(2) 0.0340(6) Uani 1 1 d . . . . .
H9X1 H -0.1007 0.4374 0.0675 0.051 Uiso 1 1 calc R U . . .
H9X2 H 0.0047 0.4713 0.1116 0.051 Uiso 1 1 calc R U . . .
H9X3 H -0.0930 0.5118 0.0998 0.051 Uiso 1 1 calc R U . . .
O2X O -0.07981(15) 0.37526(10) 0.39539(19) 0.0368(5) Uani 1 1 d . . . . .
H2X H -0.0250 0.3838 0.4413 0.055 Uiso 1 1 calc R U . . .
C7X C -0.1368(2) 0.43180(13) 0.3691(3) 0.0311(6) Uani 1 1 d . . . . .
H7X H -0.0999 0.4674 0.4165 0.037 Uiso 1 1 calc R U . . .
C5X C -0.2913(2) 0.47813(13) 0.3927(2) 0.0304(6) Uani 1 1 d . . . . .
H5X H -0.2681 0.5195 0.3817 0.037 Uiso 1 1 calc R U . . .
C4X C -0.2351(2) 0.42419(13) 0.3884(2) 0.0269(5) Uani 1 1 d . . . . .
C2X C -0.3596(2) 0.35784(14) 0.4249(2) 0.0292(6) Uani 1 1 d . . . . .
H2XA H -0.3830 0.3165 0.4358 0.035 Uiso 1 1 calc R U . . .
C3X C -0.2712(2) 0.36417(13) 0.4033(2) 0.0276(5) Uani 1 1 d . . . . .
H3X H -0.2347 0.3268 0.3987 0.033 Uiso 1 1 calc R U . . .
C1X C -0.41380(19) 0.41246(14) 0.4306(2) 0.0294(6) Uani 1 1 d . . . . .
C6X C -0.3801(2) 0.47262(14) 0.4125(2) 0.0311(6) Uani 1 1 d . . . . .
H6X H -0.4181 0.5098 0.4137 0.037 Uiso 1 1 calc R U . . .
O1X O -0.49978(15) 0.41010(12) 0.45509(19) 0.0398(5) Uani 1 1 d . . . . .
H1X H -0.5203 0.3721 0.4499 0.060 Uiso 1 1 calc R U . . .
O2W O 0.28665(19) 0.71807(13) -0.1372(2) 0.0517(7) Uani 1 1 d D . . . .
H1W2 H 0.351(2) 0.701(2) -0.123(4) 0.078 Uiso 1 1 d D U . . .
H2W2 H 0.238(3) 0.694(2) -0.116(4) 0.078 Uiso 1 1 d D U . . .
O3W O 0.09050(18) 0.40269(13) 0.55000(19) 0.0450(6) Uani 1 1 d D . . . .
H1W3 H 0.085(4) 0.400(2) 0.621(2) 0.067 Uiso 1 1 d D U . . .
H2W3 H 0.153(2) 0.387(2) 0.554(4) 0.067 Uiso 1 1 d D U . . .
Cl1 Cl -0.60036(16) 0.28119(14) 0.4384(3) 0.0642(10) Uani 0.666(9) 1 d . . P A
1
O1W O 0.2821(10) 0.3465(6) 0.5953(13) 0.116(7) Uani 0.666(9) 1 d . . P A 1
O1WA O -0.5877(12) 0.2920(7) 0.4825(16) 0.073(5) Uani 0.334(9) 1 d . . P A 2
Cl1A Cl 0.2828(3) 0.3442(2) 0.5830(7) 0.0585(14) Uani 0.334(9) 1 d . . P A 2
O4W O 0.4927(5) 0.6779(3) -0.1194(6) 0.0729(18) Uani 0.569(6) 1 d . . P B 1
O5W O 0.4265(4) 0.5535(4) -0.0889(5) 0.079(2) Uani 0.569(6) 1 d . . P B 1
O6W O 0.4726(4) 0.7809(4) -0.2998(7) 0.115(3) Uani 0.569(6) 1 d . . P B 1
O7W O 0.3923(5) 0.4150(4) -0.1988(6) 0.090(2) Uani 0.569(6) 1 d . . P B 1
O7WA O 0.4297(4) 0.4699(5) -0.1198(5) 0.076(3) Uani 0.431(6) 1 d . . P B 2
O5WA O 0.4280(6) 0.6092(5) -0.1076(7) 0.083(3) Uani 0.431(6) 1 d . . P B 2
O6WA O 0.4558(6) 0.3910(3) -0.2871(6) 0.063(2) Uani 0.431(6) 1 d . . P B 2
O4WA O 0.5232(8) 0.7090(7) -0.1665(13) 0.127(6) Uani 0.431(6) 1 d . . P B 2
O1 O 0.09211(14) 0.35638(9) 0.28569(16) 0.0281(4) Uani 1 1 d . . . . .
O2 O 0.10415(13) 0.52158(9) 0.36261(15) 0.0257(4) Uani 1 1 d . . . . .
O5 O 0.29780(14) 0.59010(9) 0.02696(16) 0.0303(4) Uani 1 1 d . . . . .
O3 O -0.07206(14) 0.61546(9) 0.24685(16) 0.0285(4) Uani 1 1 d . . . . .
O4 O -0.27740(15) 0.56676(10) 0.05666(16) 0.0326(4) Uani 1 1 d . . . . .
N4 N 0.19313(16) 0.60465(10) 0.32164(18) 0.0238(4) Uani 1 1 d . . . . .
O6 O 0.10831(15) 0.69350(9) -0.08871(16) 0.0296(4) Uani 1 1 d . . . . .
N10 N 0.26034(17) 0.62997(11) 0.17573(19) 0.0266(5) Uani 1 1 d . . . . .
N1 N 0.16051(17) 0.31305(11) 0.16205(19) 0.0270(5) Uani 1 1 d . . . . .
N11 N 0.13280(16) 0.70838(11) 0.09595(18) 0.0257(5) Uani 1 1 d . . . . .
N2 N 0.23804(16) 0.39315(11) 0.26665(18) 0.0255(5) Uani 1 1 d . . . . .
N12 N -0.01538(17) 0.72622(11) -0.02105(18) 0.0274(5) Uani 1 1 d . . . . .
N3 N 0.24599(16) 0.50497(10) 0.31690(18) 0.0242(5) Uani 1 1 d . . . . .
N5 N 0.05872(16) 0.67684(10) 0.23420(18) 0.0240(5) Uani 1 1 d . . . . .
N6 N -0.08926(16) 0.69383(11) 0.11553(18) 0.0265(5) Uani 1 1 d . . . . .
N7 N -0.23487(17) 0.65560(11) -0.02408(18) 0.0265(5) Uani 1 1 d . . . . .
C8 C -0.27532(19) 0.59654(13) -0.0242(2) 0.0260(5) Uani 1 1 d . . . . .
C15 C -0.02830(19) 0.74009(12) 0.0831(2) 0.0250(5) Uani 1 1 d . . . . .
H15 H -0.0511 0.7851 0.0870 0.030 Uiso 1 1 calc R U . . .
N8 N -0.31382(16) 0.57602(11) -0.12986(18) 0.0261(5) Uani 1 1 d . . . . .
C2 C 0.15691(19) 0.35469(12) 0.2424(2) 0.0240(5) Uani 1 1 d . . . . .
C4 C 0.17334(18) 0.54158(12) 0.3357(2) 0.0220(5) Uani 1 1 d . . . . .
C6 C -0.03727(19) 0.65716(12) 0.2026(2) 0.0237(5) Uani 1 1 d . . . . .
C3 C 0.2613(2) 0.43909(12) 0.3546(2) 0.0253(5) Uani 1 1 d . . . . .
H3A H 0.3308 0.4336 0.3997 0.030 Uiso 1 1 calc R U . . .
H3B H 0.2198 0.4303 0.4014 0.030 Uiso 1 1 calc R U . . .
C5 C 0.13064(19) 0.65618(12) 0.3350(2) 0.0241(5) Uani 1 1 d . . . . .
H5A H 0.1724 0.6933 0.3685 0.029 Uiso 1 1 calc R U . . .
H5B H 0.0957 0.6421 0.3860 0.029 Uiso 1 1 calc R U . . .
N9 N 0.33308(17) 0.53488(11) 0.19001(19) 0.0273(5) Uani 1 1 d . . . . .
C18 C 0.0786(2) 0.70736(12) -0.0118(2) 0.0254(5) Uani 1 1 d . . . . .
C12 C 0.32244(18) 0.54415(13) 0.2962(2) 0.0244(5) Uani 1 1 d . . . . .
H12 H 0.3867 0.5399 0.3557 0.029 Uiso 1 1 calc R U . . .
C1 C 0.0894(2) 0.26174(12) 0.1249(2) 0.0267(5) Uani 1 1 d . . . . .
H1A H 0.1249 0.2218 0.1192 0.032 Uiso 1 1 calc R U . . .
H1B H 0.0561 0.2545 0.1804 0.032 Uiso 1 1 calc R U . . .
C7 C -0.19547(19) 0.69315(13) 0.0743(2) 0.0274(6) Uani 1 1 d . . . . .
H7A H -0.2194 0.7378 0.0595 0.033 Uiso 1 1 calc R U . . .
H7B H -0.2210 0.6757 0.1314 0.033 Uiso 1 1 calc R U . . .
C16 C 0.29724(18) 0.58543(13) 0.1206(2) 0.0244(5) Uani 1 1 d . . . . .
C14 C 0.07590(19) 0.72806(12) 0.1655(2) 0.0238(5) Uani 1 1 d . . . . .
H14 H 0.1036 0.7674 0.2085 0.029 Uiso 1 1 calc R U . . .
C9 C -0.37813(19) 0.52105(13) -0.1594(2) 0.0275(6) Uani 1 1 d . . . . .
H9A H -0.4367 0.5330 -0.2211 0.033 Uiso 1 1 calc R U . . .
H9B H -0.4010 0.5097 -0.0970 0.033 Uiso 1 1 calc R U . . .
C11 C 0.30481(19) 0.37561(12) 0.2068(2) 0.0244(5) Uani 1 1 d . . . . .
H11 H 0.3705 0.3618 0.2566 0.029 Uiso 1 1 calc R U . . .
C10 C 0.24992(19) 0.31973(12) 0.1329(2) 0.0252(5) Uani 1 1 d . . . . .
H10 H 0.2896 0.2793 0.1466 0.030 Uiso 1 1 calc R U . . .
C17 C 0.23765(19) 0.69487(13) 0.1358(2) 0.0267(5) Uani 1 1 d . . . . .
H17A H 0.2658 0.7023 0.0760 0.032 Uiso 1 1 calc R U . . .
H17B H 0.2696 0.7253 0.1952 0.032 Uiso 1 1 calc R U . . .
C13 C 0.28023(18) 0.61316(12) 0.2895(2) 0.0240(5) Uani 1 1 d . . . . .
H13 H 0.3280 0.6434 0.3390 0.029 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1X C9X 1.477(4) . ?
N1X C8X 1.490(3) . ?
C8X C7X 1.529(4) . ?
O2X C7X 1.413(3) . ?
C7X C4X 1.512(4) . ?
C5X C6X 1.379(4) . ?
C5X C4X 1.394(4) . ?
C4X C3X 1.390(4) . ?
C2X C3X 1.385(4) . ?
C2X C1X 1.393(4) . ?
C1X O1X 1.366(3) . ?
C1X C6X 1.389(4) . ?
O1 C2 1.226(3) . ?
