 
data_04skc0011p-18
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
Tetra(tetraethylbutylammonium bromide) di(DL-tartaric acid)
tetrahydrate
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C20 H50 Br2 N2 O8'
_chemical_formula_weight          606.44
 
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'
 'Br'  'Br'  -0.2901   2.4595
 '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                    13.912(2)
_cell_length_b                    14.2967(7)
_cell_length_c                    16.456(2)
_cell_angle_alpha                 64.325(8)
_cell_angle_beta                  78.777(9)
_cell_angle_gamma                 89.720(7)
_cell_volume                      2881.6(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     13192
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.398
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1272
_exptl_absorpt_coefficient_mu     2.854
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7634
_exptl_absorpt_correction_T_max   0.9193
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             64930
_diffrn_reflns_av_R_equivalents   0.0756
_diffrn_reflns_av_sigmaI/netI     0.0673
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          3.00
_diffrn_reflns_theta_max          27.48
_reflns_number_total              13207
_reflns_number_gt                 9166
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'  
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0384P)²+4.5286P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          13207
_refine_ls_number_parameters      704
_refine_ls_number_restraints      17
_refine_ls_R_factor_all           0.0859
_refine_ls_R_factor_gt            0.0488
_refine_ls_wR_factor_ref          0.1111
_refine_ls_wR_factor_gt           0.0976
_refine_ls_goodness_of_fit_ref    1.012
_refine_ls_restrained_S_all       1.012
_refine_ls_shift/su_max           0.007
_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
Br01 Br 0.13338(3) 0.36050(3) 0.74282(3) 0.02951(10) Uani 1 1 d . . .
Br02 Br 0.77457(3) 0.41554(3) 0.73107(3) 0.03133(10) Uani 1 1 d . . .
Br03 Br 0.60250(3) -0.07585(3) 0.71625(3) 0.03074(10) Uani 1 1 d . . .
Br04 Br 0.23429(3) -0.14290(3) 0.76952(3) 0.03663(11) Uani 1 1 d . . .
C1 C 0.4941(2) 0.5064(3) 0.7648(2) 0.0206(7) Uani 1 1 d . . .
C2 C 0.5028(2) 0.4166(3) 0.7389(2) 0.0196(7) Uani 1 1 d . . .
H2 H 0.5469 0.4415 0.6764 0.024 Uiso 1 1 calc R . .
C3 C 0.4023(2) 0.3785(3) 0.7351(2) 0.0209(7) Uani 1 1 d . . .
H3 H 0.3776 0.4366 0.6851 0.025 Uiso 1 1 calc R . .
C4 C 0.4143(2) 0.2890(3) 0.7096(2) 0.0213(7) Uani 1 1 d . . .
O1A O 0.51552(19) 0.5067(2) 0.83167(18) 0.0291(6) Uani 1 1 d . . .
O1B O 0.46151(19) 0.58746(18) 0.70056(17) 0.0267(6) Uani 1 1 d . . .
H1 H 0.4560 0.6363 0.7161 0.044(13) Uiso 1 1 calc R . .
O2 O 0.54279(17) 0.33194(18) 0.80223(17) 0.0254(6) Uani 1 1 d . . .
H2A H 0.6029 0.3475 0.7957 0.038 Uiso 1 1 calc R . .
O3 O 0.33639(17) 0.3548(2) 0.81955(18) 0.0284(6) Uani 1 1 d . . .
H3A H 0.2785 0.3474 0.8139 0.043 Uiso 1 1 calc R . .
O4A O 0.37559(19) 0.19807(19) 0.77606(17) 0.0282(6) Uani 1 1 d . . .
H4 H 0.3898 0.1514 0.7589 0.049(14) Uiso 1 1 calc R . .
O4B O 0.45572(19) 0.3033(2) 0.63289(18) 0.0322(6) Uani 1 1 d . . .
C21 C 0.7041(3) 0.5743(3) 0.9122(3) 0.0299(9) Uani 1 1 d . . .
H21A H 0.6901 0.5374 0.8763 0.036 Uiso 1 1 calc R . .
H21B H 0.7547 0.6327 0.8711 0.036 Uiso 1 1 calc R . .
C22 C 0.7649(3) 0.5501(3) 1.0518(3) 0.0292(8) Uani 1 1 d . . .
H22A H 0.7956 0.5002 1.1011 0.035 Uiso 1 1 calc R . .
H22B H 0.7009 0.5633 1.0818 0.035 Uiso 1 1 calc R . .
C23 C 0.8408(3) 0.4708(3) 0.9484(3) 0.0333(9) Uani 1 1 d . . .
H23A H 0.8247 0.4370 0.9108 0.040 Uiso 1 1 calc R . .
H23B H 0.8839 0.5353 0.9062 0.040 Uiso 1 1 calc R . .
C24 C 0.6751(3) 0.4038(3) 1.0540(3) 0.0270(8) Uani 1 1 d . . .
H24A H 0.7047 0.3589 1.1063 0.032 Uiso 1 1 calc R . .
H24B H 0.6139 0.4260 1.0797 0.032 Uiso 1 1 calc R . .
C25 C 0.6115(3) 0.6188(3) 0.9389(3) 0.0328(9) Uani 1 1 d . . .
H25A H 0.5597 0.5621 0.9773 0.049 Uiso 1 1 calc R . .
H25B H 0.5901 0.6667 0.8832 0.049 Uiso 1 1 calc R . .
H25C H 0.6245 0.6565 0.9737 0.049 Uiso 1 1 calc R . .
