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#$Date: 2016-03-21 19:10:27 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178838 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/92/4109275.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4109275
loop_
_publ_author_name
'Guzmán Gil-Ramírez'
'Jordi Benet-Buchholz'
'Eduardo C. Escudero-Adán'
'Pablo Ballester'
_publ_contact_author
;
    Dr. Benet-Buchholz, Jordi
    The Institute of Chemical Research of Catalonia (ICIQ)    
    X-ray Diffraction Unit
    Avgda. Paīsos Catalans 16
    E-43007 Tarragona, Spain
;
_publ_contact_author_email       jbenet@iciq.es
_publ_contact_author_fax         '+34 977 920 224'
_publ_contact_author_phone       '+34 977 920 204'
_publ_section_title
;
 Solid-State Self-Assembly of a Calix[4]pyrrole-Resorcinarene Hybrid into
 a Hexameric Cage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3820
_journal_page_last               3821
_journal_paper_doi               10.1021/ja070037k
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C61.33 H87 Cl3.33 N7.33 O9.83'
_chemical_formula_weight         1202.55
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   21.8372(18)
_cell_length_b                   21.8372(18)
_cell_length_c                   69.813(11)
_cell_measurement_reflns_used    7208
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.51
_cell_measurement_theta_min      3.08
_cell_volume                     28831(6)
_computing_cell_refinement       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_collection       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_reduction        'SAINT+ Version 7.06A Bruker-Nonius, 2004'
_computing_molecular_graphics    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_publication_material  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_refinement  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_solution    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       84
_diffrn_reflns_limit_l_min       -84
_diffrn_reflns_number            85788
_diffrn_reflns_theta_full        25.42
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           90
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.897811
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2.1 2003 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       Plate
_exptl_crystal_F_000             11550
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         11811
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1459P)²+62.4492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2098
_refine_ls_wR_factor_ref         0.2524
_reflns_number_gt                8231
_reflns_number_total             11811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070037ksi20070103_112425_3.cif
_cod_data_source_block           ggdha4_0m
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4109275
loop_
_symmetry_equiv_pos_as_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'
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 0.48294(13) 1.00204(13) 0.07090(4) 0.0415(6) Uani 1 1 d . . .
H1B H 0.4429 1.0016 0.0728 0.050 Uiso 1 1 calc R . .
O1 O 0.38811(15) 1.21588(15) 0.05293(4) 0.0685(7) Uani 1 1 d . . .
H1A H 0.3893 1.2217 0.0649 0.103 Uiso 1 1 d R . .
C1 C 0.48930(16) 0.94283(16) 0.06918(5) 0.0419(7) Uani 1 1 d . . .
N2 N 0.49598(13) 1.12351(13) 0.10197(4) 0.0444(6) Uani 1 1 d . . .
H2C H 0.4558 1.0862 0.0986 0.053 Uiso 1 1 calc R . .
C2 C 0.55955(18) 0.96612(19) 0.06650(5) 0.0538(8) Uani 1 1 d . . .
H2A H 0.5803 0.9372 0.0649 0.065 Uiso 1 1 calc R . .
O2 O 0.4615(3) 1.1158(3) 0.00541(4) 0.1127(13) Uani 1 1 d . . .
H2B H 0.4753 1.0863 0.0042 0.169 Uiso 1 1 calc R . .
N3 N 0.38742(14) 0.99987(14) 0.13208(4) 0.0455(6) Uani 1 1 d . . .
H3C H 0.3720 0.9994 0.1204 0.055 Uiso 1 1 calc R . .
O3 O 0.20185(17) 1.06994(16) 0.13843(6) 0.0855(10) Uani 1 1 d . . .
H3B H 0.1852 1.0264 0.1367 0.128 Uiso 1 1 calc R . .
C3 C 0.59592(17) 1.04070(19) 0.06649(6) 0.0543(9) Uani 1 1 d . . .
H3A H 0.6454 1.0707 0.0649 0.065 Uiso 1 1 calc R . .
N4 N 0.37742(13) 0.87849(13) 0.10205(4) 0.0428(6) Uani 1 1 d . . .
H4B H 0.3729 0.9149 0.0987 0.051 Uiso 1 1 calc R . .
O4 O 0.35067(15) 1.22915(15) 0.08985(4) 0.0676(7) Uani 1 1 d . . .
H4A H 0.3120 1.2241 0.0860 0.101 Uiso 1 1 calc R . .
C4 C 0.54800(16) 1.06204(16) 0.06917(5) 0.0429(7) Uani 1 1 d . . .
O5 O 0.12154(14) 0.76166(16) 0.09163(4) 0.0717(8) Uani 1 1 d . . .
H5A H 0.0927 0.7866 0.0906 0.107 Uiso 1 1 d R . .
