# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is (c) The Royal Society of Chemistry 2010


data_global

_journal_coden_Cambridge         177

loop_
_publ_author_name
'Curiel, David'
'Mas-Montoya, Miriam'
'Molina, Pedro'

_publ_contact_author_name        'Curiel, David'
_publ_contact_author_email       davidcc@um.es

_publ_section_title              
;
A new building block for anion supramolecular chemistry.
Study of carbazolocarbazole as anion receptor.
;

# Attachment '- Fig-5.cif'

data_48cloros
_database_code_depnum_ccdc_archive 'CCDC 787231'
#TrackingRef '- Fig-5.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H82 Cl N3 O2'
_chemical_formula_weight         840.68

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1884(12)
_cell_length_b                   15.6187(18)
_cell_length_c                   16.3086(19)
_cell_angle_alpha                101.378(2)
_cell_angle_beta                 93.392(2)
_cell_angle_gamma                95.643(2)
_cell_volume                     2523.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6007
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      28.70

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8526
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31678
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         28.74
_reflns_number_total             11915
_reflns_number_gt                10891
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+1.1594P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'NH free, Me rigid, others riding'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11915
_refine_ls_number_parameters     574
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1416
_refine_ls_wR_factor_gt          0.1377
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_restrained_S_all      1.169
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.33152(13) 0.59402(9) 0.28834(8) 0.0184(3) Uani 1 1 d . . .
H01 H 0.298(2) 0.5559(14) 0.2438(14) 0.033(6) Uiso 1 1 d . . .
N2 N 0.38138(13) 0.39457(9) 0.23255(8) 0.0186(3) Uani 1 1 d . . .
H02 H 0.334(2) 0.4257(14) 0.2053(13) 0.032(5) Uiso 1 1 d . . .
O1 O 0.59897(11) 0.75912(7) 0.51170(7) 0.0221(2) Uani 1 1 d . . .
O2 O 0.70254(11) 0.29587(7) 0.38999(7) 0.0217(2) Uani 1 1 d . . .
C1 C 0.30789(15) 0.68076(10) 0.30113(9) 0.0188(3) Uani 1 1 d . . .
C2 C 0.21622(16) 0.71962(11) 0.25728(10) 0.0217(3) Uani 1 1 d . . .
H2 H 0.1586 0.6858 0.2120 0.026 Uiso 1 1 calc R . .
C3 C 0.21267(17) 0.80908(11) 0.28241(11) 0.0250(3) Uani 1 1 d . . .
H3 H 0.1522 0.8374 0.2533 0.030 Uiso 1 1 calc R . .
C4 C 0.29639(17) 0.85909(11) 0.34991(11) 0.0255(3) Uani 1 1 d . . .
H4 H 0.2917 0.9205 0.3655 0.031 Uiso 1 1 calc R . .
C5 C 0.38577(16) 0.82031(11) 0.39416(10) 0.0224(3) Uani 1 1 d . . .
H5 H 0.4413 0.8544 0.4403 0.027 Uiso 1 1 calc R . .
C6 C 0.39259(15) 0.72989(10) 0.36945(9) 0.0188(3) Uani 1 1 d . . .
C7 C 0.47144(15) 0.66789(10) 0.39750(9) 0.0184(3) Uani 1 1 d . . .
C8 C 0.57144(15) 0.67651(10) 0.46342(9) 0.0188(3) Uani 1 1 d . . .
C9 C 0.63157(15) 0.60448(10) 0.47456(9) 0.0198(3) Uani 1 1 d . . .
H9 H 0.6981 0.6104 0.5193 0.024 Uiso 1 1 calc R . .
C10 C 0.59632(15) 0.52098(10) 0.42050(9) 0.0184(3) Uani 1 1 d . . .
C11 C 0.66593(15) 0.44915(10) 0.43368(10) 0.0197(3) Uani 1 1 d . . .
H11 H 0.7319 0.4580 0.4791 0.024 Uiso 1 1 calc R . .
C12 C 0.63973(15) 0.36785(10) 0.38236(10) 0.0183(3) Uani 1 1 d . . .
C13 C 0.54163(15) 0.35444(10) 0.31436(9) 0.0183(3) Uani 1 1 d . . .