C26 C 0.8303(3) 0.6515(3) 1.0015(3) 0.0311(9) Uani 1 1 d . . .
H26A H 0.8891 0.6427 0.9626 0.047 Uiso 1 1 calc R . .
H26B H 0.8498 0.6710 1.0466 0.047 Uiso 1 1 calc R . .
H26C H 0.7942 0.7064 0.9629 0.047 Uiso 1 1 calc R . .
C27 C 0.8970(3) 0.3988(3) 1.0167(4) 0.0516(13) Uani 1 1 d . . .
H27A H 0.9141 0.4318 1.0539 0.077 Uiso 1 1 calc R . .
H27B H 0.9573 0.3845 0.9835 0.077 Uiso 1 1 calc R . .
H27C H 0.8562 0.3333 1.0572 0.077 Uiso 1 1 calc R . .
C28 C 0.6485(3) 0.3397(3) 1.0078(3) 0.0349(9) Uani 1 1 d . . .
H28A H 0.6146 0.3816 0.9587 0.052 Uiso 1 1 calc R . .
H28B H 0.6051 0.2781 1.0535 0.052 Uiso 1 1 calc R . .
H28C H 0.7085 0.3177 0.9813 0.052 Uiso 1 1 calc R . .
N21 N 0.7461(2) 0.5002(2) 0.99182(19) 0.0203(6) Uani 1 1 d . . .
C31 C 0.8666(3) 0.0014(3) 0.7589(3) 0.0224(8) Uani 1 1 d . . .
C32 C 0.8738(2) -0.0872(3) 0.7313(2) 0.0198(7) Uani 1 1 d . . .
H32 H 0.8646 -0.0604 0.6665 0.024 Uiso 1 1 calc R . .
C33 C 0.9748(3) -0.1291(3) 0.7359(2) 0.0218(7) Uani 1 1 d . . .
H33 H 1.0254 -0.0718 0.6899 0.026 Uiso 1 1 calc R . .
C34 C 0.9790(2) -0.2169(3) 0.7078(3) 0.0230(8) Uani 1 1 d . . .
O31A O 0.8088(2) 0.0007(2) 0.82353(18) 0.0328(6) Uani 1 1 d . . .
O31B O 0.93128(19) 0.08188(19) 0.70014(18) 0.0299(6) Uani 1 1 d . . .
H31 H 0.9285 0.1284 0.7185 0.072(18) Uiso 1 1 calc R . .
O32 O 0.80169(17) -0.16969(18) 0.78898(18) 0.0273(6) Uani 1 1 d . . .
H32A H 0.7459 -0.1504 0.7806 0.041 Uiso 1 1 calc R . .
O33 O 0.99289(18) -0.1562(2) 0.82428(18) 0.0282(6) Uani 1 1 d . . .
H33A H 1.0534 -0.1607 0.8225 0.042 Uiso 1 1 calc R . .
O34A O 0.98273(19) -0.2001(2) 0.62832(18) 0.0313(6) Uani 1 1 d . . .
O34B O 0.97879(19) -0.31046(19) 0.77525(18) 0.0285(6) Uani 1 1 d . . .
H34 H 0.9789 -0.3551 0.7548 0.052(15) Uiso 1 1 calc R . .
C41 C 0.8212(3) 0.8697(3) 0.4127(2) 0.0272(8) Uani 1 1 d . . .
H41A H 0.8889 0.8710 0.4229 0.033 Uiso 1 1 calc R . .
H41B H 0.7939 0.9347 0.4105 0.033 Uiso 1 1 calc R . .
C42 C 0.7694(3) 0.7904(3) 0.5792(2) 0.0291(8) Uani 1 1 d . . .
H42A H 0.8400 0.7940 0.5809 0.035 Uiso 1 1 calc R . .
H42B H 0.7446 0.8574 0.5739 0.035 Uiso 1 1 calc R . .
C43 C 0.7971(4) 0.6767(3) 0.4983(3) 0.0463(12) Uani 1 1 d . . .
H43A H 0.7570 0.6185 0.5535 0.056 Uiso 1 1 calc R . .
H43B H 0.7862 0.6697 0.4435 0.056 Uiso 1 1 calc R . .
C44 C 0.6535(3) 0.7771(4) 0.4860(3) 0.0517(13) Uani 1 1 d . . .
H44A H 0.6165 0.7147 0.5392 0.062 Uiso 1 1 calc R . .
H44B H 0.6502 0.7701 0.4293 0.062 Uiso 1 1 calc R . .
C45 C 0.8263(3) 0.8694(3) 0.3202(3) 0.0333(9) Uani 1 1 d . . .
H45A H 0.8566 0.8073 0.3202 0.050 Uiso 1 1 calc R . .
H45B H 0.8660 0.9320 0.2714 0.050 Uiso 1 1 calc R . .
H45C H 0.7597 0.8686 0.3090 0.050 Uiso 1 1 calc R . .
C46 C 0.7148(3) 0.7041(3) 0.6693(3) 0.0389(10) Uani 1 1 d . . .
H46A H 0.6447 0.6997 0.6687 0.058 Uiso 1 1 calc R . .
H46B H 0.7232 0.7189 0.7205 0.058 Uiso 1 1 calc R . .
H46C H 0.7412 0.6377 0.6772 0.058 Uiso 1 1 calc R . .
C47 C 0.9039(4) 0.6656(4) 0.5023(3) 0.0590(15) Uani 1 1 d . . .
H47A H 0.9447 0.7208 0.4466 0.089 Uiso 1 1 calc R . .