C5 C 0.55852(16) 1.13647(17) 0.07014(5) 0.0458(7) Uani 1 1 d . . .
O6 O 0.13464(15) 0.92418(16) 0.13978(5) 0.0722(8) Uani 1 1 d . . .
H6A H 0.1058 0.9279 0.1326 0.108 Uiso 1 1 calc R . .
C6 C 0.50655(17) 1.14273(16) 0.05640(5) 0.0458(7) Uani 1 1 d . . .
C7 C 0.46865(17) 1.17527(17) 0.06156(5) 0.0479(8) Uani 1 1 d . . .
H7A H 0.4704 1.1905 0.0744 0.058 Uiso 1 1 calc R . .
O7 O 0.34548(19) 0.8866(3) 0.00600(5) 0.1162(15) Uani 1 1 d . . .
H7B H 0.3889 0.9149 0.0045 0.174 Uiso 1 1 calc R . .
O8 O 0.17538(13) 0.78477(15) 0.05421(4) 0.0653(7) Uani 1 1 d . . .
H8A H 0.1718 0.7860 0.0662 0.098 Uiso 1 1 calc R . .
C8 C 0.4282(2) 1.18590(18) 0.04820(5) 0.0546(8) Uani 1 1 d . . .
C9 C 0.4266(2) 1.1667(2) 0.02960(6) 0.0694(11) Uani 1 1 d . . .
H9A H 0.4003 1.1760 0.0204 0.083 Uiso 1 1 calc R . .
C10 C 0.4639(3) 1.1334(3) 0.02433(6) 0.0717(11) Uani 1 1 d . . .
C11 C 0.5028(2) 1.1204(2) 0.03750(5) 0.0618(9) Uani 1 1 d . . .
H11A H 0.5269 1.0963 0.0337 0.074 Uiso 1 1 calc R . .
C12 C 0.63354(19) 1.1880(2) 0.06265(6) 0.0614(10) Uani 1 1 d . . .
H12A H 0.6686 1.1869 0.0712 0.092 Uiso 1 1 calc R . .
H12B H 0.6407 1.2360 0.0623 0.092 Uiso 1 1 calc R . .
H12C H 0.6390 1.1737 0.0497 0.092 Uiso 1 1 calc R . .
C13 C 0.55487(16) 1.15790(16) 0.09033(5) 0.0451(7) Uani 1 1 d . . .
C14 C 0.60534(19) 1.21214(19) 0.10112(6) 0.0583(9) Uani 1 1 d . . .
H14A H 0.6519 1.2452 0.0970 0.070 Uiso 1 1 calc R . .
C15 C 0.5769(2) 1.2107(2) 0.11921(6) 0.0616(10) Uani 1 1 d . . .
H15A H 0.6007 1.2424 0.1295 0.074 Uiso 1 1 calc R . .
C16 C 0.50877(17) 1.15546(17) 0.11953(5) 0.0475(8) Uani 1 1 d . . .
C17 C 0.45232(18) 1.13303(18) 0.13490(5) 0.0507(8) Uani 1 1 d . . .
C18 C 0.38809(18) 1.13742(18) 0.12724(5) 0.0501(8) Uani 1 1 d . . .
C19 C 0.3229(2) 1.1004(2) 0.13600(6) 0.0608(9) Uani 1 1 d . . .
H19A H 0.3168 1.0703 0.1465 0.073 Uiso 1 1 calc R . .
C20 C 0.2670(2) 1.1068(2) 0.12966(6) 0.0603(9) Uani 1 1 d . . .
C21 C 0.2744(2) 1.1499(2) 0.11426(6) 0.0596(9) Uani 1 1 d . . .
H21A H 0.2355 1.1541 0.1099 0.071 Uiso 1 1 calc R . .
C22 C 0.33900(19) 1.18649(18) 0.10541(5) 0.0524(8) Uani 1 1 d . . .
C23 C 0.39629(19) 1.18166(18) 0.11203(5) 0.0524(8) Uani 1 1 d . . .
H23A H 0.4412 1.2087 0.1061 0.063 Uiso 1 1 calc R . .
C24 C 0.4829(2) 1.1864(2) 0.15166(6) 0.0696(11) Uani 1 1 d . . .
H24A H 0.5242 1.1861 0.1570 0.104 Uiso 1 1 calc R . .
H24B H 0.4468 1.1729 0.1617 0.104 Uiso 1 1 calc R . .
H24C H 0.4968 1.2339 0.1470 0.104 Uiso 1 1 calc R . .
C25 C 0.42960(17) 1.05992(18) 0.14242(5) 0.0475(7) Uani 1 1 d . . .
C26 C 0.44294(19) 1.0385(2) 0.15944(5) 0.0558(9) Uani 1 1 d . . .
H26A H 0.4712 1.0685 0.1695 0.067 Uiso 1 1 calc R . .