C14 C 0.49632(15) 0.28028(10) 0.24755(9) 0.0193(3) Uani 1 1 d . . .
C15 C 0.52829(17) 0.19401(11) 0.22420(11) 0.0242(3) Uani 1 1 d . . .
H15 H 0.5926 0.1726 0.2572 0.029 Uiso 1 1 calc R . .
C16 C 0.46453(19) 0.14049(11) 0.15217(12) 0.0295(4) Uani 1 1 d . . .
H16 H 0.4854 0.0819 0.1360 0.035 Uiso 1 1 calc R . .
C17 C 0.36981(18) 0.17106(11) 0.10263(11) 0.0281(4) Uani 1 1 d . . .
H17 H 0.3289 0.1331 0.0530 0.034 Uiso 1 1 calc R . .
C18 C 0.33479(17) 0.25531(11) 0.12455(10) 0.0238(3) Uani 1 1 d . . .
H18 H 0.2701 0.2758 0.0911 0.029 Uiso 1 1 calc R . .
C19 C 0.39791(15) 0.30917(10) 0.19765(10) 0.0196(3) Uani 1 1 d . . .
C20 C 0.46997(14) 0.42395(10) 0.30241(9) 0.0171(3) Uani 1 1 d . . .
C21 C 0.49445(14) 0.50927(10) 0.35429(9) 0.0167(3) Uani 1 1 d . . .
C22 C 0.43258(14) 0.58525(10) 0.34552(9) 0.0171(3) Uani 1 1 d . . .
C31 C 0.69694(15) 0.76879(10) 0.58057(10) 0.0204(3) Uani 1 1 d . . .
H31A H 0.7829 0.7544 0.5594 0.025 Uiso 1 1 calc R . .
H31B H 0.6703 0.7282 0.6177 0.025 Uiso 1 1 calc R . .
C32 C 0.71009(16) 0.86270(10) 0.62887(10) 0.0217(3) Uani 1 1 d . . .
H32A H 0.6229 0.8778 0.6473 0.026 Uiso 1 1 calc R . .
H32B H 0.7405 0.9029 0.5922 0.026 Uiso 1 1 calc R . .
C33 C 0.80877(17) 0.87408(11) 0.70498(10) 0.0248(3) Uani 1 1 d . B .
H33A H 0.8944 0.8563 0.6860 0.030 Uiso 1 1 calc R . .
H33B H 0.7764 0.8346 0.7418 0.030 Uiso 1 1 calc R . .
C34 C 0.83089(19) 0.96848(11) 0.75563(11) 0.0293(4) Uani 1 1 d D . .
H34A H 0.8830 1.0051 0.7232 0.035 Uiso 1 1 calc R A 1
H34B H 0.7438 0.9911 0.7616 0.035 Uiso 1 1 calc R A 1
C35 C 0.9009(3) 0.98018(17) 0.84194(16) 0.0257(6) Uani 0.752(5) 1 d PD B 1
H35A H 0.8514 0.9420 0.8741 0.031 Uiso 0.752(5) 1 calc PR B 1
H35B H 0.9008 1.0419 0.8718 0.031 Uiso 0.752(5) 1 calc PR B 1
C36 C 1.0421(3) 0.95824(16) 0.83967(17) 0.0303(6) Uani 0.752(5) 1 d PD B 1
H36A H 1.0926 0.9983 0.8098 0.036 Uiso 0.752(5) 1 calc PR B 1
H36B H 1.0425 0.8975 0.8075 0.036 Uiso 0.752(5) 1 calc PR B 1
C37 C 1.1115(3) 0.96584(18) 0.92651(18) 0.0404(8) Uani 0.752(5) 1 d PD B 1
H37A H 1.1053 1.0253 0.9601 0.048 Uiso 0.752(5) 1 calc PR B 1
H37B H 1.0647 0.9227 0.9548 0.048 Uiso 0.752(5) 1 calc PR B 1
C38 C 1.2548(4) 0.9504(2) 0.9248(2) 0.0581(11) Uani 0.752(5) 1 d PD B 1
H38A H 1.2623 0.8934 0.8885 0.070 Uiso 0.752(5) 1 calc PR B 1