H47B H 0.9209 0.5974 0.5061 0.089 Uiso 1 1 calc R . .
H47C H 0.9156 0.6714 0.5568 0.089 Uiso 1 1 calc R . .
C48 C 0.6026(3) 0.8723(5) 0.4829(4) 0.0628(16) Uani 1 1 d . . .
H48A H 0.6019 0.8781 0.5401 0.094 Uiso 1 1 calc R . .
H48B H 0.5348 0.8654 0.4762 0.094 Uiso 1 1 calc R . .
H48C H 0.6381 0.9349 0.4302 0.094 Uiso 1 1 calc R . .
N41 N 0.7601(2) 0.7784(2) 0.4939(2) 0.0257(7) Uani 1 1 d . . .
C61A C 0.5506(5) -0.0931(5) 1.0479(5) 0.0212(15) Uani 0.50 1 d PD . .
H61A H 0.5019 -0.1427 1.1020 0.025 Uiso 0.50 1 calc PR . .
H61B H 0.6016 -0.0711 1.0720 0.025 Uiso 0.50 1 calc PR . .
C62A C 0.5991(19) -0.1523(16) 0.9976(15) 0.032(5) Uani 0.50 1 d PD . .
H62A H 0.5521 -0.1701 0.9681 0.049 Uiso 0.50 1 calc PR . .
H62B H 0.6209 -0.2163 1.0414 0.049 Uiso 0.50 1 calc PR . .
H62C H 0.6560 -0.1092 0.9504 0.049 Uiso 0.50 1 calc PR . .
C63A C 0.5682(5) 0.0799(5) 0.9087(5) 0.0236(15) Uani 0.50 1 d PD . .
H63A H 0.5924 0.0452 0.8690 0.028 Uiso 0.50 1 calc PR . .
H63B H 0.5302 0.1375 0.8749 0.028 Uiso 0.50 1 calc PR . .
C64A C 0.6540(10) 0.1231(13) 0.9284(9) 0.028(3) Uani 0.50 1 d PD . .
H64A H 0.6304 0.1465 0.9761 0.042 Uiso 0.50 1 calc PR . .
H64B H 0.6888 0.1822 0.8719 0.042 Uiso 0.50 1 calc PR . .
H64C H 0.6989 0.0689 0.9501 0.042 Uiso 0.50 1 calc PR . .
C61B C 0.5435(6) -0.0457(5) 0.9394(5) 0.0255(16) Uani 0.50 1 d PD . .
H61C H 0.5956 0.0058 0.8905 0.031 Uiso 0.50 1 calc PR . .
H61D H 0.4921 -0.0550 0.9089 0.031 Uiso 0.50 1 calc PR . .
C62B C 0.5872(16) -0.1470(13) 0.9799(14) 0.027(4) Uani 0.50 1 d PD . .
H62D H 0.6310 -0.1435 1.0187 0.041 Uiso 0.50 1 calc PR . .
H62E H 0.6248 -0.1611 0.9301 0.041 Uiso 0.50 1 calc PR . .
H62F H 0.5345 -0.2030 1.0175 0.041 Uiso 0.50 1 calc PR . .
C63B C 0.5845(5) 0.0340(6) 1.0378(5) 0.0280(17) Uani 0.50 1 d PD . .
H63C H 0.5539 0.0632 1.0804 0.034 Uiso 0.50 1 calc PR . .
H63D H 0.6157 -0.0287 1.0737 0.034 Uiso 0.50 1 calc PR . .
C64B C 0.6631(11) 0.1133(13) 0.9631(8) 0.038(4) Uani 0.50 1 d PD . .
H64D H 0.6931 0.0856 0.9200 0.056 Uiso 0.50 1 calc PR . .
H64E H 0.7136 0.1281 0.9910 0.056 Uiso 0.50 1 calc PR . .
H64F H 0.6336 0.1776 0.9298 0.056 Uiso 0.50 1 calc PR . .
N61 N 0.5000 0.0000 1.0000 0.0227(9) Uani 1 2 d S . .
C71A C 0.0359(5) -0.1015(5) 1.0740(5) 0.0234(15) Uani 0.50 1 d PD . .
H71A H 0.0912 -0.0797 1.0937 0.028 Uiso 0.50 1 calc PR . .
H71B H -0.0185 -0.1342 1.1289 0.028 Uiso 0.50 1 calc PR . .
C72A C 0.0691(9) -0.1830(9) 1.0412(8) 0.040(2) Uani 0.50 1 d PD . .
H72A H 0.0148 -0.2063 1.0224 0.060 Uiso 0.50 1 calc PR . .
H72B H 0.0888 -0.2425 1.0915 0.060 Uiso 0.50 1 calc PR . .
H72C H 0.1251 -0.1527 0.9886 0.060 Uiso 0.50 1 calc PR . .
C73A C 0.0793(6) 0.0529(6) 0.9200(5) 0.0342(19) Uani 0.50 1 d PD . .
H73A H 0.0540 0.1144 0.8749 0.041 Uiso 0.50 1 calc PR . .
H73B H 0.0964 0.0054 0.8910 0.041 Uiso 0.50 1 calc PR . .
C74A C 0.1724(8) 0.0891(10) 0.9354(10) 0.040(2) Uani 0.50 1 d PD . .
H74A H 0.1559 0.1199 0.9786 0.060 Uiso 0.50 1 calc PR . .
H74B H 0.2111 0.1413 0.8765 0.060 Uiso 0.50 1 calc PR . .
H74C H 0.2108 0.0296 0.9611 0.060 Uiso 0.50 1 calc PR . .
