#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:11:47 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180380 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/49/7204902.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_7204902
loop_
_publ_author_name
'Danil de Namor, Angela F.'
'Kowalska, Dorota'
'Castellano, Eduardo E.'
'Piro, Oscar E.'
'Sueros Velarde, Felix J.'
'Villanueva Salas, Jose'
_publ_contact_author
;
Angela F. Danil de Namor
Laboratory of Thermochemistry
Department of Chemistry
University of Surrey
Guildford, Surrey, GU2 5XH
England
;
_publ_section_title
;
 Lower rim calix(4)arene ketone derivatives and their interaction with
 alkali metal cations. Structural and thermodynamic (solution and
 complexation) characterisation of the tetraphenyl ketone derivative
 and its sodium complex
;
_journal_issue                   18
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_page_first              4010
_journal_paper_doi               10.1039/b104355m
_journal_volume                  3
_journal_year                    2001
_chemical_formula_sum            'C80 H91 Cl N Na O14'
_chemical_formula_weight         1348.98
_chemical_name_systematic
;
sodium 5,11,17,23-tetra-tert-butyl-25,26,27,28-tetra(benzoyl)methoxy
calix(4)arene monoacetonitrile perchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 108.422(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8693(9)
_cell_length_b                   13.4590(5)
_cell_length_c                   30.405(2)
_cell_measurement_reflns_used    17881
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      1.1
_cell_volume                     7714.3(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.506
_diffrn_measured_fraction_theta_max 0.506
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_sigmaI/netI    0.0710
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            17881
_diffrn_reflns_theta_full        27.18
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.116
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.320
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         9054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.320
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.1066
_refine_ls_shift/su_max          1.040
_refine_ls_shift/su_mean         0.036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=3D(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3058
_refine_ls_wR_factor_ref         0.3416
_reflns_number_gt                6117
_reflns_number_total             9054
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            program.txt
_cod_data_source_block           s97
_cod_depositor_comments
;
The following automatic conversions were performed:
'_publ_contact_autor' tag replaced with '_publ_contact_author'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=3D(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=3D1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7714.4(7)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7204902
loop_
_symmetry_equiv_pos_as_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'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Na Na 0.44269(9) 0.43687(12) 0.15747(9) 0.0593(7) Uani 1 d . . .
C11 C 0.5081(3) 0.5671(3) 0.2634(3) 0.0500(15) Uani 1 d . . .
C12 C 0.5800(3) 0.5487(3) 0.2895(3) 0.0570(17) Uani 1 d . . .
C13 C 0.5991(3) 0.5603(4) 0.3360(3) 0.0647(19) Uani 1 d . . .
H13 H 0.6463 0.5496 0.3533 0.078 Uiso 1 calc R . .
C14 C 0.5512(3) 0.5877(4) 0.3597(3) 0.0674(18) Uani 1 d . . .
C15 C 0.4805(3) 0.6000(4) 0.3319(3) 0.0659(19) Uani 1 d . . .
H15 H 0.4470 0.6167 0.3462 0.079 Uiso 1 calc R . .
C16 C 0.4585(3) 0.5889(3) 0.2852(3) 0.0553(17) Uani 1 d . . .
C17 C 0.5759(4) 0.6039(5) 0.4105(4) 0.093(3) Uani 1 d . . .
C18 C 0.6334(9) 0.5335(13) 0.4394(5) 0.206(7) Uani 1 d . . .
H18A H 0.6787 0.5661 0.4475 0.308 Uiso 1 calc R . .
H18B H 0.6346 0.4748 0.4218 0.308 Uiso 1 calc R . .
H18C H 0.6231 0.5155 0.4672 0.308 Uiso 1 calc R . .
C19 C 0.5223(8) 0.618(3) 0.4329(7) 0.38(2) Uani 1 d . . .
H19A H 0.4779 0.5919 0.4136 0.568 Uiso 1 calc R . .
H19B H 0.5171 0.6879 0.4378 0.568 Uiso 1 calc R . .
H19C H 0.5363 0.5845 0.4622 0.568 Uiso 1 calc R . .
C110 C 0.6240(9) 0.7017(9) 0.4216(7) 0.230(8) Uani 1 d . . .
H11A H 0.6019 0.7507 0.4355 0.346 Uiso 1 calc R . .
H11B H 0.6289 0.7276 0.3934 0.346 Uiso 1 calc R . .
H11C H 0.6700 0.6855 0.4427 0.346 Uiso 1 calc R . .
O11 O 0.48709(18) 0.56412(19) 0.21515(17) 0.0565(12) Uani 1 d . . .