O2 C4 1.223(3) . ?
O5 C16 1.218(3) . ?
O3 C6 1.229(3) . ?
O4 C8 1.224(3) . ?
N4 C4 1.368(3) . ?
N4 C5 1.443(3) . ?
N4 C13 1.445(3) . ?
O6 C18 1.233(3) . ?
N10 C16 1.373(3) . ?
N10 C17 1.448(3) . ?
N10 C13 1.451(3) . ?
N1 C2 1.367(3) . ?
N1 C1 1.450(3) . ?
N1 C10 1.451(3) . ?
N11 C18 1.365(4) . ?
N11 C14 1.450(3) . ?
N11 C17 1.453(3) . ?
N2 C2 1.364(3) . ?
N2 C3 1.443(3) . ?
N2 C11 1.454(3) . ?
N12 C18 1.371(4) . ?
N12 C15 1.445(3) . ?
N12 C1 1.446(3) 3_565 ?
N3 C4 1.372(3) . ?
N3 C3 1.450(3) . ?
N3 C12 1.457(3) . ?
N5 C6 1.368(3) . ?
N5 C5 1.449(3) . ?
N5 C14 1.459(3) . ?
N6 C6 1.371(3) . ?
N6 C7 1.445(3) . ?
N6 C15 1.448(3) . ?
N7 C8 1.360(4) . ?
N7 C7 1.448(3) . ?
N7 C10 1.450(3) 3_565 ?
C8 N8 1.371(4) . ?
C15 C14 1.556(4) . ?
N8 C9 1.444(3) . ?
N8 C11 1.450(3) 3_565 ?
N9 C16 1.374(4) . ?
N9 C12 1.442(3) . ?
N9 C9 1.446(3) 3_565 ?
C12 C13 1.552(4) . ?
C1 N12 1.446(3) 3_565 ?
C9 N9 1.446(3) 3_565 ?
C11 N8 1.450(3) 3_565 ?
C11 C10 1.553(4) . ?
C10 N7 1.449(3) 3_565 ?

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
C9X N1X C8X 114.1(2) . . ?
N1X C8X C7X 109.3(2) . . ?
O2X C7X C4X 111.7(2) . . ?
O2X C7X C8X 109.6(2) . . ?
C4X C7X C8X 110.0(2) . . ?
C6X C5X C4X 121.3(3) . . ?
C3X C4X C5X 118.3(3) . . ?
C3X C4X C7X 121.6(2) . . ?
C5X C4X C7X 120.1(2) . . ?
C3X C2X C1X 119.5(3) . . ?
C2X C3X C4X 121.2(2) . . ?
O1X C1X C6X 117.3(3) . . ?
O1X C1X C2X 122.8(3) . . ?
C6X C1X C2X 120.0(3) . . ?
C5X C6X C1X 119.7(3) . . ?
C4 N4 C5 122.5(2) . . ?
C4 N4 C13 112.9(2) . . ?
C5 N4 C13 124.6(2) . . ?
C16 N10 C17 121.7(2) . . ?
C16 N10 C13 112.2(2) . . ?
C17 N10 C13 122.5(2) . . ?
C2 N1 C1 121.9(2) . . ?
C2 N1 C10 112.6(2) . . ?
C1 N1 C10 124.8(2) . . ?
C18 N11 C14 112.8(2) . . ?
C18 N11 C17 123.4(2) . . ?
C14 N11 C17 123.7(2) . . ?
C2 N2 C3 122.6(2) . . ?
C2 N2 C11 112.7(2) . . ?
C3 N2 C11 124.0(2) . . ?
C18 N12 C15 112.8(2) . . ?
C18 N12 C1 122.8(2) . 3_565 ?
C15 N12 C1 124.0(2) . 3_565 ?
C4 N3 C3 120.6(2) . . ?
C4 N3 C12 112.1(2) . . ?
C3 N3 C12 123.4(2) . . ?
C6 N5 C5 122.8(2) . . ?
C6 N5 C14 112.6(2) . . ?
C5 N5 C14 123.8(2) . . ?
C6 N6 C7 122.2(2) . . ?
C6 N6 C15 112.8(2) . . ?
C7 N6 C15 124.1(2) . . ?
C8 N7 C7 122.5(2) . . ?
C8 N7 C10 112.8(2) . 3_565 ?
C7 N7 C10 124.0(2) . 3_565 ?
O4 C8 N7 125.7(2) . . ?
O4 C8 N8 125.6(3) . . ?
N7 C8 N8 108.7(2) . . ?
N12 C15 N6 113.8(2) . . ?
N12 C15 C14 103.2(2) . . ?
N6 C15 C14 103.3(2) . . ?
C8 N8 C9 122.3(2) . . ?
C8 N8 C11 111.9(2) . 3_565 ?
C9 N8 C11 123.8(2) . 3_565 ?
O1 C2 N2 126.2(2) . . ?
O1 C2 N1 125.5(2) . . ?
N2 C2 N1 108.3(2) . . ?
O2 C4 N4 125.8(2) . . ?
O2 C4 N3 126.1(2) . . ?
N4 C4 N3 108.1(2) . . ?
O3 C6 N5 126.2(2) . . ?
O3 C6 N6 125.6(2) . . ?
N5 C6 N6 108.2(2) . . ?
N2 C3 N3 113.0(2) . . ?
N4 C5 N5 113.9(2) . . ?
C16 N9 C12 112.9(2) . . ?
C16 N9 C9 123.1(2) . 3_565 ?
C12 N9 C9 124.0(2) . 3_565 ?
O6 C18 N11 126.6(3) . . ?
O6 C18 N12 125.2(3) . . ?
N11 C18 N12 108.1(2) . . ?
N9 C12 N3 114.3(2) . . ?
N9 C12 C13 103.1(2) . . ?
N3 C12 C13 103.15(19) . . ?
N12 C1 N1 114.3(2) 3_565 . ?
N6 C7 N7 113.7(2) . . ?
O5 C16 N10 125.9(3) . . ?
O5 C16 N9 126.3(2) . . ?
N10 C16 N9 107.8(2) . . ?
N11 C14 N5 114.0(2) . . ?
N11 C14 C15 103.1(2) . . ?
N5 C14 C15 103.0(2) . . ?
N8 C9 N9 114.2(2) . 3_565 ?
N8 C11 N2 114.0(2) 3_565 . ?
N8 C11 C10 103.7(2) 3_565 . ?
N2 C11 C10 103.0(2) . . ?
N7 C10 N1 114.4(2) 3_565 . ?
N7 C10 C11 102.9(2) 3_565 . ?
N1 C10 C11 103.3(2) . . ?
N10 C17 N11 113.5(2) . . ?
N4 C13 N10 114.2(2) . . ?
N4 C13 C12 103.1(2) . . ?
N10 C13 C12 103.2(2) . . ?

_refine_diff_density_max         1.495
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.092

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_q6_oct_needle
_database_code_depnum_ccdc_archive 'CCDC 1868757'
_audit_update_record             
;
2018-11-05 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_q6_oct_needle       
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystals of cucurbit[6]uril/octopamine complex were
thin needles of poor diffraction quality, with the number of 
observed reflections being quite low (44 % of all data).
;
_vrf_PLAT260_q6_oct_needle       
;
PROBLEM: Large Average Ueq of Residue Including O12W 0.220 Check
RESPONSE: These are water molecules residing in the large channels 
formed by self-assembled cucurbit[6]uril molecules.
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'cucurbit[6]uril/(+-)-octopamine complex'
_chemical_melting_point          ?
_chemical_formula_moiety         '(C36H36N24O12). (C8H12NO2)+. Cl-.12.33(H2O)'
_chemical_formula_sum            'C44 H72.67 Cl N25 O26.33'
_chemical_formula_weight         1408.72

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   50.127(9)
_cell_length_b                   50.127(9)
_cell_length_c                   12.4583(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     27110(9)
_cell_formula_units_Z            18
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    1342
_cell_measurement_theta_min      3.52
_cell_measurement_theta_max      55.64

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_F_000             13308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.499
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.0(1))
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3
_diffrn_reflns_number            13519
_diffrn_reflns_av_unetI/netI     0.2160
_diffrn_reflns_av_R_equivalents  0.1404
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.527
_diffrn_reflns_theta_max         55.712
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.695
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.695
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.695
_reflns_number_total             7557
_reflns_number_gt                3341
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1411P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7557
_refine_ls_number_parameters     871
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.2244
_refine_ls_R_factor_gt           0.1243
_refine_ls_wR_factor_ref         0.3121
_refine_ls_wR_factor_gt          0.2721
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O -0.0205(2) 0.1629(2) 0.4177(7) 0.067(2) Uani 1 1 d . . . . .
O2W O -0.0722(4) 0.1198(5) 0.3012(15) 0.170(8) Uani 1 1 d . . . . .
O3W O -0.1394(2) 0.1983(3) 0.0060(6) 0.078(3) Uani 1 1 d . . . . .
O4W O -0.2079(2) 0.0219(3) 0.2211(6) 0.080(3) Uani 1 1 d . . . . .
O5W O 0.0563(3) 0.2766(3) 0.5560(8) 0.091(3) Uani 1 1 d . . . . .
O6W O -0.1183(3) 0.2073(3) -0.2097(8) 0.118(4) Uani 1 1 d . . . . .
O7W O -0.2910(2) 0.0212(2) 0.0699(11) 0.095(4) Uani 1 1 d . . . . .
O13W O -0.3127(6) 0.0159(5) -0.151(2) 0.238(13) Uani 1 1 d . . . . .
O12W O -0.2765(6) 0.0539(4) -0.3221(15) 0.218(12) Uani 1 1 d . . . . .
O8W O 0.0299(3) 0.0596(3) 0.3401(11) 0.121(4) Uani 1 1 d . . . . .
O9W O 0.0000 0.0000 0.388(2) 0.149(9) Uani 1 3 d S T P . .
O11W O -0.0540(5) 0.2492(5) -0.1310(15) 0.171(6) Uiso 1 1 d . . . . .
O14W O -0.0643(6) 0.2833(6) 0.0072(19) 0.104(7) Uiso 0.5 1 d . . P . .
O15W O -0.0027(7) 0.2684(7) -0.229(2) 0.134(9) Uiso 0.5 1 d . . P . .
Cl1 Cl -0.0173(4) 0.0355(4) -0.0773(12) 0.055(4) Uiso 0.2 1 d . . P A 1
Cl2 Cl -0.0232(4) 0.0477(4) -0.1196(13) 0.164(5) Uiso 0.5 1 d . . P B 2
Cl3 Cl -0.0356(6) 0.0591(6) -0.181(2) 0.160(8) Uiso 0.3 1 d . . P C 3
O2X O -0.1934(2) 0.0880(2) 0.2091(6) 0.064(2) Uani 1 1 d . . . . .
H2X H -0.1973 0.0991 0.2493 0.096 Uiso 1 1 calc R U . . .
N1X N -0.1310(2) 0.1132(3) 0.2588(7) 0.062(3) Uani 1 1 d . . . . .
H1X1 H -0.1351 0.1275 0.2868 0.093 Uiso 1 1 calc R U . . .
H1X2 H -0.1104 0.1205 0.2600 0.093 Uiso 1 1 calc R U . . .
H1X3 H -0.1408 0.0956 0.2985 0.093 Uiso 1 1 calc R U . . .
C7X C -0.1717(3) 0.1064(4) 0.1323(9) 0.060(4) Uani 1 1 d . . . . .