C71B C 0.0373(6) -0.0595(5) 0.9475(5) 0.0283(17) Uani 0.50 1 d PD . .
H71C H 0.0903 -0.0160 0.8943 0.034 Uiso 0.50 1 calc PR . .
H71D H -0.0166 -0.0765 0.9233 0.034 Uiso 0.50 1 calc PR . .
C72B C 0.0769(8) -0.1602(8) 1.0082(8) 0.035(2) Uani 0.50 1 d PD . .
H72D H 0.1296 -0.1436 1.0329 0.053 Uiso 0.50 1 calc PR . .
H72E H 0.1028 -0.1968 0.9713 0.053 Uiso 0.50 1 calc PR . .
H72F H 0.0236 -0.2048 1.0593 0.053 Uiso 0.50 1 calc PR . .
C73B C 0.0831(5) 0.0392(6) 1.0294(5) 0.0305(18) Uani 0.50 1 d PD . .
H73C H 0.0543 0.0796 1.0627 0.037 Uiso 0.50 1 calc PR . .
H73D H 0.1090 -0.0222 1.0739 0.037 Uiso 0.50 1 calc PR . .
C74B C 0.1671(8) 0.1047(10) 0.9558(10) 0.035(2) Uani 0.50 1 d PD . .
H74D H 0.1921 0.0697 0.9173 0.053 Uiso 0.50 1 calc PR . .
H74E H 0.2194 0.1158 0.9837 0.053 Uiso 0.50 1 calc PR . .
H74F H 0.1454 0.1721 0.9176 0.053 Uiso 0.50 1 calc PR . .
N71 N 0.0000 0.0000 1.0000 0.0236(9) Uani 1 2 d S . .
C81 C 0.6497(3) 0.3520(3) 0.4875(3) 0.0366(10) Uani 1 1 d . . .
H81A H 0.6267 0.3709 0.4295 0.044 Uiso 1 1 calc R . .
H81B H 0.5944 0.3110 0.5395 0.044 Uiso 1 1 calc R . .
C82 C 0.6928(3) 0.1872(3) 0.4897(3) 0.0407(10) Uani 1 1 d . . .
H82A H 0.6623 0.2079 0.4355 0.049 Uiso 1 1 calc R . .
H82B H 0.6403 0.1516 0.5459 0.049 Uiso 1 1 calc R . .
C83 C 0.8160(3) 0.3409(3) 0.4044(3) 0.0380(10) Uani 1 1 d . . .
H83A H 0.8736 0.2995 0.4093 0.046 Uiso 1 1 calc R . .
H83B H 0.8365 0.4079 0.4031 0.046 Uiso 1 1 calc R . .
C84 C 0.7778(3) 0.2608(3) 0.5713(3) 0.0412(10) Uani 1 1 d . . .
H84A H 0.8046 0.3274 0.5665 0.049 Uiso 1 1 calc R . .
H84B H 0.8332 0.2172 0.5707 0.049 Uiso 1 1 calc R . .
C85 C 0.6754(3) 0.4506(3) 0.4940(3) 0.0376(10) Uani 1 1 d . . .
H85A H 0.6967 0.4328 0.5519 0.056 Uiso 1 1 calc R . .
H85B H 0.6174 0.4901 0.4925 0.056 Uiso 1 1 calc R . .
H85C H 0.7286 0.4930 0.4418 0.056 Uiso 1 1 calc R . .
C86 C 0.7706(4) 0.1100(3) 0.4868(3) 0.0592(15) Uani 1 1 d . . .
H86A H 0.8168 0.1406 0.4268 0.089 Uiso 1 1 calc R . .
H86B H 0.7375 0.0448 0.4958 0.089 Uiso 1 1 calc R . .
H86C H 0.8065 0.0957 0.5360 0.089 Uiso 1 1 calc R . .
C87 C 0.7864(3) 0.3635(3) 0.3137(3) 0.0303(9) Uani 1 1 d . . .
H87A H 0.7648 0.2979 0.3145 0.046 Uiso 1 1 calc R . .
H87B H 0.8429 0.3982 0.2624 0.046 Uiso 1 1 calc R . .
H87C H 0.7325 0.4088 0.3059 0.046 Uiso 1 1 calc R . .
C88 C 0.7024(3) 0.2042(3) 0.6650(3) 0.0328(9) Uani 1 1 d . . .
H88A H 0.6500 0.2492 0.6683 0.049 Uiso 1 1 calc R . .
H88B H 0.7360 0.1886 0.7159 0.049 Uiso 1 1 calc R . .
H88C H 0.6739 0.1391 0.6695 0.049 Uiso 1 1 calc R . .
N81 N 0.7355(2) 0.2828(2) 0.4896(2) 0.0225(6) Uani 1 1 d . . .
O1W O 0.4006(2) 0.0329(2) 0.7501(3) 0.0557(10) Uani 1 1 d D . .
H1W H 0.4540(16) 0.010(3) 0.738(3) 0.038(13) Uiso 1 1 d D . .
H2W H 0.356(2) -0.009(3) 0.755(4) 0.062(16) Uiso 1 1 d D . .
O2W O 0.4391(2) -0.2428(2) 0.7201(3) 0.0449(8) Uani 1 1 d D . .
H21W H 0.385(2) -0.222(5) 0.734(5) 0.11(3) Uiso 1 1 d D . .
H22W H 0.483(3) -0.204(3) 0.721(4) 0.069(17) Uiso 1 1 d D . .
O3W O 0.9335(2) 0.2448(3) 0.7327(3) 0.0583(10) Uani 1 1 d D . .