H38B H 1.2914 0.9506 0.9818 0.070 Uiso 0.752(5) 1 calc PR B 1
H38C H 1.3040 0.9971 0.9031 0.070 Uiso 0.752(5) 1 calc PR B 1
C35' C 0.9501(10) 0.9697(6) 0.8279(6) 0.030(2) Uiso 0.248(5) 1 d PD B 2
H35C H 0.9536 1.0256 0.8695 0.036 Uiso 0.248(5) 1 calc PR B 2
H35D H 0.9258 0.9215 0.8574 0.036 Uiso 0.248(5) 1 calc PR B 2
C36' C 1.0883(10) 0.9607(7) 0.8002(7) 0.051(3) Uiso 0.248(5) 1 d PD B 2
H36C H 1.1059 0.9991 0.7596 0.061 Uiso 0.248(5) 1 calc PR B 2
H36D H 1.0919 0.8993 0.7706 0.061 Uiso 0.248(5) 1 calc PR B 2
C37' C 1.1975(11) 0.9841(7) 0.8718(7) 0.061(3) Uiso 0.248(5) 1 d PD B 2
H37C H 1.2849 0.9873 0.8484 0.073 Uiso 0.248(5) 1 calc PR B 2
H37D H 1.1879 1.0425 0.9064 0.073 Uiso 0.248(5) 1 calc PR B 2
C38' C 1.1897(13) 0.9167(8) 0.9252(7) 0.057(3) Uiso 0.248(5) 1 d PD B 2
H38D H 1.0972 0.9018 0.9353 0.069 Uiso 0.248(5) 1 calc PR B 2
H38E H 1.2415 0.9402 0.9789 0.069 Uiso 0.248(5) 1 calc PR B 2
H38F H 1.2254 0.8638 0.8965 0.069 Uiso 0.248(5) 1 calc PR B 2
Cl1 Cl 0.21849(4) 0.48350(3) 0.11055(2) 0.02253(10) Uani 1 1 d . . .
N9 N 0.20494(13) 0.63553(9) 0.92582(8) 0.0195(3) Uani 1 1 d . . .
C41 C 0.79942(16) 0.30738(11) 0.46009(10) 0.0206(3) Uani 1 1 d . . .
H41A H 0.7576 0.3250 0.5132 0.025 Uiso 1 1 calc R . .
H41B H 0.8704 0.3542 0.4564 0.025 Uiso 1 1 calc R . .
C42 C 0.85692(16) 0.22162(11) 0.45870(10) 0.0222(3) Uani 1 1 d . . .
H42A H 0.8975 0.2040 0.4051 0.027 Uiso 1 1 calc R . .
H42B H 0.7854 0.1751 0.4623 0.027 Uiso 1 1 calc R . .
C43 C 0.96114(16) 0.23064(11) 0.53185(10) 0.0221(3) Uani 1 1 d . . .
H43A H 0.9207 0.2510 0.5849 0.027 Uiso 1 1 calc R . .
H43B H 1.0335 0.2761 0.5268 0.027 Uiso 1 1 calc R . .
C44 C 1.01972(16) 0.14515(11) 0.53608(10) 0.0230(3) Uani 1 1 d . . .
H44A H 0.9484 0.1008 0.5448 0.028 Uiso 1 1 calc R . .
H44B H 1.0552 0.1227 0.4817 0.028 Uiso 1 1 calc R . .
C45 C 1.12981(17) 0.15588(11) 0.60607(11) 0.0244(3) Uani 1 1 d . . .
H45A H 1.1995 0.2019 0.5986 0.029 Uiso 1 1 calc R . .
H45B H 1.0934 0.1762 0.6606 0.029 Uiso 1 1 calc R . .
C46 C 1.19200(18) 0.07172(11) 0.60861(11) 0.0276(4) Uani 1 1 d . . .
H46A H 1.2271 0.0510 0.5537 0.033 Uiso 1 1 calc R . .
H46B H 1.1224 0.0260 0.6168 0.033 Uiso 1 1 calc R . .
C47 C 1.30355(18) 0.08199(12) 0.67771(12) 0.0298(4) Uani 1 1 d . . .
H47A H 1.3706 0.1304 0.6720 0.036 Uiso 1 1 calc R . .