C111 C 0.4989(3) 0.6572(3) 0.1957(3) 0.0632(18) Uani 1 d . . .
H11D H 0.5452 0.6567 0.1914 0.076 Uiso 1 calc R . .
H11E H 0.4981 0.7107 0.2169 0.076 Uiso 1 calc R . .
C112 C 0.4430(3) 0.6746(3) 0.1503(3) 0.0596(17) Uani 1 d . . .
O12 O 0.3975(2) 0.6130(3) 0.13410(18) 0.0778(14) Uani 1 d . . .
C113 C 0.4474(3) 0.7685(4) 0.1254(3) 0.0664(18) Uani 1 d . . .
C114 C 0.3993(4) 0.7857(5) 0.0832(4) 0.094(3) Uani 1 d . . .
H114 H 0.3646 0.7384 0.0701 0.113 Uiso 1 calc R . .
C115 C 0.4011(5) 0.8720(6) 0.0595(4) 0.116(3) Uani 1 d . . .
H115 H 0.3687 0.8816 0.0301 0.139 Uiso 1 calc R . .
C116 C 0.4490(7) 0.9421(6) 0.0781(5) 0.119(4) Uani 1 d . . .
H116 H 0.4494 1.0004 0.0617 0.143 Uiso 1 calc R . .
C117 C 0.4980(6) 0.9289(5) 0.1215(5) 0.108(3) Uani 1 d . . .
H117 H 0.5313 0.9780 0.1345 0.129 Uiso 1 calc R . .
C118 C 0.4969(4) 0.8420(4) 0.1452(3) 0.085(2) Uani 1 d . . .
H118 H 0.5294 0.8325 0.1745 0.102 Uiso 1 calc R . .
C12' C 0.3791(2) 0.5970(3) 0.2570(2) 0.0490(14) Uani 1 d . . .
H12A H 0.3581 0.6529 0.2680 0.059 Uiso 1 calc R . .
H12B H 0.3739 0.6079 0.2246 0.059 Uiso 1 calc R . .
C21 C 0.3282(2) 0.4258(3) 0.2290(2) 0.0483(15) Uani 1 d . . .
C22 C 0.3411(2) 0.5012(3) 0.2623(2) 0.0510(16) Uani 1 d . . .
C23 C 0.3233(3) 0.4859(3) 0.3016(2) 0.0573(17) Uani 1 d . . .
H23 H 0.3289 0.5383 0.3224 0.069 Uiso 1 calc R . .
C24 C 0.2969(3) 0.3950(4) 0.3125(3) 0.067(2) Uani 1 d . . .
C25 C 0.2901(3) 0.3194(3) 0.2792(2) 0.0573(18) Uani 1 d . . .
H25 H 0.2732 0.2578 0.2848 0.069 Uiso 1 calc R . .
C26 C 0.3068(2) 0.3315(3) 0.2395(2) 0.0533(17) Uani 1 d . . .
C27 C 0.2753(4) 0.3842(4) 0.3552(3) 0.074(2) Uani 1 d . . .
C28 C 0.2146(6) 0.4566(7) 0.3538(4) 0.148(5) Uani 1 d . . .
H28A H 0.1992 0.4455 0.3803 0.222 Uiso 1 calc R . .
H28B H 0.1756 0.4455 0.3260 0.222 Uiso 1 calc R . .
H28C H 0.2310 0.5237 0.3542 0.222 Uiso 1 calc R . .
C29 C 0.2504(6) 0.2778(5) 0.3617(4) 0.143(4) Uani 1 d . . .
H29A H 0.2872 0.2311 0.3621 0.215 Uiso 1 calc R . .
H29B H 0.2084 0.2622 0.3366 0.215 Uiso 1 calc R . .
H29C H 0.2403 0.2740 0.3905 0.215 Uiso 1 calc R . .
C210 C 0.3365(6) 0.4010(10) 0.3976(4) 0.145(4) Uani 1 d . . .
H21A H 0.3727 0.3526 0.3991 0.217 Uiso 1 calc R . .
H21B H 0.3213 0.3949 0.4244 0.217 Uiso 1 calc R . .
H21C H 0.3552 0.4665 0.3966 0.217 Uiso 1 calc R . .
C211 C 0.2745(3) 0.4785(4) 0.1528(3) 0.0628(17) Uani 1 d . . .
H21D H 0.2703 0.5493 0.1574 0.075 Uiso 1 calc R . .
H21E H 0.2336 0.4460 0.1573 0.075 Uiso 1 calc R . .
O21 O 0.33864(16) 0.4416(2) 0.18705(16) 0.0556(12) Uani 1 d . . .