H7X H -0.1670 0.1280 0.1455 0.072 Uiso 1 1 calc R U . . .
C8X C -0.1422(3) 0.1064(4) 0.1466(8) 0.066(4) Uani 1 1 d . . . . .
H8X1 H -0.1453 0.0860 0.1257 0.079 Uiso 1 1 calc R U . . .
H8X2 H -0.1264 0.1220 0.0984 0.079 Uiso 1 1 calc R U . . .
C4X C -0.1833(3) 0.0987(3) 0.0193(8) 0.049(3) Uani 1 1 d . . . . .
C5X C -0.2119(3) 0.0739(3) -0.0077(9) 0.057(4) Uani 1 1 d . . . . .
H5X H -0.2244 0.0600 0.0469 0.069 Uiso 1 1 calc R U . . .
C3X C -0.1656(3) 0.1182(4) -0.0672(9) 0.062(4) Uani 1 1 d . . . . .
H3X H -0.1459 0.1354 -0.0523 0.074 Uiso 1 1 calc R U . . .
C2X C -0.1761(5) 0.1132(5) -0.1700(11) 0.078(5) Uani 1 1 d . . . . .
H2X1 H -0.1640 0.1268 -0.2257 0.093 Uiso 1 1 calc R U . . .
C6X C -0.2226(3) 0.0688(3) -0.1147(9) 0.055(3) Uani 1 1 d . . . . .
H6X H -0.2424 0.0521 -0.1318 0.066 Uiso 1 1 calc R U . . .
C1X C -0.2045(5) 0.0880(5) -0.1921(10) 0.079(5) Uani 1 1 d . . . . .
O1X O -0.2145(4) 0.0832(4) -0.3006(7) 0.128(6) Uani 1 1 d . . . . .
H1X H -0.2325 0.0801 -0.3039 0.192 Uiso 1 1 calc R U . . .
O10 O 0.02857(16) 0.16535(17) 0.1743(5) 0.0400(18) Uani 1 1 d . . . . .
O9 O -0.00193(19) 0.09456(18) 0.3283(5) 0.047(2) Uani 1 1 d . . . . .
O2 O -0.15658(18) 0.05342(18) 0.3700(5) 0.051(2) Uani 1 1 d . . . . .
O4 O -0.0965(2) 0.1189(2) -0.0554(5) 0.052(2) Uani 1 1 d . . . . .
O1 O -0.15974(18) 0.1104(2) 0.4708(5) 0.057(2) Uani 1 1 d . . . . .
N14 N -0.0858(2) 0.1168(2) 0.6828(6) 0.034(2) Uani 1 1 d . . . . .
O3 O -0.1263(2) 0.05317(17) 0.1094(5) 0.049(2) Uani 1 1 d . . . . .
N18 N -0.0288(2) 0.0817(2) 0.1680(6) 0.045(2) Uani 1 1 d . . . . .
O6 O -0.12987(19) 0.1734(2) 0.3140(5) 0.050(2) Uani 1 1 d . . . . .
O7 O -0.0348(2) 0.15430(18) 0.6589(5) 0.049(2) Uani 1 1 d . . . . .
N3 N -0.1353(2) 0.0555(2) 0.5359(6) 0.046(3) Uani 1 1 d . . . . .
N5 N -0.0999(2) 0.0392(2) 0.2267(6) 0.042(2) Uani 1 1 d . . . . .
O11 O 0.0220(2) 0.2247(2) 0.2730(6) 0.054(2) Uani 1 1 d . . . . .
N20 N 0.0022(2) 0.1757(2) 0.0436(6) 0.041(2) Uani 1 1 d . . . . .
N21 N 0.0036(2) 0.2223(2) 0.1019(6) 0.036(2) Uani 1 1 d . . . . .
N22 N -0.0109(2) 0.2431(2) 0.2313(6) 0.044(2) Uani 1 1 d . . . . .
N17 N -0.0510(2) 0.0526(3) 0.3105(6) 0.050(3) Uani 1 1 d . . . . .
O8 O -0.03422(19) 0.0883(2) 0.5822(5) 0.053(2) Uani 1 1 d . . . . .
N15 N -0.0853(2) 0.0711(2) 0.6166(6) 0.040(2) Uani 1 1 d . . . . .
N9 N -0.0467(2) 0.2007(2) 0.0199(6) 0.042(2) Uani 1 1 d . . . . .
O5 O -0.0981(2) 0.1793(2) 0.0608(5) 0.055(2) Uani 1 1 d . . . . .
N8 N -0.0454(2) 0.1577(2) -0.0582(6) 0.036(2) Uani 1 1 d . . . . .
N19 N -0.0057(2) 0.1274(2) 0.0576(6) 0.039(2) Uani 1 1 d . . . . .
N13 N -0.0737(2) 0.1661(2) 0.6621(6) 0.043(2) Uani 1 1 d . . . . .
O12 O -0.0031(2) 0.22476(19) 0.5131(5) 0.050(2) Uani 1 1 d . . . . .
N6 N -0.0774(2) 0.0621(2) 0.0736(6) 0.049(3) Uani 1 1 d . . . . .
N7 N -0.0557(2) 0.1099(2) -0.0250(6) 0.040(2) Uani 1 1 d . . . . .
N12 N -0.1048(2) 0.1935(2) 0.4754(7) 0.047(3) Uani 1 1 d . . . . .
N10 N -0.0610(2) 0.2224(2) 0.1464(6) 0.040(2) Uani 1 1 d . . . . .
N23 N -0.0315(2) 0.2406(2) 0.4072(6) 0.042(2) Uani 1 1 d . . . . .
N11 N -0.0816(2) 0.2177(2) 0.3250(7) 0.044(2) Uani 1 1 d . . . . .
N4 N -0.1228(2) 0.0357(2) 0.4005(6) 0.044(2) Uani 1 1 d . . . . .
N16 N -0.0743(3) 0.0495(2) 0.4853(6) 0.049(3) Uani 1 1 d . . . . .
N24 N -0.0536(2) 0.2109(2) 0.5495(6) 0.044(2) Uani 1 1 d . . . . .
N2 N -0.1369(2) 0.0989(2) 0.6108(6) 0.045(2) Uani 1 1 d . . . . .
C17 C -0.0728(3) 0.0367(3) 0.2238(8) 0.041(3) Uani 1 1 d . . . . .
H17 H -0.0779 0.0148 0.2174 0.050 Uiso 1 1 calc R U . . .
N1 N -0.1249(2) 0.1478(2) 0.5864(6) 0.046(2) Uani 1 1 d . . . . .
C3 C -0.1397(3) 0.0489(3) 0.4300(8) 0.045(3) Uani 1 1 d . . . . .
C7 C -0.0690(3) 0.1273(3) -0.0458(7) 0.041(3) Uani 1 1 d . U . . .
C8 C -0.0506(3) 0.1830(3) -0.0741(7) 0.042(3) Uani 1 1 d . . . . .
H8A H -0.0362 0.1968 -0.1298 0.051 Uiso 1 1 calc R U . . .
H8B H -0.0718 0.1750 -0.1014 0.051 Uiso 1 1 calc R U . . .
C20 C -0.0155(2) 0.1603(3) -0.0518(7) 0.036(3) Uani 1 1 d . . . . .
H20 H -0.0033 0.1695 -0.1186 0.043 Uiso 1 1 calc R U . . .
C27 C -0.0620(3) 0.0713(3) 0.5632(7) 0.037(3) Uani 1 1 d . . . . .
C19 C -0.0231(2) 0.1266(3) -0.0370(7) 0.035(3) Uani 1 1 d . . . . .
H19 H -0.0167 0.1193 -0.1012 0.042 Uiso 1 1 calc R U . . .
C23 C -0.0614(3) 0.2376(3) 0.4086(7) 0.043(3) Uani 1 1 d . . . . .
H23 H -0.0602 0.2581 0.4086 0.052 Uiso 1 1 calc R U . . .
C14 C -0.1144(3) 0.1154(3) 0.6955(7) 0.042(3) Uani 1 1 d . . . . .
H14 H -0.1233 0.1077 0.7683 0.050 Uiso 1 1 calc R U . . .
C34 C -0.0079(3) 0.2580(3) 0.3287(7) 0.041(3) Uani 1 1 d . . . . .
H34A H -0.0079 0.2774 0.3143 0.049 Uiso 1 1 calc R U . . .
H34B H 0.0124 0.2636 0.3602 0.049 Uiso 1 1 calc R U . . .
C15 C -0.1150(3) 0.0462(2) 0.5838(7) 0.040(3) Uani 1 1 d . . . . .
H15 H -0.1254 0.0312 0.6435 0.048 Uiso 1 1 calc R U . . .
C13 C -0.1068(3) 0.1492(3) 0.6782(7) 0.047(3) Uani 1 1 d . . . . .
H13 H -0.1127 0.1570 0.7426 0.056 Uiso 1 1 calc R U . . .
C31 C 0.0102(3) 0.1571(3) 0.0999(7) 0.043(3) Uani 1 1 d . . . . .
C24 C -0.0765(3) 0.2194(3) 0.5118(8) 0.040(3) Uani 1 1 d . . . . .
H24 H -0.0800 0.2320 0.5659 0.048 Uiso 1 1 calc R U . . .
C26 C -0.0810(2) 0.0915(2) 0.7054(7) 0.033(3) Uani 1 1 d . . . . .
H26A H -0.0952 0.0791 0.7638 0.040 Uiso 1 1 calc R U . . .
H26B H -0.0597 0.1000 0.7327 0.040 Uiso 1 1 calc R U . . .
C25 C -0.0620(3) 0.1465(3) 0.6661(8) 0.044(3) Uani 1 1 d . . . . .
C16 C -0.1068(3) 0.0315(3) 0.4910(7) 0.053(3) Uani 1 1 d . . . . .
H16 H -0.1140 0.0093 0.5047 0.064 Uiso 1 1 calc R U . . .
C11 C -0.1075(3) 0.1931(3) 0.3638(8) 0.043(3) Uani 1 1 d . . . . .
C18 C -0.0554(3) 0.0557(3) 0.1249(8) 0.042(3) Uani 1 1 d . . . . .
H18 H -0.0495 0.0436 0.0763 0.050 Uiso 1 1 calc R U . . .
C36 C -0.0548(3) 0.1988(3) 0.6562(8) 0.049(3) Uani 1 1 d . . . . .
H36A H -0.0336 0.2047 0.6789 0.059 Uiso 1 1 calc R U . . .
H36B H -0.0627 0.2083 0.7071 0.059 Uiso 1 1 calc R U . . .
C1 C -0.1426(3) 0.1182(3) 0.5476(8) 0.048(3) Uani 1 1 d . . . . .
C30 C -0.0031(3) 0.1027(3) 0.1017(8) 0.044(3) Uani 1 1 d . . . . .
H30A H 0.0159 0.1114 0.1452 0.053 Uiso 1 1 calc R U . . .
H30B H -0.0009 0.0909 0.0421 0.053 Uiso 1 1 calc R U . . .
C5 C -0.1031(3) 0.0520(3) 0.1331(8) 0.046(3) Uani 1 1 d . . . . .
C21 C -0.0180(3) 0.2282(3) 0.0478(8) 0.045(3) Uani 1 1 d . . . . .
H21 H -0.0086 0.2423 -0.0150 0.055 Uiso 1 1 calc R U . . .
C22 C -0.0283(3) 0.2430(3) 0.1383(8) 0.045(3) Uani 1 1 d . . . . .
H22 H -0.0234 0.2643 0.1186 0.054 Uiso 1 1 calc R U . . .