H47B H 1.2674 0.0984 0.7330 0.036 Uiso 1 1 calc R . .
C48 C 1.3700(2) -0.00150(14) 0.67487(14) 0.0454(6) Uani 1 1 d . . .
H48A H 1.3052 -0.0488 0.6838 0.054 Uiso 1 1 calc R . .
H48B H 1.4428 0.0091 0.7190 0.054 Uiso 1 1 calc R . .
H48C H 1.4050 -0.0185 0.6200 0.054 Uiso 1 1 calc R . .
C51 C 0.32015(15) 0.70113(11) 0.96881(10) 0.0209(3) Uani 1 1 d . . .
H51A H 0.2929 0.7610 0.9749 0.025 Uiso 1 1 calc R . .
H51B H 0.3942 0.6975 0.9321 0.025 Uiso 1 1 calc R . .
C52 C 0.37017(16) 0.68816(11) 1.05484(10) 0.0238(3) Uani 1 1 d . . .
H52A H 0.3968 0.6282 1.0498 0.029 Uiso 1 1 calc R . .
H52B H 0.2979 0.6939 1.0929 0.029 Uiso 1 1 calc R . .
C53 C 0.48821(17) 0.75560(12) 1.09235(11) 0.0286(4) Uani 1 1 d . . .
H53A H 0.5214 0.7424 1.1463 0.034 Uiso 1 1 calc R . .
H53B H 0.5600 0.7490 1.0540 0.034 Uiso 1 1 calc R . .
C54 C 0.4578(2) 0.85018(13) 1.10763(14) 0.0421(5) Uani 1 1 d . . .
H54A H 0.4369 0.8666 1.0538 0.051 Uiso 1 1 calc R . .
H54B H 0.5349 0.8886 1.1374 0.051 Uiso 1 1 calc R . .
H54C H 0.3818 0.8565 1.1416 0.051 Uiso 1 1 calc R . .
C61 C 0.08983(15) 0.63379(10) 0.98103(10) 0.0195(3) Uani 1 1 d . . .
H61A H 0.0158 0.5929 0.9487 0.023 Uiso 1 1 calc R . .
H61B H 0.1175 0.6090 1.0298 0.023 Uiso 1 1 calc R . .
C62 C 0.03777(16) 0.72079(11) 1.01378(11) 0.0245(3) Uani 1 1 d . . .
H62A H 0.0040 0.7455 0.9663 0.029 Uiso 1 1 calc R . .
H62B H 0.1098 0.7632 1.0464 0.029 Uiso 1 1 calc R . .
C63 C -0.07343(16) 0.70506(11) 1.06958(10) 0.0233(3) Uani 1 1 d . . .
H63A H -0.1452 0.6632 1.0359 0.028 Uiso 1 1 calc R . .
H63B H -0.0392 0.6778 1.1152 0.028 Uiso 1 1 calc R . .
C64 C -0.13022(18) 0.78886(12) 1.10800(12) 0.0312(4) Uani 1 1 d . . .
H64A H -0.0605 0.8298 1.1432 0.037 Uiso 1 1 calc R . .
H64B H -0.2018 0.7748 1.1424 0.037 Uiso 1 1 calc R . .
H64C H -0.1650 0.8160 1.0632 0.037 Uiso 1 1 calc R . .
C71 C 0.16492(16) 0.66369(11) 0.84453(10) 0.0232(3) Uani 1 1 d . . .
H71A H 0.1254 0.7196 0.8589 0.028 Uiso 1 1 calc R . .
H71B H 0.2460 0.6756 0.8162 0.028 Uiso 1 1 calc R . .
C72 C 0.06802(17) 0.59862(13) 0.78268(11) 0.0296(4) Uani 1 1 d . . .
H72A H -0.0047 0.5754 0.8127 0.036 Uiso 1 1 calc R . .
H72B H 0.1137 0.5486 0.7557 0.036 Uiso 1 1 calc R . .
C73 C 0.01158(19) 0.64406(15) 0.71584(12) 0.0364(5) Uani 1 1 d . . .
H73A H -0.0448 0.6882 0.7422 0.044 Uiso 1 1 calc R . .
H73B H 0.0853 0.6754 0.6927 0.044 Uiso 1 1 calc R . .