C212 C 0.2749(3) 0.4604(3) 0.1045(3) 0.0634(19) Uani 1 d . . .
O22 O 0.3247(2) 0.4192(3) 0.09709(19) 0.0795(14) Uani 1 d . . .
C213 C 0.2109(3) 0.4911(4) 0.0654(3) 0.0695(19) Uani 1 d . . .
C214 C 0.2073(5) 0.4622(7) 0.0213(4) 0.115(3) Uani 1 d . . .
H214 H 0.2432 0.4231 0.0169 0.138 Uiso 1 calc R . .
C215 C 0.1000(6) 0.5745(8) 0.0341(6) 0.136(4) Uani 1 d . . .
H215 H 0.0634 0.6111 0.0391 0.163 Uiso 1 calc R . .
C216 C 0.0969(6) 0.5482(10) -0.0088(6) 0.149(5) Uani 1 d . . .
H216 H 0.0581 0.5688 -0.0334 0.179 Uiso 1 calc R . .
C217 C 0.1481(6) 0.4923(11) -0.0182(5) 0.154(4) Uani 1 d . . .
H217 H 0.1451 0.4744 -0.0483 0.184 Uiso 1 calc R . .
C218 C 0.1572(4) 0.5472(5) 0.0704(3) 0.089(2) Uani 1 d . . .
H218 H 0.1595 0.5681 0.1000 0.107 Uiso 1 calc R . .
C23' C 0.3004(2) 0.2438(3) 0.2057(2) 0.0599(17) Uani 1 d . . .
H23A H 0.2597 0.2033 0.2050 0.072 Uiso 1 calc R . .
H23B H 0.2935 0.2688 0.1747 0.072 Uiso 1 calc R . .
C31 C 0.4218(2) 0.1940(3) 0.2019(2) 0.0490(14) Uani 1 d . . .
C32 C 0.3684(2) 0.1802(3) 0.2215(2) 0.0517(15) Uani 1 d . . .
C33 C 0.3777(3) 0.1062(4) 0.2543(2) 0.0641(18) Uani 1 d . . .
H33 H 0.3423 0.0955 0.2678 0.077 Uiso 1 calc R . .
C34 C 0.4376(3) 0.0474(3) 0.2679(2) 0.0564(16) Uani 1 d . . .
C35 C 0.4918(3) 0.0680(3) 0.2497(2) 0.0573(16) Uani 1 d . . .
H35 H 0.5333 0.0307 0.2595 0.069 Uiso 1 calc R . .
C36 C 0.4861(2) 0.1431(3) 0.2173(2) 0.0525(16) Uani 1 d . . .
C37 C 0.4471(3) -0.0399(4) 0.3033(3) 0.072(2) Uani 1 d . . .
C38 C 0.3818(6) -0.0563(10) 0.3149(6) 0.203(8) Uani 1 d . . .
H38A H 0.3922 -0.0951 0.3427 0.305 Uiso 1 calc R . .
H38B H 0.3481 -0.0910 0.2899 0.305 Uiso 1 calc R . .
H38C H 0.3623 0.0066 0.3196 0.305 Uiso 1 calc R . .
C39 C 0.4593(8) -0.1339(6) 0.2767(5) 0.169(5) Uani 1 d . . .
H39A H 0.4881 -0.1808 0.2983 0.253 Uiso 1 calc R . .
H39B H 0.4828 -0.1151 0.2548 0.253 Uiso 1 calc R . .
H39C H 0.4144 -0.1638 0.2605 0.253 Uiso 1 calc R . .
C310 C 0.5162(6) -0.0281(8) 0.3432(5) 0.158(5) Uani 1 d . . .
H31A H 0.5247 0.0411 0.3506 0.237 Uiso 1 calc R . .
H31B H 0.5548 -0.0548 0.3343 0.237 Uiso 1 calc R . .
H31C H 0.5127 -0.0631 0.3699 0.237 Uiso 1 calc R . .
O31 O 0.41179(17) 0.2609(2) 0.16517(15) 0.0552(10) Uani 1 d . . .
C311 C 0.3850(3) 0.2118(4) 0.1205(3) 0.070(2) Uani 1 d . . .
H31D H 0.3339 0.2197 0.1085 0.084 Uiso 1 calc R . .
H31E H 0.3953 0.1413 0.1243 0.084 Uiso 1 calc R . .
C312 C 0.4176(3) 0.2538(4) 0.0863(3) 0.0603(17) Uani 1 d . . .
O32 O 0.45731(19) 0.3265(3) 0.09697(16) 0.0705(12) Uani 1 d . . .