C27 C 0.40766(19) 0.9644(2) 0.15945(5) 0.0553(9) Uani 1 1 d . . .
H27A H 0.4080 0.9354 0.1696 0.066 Uiso 1 1 calc R . .
C28 C 0.37268(17) 0.94088(18) 0.14245(5) 0.0457(7) Uani 1 1 d . . .
C29 C 0.32427(17) 0.86695(18) 0.13495(5) 0.0471(8) Uani 1 1 d . . .
C30 C 0.25404(17) 0.85928(18) 0.12760(5) 0.0470(8) Uani 1 1 d . . .
C31 C 0.21737(18) 0.81304(18) 0.11303(5) 0.0517(8) Uani 1 1 d . . .
H31A H 0.2355 0.7861 0.1072 0.062 Uiso 1 1 calc R . .
C32 C 0.15335(17) 0.80594(19) 0.10692(5) 0.0533(8) Uani 1 1 d . . .
C33 C 0.12442(18) 0.84140(19) 0.11573(5) 0.0548(9) Uani 1 1 d . . .
H33A H 0.0798 0.8346 0.1118 0.066 Uiso 1 1 calc R . .
C34 C 0.16147(18) 0.88734(19) 0.13044(5) 0.0526(8) Uani 1 1 d . . .
C35 C 0.22592(17) 0.89659(19) 0.13630(5) 0.0505(8) Uani 1 1 d . . .
H35A H 0.2511 0.9288 0.1464 0.061 Uiso 1 1 calc R . .
C36 C 0.3047(2) 0.8137(2) 0.15166(5) 0.0621(10) Uani 1 1 d . . .
H36A H 0.3478 0.8168 0.1569 0.093 Uiso 1 1 calc R . .
H36B H 0.2733 0.7656 0.1469 0.093 Uiso 1 1 calc R . .
H36C H 0.2806 0.8249 0.1617 0.093 Uiso 1 1 calc R . .
C37 C 0.35951(16) 0.84630(17) 0.11950(5) 0.0463(7) Uani 1 1 d . . .
C38 C 0.3753(2) 0.7932(2) 0.11908(6) 0.0607(10) Uani 1 1 d . . .
H38A H 0.3687 0.7618 0.1293 0.073 Uiso 1 1 calc R . .
C39 C 0.4029(2) 0.79293(19) 0.10106(6) 0.0594(9) Uani 1 1 d . . .
H39A H 0.4184 0.7615 0.0969 0.071 Uiso 1 1 calc R . .
C40 C 0.40362(16) 0.84606(16) 0.09042(5) 0.0448(7) Uani 1 1 d . . .
C41 C 0.42706(17) 0.86798(17) 0.07010(5) 0.0451(7) Uani 1 1 d . . .
C42 C 0.36745(17) 0.86013(16) 0.05672(5) 0.0465(7) Uani 1 1 d . . .
C43 C 0.3846(2) 0.8831(2) 0.03790(5) 0.0632(10) Uani 1 1 d . . .
H43A H 0.4327 0.9083 0.0340 0.076 Uiso 1 1 calc R . .
C44 C 0.3317(2) 0.8692(3) 0.02497(6) 0.0725(12) Uani 1 1 d . . .
C45 C 0.2616(2) 0.8352(2) 0.03061(6) 0.0693(11) Uani 1 1 d . . .
H45A H 0.2253 0.8255 0.0216 0.083 Uiso 1 1 calc R . .
C46 C 0.24531(18) 0.81564(18) 0.04925(5) 0.0525(8) Uani 1 1 d . . .
C47 C 0.29704(17) 0.82661(16) 0.06224(5) 0.0475(8) Uani 1 1 d . . .
H47A H 0.2845 0.8111 0.0751 0.057 Uiso 1 1 calc R . .
C48 C 0.4516(2) 0.8174(2) 0.06226(6) 0.0607(9) Uani 1 1 d . . .
H48A H 0.4888 0.8195 0.0705 0.091 Uiso 1 1 calc R . .
H48B H 0.4700 0.8318 0.0492 0.091 Uiso 1 1 calc R . .
H48C H 0.4114 0.7690 0.0620 0.091 Uiso 1 1 calc R . .
Cl1 Cl 0.34181(4) 0.99921(4) 0.088067(12) 0.0470(2) Uani 1 1 d . . .
Cl3 Cl 0.0000 1.0000 0.09965(4) 0.1042(7) Uani 1 3 d S . .
Cl4 Cl 0.00437(6) 0.77951(7) 0.075008(17) 0.0822(4) Uani 1 1 d . . .
Cl2 Cl 0.5000 1.0000 0.0000 0.0785(4) Uani 1 2 d S . .
N1A N 0.17213(18) 0.99607(18) 0.06639(5) 0.0685(9) Uani 1 1 d . . .