C74 C -0.0697(2) 0.57947(19) 0.64473(13) 0.0516(6) Uani 1 1 d . . .
H74A H -0.0150 0.5346 0.6195 0.062 Uiso 1 1 calc R . .
H74B H -0.1003 0.6109 0.6021 0.062 Uiso 1 1 calc R . .
H74C H -0.1463 0.5512 0.6667 0.062 Uiso 1 1 calc R . .
C81 C 0.24214(15) 0.54195(10) 0.90892(10) 0.0203(3) Uani 1 1 d . . .
H81A H 0.2596 0.5248 0.9635 0.024 Uiso 1 1 calc R . .
H81B H 0.1651 0.5024 0.8787 0.024 Uiso 1 1 calc R . .
C82 C 0.36131(16) 0.52678(11) 0.85853(11) 0.0244(3) Uani 1 1 d . . .
H82A H 0.4426 0.5571 0.8923 0.029 Uiso 1 1 calc R . .
H82B H 0.3517 0.5514 0.8073 0.029 Uiso 1 1 calc R . .
C83 C 0.37285(18) 0.42816(12) 0.83419(11) 0.0288(4) Uani 1 1 d . . .
H83A H 0.4633 0.4199 0.8175 0.035 Uiso 1 1 calc R . .
H83B H 0.3606 0.4019 0.8841 0.035 Uiso 1 1 calc R . .
C84 C 0.2735(2) 0.37880(13) 0.76293(12) 0.0353(4) Uani 1 1 d . . .
H84A H 0.1836 0.3823 0.7805 0.042 Uiso 1 1 calc R . .
H84B H 0.2902 0.3171 0.7488 0.042 Uiso 1 1 calc R . .
H84C H 0.2830 0.4053 0.7136 0.042 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0189(6) 0.0205(6) 0.0153(6) 0.0023(5) -0.0025(5) 0.0054(5)
N2 0.0187(6) 0.0198(6) 0.0167(6) 0.0031(5) -0.0023(5) 0.0031(5)
O1 0.0253(6) 0.0198(5) 0.0192(5) 0.0006(4) -0.0064(4) 0.0050(4)
O2 0.0240(6) 0.0200(5) 0.0216(6) 0.0052(4) -0.0040(4) 0.0069(4)
C1 0.0183(7) 0.0231(8) 0.0162(7) 0.0054(6) 0.0027(6) 0.0045(6)
C2 0.0214(7) 0.0271(8) 0.0177(7) 0.0059(6) -0.0004(6) 0.0068(6)
C3 0.0262(8) 0.0276(8) 0.0245(8) 0.0097(7) 0.0000(6) 0.0112(7)
C4 0.0296(9) 0.0208(8) 0.0277(9) 0.0059(7) 0.0024(7) 0.0084(7)
C5 0.0252(8) 0.0211(8) 0.0212(8) 0.0041(6) 0.0009(6) 0.0049(6)
C6 0.0176(7) 0.0235(8) 0.0164(7) 0.0055(6) 0.0016(6) 0.0040(6)
C7 0.0186(7) 0.0203(7) 0.0169(7) 0.0043(6) 0.0020(6) 0.0040(6)
C8 0.0198(7) 0.0208(7) 0.0148(7) 0.0017(6) 0.0002(6) 0.0020(6)
C9 0.0192(7) 0.0234(8) 0.0157(7) 0.0028(6) -0.0038(6) 0.0033(6)
C10 0.0182(7) 0.0219(7) 0.0155(7) 0.0047(6) 0.0005(6) 0.0029(6)
C11 0.0189(7) 0.0234(8) 0.0177(7) 0.0064(6) -0.0018(6) 0.0050(6)
C12 0.0187(7) 0.0190(7) 0.0189(7) 0.0066(6) 0.0021(6) 0.0052(6)
C13 0.0196(7) 0.0183(7) 0.0174(7) 0.0048(6) 0.0022(6) 0.0026(6)
C14 0.0211(7) 0.0200(7) 0.0168(7) 0.0049(6) 0.0014(6) 0.0006(6)
C15 0.0281(8) 0.0207(8) 0.0248(8) 0.0071(6) 0.0005(7) 0.0043(6)
C16 0.0376(10) 0.0188(8) 0.0305(9) 0.0021(7) 0.0003(7) 0.0029(7)
C17 0.0369(10) 0.0225(8) 0.0215(8) 0.0003(6) -0.0034(7) -0.0019(7)
C18 0.0258(8) 0.0238(8) 0.0205(8) 0.0046(6) -0.0031(6) -0.0009(6)
C19 0.0204(7) 0.0193(7) 0.0196(7) 0.0059(6) 0.0019(6) 0.0008(6)