C313 C 0.4045(3) 0.2050(4) 0.0417(3) 0.0679(19) Uani 1 d . . .
C314 C 0.4503(4) 0.2218(5) 0.0169(3) 0.093(3) Uani 1 d . . .
H314 H 0.4871 0.2672 0.0276 0.111 Uiso 1 calc R . .
C315 C 0.3437(6) 0.0898(5) -0.0171(4) 0.117(3) Uani 1 d . . .
H315 H 0.3078 0.0435 -0.0290 0.140 Uiso 1 calc R . .
C316 C 0.3919(7) 0.1098(7) -0.0398(4) 0.116(3) Uani 1 d . . .
H316 H 0.3881 0.0776 -0.0675 0.140 Uiso 1 calc R . .
C317 C 0.4422(6) 0.1725(9) -0.0232(4) 0.132(4) Uani 1 d . . .
H317 H 0.4742 0.1844 -0.0393 0.159 Uiso 1 calc R . .
C318 C 0.3492(4) 0.1396(5) 0.0239(3) 0.090(2) Uani 1 d . . .
H318 H 0.3159 0.1290 0.0391 0.108 Uiso 1 calc R . .
C34' C 0.5490(3) 0.1691(3) 0.2010(2) 0.0572(16) Uani 1 d . . .
H34A H 0.5733 0.1090 0.1970 0.069 Uiso 1 calc R . .
H34B H 0.5327 0.2035 0.1715 0.069 Uiso 1 calc R . .
C41 C 0.6003(2) 0.3384(3) 0.2326(2) 0.0477(14) Uani 1 d . . .
C42 C 0.5990(2) 0.2350(3) 0.2372(2) 0.0550(16) Uani 1 d . . .
C43 C 0.6431(3) 0.1933(4) 0.2788(3) 0.0637(18) Uani 1 d . . .
H43 H 0.6440 0.1246 0.2820 0.076 Uiso 1 calc R . .
C44 C 0.6845(3) 0.2491(4) 0.3146(3) 0.070(2) Uani 1 d . . .
C45 C 0.6804(3) 0.3527(4) 0.3094(3) 0.0629(17) Uani 1 d . . .
H45 H 0.7068 0.3924 0.3339 0.075 Uiso 1 calc R . .
C46 C 0.6390(2) 0.3975(3) 0.2695(2) 0.0528(16) Uani 1 d . . .
C47 C 0.7343(3) 0.2016(4) 0.3585(4) 0.094(3) Uani 1 d . . .
C48 C 0.7215(5) 0.2459(7) 0.4027(4) 0.131(3) Uani 1 d . . .
H48A H 0.7216 0.3171 0.4011 0.196 Uiso 1 calc R . .
H48B H 0.7586 0.2243 0.4298 0.196 Uiso 1 calc R . .
H48C H 0.6766 0.2234 0.4045 0.196 Uiso 1 calc R . .
C49 C 0.8117(4) 0.2224(7) 0.3609(5) 0.148(5) Uani 1 d . . .
H49A H 0.8203 0.1948 0.3340 0.222 Uiso 1 calc R . .
H49B H 0.8433 0.1925 0.3883 0.222 Uiso 1 calc R . .
H49C H 0.8196 0.2928 0.3618 0.222 Uiso 1 calc R . .
C410 C 0.7259(5) 0.0905(6) 0.3612(6) 0.158(6) Uani 1 d . . .
H41A H 0.6791 0.0755 0.3619 0.237 Uiso 1 calc R . .
H41B H 0.7603 0.0656 0.3888 0.237 Uiso 1 calc R . .
H41C H 0.7331 0.0597 0.3345 0.237 Uiso 1 calc R . .
O41 O 0.56367(17) 0.3833(2) 0.19024(16) 0.0534(11) Uani 1 d . . .
C411 C 0.6036(3) 0.3813(3) 0.1595(3) 0.0613(18) Uani 1 d . . .
H41D H 0.6021 0.3150 0.1467 0.074 Uiso 1 calc R . .
H41E H 0.6526 0.3970 0.1763 0.074 Uiso 1 calc R . .
C412 C 0.5755(3) 0.4550(3) 0.1204(2) 0.0569(18) Uani 1 d . . .
O42 O 0.5340(2) 0.5185(2) 0.12441(18) 0.0800(15) Uani 1 d . . .
C413 C 0.6008(3) 0.4510(3) 0.0803(3) 0.0630(19) Uani 1 d . . .
C414 C 0.5804(3) 0.5223(5) 0.0467(3) 0.081(2) Uani 1 d . . .
H414 H 0.5523 0.5747 0.0507 0.097 Uiso 1 calc R . .