C1A C 0.1813(3) 0.9380(3) 0.05901(10) 0.1072(19) Uani 1 1 d . . .
H1AA H 0.2269 0.9446 0.0633 0.161 Uiso 1 1 calc R . .
H1AB H 0.1799 0.9380 0.0450 0.161 Uiso 1 1 calc R . .
H1AC H 0.1430 0.8928 0.0638 0.161 Uiso 1 1 calc R . .
C2A C 0.2366(4) 1.0628(3) 0.06106(10) 0.113(2) Uani 1 1 d . . .
H2AA H 0.2778 1.0650 0.0673 0.170 Uiso 1 1 calc R . .
H2AB H 0.2318 1.1031 0.0652 0.170 Uiso 1 1 calc R . .
H2AC H 0.2428 1.0646 0.0471 0.170 Uiso 1 1 calc R . .
C3A C 0.1071(4) 0.9918(5) 0.05852(11) 0.140(3) Uani 1 1 d . . .
H3AA H 0.1129 1.0014 0.0447 0.210 Uiso 1 1 calc R . .
H3AB H 0.0985 1.0268 0.0649 0.210 Uiso 1 1 calc R . .
H3AC H 0.0668 0.9443 0.0607 0.210 Uiso 1 1 calc R . .
C4A C 0.1677(3) 0.9902(4) 0.08746(8) 0.1098(19) Uani 1 1 d . . .
H4AA H 0.2087 0.9882 0.0924 0.165 Uiso 1 1 calc R . .
H4AB H 0.1242 0.9470 0.0911 0.165 Uiso 1 1 calc R . .
H4AC H 0.1673 1.0314 0.0929 0.165 Uiso 1 1 calc R . .
N1B N 0.6038(2) 1.0138(2) 0.12830(5) 0.0754(10) Uani 1 1 d . . .
C1B C 0.6011(11) 1.0635(10) 0.11646(16) 0.370(8) Uani 1 1 d . . .
H1BA H 0.6249 1.1098 0.1227 0.555 Uiso 1 1 calc R . .
H1BB H 0.5517 1.0495 0.1139 0.555 Uiso 1 1 calc R . .
H1BC H 0.6250 1.0661 0.1043 0.555 Uiso 1 1 calc R . .
C2B C 0.5410(6) 0.9523(12) 0.1256(3) 0.433(19) Uani 1 1 d . . .
H2BA H 0.5503 0.9158 0.1206 0.649 Uiso 1 1 calc R . .
H2BB H 0.5119 0.9605 0.1164 0.649 Uiso 1 1 calc R . .
H2BC H 0.5158 0.9366 0.1378 0.649 Uiso 1 1 calc R . .
C3B C 0.6591(5) 1.0046(5) 0.1213(2) 0.201(5) Uani 1 1 d . . .
H3BA H 0.6933 1.0140 0.1315 0.302 Uiso 1 1 calc R . .
H3BB H 0.6826 1.0376 0.1106 0.302 Uiso 1 1 calc R . .
H3BC H 0.6398 0.9560 0.1167 0.302 Uiso 1 1 calc R . .
C4B C 0.6070(7) 1.0319(7) 0.14770(10) 0.202(5) Uani 1 1 d . . .
H4BA H 0.5734 0.9903 0.1550 0.302 Uiso 1 1 calc R . .
H4BB H 0.5949 1.0693 0.1491 0.302 Uiso 1 1 calc R . .
H4BC H 0.6549 1.0489 0.1526 0.302 Uiso 1 1 calc R . .
N1C N 0.2720(3) 1.0007(2) -0.01732(5) 0.0902(12) Uani 1 1 d . . .
C1C C 0.2743(9) 1.0637(5) -0.02254(14) 0.265(8) Uani 1 1 d . . .
H1CA H 0.2375 1.0679 -0.0156 0.398 Uiso 1 1 calc R . .
H1CB H 0.2662 1.0635 -0.0364 0.398 Uiso 1 1 calc R . .
H1CC H 0.3208 1.1040 -0.0193 0.398 Uiso 1 1 calc R . .
C2C C 0.2090(6) 0.9396(4) -0.02297(14) 0.214(6) Uani 1 1 d . . .
H2CA H 0.1701 0.9499 -0.0231 0.320 Uiso 1 1 calc R . .
H2CB H 0.1980 0.9012 -0.0139 0.320 Uiso 1 1 calc R . .
H2CC H 0.2150 0.9253 -0.0358 0.320 Uiso 1 1 calc R . .
C3C C 0.3266(5) 0.9943(7) -0.02790(12) 0.203(6) Uani 1 1 d . . .
H3CA H 0.3132 0.9850 -0.0414 0.305 Uiso 1 1 calc R . .