H31W H 0.983(2) 0.271(4) 0.739(4) 0.072(18) Uiso 1 1 d D . .
H32W H 0.887(3) 0.281(4) 0.738(4) 0.09(2) Uiso 1 1 d D . .
O4W O 0.9740(3) 0.5350(2) 0.7321(3) 0.0411(8) Uani 1 1 d . . .
H41W H 1.008(4) 0.497(4) 0.739(3) 0.048(17) Uiso 1 1 d . . .
H42W H 0.919(5) 0.506(5) 0.731(4) 0.09(2) Uiso 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
C1 O1A 1.197(4) . ?
C1 O1B 1.336(4) . ?
C1 C2 1.515(5) . ?
C2 O2 1.410(4) . ?
C2 C3 1.526(4) . ?
C2 H2 1.0000 . ?
C3 O3 1.409(4) . ?
C3 C4 1.508(5) . ?
C3 H3 1.0000 . ?
C4 O4B 1.209(4) . ?
C4 O4A 1.312(4) . ?
O1B H1 0.8400 . ?
O2 H2A 0.8400 . ?
O3 H3A 0.8400 . ?
O4A H4 0.8400 . ?
C21 N21 1.507(5) . ?
C21 C25 1.507(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N21 1.505(4) . ?
C22 C26 1.514(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C27 1.505(6) . ?
C23 N21 1.521(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C28 1.506(5) . ?
C24 N21 1.523(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C31 O31A 1.198(4) . ?
C31 O31B 1.333(4) . ?
C31 C32 1.517(5) . ?
C32 O32 1.403(4) . ?
C32 C33 1.528(5) . ?
C32 H32 1.0000 . ?
C33 O33 1.408(4) . ?
C33 C34 1.511(5) . ?
C33 H33 1.0000 . ?
C34 O34A 1.213(4) . ?
C34 O34B 1.317(4) . ?
O31B H31 0.8400 . ?
O32 H32A 0.8400 . ?
O33 H33A 0.8400 . ?
O34B H34 0.8400 . ?
C41 N41 1.507(4) . ?
C41 C45 1.513(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C46 1.511(5) . ?
C42 N41 1.514(4) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C47 1.505(7) . ?
C43 N41 1.516(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 N41 1.515(5) . ?
C44 C48 1.517(7) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C61A N61 1.478(6) . ?
C61A C62A 1.496(16) . ?
C61A H61A 0.9900 . ?
C61A H61B 0.9900 . ?
C62A H62A 0.9800 . ?
C62A H62B 0.9800 . ?
C62A H62C 0.9800 . ?
C63A C64A 1.497(12) . ?
C63A N61 1.559(6) . ?
C63A H63A 0.9900 . ?
C63A H63B 0.9900 . ?
C64A H64A 0.9800 . ?
C64A H64B 0.9800 . ?
C64A H64C 0.9800 . ?
C61B N61 1.453(7) . ?
C61B C62B 1.492(15) . ?
C61B H61C 0.9900 . ?
C61B H61D 0.9900 . ?
C62B H62D 0.9800 . ?
C62B H62E 0.9800 . ?
C62B H62F 0.9800 . ?
C63B C64B 1.508(13) . ?
C63B N61 1.599(7) . ?
C63B H63C 0.9900 . ?
C63B H63D 0.9900 . ?
C64B H64D 0.9800 . ?
C64B H64E 0.9800 . ?
C64B H64F 0.9800 . ?
N61 C61B 1.453(7) 2_657 ?
N61 C61A 1.478(6) 2_657 ?
N61 C63A 1.559(6) 2_657 ?
N61 C63B 1.599(7) 2_657 ?
C71A C72A 1.518(13) . ?
C71A N71 1.592(7) . ?
C71A H71A 0.9900 . ?
C71A H71B 0.9900 . ?
C72A H72A 0.9800 . ?
C72A H72B 0.9800 . ?
C72A H72C 0.9800 . ?
C73A N71 1.450(7) . ?
C73A C74A 1.503(12) . ?
C73A H73A 0.9900 . ?
C73A H73B 0.9900 . ?
C74A H74A 0.9800 . ?
C74A H74B 0.9800 . ?
C74A H74C 0.9800 . ?
C71B N71 1.482(7) . ?
C71B C72B 1.528(11) . ?
C71B H71C 0.9900 . ?
C71B H71D 0.9900 . ?
C72B H72D 0.9800 . ?
C72B H72E 0.9800 . ?
C72B H72F 0.9800 . ?
C73B C74B 1.479(13) . ?
C73B N71 1.531(7) . ?
C73B H73C 0.9900 . ?
C73B H73D 0.9900 . ?
C74B H74D 0.9800 . ?
C74B H74E 0.9800 . ?
C74B H74F 0.9800 . ?
N71 C73A 1.450(7) 2_557 ?
N71 C71B 1.482(7) 2_557 ?
N71 C73B 1.531(7) 2_557 ?
N71 C71A 1.592(7) 2_557 ?
C81 C85 1.509(6) . ?
C81 N81 1.544(5) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 N81 1.492(5) . ?
C82 C86 1.551(7) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 N81 1.516(5) . ?
C83 C87 1.524(6) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C84 N81 1.479(5) . ?
C84 C88 1.559(6) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
O1W H1W 0.832(18) . ?
O1W H2W 0.831(18) . ?
O2W H21W 0.833(19) . ?
O2W H22W 0.840(19) . ?
O3W H31W 0.829(19) . ?
O3W H32W 0.838(19) . ?