C20 0.0161(7) 0.0220(7) 0.0145(7) 0.0064(6) 0.0017(5) 0.0032(6)
C21 0.0161(7) 0.0198(7) 0.0146(7) 0.0041(6) 0.0011(5) 0.0034(5)
C22 0.0175(7) 0.0214(7) 0.0128(7) 0.0039(6) 0.0007(5) 0.0031(6)
C31 0.0206(7) 0.0224(8) 0.0171(7) 0.0022(6) -0.0036(6) 0.0033(6)
C32 0.0242(8) 0.0206(8) 0.0197(8) 0.0029(6) -0.0022(6) 0.0045(6)
C33 0.0306(9) 0.0206(8) 0.0213(8) 0.0037(6) -0.0060(7) 0.0004(6)
C34 0.0364(10) 0.0230(8) 0.0250(9) 0.0010(7) -0.0060(7) -0.0009(7)
C35 0.0264(14) 0.0247(12) 0.0222(12) -0.0004(9) -0.0040(10) -0.0011(10)
C36 0.0310(14) 0.0265(12) 0.0307(14) 0.0015(10) -0.0046(11) 0.0035(10)
C37 0.0440(16) 0.0286(13) 0.0445(16) 0.0077(11) -0.0210(12) -0.0020(11)
C38 0.049(2) 0.0395(17) 0.080(3) 0.0098(16) -0.0348(18) 0.0032(15)
Cl1 0.02507(19) 0.02273(19) 0.01846(18) 0.00613(14) -0.00796(14) -0.00193(14)
N9 0.0180(6) 0.0254(7) 0.0154(6) 0.0058(5) 0.0000(5) 0.0016(5)
C41 0.0214(7) 0.0242(8) 0.0172(7) 0.0061(6) -0.0019(6) 0.0061(6)
C42 0.0250(8) 0.0227(8) 0.0210(8) 0.0065(6) 0.0002(6) 0.0093(6)
C43 0.0229(8) 0.0230(8) 0.0219(8) 0.0059(6) -0.0004(6) 0.0083(6)
C44 0.0250(8) 0.0231(8) 0.0218(8) 0.0055(6) -0.0031(6) 0.0078(6)
C45 0.0256(8) 0.0235(8) 0.0240(8) 0.0050(6) -0.0043(6) 0.0064(6)
C46 0.0301(9) 0.0258(8) 0.0269(9) 0.0044(7) -0.0072(7) 0.0104(7)
C47 0.0310(9) 0.0280(9) 0.0293(9) 0.0027(7) -0.0083(7) 0.0110(7)
C48 0.0512(13) 0.0372(11) 0.0441(12) -0.0012(9) -0.0220(10) 0.0224(10)
C51 0.0177(7) 0.0232(8) 0.0213(8) 0.0058(6) 0.0001(6) -0.0014(6)
C52 0.0235(8) 0.0260(8) 0.0207(8) 0.0055(6) -0.0038(6) -0.0018(6)
C53 0.0265(9) 0.0322(9) 0.0247(9) 0.0053(7) -0.0055(7) -0.0035(7)
C54 0.0531(13) 0.0298(10) 0.0371(11) 0.0010(8) -0.0103(9) -0.0066(9)
C61 0.0149(7) 0.0261(8) 0.0177(7) 0.0061(6) 0.0012(5) 0.0008(6)
C62 0.0218(8) 0.0264(8) 0.0260(8) 0.0070(7) 0.0026(6) 0.0031(6)
C63 0.0185(7) 0.0273(8) 0.0228(8) 0.0031(6) 0.0009(6) 0.0013(6)
C64 0.0241(8) 0.0329(9) 0.0336(10) -0.0010(8) 0.0032(7) 0.0038(7)
C71 0.0232(8) 0.0316(9) 0.0175(7) 0.0115(6) 0.0008(6) 0.0040(7)
C72 0.0240(8) 0.0456(11) 0.0198(8) 0.0119(7) -0.0016(6) -0.0019(7)
C73 0.0261(9) 0.0617(13) 0.0253(9) 0.0186(9) -0.0040(7) 0.0076(9)
C74 0.0301(10) 0.0946(19) 0.0296(11) 0.0243(12) -0.0095(8) -0.0120(11)
C81 0.0193(7) 0.0224(8) 0.0187(7) 0.0042(6) 0.0008(6) 0.0001(6)
C82 0.0204(8) 0.0293(9) 0.0235(8) 0.0055(7) 0.0047(6) 0.0018(6)
C83 0.0306(9) 0.0312(9) 0.0267(9) 0.0070(7) 0.0093(7) 0.0073(7)
C84 0.0400(11) 0.0330(10) 0.0302(10) 0.0005(8) 0.0100(8) -0.0009(8)

_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
N1 C1 1.377(2) . ?