C33 C 0.0060(3) 0.2287(2) 0.2075(9) 0.037(3) Uani 1 1 d . . . . .
C29 C -0.0248(3) 0.0784(3) 0.2765(9) 0.043(3) Uani 1 1 d . . . . .
C32 C 0.0201(3) 0.2084(3) 0.0517(8) 0.040(3) Uani 1 1 d . . . . .
H32A H 0.0267 0.2172 -0.0212 0.047 Uiso 1 1 calc R U . . .
H32B H 0.0389 0.2140 0.0940 0.047 Uiso 1 1 calc R U . . .
C6 C -0.0741(3) 0.0764(3) -0.0282(8) 0.057(4) Uani 1 1 d . . . . .
H6A H -0.0948 0.0704 -0.0565 0.068 Uiso 1 1 calc R U . . .
H6B H -0.0644 0.0686 -0.0788 0.068 Uiso 1 1 calc R U . . .
C10 C -0.0813(3) 0.2279(4) 0.2140(8) 0.057(4) Uani 1 1 d . . . . .
H10A H -0.1025 0.2167 0.1844 0.069 Uiso 1 1 calc R U . . .
H10B H -0.0744 0.2502 0.2138 0.069 Uiso 1 1 calc R U . . .
C2 C -0.1522(3) 0.0667(3) 0.5970(8) 0.059(4) Uani 1 1 d . . . . .
H2A H -0.1721 0.0601 0.5608 0.071 Uiso 1 1 calc R U . . .
H2B H -0.1567 0.0569 0.6687 0.071 Uiso 1 1 calc R U . . .
C28 C -0.0553(3) 0.0407(3) 0.4200(8) 0.047(3) Uani 1 1 d . . . . .
H28A H -0.0350 0.0487 0.4546 0.057 Uiso 1 1 calc R U . . .
H28B H -0.0654 0.0180 0.4175 0.057 Uiso 1 1 calc R U . . .
C35 C -0.0261(3) 0.2253(3) 0.4917(8) 0.049(3) Uani 1 1 d . . . . .
C9 C -0.0713(3) 0.1996(3) 0.0751(7) 0.044(3) Uani 1 1 d . . . . .
C12 C -0.1291(3) 0.1725(3) 0.5454(8) 0.053(3) Uani 1 1 d . . . . .
H12A H -0.1489 0.1634 0.5059 0.064 Uiso 1 1 calc R U . . .
H12B H -0.1307 0.1842 0.6069 0.064 Uiso 1 1 calc R U . . .
C4 C -0.1264(3) 0.0203(3) 0.2975(7) 0.045(3) Uani 1 1 d . . . . .
H4A H -0.1456 0.0169 0.2625 0.054 Uiso 1 1 calc R U . . .
H4B H -0.1281 0.0000 0.3093 0.054 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2X C7X 1.396(15) . ?
N1X C8X 1.481(15) . ?
C7X C8X 1.489(19) . ?
C7X C4X 1.498(16) . ?
C4X C5X 1.390(18) . ?
C4X C3X 1.426(18) . ?
C5X C6X 1.414(16) . ?
C3X C2X 1.36(2) . ?
C2X C1X 1.38(2) . ?
C6X C1X 1.34(2) . ?
C1X O1X 1.419(17) . ?
O10 C31 1.223(12) . ?
O9 C29 1.209(14) . ?
O2 C3 1.233(14) . ?
O4 C7 1.232(13) . ?
O1 C1 1.213(13) . ?
N14 C25 1.379(15) . ?
N14 C14 1.405(14) . ?
N14 C26 1.433(14) . ?
O3 C5 1.229(14) . ?
N18 C29 1.388(14) . ?
N18 C18 1.426(14) . ?
N18 C30 1.447(15) . ?
O6 C11 1.228(14) . ?
O7 C25 1.223(13) . ?
N3 C3 1.351(14) . ?
N3 C2 1.441(17) . ?
N3 C15 1.443(15) . ?
N5 C5 1.376(13) . ?
N5 C17 1.426(15) . ?
N5 C4 1.479(14) . ?
O11 C33 1.227(12) . ?
N20 C31 1.377(14) . ?
N20 C32 1.426(15) . ?
N20 C20 1.454(13) . ?
N21 C33 1.346(13) . ?
N21 C21 1.426(14) . ?
N21 C32 1.462(14) . ?
N22 C33 1.392(14) . ?
N22 C34 1.392(13) . ?
N22 C22 1.448(13) . ?
N17 C29 1.367(15) . ?
N17 C17 1.459(14) . ?
N17 C28 1.460(14) . ?
O8 C27 1.240(13) . ?
N15 C27 1.339(14) . ?
N15 C15 1.444(14) . ?
N15 C26 1.448(13) . ?
N9 C9 1.385(15) . ?
N9 C8 1.421(13) . ?
N9 C21 1.453(15) . ?
O5 C9 1.227(14) . ?
N8 C7 1.394(15) . ?
N8 C8 1.435(14) . ?
N8 C20 1.438(13) . ?
N19 C31 1.393(15) . ?
N19 C30 1.418(14) . ?
N19 C19 1.455(12) . ?
N13 C25 1.373(16) . ?
N13 C36 1.428(15) . ?
N13 C13 1.451(15) . ?
O12 C35 1.199(14) . ?
N6 C5 1.345(16) . ?
N6 C6 1.426(14) . ?
N6 C18 1.443(14) . ?
N7 C7 1.356(15) . ?
N7 C19 1.422(14) . ?
N7 C6 1.459(16) . ?
N12 C11 1.396(14) . ?
N12 C24 1.435(15) . ?
N12 C12 1.440(15) . ?
N10 C9 1.332(15) . ?
N10 C22 1.441(15) . ?
N10 C10 1.451(15) . ?
N23 C35 1.404(16) . ?
N23 C23 1.433(14) . ?
N23 C34 1.443(15) . ?
N11 C11 1.356(16) . ?
N11 C23 1.447(15) . ?
N11 C10 1.471(14) . ?
N4 C3 1.363(17) . ?
N4 C16 1.456(14) . ?
N4 C4 1.460(14) . ?
N16 C27 1.356(14) . ?
N16 C16 1.418(16) . ?
N16 C28 1.476(16) . ?
N24 C35 1.396(16) . ?
N24 C36 1.452(14) . ?
N24 C24 1.481(14) . ?
N2 C1 1.381(15) . ?
N2 C2 1.412(16) . ?
N2 C14 1.463(14) . ?
C17 C18 1.535(15) . ?
N1 C1 1.379(16) . ?
N1 C13 1.438(14) . ?
N1 C12 1.451(16) . ?
C20 C19 1.544(16) . ?
C23 C24 1.540(16) . ?
C14 C13 1.553(18) . ?
C15 C16 1.534(17) . ?
C21 C22 1.571(16) . ?

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
O2X C7X C8X 111.3(10) . . ?
O2X C7X C4X 113.6(11) . . ?
C8X C7X C4X 111.5(10) . . ?
N1X C8X C7X 112.1(10) . . ?
C5X C4X C3X 116.1(11) . . ?
C5X C4X C7X 123.4(11) . . ?
C3X C4X C7X 120.4(12) . . ?
C4X C5X C6X 121.2(12) . . ?
C2X C3X C4X 122.4(15) . . ?
C3X C2X C1X 119.0(14) . . ?
C1X C6X C5X 119.2(15) . . ?
C6X C1X C2X 122.1(14) . . ?
C6X C1X O1X 120(2) . . ?
C2X C1X O1X 117.5(17) . . ?
C25 N14 C14 112.3(10) . . ?
C25 N14 C26 123.0(9) . . ?
C14 N14 C26 123.6(9) . . ?
C29 N18 C18 112.4(9) . . ?
C29 N18 C30 121.0(9) . . ?
C18 N18 C30 122.5(8) . . ?
C3 N3 C2 123.9(11) . . ?
C3 N3 C15 112.2(10) . . ?
C2 N3 C15 123.4(8) . . ?
C5 N5 C17 111.0(10) . . ?
C5 N5 C4 121.7(10) . . ?
C17 N5 C4 123.3(9) . . ?
C31 N20 C32 121.0(9) . . ?
C31 N20 C20 111.3(9) . . ?
C32 N20 C20 122.4(8) . . ?
C33 N21 C21 113.5(8) . . ?
C33 N21 C32 121.9(8) . . ?
C21 N21 C32 124.5(8) . . ?
C33 N22 C34 122.3(8) . . ?
C33 N22 C22 110.3(8) . . ?
C34 N22 C22 127.1(9) . . ?
C29 N17 C17 112.9(8) . . ?
C29 N17 C28 123.6(9) . . ?
C17 N17 C28 123.3(10) . . ?
C27 N15 C15 112.7(9) . . ?
C27 N15 C26 123.6(9) . . ?
C15 N15 C26 123.4(9) . . ?
C9 N9 C8 122.8(9) . . ?
C9 N9 C21 111.0(9) . . ?
C8 N9 C21 123.3(9) . . ?
C7 N8 C8 123.6(9) . . ?
C7 N8 C20 111.7(9) . . ?
C8 N8 C20 124.7(9) . . ?
C31 N19 C30 122.0(8) . . ?
C31 N19 C19 110.7(8) . . ?
C30 N19 C19 127.2(9) . . ?
C25 N13 C36 123.3(10) . . ?
C25 N13 C13 110.4(10) . . ?
C36 N13 C13 125.9(10) . . ?
C5 N6 C6 121.9(10) . . ?
C5 N6 C18 111.4(8) . . ?
C6 N6 C18 126.6(10) . . ?
C7 N7 C19 112.9(9) . . ?
C7 N7 C6 120.2(10) . . ?
C19 N7 C6 123.5(10) . . ?
C11 N12 C24 111.9(10) . . ?
C11 N12 C12 123.5(11) . . ?
C24 N12 C12 124.3(9) . . ?
C9 N10 C22 112.5(9) . . ?
C9 N10 C10 123.0(11) . . ?
C22 N10 C10 124.1(10) . . ?
C35 N23 C23 114.3(10) . . ?
C35 N23 C34 121.1(10) . . ?
C23 N23 C34 124.6(8) . . ?
C11 N11 C23 113.1(9) . . ?
C11 N11 C10 119.4(9) . . ?
C23 N11 C10 123.7(10) . . ?
C3 N4 C16 112.4(9) . . ?
C3 N4 C4 123.2(9) . . ?
C16 N4 C4 122.6(11) . . ?
C27 N16 C16 113.1(9) . . ?
C27 N16 C28 122.3(11) . . ?
C16 N16 C28 123.0(10) . . ?
C35 N24 C36 120.7(10) . . ?
C35 N24 C24 113.3(9) . . ?
C36 N24 C24 122.4(9) . . ?
C1 N2 C2 123.2(10) . . ?
C1 N2 C14 112.8(10) . . ?
C2 N2 C14 124.0(10) . . ?
N5 C17 N17 114.8(9) . . ?
N5 C17 C18 103.5(9) . . ?
N17 C17 C18 102.5(9) . . ?
C1 N1 C13 112.5(10) . . ?
C1 N1 C12 120.3(9) . . ?
C13 N1 C12 126.5(10) . . ?
O2 C3 N3 126.0(13) . . ?
O2 C3 N4 125.3(10) . . ?
N3 C3 N4 108.6(10) . . ?
O4 C7 N7 128.6(12) . . ?
O4 C7 N8 123.9(12) . . ?
N7 C7 N8 107.6(10) . . ?