O4W H41W 0.71(5) . ?
O4W H42W 0.88(7) . ?
 
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
O1A C1 O1B 124.2(3) . . ?
O1A C1 C2 125.5(3) . . ?
O1B C1 C2 110.3(3) . . ?
O2 C2 C1 111.8(3) . . ?
O2 C2 C3 108.4(3) . . ?
C1 C2 C3 110.7(3) . . ?
O2 C2 H2 108.6 . . ?
C1 C2 H2 108.6 . . ?
C3 C2 H2 108.6 . . ?
O3 C3 C4 114.7(3) . . ?
O3 C3 C2 108.9(3) . . ?
C4 C3 C2 108.9(3) . . ?
O3 C3 H3 108.1 . . ?
C4 C3 H3 108.1 . . ?
C2 C3 H3 108.1 . . ?
O4B C4 O4A 124.5(3) . . ?
O4B C4 C3 120.8(3) . . ?
O4A C4 C3 114.7(3) . . ?
C1 O1B H1 109.5 . . ?
C2 O2 H2A 109.5 . . ?
C3 O3 H3A 109.5 . . ?
C4 O4A H4 109.5 . . ?
N21 C21 C25 115.0(3) . . ?
N21 C21 H21A 108.5 . . ?
C25 C21 H21A 108.5 . . ?
N21 C21 H21B 108.5 . . ?
C25 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
N21 C22 C26 114.9(3) . . ?
N21 C22 H22A 108.5 . . ?
C26 C22 H22A 108.5 . . ?
N21 C22 H22B 108.5 . . ?
C26 C22 H22B 108.5 . . ?
H22A C22 H22B 107.5 . . ?
C27 C23 N21 114.3(3) . . ?
C27 C23 H23A 108.7 . . ?
N21 C23 H23A 108.7 . . ?
C27 C23 H23B 108.7 . . ?
N21 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
C28 C24 N21 115.3(3) . . ?
C28 C24 H24A 108.5 . . ?
N21 C24 H24A 108.5 . . ?
C28 C24 H24B 108.5 . . ?
N21 C24 H24B 108.5 . . ?
H24A C24 H24B 107.5 . . ?
C21 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C21 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C22 N21 C21 111.3(3) . . ?
C22 N21 C23 111.5(3) . . ?
C21 N21 C23 105.6(3) . . ?
C22 N21 C24 106.5(3) . . ?
C21 N21 C24 111.4(3) . . ?
C23 N21 C24 110.7(3) . . ?
O31A C31 O31B 124.2(3) . . ?
O31A C31 C32 124.7(3) . . ?
O31B C31 C32 111.1(3) . . ?
O32 C32 C31 111.7(3) . . ?
O32 C32 C33 108.4(3) . . ?
C31 C32 C33 110.5(3) . . ?
O32 C32 H32 108.7 . . ?
C31 C32 H32 108.7 . . ?
C33 C32 H32 108.7 . . ?
O33 C33 C34 114.8(3) . . ?
O33 C33 C32 109.1(3) . . ?
C34 C33 C32 108.8(3) . . ?
O33 C33 H33 108.0 . . ?
C34 C33 H33 108.0 . . ?
C32 C33 H33 108.0 . . ?
O34A C34 O34B 123.8(3) . . ?
O34A C34 C33 121.2(3) . . ?
O34B C34 C33 115.0(3) . . ?
C31 O31B H31 109.5 . . ?
C32 O32 H32A 109.5 . . ?
C33 O33 H33A 109.5 . . ?
C34 O34B H34 109.5 . . ?
N41 C41 C45 114.9(3) . . ?
N41 C41 H41A 108.5 . . ?
C45 C41 H41A 108.5 . . ?
N41 C41 H41B 108.5 . . ?
C45 C41 H41B 108.5 . . ?
H41A C41 H41B 107.5 . . ?
C46 C42 N41 114.8(3) . . ?
C46 C42 H42A 108.6 . . ?
N41 C42 H42A 108.6 . . ?
C46 C42 H42B 108.6 . . ?
N41 C42 H42B 108.6 . . ?
H42A C42 H42B 107.5 . . ?
C47 C43 N41 115.1(4) . . ?
C47 C43 H43A 108.5 . . ?
N41 C43 H43A 108.5 . . ?
C47 C43 H43B 108.5 . . ?
N41 C43 H43B 108.5 . . ?
H43A C43 H43B 107.5 . . ?
N41 C44 C48 115.2(4) . . ?
N41 C44 H44A 108.5 . . ?
C48 C44 H44A 108.5 . . ?
N41 C44 H44B 108.5 . . ?
C48 C44 H44B 108.5 . . ?
H44A C44 H44B 107.5 . . ?
C41 C45 H45A 109.5 . . ?
C41 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C41 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C41 N41 C42 106.5(3) . . ?
C41 N41 C44 111.0(3) . . ?
C42 N41 C44 110.6(3) . . ?
C41 N41 C43 110.5(3) . . ?
C42 N41 C43 110.9(3) . . ?
C44 N41 C43 107.4(3) . . ?
N61 C61A C62A 120.4(9) . . ?
N61 C61A H61A 107.2 . . ?
C62A C61A H61A 107.2 . . ?
N61 C61A H61B 107.2 . . ?
C62A C61A H61B 107.2 . . ?
H61A C61A H61B 106.9 . . ?
C61A C62A H62A 109.5 . . ?
C61A C62A H62B 109.5 . . ?
H62A C62A H62B 109.5 . . ?
C61A C62A H62C 109.5 . . ?