N1 C22 1.3832(19) . ?
N2 C19 1.374(2) . ?
N2 C20 1.3834(19) . ?
O1 C8 1.3656(19) . ?
O1 C31 1.4323(18) . ?
O2 C12 1.3698(18) . ?
O2 C41 1.4366(18) . ?
C1 C2 1.398(2) . ?
C1 C6 1.412(2) . ?
C2 C3 1.381(2) . ?
C3 C4 1.403(2) . ?
C4 C5 1.386(2) . ?
C5 C6 1.400(2) . ?
C6 C7 1.441(2) . ?
C7 C22 1.403(2) . ?
C7 C8 1.414(2) . ?
C8 C9 1.370(2) . ?
C9 C10 1.423(2) . ?
C10 C21 1.424(2) . ?
C10 C11 1.429(2) . ?
C11 C12 1.368(2) . ?
C12 C13 1.417(2) . ?
C13 C20 1.404(2) . ?
C13 C14 1.442(2) . ?
C14 C15 1.402(2) . ?
C14 C19 1.417(2) . ?
C15 C16 1.384(2) . ?
C16 C17 1.401(3) . ?
C17 C18 1.381(2) . ?
C18 C19 1.396(2) . ?
C20 C21 1.421(2) . ?
C21 C22 1.425(2) . ?
C31 C32 1.511(2) . ?
C32 C33 1.521(2) . ?
C33 C34 1.529(2) . ?
C34 C35 1.509(3) . ?
C34 C35' 1.638(9) . ?
C35 C36 1.513(4) . ?
C36 C37 1.522(3) . ?
C37 C38 1.504(5) . ?
C35' C36' 1.515(12) . ?
C36' C37' 1.527(12) . ?
C37' C38' 1.493(12) . ?
N9 C51 1.517(2) . ?
N9 C61 1.5215(19) . ?
N9 C81 1.523(2) . ?
N9 C71 1.5226(19) . ?
C41 C42 1.511(2) . ?
C42 C43 1.525(2) . ?
C43 C44 1.527(2) . ?
C44 C45 1.525(2) . ?
C45 C46 1.521(2) . ?
C46 C47 1.526(2) . ?
C47 C48 1.522(2) . ?
C51 C52 1.522(2) . ?
C52 C53 1.530(2) . ?
C53 C54 1.515(3) . ?
C61 C62 1.517(2) . ?
C62 C63 1.526(2) . ?
C63 C64 1.519(2) . ?
C71 C72 1.518(2) . ?
C72 C73 1.528(2) . ?
C73 C74 1.520(3) . ?
C81 C82 1.518(2) . ?
C82 C83 1.531(2) . ?
C83 C84 1.524(3) . ?

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
C1 N1 C22 109.08(13) . . ?
C19 N2 C20 109.28(13) . . ?
C8 O1 C31 115.89(12) . . ?
C12 O2 C41 116.17(12) . . ?
N1 C1 C2 128.71(15) . . ?
N1 C1 C6 109.33(13) . . ?
C2 C1 C6 121.96(15) . . ?
C3 C2 C1 117.38(15) . . ?