N9 C8 N8 114.2(8) . . ?
N8 C20 N20 115.2(8) . . ?
N8 C20 C19 103.2(9) . . ?
N20 C20 C19 103.6(8) . . ?
O8 C27 N15 125.9(10) . . ?
O8 C27 N16 126.3(11) . . ?
N15 C27 N16 107.8(10) . . ?
N7 C19 N19 115.3(8) . . ?
N7 C19 C20 103.8(9) . . ?
N19 C19 C20 104.4(8) . . ?
N23 C23 N11 113.5(8) . . ?
N23 C23 C24 104.4(8) . . ?
N11 C23 C24 103.0(10) . . ?
N14 C14 N2 115.2(8) . . ?
N14 C14 C13 104.1(9) . . ?
N2 C14 C13 102.4(9) . . ?
N22 C34 N23 115.5(10) . . ?
N3 C15 N15 115.5(9) . . ?
N3 C15 C16 104.2(8) . . ?
N15 C15 C16 102.7(9) . . ?
N1 C13 N13 115.3(9) . . ?
N1 C13 C14 104.6(9) . . ?
N13 C13 C14 103.9(9) . . ?
O10 C31 N20 125.5(11) . . ?
O10 C31 N19 125.6(10) . . ?
N20 C31 N19 108.9(8) . . ?
N12 C24 N24 113.6(9) . . ?
N12 C24 C23 104.0(8) . . ?
N24 C24 C23 102.4(8) . . ?
N14 C26 N15 116.4(7) . . ?
O7 C25 N13 125.1(12) . . ?
O7 C25 N14 125.7(12) . . ?
N13 C25 N14 109.2(10) . . ?
N16 C16 N4 114.1(9) . . ?
N16 C16 C15 103.3(9) . . ?
N4 C16 C15 102.5(11) . . ?
O6 C11 N11 128.6(9) . . ?
O6 C11 N12 124.0(12) . . ?
N11 C11 N12 107.5(10) . . ?
N18 C18 N6 115.7(9) . . ?
N18 C18 C17 104.3(8) . . ?
N6 C18 C17 103.5(9) . . ?
N13 C36 N24 113.1(9) . . ?
O1 C1 N1 126.4(11) . . ?
O1 C1 N2 125.8(13) . . ?
N1 C1 N2 107.7(9) . . ?
N19 C30 N18 114.8(9) . . ?
O3 C5 N6 126.8(9) . . ?
O3 C5 N5 124.0(12) . . ?
N6 C5 N5 109.2(12) . . ?
N21 C21 N9 114.3(9) . . ?
N21 C21 C22 102.7(7) . . ?
N9 C21 C22 102.5(9) . . ?
N10 C22 N22 114.5(9) . . ?
N10 C22 C21 103.6(9) . . ?
N22 C22 C21 103.8(9) . . ?
O11 C33 N21 126.8(10) . . ?
O11 C33 N22 123.9(10) . . ?
N21 C33 N22 109.1(8) . . ?
O9 C29 N17 127.4(10) . . ?
O9 C29 N18 125.7(12) . . ?
N17 C29 N18 106.8(10) . . ?
N20 C32 N21 113.3(9) . . ?
N6 C6 N7 113.8(9) . . ?
N10 C10 N11 111.5(9) . . ?
N2 C2 N3 115.0(10) . . ?
N17 C28 N16 112.4(9) . . ?
O12 C35 N24 126.1(11) . . ?
O12 C35 N23 128.9(12) . . ?
N24 C35 N23 105.0(11) . . ?
O5 C9 N10 127.0(11) . . ?
O5 C9 N9 122.9(11) . . ?
N10 C9 N9 110.0(11) . . ?
N12 C12 N1 114.0(9) . . ?
N4 C4 N5 110.5(9) . . ?

_refine_diff_density_max         0.614
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.098

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_q6_octop_new
_database_code_depnum_ccdc_archive 'CCDC 1868758'
_audit_update_record             
;
2018-11-05 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[Mg(C36H36N24O12).4(H2O)]2+.(C8H12NO2)+.3Cl-.8.7(H2O)'
_chemical_formula_sum            'C44 H73.4 Cl3 Mg N25 O26.70'
_chemical_formula_weight         1510.3

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'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.6334(3)
_cell_length_b                   16.0589(4)
_cell_length_c                   30.9023(8)
_cell_angle_alpha                90
_cell_angle_beta                 99.950(3)
_cell_angle_gamma                90
_cell_volume                     6175.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    10094
_cell_measurement_theta_min      3.99
_cell_measurement_theta_max      71.30

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_F_000             3056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    2.382
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.57763
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3
_diffrn_reflns_number            22351
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         6.437
_diffrn_reflns_theta_max         65.077
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.936
_reflns_number_total             10470
_reflns_number_gt                7618
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1975P)²+22.9584P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10470
_refine_ls_number_parameters     952
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1530
_refine_ls_R_factor_gt           0.1140
_refine_ls_wR_factor_ref         0.3330
_refine_ls_wR_factor_gt          0.3056
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2W O 0.4634(4) 0.4665(3) 0.0364(2) 0.0528(14) Uani 1 1 d . . . . .
O3W O 0.3781(4) 0.5864(4) 0.08972(18) 0.0578(15) Uani 1 1 d . . . . .
O4W O 0.3814(5) 0.4200(5) 0.1218(2) 0.080(2) Uani 1 1 d . . . . .
O5W O 0.2763(5) 0.1946(3) 0.22449(18) 0.0542(14) Uani 1 1 d . . . . .
O6W O 0.3253(6) 0.2597(5) 0.1442(2) 0.088(2) Uani 1 1 d . . . . .
O7W O 0.5332(6) 0.3030(4) -0.0413(2) 0.0731(19) Uani 1 1 d . . . . .
O8W O 0.4944(5) 0.6978(4) 0.1907(2) 0.0683(17) Uiso 1 1 d . . . . .
Cl1 Cl 0.4938(3) 0.89050(17) 0.05649(10) 0.0636(7) Uani 0.8 1 d . . P A 1
O15W O 0.2973(10) 0.8461(7) -0.0157(3) 0.101(3) Uani 0.8 1 d . . P B 1
O9W O 0.5977(6) 0.8117(7) 0.1498(3) 0.081(3) Uani 0.8 1 d . . P C 1
Cl1A Cl 0.4196(11) 0.8811(9) 0.0257(4) 0.075(3) Uani 0.2 1 d . . P D 2
O13W O 0.624(3) 0.894(2) 0.0897(11) 0.072(9) Uiso 0.2 1 d . . P E 2
O9WA O 0.521(2) 0.852(2) 0.1607(11) 0.075(10) Uani 0.2 1 d . . P F 2
Cl2 Cl 0.8220(3) 1.0106(2) 0.08287(13) 0.0729(13) Uani 0.716(7) 1 d . . P G 1
O11W O 0.882(3) 1.086(2) -0.0055(11) 0.152(11) Uiso 0.4 1 d . . P H 1
O10W O 1.0392(10) 0.9321(9) 0.0587(4) 0.105(4) Uiso 0.716(7) 1 d . . P G 1
O11A O 0.992(3) 1.018(2) 0.0226(11) 0.124(11) Uiso 0.3 1 d . . P G 1
O12W O 0.754(2) 0.9447(19) 0.0929(10) 0.094(10) Uani 0.284(7) 1 d . . P E 2
Cl2A Cl 0.8869(9) 1.0365(7) 0.0315(3) 0.092(4) Uani 0.284(7) 1 d . . P G 2
Cl3 Cl 0.2345(9) 0.7217(8) -0.0133(3) 0.152(5) Uani 0.479(10) 1 d . . P I 1
O14W O 0.3270(12) 0.8509(10) 0.1136(5) 0.077(5) Uani 0.479(10) 1 d . . P I 1
Cl3A Cl 0.2518(7) 0.7044(5) 0.1240(3) 0.122(3) Uani 0.521(10) 1 d . . P I 2
O16W O 0.1856(8) 0.7111(7) 0.0100(4) 0.045(3) Uani 0.521(10) 1 d . . P I 2
C8X C 0.6738(10) 0.5727(9) 0.1287(4) 0.033(3) Uiso 0.4 1 d . . P J 1
H8X1 H 0.7384 0.5640 0.1514 0.040 Uiso 0.4 1 calc R U P J 1
H8X2 H 0.6415 0.6268 0.1346 0.040 Uiso 0.4 1 calc R U P J 1
O1X O 1.0668(13) 0.7798(11) 0.0751(5) 0.052(4) Uiso 0.4 1 d D . P J 1
H1X H 1.0554 0.8314 0.0744 0.078 Uiso 0.4 1 calc R U P J 1
C1X C 0.9708(14) 0.7374(14) 0.0782(6) 0.040(5) Uiso 0.4 1 d D . P J 1
C2X C 0.9882(12) 0.6536(10) 0.0745(5) 0.026(3) Uiso 0.4 1 d . . P J 1
H2X H 1.0571 0.6337 0.0712 0.031 Uiso 0.4 1 calc R U P J 1
C3X C 0.8957(15) 0.5920(11) 0.0758(4) 0.022(3) Uiso 0.4 1 d . . P J 1
H3X H 0.9030 0.5332 0.0742 0.026 Uiso 0.4 1 calc R U P J 1
C4X C 0.8069(17) 0.6292(13) 0.0792(6) 0.033(5) Uiso 0.4 1 d . . P J 1
C5X C 0.7902(14) 0.7198(10) 0.0823(4) 0.018(3) Uiso 0.4 1 d . . P J 1
H5X H 0.7219 0.7419 0.0850 0.021 Uiso 0.4 1 calc R U P J 1
C6X C 0.8752(16) 0.7702(13) 0.0811(5) 0.024(3) Uiso 0.4 1 d . . P J 1
H6X H 0.8670 0.8289 0.0823 0.029 Uiso 0.4 1 calc R U P J 1
C7X C 0.7064(10) 0.5749(7) 0.0832(3) 0.033(2) Uiso 0.4 1 d . . P J 1
H7X H 0.6439 0.5944 0.0612 0.040 Uiso 0.4 1 calc R U P J 1
O2X O 0.7301(17) 0.4865(10) 0.0739(5) 0.048(4) Uiso 0.4 1 d . . P J 1
H2X1 H 0.7495 0.4833 0.0493 0.071 Uiso 0.4 1 calc R U P J 1
N1X N 0.5965(9) 0.5058(7) 0.1312(3) 0.040(2) Uiso 0.4 1 d . . P J 1