H3CB H 0.3311 0.9553 -0.0226 0.305 Uiso 1 1 calc R . .
H3CC H 0.3719 1.0385 -0.0267 0.305 Uiso 1 1 calc R . .
C4C C 0.2798(6) 0.9990(6) 0.00394(9) 0.188(4) Uani 1 1 d . . .
H4CA H 0.2412 1.0018 0.0103 0.281 Uiso 1 1 calc R . .
H4CB H 0.3252 1.0393 0.0079 0.281 Uiso 1 1 calc R . .
H4CC H 0.2781 0.9549 0.0076 0.281 Uiso 1 1 calc R . .
N1D N 0.3333 0.6667 0.00061(12) 0.101(2) Uani 1 3 d SD . .
C1D C 0.3333 0.6667 -0.02030(19) 0.65(6) Uani 1 3 d SD . .
H1DA H 0.3413 0.6296 -0.0249 0.968 Uiso 1 1 d R . .
C2D C 0.2955(15) 0.6973(17) 0.0094(4) 0.57(2) Uani 1 1 d D . .
H2DA H 0.3162 0.7209 0.0216 0.858 Uiso 1 1 d R . .
H2DB H 0.2447 0.6649 0.0111 0.858 Uiso 1 1 d R . .
H2DC H 0.3028 0.7328 -0.0003 0.858 Uiso 1 1 d R . .
O2W O 0.0058(3) 0.8985(2) 0.12893(9) 0.1273(15) Uani 1 1 d D . .
H2WY H -0.0425(18) 0.871(4) 0.1335(12) 0.191 Uiso 1 1 d D . .
H2WX H -0.001(4) 0.924(4) 0.1188(9) 0.191 Uiso 1 1 d D . .
O3W O 0.0000 1.0000 0.0277(4) 0.281(18) Uani 0.50 3 d SP . .
O4W O 0.6667 1.3333 0.1681(8) 0.45(4) Uani 0.50 3 d SP . .
O1W O 0.1318(4) 1.0144(5) 0.01059(8) 0.309(4) Uani 0.50 1 d PD A 1
H1W H 0.0986 0.9541 0.0084 0.463 Uiso 0.50 1 d PRD A 1
H2W H 0.1458 1.0690 0.0006 0.463 Uiso 0.50 1 d PRD A 1
Cl5 Cl 0.1318(4) 1.0144(5) 0.01059(8) 0.309(4) Uani 0.50 1 d P B 2
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'
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
C1 N1 C4 110.3(2) . .
C2 C1 N1 106.6(3) . .
C2 C1 C41 129.9(3) . .
N1 C1 C41 123.6(3) . .
C16 N2 C13 110.6(3) . .
C1 C2 C3 108.0(3) . .
C28 N3 C25 110.5(3) . .
C4 C3 C2 108.1(3) . .
C37 N4 C40 110.4(3) . .
C3 C4 N1 107.0(3) . .
C3 C4 C5 130.0(3) . .
N1 C4 C5 123.0(3) . .
C13 C5 C4 111.8(3) . .
C13 C5 C12 107.1(3) . .
C4 C5 C12 107.5(3) . .
C13 C5 C6 113.6(3) . .
C4 C5 C6 109.9(3) . .
C12 C5 C6 106.5(3) . .
C7 C6 C11 118.8(3) . .
C7 C6 C5 122.6(3) . .
C11 C6 C5 118.3(3) . .
C6 C7 C8 120.6(3) . .
C9 C8 O1 117.0(3) . .
C9 C8 C7 120.9(4) . .
O1 C8 C7 122.2(3) . .
C8 C9 C10 118.9(4) . .
O2 C10 C11 121.9(4) . .
O2 C10 C9 117.0(4) . .
C11 C10 C9 121.1(4) . .
C10 C11 C6 119.7(4) . .
C14 C13 N2 105.9(3) . .
C14 C13 C5 129.9(3) . .
N2 C13 C5 124.3(3) . .
C13 C14 C15 108.7(3) . .
C16 C15 C14 108.0(3) . .
N2 C16 C15 106.8(3) . .
N2 C16 C17 122.9(3) . .
C15 C16 C17 130.1(3) . .
C25 C17 C16 111.8(3) . .
C25 C17 C24 108.8(3) . .
C16 C17 C24 108.5(3) . .
C25 C17 C18 110.9(3) . .
C16 C17 C18 110.5(3) . .
C24 C17 C18 106.1(3) . .
C19 C18 C23 119.0(3) . .
C19 C18 C17 120.8(3) . .
C23 C18 C17 120.2(3) . .
C20 C19 C18 120.5(4) . .
C19 C20 O3 120.6(4) . .
C19 C20 C21 120.9(4) . .
O3 C20 C21 118.5(4) . .
C22 C21 C20 118.8(3) . .