C415 C 0.6003(5) 0.5189(6) 0.0068(3) 0.098(3) Uani 1 d . . .
H415 H 0.5851 0.5675 -0.0159 0.117 Uiso 1 calc R . .
C416 C 0.6430(6) 0.4426(7) 0.0016(4) 0.122(4) Uani 1 d . . .
H416 H 0.6564 0.4381 -0.0250 0.147 Uiso 1 calc R . .
C417 C 0.6657(6) 0.3731(6) 0.0361(4) 0.122(4) Uani 1 d . . .
H417 H 0.6960 0.3229 0.0329 0.146 Uiso 1 calc R . .
C418 C 0.6453(4) 0.3750(4) 0.0743(3) 0.093(3) Uani 1 d . . .
H418 H 0.6608 0.3259 0.0967 0.111 Uiso 1 calc R . .
C41' C 0.6335(3) 0.5122(3) 0.2660(2) 0.0597(18) Uani 1 d . . .
H41F H 0.6796 0.5416 0.2810 0.072 Uiso 1 calc R . .
H41G H 0.6181 0.5321 0.2336 0.072 Uiso 1 calc R . .
Cl Cl 0.67875(9) 0.10438(13) 0.13149(10) 0.1025(9) Uani 1 d . . .
O1 O 0.6090(2) 0.1302(3) 0.1086(2) 0.110(2) Uani 1 d . . .
O2 O 0.6796(5) 0.0164(5) 0.1537(4) 0.208(5) Uani 1 d . . .
O3 O 0.7149(4) 0.0775(9) 0.1035(4) 0.226(6) Uani 1 d . . .
O4 O 0.7118(5) 0.1795(6) 0.1563(5) 0.234(6) Uani 1 d . . .
C1 C 0.4979(4) 0.3116(5) 0.3251(4) 0.102(3) Uani 1 d . . .
H1A H 0.5338 0.2819 0.3143 0.153 Uiso 1 calc R . .
H1B H 0.5074 0.3813 0.3302 0.153 Uiso 1 calc R . .
H1C H 0.4523 0.3026 0.3022 0.153 Uiso 1 calc R . .
C2 C 0.4984(6) 0.2672(7) 0.3657(6) 0.132(4) Uani 1 d . . .
N N 0.4941(10) 0.2323(10) 0.3989(6) 0.226(7) Uani 1 d . . .
C3 C 0.6467(8) 0.9386(9) 0.2393(6) 0.183(6) Uani 1 d . . .
H3A H 0.6881 0.9760 0.2398 0.275 Uiso 1 calc R . .
H3B H 0.6147 0.9804 0.2489 0.275 Uiso 1 calc R . .
H3C H 0.6235 0.9148 0.2084 0.275 Uiso 1 calc R . .
C4 C 0.6715(13) 0.838(3) 0.2768(16) 0.58(5) Uani 1 d . . .
H4A H 0.7081 0.8602 0.3046 0.692 Uiso 1 calc R . .
H4B H 0.6309 0.8180 0.2858 0.692 Uiso 1 calc R . .
O5 O 0.6962(9) 0.7576(13) 0.2591(7) 0.302(8) Uani 1 d . . .
O1W O 0.1553(8) 0.2237(9) 0.0707(12) 0.50(2) Uani 1 d . . .
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'
O O 0.0106 0.0060 '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'
Na Na 0.0362 0.0249 '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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
O41 Na O11 79.81(13) . . ?
O41 Na O32 77.85(14) . . ?
O11 Na O32 150.86(13) . . ?
O41 Na O31 85.38(12) . . ?
O11 Na O31 130.95(17) . . ?
O32 Na O31 65.38(13) . . ?
O41 Na O22 149.55(15) . . ?
O11 Na O22 130.33(13) . . ?
O32 Na O22 72.30(14) . . ?
O31 Na O22 76.98(14) . . ?
O41 Na O21 133.64(16) . . ?
O11 Na O21 82.80(12) . . ?
O32 Na O21 126.30(14) . . ?
O31 Na O21 74.46(10) . . ?
O22 Na O21 64.87(15) . . ?
O41 Na O12 127.66(13) . . ?
O11 Na O12 63.81(15) . . ?
O32 Na O12 117.89(18) . . ?
O31 Na O12 146.92(13) . . ?
O22 Na O12 73.59(14) . . ?
O21 Na O12 79.58(12) . . ?
O41 Na O42 63.59(14) . . ?
O11 Na O42 80.79(14) . . ?
O32 Na O42 72.63(13) . . ?
O31 Na O42 132.07(12) . . ?
O22 Na O42 111.55(18) . . ?