H1X1 H 0.5781 0.5055 0.1584 0.059 Uiso 0.4 1 calc R U P J 1
H1X2 H 0.6267 0.4561 0.1262 0.059 Uiso 0.4 1 calc R U P J 1
H1X3 H 0.5368 0.5143 0.1106 0.059 Uiso 0.4 1 calc R U P J 1
C1XA C 0.9079(15) 0.7930(9) 0.0812(7) 0.048(9) Uiso 0.25 1 d DG . P K 2
C6XA C 0.7993(15) 0.7991(9) 0.0835(8) 0.061(9) Uiso 0.25 1 d G . P K 2
H6XA H 0.7667 0.8523 0.0842 0.073 Uiso 0.25 1 calc R U P K 2
C5XA C 0.7383(11) 0.7274(12) 0.0848(7) 0.035(6) Uiso 0.25 1 d G . P K 2
H5XA H 0.6640 0.7316 0.0863 0.041 Uiso 0.25 1 calc R U P K 2
C4XA C 0.7859(13) 0.6496(10) 0.0837(6) 0.011(5) Uiso 0.25 1 d G . P K 2
C3XA C 0.8946(14) 0.6435(9) 0.0814(6) 0.042(7) Uiso 0.25 1 d G . P K 2
H3XA H 0.9271 0.5903 0.0807 0.050 Uiso 0.25 1 calc R U P K 2
C2XA C 0.9556(11) 0.7152(12) 0.0802(7) 0.022(8) Uiso 0.25 1 d G . P K 2
H2XA H 1.0298 0.7110 0.0786 0.026 Uiso 0.25 1 calc R U P K 2
C8XA C 0.6738(10) 0.5727(9) 0.1287(4) 0.033(3) Uiso 0.25 1 d . . P K 2
H8X3 H 0.7384 0.5640 0.1514 0.040 Uiso 0.25 1 calc R U P K 2
H8X4 H 0.6415 0.6268 0.1346 0.040 Uiso 0.25 1 calc R U P K 2
N1XA N 0.5965(9) 0.5058(7) 0.1312(3) 0.040(2) Uiso 0.25 1 d . . P K 2
H1X4 H 0.5782 0.5055 0.1584 0.059 Uiso 0.25 1 calc R U P K 2
H1X5 H 0.6266 0.4561 0.1262 0.059 Uiso 0.25 1 calc R U P K 2
H1X6 H 0.5367 0.5144 0.1106 0.059 Uiso 0.25 1 calc R U P K 2
O1XA O 0.971(3) 0.8643(18) 0.0816(12) 0.107(11) Uiso 0.25 1 d D . P K 2
H1XA H 0.9330 0.9067 0.0832 0.161 Uiso 0.25 1 calc R U P K 2
C7XA C 0.7064(10) 0.5749(7) 0.0832(3) 0.033(2) Uiso 0.25 1 d . . P K 2
H7XA H 0.6434 0.5785 0.0588 0.040 Uiso 0.25 1 calc R U P K 2
O2XA O 0.7661(19) 0.4996(15) 0.0824(7) 0.041(6) Uiso 0.25 1 d . . P K 2
H2X2 H 0.7882 0.4958 0.0584 0.061 Uiso 0.25 1 calc R U P K 2
C4XB C 0.7631(10) 0.6165(8) 0.0823(4) 0.023(4) Uiso 0.35 1 d G . P L 3
C3XB C 0.8604(11) 0.5790(7) 0.0787(4) 0.017(4) Uiso 0.35 1 d G . P L 3
H3XB H 0.8654 0.5201 0.0774 0.020 Uiso 0.35 1 calc R U P L 3
C2XB C 0.9504(10) 0.6278(10) 0.0769(4) 0.025(4) Uiso 0.35 1 d G . P L 3
H2XB H 1.0169 0.6022 0.0744 0.030 Uiso 0.35 1 calc R U P L 3
C1XB C 0.9432(12) 0.7141(9) 0.0787(6) 0.10(2) Uiso 0.35 1 d DG . P L 3
C6XB C 0.8459(15) 0.7515(7) 0.0823(6) 0.045(7) Uiso 0.35 1 d G . P L 3
H6XB H 0.8409 0.8105 0.0835 0.054 Uiso 0.35 1 calc R U P L 3
C5XB C 0.7559(11) 0.7027(9) 0.0841(5) 0.034(5) Uiso 0.35 1 d G . P L 3
H5XB H 0.6894 0.7283 0.0865 0.041 Uiso 0.35 1 calc R U P L 3
O1XB O 1.0329(19) 0.7664(17) 0.0773(9) 0.088(8) Uiso 0.35 1 d D . P L 3
H1XB H 1.0146 0.8164 0.0792 0.132 Uiso 0.35 1 calc R U P L 3
C7XB C 0.662(2) 0.5626(15) 0.0858(6) 0.043(5) Uiso 0.35 1 d D . P L 3
H7XB H 0.5965 0.5897 0.0687 0.051 Uiso 0.35 1 calc R U P L 3
O2XB O 0.6760(15) 0.4862(10) 0.0683(5) 0.046(4) Uiso 0.35 1 d . . P L 3
H2X3 H 0.6224 0.4561 0.0698 0.069 Uiso 0.35 1 calc R U P L 3
N1XB N 0.5643(18) 0.5074(14) 0.1401(7) 0.051(6) Uiso 0.35 1 d . . P L 3
H1X7 H 0.5595 0.5046 0.1691 0.076 Uiso 0.35 1 calc R U P L 3
H1X8 H 0.5747 0.4554 0.1299 0.076 Uiso 0.35 1 calc R U P L 3
H1X9 H 0.5024 0.5290 0.1248 0.076 Uiso 0.35 1 calc R U P L 3
C8XB C 0.652(3) 0.559(2) 0.1345(8) 0.060(10) Uiso 0.35 1 d D . P L 3
H8X5 H 0.7195 0.5367 0.1519 0.072 Uiso 0.35 1 calc R U P L 3
H8X6 H 0.6411 0.6160 0.1453 0.072 Uiso 0.35 1 calc R U P L 3
O1W O 0.2581(16) 0.5438(14) 0.0056(7) 0.015(8) Uiso 0.28(6) 1 d . . P M 1
O1WA O 0.216(4) 0.5480(8) 0.0033(7) 0.086(6) Uani 0.72(6) 1 d . . P M 2
O4 O 0.7236(3) 0.3737(3) 0.15928(14) 0.0325(10) Uani 1 1 d . . . . .
O8 O 0.1216(3) 0.0846(2) 0.12980(11) 0.0194(8) Uani 1 1 d . . . . .
Mg1 Mg 0.3143(3) 0.4831(2) 0.06155(11) 0.0695(9) Uani 1 1 d . . . . .
O9 O 0.4014(3) 0.0065(2) 0.16072(12) 0.0210(8) Uani 1 1 d . . . . .
O1 O 0.1763(3) 0.4972(3) 0.08716(13) 0.0251(9) Uani 1 1 d . . . . .
O2 O 0.2707(3) 0.3717(3) 0.03006(12) 0.0239(9) Uani 1 1 d . . . . .
O11 O 0.4376(3) 0.2221(3) 0.30637(14) 0.0309(10) Uani 1 1 d . . . . .
O7 O 0.0132(4) 0.2231(2) 0.19293(13) 0.0286(9) Uani 1 1 d . . . . .
N4 N 0.2605(3) 0.2281(3) 0.02933(13) 0.0170(9) Uani 1 1 d . . . . .
O12 O 0.1771(3) 0.2919(3) 0.28939(15) 0.0319(10) Uani 1 1 d . . . . .
O3 O 0.5469(3) 0.3075(3) 0.06000(17) 0.0429(13) Uani 1 1 d . . . . .
N2 N 0.0411(3) 0.3997(3) 0.08133(14) 0.0176(9) Uani 1 1 d . . . . .
N13 N 0.0076(3) 0.3652(3) 0.18459(14) 0.0176(9) Uani 1 1 d . . . . .
O10 O 0.5697(3) 0.0718(3) 0.25589(13) 0.0252(9) Uani 1 1 d . . . . .
N15 N 0.0613(3) 0.1881(3) 0.08019(13) 0.0147(9) Uani 1 1 d . . . . .
O6 O 0.3563(3) 0.5545(3) 0.18337(13) 0.0339(10) Uani 1 1 d . . . . .
N14 N -0.0181(3) 0.2865(3) 0.12472(14) 0.0180(9) Uani 1 1 d . . . . .
N18 N 0.5463(3) 0.0665(3) 0.13611(14) 0.0160(9) Uani 1 1 d . . . . .
N10 N 0.5384(4) 0.4797(3) 0.28114(16) 0.0232(10) Uani 1 1 d . . . . .
N22 N 0.4642(3) 0.3630(3) 0.31622(16) 0.0242(10) Uani 1 1 d . . . . .
N12 N 0.1983(4) 0.5203(3) 0.20820(14) 0.0207(10) Uani 1 1 d . . . . .
O5 O 0.6271(3) 0.5128(3) 0.22429(13) 0.0275(9) Uani 1 1 d . . . . .
N3 N 0.1152(3) 0.3005(3) 0.03553(14) 0.0161(9) Uani 1 1 d . . . . .
N24 N 0.1279(3) 0.4125(3) 0.24970(14) 0.0187(9) Uani 1 1 d . . . . .
N17 N 0.3869(3) 0.0732(3) 0.09367(14) 0.0167(9) Uani 1 1 d . . . . .
N11 N 0.3527(4) 0.5174(3) 0.25512(15) 0.0224(10) Uani 1 1 d . . . . .
N20 N 0.6833(4) 0.1848(3) 0.26234(15) 0.0209(10) Uani 1 1 d . . . . .
N21 N 0.6007(4) 0.2860(3) 0.30418(15) 0.0214(10) Uani 1 1 d . . . . .
N16 N 0.2001(3) 0.1113(3) 0.06901(14) 0.0173(9) Uani 1 1 d . . . . .
N8 N 0.7509(4) 0.3027(3) 0.22541(16) 0.0246(10) Uani 1 1 d . . . . .
N23 N 0.2798(3) 0.4115(3) 0.29754(15) 0.0217(10) Uani 1 1 d . . . . .
N7 N 0.7224(4) 0.2290(3) 0.16361(16) 0.0252(11) Uani 1 1 d . . . . .
C27 C 0.1272(4) 0.1236(3) 0.09684(16) 0.0153(10) Uani 1 1 d . . . . .
C20 C 0.7667(4) 0.2177(3) 0.24059(18) 0.0202(11) Uani 1 1 d . . . . .
H20 H 0.8398 0.2091 0.2585 0.024 Uiso 1 1 calc R U . . .
N9 N 0.6781(4) 0.4038(3) 0.27183(16) 0.0252(11) Uani 1 1 d . . . . .
C26 C -0.0322(4) 0.2110(3) 0.09834(17) 0.0161(10) Uani 1 1 d . . . . .
H26A H -0.0506 0.1646 0.1168 0.019 Uiso 1 1 calc R U . . .
H26B H -0.0935 0.2189 0.0740 0.019 Uiso 1 1 calc R U . . .
N1 N 0.0796(3) 0.4738(3) 0.14258(14) 0.0186(9) Uani 1 1 d . . . . .
C25 C 0.0029(4) 0.2846(3) 0.16982(18) 0.0191(11) Uani 1 1 d . . . . .
N19 N 0.6683(3) 0.1074(3) 0.20213(14) 0.0217(10) Uani 1 1 d . . . . .
N6 N 0.6005(3) 0.1877(3) 0.09837(16) 0.0238(11) Uani 1 1 d . . . . .
C12 C 0.1221(5) 0.5439(3) 0.16958(18) 0.0222(11) Uani 1 1 d . . . . .
H12A H 0.1579 0.5825 0.1516 0.027 Uiso 1 1 calc R U . . .
H12B H 0.0618 0.5743 0.1790 0.027 Uiso 1 1 calc R U . . .
C4 C 0.3638(4) 0.2143(4) 0.01643(17) 0.0219(12) Uani 1 1 d . . . . .
H4A H 0.3554 0.1719 -0.0071 0.026 Uiso 1 1 calc R U . . .
H4B H 0.3874 0.2667 0.0042 0.026 Uiso 1 1 calc R U . . .
C15 C 0.0797(4) 0.2153(3) 0.03702(15) 0.0144(10) Uani 1 1 d . . . . .
H15 H 0.0167 0.2031 0.0135 0.017 Uiso 1 1 calc R U . . .