H62A C62A H62C 109.5 . . ?
H62B C62A H62C 109.5 . . ?
C64A C63A N61 110.8(7) . . ?
C64A C63A H63A 109.5 . . ?
N61 C63A H63A 109.5 . . ?
C64A C63A H63B 109.5 . . ?
N61 C63A H63B 109.5 . . ?
H63A C63A H63B 108.1 . . ?
C63A C64A H64A 109.5 . . ?
C63A C64A H64B 109.5 . . ?
H64A C64A H64B 109.5 . . ?
C63A C64A H64C 109.5 . . ?
H64A C64A H64C 109.5 . . ?
H64B C64A H64C 109.5 . . ?
N61 C61B C62B 118.7(9) . . ?
N61 C61B H61C 107.6 . . ?
C62B C61B H61C 107.6 . . ?
N61 C61B H61D 107.6 . . ?
C62B C61B H61D 107.6 . . ?
H61C C61B H61D 107.1 . . ?
C61B C62B H62D 109.5 . . ?
C61B C62B H62E 109.5 . . ?
H62D C62B H62E 109.5 . . ?
C61B C62B H62F 109.5 . . ?
H62D C62B H62F 109.5 . . ?
H62E C62B H62F 109.5 . . ?
C64B C63B N61 114.0(6) . . ?
C64B C63B H63C 108.8 . . ?
N61 C63B H63C 108.8 . . ?
C64B C63B H63D 108.8 . . ?
N61 C63B H63D 108.8 . . ?
H63C C63B H63D 107.7 . . ?
C63B C64B H64D 109.5 . . ?
C63B C64B H64E 109.5 . . ?
H64D C64B H64E 109.5 . . ?
C63B C64B H64F 109.5 . . ?
H64D C64B H64F 109.5 . . ?
H64E C64B H64F 109.5 . . ?
C61B N61 C61B 180.0(4) 2_657 . ?
C61B N61 C61A 112.2(4) 2_657 . ?
C61B N61 C61A 67.8(4) . . ?
C61B N61 C61A 67.8(4) 2_657 2_657 ?
C61B N61 C61A 112.2(4) . 2_657 ?
C61A N61 C61A 180.0(6) . 2_657 ?
C61B N61 C63A 113.3(4) 2_657 . ?
C61B N61 C63A 66.7(4) . . ?
C61A N61 C63A 111.4(4) . . ?
C61A N61 C63A 68.6(4) 2_657 . ?
C61B N61 C63A 66.7(4) 2_657 2_657 ?
C61B N61 C63A 113.3(4) . 2_657 ?
C61A N61 C63A 68.6(4) . 2_657 ?
C61A N61 C63A 111.4(4) 2_657 2_657 ?
C63A N61 C63A 180.000(1) . 2_657 ?
C61B N61 C63B 70.6(4) 2_657 . ?
C61B N61 C63B 109.4(4) . . ?
C61A N61 C63B 71.8(4) . . ?
C61A N61 C63B 108.2(4) 2_657 . ?
C63A N61 C63B 78.3(4) . . ?
C63A N61 C63B 101.7(4) 2_657 . ?
C61B N61 C63B 109.4(4) 2_657 2_657 ?
C61B N61 C63B 70.6(4) . 2_657 ?
C61A N61 C63B 108.2(4) . 2_657 ?
C61A N61 C63B 71.8(4) 2_657 2_657 ?
C63A N61 C63B 101.7(4) . 2_657 ?
C63A N61 C63B 78.3(4) 2_657 2_657 ?
C63B N61 C63B 180.0(5) . 2_657 ?
C72A C71A N71 115.5(6) . . ?
C72A C71A H71A 108.4 . . ?
N71 C71A H71A 108.4 . . ?
C72A C71A H71B 108.4 . . ?
N71 C71A H71B 108.4 . . ?
H71A C71A H71B 107.5 . . ?
C71A C72A H72A 109.5 . . ?
C71A C72A H72B 109.5 . . ?
H72A C72A H72B 109.5 . . ?
C71A C72A H72C 109.5 . . ?
H72A C72A H72C 109.5 . . ?
H72B C72A H72C 109.5 . . ?
N71 C73A C74A 117.4(7) . . ?
N71 C73A H73A 108.0 . . ?
C74A C73A H73A 108.0 . . ?
N71 C73A H73B 108.0 . . ?
C74A C73A H73B 108.0 . . ?
H73A C73A H73B 107.2 . . ?
C73A C74A H74A 109.5 . . ?
C73A C74A H74B 109.5 . . ?
H74A C74A H74B 109.5 . . ?
C73A C74A H74C 109.5 . . ?
H74A C74A H74C 109.5 . . ?
H74B C74A H74C 109.5 . . ?
N71 C71B C72B 111.3(7) . . ?
N71 C71B H71C 109.4 . . ?
C72B C71B H71C 109.4 . . ?
N71 C71B H71D 109.4 . . ?
C72B C71B H71D 109.4 . . ?
H71C C71B H71D 108.0 . . ?
C71B C72B H72D 109.5 . . ?
C71B C72B H72E 109.5 . . ?
H72D C72B H72E 109.5 . . ?
C71B C72B H72F 109.5 . . ?
H72D C72B H72F 109.5 . . ?
H72E C72B H72F 109.5 . . ?
C74B C73B N71 117.3(7) . . ?
C74B C73B H73C 108.0 . . ?
N71 C73B H73C 108.0 . . ?
C74B C73B H73D 108.0 . . ?
N71 C73B H73D 108.0 . . ?
H73C C73B H73D 107.2 . . ?