O4 C22 C21 122.7(3) . .
O4 C22 C23 116.6(3) . .
C21 C22 C23 120.7(3) . .
C22 C23 C18 120.1(3) . .
C26 C25 N3 106.7(3) . .
C26 C25 C17 130.8(3) . .
N3 C25 C17 122.4(3) . .
C25 C26 C27 108.0(3) . .
C28 C27 C26 108.3(3) . .
C27 C28 N3 106.4(3) . .
C27 C28 C29 131.5(3) . .
N3 C28 C29 122.1(3) . .
C28 C29 C37 112.0(3) . .
C28 C29 C30 110.9(3) . .
C37 C29 C30 110.8(3) . .
C28 C29 C36 108.9(3) . .
C37 C29 C36 107.6(3) . .
C30 C29 C36 106.4(3) . .
C31 C30 C35 119.4(3) . .
C31 C30 C29 120.5(3) . .
C35 C30 C29 120.0(3) . .
C30 C31 C32 119.5(3) . .
C33 C32 O5 122.3(3) . .
C33 C32 C31 121.4(3) . .
O5 C32 C31 116.3(3) . .
C32 C33 C34 118.6(3) . .
O6 C34 C33 120.8(3) . .
O6 C34 C35 118.4(3) . .
C33 C34 C35 120.7(3) . .
C34 C35 C30 120.3(3) . .
N4 C37 C38 106.8(3) . .
N4 C37 C29 122.6(3) . .
C38 C37 C29 130.4(3) . .
C37 C38 C39 108.4(3) . .
C40 C39 C38 107.9(3) . .
C39 C40 N4 106.5(3) . .
C39 C40 C41 129.7(3) . .
N4 C40 C41 123.8(3) . .
C40 C41 C1 111.3(3) . .
C40 C41 C42 113.7(3) . .
C1 C41 C42 110.2(3) . .
C40 C41 C48 106.9(3) . .
C1 C41 C48 108.1(3) . .
C42 C41 C48 106.3(3) . .
C47 C42 C43 118.8(3) . .
C47 C42 C41 122.8(3) . .
C43 C42 C41 118.2(3) . .
C44 C43 C42 119.7(4) . .
O7 C44 C43 122.0(4) . .
O7 C44 C45 117.1(4) . .
C43 C44 C45 120.9(4) . .
C46 C45 C44 119.1(4) . .
C45 C46 O8 116.7(3) . .
C45 C46 C47 120.9(3) . .
O8 C46 C47 122.4(3) . .
C46 C47 C42 120.4(3) . .
C1A N1A C4A 107.8(5) . .
C1A N1A C2A 106.8(4) . .
C4A N1A C2A 109.0(4) . .
C1A N1A C3A 110.7(5) . .
C4A N1A C3A 110.2(5) . .
C2A N1A C3A 112.2(5) . .
C2B N1B C1B 105.7(13) . .
C2B N1B C4B 107.1(9) . .
C1B N1B C4B 111.7(8) . .
C2B N1B C3B 108.8(11) . .
C1B N1B C3B 106.0(9) . .
C4B N1B C3B 116.9(8) . .
C1C N1C C2C 113.3(10) . .
C1C N1C C3C 109.3(8) . .
C2C N1C C3C 103.0(7) . .
C1C N1C C4C 109.5(7) . .
C2C N1C C4C 108.8(7) . .
C3C N1C C4C 112.9(7) . .
C2D N1D C2D 103.1(14) 2_665 .
C2D N1D C2D 103.1(14) 2_665 3_565
C2D N1D C2D 103.1(14) . 3_565
C2D N1D C1D 115.3(12) 2_665 .
C2D N1D C1D 115.3(12) . .
C2D N1D C1D 115.3(12) 3_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C1 1.373(4) .
N1 C4 1.374(4) .
O1 C8 1.369(4) .
C1 C2 1.366(4) .
C1 C41 1.517(4) .
N2 C16 1.368(4) .
N2 C13 1.383(4) .
C2 C3 1.411(5) .
O2 C10 1.369(5) .
N3 C28 1.368(4) .
N3 C25 1.372(4) .
O3 C20 1.379(5) .
C3 C4 1.354(5) .
N4 C37 1.363(4) .
N4 C40 1.376(4) .
O4 C22 1.369(4) .
C4 C5 1.525(5) .
O5 C32 1.373(4) .
C5 C13 1.499(5) .
C5 C12 1.543(5) .
C5 C6 1.544(5) .
O6 C34 1.374(4) .
C6 C7 1.381(5) .
C6 C11 1.395(5) .
C7 C8 1.382(5) .
O7 C44 1.369(5) .
O8 C46 1.370(4) .
C8 C9 1.359(6) .
C9 C10 1.387(6) .
C10 C11 1.374(6) .
C13 C14 1.371(5) .