C14 C -0.0370(4) 0.3699(3) 0.10740(16) 0.0154(10) Uani 1 1 d . . . . .
H14 H -0.1124 0.3772 0.0916 0.018 Uiso 1 1 calc R U . . .
C3 C 0.2208(4) 0.3064(3) 0.03176(15) 0.0173(11) Uani 1 1 d . . . . .
C16 C 0.1810(4) 0.1641(3) 0.03080(15) 0.0152(10) Uani 1 1 d . . . . .
H16 H 0.1677 0.1309 0.0030 0.018 Uiso 1 1 calc R U . . .
C17 C 0.4590(4) 0.1010(4) 0.06492(17) 0.0206(12) Uani 1 1 d . . . . .
H17 H 0.4582 0.0630 0.0392 0.025 Uiso 1 1 calc R U . . .
C30 C 0.6295(4) 0.0413(4) 0.17187(17) 0.0207(11) Uani 1 1 d . . . . .
H30A H 0.6013 -0.0041 0.1883 0.025 Uiso 1 1 calc R U . . .
H30B H 0.6907 0.0186 0.1595 0.025 Uiso 1 1 calc R U . . .
C32 C 0.6648(5) 0.2115(4) 0.30528(18) 0.0250(12) Uani 1 1 d . . . . .
H32A H 0.6284 0.1660 0.3186 0.030 Uiso 1 1 calc R U . . .
H32B H 0.7351 0.2214 0.3244 0.030 Uiso 1 1 calc R U . . .
N5 N 0.4457(3) 0.1873(3) 0.05171(15) 0.0217(10) Uani 1 1 d . . . . .
C13 C -0.0136(4) 0.4249(3) 0.14928(17) 0.0174(11) Uani 1 1 d . . . . .
H13 H -0.0762 0.4613 0.1522 0.021 Uiso 1 1 calc R U . . .
C2 C 0.0474(4) 0.3728(3) 0.03730(16) 0.0164(10) Uani 1 1 d . . . . .
H2A H 0.0753 0.4193 0.0215 0.020 Uiso 1 1 calc R U . . .
H2B H -0.0260 0.3598 0.0217 0.020 Uiso 1 1 calc R U . . .
C24 C 0.1652(4) 0.4972(3) 0.24917(17) 0.0193(11) Uani 1 1 d . . . . .
H24 H 0.1126 0.5377 0.2579 0.023 Uiso 1 1 calc R U . . .
C18 C 0.5702(4) 0.1019(4) 0.09581(17) 0.0210(12) Uani 1 1 d . . . . .
H18 H 0.6239 0.0673 0.0836 0.025 Uiso 1 1 calc R U . . .
C35 C 0.1938(4) 0.3645(4) 0.27975(17) 0.0219(12) Uani 1 1 d . . . . .
C31 C 0.6328(4) 0.1176(3) 0.24167(17) 0.0197(11) Uani 1 1 d . . . . .
C19 C 0.7514(4) 0.1667(4) 0.19712(17) 0.0191(11) Uani 1 1 d . . . . .
H19 H 0.8194 0.1378 0.1935 0.023 Uiso 1 1 calc R U . . .
C1 C 0.1071(4) 0.4595(3) 0.10262(17) 0.0174(11) Uani 1 1 d . U . . .
C29 C 0.4407(4) 0.0441(3) 0.13320(16) 0.0150(10) Uani 1 1 d . . . . .
C5 C 0.5322(4) 0.2352(4) 0.06915(19) 0.0238(12) Uani 1 1 d . . . . .
C10 C 0.4589(4) 0.5465(4) 0.27378(19) 0.0225(12) Uani 1 1 d . . . . .
H10A H 0.4559 0.5744 0.3021 0.027 Uiso 1 1 calc R U . . .
H10B H 0.4821 0.5883 0.2538 0.027 Uiso 1 1 calc R U . . .
C9 C 0.6148(4) 0.4692(4) 0.25537(18) 0.0218(12) Uani 1 1 d . . . . .
C34 C 0.3642(4) 0.3820(4) 0.33179(19) 0.0295(14) Uani 1 1 d . . . . .
H34A H 0.3389 0.3312 0.3451 0.035 Uiso 1 1 calc R U . . .
H34B H 0.3787 0.4249 0.3551 0.035 Uiso 1 1 calc R U . . .
C22 C 0.5504(4) 0.4230(4) 0.31771(18) 0.0257(13) Uani 1 1 d . . . . .
H22 H 0.5648 0.4531 0.3465 0.031 Uiso 1 1 calc R U . . .
C33 C 0.4940(4) 0.2849(4) 0.30848(17) 0.0226(12) Uani 1 1 d . . . . .
C28 C 0.2779(4) 0.0444(3) 0.07546(17) 0.0185(11) Uani 1 1 d . . . . .
H28A H 0.2790 0.0166 0.0469 0.022 Uiso 1 1 calc R U . . .
H28B H 0.2552 0.0027 0.0956 0.022 Uiso 1 1 calc R U . . .
C23 C 0.2721(4) 0.4962(4) 0.28191(17) 0.0187(11) Uani 1 1 d . . . . .
H23 H 0.2717 0.5369 0.3064 0.022 Uiso 1 1 calc R U . . .
C8 C 0.7697(4) 0.3763(4) 0.2533(2) 0.0253(13) Uani 1 1 d . . . . .
H8A H 0.8297 0.3644 0.2776 0.030 Uiso 1 1 calc R U . . .
H8B H 0.7927 0.4224 0.2358 0.030 Uiso 1 1 calc R U . . .
C36 C 0.0207(4) 0.3868(3) 0.23063(16) 0.0180(11) Uani 1 1 d . . . . .
H36A H -0.0298 0.4324 0.2342 0.022 Uiso 1 1 calc R U . . .
H36B H 0.0008 0.3380 0.2471 0.022 Uiso 1 1 calc R U . . .
C21 C 0.6467(4) 0.3684(4) 0.31086(18) 0.0228(12) Uani 1 1 d . . . . .
H21 H 0.7064 0.3705 0.3367 0.027 Uiso 1 1 calc R U . . .
C6 C 0.7084(4) 0.2138(4) 0.11663(18) 0.0253(13) Uani 1 1 d . . . . .
H6A H 0.7254 0.2654 0.1017 0.030 Uiso 1 1 calc R U . . .
H6B H 0.7597 0.1703 0.1109 0.030 Uiso 1 1 calc R U . . .
C7 C 0.7300(4) 0.3092(4) 0.18051(19) 0.0241(12) Uani 1 1 d . . . . .
C11 C 0.3070(5) 0.5329(4) 0.21287(18) 0.0237(12) 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
O2W Mg1 2.174(7) . ?
O3W Mg1 1.979(7) . ?
O4W Mg1 2.161(8) . ?
O13W O12W 1.82(5) . ?
O10W O11A 1.81(4) . ?
O11A O11A 1.56(7) 3_775 ?
C8X N1X 1.463(18) . ?
C8X C7X 1.530(16) . ?
O1X C1X 1.408(18) . ?
C1X C6X 1.33(2) . ?
C1X C2X 1.37(3) . ?
C2X C3X 1.54(2) . ?
C3X C4X 1.29(3) . ?
C4X C5X 1.48(3) . ?
C4X C7X 1.56(2) . ?
C5X C6X 1.35(3) . ?
C7X O2X 1.49(2) . ?
C1XA C6XA 1.3900 . ?
C1XA C2XA 1.3900 . ?
C1XA O1XA 1.395(19) . ?
C6XA C5XA 1.3900 . ?
C5XA C4XA 1.3900 . ?
C4XA C3XA 1.3900 . ?
C3XA C2XA 1.3900 . ?
C4XB C3XB 1.3900 . ?
C4XB C5XB 1.3900 . ?
C4XB C7XB 1.56(3) . ?
C3XB C2XB 1.3900 . ?
C2XB C1XB 1.3900 . ?
C1XB C6XB 1.3900 . ?
C1XB O1XB 1.417(18) . ?
C6XB C5XB 1.3900 . ?
C7XB O2XB 1.37(3) . ?
C7XB C8XB 1.534(18) . ?
N1XB C8XB 1.42(4) . ?
O1W Mg1 2.00(2) . ?
O1WA Mg1 2.26(3) . ?
O4 C7 1.221(7) . ?
O8 C27 1.209(6) . ?
Mg1 O1 2.047(5) . ?
Mg1 O2 2.066(6) . ?
O9 C29 1.217(6) . ?
O1 C1 1.226(7) . ?
O2 C3 1.229(7) . ?
O11 C33 1.229(7) . ?
O7 C25 1.212(7) . ?
N4 C3 1.361(7) . ?
N4 C16 1.443(7) . ?
N4 C4 1.446(6) . ?
O12 C35 1.231(7) . ?
O3 C5 1.216(7) . ?
N2 C1 1.364(7) . ?
N2 C2 1.443(6) . ?
N2 C14 1.458(6) . ?
N13 C25 1.371(7) . ?
N13 C13 1.442(7) . ?
N13 C36 1.446(6) . ?
O10 C31 1.221(7) . ?
N15 C27 1.372(6) . ?
N15 C26 1.440(6) . ?
N15 C15 1.460(6) . ?
O6 C11 1.239(7) . ?
N14 C25 1.374(7) . ?
N14 C14 1.448(7) . ?
N14 C26 1.455(6) . ?
N18 C29 1.371(6) . ?
N18 C30 1.445(6) . ?
N18 C18 1.447(6) . ?
N10 C9 1.364(7) . ?
N10 C22 1.438(7) . ?
N10 C10 1.460(7) . ?
N22 C33 1.342(8) . ?
N22 C22 1.449(7) . ?
N22 C34 1.459(7) . ?
N12 C11 1.371(7) . ?
N12 C24 1.448(6) . ?
N12 C12 1.448(7) . ?
O5 C9 1.220(7) . ?
N3 C3 1.362(7) . ?
N3 C15 1.444(7) . ?
N3 C2 1.450(7) . ?
N24 C35 1.372(7) . ?
N24 C24 1.440(7) . ?
N24 C36 1.442(6) . ?
N17 C29 1.373(6) . ?
N17 C17 1.449(6) . ?
N17 C28 1.469(6) . ?
N11 C11 1.357(8) . ?
N11 C10 1.444(7) . ?
N11 C23 1.459(6) . ?
N20 C31 1.357(7) . ?
N20 C20 1.444(7) . ?
N20 C32 1.451(7) . ?
N21 C33 1.378(7) . ?
N21 C32 1.442(8) . ?
N21 C21 1.446(7) . ?
N16 C27 1.378(6) . ?
N16 C16 1.440(6) . ?
N16 C28 1.447(7) . ?
N8 C7 1.371(8) . ?
N8 C20 1.447(7) . ?
N8 C8 1.457(8) . ?
N23 C35 1.359(7) . ?
N23 C23 1.441(8) . ?
N23 C34 1.447(7) . ?
N7 C7 1.386(8) . ?
N7 C19 1.441(7) . ?
N7 C6 1.452(7) . ?
C20 C19 1.556(7) . ?
N9 C9 1.365(7) . ?
N9 C8 1.447(7) . ?
N9 C21 1.450(7) . ?
N1 C1 1.359(7) . ?
N1 C12 1.449(7) . ?
N1 C13 1.459(6) . ?
N19 C31 1.382(7) . ?
N19 C30 1.443(7) . ?
N19 C19 1.446(7) . ?
N6 C5 1.369(7) . ?