O21 Na O42 153.06(12) . . ?
O12 Na O42 74.03(12) . . ?
C16 C11 O11 119.4(5) . . ?
C16 C11 C12 120.8(7) . . ?
O11 C11 C12 119.8(5) . . ?
C13 C12 C11 117.6(5) . . ?
C13 C12 C41' 121.1(5) . . ?
C11 C12 C41' 121.2(7) . . ?
C12 C13 C14 123.6(6) . . ?
C15 C14 C13 115.5(7) . . ?
C15 C14 C17 123.4(6) . . ?
C13 C14 C17 121.1(6) . . ?
C16 C15 C14 123.3(6) . . ?
C15 C16 C11 118.9(5) . . ?
C15 C16 C12' 120.6(5) . . ?
C11 C16 C12' 120.4(6) . . ?
C19 C17 C14 117.3(9) . . ?
C19 C17 C18 109.8(15) . . ?
C14 C17 C18 116.7(8) . . ?
C19 C17 C110 105.7(15) . . ?
C14 C17 C110 108.7(9) . . ?
C18 C17 C110 95.8(10) . . ?
C11 O11 C111 112.0(4) . . ?
C11 O11 Na 134.9(3) . . ?
C111 O11 Na 113.0(4) . . ?
O11 C111 C112 110.4(4) . . ?
O12 C112 C113 122.0(7) . . ?
O12 C112 C111 120.7(5) . . ?
C113 C112 C111 117.3(5) . . ?
C112 O12 Na 111.7(4) . . ?
C114 C113 C118 118.6(6) . . ?
C114 C113 C112 119.2(6) . . ?
C118 C113 C112 122.1(7) . . ?
C113 C114 C115 120.9(8) . . ?
C116 C115 C114 120.7(11) . . ?
C115 C116 C117 120.5(8) . . ?
C118 C117 C116 119.1(8) . . ?
C117 C118 C113 120.3(9) . . ?
C22 C12' C16 109.5(4) . . ?
O21 C21 C22 120.9(4) . . ?
O21 C21 C26 119.7(5) . . ?
C22 C21 C26 119.4(5) . . ?
C23 C22 C21 119.0(4) . . ?
C23 C22 C12' 119.6(5) . . ?
C21 C22 C12' 121.3(5) . . ?
C22 C23 C24 123.7(5) . . ?
C25 C24 C23 114.6(6) . . ?
C25 C24 C27 124.2(4) . . ?
C23 C24 C27 121.1(5) . . ?
C26 C25 C24 123.7(4) . . ?
C25 C26 C21 119.0(5) . . ?
C25 C26 C23' 120.5(4) . . ?
C21 C26 C23' 120.5(5) . . ?
C210 C27 C24 110.9(6) . . ?
C210 C27 C28 110.3(8) . . ?
C24 C27 C28 110.5(6) . . ?
C210 C27 C29 103.8(9) . . ?
C24 C27 C29 113.0(6) . . ?
C28 C27 C29 108.0(6) . . ?
O21 C211 C212 111.9(4) . . ?
C21 O21 C211 111.3(3) . . ?
C21 O21 Na 135.6(3) . . ?
C211 O21 Na 112.8(3) . . ?
O22 C212 C211 121.0(6) . . ?
O22 C212 C213 120.9(7) . . ?
C211 C212 C213 118.0(5) . . ?
C212 O22 Na 116.8(4) . . ?
C218 C213 C214 117.8(8) . . ?
C218 C213 C212 124.4(7) . . ?
C214 C213 C212 117.8(6) . . ?
C213 C214 C217 120.5(9) . . ?
C216 C215 C218 119.4(10) . . ?
C215 C216 C217 122.8(13) . . ?
C216 C217 C214 116.4(12) . . ?
C213 C218 C215 123.0(9) . . ?
C32 C23' C26 109.7(5) . . ?
C32 C31 C36 122.4(5) . . ?
C32 C31 O31 119.7(4) . . ?
C36 C31 O31 117.8(4) . . ?
C33 C32 C31 117.5(4) . . ?
C33 C32 C23' 122.0(4) . . ?
C31 C32 C23' 120.4(5) . . ?
C34 C33 C32 122.4(4) . . ?
C33 C34 C35 118.2(5) . . ?
C33 C34 C37 122.8(4) . . ?
C35 C34 C37 119.0(4) . . ?
C34 C35 C36 122.0(4) . . ?
C31 C36 C35 117.0(4) . . ?
C31 C36 C34' 122.6(5) . . ?
C35 C36 C34' 120.4(4) . . ?
C38 C37 C310 117.9(10) . . ?
C38 C37 C34 110.8(6) . . ?