C14 C15 1.400(6) .
C15 C16 1.369(5) .
C16 C17 1.519(5) .
C17 C25 1.510(5) .
C17 C24 1.548(5) .
C17 C18 1.548(5) .
C18 C19 1.379(5) .
C18 C23 1.385(5) .
C19 C20 1.370(6) .
C20 C21 1.384(6) .
C21 C22 1.372(5) .
C22 C23 1.386(5) .
C25 C26 1.360(5) .
C26 C27 1.402(5) .
C27 C28 1.365(5) .
C28 C29 1.514(5) .
C29 C37 1.518(5) .
C29 C30 1.545(5) .
C29 C36 1.549(5) .
C30 C31 1.373(5) .
C30 C35 1.382(5) .
C31 C32 1.394(5) .
C32 C33 1.366(5) .
C33 C34 1.380(5) .
C34 C35 1.380(5) .
C37 C38 1.366(5) .
C38 C39 1.396(6) .
C39 C40 1.371(5) .
C40 C41 1.502(5) .
C41 C42 1.541(5) .
C41 C48 1.548(5) .
C42 C47 1.387(5) .
C42 C43 1.389(5) .
C43 C44 1.375(6) .
C44 C45 1.384(6) .
C45 C46 1.360(6) .
C46 C47 1.373(5) .
N1A C1A 1.471(6) .
N1A C4A 1.475(7) .
N1A C2A 1.481(7) .
N1A C3A 1.482(7) .
N1B C2B 1.370(13) .
N1B C1B 1.388(10) .
N1B C4B 1.403(8) .
N1B C3B 1.408(8) .
N1C C1C 1.400(9) .
N1C C2C 1.413(8) .
N1C C3C 1.466(9) .
N1C C4C 1.497(7) .
N1D C2D 1.436(9) 2_665
N1D C2D 1.436(9) .
N1D C2D 1.436(9) 3_565
N1D C1D 1.460(10) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C4 N1 C1 C2 0.6(4)
C4 N1 C1 C41 -179.0(3)
N1 C1 C2 C3 -0.4(4)
C41 C1 C2 C3 179(66)
C1 C2 C3 C4 0.1(4)
C2 C3 C4 N1 0.2(4)
C2 C3 C4 C5 -179(66)
C1 N1 C4 C3 -0.5(4)
C1 N1 C4 C5 179.1(3)
C3 C4 C5 C13 -103.8(4)
N1 C4 C5 C13 76.7(4)
C3 C4 C5 C12 13.5(5)
N1 C4 C5 C12 -166.0(3)
C3 C4 C5 C6 129.1(4)
N1 C4 C5 C6 -50.4(4)
C13 C5 C6 C7 9.5(4)
C4 C5 C6 C7 135.7(3)
C12 C5 C6 C7 -108.1(4)
C13 C5 C6 C11 -176.5(3)
C4 C5 C6 C11 -50.3(4)
C12 C5 C6 C11 65.9(4)
C11 C6 C7 C8 -0.5(5)
C5 C6 C7 C8 173.5(3)
C6 C7 C8 C9 -2.2(5)
C6 C7 C8 O1 177.8(3)
O1 C8 C9 C10 -177.2(4)
C7 C8 C9 C10 2.8(6)
C8 C9 C10 O2 -179.2(4)
C8 C9 C10 C11 -0.8(7)
O2 C10 C11 C6 176.6(4)
C9 C10 C11 C6 -1.8(7)
C7 C6 C11 C10 2.4(6)
C5 C6 C11 C10 -171.8(4)
C16 N2 C13 C14 0.5(4)
C16 N2 C13 C5 -179.9(3)
C4 C5 C13 C14 118.0(4)
C12 C5 C13 C14 0.5(5)
C6 C5 C13 C14 -116.9(4)
C4 C5 C13 N2 -61.6(4)
C12 C5 C13 N2 -179.1(3)
C6 C5 C13 N2 63.6(4)
N2 C13 C14 C15 -0.2(4)
C5 C13 C14 C15 -179.9(3)
C13 C14 C15 C16 -0.1(5)
C13 N2 C16 C15 -0.5(4)
C13 N2 C16 C17 175.3(3)
C14 C15 C16 N2 0.4(4)
C14 C15 C16 C17 -175.1(4)
N2 C16 C17 C25 67.0(4)
C15 C16 C17 C25 -118.2(4)
N2 C16 C17 C24 -173.0(3)
C15 C16 C17 C24 1.8(5)
N2 C16 C17 C18 -57.0(4)
C15 C16 C17 C18 117.8(4)
C25 C17 C18 C19 35.5(4)
C16 C17 C18 C19 160.0(3)
C24 C17 C18 C19 -82.6(4)
C25 C17 C18 C23 -147.9(3)