N6 C18 1.429(8) . ?
N6 C6 1.444(7) . ?
C4 N5 1.434(7) . ?
C15 C16 1.560(7) . ?
C14 C13 1.552(7) . ?
C17 N5 1.447(7) . ?
C17 C18 1.556(7) . ?
N5 C5 1.369(7) . ?
C24 C23 1.541(7) . ?
C22 C21 1.544(8) . ?

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
O11A O11A O10W 101(3) 3_775 . ?
N1X C8X C7X 110.7(10) . . ?
C6X C1X C2X 123.5(19) . . ?
C6X C1X O1X 128(2) . . ?
C2X C1X O1X 108.5(15) . . ?
C1X C2X C3X 119.8(14) . . ?
C4X C3X C2X 112.3(15) . . ?
C3X C4X C5X 126.7(17) . . ?
C3X C4X C7X 118.5(17) . . ?
C5X C4X C7X 114.7(16) . . ?
C6X C5X C4X 117.8(15) . . ?
C1X C6X C5X 119.9(18) . . ?
O2X C7X C8X 104.6(11) . . ?
O2X C7X C4X 108.8(14) . . ?
C8X C7X C4X 115.9(11) . . ?
C6XA C1XA C2XA 120.0 . . ?
C6XA C1XA O1XA 121(2) . . ?
C2XA C1XA O1XA 119(2) . . ?
C1XA C6XA C5XA 120.0 . . ?
C6XA C5XA C4XA 120.0 . . ?
C3XA C4XA C5XA 120.0 . . ?
C4XA C3XA C2XA 120.0 . . ?
C3XA C2XA C1XA 120.0 . . ?
C3XB C4XB C5XB 120.0 . . ?
C3XB C4XB C7XB 120.8(12) . . ?
C5XB C4XB C7XB 119.2(12) . . ?
C2XB C3XB C4XB 120.0 . . ?
C3XB C2XB C1XB 120.0 . . ?
C6XB C1XB C2XB 120.0 . . ?
C6XB C1XB O1XB 117.9(16) . . ?
C2XB C1XB O1XB 122.1(16) . . ?
C5XB C6XB C1XB 120.0 . . ?
C6XB C5XB C4XB 120.0 . . ?
O2XB C7XB C8XB 113(2) . . ?
O2XB C7XB C4XB 107.8(18) . . ?
C8XB C7XB C4XB 107.1(19) . . ?
N1XB C8XB C7XB 110(2) . . ?
O3W Mg1 O1W 91.6(6) . . ?
O3W Mg1 O1 92.7(2) . . ?
O1W Mg1 O1 94.7(8) . . ?
O3W Mg1 O2 171.3(3) . . ?
O1W Mg1 O2 89.4(6) . . ?
O1 Mg1 O2 95.9(2) . . ?
O3W Mg1 O4W 86.8(3) . . ?
O1W Mg1 O4W 177.6(6) . . ?
O1 Mg1 O4W 87.3(2) . . ?
O2 Mg1 O4W 91.9(3) . . ?
O3W Mg1 O2W 87.0(3) . . ?
O1W Mg1 O2W 87.2(8) . . ?
O1 Mg1 O2W 178.1(3) . . ?
O2 Mg1 O2W 84.4(2) . . ?
O4W Mg1 O2W 90.9(3) . . ?
O3W Mg1 O1WA 95.1(6) . . ?
O1 Mg1 O1WA 82.5(7) . . ?
O2 Mg1 O1WA 87.7(5) . . ?
O4W Mg1 O1WA 169.7(8) . . ?
O2W Mg1 O1WA 99.3(7) . . ?
C1 O1 Mg1 143.9(4) . . ?
C3 O2 Mg1 144.6(4) . . ?
C3 N4 C16 113.0(4) . . ?
C3 N4 C4 121.0(4) . . ?
C16 N4 C4 124.5(5) . . ?
C1 N2 C2 122.4(4) . . ?
C1 N2 C14 112.4(4) . . ?
C2 N2 C14 125.2(4) . . ?
C25 N13 C13 112.6(4) . . ?
C25 N13 C36 123.0(4) . . ?
C13 N13 C36 124.0(4) . . ?
C27 N15 C26 122.1(4) . . ?
C27 N15 C15 112.7(4) . . ?
C26 N15 C15 123.4(4) . . ?
C25 N14 C14 112.7(4) . . ?
C25 N14 C26 122.2(4) . . ?
C14 N14 C26 124.6(4) . . ?
C29 N18 C30 123.2(4) . . ?
C29 N18 C18 113.1(4) . . ?
C30 N18 C18 122.4(4) . . ?
C9 N10 C22 113.1(5) . . ?
C9 N10 C10 122.4(5) . . ?
C22 N10 C10 124.3(5) . . ?
C33 N22 C22 113.2(5) . . ?
C33 N22 C34 122.6(5) . . ?
C22 N22 C34 122.6(5) . . ?
C11 N12 C24 112.4(4) . . ?
C11 N12 C12 123.9(5) . . ?
C24 N12 C12 122.5(4) . . ?
C3 N3 C15 112.5(4) . . ?
C3 N3 C2 122.8(4) . . ?
C15 N3 C2 124.7(4) . . ?
C35 N24 C24 112.1(4) . . ?
C35 N24 C36 122.2(5) . . ?
C24 N24 C36 123.5(5) . . ?
C29 N17 C17 112.5(4) . . ?
C29 N17 C28 121.4(4) . . ?
C17 N17 C28 120.6(4) . . ?
C11 N11 C10 122.5(5) . . ?
C11 N11 C23 111.4(4) . . ?
C10 N11 C23 122.7(4) . . ?
C31 N20 C20 113.2(4) . . ?
C31 N20 C32 121.9(5) . . ?
C20 N20 C32 124.3(4) . . ?
C33 N21 C32 122.9(5) . . ?
C33 N21 C21 111.9(5) . . ?
C32 N21 C21 123.1(4) . . ?
C27 N16 C16 113.0(4) . . ?
C27 N16 C28 122.1(4) . . ?
C16 N16 C28 124.3(4) . . ?
C7 N8 C20 113.1(5) . . ?
C7 N8 C8 121.3(5) . . ?
C20 N8 C8 125.1(5) . . ?
C35 N23 C23 112.7(4) . . ?
C35 N23 C34 123.4(5) . . ?
C23 N23 C34 123.6(5) . . ?
C7 N7 C19 112.4(5) . . ?
C7 N7 C6 121.4(5) . . ?
C19 N7 C6 125.0(5) . . ?
O8 C27 N15 126.0(5) . . ?
O8 C27 N16 126.4(5) . . ?
N15 C27 N16 107.6(4) . . ?
N20 C20 N8 115.1(4) . . ?
N20 C20 C19 102.6(4) . . ?
N8 C20 C19 103.1(4) . . ?
C9 N9 C8 123.0(5) . . ?
C9 N9 C21 112.6(4) . . ?
C8 N9 C21 124.3(5) . . ?
N15 C26 N14 113.7(4) . . ?
C1 N1 C12 121.8(4) . . ?
C1 N1 C13 112.2(4) . . ?
C12 N1 C13 124.4(4) . . ?
O7 C25 N13 125.4(5) . . ?
O7 C25 N14 126.8(5) . . ?
N13 C25 N14 107.8(5) . . ?
C31 N19 C30 122.3(4) . . ?
C31 N19 C19 111.6(4) . . ?
C30 N19 C19 125.9(4) . . ?
C5 N6 C18 111.6(5) . . ?
C5 N6 C6 122.7(5) . . ?
C18 N6 C6 121.9(5) . . ?
N12 C12 N1 113.5(5) . . ?
N5 C4 N4 113.8(4) . . ?
N3 C15 N15 114.3(4) . . ?
N3 C15 C16 103.2(4) . . ?
N15 C15 C16 102.6(4) . . ?
N14 C14 N2 115.1(4) . . ?
N14 C14 C13 102.9(4) . . ?
N2 C14 C13 103.0(4) . . ?
O2 C3 N4 126.1(5) . . ?
O2 C3 N3 125.5(5) . . ?
N4 C3 N3 108.4(4) . . ?
N16 C16 N4 115.2(4) . . ?
N16 C16 C15 103.5(4) . . ?
N4 C16 C15 102.7(4) . . ?
N5 C17 N17 114.4(4) . . ?
N5 C17 C18 102.3(4) . . ?
N17 C17 C18 102.9(4) . . ?
N19 C30 N18 114.2(4) . . ?
N21 C32 N20 113.7(4) . . ?
C5 N5 C4 123.5(5) . . ?
C5 N5 C17 112.4(4) . . ?
C4 N5 C17 122.5(5) . . ?
N13 C13 N1 114.6(4) . . ?
N13 C13 C14 103.7(4) . . ?
N1 C13 C14 103.3(4) . . ?
N2 C2 N3 113.9(4) . . ?
N24 C24 N12 113.3(4) . . ?
N24 C24 C23 103.6(4) . . ?
N12 C24 C23 103.0(4) . . ?
N6 C18 N18 115.1(5) . . ?
N6 C18 C17 104.3(4) . . ?
N18 C18 C17 103.0(4) . . ?
O12 C35 N23 125.9(5) . . ?
O12 C35 N24 126.0(5) . . ?
N23 C35 N24 108.1(5) . . ?
O10 C31 N20 126.4(5) . . ?
O10 C31 N19 125.3(5) . . ?
N20 C31 N19 108.2(5) . . ?
N7 C19 N19 115.9(4) . . ?
N7 C19 C20 103.5(4) . . ?
N19 C19 C20 103.8(4) . . ?
O1 C1 N1 125.6(5) . . ?
O1 C1 N2 125.3(5) . . ?
N1 C1 N2 109.0(4) . . ?
O9 C29 N18 126.5(5) . . ?
O9 C29 N17 126.3(4) . . ?
N18 C29 N17 107.2(4) . . ?
O3 C5 N6 125.5(5) . . ?
O3 C5 N5 126.0(5) . . ?
N6 C5 N5 108.4(5) . . ?
N11 C10 N10 113.0(5) . . ?
O5 C9 N10 126.1(5) . . ?
O5 C9 N9 126.1(5) . . ?
N10 C9 N9 107.8(5) . . ?
N23 C34 N22 113.4(5) . . ?
N10 C22 N22 114.8(5) . . ?
N10 C22 C21 103.3(4) . . ?
N22 C22 C21 102.9(5) . . ?
O11 C33 N22 126.7(5) . . ?
O11 C33 N21 124.9(6) . . ?
N22 C33 N21 108.4(5) . . ?
N16 C28 N17 112.8(4) . . ?
N23 C23 N11 113.3(4) . . ?
N23 C23 C24 103.3(4) . . ?
N11 C23 C24 104.1(4) . . ?
N9 C8 N8 115.0(4) . . ?
N24 C36 N13 114.2(4) . . ?
N21 C21 N9 113.7(5) . . ?
N21 C21 C22 103.5(4) . . ?
N9 C21 C22 103.1(4) . . ?
N6 C6 N7 112.6(4) . . ?
O4 C7 N8 126.3(6) . . ?
O4 C7 N7 126.2(5) . . ?
N8 C7 N7 107.4(5) . . ?
O6 C11 N11 125.1(5) . . ?
O6 C11 N12 125.8(5) . . ?
N11 C11 N12 109.1(4) . . ?

_refine_diff_density_max         0.899
_refine_diff_density_min         -1.785
_refine_diff_density_rms         0.137

_shelxl_version_number           2013-3