C310 C37 C34 110.6(5) . . ?
C38 C37 C39 107.2(8) . . ?
C310 C37 C39 104.4(8) . . ?
C34 C37 C39 104.9(7) . . ?
C31 O31 C311 111.8(4) . . ?
C31 O31 Na 135.6(3) . . ?
C311 O31 Na 112.0(3) . . ?
O31 C311 C312 111.5(4) . . ?
O32 C312 C313 121.0(5) . . ?
O32 C312 C311 119.8(6) . . ?
C313 C312 C311 119.2(5) . . ?
C312 O32 Na 117.4(3) . . ?
C314 C313 C318 118.2(7) . . ?
C314 C313 C312 119.0(6) . . ?
C318 C313 C312 122.8(6) . . ?
C317 C314 C313 120.3(7) . . ?
C316 C315 C318 119.1(8) . . ?
C317 C316 C315 120.8(10) . . ?
C316 C317 C314 122.2(10) . . ?
C313 C318 C315 119.3(8) . . ?
C42 C34' C36 108.5(4) . . ?
C46 C41 C42 120.7(6) . . ?
C46 C41 O41 119.2(4) . . ?
C42 C41 O41 120.1(5) . . ?
C41 C42 C43 117.4(5) . . ?
C41 C42 C34' 122.6(6) . . ?
C43 C42 C34' 119.9(4) . . ?
C44 C43 C42 123.0(5) . . ?
C43 C44 C45 117.3(6) . . ?
C43 C44 C47 121.8(5) . . ?
C45 C44 C47 120.9(6) . . ?
C46 C45 C44 122.3(6) . . ?
C45 C46 C41 119.0(4) . . ?
C45 C46 C41' 120.6(5) . . ?
C41 C46 C41' 120.4(5) . . ?
C410 C47 C44 114.2(8) . . ?
C410 C47 C49 107.6(6) . . ?
C44 C47 C49 109.1(7) . . ?
C410 C47 C48 106.3(10) . . ?
C44 C47 C48 110.8(6) . . ?
C49 C47 C48 108.7(8) . . ?
C41 O41 C411 111.4(4) . . ?
C41 O41 Na 132.2(2) . . ?
C411 O41 Na 115.5(4) . . ?
O41 C411 C412 111.5(4) . . ?
O42 C412 C413 122.2(6) . . ?
O42 C412 C411 118.2(5) . . ?
C413 C412 C411 119.6(4) . . ?
C412 O42 Na 108.7(3) . . ?
C414 C413 C418 117.7(6) . . ?
C414 C413 C412 120.0(5) . . ?
C418 C413 C412 122.4(6) . . ?
C413 C414 C415 122.0(6) . . ?
C416 C415 C414 118.8(8) . . ?
C417 C416 C415 119.2(8) . . ?
C418 C417 C416 122.1(7) . . ?
C417 C418 C413 120.1(8) . . ?
C12 C41' C46 109.2(4) . . ?
O4 Cl O3 107.8(7) . . ?
O4 Cl O2 117.5(8) . . ?
O3 Cl O2 99.1(8) . . ?
O4 Cl O1 109.7(4) . . ?
O3 Cl O1 113.8(7) . . ?
O2 Cl O1 108.8(4) . . ?
N C2 C1 175.4(14) . . ?
O5 C4 C3 115(3) . . ?
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
Na O41 2.403(4) . ?
Na O11 2.410(5) . ?
Na O32 2.452(4) . ?
Na O31 2.476(3) . ?
Na O22 2.490(5) . ?
Na O21 2.502(3) . ?
Na O12 2.555(4) . ?
Na O42 2.582(4) . ?
C11 C16 1.382(7) . ?
C11 O11 1.392(7) . ?
C11 C12 1.421(8) . ?
C12 C13 1.353(9) . ?
C12 C41' 1.536(7) . ?
C13 C14 1.412(9) . ?
C14 C15 1.402(10) . ?
C14 C17 1.481(11) . ?
C15 C16 1.356(9) . ?
C16 C12' 1.542(8) . ?
C17 C19 1.448(14) . ?
C17 C18 1.530(16) . ?
C17 C110 1.598(14) . ?
O11 C111 1.436(6) . ?
C111 C112 1.491(10) . ?
C112 O12 1.211(6) . ?
C112 C113 1.490(8) . ?
C113 C114 1.356(11) . ?
C113 C118 1.391(9) . ?
C114 C115 1.375(11) . ?
C115 C116 1.332(14) . ?
C116 C117 1.382(15) . ?
C117 C118 1.378(11) . ?
C12' C22 1.528(6) . ?