C16 C17 C18 C23 -23.4(4)
C24 C17 C18 C23 94.0(4)
C23 C18 C19 C20 0.6(6)
C17 C18 C19 C20 177.3(3)
C18 C19 C20 O3 -179.9(4)
C18 C19 C20 C21 0.5(6)
C19 C20 C21 C22 -0.1(6)
O3 C20 C21 C22 -179.7(4)
C20 C21 C22 O4 178.6(3)
C20 C21 C22 C23 -1.5(6)
O4 C22 C23 C18 -177.5(3)
C21 C22 C23 C18 2.6(5)
C19 C18 C23 C22 -2.2(5)
C17 C18 C23 C22 -178.8(3)
C28 N3 C25 C26 1.3(4)
C28 N3 C25 C17 -177.7(3)
C16 C17 C25 C26 107.0(4)
C24 C17 C25 C26 -12.8(5)
C18 C17 C25 C26 -129.1(4)
C16 C17 C25 N3 -74.2(4)
C24 C17 C25 N3 166.0(3)
C18 C17 C25 N3 49.7(4)
N3 C25 C26 C27 -0.6(4)
C17 C25 C26 C27 178.3(3)
C25 C26 C27 C28 -0.2(4)
C26 C27 C28 N3 1.0(4)
C26 C27 C28 C29 -177.3(3)
C25 N3 C28 C27 -1.4(4)
C25 N3 C28 C29 177.0(3)
C27 C28 C29 C37 -107.5(4)
N3 C28 C29 C37 74.4(4)
C27 C28 C29 C30 128.1(4)
N3 C28 C29 C30 -49.9(4)
C27 C28 C29 C36 11.4(5)
N3 C28 C29 C36 -166.7(3)
C28 C29 C30 C31 150.3(3)
C37 C29 C30 C31 25.2(4)
C36 C29 C30 C31 -91.5(4)
C28 C29 C30 C35 -32.9(4)
C37 C29 C30 C35 -157.9(3)
C36 C29 C30 C35 85.4(4)
C35 C30 C31 C32 1.8(5)
C29 C30 C31 C32 178.6(3)
C30 C31 C32 C33 -3.3(5)
C30 C31 C32 O5 176.6(3)
O5 C32 C33 C34 -177.1(3)
C31 C32 C33 C34 2.8(5)
C32 C33 C34 O6 -179.9(3)
C32 C33 C34 C35 -0.9(5)
O6 C34 C35 C30 178.5(3)
C33 C34 C35 C30 -0.6(5)
C31 C30 C35 C34 0.2(5)
C29 C30 C35 C34 -176.7(3)
C40 N4 C37 C38 0.8(4)
C40 N4 C37 C29 -175.6(3)
C28 C29 C37 N4 -66.6(4)
C30 C29 C37 N4 57.8(4)
C36 C29 C37 N4 173.8(3)
C28 C29 C37 C38 118.0(4)
C30 C29 C37 C38 -117.6(4)
C36 C29 C37 C38 -1.6(5)
N4 C37 C38 C39 -0.3(4)
C29 C37 C38 C39 175.6(4)
C37 C38 C39 C40 -0.2(5)
C38 C39 C40 N4 0.7(4)
C38 C39 C40 C41 -179.1(3)
C37 N4 C40 C39 -0.9(4)
C37 N4 C40 C41 178.9(3)
C39 C40 C41 C1 -117.3(4)
N4 C40 C41 C1 63.0(4)
C39 C40 C41 C42 117.5(4)
N4 C40 C41 C42 -62.2(4)
C39 C40 C41 C48 0.6(5)
N4 C40 C41 C48 -179.2(3)
C2 C1 C41 C40 102.5(4)
N1 C1 C41 C40 -78.0(4)
C2 C1 C41 C42 -130.3(4)
N1 C1 C41 C42 49.2(4)
C2 C1 C41 C48 -14.5(5)
N1 C1 C41 C48 165.0(3)
C40 C41 C42 C47 -8.7(4)
C1 C41 C42 C47 -134.5(3)
C48 C41 C42 C47 108.6(4)
C40 C41 C42 C43 176.1(3)
C1 C41 C42 C43 50.4(4)
C48 C41 C42 C43 -66.5(4)
C47 C42 C43 C44 -3.1(6)
C41 C42 C43 C44 172.2(4)
C42 C43 C44 O7 -175.7(5)
C42 C43 C44 C45 2.6(7)
O7 C44 C45 C46 178.7(5)
C43 C44 C45 C46 0.3(7)
C44 C45 C46 O8 177.3(4)
C44 C45 C46 C47 -2.8(7)
C45 C46 C47 C42 2.2(5)
O8 C46 C47 C42 -177.9(3)
C43 C42 C47 C46 0.8(5)
C41 C42 C47 C46 -174.3(3)