C73B C74B H74D 109.5 . . ?
C73B C74B H74E 109.5 . . ?
H74D C74B H74E 109.5 . . ?
C73B C74B H74F 109.5 . . ?
H74D C74B H74F 109.5 . . ?
H74E C74B H74F 109.5 . . ?
C73A N71 C73A 180.000(1) 2_557 . ?
C73A N71 C71B 116.2(4) 2_557 . ?
C73A N71 C71B 63.8(4) . . ?
C73A N71 C71B 63.8(4) 2_557 2_557 ?
C73A N71 C71B 116.2(4) . 2_557 ?
C71B N71 C71B 180.0(4) . 2_557 ?
C73A N71 C73B 108.8(4) 2_557 . ?
C73A N71 C73B 71.2(4) . . ?
C71B N71 C73B 111.5(4) . . ?
C71B N71 C73B 68.5(4) 2_557 . ?
C73A N71 C73B 71.2(4) 2_557 2_557 ?
C73A N71 C73B 108.8(4) . 2_557 ?
C71B N71 C73B 68.5(4) . 2_557 ?
C71B N71 C73B 111.5(4) 2_557 2_557 ?
C73B N71 C73B 180.0(5) . 2_557 ?
C73A N71 C71A 69.9(4) 2_557 . ?
C73A N71 C71A 110.1(4) . . ?
C71B N71 C71A 76.0(4) . . ?
C71B N71 C71A 104.0(4) 2_557 . ?
C73B N71 C71A 74.3(4) . . ?
C73B N71 C71A 105.7(4) 2_557 . ?
C73A N71 C71A 110.1(4) 2_557 2_557 ?
C73A N71 C71A 69.9(4) . 2_557 ?
C71B N71 C71A 104.0(4) . 2_557 ?
C71B N71 C71A 76.0(4) 2_557 2_557 ?
C73B N71 C71A 105.7(4) . 2_557 ?
C73B N71 C71A 74.3(4) 2_557 2_557 ?
C71A N71 C71A 180.0(5) . 2_557 ?
C85 C81 N81 114.2(3) . . ?
C85 C81 H81A 108.7 . . ?
N81 C81 H81A 108.7 . . ?
C85 C81 H81B 108.7 . . ?
N81 C81 H81B 108.7 . . ?
H81A C81 H81B 107.6 . . ?
N81 C82 C86 112.7(4) . . ?
N81 C82 H82A 109.0 . . ?
C86 C82 H82A 109.0 . . ?
N81 C82 H82B 109.0 . . ?
C86 C82 H82B 109.0 . . ?
H82A C82 H82B 107.8 . . ?
N81 C83 C87 114.4(3) . . ?
N81 C83 H83A 108.7 . . ?
C87 C83 H83A 108.7 . . ?
N81 C83 H83B 108.7 . . ?
C87 C83 H83B 108.7 . . ?
H83A C83 H83B 107.6 . . ?
N81 C84 C88 113.8(3) . . ?
N81 C84 H84A 108.8 . . ?
C88 C84 H84A 108.8 . . ?
N81 C84 H84B 108.8 . . ?
C88 C84 H84B 108.8 . . ?
H84A C84 H84B 107.7 . . ?
C81 C85 H85A 109.5 . . ?
C81 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C81 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C82 C86 H86A 109.5 . . ?
C82 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C82 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C83 C87 H87A 109.5 . . ?
C83 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
C83 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C84 C88 H88A 109.5 . . ?
C84 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C84 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C84 N81 C82 113.3(3) . . ?
C84 N81 C83 107.6(3) . . ?
C82 N81 C83 111.2(3) . . ?
C84 N81 C81 110.2(3) . . ?
C82 N81 C81 105.4(3) . . ?
C83 N81 C81 108.9(3) . . ?
H1W O1W H2W 108(3) . . ?
H21W O2W H22W 108(3) . . ?
H31W O3W H32W 107(3) . . ?
H41W O4W H42W 107(5) . . ?
 
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
O2 H2A Br02  0.84 2.43 3.248(2) 163.7 .
O3 H3A Br01  0.84 2.49 3.298(3) 161.1 .
O4A H4 O1W  0.84 1.77 2.587(4) 165.5 .
O31B H31 O3W  0.84 1.78 2.607(4) 167.9 .
O32 H32A Br03  0.84 2.46 3.282(2) 166.1 .
O1W H1W Br03  0.832(18) 2.45(2) 3.273(3) 174(4) .
O1W H2W Br04  0.831(18) 2.46(2) 3.292(3) 175(4) .
O2W H21W Br04  0.833(19) 2.47(2) 3.299(3) 174(5) .
O2W H22W Br03  0.840(19) 2.44(2) 3.276(3) 174(5) .
O3W H32W Br02  0.838(19) 2.45(2) 3.281(3) 169(5) .
O4W H42W Br02  0.88(7) 2.40(7) 3.272(3) 175(5) .
O1B H1 O2W  0.84 1.77 2.593(4) 165.3 1_565
O33 H33A Br04  0.84 2.47 3.287(3) 163.5 1_655
O3W H31W Br01  0.829(19) 2.48(2) 3.311(3) 175(5) 1_655
O4W H41W Br01  0.71(5) 2.60(5) 3.299(3) 172(5) 1_655
O34B H34 O4W  0.84 1.77 2.602(4) 170.1 1_545
 
_diffrn_measured_fraction_theta_max    0.999
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.999
_refine_diff_density_max    1.246
_refine_diff_density_min   -0.785
_refine_diff_density_rms    0.099