C21 O21 1.373(7) . ?
C21 C22 1.398(8) . ?
C21 C26 1.407(6) . ?
C22 C23 1.365(9) . ?
C23 C24 1.411(7) . ?
C24 C25 1.410(9) . ?
C24 C27 1.499(10) . ?
C25 C26 1.361(9) . ?
C26 C23' 1.542(8) . ?
C27 C210 1.483(14) . ?
C27 C28 1.541(9) . ?
C27 C29 1.548(9) . ?
C211 O21 1.454(8) . ?
C211 C212 1.491(10) . ?
C212 O22 1.216(6) . ?
C212 C213 1.499(11) . ?
C213 C218 1.355(8) . ?
C213 C214 1.375(13) . ?
C214 C217 1.448(16) . ?
C215 C216 1.333(19) . ?
C215 C218 1.362(15) . ?
C216 C217 1.366(15) . ?
C23' C32 1.541(7) . ?
C31 C32 1.384(6) . ?
C31 C36 1.394(7) . ?
C31 O31 1.400(7) . ?
C32 C33 1.380(8) . ?
C33 C34 1.379(7) . ?
C34 C35 1.385(7) . ?
C34 C37 1.564(8) . ?
C35 C36 1.392(8) . ?
C36 C34' 1.523(6) . ?
C37 C38 1.465(11) . ?
C37 C310 1.527(14) . ?
C37 C39 1.561(12) . ?
O31 C311 1.453(8) . ?
C311 C312 1.499(9) . ?
C312 O32 1.235(6) . ?
C312 C313 1.452(9) . ?
C313 C314 1.373(9) . ?
C313 C318 1.379(10) . ?
C314 C317 1.350(13) . ?
C315 C316 1.374(13) . ?
C315 C318 1.387(14) . ?
C316 C317 1.283(13) . ?
C34' C42 1.514(8) . ?
C41 C46 1.392(8) . ?
C41 C42 1.399(7) . ?
C41 O41 1.401(7) . ?
C42 C43 1.408(9) . ?
C43 C44 1.364(9) . ?
C44 C45 1.403(7) . ?
C44 C47 1.526(11) . ?
C45 C46 1.373(9) . ?
C46 C41' 1.548(6) . ?
C47 C410 1.510(10) . ?
C47 C49 1.542(10) . ?
C47 C48 1.563(15) . ?
O41 C411 1.404(7) . ?
C411 C412 1.514(9) . ?
C412 O42 1.219(5) . ?
C412 C413 1.458(9) . ?
C413 C414 1.366(10) . ?
C413 C418 1.401(8) . ?
C414 C415 1.391(11) . ?
C415 C416 1.373(12) . ?
C416 C417 1.370(14) . ?
C417 C418 1.345(12) . ?
Cl O4 1.308(8) . ?
Cl O3 1.326(8) . ?
Cl O2 1.361(8) . ?
Cl O1 1.385(5) . ?
C1 C2 1.370(17) . ?
C2 N 1.143(17) . ?
C3 C4 1.73(5) . ?
C4 O5 1.37(2) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 C16 C12' C22 -77.1(6) . . . . ?
C25 C26 C23' C32 -84.4(5) . . . . ?
C35 C36 C34' C42 -80.3(6) . . . . ?
C45 C36 C41' C12 -104.2(4) . . . . ?
C12 C11 O11 C111 -85.0(5) . . . . ?
C11 O11 C111 C112 -146.8(4) . . . . ?
O11 C111 C112 O12 -2.2(7) . . . . ?
C111 C112 O12 C113 -177.9(8) . . . . ?
C112 O12 C113 C114 179.6(7) . . . . ?
C22 C21 O21 C211 -90.2(5) . . . . ?
C21 O21 C211 C212 -158.5(4) . . . . ?
O21 C211 C212 O22 0.0(7) . . . . ?
C211 C212 O22 C213 177.7(8) . . . . ?
C212 O22 C213 C214 -174.3(7) . . . . ?
C32 C31 O31 C311 -93.7(5) . . . . ?
C31 O31 C311 C312 -141.6(4) . . . . ?
O31 C311 C312 O32 -5.4(7) . . . . ?
C311 C312 O32 C313 177.0(9) . . . . ?
C312 O32 C313 C314 -164.6(8) . . . . ?
C42 C41 O41 C411 -82.8(5) . . . . ?
C41 O41 C411 C412 -162.8(4) . . . . ?
O41 C411 C412 O42 14.4(7) . . . . ?
C411 C412 O42 C413 177.2(9) . . . . ?
C412 O42 C413 C414 -177.6(8) . . . . ?