C2 C3 C4 121.50(15) . . ?
C5 C4 C3 121.08(15) . . ?
C4 C5 C6 118.65(15) . . ?
C5 C6 C1 119.42(14) . . ?
C5 C6 C7 134.94(15) . . ?
C1 C6 C7 105.64(13) . . ?
C22 C7 C8 119.65(14) . . ?
C22 C7 C6 107.67(13) . . ?
C8 C7 C6 132.67(14) . . ?
O1 C8 C9 125.49(14) . . ?
O1 C8 C7 114.92(13) . . ?
C9 C8 C7 119.59(14) . . ?
C8 C9 C10 121.31(14) . . ?
C9 C10 C21 120.78(14) . . ?
C9 C10 C11 118.57(14) . . ?
C21 C10 C11 120.65(14) . . ?
C12 C11 C10 121.51(14) . . ?
C11 C12 O2 125.28(14) . . ?
C11 C12 C13 119.37(14) . . ?
O2 C12 C13 115.34(13) . . ?
C20 C13 C12 119.50(14) . . ?
C20 C13 C14 107.40(13) . . ?
C12 C13 C14 133.08(14) . . ?
C15 C14 C19 118.94(14) . . ?
C15 C14 C13 135.23(15) . . ?
C19 C14 C13 105.83(13) . . ?
C16 C15 C14 118.83(15) . . ?
C15 C16 C17 121.30(16) . . ?
C18 C17 C16 121.28(16) . . ?
C17 C18 C19 117.58(15) . . ?
N2 C19 C18 128.88(15) . . ?
N2 C19 C14 109.05(13) . . ?
C18 C19 C14 122.06(15) . . ?
N2 C20 C13 108.39(13) . . ?
N2 C20 C21 128.85(14) . . ?
C13 C20 C21 122.71(14) . . ?
C20 C21 C10 116.20(13) . . ?
C20 C21 C22 127.41(13) . . ?
C10 C21 C22 116.33(14) . . ?
N1 C22 C7 108.25(13) . . ?
N1 C22 C21 129.46(14) . . ?
C7 C22 C21 122.28(13) . . ?
O1 C31 C32 108.60(12) . . ?
C31 C32 C33 109.91(13) . . ?
C32 C33 C34 113.00(14) . . ?
C35 C34 C33 115.47(16) . . ?
C35 C34 C35' 21.0(3) . . ?
C33 C34 C35' 105.7(4) . . ?
C34 C35 C36 112.9(2) . . ?
C35 C36 C37 113.2(2) . . ?
C38 C37 C36 113.4(3) . . ?
C36' C35' C34 117.8(7) . . ?
C35' C36' C37' 114.2(9) . . ?
C38' C37' C36' 110.3(9) . . ?
C51 N9 C61 111.44(12) . . ?
C51 N9 C81 111.70(12) . . ?
C61 N9 C81 105.05(11) . . ?
C51 N9 C71 106.37(12) . . ?
C61 N9 C71 111.08(12) . . ?
C81 N9 C71 111.31(12) . . ?
O2 C41 C42 108.69(13) . . ?
C41 C42 C43 110.69(13) . . ?
C42 C43 C44 113.40(14) . . ?
C45 C44 C43 113.14(14) . . ?
C46 C45 C44 113.40(14) . . ?
C45 C46 C47 113.86(14) . . ?
C48 C47 C46 112.62(15) . . ?
N9 C51 C52 114.90(13) . . ?
C51 C52 C53 111.24(14) . . ?
C54 C53 C52 114.37(16) . . ?
C62 C61 N9 117.01(13) . . ?
C61 C62 C63 108.59(13) . . ?
C64 C63 C62 112.97(14) . . ?
C72 C71 N9 116.03(14) . . ?
C71 C72 C73 109.70(16) . . ?
C74 C73 C72 112.23(19) . . ?
C82 C81 N9 115.77(13) . . ?
C81 C82 C83 109.79(13) . . ?
C84 C83 C82 114.20(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H01 Cl1 0.87(2) 2.30(2) 3.1547(14) 166.2(19) .
N2 H02 Cl1 0.88(2) 2.27(2) 3.1297(14) 167.7(19) .

_diffrn_measured_fraction_theta_max 0.910
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.077